# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a121228mor1_0m
_database_code_depnum_ccdc_archive 'CCDC 1023213'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H27 Br N2 O5 S2'
_chemical_formula_weight         603.54

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   11.3613(5)
_cell_length_b                   15.8902(6)
_cell_length_c                   29.9856(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5413.4(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173
_cell_measurement_reflns_used    8207
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.39
_exptl_crystal_description       Prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2480
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5473
_exptl_absorpt_correction_T_max  0.6275
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_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  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            28834
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6153
_reflns_number_gt                4935
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0476P)²+1.5748P] where P=(Fo²+2Fc²)/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         6153
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.006
_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
Br1 Br 0.69161(2) 1.031009(15) 0.524358(7) 0.02775(8) Uani 1 1 d . . .
S2 S 0.53486(5) 0.85139(3) 0.580255(17) 0.02302(12) Uani 1 1 d . . .
S3 S 0.52816(4) 0.99313(3) 0.645930(16) 0.01973(12) Uani 1 1 d . . .
N1 N 0.81313(14) 0.91876(11) 0.63782(5) 0.0189(4) Uani 1 1 d . . .
C9 C 0.72345(18) 0.94067(13) 0.60718(6) 0.0190(4) Uani 1 1 d . . .
C6 C 0.9847(2) 1.03411(14) 0.55730(7) 0.0270(5) Uani 1 1 d . . .
H6 H 0.9680 1.0654 0.5310 0.032 Uiso 1 1 calc R . .
C25 C 0.4553(2) 0.78253(13) 0.61481(7) 0.0255(5) Uani 1 1 d . . .
C20 C 0.5979(2) 1.14866(14) 0.61870(7) 0.0298(5) Uani 1 1 d . . .
H20 H 0.6574 1.1450 0.6409 0.036 Uiso 1 1 calc R . .
C5 C 1.0975(2) 1.02608(15) 0.57251(8) 0.0312(5) Uani 1 1 d . . .
H5 H 1.1596 1.0536 0.5571 0.037 Uiso 1 1 calc R . .
C19 C 0.42740(19) 1.08952(14) 0.58170(7) 0.0268(5) Uani 1 1 d . . .
H19 H 0.3715 1.0454 0.5786 0.032 Uiso 1 1 calc R . .
C8 C 0.77072(19) 0.98740(13) 0.57372(7) 0.0211(4) Uani 1 1 d . . .
C7 C 0.89401(18) 0.99497(13) 0.58146(7) 0.0210(4) Uani 1 1 d . . .
C11 C 0.84335(19) 0.88630(14) 0.72146(7) 0.0246(5) Uani 1 1 d . . .
C3 C 1.03536(18) 0.93890(15) 0.63474(7) 0.0256(5) Uani 1 1 d . . .
H3 H 1.0535 0.9053 0.6600 0.031 Uiso 1 1 calc R . .
C2 C 0.91894(18) 0.95059(13) 0.62091(7) 0.0205(4) Uani 1 1 d . . .
C14 C 0.7393(2) 0.87620(16) 0.75420(8) 0.0348(5) Uani 1 1 d . . .
H14A H 0.7670 0.8852 0.7848 0.052 Uiso 1 1 calc R . .
H14B H 0.7066 0.8193 0.7515 0.052 Uiso 1 1 calc R . .
H14C H 0.6782 0.9176 0.7471 0.052 Uiso 1 1 calc R . .
C26 C 0.3337(2) 0.78982(15) 0.61653(8) 0.0337(5) Uani 1 1 d . . .
H26 H 0.2941 0.8310 0.5991 0.040 Uiso 1 1 calc R . .
C12 C 0.8910(2) 0.97543(14) 0.72587(7) 0.0306(5) Uani 1 1 d . . .
H12A H 0.9637 0.9807 0.7085 0.046 Uiso 1 1 calc R . .
H12B H 0.9075 0.9875 0.7573 0.046 Uiso 1 1 calc R . .
H12C H 0.8325 1.0155 0.7147 0.046 Uiso 1 1 calc R . .
C10 C 0.79381(18) 0.86416(13) 0.67543(7) 0.0219(4) Uani 1 1 d . . .
C22 C 0.3274(3) 0.67659(16) 0.66999(9) 0.0424(7) Uani 1 1 d . . .
C4 C 1.1230(2) 0.97788(15) 0.61044(8) 0.0302(5) Uani 1 1 d . . .
H4 H 1.2025 0.9719 0.6197 0.036 Uiso 1 1 calc R . .
C24 C 0.5136(2) 0.72085(14) 0.63844(8) 0.0350(6) Uani 1 1 d . . .
H24 H 0.5963 0.7140 0.6356 0.042 Uiso 1 1 calc R . .
C17 C 0.4218(2) 1.15981(14) 0.55470(8) 0.0328(5) Uani 1 1 d . . .
H17 H 0.3610 1.1642 0.5331 0.039 Uiso 1 1 calc R . .
C23 C 0.4486(3) 0.66914(16) 0.66639(9) 0.0445(7) Uani 1 1 d . . .
H23 H 0.4882 0.6275 0.6835 0.053 Uiso 1 1 calc R . .
C18 C 0.5911(3) 1.21775(15) 0.59112(8) 0.0387(6) Uani 1 1 d . . .
H18 H 0.6469 1.2618 0.5943 0.046 Uiso 1 1 calc R . .
C21 C 0.2592(4) 0.6208(2) 0.70142(11) 0.0668(10) Uani 1 1 d . . .
H21A H 0.1753 0.6348 0.6997 0.100 Uiso 1 1 calc R . .
H21B H 0.2872 0.6297 0.7320 0.100 Uiso 1 1 calc R . .
H21C H 0.2708 0.5618 0.6930 0.100 Uiso 1 1 calc R . .
C27 C 0.2712(2) 0.73612(16) 0.64400(9) 0.0416(6) Uani 1 1 d . . .
H27 H 0.1879 0.7402 0.6450 0.050 Uiso 1 1 calc R . .
C16 C 0.5039(3) 1.22435(14) 0.55863(8) 0.0374(6) Uani 1 1 d . . .
C13 C 0.9358(2) 0.81909(16) 0.73340(8) 0.0364(6) Uani 1 1 d . . .
H13A H 1.0013 0.8221 0.7122 0.055 Uiso 1 1 calc R . .
H13B H 0.8997 0.7631 0.7320 0.055 Uiso 1 1 calc R . .
H13C H 0.9653 0.8293 0.7636 0.055 Uiso 1 1 calc R . .
C15 C 0.4987(4) 1.29979(17) 0.52846(9) 0.0603(9) Uani 1 1 d . . .
H15A H 0.5789 1.3178 0.5211 0.090 Uiso 1 1 calc R . .
H15B H 0.4573 1.3457 0.5436 0.090 Uiso 1 1 calc R . .
H15C H 0.4567 1.2850 0.5010 0.090 Uiso 1 1 calc R . .
N2 N 0.60401(14) 0.92191(10) 0.61554(5) 0.0189(3) Uani 1 1 d . . .
O5 O 0.41461(13) 0.95650(9) 0.65223(5) 0.0253(3) Uani 1 1 d . . .
O1 O 0.73389(15) 0.80295(10) 0.66976(5) 0.0341(4) Uani 1 1 d . . .
O3 O 0.63166(14) 0.80843(10) 0.56036(5) 0.0315(4) Uani 1 1 d . . .
O4 O 0.60240(14) 1.01100(10) 0.68334(5) 0.0265(3) Uani 1 1 d . . .
O2 O 0.45322(14) 0.89725(10) 0.55359(5) 0.0318(4) Uani 1 1 d . . .
C28 C 0.51624(18) 1.08433(13) 0.61347(7) 0.0220(4) Uani 1 1 d . . .


