# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1044769'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), H2 O'
_chemical_formula_sum            'C50 H46 N2 O7 S2'
_chemical_formula_weight         851.01

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   13.412(4)
_cell_length_b                   13.544(3)
_cell_length_c                   14.951(4)
_cell_angle_alpha                113.82(2)
_cell_angle_beta                 90.15(2)
_cell_angle_gamma                111.63(2)
_cell_volume                     2272.8(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2312
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9635
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13476
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         27.56
_reflns_number_total             10365
_reflns_number_gt                6853
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0535P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10365
_refine_ls_number_parameters     574
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1406
_refine_ls_wR_factor_gt          0.1165
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.20210(4) 0.96224(4) 0.49849(4) 0.03324(14) Uani 1 1 d . . .
S2 S 0.21827(5) 0.29617(5) -0.18198(4) 0.04072(15) Uani 1 1 d . . .
O1 O 0.23761(14) 0.93195(13) 0.57118(10) 0.0527(4) Uani 1 1 d . . .
O1W O 0.44642(14) 0.23056(16) -0.31858(13) 0.0569(5) Uani 1 1 d D . .
H1W1 H 0.418(2) 0.276(2) -0.2831(15) 0.085 Uiso 1 1 d D . .
H1W2 H 0.4081(19) 0.189(2) -0.3768(10) 0.085 Uiso 1 1 d D . .
O2 O 0.09087(12) 0.95247(12) 0.49572(10) 0.0447(4) Uani 1 1 d . . .
O3 O 0.27565(12) 1.07934(12) 0.50950(11) 0.0435(4) Uani 1 1 d . . .
O4 O 0.13892(15) 0.28031(16) -0.25718(11) 0.0674(5) Uani 1 1 d . . .
O5 O 0.19360(14) 0.19131(13) -0.16591(12) 0.0566(5) Uani 1 1 d . . .
O6 O 0.32867(14) 0.34339(14) -0.19778(12) 0.0615(5) Uani 1 1 d . . .
N1 N 0.33179(15) 1.07629(15) 0.76692(12) 0.0371(4) Uani 1 1 d D . .
H1N1 H 0.2944(13) 1.0174(11) 0.7119(10) 0.056 Uiso 1 1 d D . .
H1N2 H 0.2894(13) 1.1117(15) 0.7938(13) 0.056 Uiso 1 1 d D . .
H1N3 H 0.3816(12) 1.1274(13) 0.7510(14) 0.056 Uiso 1 1 d D . .
N2 N 0.12809(14) 0.20170(14) -0.46087(12) 0.0342(4) Uani 1 1 d D . .
H2N1 H 0.1656(13) 0.1586(14) -0.4739(13) 0.051 Uiso 1 1 d D . .
H2N2 H 0.0591(8) 0.1509(14) -0.4780(13) 0.051 Uiso 1 1 d D . .
H2N3 H 0.1375(14) 0.2367(15) -0.3954(7) 0.051 Uiso 1 1 d D . .
C1 C 0.38220(17) 1.04436(18) 0.83559(14) 0.0354(5) Uani 1 1 d . . .
C2 C 0.29375(18) 0.93778(18) 0.84231(15) 0.0390(5) Uani 1 1 d . . .
C3 C 0.1889(2) 0.9305(2) 0.8485(2) 0.0613(7) Uani 1 1 d . . .
H3A H 0.1707 0.9895 0.8463 0.074 Uiso 1 1 calc R . .
C4 C 0.1102(2) 0.8356(3) 0.8578(2) 0.0821(10) Uani 1 1 d . . .
H4A H 0.0397 0.8314 0.8615 0.098 Uiso 1 1 calc R . .
C5 C 0.1359(3) 0.7481(3) 0.8616(2) 0.0852(10) Uani 1 1 d . . .
H5A H 0.0830 0.6845 0.8675 0.102 Uiso 1 1 calc R . .
C6 C 0.2393(3) 0.7551(3) 0.8565(2) 0.0803(9) Uani 1 1 d . . .
H6A H 0.2576 0.6968 0.8603 0.096 Uiso 1 1 calc R . .
C7 C 0.3175(2) 0.8485(2) 0.8459(2) 0.0596(7) Uani 1 1 d . . .
H7A H 0.3875 0.8511 0.8410 0.072 Uiso 1 1 calc R . .
C8 C 0.47592(18) 1.01512(19) 0.79205(16) 0.0386(5) Uani 1 1 d . . .
C9 C 0.4609(2) 0.9408(2) 0.69201(17) 0.0496(6) Uani 1 1 d . . .
H9A H 0.3948 0.9125 0.6510 0.060 Uiso 1 1 calc R . .
C10 C 0.5430(2) 0.9085(2) 0.6528(2) 0.0619(7) Uani 1 1 d . . .
H10A H 0.5326 0.8597 0.5854 0.074 Uiso 1 1 calc R . .
C11 C 0.6404(2) 0.9483(2) 0.7132(2) 0.0631(7) Uani 1 1 d . . .
H11A H 0.6954 0.9256 0.6868 0.076 Uiso 1 1 calc R . .
C12 C 0.6563(2) 1.0210(3) 0.8115(2) 0.0636(7) Uani 1 1 d . . .
H12A H 0.7223 1.0480 0.8521 0.076 Uiso 1 1 calc R . .
C13 C 0.5748(2) 1.0550(2) 0.85152(19) 0.0542(6) Uani 1 1 d . . .
H13A H 0.5865 1.1049 0.9188 0.065 Uiso 1 1 calc R . .
C14 C 0.42361(17) 1.15493(18) 0.93705(14) 0.0370(5) Uani 1 1 d . . .
C15 C 0.4107(2) 1.1442(2) 1.02418(16) 0.0504(6) Uani 1 1 d . . .
H15A H 0.3733 1.0704 1.0226 0.061 Uiso 1 1 calc R . .
C16 C 0.4536(2) 1.2445(2) 1.11526(18) 0.0662(8) Uani 1 1 d . . .
H16A H 0.4455 1.2364 1.1740 0.079 Uiso 1 1 calc R . .
C17 C 0.5074(2) 1.3541(2) 1.11919(19) 0.0639(7) Uani 1 1 d . . .
H17A H 0.5353 1.4202 1.1802 0.077 Uiso 1 1 calc R . .
C18 C 0.5200(2) 1.3659(2) 1.03231(19) 0.0623(7) Uani 1 1 d . . .
H18A H 0.5555 1.4402 1.0342 0.075 Uiso 1 1 calc R . .
C19 C 0.4794(2) 1.2666(2) 0.94206(17) 0.0518(6) Uani 1 1 d . . .
H19A H 0.4898 1.2749 0.8836 0.062 Uiso 1 1 calc R . .
C20 C 0.14698(17) 0.28545(17) -0.50869(15) 0.0359(5) Uani 1 1 d . . .
C21 C 0.05382(18) 0.32717(18) -0.49015(17) 0.0424(5) Uani 1 1 d . . .
C22 C 0.0397(2) 0.3834(2) -0.3942(2) 0.0598(7) Uani 1 1 d . . .
H22A H 0.0881 0.3979 -0.3412 0.072 Uiso 1 1 calc R . .
C23 C -0.0456(3) 0.4181(3) -0.3760(2) 0.0731(9) Uani 1 1 d . . .
H23A H -0.0535 0.4574 -0.3109 0.088 Uiso 1 1 calc R . .
C24 C -0.1188(2) 0.3949(3) -0.4538(3) 0.0750(9) Uani 1 1 d . . .
H24A H -0.1772 0.4170 -0.4416 0.090 Uiso 1 1 calc R . .
C25 C -0.1056(2) 0.3395(2) -0.5486(3) 0.0695(8) Uani 1 1 d . . .
H25A H -0.1549 0.3243 -0.6013 0.083 Uiso 1 1 calc R . .
C26 C -0.02000(19) 0.3058(2) -0.5674(2) 0.0529(6) Uani 1 1 d . . .
H26A H -0.0117 0.2683 -0.6327 0.064 Uiso 1 1 calc R . .
C27 C 0.14352(17) 0.21606(19) -0.61947(15) 0.0397(5) Uani 1 1 d . . .
C28 C 0.0774(2) 0.0961(2) -0.67214(17) 0.0507(6) Uani 1 1 d . . .
H28A H 0.0360 0.0553 -0.6386 0.061 Uiso 1 1 calc R . .
C29 C 0.0723(2) 0.0368(2) -0.77288(19) 0.0636(7) Uani 1 1 d . . .
H29A H 0.0281 -0.0433 -0.8066 0.076 Uiso 1 1 calc R . .
C30 C 0.1321(3) 0.0958(3) -0.8230(2) 0.0725(9) Uani 1 1 d . . .
H30A H 0.1293 0.0558 -0.8908 0.087 Uiso 1 1 calc R . .
C31 C 0.1969(2) 0.2149(3) -0.7729(2) 0.0734(9) Uani 1 1 d . . .
H31A H 0.2370 0.2551 -0.8075 0.088 Uiso 1 1 calc R . .
C32 C 0.2025(2) 0.2747(2) -0.67228(19) 0.0560(7) Uani 1 1 d . . .
H32A H 0.2461 0.3551 -0.6394 0.067 Uiso 1 1 calc R . .
C33 C 0.26008(18) 0.38641(18) -0.45811(15) 0.0382(5) Uani 1 1 d . . .
C34 C 0.34911(19) 0.3615(2) -0.44822(17) 0.0473(6) Uani 1 1 d . . .
H34A H 0.3399 0.2835 -0.4698 0.057 Uiso 1 1 calc R . .
C35 C 0.4520(2) 0.4510(2) -0.40663(18) 0.0601(7) Uani 1 1 d . . .
H35A H 0.5109 0.4326 -0.3993 0.072 Uiso 1 1 calc R . .
C36 C 0.4680(2) 0.5668(3) -0.37607(18) 0.0661(8) Uani 1 1 d . . .
H36A H 0.5376 0.6265 -0.3492 0.079 Uiso 1 1 calc R . .
C37 C 0.3822(3) 0.5932(2) -0.3853(2) 0.0719(9) Uani 1 1 d . . .
H37A H 0.3927 0.6715 -0.3645 0.086 Uiso 1 1 calc R . .
C38 C 0.2778(2) 0.5040(2) -0.42582(19) 0.0582(7) Uani 1 1 d . . .
H38A H 0.2192 0.5235 -0.4313 0.070 Uiso 1 1 calc R . .
C39 C 0.21050(17) 0.40612(17) -0.06944(14) 0.0380(5) Uani 1 1 d . . .
C40 C 0.2471(2) 0.4137(2) 0.01989(16) 0.0554(7) Uani 1 1 d . . .
H40A H 0.2712 0.3582 0.0216 0.066 Uiso 1 1 calc R . .
C41 C 0.2478(2) 0.5051(2) 0.10785(16) 0.0569(7) Uani 1 1 d . . .
H41A H 0.2732 0.5104 0.1682 0.068 Uiso 1 1 calc R . .
C42 C 0.21171(18) 0.58790(18) 0.10746(15) 0.0385(5) Uani 1 1 d . . .
C43 C 0.1744(2) 0.57746(19) 0.01660(15) 0.0480(6) Uani 1 1 d . . .
H43A H 0.1491 0.6320 0.0145 0.058 Uiso 1 1 calc R . .
C44 C 0.1739(2) 0.48747(19) -0.07146(16) 0.0471(6) Uani 1 1 d . . .
H44A H 0.1487 0.4822 -0.1319 0.057 Uiso 1 1 calc R . .
C45 C 0.21157(18) 0.68470(18) 0.20236(14) 0.0377(5) Uani 1 1 d . . .
C46 C 0.29474(18) 0.73687(19) 0.28390(15) 0.0445(6) Uani 1 1 d . . .
H46A H 0.3522 0.7132 0.2780 0.053 Uiso 1 1 calc R . .
C47 C 0.29302(18) 0.82288(19) 0.37299(15) 0.0421(5) Uani 1 1 d . . .
H47A H 0.3492 0.8574 0.4267 0.050 Uiso 1 1 calc R . .
C48 C 0.20756(16) 0.85746(16) 0.38208(14) 0.0316(4) Uani 1 1 d . . .
C49 C 0.12586(17) 0.80956(17) 0.30153(14) 0.0368(5) Uani 1 1 d . . .
H49A H 0.0696 0.8351 0.3070 0.044 Uiso 1 1 calc R . .
C50 C 0.12880(18) 0.72283(18) 0.21235(15) 0.0397(5) Uani 1 1 d . . .
H50A H 0.0735 0.6899 0.1583 0.048 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.4414(16) . ?
S1 O2 1.4472(15) . ?
S1 O3 1.4664(15) . ?
S1 C48 1.770(2) . ?
S2 O4 1.4398(16) . ?
S2 O6 1.4432(18) . ?
S2 O5 1.4539(17) . ?
S2 C39 1.775(2) . ?
O1W H1W1 0.85(2) . ?
O1W H1W2 0.85(2) . ?
N1 C1 1.506(3) . ?
N1 H1N1 0.86(2) . ?
N1 H1N2 0.86(2) . ?
N1 H1N3 0.88(2) . ?
N2 C20 1.519(2) . ?
N2 H2N1 0.86(2) . ?
N2 H2N2 0.88(2) . ?
N2 H2N3 0.88(2) . ?
C1 C8 1.524(3) . ?
C1 C2 1.535(3) . ?
C1 C14 1.549(3) . ?
C2 C3 1.379(3) . ?
C2 C7 1.380(3) . ?
C3 C4 1.390(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.372(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.360(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.382(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.385(3) . ?
C8 C9 1.387(3) . ?
C9 C10 1.378(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.377(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.360(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.385(3) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.372(3) . ?
C14 C19 1.389(3) . ?
C15 C16 1.398(3) . ?
C15 H15A 0.9300 . ?
C16 C17 1.367(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.375(3) . ?
C17 H17A 0.9300 . ?
C18 C19 1.384(3) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C27 1.529(3) . ?
C20 C21 1.534(3) . ?
C20 C33 1.540(3) . ?
C21 C22 1.378(3) . ?
C21 C26 1.383(3) . ?
C22 C23 1.378(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.373(4) . ?
C23 H23A 0.9300 . ?
C24 C25 1.358(4) . ?
C24 H24A 0.9300 . ?
C25 C26 1.375(3) . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9300 . ?
C27 C32 1.388(3) . ?
C27 C28 1.396(3) . ?
C28 C29 1.378(3) . ?
C28 H28A 0.9300 . ?
C29 C30 1.362(4) . ?
C29 H29A 0.9300 . ?
C30 C31 1.381(4) . ?
C30 H30A 0.9300 . ?
C31 C32 1.377(4) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
C33 C34 1.378(3) . ?
C33 C38 1.387(3) . ?
C34 C35 1.383(3) . ?
C34 H34A 0.9300 . ?
C35 C36 1.374(4) . ?
C35 H35A 0.9300 . ?
C36 C37 1.346(4) . ?
C36 H36A 0.9300 . ?
C37 C38 1.395(4) . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9300 . ?
C39 C44 1.372(3) . ?
C39 C40 1.373(3) . ?
C40 C41 1.393(3) . ?
C40 H40A 0.9300 . ?
C41 C42 1.377(3) . ?
C41 H41A 0.9300 . ?
C42 C43 1.380(3) . ?
C42 C45 1.494(3) . ?
C43 C44 1.384(3) . ?
C43 H43A 0.9300 . ?
C44 H44A 0.9300 . ?
C45 C50 1.372(3) . ?
C45 C46 1.395(3) . ?
C46 C47 1.378(3) . ?
C46 H46A 0.9300 . ?
C47 C48 1.377(3) . ?
C47 H47A 0.9300 . ?
C48 C49 1.382(3) . ?
C49 C50 1.389(3) . ?
C49 H49A 0.9300 . ?
C50 H50A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 S1 O2 113.99(10) . . ?
O1 S1 O3 112.33(10) . . ?
O2 S1 O3 110.18(9) . . ?
O1 S1 C48 105.41(9) . . ?
O2 S1 C48 107.03(9) . . ?
O3 S1 C48 107.45(9) . . ?
O4 S2 O6 112.81(12) . . ?
O4 S2 O5 113.08(11) . . ?
O6 S2 O5 112.43(11) . . ?
O4 S2 C39 105.85(10) . . ?
O6 S2 C39 105.55(10) . . ?
O5 S2 C39 106.37(10) . . ?
H1W1 O1W H1W2 109.2(15) . . ?
C1 N1 H1N1 114.3(14) . . ?
C1 N1 H1N2 113.2(14) . . ?
H1N1 N1 H1N2 106.9(13) . . ?
C1 N1 H1N3 111.6(15) . . ?
H1N1 N1 H1N3 106.2(13) . . ?
H1N2 N1 H1N3 103.9(12) . . ?
C20 N2 H2N1 118.4(14) . . ?
C20 N2 H2N2 110.2(13) . . ?
H2N1 N2 H2N2 105.1(12) . . ?
C20 N2 H2N3 113.7(13) . . ?
H2N1 N2 H2N3 105.0(12) . . ?
H2N2 N2 H2N3 103.0(12) . . ?
N1 C1 C8 107.75(16) . . ?
N1 C1 C2 108.02(17) . . ?
C8 C1 C2 111.43(17) . . ?
N1 C1 C14 105.93(16) . . ?
C8 C1 C14 111.44(17) . . ?
C2 C1 C14 111.97(17) . . ?
C3 C2 C7 117.9(2) . . ?
C3 C2 C1 120.9(2) . . ?
C7 C2 C1 121.1(2) . . ?
C2 C3 C4 120.5(3) . . ?
C2 C3 H3A 119.7 . . ?
C4 C3 H3A 119.7 . . ?
C5 C4 C3 120.5(3) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C6 C5 C4 119.4(3) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C5 C6 C7 120.3(3) . . ?
C5 C6 H6A 119.8 . . ?
C7 C6 H6A 119.8 . . ?
C2 C7 C6 121.3(3) . . ?
C2 C7 H7A 119.3 . . ?
C6 C7 H7A 119.3 . . ?
C13 C8 C9 118.5(2) . . ?
C13 C8 C1 121.4(2) . . ?
C9 C8 C1 120.0(2) . . ?
C10 C9 C8 120.6(2) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C11 C12 C13 120.4(3) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C8 C13 C12 120.4(2) . . ?
C8 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C15 C14 C19 118.5(2) . . ?
C15 C14 C1 120.8(2) . . ?
C19 C14 C1 120.66(19) . . ?
C14 C15 C16 120.0(2) . . ?
C14 C15 H15A 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C17 C16 C15 121.0(2) . . ?
C17 C16 H16A 119.5 . . ?
C15 C16 H16A 119.5 . . ?
C16 C17 C18 119.5(2) . . ?
C16 C17 H17A 120.2 . . ?
C18 C17 H17A 120.2 . . ?
C17 C18 C19 119.7(2) . . ?
C17 C18 H18A 120.2 . . ?
C19 C18 H18A 120.2 . . ?
C18 C19 C14 121.3(2) . . ?
C18 C19 H19A 119.3 . . ?
C14 C19 H19A 119.3 . . ?
N2 C20 C27 107.59(16) . . ?
N2 C20 C21 105.68(16) . . ?
C27 C20 C21 111.98(17) . . ?
N2 C20 C33 106.99(16) . . ?
C27 C20 C33 111.18(17) . . ?
C21 C20 C33 113.00(17) . . ?
C22 C21 C26 118.4(2) . . ?
C22 C21 C20 119.7(2) . . ?
C26 C21 C20 121.8(2) . . ?
C23 C22 C21 120.6(3) . . ?
C23 C22 H22A 119.7 . . ?
C21 C22 H22A 119.7 . . ?
C24 C23 C22 120.1(3) . . ?
C24 C23 H23A 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H24A 120.1 . . ?
C23 C24 H24A 120.1 . . ?
C24 C25 C26 120.6(3) . . ?
C24 C25 H25A 119.7 . . ?
C26 C25 H25A 119.7 . . ?
C25 C26 C21 120.6(3) . . ?
C25 C26 H26A 119.7 . . ?
C21 C26 H26A 119.7 . . ?
C32 C27 C28 117.8(2) . . ?
C32 C27 C20 119.5(2) . . ?
C28 C27 C20 122.5(2) . . ?
C29 C28 C27 121.4(2) . . ?
C29 C28 H28A 119.3 . . ?
C27 C28 H28A 119.3 . . ?
C30 C29 C28 119.9(3) . . ?
C30 C29 H29A 120.1 . . ?
C28 C29 H29A 120.1 . . ?
C29 C30 C31 120.0(3) . . ?
C29 C30 H30A 120.0 . . ?
C31 C30 H30A 120.0 . . ?
C32 C31 C30 120.5(3) . . ?
C32 C31 H31A 119.7 . . ?
C30 C31 H31A 119.7 . . ?
C31 C32 C27 120.5(3) . . ?
C31 C32 H32A 119.7 . . ?
C27 C32 H32A 119.7 . . ?
C34 C33 C38 117.6(2) . . ?
C34 C33 C20 120.18(19) . . ?
C38 C33 C20 122.2(2) . . ?
C33 C34 C35 120.9(2) . . ?
C33 C34 H34A 119.6 . . ?
C35 C34 H34A 119.6 . . ?
C36 C35 C34 120.6(3) . . ?
C36 C35 H35A 119.7 . . ?
C34 C35 H35A 119.7 . . ?
C37 C36 C35 119.5(3) . . ?
C37 C36 H36A 120.3 . . ?
C35 C36 H36A 120.3 . . ?
C36 C37 C38 120.5(3) . . ?
C36 C37 H37A 119.8 . . ?
C38 C37 H37A 119.8 . . ?
C33 C38 C37 120.9(3) . . ?
C33 C38 H38A 119.5 . . ?
C37 C38 H38A 119.5 . . ?
C44 C39 C40 119.97(19) . . ?
C44 C39 S2 120.21(16) . . ?
C40 C39 S2 119.72(17) . . ?
C39 C40 C41 119.4(2) . . ?
C39 C40 H40A 120.3 . . ?
C41 C40 H40A 120.3 . . ?
C42 C41 C40 121.5(2) . . ?
C42 C41 H41A 119.2 . . ?
C40 C41 H41A 119.2 . . ?
C41 C42 C43 117.79(19) . . ?
C41 C42 C45 121.01(19) . . ?
C43 C42 C45 121.2(2) . . ?
C42 C43 C44 121.3(2) . . ?
C42 C43 H43A 119.3 . . ?
C44 C43 H43A 119.3 . . ?
C39 C44 C43 120.0(2) . . ?
C39 C44 H44A 120.0 . . ?
C43 C44 H44A 120.0 . . ?
C50 C45 C46 118.33(18) . . ?
C50 C45 C42 121.05(19) . . ?
C46 C45 C42 120.60(19) . . ?
C47 C46 C45 121.0(2) . . ?
C47 C46 H46A 119.5 . . ?
C45 C46 H46A 119.5 . . ?
C48 C47 C46 119.60(19) . . ?
C48 C47 H47A 120.2 . . ?
C46 C47 H47A 120.2 . . ?
C47 C48 C49 120.42(18) . . ?
C47 C48 S1 119.38(15) . . ?
C49 C48 S1 120.19(16) . . ?
C48 C49 C50 119.2(2) . . ?
C48 C49 H49A 120.4 . . ?
C50 C49 H49A 120.4 . . ?
C45 C50 C49 121.40(19) . . ?
C45 C50 H50A 119.3 . . ?
C49 C50 H50A 119.3 . . ?

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
N1 C1 C2 C3 -40.8(3) . . . . ?
C8 C1 C2 C3 -159.0(2) . . . . ?
C14 C1 C2 C3 75.4(3) . . . . ?
N1 C1 C2 C7 141.4(2) . . . . ?
C8 C1 C2 C7 23.3(3) . . . . ?
C14 C1 C2 C7 -102.3(2) . . . . ?
C7 C2 C3 C4 -0.1(4) . . . . ?
C1 C2 C3 C4 -177.9(2) . . . . ?
C2 C3 C4 C5 0.4(5) . . . . ?
C3 C4 C5 C6 0.3(5) . . . . ?
C4 C5 C6 C7 -1.2(5) . . . . ?
C3 C2 C7 C6 -0.8(4) . . . . ?
C1 C2 C7 C6 177.0(2) . . . . ?
C5 C6 C7 C2 1.5(5) . . . . ?
N1 C1 C8 C13 137.4(2) . . . . ?
C2 C1 C8 C13 -104.3(2) . . . . ?
C14 C1 C8 C13 21.6(3) . . . . ?
N1 C1 C8 C9 -46.9(3) . . . . ?
C2 C1 C8 C9 71.4(2) . . . . ?
C14 C1 C8 C9 -162.73(19) . . . . ?
C13 C8 C9 C10 -0.6(4) . . . . ?
C1 C8 C9 C10 -176.5(2) . . . . ?
C8 C9 C10 C11 1.1(4) . . . . ?
C9 C10 C11 C12 -0.9(4) . . . . ?
C10 C11 C12 C13 0.2(4) . . . . ?
C9 C8 C13 C12 -0.1(4) . . . . ?
C1 C8 C13 C12 175.7(2) . . . . ?
C11 C12 C13 C8 0.2(4) . . . . ?
N1 C1 C14 C15 138.9(2) . . . . ?
C8 C1 C14 C15 -104.2(2) . . . . ?
C2 C1 C14 C15 21.4(3) . . . . ?
N1 C1 C14 C19 -44.3(3) . . . . ?
C8 C1 C14 C19 72.6(3) . . . . ?
C2 C1 C14 C19 -161.8(2) . . . . ?
C19 C14 C15 C16 -0.3(4) . . . . ?
C1 C14 C15 C16 176.6(2) . . . . ?
C14 C15 C16 C17 1.0(4) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
C16 C17 C18 C19 -0.9(4) . . . . ?
C17 C18 C19 C14 1.6(4) . . . . ?
C15 C14 C19 C18 -1.0(4) . . . . ?
C1 C14 C19 C18 -177.9(2) . . . . ?
N2 C20 C21 C22 58.3(3) . . . . ?
C27 C20 C21 C22 175.1(2) . . . . ?
C33 C20 C21 C22 -58.4(3) . . . . ?
N2 C20 C21 C26 -119.0(2) . . . . ?
C27 C20 C21 C26 -2.2(3) . . . . ?
C33 C20 C21 C26 124.3(2) . . . . ?
C26 C21 C22 C23 -0.5(4) . . . . ?
C20 C21 C22 C23 -177.9(2) . . . . ?
C21 C22 C23 C24 1.3(4) . . . . ?
C22 C23 C24 C25 -1.3(4) . . . . ?
C23 C24 C25 C26 0.5(4) . . . . ?
C24 C25 C26 C21 0.3(4) . . . . ?
C22 C21 C26 C25 -0.3(4) . . . . ?
C20 C21 C26 C25 177.0(2) . . . . ?
N2 C20 C27 C32 -151.8(2) . . . . ?
C21 C20 C27 C32 92.5(2) . . . . ?
C33 C20 C27 C32 -34.9(3) . . . . ?
N2 C20 C27 C28 32.5(3) . . . . ?
C21 C20 C27 C28 -83.2(2) . . . . ?
C33 C20 C27 C28 149.3(2) . . . . ?
C32 C27 C28 C29 1.3(3) . . . . ?
C20 C27 C28 C29 177.1(2) . . . . ?
C27 C28 C29 C30 -0.4(4) . . . . ?
C28 C29 C30 C31 -0.6(4) . . . . ?
C29 C30 C31 C32 0.6(5) . . . . ?
C30 C31 C32 C27 0.4(4) . . . . ?
C28 C27 C32 C31 -1.3(4) . . . . ?
C20 C27 C32 C31 -177.2(2) . . . . ?
N2 C20 C33 C34 49.5(2) . . . . ?
C27 C20 C33 C34 -67.7(2) . . . . ?
C21 C20 C33 C34 165.36(19) . . . . ?
N2 C20 C33 C38 -134.0(2) . . . . ?
C27 C20 C33 C38 108.8(2) . . . . ?
C21 C20 C33 C38 -18.1(3) . . . . ?
C38 C33 C34 C35 0.6(3) . . . . ?
C20 C33 C34 C35 177.3(2) . . . . ?
C33 C34 C35 C36 -1.3(4) . . . . ?
C34 C35 C36 C37 1.1(4) . . . . ?
C35 C36 C37 C38 -0.2(4) . . . . ?
C34 C33 C38 C37 0.3(4) . . . . ?
C20 C33 C38 C37 -176.4(2) . . . . ?
C36 C37 C38 C33 -0.5(4) . . . . ?
O4 S2 C39 C44 -25.6(2) . . . . ?
O6 S2 C39 C44 94.2(2) . . . . ?
O5 S2 C39 C44 -146.15(19) . . . . ?
O4 S2 C39 C40 158.1(2) . . . . ?
O6 S2 C39 C40 -82.1(2) . . . . ?
O5 S2 C39 C40 37.6(2) . . . . ?
C44 C39 C40 C41 -0.7(4) . . . . ?
S2 C39 C40 C41 175.6(2) . . . . ?
C39 C40 C41 C42 0.5(4) . . . . ?
C40 C41 C42 C43 0.1(4) . . . . ?
C40 C41 C42 C45 179.2(2) . . . . ?
C41 C42 C43 C44 -0.5(4) . . . . ?
C45 C42 C43 C44 -179.6(2) . . . . ?
C40 C39 C44 C43 0.3(4) . . . . ?
S2 C39 C44 C43 -175.95(18) . . . . ?
C42 C43 C44 C39 0.3(4) . . . . ?
C41 C42 C45 C50 -142.3(2) . . . . ?
C43 C42 C45 C50 36.8(3) . . . . ?
C41 C42 C45 C46 36.3(3) . . . . ?
C43 C42 C45 C46 -144.6(2) . . . . ?
C50 C45 C46 C47 1.3(3) . . . . ?
C42 C45 C46 C47 -177.3(2) . . . . ?
C45 C46 C47 C48 0.5(4) . . . . ?
C46 C47 C48 C49 -2.3(3) . . . . ?
C46 C47 C48 S1 176.66(17) . . . . ?
O1 S1 C48 C47 -39.6(2) . . . . ?
O2 S1 C48 C47 -161.31(17) . . . . ?
O3 S1 C48 C47 80.37(19) . . . . ?
O1 S1 C48 C49 139.40(18) . . . . ?
O2 S1 C48 C49 17.7(2) . . . . ?
O3 S1 C48 C49 -100.62(18) . . . . ?
C47 C48 C49 C50 2.5(3) . . . . ?
S1 C48 C49 C50 -176.55(16) . . . . ?
C46 C45 C50 C49 -1.2(3) . . . . ?
C42 C45 C50 C49 177.5(2) . . . . ?
C48 C49 C50 C45 -0.7(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O6 0.85(2) 1.941(12) 2.767(2) 165(3) .
O1W H1W2 O3 0.85(2) 2.062(14) 2.882(2) 161(3) 1_544
N1 H1N1 O1 0.86(2) 1.928(12) 2.743(2) 157.7(18) .
N1 H1N2 O5 0.86(2) 1.917(10) 2.783(2) 171(2) 1_566
N1 H1N3 O1W 0.88(2) 2.018(13) 2.857(3) 158.9(19) 1_566
N2 H2N1 O3 0.86(2) 2.085(9) 2.948(2) 171.2(17) 1_544
N2 H2N2 O2 0.88(2) 1.923(10) 2.801(2) 172.0(17) 2_565
N2 H2N3 O4 0.88(2) 1.904(10) 2.774(2) 168.1(19) .

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.051
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1044770'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), C H4 O'
_chemical_formula_sum            'C51 H48 N2 O7 S2'
_chemical_formula_weight         865.03

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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   15.2630(4)
_cell_length_b                   15.5332(3)
_cell_length_c                   19.3594(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.221(3)
_cell_angle_gamma                90.00
_cell_volume                     4517.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4412
_cell_measurement_theta_min      3.35
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9614
_exptl_absorpt_correction_T_max  0.9729
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17314
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         27.56
_reflns_number_total             10303
_reflns_number_gt                7147
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0507P)²+1.4502P] where P=(Fo²+2Fc²)/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         10303
_refine_ls_number_parameters     581
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1320
_refine_ls_wR_factor_gt          0.1157
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.47972(3) 0.38402(3) 0.12606(3) 0.03519(13) Uani 1 1 d . . .
S2 S 0.44793(4) -0.29891(3) 0.12363(3) 0.04034(14) Uani 1 1 d . . .
O1 O 0.43042(10) 0.40689(9) 0.18095(8) 0.0478(4) Uani 1 1 d . . .
O2 O 0.43729(12) 0.41284(9) 0.05691(8) 0.0560(4) Uani 1 1 d . . .
O3 O 0.57246(10) 0.40914(9) 0.14235(9) 0.0498(4) Uani 1 1 d . . .
O4 O 0.35657(11) -0.31853(11) 0.12791(11) 0.0701(6) Uani 1 1 d . . .
O5 O 0.47072(15) -0.32849(10) 0.05865(10) 0.0723(6) Uani 1 1 d . . .
O6 O 0.51009(10) -0.32602(9) 0.18542(8) 0.0475(4) Uani 1 1 d . . .
O7 O 0.26909(15) -0.35145(17) 0.24096(12) 0.0880(7) Uani 1 1 d D . .
H7O H 0.288(3) -0.335(3) 0.2043(14) 0.132 Uiso 1 1 d D . .
N1 N 0.64461(10) 0.45428(11) 0.02002(10) 0.0358(4) Uani 1 1 d D . .
H1N1 H 0.6233(13) 0.5008(8) -0.0018(9) 0.054 Uiso 1 1 d D . .
H1N2 H 0.6171(13) 0.4468(12) 0.0547(7) 0.054 Uiso 1 1 d D . .
H1N3 H 0.6303(14) 0.4121(9) -0.0091(8) 0.054 Uiso 1 1 d D . .
N2 N 0.43256(11) -0.44458(11) 0.26475(9) 0.0366(4) Uani 1 1 d D . .
H2N1 H 0.4645(11) -0.4080(9) 0.2458(11) 0.055 Uiso 1 1 d D . .
H2N2 H 0.3785(7) -0.4249(11) 0.2569(12) 0.055 Uiso 1 1 d D . .
H2N3 H 0.4326(12) -0.4922(8) 0.2418(11) 0.055 Uiso 1 1 d D . .
C1 C 0.74358(12) 0.46173(12) 0.04662(11) 0.0324(4) Uani 1 1 d . . .
C2 C 0.76217(13) 0.54794(13) 0.08488(11) 0.0346(4) Uani 1 1 d . . .
C3 C 0.84985(15) 0.57556(16) 0.10335(13) 0.0520(6) Uani 1 1 d . . .
H3A H 0.8956 0.5406 0.0936 0.062 Uiso 1 1 calc R . .
C4 C 0.87027(18) 0.65387(18) 0.13589(15) 0.0653(8) Uani 1 1 d . . .
H4A H 0.9293 0.6712 0.1478 0.078 Uiso 1 1 calc R . .
C5 C 0.80347(19) 0.70616(18) 0.15063(15) 0.0691(8) Uani 1 1 d . . .
H5A H 0.8168 0.7594 0.1720 0.083 Uiso 1 1 calc R . .
C6 C 0.71718(19) 0.67903(19) 0.13354(16) 0.0766(9) Uani 1 1 d . . .
H6A H 0.6718 0.7141 0.1438 0.092 Uiso 1 1 calc R . .
C7 C 0.69604(15) 0.60064(16) 0.10129(14) 0.0563(7) Uani 1 1 d . . .
H7A H 0.6369 0.5833 0.0905 0.068 Uiso 1 1 calc R . .
C8 C 0.79212(13) 0.46058(13) -0.01653(11) 0.0370(5) Uani 1 1 d . . .
C9 C 0.86979(16) 0.41382(17) -0.01514(15) 0.0593(7) Uani 1 1 d . . .
H9A H 0.8912 0.3793 0.0234 0.071 Uiso 1 1 calc R . .
C10 C 0.9157(2) 0.4180(2) -0.07052(19) 0.0758(9) Uani 1 1 d . . .
H10A H 0.9677 0.3863 -0.0690 0.091 Uiso 1 1 calc R . .
C11 C 0.8850(2) 0.4686(2) -0.12758(18) 0.0773(9) Uani 1 1 d . . .
H11A H 0.9161 0.4713 -0.1647 0.093 Uiso 1 1 calc R . .
C12 C 0.8084(2) 0.51510(19) -0.12982(15) 0.0676(8) Uani 1 1 d . . .
H12A H 0.7871 0.5490 -0.1688 0.081 Uiso 1 1 calc R . .
C13 C 0.76254(16) 0.51174(15) -0.07427(13) 0.0501(6) Uani 1 1 d . . .
H13A H 0.7111 0.5444 -0.0759 0.060 Uiso 1 1 calc R . .
C14 C 0.76641(13) 0.38272(13) 0.09429(12) 0.0380(5) Uani 1 1 d . . .
C15 C 0.80084(15) 0.38874(16) 0.16492(13) 0.0506(6) Uani 1 1 d . . .
H15A H 0.8147 0.4424 0.1852 0.061 Uiso 1 1 calc R . .
C16 C 0.81492(17) 0.3148(2) 0.20609(15) 0.0660(8) Uani 1 1 d . . .
H16A H 0.8386 0.3196 0.2536 0.079 Uiso 1 1 calc R . .
C17 C 0.79446(19) 0.2360(2) 0.17764(19) 0.0727(9) Uani 1 1 d . . .
H17A H 0.8041 0.1870 0.2056 0.087 Uiso 1 1 calc R . .
C18 C 0.7598(2) 0.22885(17) 0.10803(19) 0.0731(8) Uani 1 1 d . . .
H18A H 0.7451 0.1749 0.0886 0.088 Uiso 1 1 calc R . .
C19 C 0.74613(16) 0.30167(15) 0.06603(15) 0.0558(6) Uani 1 1 d . . .
H19A H 0.7232 0.2960 0.0184 0.067 Uiso 1 1 calc R . .
C20 C 0.46456(13) -0.45856(12) 0.34241(10) 0.0331(4) Uani 1 1 d . . .
C21 C 0.56472(13) -0.47603(12) 0.35581(11) 0.0352(5) Uani 1 1 d . . .
C22 C 0.61345(14) -0.46454(14) 0.42281(12) 0.0426(5) Uani 1 1 d . . .
H22A H 0.5857 -0.4416 0.4577 0.051 Uiso 1 1 calc R . .
C23 C 0.70243(15) -0.48664(15) 0.43858(14) 0.0525(6) Uani 1 1 d . . .
H23A H 0.7337 -0.4792 0.4840 0.063 Uiso 1 1 calc R . .
C24 C 0.74490(17) -0.51949(18) 0.38781(16) 0.0638(7) Uani 1 1 d . . .
H24A H 0.8047 -0.5347 0.3983 0.077 Uiso 1 1 calc R . .
C25 C 0.69740(18) -0.52961(19) 0.32094(17) 0.0719(8) Uani 1 1 d . . .
H25A H 0.7260 -0.5510 0.2859 0.086 Uiso 1 1 calc R . .
C26 C 0.60794(16) -0.50866(16) 0.30464(14) 0.0545(6) Uani 1 1 d . . .
H26A H 0.5770 -0.5166 0.2592 0.065 Uiso 1 1 calc R . .
C27 C 0.41194(14) -0.53673(13) 0.36239(11) 0.0378(5) Uani 1 1 d . . .
C28 C 0.45326(16) -0.60542(14) 0.39914(13) 0.0506(6) Uani 1 1 d . . .
H28A H 0.5149 -0.6059 0.4118 0.061 Uiso 1 1 calc R . .
C29 C 0.4041(2) -0.67442(16) 0.41771(15) 0.0667(8) Uani 1 1 d . . .
H29A H 0.4331 -0.7199 0.4434 0.080 Uiso 1 1 calc R . .
C30 C 0.3140(2) -0.67601(18) 0.39858(15) 0.0703(8) Uani 1 1 d . . .
H30A H 0.2815 -0.7224 0.4109 0.084 Uiso 1 1 calc R . .
C31 C 0.27154(18) -0.6084(2) 0.36095(16) 0.0717(8) Uani 1 1 d . . .
H31A H 0.2100 -0.6094 0.3474 0.086 Uiso 1 1 calc R . .
C32 C 0.31984(16) -0.53873(17) 0.34305(14) 0.0586(7) Uani 1 1 d . . .
H32A H 0.2904 -0.4930 0.3179 0.070 Uiso 1 1 calc R . .
C33 C 0.44322(13) -0.37509(13) 0.37898(11) 0.0368(5) Uani 1 1 d . . .
C34 C 0.39275(16) -0.37337(16) 0.43182(12) 0.0510(6) Uani 1 1 d . . .
H34A H 0.3709 -0.4245 0.4471 0.061 Uiso 1 1 calc R . .
C35 C 0.37451(19) -0.2959(2) 0.46226(15) 0.0679(8) Uani 1 1 d . . .
H35A H 0.3406 -0.2956 0.4977 0.082 Uiso 1 1 calc R . .
C36 C 0.4059(2) -0.22027(18) 0.44046(16) 0.0705(8) Uani 1 1 d . . .
H36A H 0.3928 -0.1685 0.4604 0.085 Uiso 1 1 calc R . .
C37 C 0.4570(2) -0.22096(16) 0.38894(15) 0.0653(7) Uani 1 1 d . . .
H37A H 0.4789 -0.1695 0.3743 0.078 Uiso 1 1 calc R . .
C38 C 0.47634(16) -0.29747(14) 0.35865(13) 0.0488(6) Uani 1 1 d . . .
H38A H 0.5119 -0.2971 0.3243 0.059 Uiso 1 1 calc R . .
C39 C 0.47716(13) 0.27004(12) 0.12175(11) 0.0337(4) Uani 1 1 d . . .
C40 C 0.53958(16) 0.22298(14) 0.16586(14) 0.0572(7) Uani 1 1 d . . .
H40A H 0.5846 0.2508 0.1964 0.069 Uiso 1 1 calc R . .
C41 C 0.53536(16) 0.13352(14) 0.16483(15) 0.0597(7) Uani 1 1 d . . .
H41A H 0.5777 0.1020 0.1951 0.072 Uiso 1 1 calc R . .
C42 C 0.46921(14) 0.09061(12) 0.11958(12) 0.0391(5) Uani 1 1 d . . .
C43 C 0.40843(15) 0.13943(14) 0.07437(13) 0.0522(6) Uani 1 1 d . . .
H43A H 0.3640 0.1119 0.0430 0.063 Uiso 1 1 calc R . .
C44 C 0.41248(15) 0.22866(13) 0.07485(13) 0.0502(6) Uani 1 1 d . . .
H44A H 0.3716 0.2604 0.0436 0.060 Uiso 1 1 calc R . .
C45 C 0.46385(14) -0.00514(12) 0.12015(12) 0.0391(5) Uani 1 1 d . . .
C46 C 0.48326(16) -0.05021(13) 0.18308(13) 0.0503(6) Uani 1 1 d . . .
H46A H 0.4997 -0.0202 0.2249 0.060 Uiso 1 1 calc R . .
C47 C 0.47838(16) -0.13962(13) 0.18424(12) 0.0472(6) Uani 1 1 d . . .
H47A H 0.4904 -0.1690 0.2267 0.057 Uiso 1 1 calc R . .
C48 C 0.45558(13) -0.18476(12) 0.12193(11) 0.0344(4) Uani 1 1 d . . .
C49 C 0.43658(15) -0.14127(13) 0.05923(12) 0.0419(5) Uani 1 1 d . . .
H49A H 0.4217 -0.1715 0.0173 0.050 Uiso 1 1 calc R . .
C50 C 0.43979(15) -0.05166(13) 0.05881(12) 0.0437(5) Uani 1 1 d . . .
H50A H 0.4254 -0.0225 0.0164 0.052 Uiso 1 1 calc R . .
C51 C 0.2182(3) -0.2960(3) 0.2732(2) 0.1268(16) Uani 1 1 d . . .
H51A H 0.2446 -0.2397 0.2763 0.190 Uiso 1 1 calc R . .
H51B H 0.2156 -0.3167 0.3195 0.190 Uiso 1 1 calc R . .
H51C H 0.1591 -0.2930 0.2462 0.190 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.4481(15) . ?
S1 O2 1.4505(16) . ?
S1 O1 1.4509(15) . ?
S1 C39 1.7726(19) . ?
S2 O5 1.4386(18) . ?
S2 O4 1.4440(17) . ?
S2 O6 1.4512(16) . ?
S2 C48 1.7776(19) . ?
O7 C51 1.381(4) . ?
O7 H7O 0.85(3) . ?
N1 C1 1.511(2) . ?
N1 H1N1 0.86(2) . ?
N1 H1N2 0.86(2) . ?
N1 H1N3 0.86(2) . ?
N2 C20 1.512(3) . ?
N2 H2N1 0.86(2) . ?
N2 H2N2 0.86(2) . ?
N2 H2N3 0.86(2) . ?
C1 C2 1.532(3) . ?
C1 C14 1.538(3) . ?
C1 C8 1.538(3) . ?
C2 C7 1.380(3) . ?
C2 C3 1.390(3) . ?
C3 C4 1.380(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.373(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.366(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.380(3) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.380(3) . ?
C8 C9 1.386(3) . ?
C9 C10 1.383(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.368(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.370(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.384(3) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.378(3) . ?
C14 C19 1.386(3) . ?
C15 C16 1.392(3) . ?
C15 H15A 0.9300 . ?
C16 C17 1.356(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.362(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.387(3) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.529(3) . ?
C20 C33 1.540(3) . ?
C20 C27 1.542(3) . ?
C21 C26 1.380(3) . ?
C21 C22 1.387(3) . ?
C22 C23 1.381(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.368(4) . ?
C23 H23A 0.9300 . ?
C24 C25 1.376(4) . ?
C24 H24A 0.9300 . ?
C25 C26 1.385(3) . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9300 . ?
C27 C28 1.372(3) . ?
C27 C32 1.389(3) . ?
C28 C29 1.392(3) . ?
C28 H28A 0.9300 . ?
C29 C30 1.359(4) . ?
C29 H29A 0.9300 . ?
C30 C31 1.373(4) . ?
C30 H30A 0.9300 . ?
C31 C32 1.388(3) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
C33 C34 1.386(3) . ?
C33 C38 1.391(3) . ?
C34 C35 1.389(3) . ?
C34 H34A 0.9300 . ?
C35 C36 1.364(4) . ?
C35 H35A 0.9300 . ?
C36 C37 1.371(4) . ?
C36 H36A 0.9300 . ?
C37 C38 1.380(3) . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9300 . ?
C39 C40 1.372(3) . ?
C39 C44 1.376(3) . ?
C40 C41 1.391(3) . ?
C40 H40A 0.9300 . ?
C41 C42 1.385(3) . ?
C41 H41A 0.9300 . ?
C42 C43 1.383(3) . ?
C42 C45 1.490(3) . ?
C43 C44 1.387(3) . ?
C43 H43A 0.9300 . ?
C44 H44A 0.9300 . ?
C45 C50 1.383(3) . ?
C45 C46 1.391(3) . ?
C46 C47 1.391(3) . ?
C46 H46A 0.9300 . ?
C47 C48 1.385(3) . ?
C47 H47A 0.9300 . ?
C48 C49 1.374(3) . ?
C49 C50 1.393(3) . ?
C49 H49A 0.9300 . ?
C50 H50A 0.9300 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?

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
O3 S1 O2 112.14(10) . . ?
O3 S1 O1 112.86(10) . . ?
O2 S1 O1 113.31(10) . . ?
O3 S1 C39 106.97(9) . . ?
O2 S1 C39 105.21(10) . . ?
O1 S1 C39 105.61(9) . . ?
O5 S2 O4 111.63(13) . . ?
O5 S2 O6 113.83(11) . . ?
O4 S2 O6 112.85(10) . . ?
O5 S2 C48 105.99(10) . . ?
O4 S2 C48 106.19(10) . . ?
O6 S2 C48 105.61(9) . . ?
C51 O7 H7O 120(3) . . ?
C1 N1 H1N1 111.5(14) . . ?
C1 N1 H1N2 110.0(15) . . ?
H1N1 N1 H1N2 107.4(13) . . ?
C1 N1 H1N3 113.6(14) . . ?
H1N1 N1 H1N3 106.4(12) . . ?
H1N2 N1 H1N3 107.7(13) . . ?
C20 N2 H2N1 114.0(15) . . ?
C20 N2 H2N2 110.8(15) . . ?
H2N1 N2 H2N2 106.4(13) . . ?
C20 N2 H2N3 111.1(15) . . ?
H2N1 N2 H2N3 106.9(13) . . ?
H2N2 N2 H2N3 107.4(13) . . ?
N1 C1 C2 108.65(15) . . ?
N1 C1 C14 104.46(15) . . ?
C2 C1 C14 113.86(17) . . ?
N1 C1 C8 108.76(16) . . ?
C2 C1 C8 108.69(15) . . ?
C14 C1 C8 112.21(16) . . ?
C7 C2 C3 117.9(2) . . ?
C7 C2 C1 123.34(18) . . ?
C3 C2 C1 118.77(18) . . ?
C4 C3 C2 121.2(2) . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 H3A 119.4 . . ?
C5 C4 C3 120.0(2) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C6 C5 C4 119.1(2) . . ?
C6 C5 H5A 120.4 . . ?
C4 C5 H5A 120.4 . . ?
C5 C6 C7 121.3(2) . . ?
C5 C6 H6A 119.4 . . ?
C7 C6 H6A 119.4 . . ?
C2 C7 C6 120.4(2) . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C13 C8 C9 118.2(2) . . ?
C13 C8 C1 120.16(18) . . ?
C9 C8 C1 121.4(2) . . ?
C10 C9 C8 120.6(3) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C10 C11 C12 119.8(3) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 H12A 119.9 . . ?
C13 C12 H12A 119.9 . . ?
C8 C13 C12 120.9(2) . . ?
C8 C13 H13A 119.6 . . ?
C12 C13 H13A 119.6 . . ?
C15 C14 C19 118.2(2) . . ?
C15 C14 C1 123.2(2) . . ?
C19 C14 C1 118.5(2) . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C17 C16 C15 120.7(3) . . ?
C17 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C17 C18 C19 120.3(3) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C14 C19 C18 120.6(3) . . ?
C14 C19 H19A 119.7 . . ?
C18 C19 H19A 119.7 . . ?
N2 C20 C21 109.34(16) . . ?
N2 C20 C33 106.19(15) . . ?
C21 C20 C33 110.99(16) . . ?
N2 C20 C27 105.77(15) . . ?
C21 C20 C27 111.55(16) . . ?
C33 C20 C27 112.68(16) . . ?
C26 C21 C22 118.2(2) . . ?
C26 C21 C20 122.3(2) . . ?
C22 C21 C20 119.34(18) . . ?
C23 C22 C21 121.2(2) . . ?
C23 C22 H22A 119.4 . . ?
C21 C22 H22A 119.4 . . ?
C24 C23 C22 120.4(2) . . ?
C24 C23 H23A 119.8 . . ?
C22 C23 H23A 119.8 . . ?
C23 C24 C25 118.7(2) . . ?
C23 C24 H24A 120.6 . . ?
C25 C24 H24A 120.6 . . ?
C24 C25 C26 121.4(3) . . ?
C24 C25 H25A 119.3 . . ?
C26 C25 H25A 119.3 . . ?
C21 C26 C25 120.0(2) . . ?
C21 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C28 C27 C32 118.2(2) . . ?
C28 C27 C20 122.02(19) . . ?
C32 C27 C20 119.8(2) . . ?
C27 C28 C29 120.9(2) . . ?
C27 C28 H28A 119.6 . . ?
C29 C28 H28A 119.6 . . ?
C30 C29 C28 120.6(3) . . ?
C30 C29 H29A 119.7 . . ?
C28 C29 H29A 119.7 . . ?
C29 C30 C31 119.4(2) . . ?
C29 C30 H30A 120.3 . . ?
C31 C30 H30A 120.3 . . ?
C30 C31 C32 120.5(3) . . ?
C30 C31 H31A 119.8 . . ?
C32 C31 H31A 119.8 . . ?
C31 C32 C27 120.5(3) . . ?
C31 C32 H32A 119.8 . . ?
C27 C32 H32A 119.8 . . ?
C34 C33 C38 118.0(2) . . ?
C34 C33 C20 123.11(19) . . ?
C38 C33 C20 118.87(19) . . ?
C33 C34 C35 120.6(2) . . ?
C33 C34 H34A 119.7 . . ?
C35 C34 H34A 119.7 . . ?
C36 C35 C34 120.4(3) . . ?
C36 C35 H35A 119.8 . . ?
C34 C35 H35A 119.8 . . ?
C35 C36 C37 119.7(2) . . ?
C35 C36 H36A 120.2 . . ?
C37 C36 H36A 120.2 . . ?
C36 C37 C38 120.5(3) . . ?
C36 C37 H37A 119.7 . . ?
C38 C37 H37A 119.7 . . ?
C37 C38 C33 120.7(2) . . ?
C37 C38 H38A 119.6 . . ?
C33 C38 H38A 119.6 . . ?
C40 C39 C44 119.95(18) . . ?
C40 C39 S1 119.73(16) . . ?
C44 C39 S1 120.32(15) . . ?
C39 C40 C41 119.9(2) . . ?
C39 C40 H40A 120.1 . . ?
C41 C40 H40A 120.1 . . ?
C42 C41 C40 121.1(2) . . ?
C42 C41 H41A 119.4 . . ?
C40 C41 H41A 119.4 . . ?
C43 C42 C41 117.92(19) . . ?
C43 C42 C45 121.36(19) . . ?
C41 C42 C45 120.72(19) . . ?
C42 C43 C44 121.3(2) . . ?
C42 C43 H43A 119.4 . . ?
C44 C43 H43A 119.4 . . ?
C39 C44 C43 119.8(2) . . ?
C39 C44 H44A 120.1 . . ?
C43 C44 H44A 120.1 . . ?
C50 C45 C46 118.16(18) . . ?
C50 C45 C42 121.5(2) . . ?
C46 C45 C42 120.4(2) . . ?
C45 C46 C47 120.9(2) . . ?
C45 C46 H46A 119.6 . . ?
C47 C46 H46A 119.6 . . ?
C48 C47 C46 119.8(2) . . ?
C48 C47 H47A 120.1 . . ?
C46 C47 H47A 120.1 . . ?
C49 C48 C47 120.08(18) . . ?
C49 C48 S2 120.15(16) . . ?
C47 C48 S2 119.74(16) . . ?
C48 C49 C50 119.6(2) . . ?
C48 C49 H49A 120.2 . . ?
C50 C49 H49A 120.2 . . ?
C45 C50 C49 121.4(2) . . ?
C45 C50 H50A 119.3 . . ?
C49 C50 H50A 119.3 . . ?
O7 C51 H51A 109.5 . . ?
O7 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O7 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C7 10.0(3) . . . . ?
C14 C1 C2 C7 -106.0(2) . . . . ?
C8 C1 C2 C7 128.2(2) . . . . ?
N1 C1 C2 C3 -169.11(19) . . . . ?
C14 C1 C2 C3 75.0(2) . . . . ?
C8 C1 C2 C3 -50.9(2) . . . . ?
C7 C2 C3 C4 -1.2(4) . . . . ?
C1 C2 C3 C4 177.9(2) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C3 C4 C5 C6 0.9(5) . . . . ?
C4 C5 C6 C7 -0.6(5) . . . . ?
C3 C2 C7 C6 1.5(4) . . . . ?
C1 C2 C7 C6 -177.6(2) . . . . ?
C5 C6 C7 C2 -0.6(5) . . . . ?
N1 C1 C8 C13 47.1(2) . . . . ?
C2 C1 C8 C13 -71.0(2) . . . . ?
C14 C1 C8 C13 162.19(19) . . . . ?
N1 C1 C8 C9 -137.8(2) . . . . ?
C2 C1 C8 C9 104.1(2) . . . . ?
C14 C1 C8 C9 -22.7(3) . . . . ?
C13 C8 C9 C10 -0.5(4) . . . . ?
C1 C8 C9 C10 -175.7(2) . . . . ?
C8 C9 C10 C11 0.0(4) . . . . ?
C9 C10 C11 C12 -0.1(5) . . . . ?
C10 C11 C12 C13 0.7(4) . . . . ?
C9 C8 C13 C12 1.1(3) . . . . ?
C1 C8 C13 C12 176.4(2) . . . . ?
C11 C12 C13 C8 -1.2(4) . . . . ?
N1 C1 C14 C15 -118.7(2) . . . . ?
C2 C1 C14 C15 -0.3(3) . . . . ?
C8 C1 C14 C15 123.7(2) . . . . ?
N1 C1 C14 C19 57.0(2) . . . . ?
C2 C1 C14 C19 175.41(18) . . . . ?
C8 C1 C14 C19 -60.6(2) . . . . ?
C19 C14 C15 C16 0.3(3) . . . . ?
C1 C14 C15 C16 176.00(19) . . . . ?
C14 C15 C16 C17 -0.5(4) . . . . ?
C15 C16 C17 C18 0.0(4) . . . . ?
C16 C17 C18 C19 0.7(4) . . . . ?
C15 C14 C19 C18 0.4(3) . . . . ?
C1 C14 C19 C18 -175.5(2) . . . . ?
C17 C18 C19 C14 -0.9(4) . . . . ?
N2 C20 C21 C26 -24.4(3) . . . . ?
C33 C20 C21 C26 -141.2(2) . . . . ?
C27 C20 C21 C26 92.3(2) . . . . ?
N2 C20 C21 C22 160.20(17) . . . . ?
C33 C20 C21 C22 43.4(2) . . . . ?
C27 C20 C21 C22 -83.2(2) . . . . ?
C26 C21 C22 C23 -1.3(3) . . . . ?
C20 C21 C22 C23 174.35(19) . . . . ?
C21 C22 C23 C24 0.9(4) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C23 C24 C25 C26 -1.1(5) . . . . ?
C22 C21 C26 C25 0.5(3) . . . . ?
C20 C21 C26 C25 -175.0(2) . . . . ?
C24 C25 C26 C21 0.7(4) . . . . ?
N2 C20 C27 C28 129.7(2) . . . . ?
C21 C20 C27 C28 10.9(3) . . . . ?
C33 C20 C27 C28 -114.7(2) . . . . ?
N2 C20 C27 C32 -50.4(3) . . . . ?
C21 C20 C27 C32 -169.2(2) . . . . ?
C33 C20 C27 C32 65.2(3) . . . . ?
C32 C27 C28 C29 -1.2(4) . . . . ?
C20 C27 C28 C29 178.7(2) . . . . ?
C27 C28 C29 C30 1.3(4) . . . . ?
C28 C29 C30 C31 -0.4(4) . . . . ?
C29 C30 C31 C32 -0.6(5) . . . . ?
C30 C31 C32 C27 0.6(4) . . . . ?
C28 C27 C32 C31 0.3(4) . . . . ?
C20 C27 C32 C31 -179.7(2) . . . . ?
N2 C20 C33 C34 124.5(2) . . . . ?
C21 C20 C33 C34 -116.8(2) . . . . ?
C27 C20 C33 C34 9.1(3) . . . . ?
N2 C20 C33 C38 -55.9(2) . . . . ?
C21 C20 C33 C38 62.8(2) . . . . ?
C27 C20 C33 C38 -171.28(19) . . . . ?
C38 C33 C34 C35 1.4(3) . . . . ?
C20 C33 C34 C35 -179.1(2) . . . . ?
C33 C34 C35 C36 0.1(4) . . . . ?
C34 C35 C36 C37 -1.0(4) . . . . ?
C35 C36 C37 C38 0.5(4) . . . . ?
C36 C37 C38 C33 1.0(4) . . . . ?
C34 C33 C38 C37 -1.9(3) . . . . ?
C20 C33 C38 C37 178.5(2) . . . . ?
O3 S1 C39 C40 35.0(2) . . . . ?
O2 S1 C39 C40 154.4(2) . . . . ?
O1 S1 C39 C40 -85.5(2) . . . . ?
O3 S1 C39 C44 -145.60(19) . . . . ?
O2 S1 C39 C44 -26.2(2) . . . . ?
O1 S1 C39 C44 93.9(2) . . . . ?
C44 C39 C40 C41 -2.3(4) . . . . ?
S1 C39 C40 C41 177.1(2) . . . . ?
C39 C40 C41 C42 0.4(4) . . . . ?
C40 C41 C42 C43 1.3(4) . . . . ?
C40 C41 C42 C45 -178.4(2) . . . . ?
C41 C42 C43 C44 -1.0(4) . . . . ?
C45 C42 C43 C44 178.7(2) . . . . ?
C40 C39 C44 C43 2.6(4) . . . . ?
S1 C39 C44 C43 -176.77(19) . . . . ?
C42 C43 C44 C39 -1.0(4) . . . . ?
C43 C42 C45 C50 37.9(3) . . . . ?
C41 C42 C45 C50 -142.4(2) . . . . ?
C43 C42 C45 C46 -142.2(2) . . . . ?
C41 C42 C45 C46 37.5(3) . . . . ?
C50 C45 C46 C47 -0.1(3) . . . . ?
C42 C45 C46 C47 179.9(2) . . . . ?
C45 C46 C47 C48 1.2(4) . . . . ?
C46 C47 C48 C49 -0.9(3) . . . . ?
C46 C47 C48 S2 -179.16(18) . . . . ?
O5 S2 C48 C49 31.6(2) . . . . ?
O4 S2 C48 C49 -87.23(19) . . . . ?
O6 S2 C48 C49 152.71(17) . . . . ?
O5 S2 C48 C47 -150.15(18) . . . . ?
O4 S2 C48 C47 91.0(2) . . . . ?
O6 S2 C48 C47 -29.1(2) . . . . ?
C47 C48 C49 C50 -0.5(3) . . . . ?
S2 C48 C49 C50 177.77(17) . . . . ?
C46 C45 C50 C49 -1.3(3) . . . . ?
C42 C45 C50 C49 178.7(2) . . . . ?
C48 C49 C50 C45 1.6(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7O O4 0.85(3) 1.977(15) 2.806(3) 165(4) .
N1 H1N1 O2 0.86(2) 1.856(10) 2.717(2) 170(2) 3_665
N1 H1N2 O3 0.86(2) 2.024(9) 2.870(2) 167.6(19) .
N1 H1N3 O5 0.86(2) 2.111(15) 2.878(3) 147.1(18) 3_655
N2 H2N1 O6 0.86(2) 1.940(11) 2.792(2) 166(2) .
N2 H2N2 O7 0.86(2) 2.001(10) 2.850(3) 165.9(17) .
N2 H2N3 O1 0.86(2) 1.958(10) 2.817(2) 174(2) 1_545