_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
Br1 C8 1.865(2) . ?
S2 O2 1.4250(16) . ?
S2 O3 1.4253(16) . ?
S2 N2 1.7300(17) . ?
S2 C25 1.757(2) . ?
S3 O5 1.4280(15) . ?
S3 O4 1.4318(15) . ?
S3 N2 1.6891(17) . ?
S3 C28 1.751(2) . ?
N1 C2 1.399(3) . ?
N1 C9 1.415(2) . ?
N1 C10 1.440(3) . ?
C9 C8 1.359(3) . ?
C9 N2 1.412(3) . ?
C6 C5 1.367(3) . ?
C6 C7 1.404(3) . ?
C6 H6 0.9500 . ?
C25 C24 1.379(3) . ?
C25 C26 1.387(3) . ?
C20 C18 1.377(3) . ?
C20 C28 1.390(3) . ?
C20 H20 0.9500 . ?
C5 C4 1.401(3) . ?
C5 H5 0.9500 . ?
C19 C17 1.381(3) . ?
C19 C28 1.391(3) . ?
C19 H19 0.9500 . ?
C8 C7 1.425(3) . ?
C7 C2 1.406(3) . ?
C11 C12 1.522(3) . ?
C11 C10 1.531(3) . ?
C11 C13 1.540(3) . ?
C11 C14 1.545(3) . ?
C3 C4 1.380(3) . ?
C3 C2 1.399(3) . ?
C3 H3 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C26 C27 1.382(3) . ?
C26 H26 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C10 O1 1.199(3) . ?
C22 C27 1.382(4) . ?
C22 C23 1.386(4) . ?
C22 C21 1.508(4) . ?
C4 H4 0.9500 . ?
C24 C23 1.387(4) . ?
C24 H24 0.9500 . ?
C17 C16 1.391(3) . ?
C17 H17 0.9500 . ?
C23 H23 0.9500 . ?
C18 C16 1.393(4) . ?
C18 H18 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C27 H27 0.9500 . ?
C16 C15 1.503(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 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
O2 S2 O3 120.82(10) . . ?
O2 S2 N2 107.91(9) . . ?
O3 S2 N2 102.47(9) . . ?
O2 S2 C25 108.31(11) . . ?
O3 S2 C25 110.22(10) . . ?
N2 S2 C25 106.05(9) . . ?
O5 S3 O4 120.62(9) . . ?
O5 S3 N2 105.03(9) . . ?
O4 S3 N2 104.77(9) . . ?
O5 S3 C28 109.94(10) . . ?
O4 S3 C28 108.47(10) . . ?
N2 S3 C28 107.11(9) . . ?
C2 N1 C9 107.12(16) . . ?
C2 N1 C10 129.24(17) . . ?
C9 N1 C10 123.16(16) . . ?
C8 C9 N2 128.79(18) . . ?
C8 C9 N1 109.22(18) . . ?
N2 C9 N1 121.65(17) . . ?
C5 C6 C7 118.3(2) . . ?
C5 C6 H6 120.8 . . ?
C7 C6 H6 120.8 . . ?
C24 C25 C26 121.3(2) . . ?
C24 C25 S2 119.86(18) . . ?
C26 C25 S2 118.85(18) . . ?
C18 C20 C28 118.8(2) . . ?
C18 C20 H20 120.6 . . ?
C28 C20 H20 120.6 . . ?
C6 C5 C4 121.0(2) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C17 C19 C28 118.9(2) . . ?
C17 C19 H19 120.6 . . ?
C28 C19 H19 120.6 . . ?
C9 C8 C7 108.32(18) . . ?
C9 C8 Br1 126.76(16) . . ?
C7 C8 Br1 124.87(15) . . ?
C6 C7 C2 120.6(2) . . ?
C6 C7 C8 132.4(2) . . ?
C2 C7 C8 107.02(17) . . ?
C12 C11 C10 115.01(17) . . ?
C12 C11 C13 112.49(19) . . ?
C10 C11 C13 107.51(19) . . ?
C12 C11 C14 108.27(19) . . ?
C10 C11 C14 105.52(17) . . ?
C13 C11 C14 107.58(19) . . ?
C4 C3 C2 117.8(2) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
C3 C2 N1 131.08(19) . . ?
C3 C2 C7 120.43(19) . . ?
N1 C2 C7 108.24(18) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C27 C26 C25 118.8(2) . . ?
C27 C26 H26 120.6 . . ?
C25 C26 H26 120.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C10 N1 117.65(19) . . ?
O1 C10 C11 121.51(19) . . ?
N1 C10 C11 120.77(17) . . ?
C27 C22 C23 118.3(2) . . ?
C27 C22 C21 121.1(3) . . ?
C23 C22 C21 120.6(3) . . ?
C3 C4 C5 121.7(2) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C25 C24 C23 118.4(2) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C19 C17 C16 121.0(2) . . ?
C19 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C22 C23 C24 121.7(3) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C20 C18 C16 121.4(2) . . ?
C20 C18 H18 119.3 . . ?
C16 C18 H18 119.3 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C27 C26 121.4(3) . . ?
C22 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C17 C16 C18 118.7(2) . . ?
C17 C16 C15 120.7(2) . . ?
C18 C16 C15 120.6(2) . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C9 N2 S3 116.41(13) . . ?
C9 N2 S2 117.68(13) . . ?
S3 N2 S2 122.16(10) . . ?
C20 C28 C19 121.2(2) . . ?
C20 C28 S3 119.64(17) . . ?
C19 C28 S3 119.09(16) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.086
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a130112mor2
_database_code_depnum_ccdc_archive 'CCDC 1023214'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H35 Cl6 I N2 O5 S2'
_chemical_formula_weight         967.37

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'
I I -0.4742 1.8119 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   18.254(3)
_cell_length_b                   9.5783(15)
_cell_length_c                   23.967(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.187(2)
_cell_angle_gamma                90.00
_cell_volume                     4157.7(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    3919
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      23.95
_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1944
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6969
_exptl_absorpt_correction_T_max  0.8812
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_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  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            22389
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         27.56
_reflns_number_total             9335
_reflns_number_gt                5611
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1180P)²+0.0000P] where P=(Fo²+2Fc²)/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         9335
_refine_ls_number_parameters     539
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.2139
_refine_ls_wR_factor_gt          0.1797
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C34A C 0.7363(10) 0.154(2) 0.1849(8) 0.074(7) Uani 0.504(16) 1 d PD A 1
H34A H 0.7666 0.0940 0.1625 0.089 Uiso 0.504(16) 1 calc PR A 1
Cl1A Cl 0.6654(7) 0.0649(14) 0.1980(8) 0.188(7) Uani 0.504(16) 1 d PD A 1
Cl2A Cl 0.7137(9) 0.3072(10) 0.1465(5) 0.164(5) Uani 0.504(16) 1 d PD A 1
Cl3A Cl 0.7879(7) 0.1840(17) 0.2515(7) 0.205(8) Uani 0.504(16) 1 d PD A 1
C34B C 0.7378(15) 0.128(2) 0.1733(10) 0.166(15) Uani 0.496(16) 1 d PDU A 2
H34B H 0.7643 0.0770 0.1455 0.200 Uiso 0.496(16) 1 calc PR A 2
Cl1B Cl 0.7107(12) 0.0243(17) 0.2193(7) 0.210(8) Uani 0.496(16) 1 d PDU A 2
Cl2B Cl 0.6639(12) 0.224(3) 0.1404(6) 0.258(13) Uani 0.496(16) 1 d PD A 2
Cl3B Cl 0.7965(12) 0.2492(19) 0.2131(8) 0.377(17) Uani 0.496(16) 1 d PD A 2
C35A C 0.6045(11) 0.721(2) 0.0549(8) 0.077(7) Uani 0.490(10) 1 d PD B 3
H35A H 0.6489 0.7474 0.0368 0.092 Uiso 0.490(10) 1 calc PR B 3
Cl4A Cl 0.5222(5) 0.7320(16) 0.0050(5) 0.194(9) Uani 0.490(10) 1 d PD B 3
Cl5A Cl 0.5946(15) 0.829(2) 0.1090(11) 0.384(16) Uani 0.490(10) 1 d PD B 3
Cl6A Cl 0.6101(7) 0.5545(11) 0.0753(4) 0.150(4) Uani 0.490(10) 1 d PD B 3
C35B C 0.5968(15) 0.743(3) 0.0681(11) 0.32(2) Uani 0.510(10) 1 d PDU B 4
H35B H 0.6401 0.7404 0.0464 0.383 Uiso 0.510(10) 1 calc PR B 4
Cl4B Cl 0.5583(6) 0.9105(15) 0.0500(5) 0.183(6) Uani 0.510(10) 1 d PD B 4
Cl5B Cl 0.6373(7) 0.7373(15) 0.1344(4) 0.172(5) Uani 0.510(10) 1 d PD B 4
Cl6B Cl 0.5498(10) 0.606(2) 0.0440(10) 0.365(16) Uani 0.510(10) 1 d PDU B 4
C1 C 0.2259(4) 0.9957(6) 0.1432(2) 0.0361(13) Uani 1 1 d . . .
H1 H 0.2316 1.0908 0.1332 0.043 Uiso 1 1 calc R . .
C2 C 0.1629(3) 0.9223(7) 0.1349(2) 0.0353(14) Uani 1 1 d . . .
C3 C 0.1745(3) 0.7823(6) 0.1546(2) 0.0350(14) Uani 1 1 d . . .
C4 C 0.1300(4) 0.6643(7) 0.1555(3) 0.0429(15) Uani 1 1 d . . .
H4 H 0.0788 0.6683 0.1419 0.051 Uiso 1 1 calc R . .
C5 C 0.1619(5) 0.5421(8) 0.1765(3) 0.0530(19) Uani 1 1 d . . .
H5 H 0.1326 0.4602 0.1763 0.064 Uiso 1 1 calc R . .
C6 C 0.2352(5) 0.5358(7) 0.1979(3) 0.0510(19) Uani 1 1 d . . .
H6 H 0.2549 0.4501 0.2131 0.061 Uiso 1 1 calc R . .
C7 C 0.2817(4) 0.6520(7) 0.1981(3) 0.0458(16) Uani 1 1 d . . .
H7 H 0.3326 0.6464 0.2122 0.055 Uiso 1 1 calc R . .
C8 C 0.2499(4) 0.7766(6) 0.1765(2) 0.0365(14) Uani 1 1 d . . .
C9 C 0.3570(4) 0.9435(8) 0.1860(3) 0.0428(15) Uani 1 1 d . . .
C10 C 0.3906(3) 1.0768(8) 0.1672(3) 0.0458(17) Uani 1 1 d . . .
C11 C 0.3520(4) 1.2101(8) 0.1870(3) 0.0552(19) Uani 1 1 d . . .
H11A H 0.3111 1.2365 0.1585 0.083 Uiso 1 1 calc R . .
H11B H 0.3878 1.2867 0.1923 0.083 Uiso 1 1 calc R . .
H11C H 0.3330 1.1907 0.2227 0.083 Uiso 1 1 calc R . .
C12 C 0.4710(4) 1.0805(10) 0.1942(4) 0.067(2) Uani 1 1 d . . .
H12A H 0.4728 1.0756 0.2351 0.101 Uiso 1 1 calc R . .
H12B H 0.4941 1.1675 0.1838 0.101 Uiso 1 1 calc R . .
H12C H 0.4976 1.0008 0.1808 0.101 Uiso 1 1 calc R . .
C13 C 0.3887(4) 1.0770(10) 0.1024(3) 0.065(2) Uani 1 1 d . . .
H13A H 0.4131 0.9929 0.0907 0.098 Uiso 1 1 calc R . .
H13B H 0.4144 1.1600 0.0909 0.098 Uiso 1 1 calc R . .
H13C H 0.3373 1.0784 0.0848 0.098 Uiso 1 1 calc R . .
C14 C 0.0112(3) 0.9796(6) 0.1725(3) 0.0365(14) Uani 1 1 d . . .
C15 C 0.0313(4) 1.0726(7) 0.2165(3) 0.0443(16) Uani 1 1 d . . .
H15 H 0.0671 1.1433 0.2134 0.053 Uiso 1 1 calc R . .
C16 C -0.0021(5) 1.0589(9) 0.2642(3) 0.0577(19) Uani 1 1 d . . .
H16 H 0.0115 1.1203 0.2949 0.069 Uiso 1 1 calc R . .
C17 C -0.0546(5) 0.9593(9) 0.2689(3) 0.060(2) Uani 1 1 d . . .
H17 H -0.0775 0.9518 0.3022 0.072 Uiso 1 1 calc R . .
C18 C -0.0740(4) 0.8685(8) 0.2236(3) 0.0555(19) Uani 1 1 d . . .
H18 H -0.1107 0.7993 0.2262 0.067 Uiso 1 1 calc R . .
C19 C -0.0407(4) 0.8786(7) 0.1758(3) 0.0461(16) Uani 1 1 d . . .
H19 H -0.0535 0.8162 0.1454 0.055 Uiso 1 1 calc R . .
C20 C 0.7959(4) 1.1897(7) 0.0096(3) 0.0389(15) Uani 1 1 d . . .
C21 C 0.8220(4) 1.3100(7) -0.0114(3) 0.0421(15) Uani 1 1 d . . .
H21 H 0.8736 1.3273 -0.0072 0.050 Uiso 1 1 calc R . .
C22 C 0.7742(4) 1.4061(7) -0.0384(3) 0.0504(18) Uani 1 1 d . . .
H22 H 0.7932 1.4891 -0.0528 0.060 Uiso 1 1 calc R . .
C23 C 0.6995(4) 1.3839(7) -0.0448(3) 0.0486(18) Uani 1 1 d . . .
C24 C 0.6736(4) 1.2633(9) -0.0230(4) 0.070(2) Uani 1 1 d . . .
H24 H 0.6219 1.2478 -0.0256 0.084 Uiso 1 1 calc R . .
C25 C 0.7215(4) 1.1643(8) 0.0025(4) 0.064(2) Uani 1 1 d . . .
H25 H 0.7030 1.0788 0.0151 0.077 Uiso 1 1 calc R . .
C26 C 0.6469(6) 1.4900(8) -0.0748(4) 0.074(3) Uani 1 1 d . . .
H26A H 0.6752 1.5670 -0.0884 0.111 Uiso 1 1 calc R . .
H26B H 0.6144 1.5263 -0.0486 0.111 Uiso 1 1 calc R . .
H26C H 0.6171 1.4452 -0.1067 0.111 Uiso 1 1 calc R . .
C27 C 0.8615(4) 0.6889(7) 0.0432(3) 0.0438(16) Uani 1 1 d . . .
C28 C 0.9300(4) 0.6374(7) 0.0357(3) 0.0502(18) Uani 1 1 d . . .
H28 H 0.9546 0.6688 0.0053 0.060 Uiso 1 1 calc R . .
C29 C 0.9620(5) 0.5393(8) 0.0730(4) 0.066(3) Uani 1 1 d . . .
H29 H 1.0093 0.5029 0.0684 0.080 Uiso 1 1 calc R . .
C30 C 0.9267(7) 0.4935(8) 0.1168(4) 0.078(3) Uani 1 1 d . . .
C31 C 0.8581(5) 0.5475(10) 0.1241(3) 0.070(2) Uani 1 1 d . . .
H31 H 0.8336 0.5169 0.1546 0.083 Uiso 1 1 calc R . .
C32 C 0.8251(5) 0.6465(9) 0.0866(3) 0.066(2) Uani 1 1 d . . .
H32 H 0.7781 0.6841 0.0912 0.079 Uiso 1 1 calc R . .
C33 C 0.9625(6) 0.3792(9) 0.1561(4) 0.103(4) Uani 1 1 d . . .
H33A H 1.0096 0.3513 0.1438 0.155 Uiso 1 1 calc R . .
H33B H 0.9296 0.2982 0.1549 0.155 Uiso 1 1 calc R . .
H33C H 0.9712 0.4152 0.1946 0.155 Uiso 1 1 calc R . .
I1 I 0.06185(2) 1.00241(4) 0.098521(15) 0.03452(15) Uani 1 1 d . . .
N1 N 0.2816(3) 0.9088(5) 0.1688(2) 0.0387(12) Uani 1 1 d . . .
N2 N 0.8646(3) 0.9454(6) -0.0034(2) 0.0380(12) Uani 1 1 d . . .
O1 O 0.3928(3) 0.8570(5) 0.2145(2) 0.0564(13) Uani 1 1 d . . .
O2 O 0.9283(3) 1.1299(5) 0.0537(2) 0.0543(13) Uani 1 1 d . . .
O3 O 0.8257(4) 1.0097(5) 0.0912(2) 0.0620(15) Uani 1 1 d . . .
O4 O 0.7425(3) 0.8236(6) 0.0049(2) 0.0608(14) Uani 1 1 d . . .
O5 O 0.8259(3) 0.7496(5) -0.06236(18) 0.0556(13) Uani 1 1 d . . .
S1 S 0.85674(9) 1.0629(2) 0.04310(7) 0.0410(4) Uani 1 1 d . . .
S2 S 0.81664(10) 0.80621(18) -0.00789(7) 0.0440(4) Uani 1 1 d . . .


_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
C34A Cl1A 1.615(17) . ?
C34A Cl2A 1.752(19) . ?
C34A Cl3A 1.773(19) . ?
C34A H34A 1.0000 . ?
C34B Cl1B 1.61(2) . ?
C34B Cl2B 1.74(2) . ?
C34B Cl3B 1.77(2) . ?
C34B H34B 1.0000 . ?
C35A Cl6A 1.67(2) . ?
C35A Cl5A 1.69(2) . ?
C35A Cl4A 1.80(2) . ?
C35A H35A 1.0000 . ?
C35B Cl6B 1.63(2) . ?
C35B Cl5B 1.67(2) . ?
C35B Cl4B 1.78(2) . ?
C35B H35B 1.0000 . ?
C1 C2 1.341(9) . ?
C1 N1 1.397(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.428(8) . ?
C2 I1 2.085(6) . ?
C3 C4 1.394(9) . ?
C3 C8 1.411(8) . ?
C4 C5 1.375(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.399(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.398(9) . ?
C7 H7 0.9500 . ?
C8 N1 1.414(8) . ?
C9 O1 1.212(7) . ?
C9 N1 1.425(8) . ?
C9 C10 1.510(10) . ?
C10 C12 1.528(9) . ?
C10 C13 1.548(10) . ?
C10 C11 1.560(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.363(9) . ?
C14 C15 1.393(9) . ?
C14 I1 2.111(6) . ?
C15 C16 1.369(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.366(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.401(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.365(10) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.366(9) . ?
C20 C25 1.369(10) . ?
C20 S1 1.769(6) . ?
C21 C22 1.373(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.369(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.376(10) . ?
C23 C26 1.516(10) . ?
C24 C25 1.379(10) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C32 1.364(10) . ?
C27 C28 1.377(10) . ?
C27 S2 1.783(6) . ?
C28 C29 1.376(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.371(15) . ?
C29 H29 0.9500 . ?
C30 C31 1.386(15) . ?
C30 C33 1.536(11) . ?
C31 C32 1.391(11) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
N2 S2 1.591(6) . ?
N2 S1 1.603(6) . ?
O2 S1 1.449(5) . ?
O3 S1 1.439(5) . ?
O4 S2 1.435(5) . ?
O5 S2 1.443(5) . ?