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.043
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1044771'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), C2 H6 O'
_chemical_formula_sum            'C52 H50 N2 O7 S2'
_chemical_formula_weight         879.06

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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   15.3836(5)
_cell_length_b                   15.5242(3)
_cell_length_c                   19.5258(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.466(3)
_cell_angle_gamma                90.00
_cell_volume                     4585.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3750
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9634
_exptl_absorpt_correction_T_max  0.9748
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16228
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.56
_reflns_number_total             10476
_reflns_number_gt                7340
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0465P)²+2.1250P] where P=(Fo²+2Fc²)/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         10476
_refine_ls_number_parameters     595
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.1356
_refine_ls_wR_factor_gt          0.1194
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.48342(4) 0.38418(3) 0.12352(3) 0.03233(14) Uani 1 1 d . . .
S2 S 0.44791(4) -0.29891(3) 0.12275(3) 0.03910(15) Uani 1 1 d . . .
O1 O 0.50680(11) -0.32581(10) 0.18586(8) 0.0457(4) Uani 1 1 d . . .
O2 O 0.47369(16) -0.32938(11) 0.05997(9) 0.0710(6) Uani 1 1 d . . .
O3 O 0.35612(13) -0.31816(12) 0.12335(11) 0.0689(6) Uani 1 1 d . . .
O4 O 0.43558(12) 0.40571(10) 0.17848(8) 0.0466(4) Uani 1 1 d . . .
O5 O 0.57538(11) 0.40962(10) 0.13946(9) 0.0472(4) Uani 1 1 d . . .
O6 O 0.43992(13) 0.41395(10) 0.05584(8) 0.0548(5) Uani 1 1 d . . .
O7 O 0.27461(16) 0.63743(16) 0.23464(11) 0.0768(6) Uani 1 1 d D . .
H7O H 0.287(3) 0.656(3) 0.1965(12) 0.115 Uiso 1 1 d D . .
N1 N 0.43515(13) 0.55148(11) 0.26492(9) 0.0338(4) Uani 1 1 d D . .
H1N1 H 0.4676(11) 0.5881(10) 0.2471(11) 0.051 Uiso 1 1 d D . .
H1N2 H 0.3815(7) 0.5720(12) 0.2563(12) 0.051 Uiso 1 1 d D . .
H1N3 H 0.4348(13) 0.5044(8) 0.2411(10) 0.051 Uiso 1 1 d D . .
N2 N 0.35393(12) -0.45377(11) -0.01912(10) 0.0348(4) Uani 1 1 d D . .
H2N1 H 0.3780(14) -0.4988(9) 0.0031(9) 0.052 Uiso 1 1 d D . .
H2N2 H 0.3821(14) -0.4452(12) -0.0533(8) 0.052 Uiso 1 1 d D . .
H2N3 H 0.3658(15) -0.4105(9) 0.0091(8) 0.052 Uiso 1 1 d D . .
C1 C 0.4165(2) 0.77971(19) 0.43849(15) 0.0633(8) Uani 1 1 d . . .
H1A H 0.4051 0.8321 0.4582 0.076 Uiso 1 1 calc R . .
C2 C 0.4655(2) 0.77716(17) 0.38699(14) 0.0595(8) Uani 1 1 d . . .
H2A H 0.4880 0.8280 0.3720 0.071 Uiso 1 1 calc R . .
C3 C 0.48199(17) 0.69963(15) 0.35680(13) 0.0454(6) Uani 1 1 d . . .
H3A H 0.5160 0.6988 0.3220 0.054 Uiso 1 1 calc R . .
C4 C 0.44827(15) 0.62306(14) 0.37790(11) 0.0340(5) Uani 1 1 d . . .
C5 C 0.39993(18) 0.62671(17) 0.43105(12) 0.0477(6) Uani 1 1 d . . .
H5A H 0.3778 0.5762 0.4469 0.057 Uiso 1 1 calc R . .
C6 C 0.3841(2) 0.7049(2) 0.46107(14) 0.0610(8) Uani 1 1 d . . .
H6A H 0.3513 0.7064 0.4967 0.073 Uiso 1 1 calc R . .
C7 C 0.46663(14) 0.53806(13) 0.34204(10) 0.0308(5) Uani 1 1 d . . .
C8 C 0.41259(15) 0.46265(14) 0.36293(11) 0.0349(5) Uani 1 1 d . . .
C9 C 0.45099(18) 0.39410(15) 0.40169(13) 0.0474(6) Uani 1 1 d . . .
H9A H 0.5122 0.3912 0.4141 0.057 Uiso 1 1 calc R . .
C10 C 0.3993(2) 0.32923(18) 0.42246(15) 0.0647(8) Uani 1 1 d . . .
H10A H 0.4264 0.2837 0.4491 0.078 Uiso 1 1 calc R . .
C11 C 0.3096(2) 0.3312(2) 0.40442(15) 0.0667(9) Uani 1 1 d . . .
H11A H 0.2755 0.2875 0.4185 0.080 Uiso 1 1 calc R . .
C12 C 0.2704(2) 0.3986(2) 0.36526(16) 0.0655(8) Uani 1 1 d . . .
H12A H 0.2091 0.4002 0.3523 0.079 Uiso 1 1 calc R . .
C13 C 0.32063(18) 0.46435(18) 0.34469(14) 0.0543(7) Uani 1 1 d . . .
H13A H 0.2929 0.5100 0.3185 0.065 Uiso 1 1 calc R . .
C14 C 0.56568(15) 0.51859(13) 0.35555(11) 0.0331(5) Uani 1 1 d . . .
C15 C 0.60847(18) 0.48563(18) 0.30497(13) 0.0529(7) Uani 1 1 d . . .
H15A H 0.5774 0.4777 0.2599 0.063 Uiso 1 1 calc R . .
C16 C 0.6970(2) 0.4644(2) 0.32076(16) 0.0687(9) Uani 1 1 d . . .
H16A H 0.7248 0.4432 0.2858 0.082 Uiso 1 1 calc R . .
C17 C 0.74499(19) 0.47387(19) 0.38712(16) 0.0623(8) Uani 1 1 d . . .
H17A H 0.8043 0.4584 0.3974 0.075 Uiso 1 1 calc R . .
C18 C 0.70316(17) 0.50662(17) 0.43760(14) 0.0496(6) Uani 1 1 d . . .
H18A H 0.7344 0.5134 0.4828 0.059 Uiso 1 1 calc R . .
C19 C 0.61515(16) 0.52968(14) 0.42211(12) 0.0397(5) Uani 1 1 d . . .
H19A H 0.5883 0.5531 0.4569 0.048 Uiso 1 1 calc R . .
C20 C 0.2050(2) -0.2338(2) -0.17405(19) 0.0711(10) Uani 1 1 d . . .
H20A H 0.1955 -0.1845 -0.2015 0.085 Uiso 1 1 calc R . .
C21 C 0.1860(2) -0.3127(2) -0.20307(15) 0.0635(8) Uani 1 1 d . . .
H21A H 0.1636 -0.3170 -0.2505 0.076 Uiso 1 1 calc R . .
C22 C 0.19975(17) -0.38682(18) -0.16292(13) 0.0489(6) Uani 1 1 d . . .
H22A H 0.1865 -0.4403 -0.1836 0.059 Uiso 1 1 calc R . .
C23 C 0.23279(14) -0.38167(14) -0.09264(11) 0.0349(5) Uani 1 1 d . . .
C24 C 0.25184(18) -0.30075(16) -0.06352(14) 0.0503(6) Uani 1 1 d . . .
H24A H 0.2741 -0.2960 -0.0161 0.060 Uiso 1 1 calc R . .
C25 C 0.2383(2) -0.22709(19) -0.10389(18) 0.0684(9) Uani 1 1 d . . .
H25A H 0.2516 -0.1733 -0.0837 0.082 Uiso 1 1 calc R . .
C26 C 0.25584(14) -0.46120(13) -0.04610(10) 0.0313(5) Uani 1 1 d . . .
C27 C 0.20741(15) -0.46243(14) 0.01625(11) 0.0350(5) Uani 1 1 d . . .
C28 C 0.13031(18) -0.41665(19) 0.01494(14) 0.0541(7) Uani 1 1 d . . .
H28A H 0.1095 -0.3807 -0.0226 0.065 Uiso 1 1 calc R . .
C29 C 0.0837(2) -0.4237(2) 0.06897(17) 0.0693(9) Uani 1 1 d . . .
H29A H 0.0317 -0.3927 0.0675 0.083 Uiso 1 1 calc R . .
C30 C 0.1138(2) -0.4760(2) 0.12446(16) 0.0693(9) Uani 1 1 d . . .
H30A H 0.0822 -0.4809 0.1606 0.083 Uiso 1 1 calc R . .
C31 C 0.1907(2) -0.5212(2) 0.12664(14) 0.0640(8) Uani 1 1 d . . .
H31A H 0.2117 -0.5562 0.1647 0.077 Uiso 1 1 calc R . .
C32 C 0.23712(18) -0.51531(16) 0.07272(12) 0.0465(6) Uani 1 1 d . . .
H32A H 0.2887 -0.5470 0.0743 0.056 Uiso 1 1 calc R . .
C33 C 0.23780(15) -0.54713(14) -0.08510(11) 0.0346(5) Uani 1 1 d . . .
C34 C 0.30356(18) -0.59852(18) -0.10218(14) 0.0559(7) Uani 1 1 d . . .
H34A H 0.3622 -0.5809 -0.0911 0.067 Uiso 1 1 calc R . .
C35 C 0.2827(2) -0.6764(2) -0.13589(17) 0.0784(10) Uani 1 1 d . . .
H35A H 0.3278 -0.7109 -0.1467 0.094 Uiso 1 1 calc R . .
C36 C 0.1971(2) -0.7034(2) -0.15351(17) 0.0745(9) Uani 1 1 d . . .
H36A H 0.1837 -0.7560 -0.1757 0.089 Uiso 1 1 calc R . .
C37 C 0.1310(2) -0.6517(2) -0.13800(16) 0.0696(9) Uani 1 1 d . . .
H37A H 0.0724 -0.6689 -0.1506 0.083 Uiso 1 1 calc R . .
C38 C 0.15081(17) -0.57463(18) -0.10395(14) 0.0542(7) Uani 1 1 d . . .
H38A H 0.1053 -0.5405 -0.0934 0.065 Uiso 1 1 calc R . .
C39 C 0.48165(15) 0.27033(13) 0.11784(11) 0.0319(5) Uani 1 1 d . . .
C40 C 0.41459(17) 0.22875(14) 0.07353(13) 0.0465(6) Uani 1 1 d . . .
H40A H 0.3723 0.2605 0.0439 0.056 Uiso 1 1 calc R . .
C41 C 0.41052(18) 0.13997(15) 0.07331(13) 0.0481(6) Uani 1 1 d . . .
H41A H 0.3650 0.1126 0.0433 0.058 Uiso 1 1 calc R . .
C42 C 0.47224(15) 0.09061(13) 0.11637(11) 0.0363(5) Uani 1 1 d . . .
C43 C 0.54079(18) 0.13324(15) 0.15873(14) 0.0521(7) Uani 1 1 d . . .
H43A H 0.5845 0.1015 0.1870 0.063 Uiso 1 1 calc R . .
C44 C 0.54547(17) 0.22271(14) 0.15973(14) 0.0491(6) Uani 1 1 d . . .
H44A H 0.5918 0.2503 0.1887 0.059 Uiso 1 1 calc R . .
C45 C 0.46621(15) -0.00510(13) 0.11763(11) 0.0365(5) Uani 1 1 d . . .
C46 C 0.44022(16) -0.05227(14) 0.05700(12) 0.0399(5) Uani 1 1 d . . .
H46A H 0.4252 -0.0235 0.0147 0.048 Uiso 1 1 calc R . .
C47 C 0.43614(16) -0.14151(14) 0.05813(11) 0.0382(5) Uani 1 1 d . . .
H47A H 0.4200 -0.1721 0.0168 0.046 Uiso 1 1 calc R . .
C48 C 0.45618(15) -0.18494(13) 0.12081(11) 0.0327(5) Uani 1 1 d . . .
C49 C 0.48049(18) -0.13881(14) 0.18191(12) 0.0443(6) Uani 1 1 d . . .
H49A H 0.4929 -0.1676 0.2243 0.053 Uiso 1 1 calc R . .
C50 C 0.48633(18) -0.05008(14) 0.18014(12) 0.0476(6) Uani 1 1 d . . .
H50A H 0.5040 -0.0199 0.2215 0.057 Uiso 1 1 calc R . .
C51 C 0.2432(6) 0.7105(6) 0.2684(6) 0.104(3) Uani 0.50 1 d PD A 1
H51A H 0.2707 0.7626 0.2552 0.124 Uiso 0.50 1 calc PR A 1
H51B H 0.2593 0.7040 0.3185 0.124 Uiso 0.50 1 calc PR A 1
C51' C 0.2006(8) 0.6767(5) 0.2594(6) 0.104(3) Uani 0.50 1 d PD A 2
H51C H 0.1501 0.6817 0.2218 0.124 Uiso 0.50 1 calc PR A 2
H51D H 0.1835 0.6422 0.2962 0.124 Uiso 0.50 1 calc PR A 2
C52 C 0.1429(5) 0.7180(6) 0.2478(4) 0.100(2) Uani 0.50 1 d PD A 1
H52A H 0.1227 0.7666 0.2709 0.150 Uiso 0.50 1 calc PR A 1
H52B H 0.1157 0.6665 0.2611 0.150 Uiso 0.50 1 calc PR A 1
H52C H 0.1272 0.7257 0.1983 0.150 Uiso 0.50 1 calc PR A 1
C52' C 0.2290(5) 0.7590(5) 0.2848(4) 0.100(2) Uani 0.50 1 d PD A 2
H52D H 0.1820 0.7874 0.3022 0.150 Uiso 0.50 1 calc PR A 2
H52E H 0.2453 0.7925 0.2478 0.150 Uiso 0.50 1 calc PR A 2
H52F H 0.2792 0.7531 0.3218 0.150 Uiso 0.50 1 calc PR A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O6 1.4446(17) . ?
S1 O4 1.4464(15) . ?
S1 O5 1.4471(17) . ?
S1 C39 1.771(2) . ?
S2 O2 1.4355(18) . ?
S2 O3 1.445(2) . ?
S2 O1 1.4519(17) . ?
S2 C48 1.775(2) . ?
O7 C51 1.439(8) . ?
O7 C51' 1.451(11) . ?
O7 H7O 0.85(3) . ?
N1 C7 1.510(3) . ?
N1 H1N1 0.86(2) . ?
N1 H1N2 0.86(2) . ?
N1 H1N3 0.86(2) . ?
N2 C26 1.510(3) . ?
N2 H2N1 0.86(2) . ?
N2 H2N2 0.86(2) . ?
N2 H2N3 0.86(2) . ?
C1 C2 1.362(4) . ?
C1 C6 1.368(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.384(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.389(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.383(3) . ?
C4 C7 1.544(3) . ?
C5 C6 1.389(3) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C14 1.529(3) . ?
C7 C8 1.533(3) . ?
C8 C9 1.375(3) . ?
C8 C13 1.395(3) . ?
C9 C10 1.388(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.361(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.370(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.383(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.381(3) . ?
C14 C19 1.392(3) . ?
C15 C16 1.380(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.378(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.369(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.380(3) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.358(4) . ?
C20 C25 1.377(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.387(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.376(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.388(3) . ?
C23 C26 1.536(3) . ?
C24 C25 1.383(4) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C33 1.536(3) . ?
C26 C27 1.539(3) . ?
C27 C28 1.379(3) . ?
C27 C32 1.384(3) . ?
C28 C29 1.383(4) . ?
C28 H28A 0.9300 . ?
C29 C30 1.366(4) . ?
C29 H29A 0.9300 . ?
C30 C31 1.370(4) . ?
C30 H30A 0.9300 . ?
C31 C32 1.379(3) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
C33 C34 1.376(3) . ?
C33 C38 1.389(3) . ?
C34 C35 1.386(4) . ?
C34 H34A 0.9300 . ?
C35 C36 1.365(4) . ?
C35 H35A 0.9300 . ?
C36 C37 1.371(4) . ?
C36 H36A 0.9300 . ?
C37 C38 1.376(4) . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9300 . ?
C39 C44 1.374(3) . ?
C39 C40 1.380(3) . ?
C40 C41 1.380(3) . ?
C40 H40A 0.9300 . ?
C41 C42 1.380(3) . ?
C41 H41A 0.9300 . ?
C42 C43 1.385(3) . ?
C42 C45 1.489(3) . ?
C43 C44 1.391(3) . ?
C43 H43A 0.9300 . ?
C44 H44A 0.9300 . ?
C45 C46 1.388(3) . ?
C45 C50 1.391(3) . ?
C46 C47 1.387(3) . ?
C46 H46A 0.9300 . ?
C47 C48 1.382(3) . ?
C47 H47A 0.9300 . ?
C48 C49 1.383(3) . ?
C49 C50 1.381(3) . ?
C49 H49A 0.9300 . ?
C50 H50A 0.9300 . ?
C51 C52 1.526(8) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C51' C52' 1.411(8) . ?
C51' H51C 0.9700 . ?
C51' H51D 0.9700 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C52' H52D 0.9600 . ?
C52' H52E 0.9600 . ?
C52' H52F 0.9600 . ?