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
Cl1A C34A Cl2A 113.7(12) . . ?
Cl1A C34A Cl3A 105.0(13) . . ?
Cl2A C34A Cl3A 113.7(13) . . ?
Cl1A C34A H34A 108.0 . . ?
Cl2A C34A H34A 108.0 . . ?
Cl3A C34A H34A 108.0 . . ?
Cl1B C34B Cl2B 110.5(17) . . ?
Cl1B C34B Cl3B 104.5(15) . . ?
Cl2B C34B Cl3B 106.4(16) . . ?
Cl1B C34B H34B 111.7 . . ?
Cl2B C34B H34B 111.7 . . ?
Cl3B C34B H34B 111.7 . . ?
Cl6A C35A Cl5A 111.8(15) . . ?
Cl6A C35A Cl4A 105.5(12) . . ?
Cl5A C35A Cl4A 108.2(15) . . ?
Cl6A C35A H35A 110.4 . . ?
Cl5A C35A H35A 110.4 . . ?
Cl4A C35A H35A 110.4 . . ?
Cl6B C35B Cl5B 118(2) . . ?
Cl6B C35B Cl4B 117.5(19) . . ?
Cl5B C35B Cl4B 112.1(14) . . ?
Cl6B C35B H35B 102.1 . . ?
Cl5B C35B H35B 102.1 . . ?
Cl4B C35B H35B 102.1 . . ?
C2 C1 N1 108.5(5) . . ?
C2 C1 H1 125.8 . . ?
N1 C1 H1 125.8 . . ?
C1 C2 C3 110.7(5) . . ?
C1 C2 I1 124.4(5) . . ?
C3 C2 I1 124.8(5) . . ?
C4 C3 C8 120.4(6) . . ?
C4 C3 C2 134.7(6) . . ?
C8 C3 C2 104.9(5) . . ?
C5 C4 C3 118.3(7) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C6 C5 C4 121.6(7) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C7 121.9(7) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C8 C7 C6 117.0(7) . . ?
C8 C7 H7 121.5 . . ?
C6 C7 H7 121.5 . . ?
C7 C8 C3 120.8(6) . . ?
C7 C8 N1 130.9(6) . . ?
C3 C8 N1 108.2(5) . . ?
O1 C9 N1 115.9(7) . . ?
O1 C9 C10 122.3(6) . . ?
N1 C9 C10 121.7(5) . . ?
C9 C10 C12 107.4(6) . . ?
C9 C10 C13 109.9(6) . . ?
C12 C10 C13 108.9(6) . . ?
C9 C10 C11 112.7(6) . . ?
C12 C10 C11 107.4(6) . . ?
C13 C10 C11 110.4(6) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 121.9(6) . . ?
C19 C14 I1 120.2(5) . . ?
C15 C14 I1 117.9(5) . . ?
C16 C15 C14 117.9(7) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C17 C16 C15 121.7(8) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 118.8(7) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
C19 C18 C17 120.7(7) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C14 C19 C18 119.0(7) . . ?
C14 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C21 C20 C25 119.3(6) . . ?
C21 C20 S1 121.2(5) . . ?
C25 C20 S1 119.4(5) . . ?
C20 C21 C22 120.6(7) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C23 C22 C21 120.9(7) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 118.2(6) . . ?
C22 C23 C26 120.8(7) . . ?
C24 C23 C26 121.0(7) . . ?
C23 C24 C25 121.1(7) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C20 C25 C24 119.8(7) . . ?
C20 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C27 C28 122.0(7) . . ?
C32 C27 S2 119.1(6) . . ?
C28 C27 S2 118.8(5) . . ?
C29 C28 C27 118.5(8) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C30 C29 C28 121.0(9) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C29 C30 C31 119.7(8) . . ?
C29 C30 C33 119.5(11) . . ?
C31 C30 C33 120.8(10) . . ?
C30 C31 C32 119.9(8) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C27 C32 C31 118.9(9) . . ?
C27 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C2 I1 C14 93.9(2) . . ?
C1 N1 C8 107.6(5) . . ?
C1 N1 C9 127.7(6) . . ?
C8 N1 C9 124.6(5) . . ?
S2 N2 S1 122.6(3) . . ?
O3 S1 O2 116.9(3) . . ?
O3 S1 N2 112.7(3) . . ?
O2 S1 N2 106.0(3) . . ?
O3 S1 C20 108.6(3) . . ?
O2 S1 C20 106.0(3) . . ?
N2 S1 C20 105.8(3) . . ?
O4 S2 O5 117.2(3) . . ?
O4 S2 N2 114.5(3) . . ?
O5 S2 N2 104.5(3) . . ?
O4 S2 C27 106.9(3) . . ?
O5 S2 C27 106.8(3) . . ?
N2 S2 C27 106.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.669
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.206
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_I
_database_code_depnum_ccdc_archive 'CCDC 1023215'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            a131207mor1
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H18 N2 O2 S'
_chemical_formula_iupac          ?
_chemical_formula_weight         374.44

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9285(7)
_cell_length_b                   10.1079(7)
_cell_length_c                   10.4705(7)
_cell_angle_alpha                66.6900(10)
_cell_angle_beta                 76.0070(10)
_cell_angle_gamma                89.8540(10)
_cell_volume                     931.25(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    173.(2)

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             392

_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
;
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.98

_exptl_special_details           'SADABS Sheldrick 1996'

_diffrn_ambient_temperature      173.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'graphite '

_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            5301
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       13

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_reflns_number_total             4050
_reflns_number_gt                3111
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1206
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_number_reflns         4050
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0556P)²+0.2277P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.415
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S1 0.44293(5) -0.04079(5) 0.27327(5) 0.02234(14) Uani d . . . 1 . .
O O1 0.38027(16) -0.14859(15) 0.41436(14) 0.0313(3) Uani d . . . 1 . .
O O2 0.42717(14) -0.07083(14) 0.15277(14) 0.0254(3) Uani d . . . 1 . .
N N1 0.38425(17) 0.11014(17) 0.26730(17) 0.0238(4) Uani d . . . 1 . .
N N2 0.43038(17) 0.22792(17) 0.00804(16) 0.0238(4) Uani d . . . 1 . .
H H2 0.472 0.1607 -0.0155 0.029 Uiso calc U . R 1 . .
C C9 0.3207(2) 0.3531(2) 0.1366(2) 0.0244(4) Uani d . . . 1 . .
C C8 0.38491(19) 0.2175(2) 0.1443(2) 0.0222(4) Uani d . . . 1 . .
C C5 0.6229(2) -0.0134(2) 0.2550(2) 0.0245(4) Uani d . . . 1 . .
C C6 0.7167(2) 0.0395(2) 0.1200(2) 0.0293(5) Uani d . . . 1 . .
H H6 0.6858 0.0547 0.0367 0.035 Uiso calc U . R 1 . .
C C10 0.3349(2) 0.4397(2) -0.0168(2) 0.0265(4) Uani d . . . 1 . .
C C4 0.6676(2) -0.0387(2) 0.3777(2) 0.0307(5) Uani d . . . 1 . .
H H4 0.6033 -0.0773 0.4703 0.037 Uiso calc U . R 1 . .
C C16 0.2628(2) 0.3735(2) 0.2569(2) 0.0300(5) Uani d . . . 1 . .
H H16 0.283 0.309 0.3432 0.036 Uiso calc U . R 1 . .
C C11 0.4026(2) 0.3604(2) -0.0919(2) 0.0253(4) Uani d . . . 1 . .
C C15 0.3041(2) 0.5789(2) -0.0963(2) 0.0329(5) Uani d . . . 1 . .
H H15 0.2609 0.6371 -0.0489 0.039 Uiso calc U . R 1 . .
C C17 0.1717(2) 0.4853(2) 0.2682(2) 0.0350(5) Uani d . . . 1 . .
C C3 0.8079(2) -0.0065(2) 0.3626(3) 0.0373(5) Uani d . . . 1 . .
H H3 0.8389 -0.0226 0.4461 0.045 Uiso calc U . R 1 . .
C C2 0.9038(2) 0.0488(2) 0.2286(3) 0.0370(5) Uani d . . . 1 . .
C C13 0.4017(2) 0.5477(2) -0.3161(2) 0.0360(5) Uani d . . . 1 . .
H H13 0.4226 0.5856 -0.4182 0.043 Uiso calc U . R 1 . .
C C12 0.4358(2) 0.4094(2) -0.2395(2) 0.0319(5) Uani d . . . 1 . .
H H12 0.48 0.3519 -0.2872 0.038 Uiso calc U . R 1 . .
C C14 0.3375(2) 0.6301(2) -0.2444(2) 0.0376(5) Uani d . . . 1 . .
H H14 0.3161 0.7242 -0.2987 0.045 Uiso calc U . R 1 . .
C C7 0.8565(2) 0.0701(2) 0.1080(2) 0.0349(5) Uani d . . . 1 . .
H H7 0.9212 0.1064 0.0156 0.042 Uiso calc U . R 1 . .
C C18 0.0596(3) 0.5086(3) 0.2053(3) 0.0424(6) Uani d . . . 1 . .
H H18 0.0472 0.4566 0.15 0.051 Uiso calc U . R 1 . .
C C22 0.1878(3) 0.5620(3) 0.3489(3) 0.0475(6) Uani d . . . 1 . .
H H22 0.2616 0.5454 0.3949 0.057 Uiso calc U . R 1 . .
C C19 -0.0332(3) 0.6061(3) 0.2224(3) 0.0539(7) Uani d . . . 1 . .
H H19 -0.1099 0.6196 0.1806 0.065 Uiso calc U . R 1 . .
C C20 -0.0142(3) 0.6834(3) 0.3003(3) 0.0640(9) Uani d . . . 1 . .
H H20 -0.0774 0.7513 0.3112 0.077 Uiso calc U . R 1 . .
C C21 0.0964(3) 0.6630(3) 0.3628(3) 0.0639(9) Uani d . . . 1 . .
H H21 0.1099 0.7179 0.4152 0.077 Uiso calc U . R 1 . .
C C1 1.0556(3) 0.0826(3) 0.2126(3) 0.0561(7) Uani d . . . 1 . .
H H1A 1.0654 0.1102 0.29 0.084 Uiso calc U . R 1 . .
H H1B 1.0961 0.1628 0.1191 0.084 Uiso calc U . R 1 . .
H H1C 1.1045 -0.0031 0.2184 0.084 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 O1 . 1.4289(14) ?
S1 O2 . 1.4517(13) ?
S1 N1 . 1.6151(16) ?
S1 C5 . 1.761(2) ?
N1 C8 . 1.314(2) ?
N2 C8 . 1.349(2) ?
N2 C11 . 1.412(2) ?
N2 H2 . 0.88 ?
C9 C16 . 1.346(3) ?
C9 C10 . 1.465(3) ?
C9 C8 . 1.492(3) ?
C5 C6 . 1.386(3) ?
C5 C4 . 1.388(3) ?
C6 C7 . 1.387(3) ?
C6 H6 . 0.95 ?
C10 C11 . 1.397(3) ?
C10 C15 . 1.401(3) ?
C4 C3 . 1.388(3) ?
C4 H4 . 0.95 ?
C16 C17 . 1.469(3) ?
C16 H16 . 0.95 ?
C11 C12 . 1.375(3) ?
C15 C14 . 1.378(3) ?
C15 H15 . 0.95 ?
C17 C22 . 1.388(3) ?
C17 C18 . 1.399(3) ?
C3 C2 . 1.387(3) ?
C3 H3 . 0.95 ?
C2 C7 . 1.390(3) ?
C2 C1 . 1.501(3) ?
C13 C14 . 1.387(3) ?
C13 C12 . 1.398(3) ?
C13 H13 . 0.95 ?
C12 H12 . 0.95 ?
C14 H14 . 0.95 ?
C7 H7 . 0.95 ?
C18 C19 . 1.381(3) ?
C18 H18 . 0.95 ?
C22 C21 . 1.391(3) ?
C22 H22 . 0.95 ?
C19 C20 . 1.375(4) ?
C19 H19 . 0.95 ?
C20 C21 . 1.385(4) ?
C20 H20 . 0.95 ?
C21 H21 . 0.95 ?
C1 H1A . 0.98 ?
C1 H1B . 0.98 ?
C1 H1C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 S1 O2 . . 116.77(9) ?
O1 S1 N1 . . 106.96(8) ?
O2 S1 N1 . . 111.71(8) ?
O1 S1 C5 . . 108.28(9) ?
O2 S1 C5 . . 107.70(9) ?
N1 S1 C5 . . 104.72(9) ?
C8 N1 S1 . . 121.48(13) ?
C8 N2 C11 . . 111.31(15) ?
C8 N2 H2 . . 124.3 ?
C11 N2 H2 . . 124.3 ?
C16 C9 C10 . . 133.37(18) ?
C16 C9 C8 . . 121.14(18) ?
C10 C9 C8 . . 105.47(16) ?
N1 C8 N2 . . 130.29(17) ?
N1 C8 C9 . . 122.42(17) ?
N2 C8 C9 . . 107.16(16) ?
C6 C5 C4 . . 120.85(19) ?
C6 C5 S1 . . 120.46(15) ?
C4 C5 S1 . . 118.61(16) ?
C5 C6 C7 . . 119.2(2) ?
C5 C6 H6 . . 120.4 ?
C7 C6 H6 . . 120.4 ?
C11 C10 C15 . . 118.27(19) ?
C11 C10 C9 . . 107.29(16) ?
C15 C10 C9 . . 134.30(19) ?
C3 C4 C5 . . 118.8(2) ?
C3 C4 H4 . . 120.6 ?
C5 C4 H4 . . 120.6 ?
C9 C16 C17 . . 126.7(2) ?
C9 C16 H16 . . 116.7 ?
C17 C16 H16 . . 116.7 ?
C12 C11 C10 . . 123.59(18) ?
C12 C11 N2 . . 127.64(18) ?
C10 C11 N2 . . 108.77(17) ?
C14 C15 C10 . . 118.9(2) ?
C14 C15 H15 . . 120.6 ?
C10 C15 H15 . . 120.6 ?
C22 C17 C18 . . 118.7(2) ?
C22 C17 C16 . . 121.5(2) ?
C18 C17 C16 . . 119.7(2) ?
C2 C3 C4 . . 121.6(2) ?
C2 C3 H3 . . 119.2 ?
C4 C3 H3 . . 119.2 ?
C3 C2 C7 . . 118.3(2) ?
C3 C2 C1 . . 121.5(2) ?
C7 C2 C1 . . 120.2(2) ?
C14 C13 C12 . . 120.7(2) ?
C14 C13 H13 . . 119.7 ?
C12 C13 H13 . . 119.7 ?
C11 C12 C13 . . 116.9(2) ?
C11 C12 H12 . . 121.5 ?
C13 C12 H12 . . 121.5 ?
C15 C14 C13 . . 121.65(19) ?
C15 C14 H14 . . 119.2 ?
C13 C14 H14 . . 119.2 ?
C6 C7 C2 . . 121.2(2) ?
C6 C7 H7 . . 119.4 ?
C2 C7 H7 . . 119.4 ?
C19 C18 C17 . . 121.0(3) ?
C19 C18 H18 . . 119.5 ?
C17 C18 H18 . . 119.5 ?
C17 C22 C21 . . 120.3(3) ?
C17 C22 H22 . . 119.8 ?
C21 C22 H22 . . 119.8 ?
C20 C19 C18 . . 119.7(3) ?
C20 C19 H19 . . 120.2 ?
C18 C19 H19 . . 120.2 ?
C19 C20 C21 . . 120.4(2) ?
C19 C20 H20 . . 119.8 ?
C21 C20 H20 . . 119.8 ?
C20 C21 C22 . . 119.9(3) ?
C20 C21 H21 . . 120.1 ?
C22 C21 H21 . . 120.1 ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_I
_database_code_depnum_ccdc_archive 'CCDC 1023216'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            a140201mor2
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H22 N2 O3 S'
_chemical_formula_iupac          ?
_chemical_formula_weight         418.50

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8453(4)
_cell_length_b                   11.1232(7)
_cell_length_c                   14.3467(9)
_cell_angle_alpha                95.8640(10)
_cell_angle_beta                 94.6170(10)
_cell_angle_gamma                106.1630(10)
_cell_volume                     1036.91(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    173.(2)

_exptl_crystal_description       Needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440

_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
;
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_T_max  0.98

_exptl_special_details           'SADABS Sheldrick 1996'

_diffrn_ambient_temperature      173.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'graphite '