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
O6 S1 O4 113.03(11) . . ?
O6 S1 O5 112.45(11) . . ?
O4 S1 O5 112.75(10) . . ?
O6 S1 C39 105.22(10) . . ?
O4 S1 C39 105.84(9) . . ?
O5 S1 C39 106.81(10) . . ?
O2 S2 O3 111.14(14) . . ?
O2 S2 O1 113.79(12) . . ?
O3 S2 O1 113.18(11) . . ?
O2 S2 C48 106.16(10) . . ?
O3 S2 C48 106.27(11) . . ?
O1 S2 C48 105.59(10) . . ?
C51 O7 H7O 106(3) . . ?
C51' O7 H7O 118(3) . . ?
C7 N1 H1N1 112.6(15) . . ?
C7 N1 H1N2 111.4(15) . . ?
H1N1 N1 H1N2 106.0(13) . . ?
C7 N1 H1N3 112.8(15) . . ?
H1N1 N1 H1N3 106.6(13) . . ?
H1N2 N1 H1N3 107.0(13) . . ?
C26 N2 H2N1 114.9(15) . . ?
C26 N2 H2N2 110.4(15) . . ?
H2N1 N2 H2N2 106.2(13) . . ?
C26 N2 H2N3 111.3(16) . . ?
H2N1 N2 H2N3 106.5(13) . . ?
H2N2 N2 H2N3 107.0(13) . . ?
C2 C1 C6 119.7(2) . . ?
C2 C1 H1A 120.1 . . ?
C6 C1 H1A 120.1 . . ?
C1 C2 C3 120.6(3) . . ?
C1 C2 H2A 119.7 . . ?
C3 C2 H2A 119.7 . . ?
C2 C3 C4 120.7(2) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C5 C4 C3 117.9(2) . . ?
C5 C4 C7 122.9(2) . . ?
C3 C4 C7 119.21(19) . . ?
C4 C5 C6 120.8(2) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
C1 C6 C5 120.2(3) . . ?
C1 C6 H6A 119.9 . . ?
C5 C6 H6A 119.9 . . ?
N1 C7 C14 109.17(16) . . ?
N1 C7 C8 106.23(16) . . ?
C14 C7 C8 112.01(17) . . ?
N1 C7 C4 106.41(16) . . ?
C14 C7 C4 110.46(17) . . ?
C8 C7 C4 112.29(17) . . ?
C9 C8 C13 118.0(2) . . ?
C9 C8 C7 122.5(2) . . ?
C13 C8 C7 119.4(2) . . ?
C8 C9 C10 120.7(3) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C11 C10 C9 121.0(3) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C10 C11 C12 119.1(3) . . ?
C10 C11 H11A 120.5 . . ?
C12 C11 H11A 120.5 . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C12 C13 C8 120.4(3) . . ?
C12 C13 H13A 119.8 . . ?
C8 C13 H13A 119.8 . . ?
C15 C14 C19 117.6(2) . . ?
C15 C14 C7 122.7(2) . . ?
C19 C14 C7 119.69(19) . . ?
C16 C15 C14 120.5(2) . . ?
C16 C15 H15A 119.7 . . ?
C14 C15 H15A 119.7 . . ?
C17 C16 C15 121.5(3) . . ?
C17 C16 H16A 119.2 . . ?
C15 C16 H16A 119.2 . . ?
C18 C17 C16 118.3(3) . . ?
C18 C17 H17A 120.8 . . ?
C16 C17 H17A 120.8 . . ?
C17 C18 C19 120.6(3) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
C18 C19 C14 121.4(2) . . ?
C18 C19 H19A 119.3 . . ?
C14 C19 H19A 119.3 . . ?
C21 C20 C25 119.8(3) . . ?
C21 C20 H20A 120.1 . . ?
C25 C20 H20A 120.1 . . ?
C20 C21 C22 120.9(3) . . ?
C20 C21 H21A 119.6 . . ?
C22 C21 H21A 119.6 . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H22A 119.8 . . ?
C21 C22 H22A 119.8 . . ?
C22 C23 C24 118.2(2) . . ?
C22 C23 C26 123.2(2) . . ?
C24 C23 C26 118.4(2) . . ?
C25 C24 C23 121.1(3) . . ?
C25 C24 H24A 119.5 . . ?
C23 C24 H24A 119.5 . . ?
C20 C25 C24 119.7(3) . . ?
C20 C25 H25A 120.2 . . ?
C24 C25 H25A 120.2 . . ?
N2 C26 C23 104.70(16) . . ?
N2 C26 C33 108.56(17) . . ?
C23 C26 C33 113.78(17) . . ?
N2 C26 C27 108.77(17) . . ?
C23 C26 C27 112.67(17) . . ?
C33 C26 C27 108.16(17) . . ?
C28 C27 C32 118.6(2) . . ?
C28 C27 C26 121.2(2) . . ?
C32 C27 C26 120.0(2) . . ?
C27 C28 C29 120.5(3) . . ?
C27 C28 H28A 119.7 . . ?
C29 C28 H28A 119.7 . . ?
C30 C29 C28 120.3(3) . . ?
C30 C29 H29A 119.8 . . ?
C28 C29 H29A 119.8 . . ?
C29 C30 C31 119.7(3) . . ?
C29 C30 H30A 120.2 . . ?
C31 C30 H30A 120.2 . . ?
C30 C31 C32 120.4(3) . . ?
C30 C31 H31A 119.8 . . ?
C32 C31 H31A 119.8 . . ?
C31 C32 C27 120.4(3) . . ?
C31 C32 H32A 119.8 . . ?
C27 C32 H32A 119.8 . . ?
C34 C33 C38 118.2(2) . . ?
C34 C33 C26 123.3(2) . . ?
C38 C33 C26 118.5(2) . . ?
C33 C34 C35 120.2(3) . . ?
C33 C34 H34A 119.9 . . ?
C35 C34 H34A 119.9 . . ?
C36 C35 C34 121.1(3) . . ?
C36 C35 H35A 119.4 . . ?
C34 C35 H35A 119.4 . . ?
C35 C36 C37 119.0(3) . . ?
C35 C36 H36A 120.5 . . ?
C37 C36 H36A 120.5 . . ?
C36 C37 C38 120.5(3) . . ?
C36 C37 H37A 119.7 . . ?
C38 C37 H37A 119.8 . . ?
C37 C38 C33 120.9(3) . . ?
C37 C38 H38A 119.6 . . ?
C33 C38 H38A 119.6 . . ?
C44 C39 C40 119.6(2) . . ?
C44 C39 S1 119.90(17) . . ?
C40 C39 S1 120.48(17) . . ?
C41 C40 C39 119.8(2) . . ?
C41 C40 H40A 120.1 . . ?
C39 C40 H40A 120.1 . . ?
C40 C41 C42 121.8(2) . . ?
C40 C41 H41A 119.1 . . ?
C42 C41 H41A 119.1 . . ?
C41 C42 C43 117.6(2) . . ?
C41 C42 C45 121.7(2) . . ?
C43 C42 C45 120.7(2) . . ?
C42 C43 C44 121.2(2) . . ?
C42 C43 H43A 119.4 . . ?
C44 C43 H43A 119.4 . . ?
C39 C44 C43 120.0(2) . . ?
C39 C44 H44A 120.0 . . ?
C43 C44 H44A 120.0 . . ?
C46 C45 C50 117.9(2) . . ?
C46 C45 C42 121.4(2) . . ?
C50 C45 C42 120.7(2) . . ?
C47 C46 C45 121.4(2) . . ?
C47 C46 H46A 119.3 . . ?
C45 C46 H46A 119.3 . . ?
C48 C47 C46 119.8(2) . . ?
C48 C47 H47A 120.1 . . ?
C46 C47 H47A 120.1 . . ?
C47 C48 C49 119.54(19) . . ?
C47 C48 S2 119.99(16) . . ?
C49 C48 S2 120.45(16) . . ?
C50 C49 C48 120.2(2) . . ?
C50 C49 H49A 119.9 . . ?
C48 C49 H49A 119.9 . . ?
C49 C50 C45 121.2(2) . . ?
C49 C50 H50A 119.4 . . ?
C45 C50 H50A 119.4 . . ?
O7 C51 C52 110.3(7) . . ?
O7 C51 H51A 109.6 . . ?
C52 C51 H51A 109.6 . . ?
O7 C51 H51B 109.6 . . ?
C52 C51 H51B 109.6 . . ?
H51A C51 H51B 108.1 . . ?
C52' C51' O7 106.6(8) . . ?
C52' C51' H51C 110.4 . . ?
O7 C51' H51C 110.4 . . ?
C52' C51' H51D 110.4 . . ?
O7 C51' H51D 110.4 . . ?
H51C C51' H51D 108.6 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51' C52' H52D 109.5 . . ?
C51' C52' H52E 109.5 . . ?
H52D C52' H52E 109.5 . . ?
C51' C52' H52F 109.5 . . ?
H52D C52' H52F 109.5 . . ?
H52E C52' H52F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.7(5) . . . . ?
C1 C2 C3 C4 0.6(4) . . . . ?
C2 C3 C4 C5 -1.7(4) . . . . ?
C2 C3 C4 C7 178.9(2) . . . . ?
C3 C4 C5 C6 1.5(4) . . . . ?
C7 C4 C5 C6 -179.1(2) . . . . ?
C2 C1 C6 C5 -0.9(5) . . . . ?
C4 C5 C6 C1 -0.2(4) . . . . ?
C5 C4 C7 N1 125.7(2) . . . . ?
C3 C4 C7 N1 -54.8(3) . . . . ?
C5 C4 C7 C14 -115.9(2) . . . . ?
C3 C4 C7 C14 63.5(3) . . . . ?
C5 C4 C7 C8 9.9(3) . . . . ?
C3 C4 C7 C8 -170.6(2) . . . . ?
N1 C7 C8 C9 131.2(2) . . . . ?
C14 C7 C8 C9 12.1(3) . . . . ?
C4 C7 C8 C9 -112.9(2) . . . . ?
N1 C7 C8 C13 -51.5(3) . . . . ?
C14 C7 C8 C13 -170.6(2) . . . . ?
C4 C7 C8 C13 64.5(3) . . . . ?
C13 C8 C9 C10 -0.6(4) . . . . ?
C7 C8 C9 C10 176.8(2) . . . . ?
C8 C9 C10 C11 0.7(4) . . . . ?
C9 C10 C11 C12 -0.1(4) . . . . ?
C10 C11 C12 C13 -0.6(5) . . . . ?
C11 C12 C13 C8 0.7(4) . . . . ?
C9 C8 C13 C12 -0.1(4) . . . . ?
C7 C8 C13 C12 -177.5(2) . . . . ?
N1 C7 C14 C15 -23.2(3) . . . . ?
C8 C7 C14 C15 94.2(2) . . . . ?
C4 C7 C14 C15 -139.8(2) . . . . ?
N1 C7 C14 C19 160.40(18) . . . . ?
C8 C7 C14 C19 -82.2(2) . . . . ?
C4 C7 C14 C19 43.7(3) . . . . ?
C19 C14 C15 C16 0.3(4) . . . . ?
C7 C14 C15 C16 -176.2(2) . . . . ?
C14 C15 C16 C17 1.1(5) . . . . ?
C15 C16 C17 C18 -1.1(5) . . . . ?
C16 C17 C18 C19 -0.2(4) . . . . ?
C17 C18 C19 C14 1.6(4) . . . . ?
C15 C14 C19 C18 -1.6(3) . . . . ?
C7 C14 C19 C18 175.0(2) . . . . ?
C25 C20 C21 C22 0.1(5) . . . . ?
C20 C21 C22 C23 0.1(4) . . . . ?
C21 C22 C23 C24 0.0(4) . . . . ?
C21 C22 C23 C26 -175.5(2) . . . . ?
C22 C23 C24 C25 -0.1(4) . . . . ?
C26 C23 C24 C25 175.5(2) . . . . ?
C21 C20 C25 C24 -0.2(5) . . . . ?
C23 C24 C25 C20 0.3(4) . . . . ?
C22 C23 C26 N2 117.9(2) . . . . ?
C24 C23 C26 N2 -57.6(2) . . . . ?
C22 C23 C26 C33 -0.5(3) . . . . ?
C24 C23 C26 C33 -175.9(2) . . . . ?
C22 C23 C26 C27 -124.1(2) . . . . ?
C24 C23 C26 C27 60.5(3) . . . . ?
N2 C26 C27 C28 138.0(2) . . . . ?
C23 C26 C27 C28 22.4(3) . . . . ?
C33 C26 C27 C28 -104.2(2) . . . . ?
N2 C26 C27 C32 -47.1(3) . . . . ?
C23 C26 C27 C32 -162.7(2) . . . . ?
C33 C26 C27 C32 70.7(3) . . . . ?
C32 C27 C28 C29 -0.1(4) . . . . ?
C26 C27 C28 C29 174.8(2) . . . . ?
C27 C28 C29 C30 0.2(5) . . . . ?
C28 C29 C30 C31 0.4(5) . . . . ?
C29 C30 C31 C32 -1.0(5) . . . . ?
C30 C31 C32 C27 1.1(4) . . . . ?
C28 C27 C32 C31 -0.5(4) . . . . ?
C26 C27 C32 C31 -175.6(2) . . . . ?
N2 C26 C33 C34 -10.8(3) . . . . ?
C23 C26 C33 C34 105.3(3) . . . . ?
C27 C26 C33 C34 -128.7(2) . . . . ?
N2 C26 C33 C38 169.0(2) . . . . ?
C23 C26 C33 C38 -74.9(3) . . . . ?
C27 C26 C33 C38 51.1(3) . . . . ?
C38 C33 C34 C35 -1.4(4) . . . . ?
C26 C33 C34 C35 178.4(3) . . . . ?
C33 C34 C35 C36 0.7(5) . . . . ?
C34 C35 C36 C37 0.7(6) . . . . ?
C35 C36 C37 C38 -1.3(5) . . . . ?
C36 C37 C38 C33 0.6(5) . . . . ?
C34 C33 C38 C37 0.8(4) . . . . ?
C26 C33 C38 C37 -179.0(2) . . . . ?
O6 S1 C39 C44 153.4(2) . . . . ?
O4 S1 C39 C44 -86.7(2) . . . . ?
O5 S1 C39 C44 33.7(2) . . . . ?
O6 S1 C39 C40 -29.1(2) . . . . ?
O4 S1 C39 C40 90.8(2) . . . . ?
O5 S1 C39 C40 -148.83(19) . . . . ?
C44 C39 C40 C41 2.1(4) . . . . ?
S1 C39 C40 C41 -175.3(2) . . . . ?
C39 C40 C41 C42 -0.2(4) . . . . ?
C40 C41 C42 C43 -2.0(4) . . . . ?
C40 C41 C42 C45 178.1(2) . . . . ?
C41 C42 C43 C44 2.3(4) . . . . ?
C45 C42 C43 C44 -177.8(2) . . . . ?
C40 C39 C44 C43 -1.8(4) . . . . ?
S1 C39 C44 C43 175.6(2) . . . . ?
C42 C43 C44 C39 -0.4(4) . . . . ?
C41 C42 C45 C46 39.4(3) . . . . ?
C43 C42 C45 C46 -140.5(3) . . . . ?
C41 C42 C45 C50 -140.4(3) . . . . ?
C43 C42 C45 C50 39.8(4) . . . . ?
C50 C45 C46 C47 -1.4(4) . . . . ?
C42 C45 C46 C47 178.8(2) . . . . ?
C45 C46 C47 C48 1.6(4) . . . . ?
C46 C47 C48 C49 -0.2(4) . . . . ?
C46 C47 C48 S2 178.15(19) . . . . ?
O2 S2 C48 C47 34.8(2) . . . . ?
O3 S2 C48 C47 -83.6(2) . . . . ?
O1 S2 C48 C47 155.96(19) . . . . ?
O2 S2 C48 C49 -146.8(2) . . . . ?
O3 S2 C48 C49 94.8(2) . . . . ?
O1 S2 C48 C49 -25.7(2) . . . . ?
C47 C48 C49 C50 -1.2(4) . . . . ?
S2 C48 C49 C50 -179.6(2) . . . . ?
C48 C49 C50 C45 1.4(4) . . . . ?
C46 C45 C50 C49 -0.1(4) . . . . ?
C42 C45 C50 C49 179.7(2) . . . . ?
C51' O7 C51 C52 -24.3(10) . . . . ?
C51 O7 C51' C52' 3.7(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7O O3 0.85(3) 1.967(17) 2.786(3) 160(4) 1_565
N1 H1N1 O1 0.86(2) 1.961(12) 2.801(2) 162(2) 1_565
N1 H1N2 O7 0.86(2) 1.913(10) 2.775(3) 169.1(19) .
N1 H1N3 O4 0.86(2) 1.962(10) 2.824(2) 174(2) .
N2 H2N1 O6 0.86(2) 1.856(10) 2.721(2) 173(2) 1_545
N2 H2N2 O5 0.86(2) 1.990(9) 2.846(2) 168(2) 3_655
N2 H2N3 O2 0.86(2) 2.174(17) 2.911(3) 143(2) .

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.046
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1044772'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), 3(C3 H8 O)'
_chemical_formula_sum            'C59 H68 N2 O9 S2'
_chemical_formula_weight         1013.27

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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   15.4604(5)
_cell_length_b                   19.5093(7)
_cell_length_c                   18.6701(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.156(3)
_cell_angle_gamma                90.00
_cell_volume                     5598.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3488
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2160
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9675
_exptl_absorpt_correction_T_max  0.9747
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17165
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         25.01
_reflns_number_total             9838
_reflns_number_gt                6409
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0909P)²+2.3540P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9838
_refine_ls_number_parameters     704
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_ref         0.2033
_refine_ls_wR_factor_gt          0.1816
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.38680(5) 0.23892(5) 0.75599(4) 0.0526(3) Uani 1 1 d . . .
S2 S 0.29609(5) 0.25681(6) 0.73800(5) 0.0627(3) Uani 1 1 d . . .
O1 O -0.40145(14) 0.20891(14) 0.82486(12) 0.0698(7) Uani 1 1 d . . .
O2 O -0.41910(14) 0.19702(13) 0.69477(12) 0.0649(7) Uani 1 1 d . . .
O3 O -0.41855(15) 0.30876(13) 0.74747(13) 0.0702(7) Uani 1 1 d . . .
O4 O 0.31337(15) 0.22237(15) 0.67217(13) 0.0762(8) Uani 1 1 d . . .
O5 O 0.32004(18) 0.32975(16) 0.73976(18) 0.0966(10) Uani 1 1 d . . .
O6 O 0.33260(16) 0.22290(17) 0.80216(14) 0.0875(9) Uani 1 1 d . . .
O7 O 0.43160(19) 0.41259(14) 0.67568(16) 0.0817(8) Uani 1 1 d D . .
H7O H 0.391(2) 0.393(2) 0.696(3) 0.123 Uiso 1 1 d D . .
O8 O -0.4920(2) 0.42340(15) 0.82968(14) 0.0805(8) Uani 1 1 d D . .
H8O H -0.498(3) 0.415(3) 0.7848(8) 0.121 Uiso 1 1 d D . .
O9 O -0.4143(19) 0.0382(13) 0.8238(12) 0.354(9) Uani 0.50 1 d PD A 1
H9O H -0.3613 0.0336 0.8262 0.530 Uiso 0.50 1 calc PR A 1
O9' O -0.435(2) 0.0406(12) 0.7845(9) 0.354(9) Uani 0.50 1 d PD B 2
H9'O H -0.4281 0.0815 0.7936 0.530 Uiso 0.50 1 calc PR B 2
N1 N -0.52798(16) 0.29196(14) 0.88511(13) 0.0457(6) Uani 1 1 d D . .
H1N1 H -0.4844(11) 0.2677(11) 0.8745(16) 0.069 Uiso 1 1 d D . .
H1N2 H -0.5740(10) 0.2759(12) 0.8612(15) 0.069 Uiso 1 1 d D . .
H1N3 H -0.5200(16) 0.3333(6) 0.8703(16) 0.069 Uiso 1 1 d D . .
N2 N 0.45265(16) 0.28024(14) 0.61066(13) 0.0446(6) Uani 1 1 d D . .
H2N2 H 0.4955(11) 0.2583(11) 0.6326(15) 0.067 Uiso 1 1 d D . .
H2N3 H 0.4529(16) 0.3215(6) 0.6274(16) 0.067 Uiso 1 1 d D . .
H2N1 H 0.4050(10) 0.2612(12) 0.6213(16) 0.067 Uiso 1 1 d D . .
C1 C -0.53523(19) 0.29160(15) 0.96583(15) 0.0437(7) Uani 1 1 d . . .
C2 C -0.62556(19) 0.31966(15) 0.97855(17) 0.0445(7) Uani 1 1 d . . .
C3 C -0.6609(2) 0.30273(19) 1.0413(2) 0.0668(10) Uani 1 1 d . . .
H3A H -0.6311 0.2727 1.0739 0.080 Uiso 1 1 calc R . .
C4 C -0.7396(3) 0.3296(2) 1.0564(3) 0.0868(14) Uani 1 1 d . . .
H4A H -0.7621 0.3182 1.0991 0.104 Uiso 1 1 calc R . .
C5 C -0.7843(3) 0.3730(2) 1.0086(3) 0.0828(13) Uani 1 1 d . . .
H5A H -0.8376 0.3908 1.0185 0.099 Uiso 1 1 calc R . .
C6 C -0.7511(3) 0.3904(2) 0.9460(3) 0.0773(12) Uani 1 1 d . . .
H6A H -0.7816 0.4201 0.9135 0.093 Uiso 1 1 calc R . .
C7 C -0.6712(2) 0.36346(18) 0.9310(2) 0.0595(9) Uani 1 1 d . . .
H7A H -0.6489 0.3753 0.8884 0.071 Uiso 1 1 calc R . .
C8 C -0.52531(19) 0.21652(15) 0.99172(16) 0.0454(7) Uani 1 1 d . . .
C9 C -0.4832(3) 0.20075(19) 1.05895(18) 0.0696(11) Uani 1 1 d . . .
H9A H -0.4560 0.2352 1.0875 0.084 Uiso 1 1 calc R . .
C10 C -0.4816(3) 0.1338(2) 1.0836(2) 0.0847(13) Uani 1 1 d . . .
H10A H -0.4541 0.1239 1.1292 0.102 Uiso 1 1 calc R . .
C11 C -0.5193(3) 0.0826(2) 1.0430(2) 0.0774(12) Uani 1 1 d . . .
H11A H -0.5179 0.0379 1.0604 0.093 Uiso 1 1 calc R . .
C12 C -0.5599(3) 0.09704(18) 0.9753(2) 0.0726(11) Uani 1 1 d . . .
H12A H -0.5853 0.0620 0.9466 0.087 Uiso 1 1 calc R . .
C13 C -0.5627(2) 0.16371(17) 0.95014(19) 0.0568(9) Uani 1 1 d . . .
H13A H -0.5902 0.1731 0.9044 0.068 Uiso 1 1 calc R . .
C14 C -0.4614(2) 0.33751(16) 0.99981(16) 0.0465(7) Uani 1 1 d . . .
C15 C -0.4774(2) 0.39730(17) 1.03637(18) 0.0574(9) Uani 1 1 d . . .
H15A H -0.5344 0.4102 1.0411 0.069 Uiso 1 1 calc R . .
C16 C -0.4090(3) 0.43820(19) 1.0660(2) 0.0741(11) Uani 1 1 d . . .
H16A H -0.4205 0.4783 1.0901 0.089 Uiso 1 1 calc R . .
C17 C -0.3243(3) 0.4196(2) 1.0597(2) 0.0810(12) Uani 1 1 d . . .
H17A H -0.2785 0.4466 1.0798 0.097 Uiso 1 1 calc R . .
C18 C -0.3081(2) 0.3607(2) 1.0233(2) 0.0765(11) Uani 1 1 d . . .
H18A H -0.2510 0.3481 1.0187 0.092 Uiso 1 1 calc R . .
C19 C -0.3752(2) 0.32010(19) 0.9937(2) 0.0627(9) Uani 1 1 d . . .
H19A H -0.3628 0.2804 0.9691 0.075 Uiso 1 1 calc R . .
C20 C 0.45494(19) 0.28174(15) 0.52994(15) 0.0438(7) Uani 1 1 d . . .
C21 C 0.4336(2) 0.20900(16) 0.50167(16) 0.0468(8) Uani 1 1 d . . .
C22 C 0.4627(2) 0.15190(18) 0.53997(19) 0.0636(9) Uani 1 1 d . . .
H22A H 0.4943 0.1571 0.5849 0.076 Uiso 1 1 calc R . .
C23 C 0.4457(3) 0.08656(19) 0.5128(2) 0.0796(12) Uani 1 1 d . . .
H23A H 0.4649 0.0485 0.5400 0.095 Uiso 1 1 calc R . .
C24 C 0.4010(3) 0.0776(2) 0.4466(2) 0.0790(12) Uani 1 1 d . . .
H24A H 0.3905 0.0338 0.4280 0.095 Uiso 1 1 calc R . .
C25 C 0.3718(3) 0.1335(2) 0.4079(2) 0.0796(12) Uani 1 1 d . . .
H25A H 0.3412 0.1276 0.3626 0.096 Uiso 1 1 calc R . .
C26 C 0.3867(3) 0.19908(18) 0.43460(18) 0.0664(10) Uani 1 1 d . . .
H26A H 0.3654 0.2367 0.4076 0.080 Uiso 1 1 calc R . .
C27 C 0.3863(2) 0.33421(16) 0.50011(17) 0.0512(8) Uani 1 1 d . . .
C28 C 0.3009(2) 0.3269(2) 0.5135(2) 0.0711(11) Uani 1 1 d . . .
H28A H 0.2857 0.2903 0.5416 0.085 Uiso 1 1 calc R . .
C29 C 0.2371(3) 0.3726(2) 0.4862(3) 0.0895(13) Uani 1 1 d . . .
H29A H 0.1797 0.3663 0.4953 0.107 Uiso 1 1 calc R . .
C30 C 0.2594(3) 0.4275(2) 0.4457(3) 0.0919(14) Uani 1 1 d . . .
H30A H 0.2172 0.4587 0.4274 0.110 Uiso 1 1 calc R . .
C31 C 0.3438(3) 0.4357(2) 0.4326(2) 0.0872(13) Uani 1 1 d . . .
H31A H 0.3590 0.4731 0.4056 0.105 Uiso 1 1 calc R . .
C32 C 0.4073(3) 0.38940(19) 0.4588(2) 0.0677(10) Uani 1 1 d . . .
H32A H 0.4644 0.3954 0.4486 0.081 Uiso 1 1 calc R . .
C33 C 0.5468(2) 0.30283(16) 0.51539(17) 0.0504(8) Uani 1 1 d . . .
C34 C 0.5818(3) 0.2811(2) 0.4542(2) 0.0702(11) Uani 1 1 d . . .
H34A H 0.5504 0.2509 0.4228 0.084 Uiso 1 1 calc R . .
C35 C 0.6618(3) 0.3034(2) 0.4390(3) 0.0941(15) Uani 1 1 d . . .
H35A H 0.6839 0.2882 0.3973 0.113 Uiso 1 1 calc R . .
C36 C 0.7095(3) 0.3473(2) 0.4838(3) 0.0880(14) Uani 1 1 d . . .
H36A H 0.7635 0.3624 0.4727 0.106 Uiso 1 1 calc R . .
C37 C 0.6771(3) 0.3693(2) 0.5458(3) 0.0824(12) Uani 1 1 d . . .
H37A H 0.7096 0.3989 0.5772 0.099 Uiso 1 1 calc R . .
C38 C 0.5956(2) 0.34724(19) 0.5614(2) 0.0652(10) Uani 1 1 d . . .
H38A H 0.5737 0.3624 0.6031 0.078 Uiso 1 1 calc R . .
C39 C 0.18195(19) 0.25340(18) 0.73963(16) 0.0506(8) Uani 1 1 d . . .
C40 C 0.1365(2) 0.19444(18) 0.71775(18) 0.0548(8) Uani 1 1 d . . .
H40A H 0.1656 0.1572 0.7005 0.066 Uiso 1 1 calc R . .
C41 C 0.04768(19) 0.19103(17) 0.72159(17) 0.0512(8) Uani 1 1 d . . .
H41A H 0.0176 0.1512 0.7073 0.061 Uiso 1 1 calc R . .
C42 C 0.00308(19) 0.24619(16) 0.74645(15) 0.0443(7) Uani 1 1 d . . .
C43 C 0.0495(2) 0.30433(18) 0.76891(18) 0.0563(9) Uani 1 1 d . . .
H43A H 0.0205 0.3415 0.7863 0.068 Uiso 1 1 calc R . .
C44 C 0.1389(2) 0.3081(2) 0.76592(18) 0.0614(9) Uani 1 1 d . . .
H44A H 0.1694 0.3474 0.7816 0.074 Uiso 1 1 calc R . .
C45 C -0.09311(19) 0.24372(16) 0.74790(15) 0.0444(7) Uani 1 1 d . . .
C46 C -0.13324(19) 0.18661(17) 0.77465(17) 0.0491(8) Uani 1 1 d . . .
H46A H -0.1000 0.1487 0.7902 0.059 Uiso 1 1 calc R . .
C47 C -0.22241(19) 0.18585(17) 0.77829(17) 0.0494(8) Uani 1 1 d . . .
H47A H -0.2486 0.1479 0.7969 0.059 Uiso 1 1 calc R . .
C48 C -0.27205(19) 0.24166(16) 0.75416(15) 0.0440(7) Uani 1 1 d . . .
C49 C -0.2335(2) 0.29799(18) 0.72689(18) 0.0556(9) Uani 1 1 d . . .
H49A H -0.2673 0.3355 0.7107 0.067 Uiso 1 1 calc R . .
C50 C -0.1445(2) 0.29893(18) 0.72354(18) 0.0564(9) Uani 1 1 d . . .
H50A H -0.1188 0.3371 0.7047 0.068 Uiso 1 1 calc R . .
C51 C 0.423(2) 0.4770(11) 0.6396(18) 0.120(6) Uani 0.50 1 d PD C 1
H51A H 0.3986 0.4718 0.5898 0.144 Uiso 0.50 1 calc PR C 1
H51B H 0.4781 0.5009 0.6414 0.144 Uiso 0.50 1 calc PR C 1
C51' C 0.397(2) 0.4745(11) 0.6446(17) 0.120(6) Uani 0.50 1 d PD C 2
H51C H 0.3502 0.4601 0.6087 0.144 Uiso 0.50 1 calc PR C 2
H51D H 0.4420 0.4927 0.6179 0.144 Uiso 0.50 1 calc PR C 2
C52 C 0.3619(16) 0.5124(11) 0.6828(16) 0.203(6) Uani 0.50 1 d PD C 1
H52A H 0.3759 0.5609 0.6850 0.244 Uiso 0.50 1 calc PR C 1
H52B H 0.3695 0.4947 0.7316 0.244 Uiso 0.50 1 calc PR C 1
C52' C 0.3617(18) 0.5344(10) 0.6801(17) 0.203(6) Uani 0.50 1 d PD C 2
H52C H 0.3383 0.5680 0.6448 0.244 Uiso 0.50 1 calc PR C 2
H52D H 0.4064 0.5561 0.7129 0.244 Uiso 0.50 1 calc PR C 2
C53 C 0.2691(15) 0.5040(15) 0.6532(13) 0.224(9) Uani 0.50 1 d PD C 1
H53A H 0.2327 0.5295 0.6822 0.335 Uiso 0.50 1 calc PR C 1
H53B H 0.2537 0.4564 0.6538 0.335 Uiso 0.50 1 calc PR C 1
H53C H 0.2612 0.5208 0.6046 0.335 Uiso 0.50 1 calc PR C 1
C53' C 0.2912(16) 0.5052(14) 0.7202(13) 0.224(9) Uani 0.50 1 d PD C 2
H53D H 0.2619 0.5417 0.7422 0.335 Uiso 0.50 1 calc PR C 2
H53E H 0.3162 0.4743 0.7567 0.335 Uiso 0.50 1 calc PR C 2
H53F H 0.2502 0.4809 0.6872 0.335 Uiso 0.50 1 calc PR C 2
C54 C -0.4043(7) 0.4412(10) 0.8473(14) 0.098(4) Uani 0.50 1 d PD D 1
H54A H -0.3695 0.4052 0.8288 0.118 Uiso 0.50 1 calc PR D 1
H54D H -0.3928 0.4399 0.8994 0.118 Uiso 0.50 1 calc PR D 1
C54' C -0.4193(8) 0.4619(10) 0.8579(13) 0.098(4) Uani 0.50 1 d PD D 2
H54B H -0.3822 0.4348 0.8923 0.118 Uiso 0.50 1 calc PR D 2
H54C H -0.4376 0.5026 0.8821 0.118 Uiso 0.50 1 calc PR D 2
C55 C -0.3705(15) 0.5077(10) 0.8229(12) 0.160(5) Uani 0.50 1 d PD D 1
H55A H -0.3262 0.5266 0.8581 0.191 Uiso 0.50 1 calc PR D 1
H55B H -0.4167 0.5409 0.8123 0.191 Uiso 0.50 1 calc PR D 1
C55' C -0.3720(12) 0.4812(11) 0.7958(14) 0.160(5) Uani 0.50 1 d PD D 2
H55C H -0.4064 0.5147 0.7668 0.191 Uiso 0.50 1 calc PR D 2
H55D H -0.3668 0.4409 0.7661 0.191 Uiso 0.50 1 calc PR D 2
C56 C -0.3329(10) 0.4844(6) 0.7555(7) 0.135(4) Uani 0.50 1 d PD D 1
H56A H -0.3047 0.5224 0.7349 0.202 Uiso 0.50 1 calc PR D 1
H56B H -0.3789 0.4676 0.7213 0.202 Uiso 0.50 1 calc PR D 1
H56C H -0.2914 0.4485 0.7674 0.202 Uiso 0.50 1 calc PR D 1
C56' C -0.2828(8) 0.5103(6) 0.8158(8) 0.135(4) Uani 0.50 1 d PD D 2
H56D H -0.2619 0.5306 0.7741 0.202 Uiso 0.50 1 calc PR D 2
H56E H -0.2440 0.4743 0.8338 0.202 Uiso 0.50 1 calc PR D 2
H56F H -0.2854 0.5445 0.8524 0.202 Uiso 0.50 1 calc PR D 2
C57 C -0.4507(13) 0.0317(15) 0.7505(12) 0.39(3) Uani 0.50 1 d PD A 1
H57A H -0.4471 -0.0149 0.7329 0.616 Uiso 0.50 1 calc PR A 1
H57B H -0.4240 0.0628 0.7189 0.616 Uiso 0.50 1 calc PR A 1
C57' C -0.4500(14) 0.0313(13) 0.7085(10) 0.39(3) Uani 0.50 1 d PD B 2
H57C H -0.4133 -0.0043 0.6917 0.616 Uiso 0.50 1 calc PR B 2
H57D H -0.4420 0.0735 0.6825 0.616 Uiso 0.50 1 calc PR B 2
C58 C -0.5429(14) 0.0520(13) 0.7602(12) 0.229(9) Uani 0.50 1 d PD A 1
H58A H -0.5574 0.0358 0.8065 0.275 Uiso 0.50 1 calc PR A 1
H58B H -0.5476 0.1016 0.7597 0.275 Uiso 0.50 1 calc PR A 1
C58' C -0.5440(14) 0.0099(8) 0.7028(11) 0.229(9) Uani 0.50 1 d PD B 2
H58C H -0.5626 -0.0043 0.6538 0.275 Uiso 0.50 1 calc PR B 2
H58D H -0.5503 -0.0290 0.7342 0.275 Uiso 0.50 1 calc PR B 2
C59 C -0.6061(12) 0.0225(13) 0.7013(16) 0.369(16) Uani 0.50 1 d PD A 1
H59A H -0.6645 0.0323 0.7112 0.553 Uiso 0.50 1 calc PR A 1
H59B H -0.5982 -0.0262 0.6992 0.553 Uiso 0.50 1 calc PR A 1
H59C H -0.5961 0.0425 0.6560 0.553 Uiso 0.50 1 calc PR A 1
C59' C -0.6010(18) 0.0673(13) 0.723(2) 0.369(16) Uani 0.50 1 d PD B 2
H59D H -0.6462 0.0754 0.6847 0.553 Uiso 0.50 1 calc PR B 2
H59E H -0.5668 0.1081 0.7318 0.553 Uiso 0.50 1 calc PR B 2
H59F H -0.6266 0.0551 0.7661 0.553 Uiso 0.50 1 calc PR B 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.450(2) . ?
S1 O3 1.451(3) . ?
S1 O1 1.453(2) . ?
S1 C48 1.779(3) . ?
S2 O6 1.430(3) . ?
S2 O4 1.450(2) . ?
S2 O5 1.470(3) . ?
S2 C39 1.769(3) . ?
O7 C51' 1.420(9) . ?
O7 C51 1.426(9) . ?
O7 H7O 0.85(4) . ?
O8 C54 1.405(9) . ?
O8 C54' 1.408(9) . ?
O8 H8O 0.85(4) . ?
O9 C57 1.428(10) . ?
O9 H9O 0.8200 . ?
O9' C57' 1.425(10) . ?
O9' H9'O 0.8200 . ?
N1 C1 1.523(4) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
N2 C20 1.511(4) . ?
N2 H2N2 0.86(3) . ?
N2 H2N3 0.86(3) . ?
N2 H2N1 0.86(3) . ?
C1 C14 1.534(4) . ?
C1 C2 1.542(4) . ?
C1 C8 1.545(4) . ?
C2 C7 1.372(4) . ?
C2 C3 1.385(4) . ?
C3 C4 1.382(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.364(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.369(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.398(5) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.379(4) . ?
C8 C9 1.385(5) . ?
C9 C10 1.384(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.349(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.378(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.387(4) . ?
C14 C19 1.392(4) . ?
C15 C16 1.391(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.376(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.370(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.374(5) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C33 1.531(4) . ?
C20 C27 1.536(4) . ?
C20 C21 1.537(4) . ?
C21 C22 1.373(4) . ?
C21 C26 1.392(5) . ?
C22 C23 1.387(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.362(5) . ?
C23 H23A 0.9300 . ?
C24 C25 1.357(5) . ?
C24 H24A 0.9300 . ?
C25 C26 1.383(5) . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9300 . ?
C27 C28 1.377(5) . ?
C27 C32 1.383(5) . ?
C28 C29 1.386(5) . ?
C28 H28A 0.9300 . ?
C29 C30 1.376(6) . ?
C29 H29A 0.9300 . ?
C30 C31 1.362(6) . ?
C30 H30A 0.9300 . ?
C31 C32 1.385(5) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
C33 C34 1.382(4) . ?
C33 C38 1.385(5) . ?
C34 C35 1.370(5) . ?
C34 H34A 0.9300 . ?
C35 C36 1.358(6) . ?
C35 H35A 0.9300 . ?
C36 C37 1.379(6) . ?
C36 H36A 0.9300 . ?
C37 C38 1.391(5) . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9300 . ?
C39 C44 1.376(5) . ?
C39 C40 1.387(4) . ?
C40 C41 1.384(4) . ?
C40 H40A 0.9300 . ?
C41 C42 1.385(4) . ?
C41 H41A 0.9300 . ?
C42 C43 1.383(4) . ?
C42 C45 1.491(4) . ?
C43 C44 1.392(4) . ?
C43 H43A 0.9300 . ?
C44 H44A 0.9300 . ?
C45 C50 1.386(4) . ?
C45 C46 1.394(4) . ?
C46 C47 1.388(4) . ?
C46 H46A 0.9300 . ?
C47 C48 1.380(4) . ?
C47 H47A 0.9300 . ?
C48 C49 1.373(4) . ?
C49 C50 1.385(4) . ?
C49 H49A 0.9300 . ?
C50 H50A 0.9300 . ?
C51 C52 1.477(10) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C51' C52' 1.476(10) . ?
C51' H51C 0.9700 . ?
C51' H51D 0.9700 . ?
C52 C53 1.489(10) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52' C53' 1.500(10) . ?
C52' H52C 0.9700 . ?
C52' H52D 0.9700 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C53' H53D 0.9600 . ?
C53' H53E 0.9600 . ?
C53' H53F 0.9600 . ?
C54 C55 1.487(10) . ?
C54 H54A 0.9700 . ?
C54 H54D 0.9700 . ?
C54' C55' 1.485(10) . ?
C54' H54B 0.9700 . ?
C54' H54C 0.9700 . ?
C55 C56 1.512(10) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C55' C56' 1.501(10) . ?
C55' H55C 0.9700 . ?
C55' H55D 0.9700 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C56' H56D 0.9600 . ?
C56' H56E 0.9600 . ?
C56' H56F 0.9600 . ?
C57 C58 1.509(10) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C57' C58' 1.505(10) . ?
C57' H57C 0.9700 . ?
C57' H57D 0.9700 . ?
C58 C59 1.505(10) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58' C59' 1.499(10) . ?
C58' H58C 0.9700 . ?
C58' H58D 0.9700 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C59' H59D 0.9600 . ?
C59' H59E 0.9600 . ?
C59' H59F 0.9600 . ?

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 S1 O3 111.05(15) . . ?
O2 S1 O1 113.42(16) . . ?
O3 S1 O1 113.11(15) . . ?
O2 S1 C48 105.18(13) . . ?
O3 S1 C48 107.21(15) . . ?
O1 S1 C48 106.24(14) . . ?
O6 S2 O4 113.79(18) . . ?
O6 S2 O5 110.7(2) . . ?
O4 S2 O5 113.50(17) . . ?
O6 S2 C39 105.83(15) . . ?
O4 S2 C39 105.77(15) . . ?
O5 S2 C39 106.58(17) . . ?
C51' O7 H7O 107(4) . . ?
C51 O7 H7O 124(4) . . ?
C54 O8 H8O 106(4) . . ?
C54' O8 H8O 118(4) . . ?
C57 O9 H9O 109.5 . . ?
C57' O9' H9'O 109.5 . . ?
C1 N1 H1N1 111(2) . . ?
C1 N1 H1N2 112(2) . . ?
H1N1 N1 H1N2 107.8(15) . . ?
C1 N1 H1N3 110(2) . . ?
H1N1 N1 H1N3 107.1(15) . . ?
H1N2 N1 H1N3 108.2(15) . . ?
C20 N2 H2N2 113(2) . . ?
C20 N2 H2N3 110(2) . . ?
H2N2 N2 H2N3 108.7(15) . . ?
C20 N2 H2N1 110(2) . . ?
H2N2 N2 H2N1 108.0(15) . . ?
H2N3 N2 H2N1 106.7(14) . . ?
N1 C1 C14 106.0(2) . . ?
N1 C1 C2 108.3(2) . . ?
C14 C1 C2 112.0(2) . . ?
N1 C1 C8 107.4(2) . . ?
C14 C1 C8 112.3(3) . . ?
C2 C1 C8 110.5(2) . . ?
C7 C2 C3 118.3(3) . . ?
C7 C2 C1 122.2(3) . . ?
C3 C2 C1 119.4(3) . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 H3A 119.4 . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
C5 C6 C7 119.8(4) . . ?
C5 C6 H6A 120.1 . . ?
C7 C6 H6A 120.1 . . ?
C2 C7 C6 120.6(3) . . ?
C2 C7 H7A 119.7 . . ?
C6 C7 H7A 119.7 . . ?
C13 C8 C9 118.2(3) . . ?
C13 C8 C1 120.7(3) . . ?
C9 C8 C1 121.0(3) . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9A 120.0 . . ?
C8 C9 H9A 120.0 . . ?
C11 C10 C9 121.4(4) . . ?
C11 C10 H10A 119.3 . . ?
C9 C10 H10A 119.3 . . ?
C10 C11 C12 119.4(4) . . ?
C10 C11 H11A 120.3 . . ?
C12 C11 H11A 120.3 . . ?
C11 C12 C13 119.9(4) . . ?
C11 C12 H12A 120.1 . . ?
C13 C12 H12A 120.1 . . ?
C8 C13 C12 121.1(3) . . ?
C8 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
C15 C14 C19 117.9(3) . . ?
C15 C14 C1 122.1(3) . . ?
C19 C14 C1 120.0(3) . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
C17 C16 C15 120.3(4) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C18 C17 C16 119.3(4) . . ?
C18 C17 H17A 120.3 . . ?
C16 C17 H17A 120.3 . . ?
C17 C18 C19 120.8(4) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C18 C19 C14 120.9(3) . . ?
C18 C19 H19A 119.5 . . ?
C14 C19 H19A 119.5 . . ?
N2 C20 C33 107.7(2) . . ?
N2 C20 C27 106.6(2) . . ?
C33 C20 C27 112.0(3) . . ?
N2 C20 C21 107.3(2) . . ?
C33 C20 C21 110.8(2) . . ?
C27 C20 C21 112.1(2) . . ?
C22 C21 C26 117.7(3) . . ?
C22 C21 C20 121.6(3) . . ?
C26 C21 C20 120.6(3) . . ?
C21 C22 C23 121.1(3) . . ?
C21 C22 H22A 119.4 . . ?
C23 C22 H22A 119.4 . . ?
C24 C23 C22 120.5(4) . . ?
C24 C23 H23A 119.8 . . ?
C22 C23 H23A 119.8 . . ?
C25 C24 C23 119.2(4) . . ?
C25 C24 H24A 120.4 . . ?
C23 C24 H24A 120.4 . . ?
C24 C25 C26 121.2(4) . . ?
C24 C25 H25A 119.4 . . ?
C26 C25 H25A 119.4 . . ?
C25 C26 C21 120.2(3) . . ?
C25 C26 H26A 119.9 . . ?
C21 C26 H26A 119.9 . . ?
C28 C27 C32 118.0(3) . . ?
C28 C27 C20 120.2(3) . . ?
C32 C27 C20 121.7(3) . . ?
C27 C28 C29 121.6(4) . . ?
C27 C28 H28A 119.2 . . ?
C29 C28 H28A 119.2 . . ?
C30 C29 C28 119.6(4) . . ?
C30 C29 H29A 120.2 . . ?
C28 C29 H29A 120.2 . . ?
C31 C30 C29 119.4(4) . . ?
C31 C30 H30A 120.3 . . ?
C29 C30 H30A 120.3 . . ?
C30 C31 C32 121.1(4) . . ?
C30 C31 H31A 119.5 . . ?
C32 C31 H31A 119.5 . . ?
C27 C32 C31 120.3(4) . . ?
C27 C32 H32A 119.8 . . ?
C31 C32 H32A 119.8 . . ?
C34 C33 C38 118.0(3) . . ?
C34 C33 C20 121.1(3) . . ?
C38 C33 C20 120.8(3) . . ?
C35 C34 C33 121.1(4) . . ?
C35 C34 H34A 119.5 . . ?
C33 C34 H34A 119.5 . . ?
C36 C35 C34 121.0(4) . . ?
C36 C35 H35A 119.5 . . ?
C34 C35 H35A 119.5 . . ?
C35 C36 C37 119.5(4) . . ?
C35 C36 H36A 120.3 . . ?
C37 C36 H36A 120.3 . . ?
C36 C37 C38 119.8(4) . . ?
C36 C37 H37A 120.1 . . ?
C38 C37 H37A 120.1 . . ?
C33 C38 C37 120.6(3) . . ?
C33 C38 H38A 119.7 . . ?
C37 C38 H38A 119.7 . . ?
C44 C39 C40 120.0(3) . . ?
C44 C39 S2 119.9(3) . . ?
C40 C39 S2 120.1(3) . . ?
C41 C40 C39 119.9(3) . . ?
C41 C40 H40A 120.0 . . ?
C39 C40 H40A 120.0 . . ?
C40 C41 C42 120.8(3) . . ?
C40 C41 H41A 119.6 . . ?
C42 C41 H41A 119.6 . . ?
C43 C42 C41 118.6(3) . . ?
C43 C42 C45 120.5(3) . . ?
C41 C42 C45 121.0(3) . . ?
C42 C43 C44 121.1(3) . . ?
C42 C43 H43A 119.4 . . ?
C44 C43 H43A 119.4 . . ?
C39 C44 C43 119.5(3) . . ?
C39 C44 H44A 120.2 . . ?
C43 C44 H44A 120.2 . . ?
C50 C45 C46 118.5(3) . . ?
C50 C45 C42 120.4(3) . . ?
C46 C45 C42 121.0(3) . . ?
C47 C46 C45 120.6(3) . . ?
C47 C46 H46A 119.7 . . ?
C45 C46 H46A 119.7 . . ?
C48 C47 C46 119.8(3) . . ?
C48 C47 H47A 120.1 . . ?
C46 C47 H47A 120.1 . . ?
C49 C48 C47 120.3(3) . . ?
C49 C48 S1 120.3(2) . . ?
C47 C48 S1 119.4(2) . . ?
C48 C49 C50 120.0(3) . . ?
C48 C49 H49A 120.0 . . ?
C50 C49 H49A 120.0 . . ?
C49 C50 C45 120.8(3) . . ?
C49 C50 H50A 119.6 . . ?
C45 C50 H50A 119.6 . . ?
O7 C51 C52 100.8(15) . . ?
O7 C51 H51A 111.6 . . ?
C52 C51 H51A 111.6 . . ?
O7 C51 H51B 111.6 . . ?
C52 C51 H51B 111.6 . . ?
H51A C51 H51B 109.4 . . ?
O7 C51' C52' 129(2) . . ?
O7 C51' H51C 105.0 . . ?
C52' C51' H51C 105.0 . . ?
O7 C51' H51D 105.0 . . ?
C52' C51' H51D 105.0 . . ?
H51C C51' H51D 105.8 . . ?
C51 C52 C53 113(2) . . ?
C51 C52 H52A 109.0 . . ?
C53 C52 H52A 109.0 . . ?
C51 C52 H52B 109.0 . . ?
C53 C52 H52B 109.0 . . ?
H52A C52 H52B 107.8 . . ?
C51' C52' C53' 104(2) . . ?
C51' C52' H52C 110.9 . . ?
C53' C52' H52C 110.9 . . ?
C51' C52' H52D 110.9 . . ?
C53' C52' H52D 110.9 . . ?
H52C C52' H52D 109.0 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52' C53' H53D 109.5 . . ?
C52' C53' H53E 109.5 . . ?
H53D C53' H53E 109.5 . . ?
C52' C53' H53F 109.5 . . ?
H53D C53' H53F 109.5 . . ?
H53E C53' H53F 109.5 . . ?
O8 C54 C55 120.4(16) . . ?
O8 C54 H54A 107.2 . . ?
C55 C54 H54A 107.2 . . ?
O8 C54 H54D 107.2 . . ?
C55 C54 H54D 107.2 . . ?
H54A C54 H54D 106.9 . . ?
O8 C54' C55' 106.4(13) . . ?
O8 C54' H54B 110.4 . . ?
C55' C54' H54B 110.4 . . ?
O8 C54' H54C 110.4 . . ?
C55' C54' H54C 110.4 . . ?
H54B C54' H54C 108.6 . . ?
C54 C55 C56 99.9(15) . . ?
C54 C55 H55A 111.8 . . ?
C56 C55 H55A 111.8 . . ?
C54 C55 H55B 111.8 . . ?
C56 C55 H55B 111.8 . . ?
H55A C55 H55B 109.5 . . ?
C54' C55' C56' 114.6(15) . . ?
C54' C55' H55C 108.6 . . ?
C56' C55' H55C 108.6 . . ?
C54' C55' H55D 108.6 . . ?
C56' C55' H55D 108.6 . . ?
H55C C55' H55D 107.6 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55' C56' H56D 109.5 . . ?
C55' C56' H56E 109.5 . . ?
H56D C56' H56E 109.5 . . ?
C55' C56' H56F 109.5 . . ?
H56D C56' H56F 109.5 . . ?
H56E C56' H56F 109.5 . . ?
O9 C57 C58 98.2(9) . . ?
O9 C57 H57A 112.1 . . ?
C58 C57 H57A 112.1 . . ?
O9 C57 H57B 112.1 . . ?
C58 C57 H57B 112.1 . . ?
H57A C57 H57B 109.8 . . ?
O9' C57' C58' 99.4(9) . . ?
O9' C57' H57C 111.9 . . ?
C58' C57' H57C 111.9 . . ?
O9' C57' H57D 111.9 . . ?
C58' C57' H57D 111.9 . . ?
H57C C57' H57D 109.6 . . ?
C59 C58 C57 111.1(10) . . ?
C59 C58 H58A 109.4 . . ?
C57 C58 H58A 109.4 . . ?
C59 C58 H58B 109.4 . . ?
C57 C58 H58B 109.4 . . ?
H58A C58 H58B 108.0 . . ?
C59' C58' C57' 111.4(10) . . ?
C59' C58' H58C 109.3 . . ?
C57' C58' H58C 109.3 . . ?
C59' C58' H58D 109.3 . . ?
C57' C58' H58D 109.3 . . ?
H58C C58' H58D 108.0 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58' C59' H59D 109.5 . . ?
C58' C59' H59E 109.5 . . ?
H59D C59' H59E 109.5 . . ?
C58' C59' H59F 109.5 . . ?
H59D C59' H59F 109.5 . . ?
H59E C59' H59F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C7 -25.7(4) . . . . ?
C14 C1 C2 C7 90.9(4) . . . . ?
C8 C1 C2 C7 -143.0(3) . . . . ?
N1 C1 C2 C3 157.1(3) . . . . ?
C14 C1 C2 C3 -86.3(4) . . . . ?
C8 C1 C2 C3 39.7(4) . . . . ?
C7 C2 C3 C4 -0.7(5) . . . . ?
C1 C2 C3 C4 176.7(4) . . . . ?
C2 C3 C4 C5 0.8(7) . . . . ?
C3 C4 C5 C6 -0.6(7) . . . . ?
C4 C5 C6 C7 0.2(7) . . . . ?
C3 C2 C7 C6 0.3(5) . . . . ?
C1 C2 C7 C6 -176.9(3) . . . . ?
C5 C6 C7 C2 -0.1(6) . . . . ?
N1 C1 C8 C13 -39.3(4) . . . . ?
C14 C1 C8 C13 -155.5(3) . . . . ?
C2 C1 C8 C13 78.7(3) . . . . ?
N1 C1 C8 C9 144.6(3) . . . . ?
C14 C1 C8 C9 28.4(4) . . . . ?
C2 C1 C8 C9 -97.5(4) . . . . ?
C13 C8 C9 C10 -1.9(5) . . . . ?
C1 C8 C9 C10 174.4(3) . . . . ?
C8 C9 C10 C11 1.1(7) . . . . ?
C9 C10 C11 C12 0.3(7) . . . . ?
C10 C11 C12 C13 -0.9(6) . . . . ?
C9 C8 C13 C12 1.3(5) . . . . ?
C1 C8 C13 C12 -175.0(3) . . . . ?
C11 C12 C13 C8 0.1(6) . . . . ?
N1 C1 C14 C15 117.2(3) . . . . ?
C2 C1 C14 C15 -0.8(4) . . . . ?
C8 C1 C14 C15 -125.8(3) . . . . ?
N1 C1 C14 C19 -62.0(4) . . . . ?
C2 C1 C14 C19 -180.0(3) . . . . ?
C8 C1 C14 C19 55.0(4) . . . . ?
C19 C14 C15 C16 -0.2(5) . . . . ?
C1 C14 C15 C16 -179.3(3) . . . . ?
C14 C15 C16 C17 -0.4(6) . . . . ?
C15 C16 C17 C18 0.6(6) . . . . ?
C16 C17 C18 C19 -0.4(7) . . . . ?
C17 C18 C19 C14 -0.1(6) . . . . ?
C15 C14 C19 C18 0.4(5) . . . . ?
C1 C14 C19 C18 179.6(3) . . . . ?
N2 C20 C21 C22 -37.0(4) . . . . ?
C33 C20 C21 C22 80.3(4) . . . . ?
C27 C20 C21 C22 -153.7(3) . . . . ?
N2 C20 C21 C26 145.5(3) . . . . ?
C33 C20 C21 C26 -97.2(4) . . . . ?
C27 C20 C21 C26 28.8(4) . . . . ?
C26 C21 C22 C23 -0.1(5) . . . . ?
C20 C21 C22 C23 -177.7(3) . . . . ?
C21 C22 C23 C24 1.3(6) . . . . ?
C22 C23 C24 C25 -1.2(7) . . . . ?
C23 C24 C25 C26 0.0(7) . . . . ?
C24 C25 C26 C21 1.1(6) . . . . ?
C22 C21 C26 C25 -1.0(5) . . . . ?
C20 C21 C26 C25 176.6(3) . . . . ?
N2 C20 C27 C28 -56.9(4) . . . . ?
C33 C20 C27 C28 -174.4(3) . . . . ?
C21 C20 C27 C28 60.2(4) . . . . ?
N2 C20 C27 C32 123.8(3) . . . . ?
C33 C20 C27 C32 6.2(4) . . . . ?
C21 C20 C27 C32 -119.1(3) . . . . ?
C32 C27 C28 C29 0.6(6) . . . . ?
C20 C27 C28 C29 -178.8(4) . . . . ?
C27 C28 C29 C30 -1.1(7) . . . . ?
C28 C29 C30 C31 0.4(7) . . . . ?
C29 C30 C31 C32 0.7(7) . . . . ?
C28 C27 C32 C31 0.5(5) . . . . ?
C20 C27 C32 C31 179.9(3) . . . . ?
C30 C31 C32 C27 -1.2(6) . . . . ?
N2 C20 C33 C34 151.2(3) . . . . ?
C27 C20 C33 C34 -92.0(4) . . . . ?
C21 C20 C33 C34 34.1(4) . . . . ?
N2 C20 C33 C38 -32.2(4) . . . . ?
C27 C20 C33 C38 84.6(4) . . . . ?
C21 C20 C33 C38 -149.3(3) . . . . ?
C38 C33 C34 C35 -0.7(6) . . . . ?
C20 C33 C34 C35 175.9(4) . . . . ?
C33 C34 C35 C36 0.3(7) . . . . ?
C34 C35 C36 C37 0.5(7) . . . . ?
C35 C36 C37 C38 -0.9(7) . . . . ?
C34 C33 C38 C37 0.3(6) . . . . ?
C20 C33 C38 C37 -176.3(3) . . . . ?
C36 C37 C38 C33 0.5(6) . . . . ?
O6 S2 C39 C44 96.0(3) . . . . ?
O4 S2 C39 C44 -143.0(3) . . . . ?
O5 S2 C39 C44 -21.9(3) . . . . ?
O6 S2 C39 C40 -80.9(3) . . . . ?
O4 S2 C39 C40 40.1(3) . . . . ?
O5 S2 C39 C40 161.2(3) . . . . ?
C44 C39 C40 C41 0.8(5) . . . . ?
S2 C39 C40 C41 177.6(3) . . . . ?
C39 C40 C41 C42 0.6(5) . . . . ?
C40 C41 C42 C43 -1.4(5) . . . . ?
C40 C41 C42 C45 177.5(3) . . . . ?
C41 C42 C43 C44 0.8(5) . . . . ?
C45 C42 C43 C44 -178.1(3) . . . . ?
C40 C39 C44 C43 -1.3(5) . . . . ?
S2 C39 C44 C43 -178.2(3) . . . . ?
C42 C43 C44 C39 0.5(5) . . . . ?
C43 C42 C45 C50 44.0(4) . . . . ?
C41 C42 C45 C50 -134.9(3) . . . . ?
C43 C42 C45 C46 -135.0(3) . . . . ?
C41 C42 C45 C46 46.1(4) . . . . ?
C50 C45 C46 C47 -1.5(5) . . . . ?
C42 C45 C46 C47 177.6(3) . . . . ?
C45 C46 C47 C48 1.0(5) . . . . ?
C46 C47 C48 C49 -0.3(5) . . . . ?
C46 C47 C48 S1 177.7(2) . . . . ?
O2 S1 C48 C49 100.6(3) . . . . ?
O3 S1 C48 C49 -17.7(3) . . . . ?
O1 S1 C48 C49 -138.9(3) . . . . ?
O2 S1 C48 C47 -77.4(3) . . . . ?
O3 S1 C48 C47 164.3(2) . . . . ?
O1 S1 C48 C47 43.1(3) . . . . ?
C47 C48 C49 C50 0.0(5) . . . . ?
S1 C48 C49 C50 -178.0(3) . . . . ?
C48 C49 C50 C45 -0.5(5) . . . . ?
C46 C45 C50 C49 1.2(5) . . . . ?
C42 C45 C50 C49 -177.9(3) . . . . ?
C51' O7 C51 C52 37(9) . . . . ?
C51 O7 C51' C52' -115(13) . . . . ?
O7 C51 C52 C53 -93(3) . . . . ?
O7 C51' C52' C53' -56(4) . . . . ?
C54' O8 C54 C55 -56(5) . . . . ?
C54 O8 C54' C55' 63(6) . . . . ?
O8 C54 C55 C56 -96(2) . . . . ?
O8 C54' C55' C56' -168.2(17) . . . . ?
O9 C57 C58 C59 -156(3) . . . . ?
O9' C57' C58' C59' 66(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7O O5 0.85(4) 1.892(17) 2.731(4) 165(5) .
O8 H8O O7 0.85(4) 2.20(2) 2.996(4) 156(5) 1_455
O8 H8O O3 0.85(4) 2.55(5) 3.004(4) 115(4) .
O9' H9'O O1 0.82 2.58 3.40(2) 177.6 .
N1 H1N1 O1 0.86(3) 2.019(14) 2.862(3) 165(3) .
N1 H1N2 O6 0.86(3) 2.006(11) 2.854(4) 169(2) 1_455
N1 H1N3 O8 0.86(3) 1.980(11) 2.842(4) 174(3) .
N2 H2N2 O2 0.86(3) 2.047(12) 2.892(4) 169(3) 1_655
N2 H2N2 O3 0.86(3) 2.59(3) 3.116(4) 120(2) 1_655
N2 H2N3 O7 0.86(3) 2.035(12) 2.886(4) 169(3) .
N2 H2N1 O4 0.86(3) 1.942(14) 2.786(3) 164(3) .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.047
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1044773'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), 2(C4 H10 O)'
_chemical_formula_sum            'C58 H64 N2 O8 S2'
_chemical_formula_weight         981.23