_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            5925
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_reflns_number_total             4519
_reflns_number_gt                3520
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1302
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_number_reflns         4519
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0675P)²+0.2793P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.659
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S1 0.31565(7) 0.58954(4) 0.40494(4) 0.02611(15) Uani d . . . 1 . .
O O1 0.3438(2) 0.13369(14) 0.17623(10) 0.0333(4) Uani d . . . 1 . .
N N1 0.0739(2) 0.31753(14) 0.41677(11) 0.0224(3) Uani d . . . 1 . .
H H1 0.0334 0.3718 0.4537 0.027 Uiso calc . . R 1 . .
O O2 0.2108(2) 0.57076(12) 0.48841(9) 0.0271(3) Uani d . . . 1 . .
O O3 0.5084(2) 0.68554(13) 0.41539(12) 0.0388(4) Uani d . . . 1 . .
N N2 0.3508(2) 0.46105(14) 0.35499(11) 0.0249(4) Uani d . . . 1 . .
C C1 0.2291(3) 0.34984(17) 0.36464(13) 0.0206(4) Uani d . . . 1 . .
C C11 0.2627(3) 0.23459(18) 0.20376(13) 0.0247(4) Uani d . . . 1 . .
H H11 0.3633 0.3157 0.1943 0.03 Uiso calc . . R 1 . .
C C12 0.0645(3) 0.22120(18) 0.14490(13) 0.0252(4) Uani d . . . 1 . .
C C8 -0.0169(3) 0.18565(16) 0.40525(13) 0.0212(4) Uani d . . . 1 . .
C C13 -0.0494(3) 0.1069(2) 0.09339(14) 0.0301(4) Uani d . . . 1 . .
H H13 -0.0022 0.0344 0.0955 0.036 Uiso calc . . R 1 . .
C C2 0.2542(3) 0.23060(17) 0.31137(13) 0.0216(4) Uani d . . . 1 . .
C C3 0.0798(3) 0.12951(17) 0.33937(13) 0.0218(4) Uani d . . . 1 . .
C C4 0.0144(3) -0.00036(18) 0.31564(14) 0.0285(4) Uani d . . . 1 . .
H H4 0.0781 -0.0407 0.2707 0.034 Uiso calc . . R 1 . .
C C22 -0.0637(3) 0.57819(18) 0.31943(14) 0.0297(4) Uani d . . . 1 . .
H H22 -0.1185 0.5304 0.3674 0.036 Uiso calc . . R 1 . .
C C18 0.1478(3) 0.62583(18) 0.31967(14) 0.0286(4) Uani d . . . 1 . .
C C7 -0.1729(3) 0.11767(17) 0.45058(14) 0.0249(4) Uani d . . . 1 . .
H H7 -0.2339 0.1579 0.4968 0.03 Uiso calc . . R 1 . .
C C9 0.4649(3) 0.2110(2) 0.33775(15) 0.0290(4) Uani d . . . 1 . .
H H9A 0.5743 0.2925 0.3485 0.035 Uiso calc . . R 1 . .
H H9B 0.4653 0.1683 0.395 0.035 Uiso calc . . R 1 . .
C C6 -0.2370(3) -0.01269(18) 0.42569(15) 0.0295(4) Uani d . . . 1 . .
H H6 -0.3449 -0.0627 0.4552 0.035 Uiso calc . . R 1 . .
C C21 -0.1923(4) 0.6012(2) 0.24883(16) 0.0364(5) Uani d . . . 1 . .
H H21 -0.3363 0.5682 0.2482 0.044 Uiso calc . . R 1 . .
C C5 -0.1466(3) -0.07074(18) 0.35895(16) 0.0325(5) Uani d . . . 1 . .
H H5 -0.1948 -0.1597 0.3424 0.039 Uiso calc . . R 1 . .
C C17 -0.0072(4) 0.3260(2) 0.14025(16) 0.0377(5) Uani d . . . 1 . .
H H17 0.0699 0.4053 0.1739 0.045 Uiso calc . . R 1 . .
C C15 -0.3020(4) 0.2012(2) 0.03634(16) 0.0410(6) Uani d . . . 1 . .
H H15 -0.4276 0.1942 -0.0002 0.049 Uiso calc . . R 1 . .
C C14 -0.2311(3) 0.0975(2) 0.03898(15) 0.0357(5) Uani d . . . 1 . .
H H14 -0.3067 0.0191 0.0035 0.043 Uiso calc . . R 1 . .
C C16 -0.1912(4) 0.3156(2) 0.08668(17) 0.0452(6) Uani d . . . 1 . .
H H16 -0.2405 0.3872 0.0848 0.054 Uiso calc . . R 1 . .
C C19 0.2290(4) 0.6974(2) 0.25057(18) 0.0417(6) Uani d . . . 1 . .
H H19 0.373 0.7305 0.2512 0.05 Uiso calc . . R 1 . .
C C10 0.4920(4) 0.1272(2) 0.25096(15) 0.0377(5) Uani d . . . 1 . .
H H10A 0.6323 0.1581 0.2331 0.045 Uiso calc . . R 1 . .
H H10B 0.4687 0.0391 0.2644 0.045 Uiso calc . . R 1 . .
C C20 0.0966(5) 0.7195(2) 0.18087(19) 0.0503(7) Uani d . . . 1 . .
H H20 0.1513 0.7683 0.1334 0.06 Uiso calc . . R 1 . .
C C23 -0.1144(4) 0.6721(2) 0.17842(17) 0.0455(6) Uani d . . . 1 . .
C C24 -0.2565(6) 0.6994(4) 0.1028(2) 0.0735(10) Uani d . . . 1 . .
H H24A -0.2674 0.785 0.1184 0.11 Uiso calc . . R 1 . .
H H24B -0.3922 0.6383 0.099 0.11 Uiso calc . . R 1 . .
H H24C -0.2022 0.6926 0.042 0.11 Uiso calc . . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 O3 . 1.4335(14) ?
S1 O2 . 1.4488(14) ?
S1 N2 . 1.6198(16) ?
S1 C18 . 1.764(2) ?
O1 C11 . 1.420(2) ?
O1 C10 . 1.437(3) ?
N1 C1 . 1.337(2) ?
N1 C8 . 1.411(2) ?
N1 H1 . 0.88 ?
N2 C1 . 1.313(2) ?
C1 C2 . 1.521(2) ?
C11 C12 . 1.501(3) ?
C11 C2 . 1.554(3) ?
C11 H11 . 1.0 ?
C12 C17 . 1.390(3) ?
C12 C13 . 1.391(3) ?
C8 C7 . 1.377(3) ?
C8 C3 . 1.390(3) ?
C13 C14 . 1.386(3) ?
C13 H13 . 0.95 ?
C2 C3 . 1.508(2) ?
C2 C9 . 1.541(3) ?
C3 C4 . 1.385(3) ?
C4 C5 . 1.394(3) ?
C4 H4 . 0.95 ?
C22 C21 . 1.379(3) ?
C22 C18 . 1.396(3) ?
C22 H22 . 0.95 ?
C18 C19 . 1.389(3) ?
C7 C6 . 1.392(3) ?
C7 H7 . 0.95 ?
C9 C10 . 1.533(3) ?
C9 H9A . 0.99 ?
C9 H9B . 0.99 ?
C6 C5 . 1.381(3) ?
C6 H6 . 0.95 ?
C21 C23 . 1.394(3) ?
C21 H21 . 0.95 ?
C5 H5 . 0.95 ?
C17 C16 . 1.391(3) ?
C17 H17 . 0.95 ?
C15 C14 . 1.373(3) ?
C15 C16 . 1.379(3) ?
C15 H15 . 0.95 ?
C14 H14 . 0.95 ?
C16 H16 . 0.95 ?
C19 C20 . 1.382(4) ?
C19 H19 . 0.95 ?
C10 H10A . 0.99 ?
C10 H10B . 0.99 ?
C20 C23 . 1.389(4) ?
C20 H20 . 0.95 ?
C23 C24 . 1.508(4) ?
C24 H24A . 0.98 ?
C24 H24B . 0.98 ?
C24 H24C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 S1 O2 . . 117.12(9) ?
O3 S1 N2 . . 107.27(9) ?
O2 S1 N2 . . 112.78(8) ?
O3 S1 C18 . . 108.55(10) ?
O2 S1 C18 . . 106.97(9) ?
N2 S1 C18 . . 103.20(9) ?
C11 O1 C10 . . 108.68(15) ?
C1 N1 C8 . . 111.69(15) ?
C1 N1 H1 . . 124.2 ?
C8 N1 H1 . . 124.2 ?
C1 N2 S1 . . 121.12(14) ?
N2 C1 N1 . . 130.74(17) ?
N2 C1 C2 . . 120.47(16) ?
N1 C1 C2 . . 108.78(15) ?
O1 C11 C12 . . 110.95(15) ?
O1 C11 C2 . . 103.07(15) ?
C12 C11 C2 . . 116.83(16) ?
O1 C11 H11 . . 108.6 ?
C12 C11 H11 . . 108.6 ?
C2 C11 H11 . . 108.6 ?
C17 C12 C13 . . 118.59(19) ?
C17 C12 C11 . . 119.49(18) ?
C13 C12 C11 . . 121.91(18) ?
C7 C8 C3 . . 123.00(17) ?
C7 C8 N1 . . 128.19(17) ?
C3 C8 N1 . . 108.80(16) ?
C14 C13 C12 . . 120.7(2) ?
C14 C13 H13 . . 119.7 ?
C12 C13 H13 . . 119.7 ?
C3 C2 C1 . . 102.09(15) ?
C3 C2 C9 . . 112.89(16) ?
C1 C2 C9 . . 112.80(15) ?
C3 C2 C11 . . 116.23(15) ?
C1 C2 C11 . . 114.21(15) ?
C9 C2 C11 . . 99.20(15) ?
C4 C3 C8 . . 119.19(18) ?
C4 C3 C2 . . 132.25(18) ?
C8 C3 C2 . . 108.45(15) ?
C3 C4 C5 . . 118.75(19) ?
C3 C4 H4 . . 120.6 ?
C5 C4 H4 . . 120.6 ?
C21 C22 C18 . . 119.3(2) ?
C21 C22 H22 . . 120.3 ?
C18 C22 H22 . . 120.3 ?
C19 C18 C22 . . 120.7(2) ?
C19 C18 S1 . . 119.06(18) ?
C22 C18 S1 . . 120.19(15) ?
C8 C7 C6 . . 117.01(18) ?
C8 C7 H7 . . 121.5 ?
C6 C7 H7 . . 121.5 ?
C10 C9 C2 . . 103.03(16) ?
C10 C9 H9A . . 111.2 ?
C2 C9 H9A . . 111.2 ?
C10 C9 H9B . . 111.2 ?
C2 C9 H9B . . 111.2 ?
H9A C9 H9B . . 109.1 ?
C5 C6 C7 . . 121.21(19) ?
C5 C6 H6 . . 119.4 ?
C7 C6 H6 . . 119.4 ?
C22 C21 C23 . . 121.0(2) ?
C22 C21 H21 . . 119.5 ?
C23 C21 H21 . . 119.5 ?
C6 C5 C4 . . 120.81(18) ?
C6 C5 H5 . . 119.6 ?
C4 C5 H5 . . 119.6 ?
C12 C17 C16 . . 120.5(2) ?
C12 C17 H17 . . 119.8 ?
C16 C17 H17 . . 119.8 ?
C14 C15 C16 . . 120.1(2) ?
C14 C15 H15 . . 119.9 ?
C16 C15 H15 . . 119.9 ?
C15 C14 C13 . . 120.1(2) ?
C15 C14 H14 . . 119.9 ?
C13 C14 H14 . . 119.9 ?
C15 C16 C17 . . 120.0(2) ?
C15 C16 H16 . . 120.0 ?
C17 C16 H16 . . 120.0 ?
C20 C19 C18 . . 118.8(2) ?
C20 C19 H19 . . 120.6 ?
C18 C19 H19 . . 120.6 ?
O1 C10 C9 . . 106.71(16) ?
O1 C10 H10A . . 110.4 ?
C9 C10 H10A . . 110.4 ?
O1 C10 H10B . . 110.4 ?
C9 C10 H10B . . 110.4 ?
H10A C10 H10B . . 108.6 ?
C19 C20 C23 . . 121.7(2) ?
C19 C20 H20 . . 119.1 ?
C23 C20 H20 . . 119.1 ?
C20 C23 C21 . . 118.5(2) ?
C20 C23 C24 . . 120.9(2) ?
C21 C23 C24 . . 120.6(3) ?
C23 C24 H24A . . 109.5 ?
C23 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C23 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_I
_database_code_depnum_ccdc_archive 'CCDC 1023217'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            a140723mor1
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H30 N3 O5 S2'
_chemical_formula_iupac          ?
_chemical_formula_weight         540.66

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5145(9)
_cell_length_b                   11.3505(10)
_cell_length_c                   12.4229(11)
_cell_angle_alpha                79.1933(10)
_cell_angle_beta                 86.0059(12)
_cell_angle_gamma                82.6050(12)
_cell_volume                     1305.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    173.(2)

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             570

_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_T_max  0.98

_exptl_special_details           'SADABS (Sheldrick 1996)'

_diffrn_ambient_temperature      173.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              ?