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.2879(11)
_cell_length_b                   11.4520(10)
_cell_length_c                   11.8164(8)
_cell_angle_alpha                103.006(7)
_cell_angle_beta                 93.516(7)
_cell_angle_gamma                91.882(8)
_cell_volume                     1352.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1643
_cell_measurement_theta_min      3.57
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             522
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9656
_exptl_absorpt_correction_T_max  0.9759
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7296
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.57
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4738
_reflns_number_gt                3049
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.1150P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4738
_refine_ls_number_parameters     334
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.2143
_refine_ls_wR_factor_gt          0.1897
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.13452(8) 0.85210(7) 0.57392(7) 0.0524(3) Uani 1 1 d . . .
O1 O -0.1288(2) 0.89044(19) 0.46496(19) 0.0574(6) Uani 1 1 d . . .
O2 O -0.0143(2) 0.8039(2) 0.6097(2) 0.0714(7) Uani 1 1 d . . .
O3 O -0.1819(2) 0.9453(2) 0.6661(2) 0.0706(7) Uani 1 1 d . . .
O4 O 0.2261(3) 0.7801(3) 0.5173(3) 0.0897(9) Uani 1 1 d D . .
H4O H 0.155(3) 0.794(5) 0.549(4) 0.135 Uiso 1 1 d D . .
N1 N 0.0772(3) 0.8261(2) 0.3278(2) 0.0511(7) Uani 1 1 d D . .
H1N1 H 0.106(2) 0.8965(16) 0.322(3) 0.077 Uiso 1 1 d D . .
H1N2 H 0.0036(16) 0.837(3) 0.361(3) 0.077 Uiso 1 1 d D . .
H1N3 H 0.131(2) 0.806(3) 0.379(2) 0.077 Uiso 1 1 d D . .
C1 C 0.0609(3) 0.7310(3) 0.2143(3) 0.0533(8) Uani 1 1 d . . .
C2 C 0.1984(4) 0.6919(4) 0.1856(3) 0.0680(11) Uani 1 1 d . . .
C3 C 0.2980(4) 0.7770(5) 0.1929(4) 0.0950(15) Uani 1 1 d . . .
H3A H 0.2805 0.8576 0.2167 0.114 Uiso 1 1 calc R . .
C4 C 0.4245(5) 0.7461(8) 0.1657(5) 0.136(2) Uani 1 1 d . . .
H4A H 0.4911 0.8045 0.1715 0.163 Uiso 1 1 calc R . .
C5 C 0.4466(7) 0.6248(10) 0.1297(5) 0.153(4) Uani 1 1 d . . .
H5A H 0.5302 0.6013 0.1125 0.184 Uiso 1 1 calc R . .
C6 C 0.3494(8) 0.5408(8) 0.1191(5) 0.142(3) Uani 1 1 d . . .
H6A H 0.3661 0.4603 0.0924 0.171 Uiso 1 1 calc R . .
C7 C 0.2261(5) 0.5722(4) 0.1472(3) 0.0947(15) Uani 1 1 d . . .
H7A H 0.1604 0.5128 0.1405 0.114 Uiso 1 1 calc R . .
C8 C -0.0261(4) 0.6279(3) 0.2360(3) 0.0599(9) Uani 1 1 d . . .
C9 C 0.0064(5) 0.5755(3) 0.3283(3) 0.0864(14) Uani 1 1 d . . .
H9A H 0.0798 0.6043 0.3779 0.104 Uiso 1 1 calc R . .
C10 C -0.0692(6) 0.4812(4) 0.3470(4) 0.1070(17) Uani 1 1 d . . .
H10A H -0.0450 0.4456 0.4081 0.128 Uiso 1 1 calc R . .
C11 C -0.1802(6) 0.4387(4) 0.2767(4) 0.1004(15) Uani 1 1 d . . .
H11A H -0.2330 0.3774 0.2920 0.121 Uiso 1 1 calc R . .
C12 C -0.2113(5) 0.4875(4) 0.1847(4) 0.0883(13) Uani 1 1 d . . .
H12A H -0.2839 0.4570 0.1346 0.106 Uiso 1 1 calc R . .
C13 C -0.1360(4) 0.5828(3) 0.1646(3) 0.0695(10) Uani 1 1 d . . .
H13A H -0.1600 0.6165 0.1022 0.083 Uiso 1 1 calc R . .
C14 C -0.0020(3) 0.7872(3) 0.1198(3) 0.0549(8) Uani 1 1 d . . .
C15 C 0.0299(4) 0.7538(4) 0.0059(3) 0.0679(10) Uani 1 1 d . . .
H15A H 0.0945 0.6992 -0.0128 0.081 Uiso 1 1 calc R . .
C16 C -0.0308(4) 0.7987(4) -0.0811(4) 0.0824(12) Uani 1 1 d . . .
H16A H -0.0075 0.7741 -0.1573 0.099 Uiso 1 1 calc R . .
C17 C -0.1248(5) 0.8790(4) -0.0554(4) 0.0903(14) Uani 1 1 d . . .
H17A H -0.1661 0.9099 -0.1137 0.108 Uiso 1 1 calc R . .
C18 C -0.1582(5) 0.9140(5) 0.0570(4) 0.0989(15) Uani 1 1 d . . .
H18A H -0.2226 0.9690 0.0748 0.119 Uiso 1 1 calc R . .
C19 C -0.0983(4) 0.8694(4) 0.1435(4) 0.0782(12) Uani 1 1 d . . .
H19A H -0.1225 0.8944 0.2194 0.094 Uiso 1 1 calc R . .
C20 C -0.2534(3) 0.7330(3) 0.5472(3) 0.0472(8) Uani 1 1 d . . .
C21 C -0.2607(4) 0.6553(4) 0.6195(4) 0.1018(17) Uani 1 1 d . . .
H21A H -0.1992 0.6633 0.6822 0.122 Uiso 1 1 calc R . .
C22 C -0.3560(4) 0.5667(4) 0.6013(4) 0.1018(18) Uani 1 1 d . . .
H22A H -0.3588 0.5166 0.6532 0.122 Uiso 1 1 calc R . .
C23 C -0.4486(3) 0.5484(3) 0.5093(3) 0.0498(8) Uani 1 1 d . . .
C24 C -0.4400(4) 0.6251(4) 0.4368(4) 0.0927(15) Uani 1 1 d . . .
H24A H -0.5000 0.6155 0.3728 0.111 Uiso 1 1 calc R . .
C25 C -0.3450(5) 0.7165(4) 0.4554(4) 0.0930(15) Uani 1 1 d . . .
H25A H -0.3432 0.7678 0.4047 0.112 Uiso 1 1 calc R . .
C26 C 0.3263(6) 0.8723(6) 0.5619(6) 0.129(2) Uani 0.50 1 d PD A 1
H26A H 0.2962 0.9504 0.5565 0.155 Uiso 0.50 1 calc PR A 1
H26B H 0.4038 0.8570 0.5191 0.155 Uiso 0.50 1 calc PR A 1
C26' C 0.3263(6) 0.8723(6) 0.5619(6) 0.129(2) Uani 0.50 1 d PD A 2
H26C H 0.2845 0.9454 0.5959 0.155 Uiso 0.50 1 calc PR A 2
H26D H 0.3718 0.8874 0.4967 0.155 Uiso 0.50 1 calc PR A 2
C27 C 0.3546(12) 0.8668(18) 0.6890(10) 0.154(4) Uani 0.50 1 d PD A 1
H27A H 0.2826 0.9016 0.7320 0.185 Uiso 0.50 1 calc PR A 1
H27D H 0.3542 0.7829 0.6921 0.185 Uiso 0.50 1 calc PR A 1
C27' C 0.4258(11) 0.8483(16) 0.6509(10) 0.154(4) Uani 0.50 1 d PD A 2
H27B H 0.4459 0.7644 0.6292 0.185 Uiso 0.50 1 calc PR A 2
H27C H 0.5051 0.8953 0.6475 0.185 Uiso 0.50 1 calc PR A 2
C28 C 0.4761(13) 0.9253(17) 0.7512(14) 0.256(9) Uani 0.50 1 d PD A 1
H28A H 0.4683 1.0115 0.7739 0.307 Uiso 0.50 1 calc PR A 1
H28B H 0.5486 0.9088 0.7022 0.307 Uiso 0.50 1 calc PR A 1
C28' C 0.3910(13) 0.874(2) 0.7670(12) 0.256(9) Uani 0.50 1 d PD A 2
H28C H 0.3232 0.8151 0.7736 0.307 Uiso 0.50 1 calc PR A 2
H28D H 0.3537 0.9517 0.7835 0.307 Uiso 0.50 1 calc PR A 2
C29 C 0.4971(13) 0.8734(17) 0.8583(8) 0.417(14) Uani 0.50 1 d PD A 1
H29A H 0.5757 0.9091 0.9024 0.625 Uiso 0.50 1 calc PR A 1
H29B H 0.5046 0.7882 0.8345 0.625 Uiso 0.50 1 calc PR A 1
H29C H 0.4245 0.8902 0.9057 0.625 Uiso 0.50 1 calc PR A 1
C29' C 0.4971(13) 0.8734(17) 0.8583(8) 0.417(14) Uani 0.50 1 d PD A 2
H29D H 0.4631 0.8945 0.9337 0.625 Uiso 0.50 1 calc PR A 2
H29E H 0.5655 0.9307 0.8532 0.625 Uiso 0.50 1 calc PR A 2
H29F H 0.5313 0.7949 0.8469 0.625 Uiso 0.50 1 calc PR A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.449(2) . ?
S1 O1 1.455(2) . ?
S1 O3 1.463(2) . ?
S1 C20 1.763(3) . ?
O4 C26 1.438(6) . ?
O4 H4O 0.85(4) . ?
N1 C1 1.522(4) . ?
N1 H1N1 0.86(4) . ?
N1 H1N2 0.86(4) . ?
N1 H1N3 0.86(4) . ?
C1 C14 1.530(4) . ?
C1 C2 1.533(5) . ?
C1 C8 1.535(5) . ?
C2 C3 1.376(6) . ?
C2 C7 1.388(6) . ?
C3 C4 1.397(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.389(11) . ?
C4 H4A 0.9300 . ?
C5 C6 1.345(10) . ?
C5 H5A 0.9300 . ?
C6 C7 1.369(8) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.381(5) . ?
C8 C9 1.388(5) . ?
C9 C10 1.377(6) . ?
C9 H9A 0.9300 . ?
C10 C11 1.377(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.356(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.389(6) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.378(5) . ?
C14 C19 1.386(5) . ?
C15 C16 1.376(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.357(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.367(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.365(5) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.367(5) . ?
C20 C25 1.368(5) . ?
C21 C22 1.360(5) . ?
C21 H21A 0.9300 . ?
C22 C23 1.375(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.362(5) . ?
C23 C23 1.478(6) 2_466 ?
C24 C25 1.379(5) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.528(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.470(9) . ?
C27 H27A 0.9700 . ?
C27 H27D 0.9700 . ?
C27' C28' 1.407(9) . ?
C27' H27B 0.9700 . ?
C27' H27C 0.9700 . ?
C28 C29 1.521(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28' H28C 0.9700 . ?
C28' H28D 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?

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 S1 O1 113.37(14) . . ?
O2 S1 O3 112.78(16) . . ?
O1 S1 O3 112.02(14) . . ?
O2 S1 C20 106.22(13) . . ?
O1 S1 C20 105.96(14) . . ?
O3 S1 C20 105.77(14) . . ?
C26 O4 H4O 113(4) . . ?
C1 N1 H1N1 115(2) . . ?
C1 N1 H1N2 112(2) . . ?
H1N1 N1 H1N2 106.1(15) . . ?
C1 N1 H1N3 113(2) . . ?
H1N1 N1 H1N3 105.2(15) . . ?
H1N2 N1 H1N3 105.5(14) . . ?
N1 C1 C14 108.6(2) . . ?
N1 C1 C2 106.1(3) . . ?
C14 C1 C2 111.1(3) . . ?
N1 C1 C8 107.2(2) . . ?
C14 C1 C8 111.4(3) . . ?
C2 C1 C8 112.1(3) . . ?
C3 C2 C7 117.9(4) . . ?
C3 C2 C1 119.9(3) . . ?
C7 C2 C1 122.2(4) . . ?
C2 C3 C4 122.1(5) . . ?
C2 C3 H3A 118.9 . . ?
C4 C3 H3A 118.9 . . ?
C5 C4 C3 117.3(7) . . ?
C5 C4 H4A 121.4 . . ?
C3 C4 H4A 121.4 . . ?
C6 C5 C4 121.2(6) . . ?
C6 C5 H5A 119.4 . . ?
C4 C5 H5A 119.4 . . ?
C5 C6 C7 120.9(7) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C6 C7 C2 120.6(6) . . ?
C6 C7 H7A 119.7 . . ?
C2 C7 H7A 119.7 . . ?
C13 C8 C9 118.0(4) . . ?
C13 C8 C1 122.0(3) . . ?
C9 C8 C1 119.9(3) . . ?
C10 C9 C8 120.5(4) . . ?
C10 C9 H9A 119.8 . . ?
C8 C9 H9A 119.8 . . ?
C9 C10 C11 120.9(4) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 H10A 119.5 . . ?
C12 C11 C10 119.0(4) . . ?
C12 C11 H11A 120.5 . . ?
C10 C11 H11A 120.5 . . ?
C11 C12 C13 120.7(4) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C8 C13 C12 120.8(4) . . ?
C8 C13 H13A 119.6 . . ?
C12 C13 H13A 119.6 . . ?
C15 C14 C19 116.8(3) . . ?
C15 C14 C1 121.4(3) . . ?
C19 C14 C1 121.7(3) . . ?
C16 C15 C14 122.0(4) . . ?
C16 C15 H15A 119.0 . . ?
C14 C15 H15A 119.0 . . ?
C17 C16 C15 119.8(4) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C16 C17 C18 119.4(4) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
C19 C18 C17 120.9(4) . . ?
C19 C18 H18A 119.6 . . ?
C17 C18 H18A 119.6 . . ?
C18 C19 C14 121.0(4) . . ?
C18 C19 H19A 119.5 . . ?
C14 C19 H19A 119.5 . . ?
C21 C20 C25 117.1(3) . . ?
C21 C20 S1 121.4(3) . . ?
C25 C20 S1 121.4(2) . . ?
C22 C21 C20 121.2(3) . . ?
C22 C21 H21A 119.4 . . ?
C20 C21 H21A 119.4 . . ?
C21 C22 C23 122.5(3) . . ?
C21 C22 H22A 118.8 . . ?
C23 C22 H22A 118.8 . . ?
C24 C23 C22 116.1(3) . . ?
C24 C23 C23 122.2(4) . 2_466 ?
C22 C23 C23 121.8(3) . 2_466 ?
C23 C24 C25 121.9(3) . . ?
C23 C24 H24A 119.0 . . ?
C25 C24 H24A 119.0 . . ?
C20 C25 C24 121.2(3) . . ?
C20 C25 H25A 119.4 . . ?
C24 C25 H25A 119.4 . . ?
O4 C26 C27 104.8(7) . . ?
O4 C26 H26A 110.8 . . ?
C27 C26 H26A 110.8 . . ?
O4 C26 H26B 110.8 . . ?
C27 C26 H26B 110.8 . . ?
H26A C26 H26B 108.9 . . ?
C28 C27 C26 118.7(12) . . ?
C28 C27 H27A 107.6 . . ?
C26 C27 H27A 107.6 . . ?
C28 C27 H27D 107.6 . . ?
C26 C27 H27D 107.6 . . ?
H27A C27 H27D 107.1 . . ?
C28' C27' H27B 108.2 . . ?
C28' C27' H27C 108.2 . . ?
H27B C27' H27C 107.3 . . ?
C27 C28 C29 106.2(10) . . ?
C27 C28 H28A 110.5 . . ?
C29 C28 H28A 110.5 . . ?
C27 C28 H28B 110.5 . . ?
C29 C28 H28B 110.5 . . ?
H28A C28 H28B 108.7 . . ?
C27' C28' H28C 108.1 . . ?
C27' C28' H28D 108.1 . . ?
H28C C28' H28D 107.3 . . ?
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 . . ?

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
N1 C1 C2 C3 -46.7(4) . . . . ?
C14 C1 C2 C3 71.1(4) . . . . ?
C8 C1 C2 C3 -163.4(3) . . . . ?
N1 C1 C2 C7 136.1(3) . . . . ?
C14 C1 C2 C7 -106.1(4) . . . . ?
C8 C1 C2 C7 19.4(4) . . . . ?
C7 C2 C3 C4 -1.5(6) . . . . ?
C1 C2 C3 C4 -178.9(4) . . . . ?
C2 C3 C4 C5 0.5(8) . . . . ?
C3 C4 C5 C6 1.4(9) . . . . ?
C4 C5 C6 C7 -2.1(10) . . . . ?
C5 C6 C7 C2 1.0(8) . . . . ?
C3 C2 C7 C6 0.8(6) . . . . ?
C1 C2 C7 C6 178.1(4) . . . . ?
N1 C1 C8 C13 128.0(3) . . . . ?
C14 C1 C8 C13 9.4(4) . . . . ?
C2 C1 C8 C13 -115.9(4) . . . . ?
N1 C1 C8 C9 -53.3(4) . . . . ?
C14 C1 C8 C9 -172.0(3) . . . . ?
C2 C1 C8 C9 62.7(4) . . . . ?
C13 C8 C9 C10 0.2(6) . . . . ?
C1 C8 C9 C10 -178.5(4) . . . . ?
C8 C9 C10 C11 -1.6(8) . . . . ?
C9 C10 C11 C12 3.0(8) . . . . ?
C10 C11 C12 C13 -2.9(7) . . . . ?
C9 C8 C13 C12 -0.1(6) . . . . ?
C1 C8 C13 C12 178.5(3) . . . . ?
C11 C12 C13 C8 1.6(6) . . . . ?
N1 C1 C14 C15 145.4(3) . . . . ?
C2 C1 C14 C15 29.1(5) . . . . ?
C8 C1 C14 C15 -96.8(4) . . . . ?
N1 C1 C14 C19 -37.9(4) . . . . ?
C2 C1 C14 C19 -154.3(4) . . . . ?
C8 C1 C14 C19 79.9(4) . . . . ?
C19 C14 C15 C16 -0.4(6) . . . . ?
C1 C14 C15 C16 176.4(3) . . . . ?
C14 C15 C16 C17 0.4(6) . . . . ?
C15 C16 C17 C18 -0.2(7) . . . . ?
C16 C17 C18 C19 0.0(8) . . . . ?
C17 C18 C19 C14 0.0(7) . . . . ?
C15 C14 C19 C18 0.2(6) . . . . ?
C1 C14 C19 C18 -176.6(4) . . . . ?
O2 S1 C20 C21 41.7(4) . . . . ?
O1 S1 C20 C21 162.6(3) . . . . ?
O3 S1 C20 C21 -78.4(4) . . . . ?
O2 S1 C20 C25 -140.4(3) . . . . ?
O1 S1 C20 C25 -19.5(4) . . . . ?
O3 S1 C20 C25 99.6(4) . . . . ?
C25 C20 C21 C22 -0.9(7) . . . . ?
S1 C20 C21 C22 177.1(4) . . . . ?
C20 C21 C22 C23 1.2(8) . . . . ?
C21 C22 C23 C24 -0.4(7) . . . . ?
C21 C22 C23 C23 179.9(5) . . . 2_466 ?
C22 C23 C24 C25 -0.7(7) . . . . ?
C23 C23 C24 C25 179.0(5) 2_466 . . . ?
C21 C20 C25 C24 -0.2(7) . . . . ?
S1 C20 C25 C24 -178.2(4) . . . . ?
C23 C24 C25 C20 1.0(8) . . . . ?
O4 C26 C27 C28 163.2(15) . . . . ?
C26 C27 C28 C29 -162.9(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4O O2 0.85(4) 1.916(14) 2.762(4) 172(6) .
N1 H1N1 O3 0.86(4) 1.918(12) 2.781(4) 171(3) 2_576
N1 H1N2 O1 0.86(4) 1.914(15) 2.765(3) 165(3) .
N1 H1N3 O4 0.86(4) 1.934(13) 2.793(4) 168(3) .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.049
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1044774'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), 2(C5 H12 O)'
_chemical_formula_sum            'C60 H68 N2 O8 S2'
_chemical_formula_weight         1009.28

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.4668(7)
_cell_length_b                   11.3787(7)
_cell_length_c                   11.8377(8)
_cell_angle_alpha                103.561(6)
_cell_angle_beta                 92.449(6)
_cell_angle_gamma                92.814(5)
_cell_volume                     1366.76(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1485
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             538
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9715
_exptl_absorpt_correction_T_max  0.9789
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6686
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4805
_reflns_number_gt                3306
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0651P)²+0.4340P] where P=(Fo²+2Fc²)/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         4805
_refine_ls_number_parameters     352
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1570
_refine_ls_wR_factor_gt          0.1417
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.13279(7) 0.64881(6) 0.92542(7) 0.0451(2) Uani 1 1 d . . .
O1 O 0.12654(19) 0.60855(18) 1.03266(17) 0.0533(5) Uani 1 1 d . . .
O2 O 0.0159(2) 0.6975(2) 0.8922(2) 0.0668(6) Uani 1 1 d . . .
O3 O 0.1781(2) 0.55662(18) 0.83174(18) 0.0619(6) Uani 1 1 d . . .
O4 O -0.2233(3) 0.7147(3) 0.9876(2) 0.0814(8) Uani 1 1 d D . .
H4O H -0.155(3) 0.706(4) 0.951(4) 0.122 Uiso 1 1 d D . .
N1 N -0.0732(2) 0.6745(2) 1.17387(19) 0.0406(6) Uani 1 1 d D . .
H1N1 H -0.104(2) 0.6055(15) 1.183(2) 0.061 Uiso 1 1 d D . .
H1N2 H -0.0020(14) 0.659(2) 1.138(2) 0.061 Uiso 1 1 d D . .
H1N3 H -0.1253(18) 0.694(2) 1.1224(18) 0.061 Uiso 1 1 d D . .
C1 C -0.0572(3) 0.7715(2) 1.2857(2) 0.0409(7) Uani 1 1 d . . .
C2 C -0.1912(3) 0.8134(3) 1.3148(2) 0.0477(7) Uani 1 1 d . . .
C3 C -0.2935(3) 0.7298(4) 1.3044(3) 0.0689(10) Uani 1 1 d . . .
H3A H -0.2806 0.6477 1.2789 0.083 Uiso 1 1 calc R . .
C4 C -0.4150(4) 0.7659(5) 1.3312(4) 0.0910(13) Uani 1 1 d . . .
H4A H -0.4834 0.7086 1.3227 0.109 Uiso 1 1 calc R . .
C5 C -0.4343(5) 0.8860(6) 1.3701(4) 0.0959(16) Uani 1 1 d . . .
H5A H -0.5159 0.9106 1.3884 0.115 Uiso 1 1 calc R . .
C6 C -0.3350(5) 0.9694(4) 1.3821(3) 0.0868(14) Uani 1 1 d . . .
H6A H -0.3490 1.0511 1.4090 0.104 Uiso 1 1 calc R . .
C7 C -0.2130(4) 0.9348(3) 1.3549(3) 0.0635(9) Uani 1 1 d . . .
H7A H -0.1455 0.9931 1.3636 0.076 Uiso 1 1 calc R . .
C8 C 0.0313(3) 0.8733(2) 1.2622(2) 0.0432(7) Uani 1 1 d . . .
C9 C 0.1406(3) 0.9168(3) 1.3303(3) 0.0580(8) Uani 1 1 d . . .
H9A H 0.1631 0.8829 1.3921 0.070 Uiso 1 1 calc R . .
C10 C 0.2179(4) 1.0103(3) 1.3085(4) 0.0723(10) Uani 1 1 d . . .
H10A H 0.2914 1.0390 1.3559 0.087 Uiso 1 1 calc R . .
C11 C 0.1868(4) 1.0604(3) 1.2182(3) 0.0740(11) Uani 1 1 d . . .
H11A H 0.2395 1.1224 1.2029 0.089 Uiso 1 1 calc R . .
C12 C 0.0777(4) 1.0190(3) 1.1499(3) 0.0753(11) Uani 1 1 d . . .
H12A H 0.0557 1.0540 1.0888 0.090 Uiso 1 1 calc R . .
C13 C 0.0001(4) 0.9257(3) 1.1710(3) 0.0614(9) Uani 1 1 d . . .
H13A H -0.0736 0.8979 1.1237 0.074 Uiso 1 1 calc R . .
C14 C 0.0005(3) 0.7162(2) 1.3805(2) 0.0442(7) Uani 1 1 d . . .
C15 C -0.0312(3) 0.7542(3) 1.4948(3) 0.0591(9) Uani 1 1 d . . .
H15A H -0.0922 0.8114 1.5135 0.071 Uiso 1 1 calc R . .
C16 C 0.0254(4) 0.7092(4) 1.5816(3) 0.0724(10) Uani 1 1 d . . .
H16A H 0.0024 0.7360 1.6580 0.087 Uiso 1 1 calc R . .
C17 C 0.1152(4) 0.6254(4) 1.5558(4) 0.0803(12) Uani 1 1 d . . .
H17A H 0.1537 0.5949 1.6143 0.096 Uiso 1 1 calc R . .
C18 C 0.1479(4) 0.5868(4) 1.4435(4) 0.0816(12) Uani 1 1 d . . .
H18A H 0.2093 0.5298 1.4258 0.098 Uiso 1 1 calc R . .
C19 C 0.0916(3) 0.6307(3) 1.3560(3) 0.0642(9) Uani 1 1 d . . .
H19A H 0.1148 0.6029 1.2798 0.077 Uiso 1 1 calc R . .
C20 C 0.2518(3) 0.7687(2) 0.9530(2) 0.0392(7) Uani 1 1 d . . .
C21 C 0.3428(4) 0.7804(3) 1.0410(3) 0.0749(11) Uani 1 1 d . . .
H21A H 0.3400 0.7268 1.0894 0.090 Uiso 1 1 calc R . .
C22 C 0.4388(4) 0.8704(3) 1.0590(3) 0.0768(12) Uani 1 1 d . . .
H22A H 0.5002 0.8762 1.1196 0.092 Uiso 1 1 calc R . .
C23 C 0.4471(3) 0.9522(2) 0.9906(2) 0.0384(6) Uani 1 1 d . . .
C24 C 0.3527(3) 0.9404(3) 0.9048(3) 0.0693(10) Uani 1 1 d . . .
H24A H 0.3538 0.9949 0.8572 0.083 Uiso 1 1 calc R . .
C25 C 0.2560(3) 0.8508(3) 0.8864(3) 0.0707(11) Uani 1 1 d . . .
H25A H 0.1927 0.8464 0.8276 0.085 Uiso 1 1 calc R . .
C26 C -0.317(3) 0.620(2) 0.9426(16) 0.115(3) Uani 0.50 1 d PD A 1
H26A H -0.3824 0.6177 0.9978 0.138 Uiso 0.50 1 calc PR A 1
H26B H -0.2786 0.5424 0.9243 0.138 Uiso 0.50 1 calc PR A 1
C26' C -0.328(2) 0.628(2) 0.9669(15) 0.115(3) Uani 0.50 1 d PD A 2
H26C H -0.3990 0.6688 1.0060 0.138 Uiso 0.50 1 calc PR A 2
H26D H -0.3060 0.5669 1.0077 0.138 Uiso 0.50 1 calc PR A 2
C27 C -0.3723(16) 0.6500(11) 0.8343(14) 0.170(5) Uani 0.50 1 d PD A 1
H27A H -0.4120 0.7266 0.8575 0.204 Uiso 0.50 1 calc PR A 1
H27B H -0.3017 0.6628 0.7873 0.204 Uiso 0.50 1 calc PR A 1
C27' C -0.3802(16) 0.5622(10) 0.8482(11) 0.170(5) Uani 0.50 1 d PD A 2
H27C H -0.3178 0.5072 0.8118 0.204 Uiso 0.50 1 calc PR A 2
H27D H -0.4572 0.5141 0.8555 0.204 Uiso 0.50 1 calc PR A 2
C28 C -0.4641(14) 0.5654(12) 0.7615(11) 0.163(4) Uani 0.50 1 d PD A 1
H28A H -0.5445 0.5668 0.7996 0.195 Uiso 0.50 1 calc PR A 1
H28B H -0.4340 0.4845 0.7504 0.195 Uiso 0.50 1 calc PR A 1
C28' C -0.4098(16) 0.6427(12) 0.7746(12) 0.163(4) Uani 0.50 1 d PD A 2
H28C H -0.3317 0.6601 0.7388 0.195 Uiso 0.50 1 calc PR A 2
H28D H -0.4326 0.7184 0.8246 0.195 Uiso 0.50 1 calc PR A 2
C29 C -0.486(3) 0.595(4) 0.6451(19) 0.178(7) Uani 0.50 1 d PD A 1
H29A H -0.4038 0.5913 0.6101 0.214 Uiso 0.50 1 calc PR A 1
H29D H -0.5406 0.5283 0.5978 0.214 Uiso 0.50 1 calc PR A 1
C29' C -0.514(2) 0.605(4) 0.6790(18) 0.178(7) Uani 0.50 1 d PD A 2
H29B H -0.5053 0.5227 0.6340 0.214 Uiso 0.50 1 calc PR A 2
H29C H -0.5983 0.6117 0.7091 0.214 Uiso 0.50 1 calc PR A 2
C30 C -0.542(4) 0.708(5) 0.630(5) 0.155(9) Uani 0.50 1 d PD A 1
H30A H -0.5562 0.7042 0.5481 0.233 Uiso 0.50 1 calc PR A 1
H30B H -0.4832 0.7763 0.6639 0.233 Uiso 0.50 1 calc PR A 1
H30C H -0.6215 0.7180 0.6668 0.233 Uiso 0.50 1 calc PR A 1
C30' C -0.485(4) 0.696(5) 0.610(5) 0.155(9) Uani 0.50 1 d PD A 2
H30D H -0.5399 0.6777 0.5401 0.233 Uiso 0.50 1 calc PR A 2
H30E H -0.3973 0.6932 0.5899 0.233 Uiso 0.50 1 calc PR A 2
H30F H -0.5002 0.7752 0.6552 0.233 Uiso 0.50 1 calc PR A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.444(2) . ?
S1 O1 1.450(2) . ?
S1 O3 1.450(2) . ?
S1 C20 1.763(3) . ?
O4 C26' 1.409(9) . ?
O4 C26 1.410(8) . ?
O4 H4O 0.85(3) . ?
N1 C1 1.509(3) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.87(3) . ?
N1 H1N3 0.86(3) . ?
C1 C14 1.526(4) . ?
C1 C2 1.530(4) . ?
C1 C8 1.532(4) . ?
C2 C3 1.379(5) . ?
C2 C7 1.385(4) . ?
C3 C4 1.383(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.363(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.352(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.384(5) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.372(4) . ?
C8 C13 1.385(4) . ?
C9 C10 1.384(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.359(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.367(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.381(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.381(4) . ?
C14 C19 1.386(4) . ?
C15 C16 1.376(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.365(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.363(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.375(5) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C25 1.357(4) . ?
C20 C21 1.360(4) . ?
C21 C22 1.373(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.372(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.365(4) . ?
C23 C23 1.485(5) 2_677 ?
C24 C25 1.374(4) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.503(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26' C27' 1.496(10) . ?
C26' H26C 0.9700 . ?
C26' H26D 0.9700 . ?
C27 C28 1.429(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27' C28' 1.440(9) . ?
C27' H27C 0.9700 . ?
C27' H27D 0.9700 . ?
C28 C29 1.503(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28' C29' 1.505(10) . ?
C28' H28C 0.9700 . ?
C28' H28D 0.9700 . ?
C29 C30 1.491(10) . ?
C29 H29A 0.9700 . ?
C29 H29D 0.9700 . ?
C29' C30' 1.489(10) . ?
C29' H29B 0.9700 . ?
C29' H29C 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30' H30D 0.9600 . ?
C30' H30E 0.9600 . ?
C30' H30F 0.9600 . ?