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'Phi and Omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            7744
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13

_refine_special_details          
;
;

_reflns_number_total             5883
_reflns_number_gt                4372
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1620
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.047
_refine_ls_number_reflns         5883
_refine_ls_number_parameters     364
_refine_ls_number_restraints     32
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0887P)²+0.5599P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.776
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O6 0.510(6) 0.490(4) -0.014(3) 0.103(4) Uani d U P . 0.5 A -1
C C26 0.488(3) 0.377(2) -0.1389(13) 0.130(7) Uani d U P D 0.5 A -1
H H26A 0.4683 0.2965 -0.148 0.195 Uiso calc U P R 0.5 A -1
H H26B 0.5872 0.3864 -0.16 0.195 Uiso calc U P R 0.5 A -1
H H26C 0.4264 0.4387 -0.1857 0.195 Uiso calc U P R 0.5 A -1
C C27 0.4586(10) 0.3898(11) -0.0220(11) 0.098(3) Uani d U P D 0.5 A -1
C C28 0.4644(15) 0.5060(14) 0.0995(9) 0.115(4) Uani d U P . 0.5 A -1
H H28A 0.3608 0.5033 0.1115 0.138 Uiso calc U P R 0.5 A -1
H H28B 0.5135 0.4409 0.1532 0.138 Uiso calc U P R 0.5 A -1
C C29 0.500(4) 0.622(3) 0.1128(18) 0.175(11) Uani d U P . 0.5 A -1
H H29A 0.4714 0.6356 0.1872 0.263 Uiso calc U P R 0.5 A -1
H H29B 0.6031 0.6237 0.1009 0.263 Uiso calc U P R 0.5 A -1
H H29C 0.451 0.6859 0.0593 0.263 Uiso calc U P R 0.5 A -1
O O5 0.4140(8) 0.3565(12) 0.0600(8) 0.201(7) Uani d . P . 0.5 A -1
C C1 0.0019(2) 0.2745(2) 0.50159(18) 0.0202(5) Uani d . . . 1 . .
C C2 0.0048(2) 0.1131(2) 0.65271(18) 0.0185(5) Uani d . . . 1 . .
C C3 -0.1326(2) 0.1710(2) 0.63697(18) 0.0199(5) Uani d . . . 1 . .
C C4 -0.2490(3) 0.1342(2) 0.7009(2) 0.0265(5) Uani d . . . 1 . .
H H4 -0.3415 0.1752 0.6885 0.032 Uiso calc U . R 1 . .
C C5 -0.2253(3) 0.0350(3) 0.7840(2) 0.0292(6) Uani d . . . 1 . .
H H5 -0.3028 0.0076 0.8302 0.035 Uiso calc U . R 1 . .
C C6 -0.0898(3) -0.0251(2) 0.8007(2) 0.0290(6) Uani d . . . 1 . .
H H6 -0.0761 -0.0933 0.858 0.035 Uiso calc U . R 1 . .
C C7 0.0264(3) 0.0130(2) 0.7348(2) 0.0249(5) Uani d . . . 1 . .
H H7 0.1187 -0.0291 0.7461 0.03 Uiso calc U . R 1 . .
C C8 0.1031(2) 0.1709(2) 0.56243(18) 0.0182(5) Uani d . . . 1 . .
C C9 0.1610(3) 0.0842(2) 0.48279(19) 0.0231(5) Uani d . . . 1 . .
H H9A 0.1943 0.0031 0.524 0.028 Uiso calc U . R 1 . .
H H9B 0.0867 0.0763 0.4335 0.028 Uiso calc U . R 1 . .
C C10 0.2410(2) 0.2157(2) 0.59400(18) 0.0186(5) Uani d . . . 1 . .
H H10 0.222 0.3029 0.6003 0.022 Uiso calc U . R 1 . .
C C11 0.2834(3) 0.1416(2) 0.4177(2) 0.0273(6) Uani d . . . 1 . .
H H11A 0.3551 0.08 0.3929 0.033 Uiso calc U . R 1 . .
H H11B 0.2499 0.2014 0.3532 0.033 Uiso calc U . R 1 . .
C C12 0.2580(3) 0.1807(3) 0.7980(2) 0.0333(6) Uani d . . . 1 . .
H H12 0.2037 0.2571 0.7977 0.04 Uiso calc U . R 1 . .
C C13 0.2981(2) 0.1421(2) 0.6994(2) 0.0217(5) Uani d . . . 1 . .
C C14 0.3799(3) 0.0310(2) 0.7014(2) 0.0260(5) Uani d . . . 1 . .
H H14 0.4097 0.0046 0.6343 0.031 Uiso calc U . R 1 . .
C C15 0.4186(3) -0.0417(3) 0.8002(2) 0.0325(6) Uani d . . . 1 . .
H H15 0.4744 -0.1174 0.8005 0.039 Uiso calc U . R 1 . .
C C16 0.3758(3) -0.0037(3) 0.8980(2) 0.0384(7) Uani d . . . 1 . .
H H16 0.4004 -0.0541 0.9657 0.046 Uiso calc U . R 1 . .
C C17 0.2969(4) 0.1080(3) 0.8973(2) 0.0419(7) Uani d . . . 1 . .
H H17 0.2695 0.135 0.9644 0.05 Uiso calc U . R 1 . .
C C18 -0.1850(3) 0.3389(3) 0.2140(2) 0.0342(6) Uani d . . . 1 . .
H H18 -0.2594 0.3344 0.2692 0.041 Uiso calc U . R 1 . .
C C19 -0.1941(3) 0.2921(3) 0.1195(2) 0.0391(7) Uani d . . . 1 . .
H H19 -0.2757 0.2552 0.1108 0.047 Uiso calc U . R 1 . .
C C20 -0.0877(3) 0.2977(2) 0.0376(2) 0.0323(6) Uani d . . . 1 . .
C C21 -0.1000(4) 0.2462(3) -0.0645(2) 0.0502(9) Uani d . . . 1 . .
H H21A -0.0353 0.1712 -0.0618 0.075 Uiso calc U . R 1 . .
H H21B -0.0749 0.3047 -0.1293 0.075 Uiso calc U . R 1 . .
H H21C -0.1977 0.2292 -0.0686 0.075 Uiso calc U . R 1 . .
C C22 0.0321(3) 0.3500(3) 0.0531(2) 0.0340(6) Uani d . . . 1 . .
H H22 0.1072 0.3534 -0.0016 0.041 Uiso calc U . R 1 . .
C C23 0.0441(3) 0.3971(2) 0.1460(2) 0.0304(6) Uani d . . . 1 . .
H H23 0.1266 0.4326 0.1552 0.036 Uiso calc U . R 1 . .
C C24 -0.0651(3) 0.3924(2) 0.22632(19) 0.0233(5) Uani d . . . 1 . .
C C25 0.3758(3) 0.4289(3) 0.3916(2) 0.0367(7) Uani d . . . 1 . .
H H25A 0.3021 0.4619 0.4405 0.055 Uiso calc U . R 1 . .
H H25B 0.3325 0.4153 0.3263 0.055 Uiso calc U . R 1 . .
H H25C 0.4457 0.4863 0.3694 0.055 Uiso calc U . R 1 . .
N N1 0.3410(2) 0.20081(18) 0.49884(16) 0.0218(4) Uani d . . . 1 . .
N N2 0.0490(2) 0.35080(19) 0.42036(16) 0.0241(4) Uani d . . . 1 . .
H H2 0.1411 0.3465 0.4054 0.029 Uiso calc U . R 1 . .
N N3 -0.1299(2) 0.26535(18) 0.54528(16) 0.0222(4) Uani d . . . 1 . .
H H3 -0.2056 0.3125 0.5199 0.027 Uiso calc U . R 1 . .
O O1 0.0199(2) 0.55861(17) 0.31462(16) 0.0400(5) Uani d . . . 1 . .
O O2 -0.1964(2) 0.47067(17) 0.39392(14) 0.0335(5) Uani d . . . 1 . .
O O3 0.5542(2) 0.2388(2) 0.3829(2) 0.0548(7) Uani d . . . 1 . .