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 S1 O1 113.68(13) . . ?
O2 S1 O3 112.54(14) . . ?
O1 S1 O3 111.97(13) . . ?
O2 S1 C20 106.59(13) . . ?
O1 S1 C20 105.83(13) . . ?
O3 S1 C20 105.48(12) . . ?
C26' O4 H4O 124(4) . . ?
C26 O4 H4O 112(4) . . ?
C1 N1 H1N1 113.3(18) . . ?
C1 N1 H1N2 114.1(18) . . ?
H1N1 N1 H1N2 106.0(14) . . ?
C1 N1 H1N3 112.1(18) . . ?
H1N1 N1 H1N3 105.9(14) . . ?
H1N2 N1 H1N3 104.8(14) . . ?
N1 C1 C14 108.4(2) . . ?
N1 C1 C2 106.6(2) . . ?
C14 C1 C2 111.0(2) . . ?
N1 C1 C8 106.7(2) . . ?
C14 C1 C8 111.9(2) . . ?
C2 C1 C8 112.0(2) . . ?
C3 C2 C7 118.1(3) . . ?
C3 C2 C1 120.3(3) . . ?
C7 C2 C1 121.6(3) . . ?
C2 C3 C4 121.1(4) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C7 120.8(4) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C6 C7 C2 120.1(4) . . ?
C6 C7 H7A 120.0 . . ?
C2 C7 H7A 120.0 . . ?
C9 C8 C13 118.2(3) . . ?
C9 C8 C1 122.1(3) . . ?
C13 C8 C1 119.7(3) . . ?
C8 C9 C10 121.0(3) . . ?
C8 C9 H9A 119.5 . . ?
C10 C9 H9A 119.5 . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11A 120.2 . . ?
C12 C11 H11A 120.2 . . ?
C11 C12 C13 120.5(3) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C12 C13 C8 120.4(3) . . ?
C12 C13 H13A 119.8 . . ?
C8 C13 H13A 119.8 . . ?
C15 C14 C19 117.6(3) . . ?
C15 C14 C1 121.1(3) . . ?
C19 C14 C1 121.2(3) . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 H15A 119.3 . . ?
C14 C15 H15A 119.3 . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 H17A 120.3 . . ?
C16 C17 H17A 120.3 . . ?
C17 C18 C19 121.0(4) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C18 C19 C14 120.5(3) . . ?
C18 C19 H19A 119.8 . . ?
C14 C19 H19A 119.8 . . ?
C25 C20 C21 118.2(3) . . ?
C25 C20 S1 121.1(2) . . ?
C21 C20 S1 120.7(2) . . ?
C20 C21 C22 120.7(3) . . ?
C20 C21 H21A 119.7 . . ?
C22 C21 H21A 119.7 . . ?
C23 C22 C21 122.1(3) . . ?
C23 C22 H22A 119.0 . . ?
C21 C22 H22A 119.0 . . ?
C24 C23 C22 116.1(3) . . ?
C24 C23 C23 122.3(3) . 2_677 ?
C22 C23 C23 121.6(3) . 2_677 ?
C23 C24 C25 122.2(3) . . ?
C23 C24 H24A 118.9 . . ?
C25 C24 H24A 118.9 . . ?
C20 C25 C24 120.7(3) . . ?
C20 C25 H25A 119.7 . . ?
C24 C25 H25A 119.7 . . ?
O4 C26 C27 104.2(9) . . ?
O4 C26 H26A 110.9 . . ?
C27 C26 H26A 110.9 . . ?
O4 C26 H26B 110.9 . . ?
C27 C26 H26B 110.9 . . ?
H26A C26 H26B 108.9 . . ?
O4 C26' C27' 123.9(14) . . ?
O4 C26' H26C 106.3 . . ?
C27' C26' H26C 106.3 . . ?
O4 C26' H26D 106.3 . . ?
C27' C26' H26D 106.3 . . ?
H26C C26' H26D 106.4 . . ?
C28 C27 C26 118.6(11) . . ?
C28 C27 H27A 107.7 . . ?
C26 C27 H27A 107.7 . . ?
C28 C27 H27B 107.7 . . ?
C26 C27 H27B 107.7 . . ?
H27A C27 H27B 107.1 . . ?
C28' C27' C26' 112.5(15) . . ?
C28' C27' H27C 109.1 . . ?
C26' C27' H27C 109.1 . . ?
C28' C27' H27D 109.1 . . ?
C26' C27' H27D 109.1 . . ?
H27C C27' H27D 107.8 . . ?
C27 C28 C29 111.4(16) . . ?
C27 C28 H28A 109.3 . . ?
C29 C28 H28A 109.3 . . ?
C27 C28 H28B 109.3 . . ?
C29 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
C27' C28' C29' 119.5(17) . . ?
C27' C28' H28C 107.4 . . ?
C29' C28' H28C 107.4 . . ?
C27' C28' H28D 107.4 . . ?
C29' C28' H28D 107.4 . . ?
H28C C28' H28D 107.0 . . ?
C30 C29 C28 124(3) . . ?
C30 C29 H29A 106.4 . . ?
C28 C29 H29A 106.4 . . ?
C30 C29 H29D 106.4 . . ?
C28 C29 H29D 106.4 . . ?
H29A C29 H29D 106.5 . . ?
C30' C29' C28' 100(3) . . ?
C30' C29' H29B 111.8 . . ?
C28' C29' H29B 111.8 . . ?
C30' C29' H29C 111.8 . . ?
C28' C29' H29C 111.8 . . ?
H29B C29' H29C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29' C30' H30D 109.5 . . ?
C29' C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C29' C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 44.1(3) . . . . ?
C14 C1 C2 C3 -73.8(3) . . . . ?
C8 C1 C2 C3 160.5(3) . . . . ?
N1 C1 C2 C7 -137.6(3) . . . . ?
C14 C1 C2 C7 104.5(3) . . . . ?
C8 C1 C2 C7 -21.3(4) . . . . ?
C7 C2 C3 C4 1.1(5) . . . . ?
C1 C2 C3 C4 179.5(3) . . . . ?
C2 C3 C4 C5 -0.9(6) . . . . ?
C3 C4 C5 C6 0.2(6) . . . . ?
C4 C5 C6 C7 0.3(7) . . . . ?
C5 C6 C7 C2 0.0(6) . . . . ?
C3 C2 C7 C6 -0.7(5) . . . . ?
C1 C2 C7 C6 -179.0(3) . . . . ?
N1 C1 C8 C9 -126.1(3) . . . . ?
C14 C1 C8 C9 -7.7(4) . . . . ?
C2 C1 C8 C9 117.6(3) . . . . ?
N1 C1 C8 C13 55.2(3) . . . . ?
C14 C1 C8 C13 173.6(3) . . . . ?
C2 C1 C8 C13 -61.1(3) . . . . ?
C13 C8 C9 C10 -0.1(5) . . . . ?
C1 C8 C9 C10 -178.9(3) . . . . ?
C8 C9 C10 C11 -0.4(5) . . . . ?
C9 C10 C11 C12 0.9(6) . . . . ?
C10 C11 C12 C13 -1.0(6) . . . . ?
C11 C12 C13 C8 0.4(5) . . . . ?
C9 C8 C13 C12 0.1(5) . . . . ?
C1 C8 C13 C12 178.9(3) . . . . ?
N1 C1 C14 C15 -146.6(3) . . . . ?
C2 C1 C14 C15 -29.9(4) . . . . ?
C8 C1 C14 C15 96.0(3) . . . . ?
N1 C1 C14 C19 36.8(4) . . . . ?
C2 C1 C14 C19 153.5(3) . . . . ?
C8 C1 C14 C19 -80.6(3) . . . . ?
C19 C14 C15 C16 0.1(5) . . . . ?
C1 C14 C15 C16 -176.6(3) . . . . ?
C14 C15 C16 C17 0.1(6) . . . . ?
C15 C16 C17 C18 -0.1(6) . . . . ?
C16 C17 C18 C19 -0.2(6) . . . . ?
C17 C18 C19 C14 0.4(6) . . . . ?
C15 C14 C19 C18 -0.4(5) . . . . ?
C1 C14 C19 C18 176.3(3) . . . . ?
O2 S1 C20 C25 -38.1(3) . . . . ?
O1 S1 C20 C25 -159.4(3) . . . . ?
O3 S1 C20 C25 81.7(3) . . . . ?
O2 S1 C20 C21 142.6(3) . . . . ?
O1 S1 C20 C21 21.3(3) . . . . ?
O3 S1 C20 C21 -97.5(3) . . . . ?
C25 C20 C21 C22 -2.3(6) . . . . ?
S1 C20 C21 C22 177.0(3) . . . . ?
C20 C21 C22 C23 0.4(6) . . . . ?
C21 C22 C23 C24 1.3(6) . . . . ?
C21 C22 C23 C23 -178.8(4) . . . 2_677 ?
C22 C23 C24 C25 -1.1(5) . . . . ?
C23 C23 C24 C25 179.0(4) 2_677 . . . ?
C21 C20 C25 C24 2.5(5) . . . . ?
S1 C20 C25 C24 -176.8(3) . . . . ?
C23 C24 C25 C20 -0.8(6) . . . . ?
C26' O4 C26 C27 123(12) . . . . ?
C26 O4 C26' C27' -20(8) . . . . ?
O4 C26 C27 C28 174.9(17) . . . . ?
O4 C26' C27' C28' -53(3) . . . . ?
C26 C27 C28 C29 -167(3) . . . . ?
C26' C27' C28' C29' -152(2) . . . . ?
C27 C28 C29 C30 -64(4) . . . . ?
C27' C28' C29' C30' -165.2(19) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4O O2 0.85(3) 1.947(14) 2.788(3) 170(5) .
N1 H1N1 O3 0.86(3) 1.930(12) 2.785(3) 168(3) 2_567
N1 H1N2 O1 0.87(3) 1.896(12) 2.755(3) 167(3) .
N1 H1N3 O4 0.86(3) 1.926(12) 2.791(3) 169(2) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1044775'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), 4(C3 H7 N O)'
_chemical_formula_sum            'C62 H72 N6 O10 S2'
_chemical_formula_weight         1125.38

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.6402(6)
_cell_length_b                   11.3384(8)
_cell_length_c                   13.9981(12)
_cell_angle_alpha                83.054(6)
_cell_angle_beta                 83.325(6)
_cell_angle_gamma                86.826(5)
_cell_volume                     1507.20(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2208
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             598
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9691
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8976
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6887
_reflns_number_gt                4647
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0874P)²+0.7084P] where P=(Fo²+2Fc²)/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         6887
_refine_ls_number_parameters     365
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0679
_refine_ls_wR_factor_ref         0.1988
_refine_ls_wR_factor_gt          0.1753
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.51319(7) 0.24623(6) 0.52606(5) 0.0432(2) Uani 1 1 d . . .
O1 O 0.4600(2) 0.24335(17) 0.43349(15) 0.0550(5) Uani 1 1 d . . .
O2 O 0.4275(2) 0.1864(2) 0.60621(17) 0.0754(7) Uani 1 1 d . . .
O3 O 0.5435(2) 0.36617(18) 0.53948(17) 0.0659(6) Uani 1 1 d . . .
O4 O 0.1205(2) 0.5287(2) 0.36892(16) 0.0688(6) Uani 1 1 d . . .
O5 O 0.0571(13) -0.0317(10) 0.8947(8) 0.392(9) Uani 1 1 d . . .
N1 N 0.4066(2) 0.47430(19) 0.33491(15) 0.0397(5) Uani 1 1 d D . .
H1N1 H 0.449(2) 0.5268(16) 0.3595(19) 0.060 Uiso 1 1 d D . .
H1N2 H 0.426(2) 0.4057(11) 0.3656(18) 0.060 Uiso 1 1 d D . .
H1N3 H 0.3176(10) 0.489(2) 0.3478(19) 0.060 Uiso 1 1 d D . .
N2 N -0.0577(3) 0.6651(2) 0.35040(19) 0.0615(7) Uani 1 1 d . . .
N3 N 0.2457(4) -0.0267(3) 0.8204(3) 0.0896(10) Uani 1 1 d . . .
C1 C 0.4471(2) 0.4824(2) 0.22657(17) 0.0374(5) Uani 1 1 d . . .
C2 C 0.3941(3) 0.3715(2) 0.19194(18) 0.0403(6) Uani 1 1 d . . .
C3 C 0.4668(3) 0.3207(3) 0.1150(2) 0.0554(7) Uani 1 1 d . . .
H3A H 0.5508 0.3519 0.0862 0.066 Uiso 1 1 calc R . .
C4 C 0.4163(4) 0.2244(3) 0.0803(3) 0.0715(9) Uani 1 1 d . . .
H4A H 0.4660 0.1917 0.0281 0.086 Uiso 1 1 calc R . .
C5 C 0.2929(4) 0.1767(3) 0.1227(3) 0.0748(10) Uani 1 1 d . . .
H5A H 0.2589 0.1119 0.0993 0.090 Uiso 1 1 calc R . .
C6 C 0.2209(4) 0.2249(4) 0.1988(3) 0.0807(11) Uani 1 1 d . . .
H6A H 0.1376 0.1925 0.2279 0.097 Uiso 1 1 calc R . .
C7 C 0.2702(3) 0.3215(3) 0.2335(3) 0.0654(9) Uani 1 1 d . . .
H7A H 0.2196 0.3536 0.2856 0.079 Uiso 1 1 calc R . .
C8 C 0.3745(2) 0.5969(2) 0.18207(18) 0.0409(6) Uani 1 1 d . . .
C9 C 0.2885(3) 0.5976(3) 0.1096(2) 0.0501(7) Uani 1 1 d . . .
H9A H 0.2743 0.5270 0.0852 0.060 Uiso 1 1 calc R . .
C10 C 0.2225(3) 0.7036(3) 0.0724(2) 0.0658(9) Uani 1 1 d . . .
H10A H 0.1651 0.7029 0.0235 0.079 Uiso 1 1 calc R . .
C11 C 0.2420(4) 0.8076(3) 0.1076(3) 0.0725(10) Uani 1 1 d . . .
H11A H 0.1974 0.8777 0.0832 0.087 Uiso 1 1 calc R . .
C12 C 0.3286(4) 0.8084(3) 0.1797(3) 0.0703(9) Uani 1 1 d . . .
H12A H 0.3416 0.8792 0.2042 0.084 Uiso 1 1 calc R . .
C13 C 0.3957(3) 0.7044(3) 0.2155(2) 0.0562(7) Uani 1 1 d . . .
H13A H 0.4559 0.7063 0.2626 0.067 Uiso 1 1 calc R . .
C14 C 0.6069(3) 0.4859(2) 0.20588(19) 0.0437(6) Uani 1 1 d . . .
C15 C 0.6909(3) 0.4069(3) 0.2592(3) 0.0638(9) Uani 1 1 d . . .
H15A H 0.6503 0.3553 0.3102 0.077 Uiso 1 1 calc R . .
C16 C 0.8357(3) 0.4037(4) 0.2373(3) 0.0828(12) Uani 1 1 d . . .
H16A H 0.8913 0.3504 0.2737 0.099 Uiso 1 1 calc R . .
C17 C 0.8961(3) 0.4795(4) 0.1620(3) 0.0826(12) Uani 1 1 d . . .
H17A H 0.9927 0.4774 0.1471 0.099 Uiso 1 1 calc R . .
C18 C 0.8150(4) 0.5577(4) 0.1090(3) 0.0811(11) Uani 1 1 d . . .
H18A H 0.8562 0.6091 0.0581 0.097 Uiso 1 1 calc R . .
C19 C 0.6702(3) 0.5608(3) 0.1309(2) 0.0632(8) Uani 1 1 d . . .
H19A H 0.6155 0.6145 0.0941 0.076 Uiso 1 1 calc R . .
C20 C 0.6763(3) 0.1652(2) 0.51929(19) 0.0402(6) Uani 1 1 d . . .
C21 C 0.6803(3) 0.0437(2) 0.5418(2) 0.0562(8) Uani 1 1 d . . .
H21A H 0.5980 0.0043 0.5618 0.067 Uiso 1 1 calc R . .
C22 C 0.8070(3) -0.0196(2) 0.5345(3) 0.0613(8) Uani 1 1 d . . .
H22A H 0.8082 -0.1017 0.5505 0.074 Uiso 1 1 calc R . .
C23 C 0.9319(3) 0.0346(2) 0.5043(2) 0.0443(6) Uani 1 1 d . . .
C24 C 0.9247(3) 0.1575(2) 0.4813(3) 0.0630(9) Uani 1 1 d . . .
H24A H 1.0064 0.1973 0.4601 0.076 Uiso 1 1 calc R . .
C25 C 0.7982(3) 0.2217(2) 0.4894(3) 0.0588(8) Uani 1 1 d . . .
H25A H 0.7961 0.3039 0.4744 0.071 Uiso 1 1 calc R . .
C26 C -0.1562(4) 0.6038(4) 0.4211(3) 0.0872(12) Uani 1 1 d . . .
H26A H -0.1118 0.5329 0.4505 0.131 Uiso 1 1 calc R . .
H26B H -0.2338 0.5830 0.3902 0.131 Uiso 1 1 calc R . .
H26C H -0.1890 0.6545 0.4699 0.131 Uiso 1 1 calc R . .
C27 C -0.1070(5) 0.7750(4) 0.2987(4) 0.123(2) Uani 1 1 d . . .
H27A H -0.0325 0.8076 0.2534 0.184 Uiso 1 1 calc R . .
H27B H -0.1377 0.8308 0.3440 0.184 Uiso 1 1 calc R . .
H27C H -0.1836 0.7595 0.2646 0.184 Uiso 1 1 calc R . .
C28 C 0.0706(3) 0.6227(3) 0.3317(3) 0.0689(9) Uani 1 1 d . . .
H28A H 0.1293 0.6681 0.2858 0.083 Uiso 1 1 calc R . .
C29 C 0.3232(11) -0.0691(5) 0.7377(5) 0.191(4) Uani 1 1 d . . .
H29A H 0.4154 -0.0389 0.7293 0.286 Uiso 1 1 calc R . .
H29B H 0.2769 -0.0425 0.6813 0.286 Uiso 1 1 calc R . .
H29C H 0.3295 -0.1544 0.7466 0.286 Uiso 1 1 calc R . .
C30 C 0.3116(9) 0.0491(6) 0.8724(6) 0.177(3) Uani 1 1 d . . .
H30A H 0.4051 0.0617 0.8424 0.266 Uiso 1 1 calc R . .
H30B H 0.3145 0.0131 0.9379 0.266 Uiso 1 1 calc R . .
H30C H 0.2600 0.1239 0.8724 0.266 Uiso 1 1 calc R . .
C31 C 0.1088(15) -0.0713(12) 0.8335(10) 0.241(5) Uiso 1 1 d . . .
H31A H 0.0722 -0.1232 0.7972 0.289 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.437(2) . ?
S1 O3 1.445(2) . ?
S1 O1 1.452(2) . ?
S1 C20 1.775(2) . ?
O4 C28 1.227(4) . ?
O5 C31 1.074(13) . ?
N1 C1 1.514(3) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
N2 C28 1.311(4) . ?
N2 C26 1.433(4) . ?
N2 C27 1.449(4) . ?
N3 C30 1.411(7) . ?
N3 C29 1.422(7) . ?
N3 C31 1.424(14) . ?
C1 C2 1.535(3) . ?
C1 C14 1.536(3) . ?
C1 C8 1.539(3) . ?
C2 C3 1.383(4) . ?
C2 C7 1.385(4) . ?
C3 C4 1.381(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.375(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.358(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.379(5) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.382(4) . ?
C8 C13 1.391(4) . ?
C9 C10 1.400(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.362(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.384(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C19 1.374(4) . ?
C14 C15 1.384(4) . ?
C15 C16 1.393(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.373(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.358(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.393(4) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C25 1.367(4) . ?
C20 C21 1.375(4) . ?
C21 C22 1.382(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.381(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.392(4) . ?
C23 C23 1.491(5) 2_756 ?
C24 C25 1.386(4) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9300 . ?

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 S1 O3 113.78(15) . . ?
O2 S1 O1 113.38(15) . . ?
O3 S1 O1 110.81(13) . . ?
O2 S1 C20 105.98(12) . . ?
O3 S1 C20 106.04(12) . . ?
O1 S1 C20 106.14(11) . . ?
C1 N1 H1N1 110.4(18) . . ?
C1 N1 H1N2 114.0(18) . . ?
H1N1 N1 H1N2 107.4(14) . . ?
C1 N1 H1N3 110.7(18) . . ?
H1N1 N1 H1N3 106.9(14) . . ?
H1N2 N1 H1N3 107.2(14) . . ?
C28 N2 C26 121.7(3) . . ?
C28 N2 C27 121.3(3) . . ?
C26 N2 C27 117.0(3) . . ?
C30 N3 C29 118.2(6) . . ?
C30 N3 C31 132.0(8) . . ?
C29 N3 C31 109.9(7) . . ?
N1 C1 C2 107.08(19) . . ?
N1 C1 C14 109.05(19) . . ?
C2 C1 C14 110.69(19) . . ?
N1 C1 C8 106.59(18) . . ?
C2 C1 C8 111.5(2) . . ?
C14 C1 C8 111.7(2) . . ?
C3 C2 C7 117.7(3) . . ?
C3 C2 C1 120.5(2) . . ?
C7 C2 C1 121.7(2) . . ?
C4 C3 C2 120.9(3) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C7 120.5(3) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
C6 C7 C2 121.0(3) . . ?
C6 C7 H7A 119.5 . . ?
C2 C7 H7A 119.5 . . ?
C9 C8 C13 118.2(3) . . ?
C9 C8 C1 122.6(2) . . ?
C13 C8 C1 119.1(2) . . ?
C8 C9 C10 120.7(3) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12A 119.9 . . ?
C11 C12 H12A 119.9 . . ?
C12 C13 C8 120.9(3) . . ?
C12 C13 H13A 119.6 . . ?
C8 C13 H13A 119.6 . . ?
C19 C14 C15 118.2(3) . . ?
C19 C14 C1 121.6(3) . . ?
C15 C14 C1 120.0(2) . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C17 C16 C15 119.8(3) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C19 120.1(4) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C14 C19 C18 121.1(3) . . ?
C14 C19 H19A 119.5 . . ?
C18 C19 H19A 119.5 . . ?
C25 C20 C21 119.4(2) . . ?
C25 C20 S1 120.84(19) . . ?
C21 C20 S1 119.8(2) . . ?
C20 C21 C22 119.8(3) . . ?
C20 C21 H21A 120.1 . . ?
C22 C21 H21A 120.1 . . ?
C23 C22 C21 122.4(3) . . ?
C23 C22 H22A 118.8 . . ?
C21 C22 H22A 118.8 . . ?
C22 C23 C24 116.6(2) . . ?
C22 C23 C23 122.0(3) . 2_756 ?
C24 C23 C23 121.3(3) . 2_756 ?
C25 C24 C23 121.3(3) . . ?
C25 C24 H24A 119.3 . . ?
C23 C24 H24A 119.3 . . ?
C20 C25 C24 120.5(2) . . ?
C20 C25 H25A 119.7 . . ?
C24 C25 H25A 119.7 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O4 C28 N2 126.1(3) . . ?
O4 C28 H28A 116.9 . . ?
N2 C28 H28A 116.9 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O5 C31 N3 104.5(15) . . ?
O5 C31 H31A 127.7 . . ?
N3 C31 H31A 127.7 . . ?

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
N1 C1 C2 C3 -147.5(2) . . . . ?
C14 C1 C2 C3 -28.7(3) . . . . ?
C8 C1 C2 C3 96.3(3) . . . . ?
N1 C1 C2 C7 35.0(3) . . . . ?
C14 C1 C2 C7 153.8(3) . . . . ?
C8 C1 C2 C7 -81.2(3) . . . . ?
C7 C2 C3 C4 0.8(5) . . . . ?
C1 C2 C3 C4 -176.8(3) . . . . ?
C2 C3 C4 C5 -0.6(5) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
C4 C5 C6 C7 0.4(6) . . . . ?
C5 C6 C7 C2 -0.2(6) . . . . ?
C3 C2 C7 C6 -0.4(5) . . . . ?
C1 C2 C7 C6 177.2(3) . . . . ?
N1 C1 C8 C9 -125.3(2) . . . . ?
C2 C1 C8 C9 -8.8(3) . . . . ?
C14 C1 C8 C9 115.7(3) . . . . ?
N1 C1 C8 C13 54.8(3) . . . . ?
C2 C1 C8 C13 171.3(2) . . . . ?
C14 C1 C8 C13 -64.2(3) . . . . ?
C13 C8 C9 C10 -1.3(4) . . . . ?
C1 C8 C9 C10 178.8(2) . . . . ?
C8 C9 C10 C11 -0.2(5) . . . . ?
C9 C10 C11 C12 0.6(5) . . . . ?
C10 C11 C12 C13 0.5(5) . . . . ?
C11 C12 C13 C8 -2.0(5) . . . . ?
C9 C8 C13 C12 2.3(4) . . . . ?
C1 C8 C13 C12 -177.8(3) . . . . ?
N1 C1 C14 C19 -138.4(3) . . . . ?
C2 C1 C14 C19 104.1(3) . . . . ?
C8 C1 C14 C19 -20.8(3) . . . . ?
N1 C1 C14 C15 46.0(3) . . . . ?
C2 C1 C14 C15 -71.5(3) . . . . ?
C8 C1 C14 C15 163.6(3) . . . . ?
C19 C14 C15 C16 0.1(5) . . . . ?
C1 C14 C15 C16 175.9(3) . . . . ?
C14 C15 C16 C17 -0.2(6) . . . . ?
C15 C16 C17 C18 0.2(7) . . . . ?
C16 C17 C18 C19 -0.2(6) . . . . ?
C15 C14 C19 C18 -0.1(5) . . . . ?
C1 C14 C19 C18 -175.8(3) . . . . ?
C17 C18 C19 C14 0.2(6) . . . . ?
O2 S1 C20 C25 -146.7(3) . . . . ?
O3 S1 C20 C25 -25.5(3) . . . . ?
O1 S1 C20 C25 92.4(3) . . . . ?
O2 S1 C20 C21 35.1(3) . . . . ?
O3 S1 C20 C21 156.3(2) . . . . ?
O1 S1 C20 C21 -85.8(3) . . . . ?
C25 C20 C21 C22 0.4(5) . . . . ?
S1 C20 C21 C22 178.6(3) . . . . ?
C20 C21 C22 C23 -0.6(5) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
C21 C22 C23 C23 -179.3(3) . . . 2_756 ?
C22 C23 C24 C25 0.6(5) . . . . ?
C23 C23 C24 C25 -180.0(3) 2_756 . . . ?
C21 C20 C25 C24 0.3(5) . . . . ?
S1 C20 C25 C24 -177.9(3) . . . . ?
C23 C24 C25 C20 -0.8(5) . . . . ?
C26 N2 C28 O4 1.2(6) . . . . ?
C27 N2 C28 O4 -177.3(4) . . . . ?
C30 N3 C31 O5 1.9(16) . . . . ?
C29 N3 C31 O5 -177.3(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N1 O3 0.86(3) 1.982(17) 2.767(3) 151(2) 2_666
N1 H1N2 O1 0.86(3) 1.994(10) 2.858(3) 176(2) .
N1 H1N3 O4 0.86(3) 1.926(9) 2.791(3) 176(3) .