O O4 0.5152(2) 0.31603(18) 0.55680(17) 0.0400(5) Uani d . . . 1 . .
S S1 0.45981(7) 0.29230(6) 0.45995(6) 0.02776(18) Uani d . . . 1 . .
S S2 -0.05421(7) 0.45381(5) 0.34505(5) 0.02590(17) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O6 C27 . 1.31(3) ?
O6 C28 . 1.49(2) ?
C26 C27 . 1.491(16) ?
C26 H26A . 0.98 ?
C26 H26B . 0.98 ?
C26 H26C . 0.98 ?
C27 O5 . 1.093(13) ?
C28 C29 . 1.44(3) ?
C28 H28A . 0.99 ?
C28 H28B . 0.99 ?
C29 H29A . 0.98 ?
C29 H29B . 0.98 ?
C29 H29C . 0.98 ?
C1 N2 . 1.295(3) ?
C1 N3 . 1.340(3) ?
C1 C8 . 1.535(3) ?
C2 C7 . 1.382(3) ?
C2 C3 . 1.395(3) ?
C2 C8 . 1.516(3) ?
C3 C4 . 1.380(3) ?
C3 N3 . 1.411(3) ?
C4 C5 . 1.384(4) ?
C4 H4 . 0.95 ?
C5 C6 . 1.389(4) ?
C5 H5 . 0.95 ?
C6 C7 . 1.395(3) ?
C6 H6 . 0.95 ?
C7 H7 . 0.95 ?
C8 C9 . 1.549(3) ?
C8 C10 . 1.566(3) ?
C9 C11 . 1.517(3) ?
C9 H9A . 0.99 ?
C9 H9B . 0.99 ?
C10 N1 . 1.486(3) ?
C10 C13 . 1.510(3) ?
C10 H10 . 1.0 ?
C11 N1 . 1.481(3) ?
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
C12 C13 . 1.390(3) ?
C12 C17 . 1.394(4) ?
C12 H12 . 0.95 ?
C13 C14 . 1.391(3) ?
C14 C15 . 1.388(4) ?
C14 H14 . 0.95 ?
C15 C16 . 1.383(4) ?
C15 H15 . 0.95 ?
C16 C17 . 1.387(4) ?
C16 H16 . 0.95 ?
C17 H17 . 0.95 ?
C18 C19 . 1.388(4) ?
C18 C24 . 1.390(4) ?
C18 H18 . 0.95 ?
C19 C20 . 1.383(4) ?
C19 H19 . 0.95 ?
C20 C22 . 1.392(4) ?
C20 C21 . 1.510(4) ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C22 C23 . 1.378(4) ?
C22 H22 . 0.95 ?
C23 C24 . 1.388(3) ?
C23 H23 . 0.95 ?
C24 S2 . 1.760(2) ?
C25 S1 . 1.745(3) ?
C25 H25A . 0.98 ?
C25 H25B . 0.98 ?
C25 H25C . 0.98 ?
N1 S1 . 1.6209(19) ?
N2 S2 . 1.621(2) ?
N2 H2 . 0.88 ?
N3 H3 . 0.88 ?
O1 S2 . 1.437(2) ?
O2 S2 . 1.448(2) ?
O3 S1 . 1.431(2) ?
O4 S1 . 1.430(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C27 O6 C28 . . 103.(3) ?
C27 C26 H26A . . 109.5 ?
C27 C26 H26B . . 109.5 ?
H26A C26 H26B . . 109.5 ?
C27 C26 H26C . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
O5 C27 O6 . . 105.(2) ?
O5 C27 C26 . . 149.7(15) ?
O6 C27 C26 . . 104.8(14) ?
C29 C28 O6 . . 107.5(19) ?
C29 C28 H28A . . 110.2 ?
O6 C28 H28A . . 110.2 ?
C29 C28 H28B . . 110.2 ?
O6 C28 H28B . . 110.2 ?
H28A C28 H28B . . 108.5 ?
C28 C29 H29A . . 109.5 ?
C28 C29 H29B . . 109.5 ?
H29A C29 H29B . . 109.5 ?
C28 C29 H29C . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
N2 C1 N3 . . 130.7(2) ?
N2 C1 C8 . . 120.5(2) ?
N3 C1 C8 . . 108.75(19) ?
C7 C2 C3 . . 119.0(2) ?
C7 C2 C8 . . 132.0(2) ?
C3 C2 C8 . . 108.6(2) ?
C4 C3 C2 . . 123.1(2) ?
C4 C3 N3 . . 127.9(2) ?
C2 C3 N3 . . 108.9(2) ?
C3 C4 C5 . . 117.2(2) ?
C3 C4 H4 . . 121.4 ?
C5 C4 H4 . . 121.4 ?
C4 C5 C6 . . 120.9(2) ?
C4 C5 H5 . . 119.6 ?
C6 C5 H5 . . 119.6 ?
C5 C6 C7 . . 121.1(2) ?
C5 C6 H6 . . 119.5 ?
C7 C6 H6 . . 119.5 ?
C2 C7 C6 . . 118.7(2) ?
C2 C7 H7 . . 120.6 ?
C6 C7 H7 . . 120.6 ?
C2 C8 C1 . . 101.54(18) ?
C2 C8 C9 . . 112.15(18) ?
C1 C8 C9 . . 109.04(18) ?
C2 C8 C10 . . 119.15(19) ?
C1 C8 C10 . . 112.16(18) ?
C9 C8 C10 . . 102.78(18) ?
C11 C9 C8 . . 105.21(18) ?
C11 C9 H9A . . 110.7 ?
C8 C9 H9A . . 110.7 ?
C11 C9 H9B . . 110.7 ?
C8 C9 H9B . . 110.7 ?
H9A C9 H9B . . 108.8 ?
N1 C10 C13 . . 111.38(19) ?
N1 C10 C8 . . 103.07(17) ?
C13 C10 C8 . . 112.24(18) ?
N1 C10 H10 . . 110.0 ?
C13 C10 H10 . . 110.0 ?
C8 C10 H10 . . 110.0 ?
N1 C11 C9 . . 102.35(18) ?
N1 C11 H11A . . 111.3 ?
C9 C11 H11A . . 111.3 ?
N1 C11 H11B . . 111.3 ?
C9 C11 H11B . . 111.3 ?
H11A C11 H11B . . 109.2 ?
C13 C12 C17 . . 120.4(3) ?
C13 C12 H12 . . 119.8 ?
C17 C12 H12 . . 119.8 ?
C12 C13 C14 . . 119.0(2) ?
C12 C13 C10 . . 119.3(2) ?
C14 C13 C10 . . 121.4(2) ?
C15 C14 C13 . . 120.7(2) ?
C15 C14 H14 . . 119.6 ?
C13 C14 H14 . . 119.6 ?
C16 C15 C14 . . 120.0(3) ?
C16 C15 H15 . . 120.0 ?
C14 C15 H15 . . 120.0 ?
C15 C16 C17 . . 120.0(3) ?
C15 C16 H16 . . 120.0 ?
C17 C16 H16 . . 120.0 ?
C16 C17 C12 . . 120.0(3) ?
C16 C17 H17 . . 120.0 ?
C12 C17 H17 . . 120.0 ?
C19 C18 C24 . . 118.8(2) ?
C19 C18 H18 . . 120.6 ?
C24 C18 H18 . . 120.6 ?
C20 C19 C18 . . 121.9(3) ?
C20 C19 H19 . . 119.1 ?
C18 C19 H19 . . 119.1 ?
C19 C20 C22 . . 118.0(2) ?
C19 C20 C21 . . 120.9(3) ?
C22 C20 C21 . . 121.1(3) ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C20 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C23 C22 C20 . . 121.4(3) ?
C23 C22 H22 . . 119.3 ?
C20 C22 H22 . . 119.3 ?
C22 C23 C24 . . 119.6(2) ?
C22 C23 H23 . . 120.2 ?
C24 C23 H23 . . 120.2 ?
C23 C24 C18 . . 120.3(2) ?
C23 C24 S2 . . 120.7(2) ?
C18 C24 S2 . . 119.0(2) ?
S1 C25 H25A . . 109.5 ?
S1 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
S1 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
C11 N1 C10 . . 113.33(18) ?
C11 N1 S1 . . 119.93(16) ?
C10 N1 S1 . . 120.83(15) ?
C1 N2 S2 . . 122.91(18) ?
C1 N2 H2 . . 118.5 ?
S2 N2 H2 . . 118.5 ?
C1 N3 C3 . . 111.8(2) ?
C1 N3 H3 . . 124.1 ?
C3 N3 H3 . . 124.1 ?
O4 S1 O3 . . 119.15(15) ?
O4 S1 N1 . . 107.34(11) ?
O3 S1 N1 . . 106.06(11) ?
O4 S1 C25 . . 107.23(13) ?
O3 S1 C25 . . 108.31(15) ?
N1 S1 C25 . . 108.36(13) ?
O1 S2 O2 . . 117.40(12) ?
O1 S2 N2 . . 107.39(12) ?
O2 S2 N2 . . 112.61(11) ?
O1 S2 C24 . . 107.80(12) ?
O2 S2 C24 . . 107.51(12) ?
N2 S2 C24 . . 103.09(11) ?