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.050
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1044776'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), 4(C2 H6 O S)'
_chemical_formula_sum            'C58 H68 N2 O10 S6'
_chemical_formula_weight         1145.50

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   8.8152(6)
_cell_length_b                   9.3074(9)
_cell_length_c                   19.3273(11)
_cell_angle_alpha                87.102(6)
_cell_angle_beta                 89.767(5)
_cell_angle_gamma                63.850(8)
_cell_volume                     1421.31(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2042
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             606
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9369
_exptl_absorpt_correction_T_max  0.9452
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5696
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4950
_reflns_number_gt                3104
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0804P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4950
_refine_ls_number_parameters     355
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0669
_refine_ls_wR_factor_ref         0.1657
_refine_ls_wR_factor_gt          0.1480
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.81697(14) 1.09320(12) 0.13690(5) 0.0395(3) Uani 1 1 d . . .
S2 S 0.56192(14) 0.81781(15) 0.08603(6) 0.0495(3) Uani 1 1 d . . .
O1 O 0.7992(4) 1.1259(4) 0.20940(15) 0.0510(8) Uani 1 1 d . . .
O2 O 0.9511(6) 0.9350(4) 0.1260(2) 0.0835(13) Uani 1 1 d . . .
O3 O 0.6550(5) 1.1258(6) 0.1060(2) 0.0913(14) Uani 1 1 d . . .
O4 O 0.5810(4) 0.7721(4) 0.16193(16) 0.0535(8) Uani 1 1 d . . .
O5 O 1.0897(4) 0.5861(4) 0.2312(2) 0.0593(9) Uani 1 1 d . . .
N1 N 0.7777(4) 0.8306(4) 0.25727(15) 0.0294(7) Uani 1 1 d D . .
H1N1 H 0.725(4) 0.804(3) 0.2264(15) 0.044 Uiso 1 1 d D . .
H1N2 H 0.776(4) 0.921(2) 0.2423(17) 0.044 Uiso 1 1 d D . .
H1N3 H 0.8831(17) 0.760(3) 0.2568(19) 0.044 Uiso 1 1 d D . .
C1 C 0.7246(4) 0.8242(4) 0.33123(17) 0.0244(7) Uani 1 1 d . . .
C2 C 0.6962(4) 0.6739(4) 0.34336(19) 0.0275(8) Uani 1 1 d . . .
C3 C 0.7989(5) 0.5319(4) 0.3119(2) 0.0365(9) Uani 1 1 d . . .
H3A H 0.8829 0.5288 0.2819 0.044 Uiso 1 1 calc R . .
C4 C 0.7750(6) 0.3971(5) 0.3255(2) 0.0458(11) Uani 1 1 d . . .
H4A H 0.8438 0.3031 0.3045 0.055 Uiso 1 1 calc R . .
C5 C 0.6528(5) 0.3980(5) 0.3693(2) 0.0450(11) Uani 1 1 d . . .
H5A H 0.6384 0.3056 0.3779 0.054 Uiso 1 1 calc R . .
C6 C 0.5522(5) 0.5353(5) 0.4002(3) 0.0472(11) Uani 1 1 d . . .
H6A H 0.4684 0.5366 0.4298 0.057 Uiso 1 1 calc R . .
C7 C 0.5735(5) 0.6747(5) 0.3878(2) 0.0391(10) Uani 1 1 d . . .
H7A H 0.5049 0.7677 0.4096 0.047 Uiso 1 1 calc R . .
C8 C 0.5622(4) 0.9759(4) 0.3425(2) 0.0316(9) Uani 1 1 d . . .
C9 C 0.4358(5) 1.0392(5) 0.2913(2) 0.0470(11) Uani 1 1 d . . .
H9A H 0.4535 0.9936 0.2485 0.056 Uiso 1 1 calc R . .
C10 C 0.2866(6) 1.1673(6) 0.3034(3) 0.0697(16) Uani 1 1 d . . .
H10A H 0.2020 1.2075 0.2693 0.084 Uiso 1 1 calc R . .
C11 C 0.2614(5) 1.2349(6) 0.3637(3) 0.0493(11) Uani 1 1 d . . .
H11A H 0.1576 1.3208 0.3712 0.059 Uiso 1 1 calc R . .
C12 C 0.3822(6) 1.1833(6) 0.4150(3) 0.0573(13) Uani 1 1 d . . .
H12A H 0.3637 1.2362 0.4560 0.069 Uiso 1 1 calc R . .
C13 C 0.5334(5) 1.0495(5) 0.4046(2) 0.0407(10) Uani 1 1 d . . .
H13A H 0.6157 1.0093 0.4396 0.049 Uiso 1 1 calc R . .
C14 C 0.8737(4) 0.8152(4) 0.37733(19) 0.0289(8) Uani 1 1 d . . .
C15 C 0.9428(5) 0.7029(5) 0.4305(2) 0.0408(10) Uani 1 1 d . . .
H15A H 0.9032 0.6263 0.4390 0.049 Uiso 1 1 calc R . .
C16 C 1.0714(6) 0.7011(5) 0.4720(3) 0.0503(12) Uani 1 1 d . . .
H16A H 1.1164 0.6247 0.5085 0.060 Uiso 1 1 calc R . .
C17 C 1.1330(5) 0.8133(6) 0.4589(2) 0.0474(11) Uani 1 1 d . . .
H17A H 1.2228 0.8103 0.4851 0.057 Uiso 1 1 calc R . .
C18 C 1.0593(5) 0.9277(5) 0.4071(2) 0.0435(10) Uani 1 1 d . . .
H18A H 1.0966 1.0062 0.3993 0.052 Uiso 1 1 calc R . .
C19 C 0.9318(5) 0.9307(5) 0.3661(2) 0.0393(10) Uani 1 1 d . . .
H19A H 0.8842 1.0099 0.3308 0.047 Uiso 1 1 calc R . .
C20 C 0.8810(5) 1.2292(4) 0.09441(19) 0.0302(8) Uani 1 1 d . . .
C21 C 0.9045(6) 1.3465(5) 0.1282(2) 0.0422(10) Uani 1 1 d . . .
H21A H 0.8882 1.3557 0.1756 0.051 Uiso 1 1 calc R . .
C22 C 0.9527(6) 1.4502(5) 0.0902(2) 0.0424(10) Uani 1 1 d . . .
H22A H 0.9690 1.5280 0.1130 0.051 Uiso 1 1 calc R . .
C23 C 0.9766(4) 1.4414(4) 0.02058(19) 0.0294(8) Uani 1 1 d . . .
C24 C 0.9555(5) 1.3216(5) -0.01244(19) 0.0374(9) Uani 1 1 d . . .
H24A H 0.9741 1.3120 -0.0597 0.045 Uiso 1 1 calc R . .
C25 C 0.9087(5) 1.2191(5) 0.0227(2) 0.0357(9) Uani 1 1 d . . .
H25A H 0.8945 1.1409 -0.0007 0.043 Uiso 1 1 calc R . .
C26 C 0.5064(8) 0.6756(7) 0.0478(3) 0.0747(17) Uani 1 1 d . . .
H26A H 0.6031 0.5728 0.0489 0.112 Uiso 1 1 calc R . .
H26B H 0.4696 0.7105 0.0006 0.112 Uiso 1 1 calc R . .
H26C H 0.4167 0.6673 0.0733 0.112 Uiso 1 1 calc R . .
C27 C 0.3663(6) 0.9890(7) 0.0760(3) 0.0708(16) Uani 1 1 d . . .
H27A H 0.3756 1.0790 0.0940 0.106 Uiso 1 1 calc R . .
H27B H 0.2815 0.9702 0.1007 0.106 Uiso 1 1 calc R . .
H27C H 0.3350 1.0110 0.0277 0.106 Uiso 1 1 calc R . .
S3 S 1.2671(3) 0.5506(3) 0.25508(12) 0.0491(4) Uani 0.50 1 d P A 1
C28 C 1.4091(8) 0.4369(10) 0.2065(5) 0.125(3) Uani 0.50 1 d P A 1
H28A H 1.4143 0.3316 0.2104 0.187 Uiso 0.50 1 calc PR A 1
H28B H 1.5163 0.4312 0.2203 0.187 Uiso 0.50 1 calc PR A 1
H28C H 1.3833 0.4787 0.1594 0.187 Uiso 0.50 1 calc PR A 1
C29 C 1.2666(7) 0.7454(8) 0.2444(4) 0.0843(19) Uani 0.50 1 d P A 1
H29A H 1.1818 0.8192 0.2731 0.126 Uiso 0.50 1 calc PR A 1
H29B H 1.2422 0.7838 0.1967 0.126 Uiso 0.50 1 calc PR A 1
H29C H 1.3754 0.7363 0.2576 0.126 Uiso 0.50 1 calc PR A 1
S3' S 1.2277(3) 0.6183(3) 0.19341(12) 0.0491(4) Uani 0.50 1 d P A 2
C28' C 1.4091(8) 0.4369(10) 0.2065(5) 0.125(3) Uani 0.50 1 d P A 2
H28D H 1.3993 0.3569 0.1799 0.187 Uiso 0.50 1 calc PR A 2
H28E H 1.4214 0.4032 0.2548 0.187 Uiso 0.50 1 calc PR A 2
H28F H 1.5064 0.4508 0.1921 0.187 Uiso 0.50 1 calc PR A 2
C29' C 1.2666(7) 0.7454(8) 0.2444(4) 0.0843(19) Uani 0.50 1 d P A 2
H29D H 1.1725 0.8499 0.2406 0.126 Uiso 0.50 1 calc PR A 2
H29E H 1.3670 0.7524 0.2291 0.126 Uiso 0.50 1 calc PR A 2
H29F H 1.2818 0.7047 0.2917 0.126 Uiso 0.50 1 calc PR A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.442(3) . ?
S1 O3 1.447(4) . ?
S1 O2 1.451(4) . ?
S1 C20 1.766(4) . ?
S2 O4 1.496(3) . ?
S2 C27 1.761(5) . ?
S2 C26 1.792(6) . ?
O5 S3 1.517(3) . ?
O5 S3' 1.548(4) . ?
N1 C1 1.509(4) . ?
N1 H1N1 0.863(10) . ?
N1 H1N2 0.868(10) . ?
N1 H1N3 0.870(10) . ?
C1 C8 1.529(5) . ?
C1 C2 1.533(5) . ?
C1 C14 1.560(5) . ?
C2 C7 1.376(5) . ?
C2 C3 1.399(5) . ?
C3 C4 1.373(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.364(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.360(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.399(6) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.378(6) . ?
C8 C9 1.393(6) . ?
C9 C10 1.360(6) . ?
C9 H9A 0.9300 . ?
C10 C11 1.322(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.363(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.389(6) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.361(6) . ?
C14 C19 1.388(5) . ?
C15 C16 1.385(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.386(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.359(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.367(5) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.391(5) . ?
C20 C25 1.407(5) . ?
C21 C22 1.392(5) . ?
C21 H21A 0.9300 . ?
C22 C23 1.361(6) . ?
C22 H22A 0.9300 . ?
C23 C24 1.393(5) . ?
C23 C23 1.517(7) 2_785 ?
C24 C25 1.349(5) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
S3 C28 1.579(7) . ?
S3 C29 1.812(7) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 S1 O3 110.4(2) . . ?
O1 S1 O2 111.6(2) . . ?
O3 S1 O2 114.9(3) . . ?
O1 S1 C20 107.94(17) . . ?
O3 S1 C20 105.91(18) . . ?
O2 S1 C20 105.5(2) . . ?
O4 S2 C27 105.4(2) . . ?
O4 S2 C26 105.0(2) . . ?
C27 S2 C26 99.1(3) . . ?
S3 O5 S3' 49.91(14) . . ?
C1 N1 H1N1 116(2) . . ?
C1 N1 H1N2 116(2) . . ?
H1N1 N1 H1N2 106.6(16) . . ?
C1 N1 H1N3 105(2) . . ?
H1N1 N1 H1N3 106.5(15) . . ?
H1N2 N1 H1N3 106.0(15) . . ?
N1 C1 C8 108.7(3) . . ?
N1 C1 C2 108.3(3) . . ?
C8 C1 C2 111.0(3) . . ?
N1 C1 C14 105.9(3) . . ?
C8 C1 C14 111.6(3) . . ?
C2 C1 C14 111.3(3) . . ?
C7 C2 C3 118.9(3) . . ?
C7 C2 C1 120.3(3) . . ?
C3 C2 C1 120.7(3) . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C5 C4 C3 121.5(4) . . ?
C5 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
C6 C5 C4 119.3(4) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C5 C6 C7 120.8(4) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C2 C7 C6 119.8(4) . . ?
C2 C7 H7A 120.1 . . ?
C6 C7 H7A 120.1 . . ?
C13 C8 C9 118.2(4) . . ?
C13 C8 C1 121.1(3) . . ?
C9 C8 C1 120.7(4) . . ?
C10 C9 C8 120.5(5) . . ?
C10 C9 H9A 119.8 . . ?
C8 C9 H9A 119.8 . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 122.4(4) . . ?
C10 C11 H11A 118.8 . . ?
C12 C11 H11A 118.8 . . ?
C11 C12 C13 118.3(5) . . ?
C11 C12 H12A 120.9 . . ?
C13 C12 H12A 120.9 . . ?
C8 C13 C12 120.4(4) . . ?
C8 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C15 C14 C19 118.9(4) . . ?
C15 C14 C1 122.2(3) . . ?
C19 C14 C1 118.8(3) . . ?
C14 C15 C16 120.9(4) . . ?
C14 C15 H15A 119.5 . . ?
C16 C15 H15A 119.5 . . ?
C15 C16 C17 119.9(4) . . ?
C15 C16 H16A 120.0 . . ?
C17 C16 H16A 120.0 . . ?
C18 C17 C16 118.5(4) . . ?
C18 C17 H17A 120.7 . . ?
C16 C17 H17A 120.7 . . ?
C17 C18 C19 121.8(4) . . ?
C17 C18 H18A 119.1 . . ?
C19 C18 H18A 119.1 . . ?
C18 C19 C14 119.9(4) . . ?
C18 C19 H19A 120.1 . . ?
C14 C19 H19A 120.1 . . ?
C21 C20 C25 118.3(3) . . ?
C21 C20 S1 123.3(3) . . ?
C25 C20 S1 118.4(3) . . ?
C20 C21 C22 119.3(4) . . ?
C20 C21 H21A 120.4 . . ?
C22 C21 H21A 120.4 . . ?
C23 C22 C21 122.1(4) . . ?
C23 C22 H22A 119.0 . . ?
C21 C22 H22A 119.0 . . ?
C22 C23 C24 118.1(3) . . ?
C22 C23 C23 121.5(4) . 2_785 ?
C24 C23 C23 120.4(4) . 2_785 ?
C25 C24 C23 121.4(3) . . ?
C25 C24 H24A 119.3 . . ?
C23 C24 H24A 119.3 . . ?
C24 C25 C20 120.8(3) . . ?
C24 C25 H25A 119.6 . . ?
C20 C25 H25A 119.6 . . ?
S2 C26 H26A 109.5 . . ?
S2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
S2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
S2 C27 H27A 109.5 . . ?
S2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
S2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O5 S3 C28 113.4(4) . . ?
O5 S3 C29 102.5(3) . . ?
C28 S3 C29 106.3(4) . . ?
S3 C28 H28A 109.5 . . ?
S3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
S3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
S3 C29 H29A 109.5 . . ?
S3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
S3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

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
N1 C1 C2 C7 -146.7(3) . . . . ?
C8 C1 C2 C7 -27.5(4) . . . . ?
C14 C1 C2 C7 97.4(4) . . . . ?
N1 C1 C2 C3 36.1(4) . . . . ?
C8 C1 C2 C3 155.3(3) . . . . ?
C14 C1 C2 C3 -79.9(4) . . . . ?
C7 C2 C3 C4 0.3(6) . . . . ?
C1 C2 C3 C4 177.6(3) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
C3 C4 C5 C6 0.0(7) . . . . ?
C4 C5 C6 C7 -0.3(7) . . . . ?
C3 C2 C7 C6 -0.7(6) . . . . ?
C1 C2 C7 C6 -178.0(3) . . . . ?
C5 C6 C7 C2 0.7(6) . . . . ?
N1 C1 C8 C13 -143.5(3) . . . . ?
C2 C1 C8 C13 97.5(4) . . . . ?
C14 C1 C8 C13 -27.2(4) . . . . ?
N1 C1 C8 C9 39.4(4) . . . . ?
C2 C1 C8 C9 -79.6(4) . . . . ?
C14 C1 C8 C9 155.8(3) . . . . ?
C13 C8 C9 C10 -1.9(6) . . . . ?
C1 C8 C9 C10 175.3(4) . . . . ?
C8 C9 C10 C11 1.3(8) . . . . ?
C9 C10 C11 C12 1.4(8) . . . . ?
C10 C11 C12 C13 -3.4(8) . . . . ?
C9 C8 C13 C12 -0.1(6) . . . . ?
C1 C8 C13 C12 -177.3(4) . . . . ?
C11 C12 C13 C8 2.7(6) . . . . ?
N1 C1 C14 C15 -129.7(4) . . . . ?
C8 C1 C14 C15 112.3(4) . . . . ?
C2 C1 C14 C15 -12.2(5) . . . . ?
N1 C1 C14 C19 53.7(4) . . . . ?
C8 C1 C14 C19 -64.3(4) . . . . ?
C2 C1 C14 C19 171.2(3) . . . . ?
C19 C14 C15 C16 -1.3(6) . . . . ?
C1 C14 C15 C16 -177.9(4) . . . . ?
C14 C15 C16 C17 -1.0(7) . . . . ?
C15 C16 C17 C18 3.0(7) . . . . ?
C16 C17 C18 C19 -2.7(7) . . . . ?
C17 C18 C19 C14 0.5(7) . . . . ?
C15 C14 C19 C18 1.5(6) . . . . ?
C1 C14 C19 C18 178.2(4) . . . . ?
O1 S1 C20 C21 -1.1(4) . . . . ?
O3 S1 C20 C21 117.1(4) . . . . ?
O2 S1 C20 C21 -120.6(4) . . . . ?
O1 S1 C20 C25 179.3(3) . . . . ?
O3 S1 C20 C25 -62.4(4) . . . . ?
O2 S1 C20 C25 59.8(4) . . . . ?
C25 C20 C21 C22 0.6(6) . . . . ?
S1 C20 C21 C22 -179.0(3) . . . . ?
C20 C21 C22 C23 0.5(7) . . . . ?
C21 C22 C23 C24 -1.5(6) . . . . ?
C21 C22 C23 C23 177.9(4) . . . 2_785 ?
C22 C23 C24 C25 1.6(6) . . . . ?
C23 C23 C24 C25 -177.9(4) 2_785 . . . ?
C23 C24 C25 C20 -0.6(6) . . . . ?
C21 C20 C25 C24 -0.5(6) . . . . ?
S1 C20 C25 C24 179.1(3) . . . . ?
S3' O5 S3 C28 -59.1(4) . . . . ?
S3' O5 S3 C29 55.0(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N1 O4 0.86(4) 1.910(11) 2.767(4) 172(3) .
N1 H1N2 O1 0.86(4) 2.076(11) 2.940(4) 174(3) .
N1 H1N3 O5 0.86(4) 1.913(15) 2.754(4) 162(3) .

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.061
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1044777'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), C4 H8 O2'
_chemical_formula_sum            'C54 H52 N2 O8 S2'
_chemical_formula_weight         921.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   10.2797(10)
_cell_length_b                   10.6209(14)
_cell_length_c                   12.2253(9)
_cell_angle_alpha                81.195(9)
_cell_angle_beta                 74.204(8)
_cell_angle_gamma                69.673(11)
_cell_volume                     1201.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1661
_cell_measurement_theta_min      3.46
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             486
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9640
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7157
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.47
_diffrn_reflns_theta_max         27.57
_reflns_number_total             5493
_reflns_number_gt                3466
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0714P)²+0.4367P] where P=(Fo²+2Fc²)/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         5493
_refine_ls_number_parameters     307
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0652
_refine_ls_wR_factor_ref         0.1797
_refine_ls_wR_factor_gt          0.1549
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.07736(7) 0.86004(6) 1.15632(5) 0.0488(2) Uani 1 1 d . . .
O1 O -0.0392(3) 0.8910(3) 1.1044(2) 0.1133(11) Uani 1 1 d . . .
O2 O 0.2107(2) 0.7953(2) 1.08250(15) 0.0784(7) Uani 1 1 d . . .
O3 O 0.0757(4) 0.9750(2) 1.20284(19) 0.1220(13) Uani 1 1 d . . .
O4 O 0.0259(3) 0.6029(3) 0.9176(2) 0.0946(8) Uani 1 1 d . . .
N1 N 0.1809(2) 0.7940(2) 0.86319(18) 0.0541(6) Uani 1 1 d D . .
H1N1 H 0.199(3) 0.792(3) 0.9287(15) 0.081 Uiso 1 1 d D . .
H1N2 H 0.134(3) 0.740(2) 0.869(2) 0.081 Uiso 1 1 d D . .
H1N3 H 0.126(3) 0.8742(13) 0.850(2) 0.081 Uiso 1 1 d D . .
C1 C 0.3189(3) 0.7540(2) 0.7710(2) 0.0470(6) Uani 1 1 d . . .
C2 C 0.3756(3) 0.5999(3) 0.7756(2) 0.0481(6) Uani 1 1 d . . .
C3 C 0.4154(3) 0.5300(3) 0.6788(3) 0.0690(9) Uani 1 1 d . . .
H3A H 0.4028 0.5767 0.6096 0.083 Uiso 1 1 calc R . .
C4 C 0.4735(4) 0.3921(3) 0.6839(4) 0.0924(12) Uani 1 1 d . . .
H4A H 0.4987 0.3463 0.6184 0.111 Uiso 1 1 calc R . .
C5 C 0.4946(4) 0.3221(3) 0.7838(4) 0.0892(12) Uani 1 1 d . . .
H5A H 0.5363 0.2291 0.7859 0.107 Uiso 1 1 calc R . .
C6 C 0.4546(3) 0.3884(3) 0.8820(3) 0.0703(9) Uani 1 1 d . . .
H6A H 0.4675 0.3404 0.9507 0.084 Uiso 1 1 calc R . .
C7 C 0.3946(3) 0.5279(3) 0.8776(2) 0.0541(7) Uani 1 1 d . . .
H7A H 0.3671 0.5730 0.9438 0.065 Uiso 1 1 calc R . .
C8 C 0.4242(3) 0.8093(3) 0.7979(2) 0.0507(7) Uani 1 1 d . . .
C9 C 0.3785(4) 0.9319(3) 0.8460(2) 0.0691(9) Uani 1 1 d . . .
H9A H 0.2816 0.9803 0.8645 0.083 Uiso 1 1 calc R . .
C10 C 0.4742(6) 0.9821(4) 0.8664(3) 0.0909(12) Uani 1 1 d . . .
H10A H 0.4414 1.0636 0.9002 0.109 Uiso 1 1 calc R . .
C11 C 0.6166(6) 0.9154(5) 0.8383(3) 0.0901(13) Uani 1 1 d . . .
H11A H 0.6805 0.9515 0.8524 0.108 Uiso 1 1 calc R . .
C12 C 0.6661(4) 0.7943(4) 0.7890(3) 0.0863(11) Uani 1 1 d . . .
H12A H 0.7636 0.7487 0.7686 0.104 Uiso 1 1 calc R . .
C13 C 0.5691(3) 0.7407(3) 0.7701(3) 0.0682(9) Uani 1 1 d . . .
H13A H 0.6020 0.6578 0.7385 0.082 Uiso 1 1 calc R . .
C14 C 0.2827(3) 0.8136(3) 0.6564(2) 0.0548(7) Uani 1 1 d . . .
C15 C 0.1678(4) 0.7994(4) 0.6291(3) 0.0792(10) Uani 1 1 d . . .
H15A H 0.1103 0.7562 0.6817 0.095 Uiso 1 1 calc R . .
C16 C 0.1360(4) 0.8487(4) 0.5239(3) 0.0914(12) Uani 1 1 d . . .
H16A H 0.0579 0.8379 0.5067 0.110 Uiso 1 1 calc R . .
C17 C 0.2192(5) 0.9128(4) 0.4457(3) 0.0915(13) Uani 1 1 d . . .
H17A H 0.1976 0.9463 0.3757 0.110 Uiso 1 1 calc R . .
C18 C 0.3322(6) 0.9270(4) 0.4710(3) 0.0903(13) Uani 1 1 d . . .
H18A H 0.3896 0.9696 0.4175 0.108 Uiso 1 1 calc R . .
C19 C 0.3649(4) 0.8790(3) 0.5763(2) 0.0723(9) Uani 1 1 d . . .
H19A H 0.4428 0.8912 0.5927 0.087 Uiso 1 1 calc R . .
C20 C 0.0515(3) 0.7406(2) 1.2721(2) 0.0447(6) Uani 1 1 d . . .
C21 C 0.1615(3) 0.6336(3) 1.2926(3) 0.0744(11) Uani 1 1 d . . .
H21A H 0.2524 0.6216 1.2459 0.089 Uiso 1 1 calc R . .
C22 C 0.1401(3) 0.5411(3) 1.3830(3) 0.0807(12) Uani 1 1 d . . .
H22A H 0.2185 0.4692 1.3965 0.097 Uiso 1 1 calc R . .
C23 C 0.0105(3) 0.5508(2) 1.4523(2) 0.0504(7) Uani 1 1 d . . .
C24 C -0.1005(3) 0.6605(4) 1.4296(3) 0.1141(18) Uani 1 1 d . . .
H24A H -0.1920 0.6713 1.4749 0.137 Uiso 1 1 calc R . .
C25 C -0.0802(3) 0.7553(4) 1.3412(3) 0.1069(17) Uani 1 1 d . . .
H25A H -0.1573 0.8296 1.3292 0.128 Uiso 1 1 calc R . .
C26 C -0.0942(4) 0.6303(5) 1.0124(4) 0.1030(14) Uani 1 1 d . . .
H26A H -0.1761 0.6244 0.9913 0.124 Uiso 1 1 calc R . .
H26B H -0.1171 0.7210 1.0342 0.124 Uiso 1 1 calc R . .
C27 C 0.0635(5) 0.4676(6) 0.8892(4) 0.1068(15) Uani 1 1 d . . .
H27A H 0.1470 0.4483 0.8261 0.128 Uiso 1 1 calc R . .
H27B H -0.0143 0.4570 0.8649 0.128 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.417(2) . ?
S1 O1 1.422(3) . ?
S1 O2 1.424(2) . ?
S1 C20 1.778(2) . ?
O4 C26 1.424(4) . ?
O4 C27 1.424(5) . ?
N1 C1 1.524(3) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
C1 C8 1.523(4) . ?
C1 C2 1.532(3) . ?
C1 C14 1.533(4) . ?
C2 C3 1.383(4) . ?
C2 C7 1.384(4) . ?
C3 C4 1.375(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.358(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.376(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.391(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.383(4) . ?
C8 C9 1.386(4) . ?
C9 C10 1.361(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.358(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.375(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.390(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.373(5) . ?
C14 C19 1.379(4) . ?
C15 C16 1.393(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.367(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.341(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.396(5) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.344(4) . ?
C20 C25 1.358(4) . ?
C21 C22 1.385(3) . ?
C21 H21A 0.9300 . ?
C22 C23 1.350(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.373(4) . ?
C23 C23 1.487(4) 2_568 ?
C24 C25 1.384(4) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.490(6) 2_567 ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C26 1.490(6) 2_567 ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?

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
O3 S1 O1 111.0(2) . . ?
O3 S1 O2 113.45(19) . . ?
O1 S1 O2 112.46(17) . . ?
O3 S1 C20 107.07(13) . . ?
O1 S1 C20 106.55(13) . . ?
O2 S1 C20 105.80(12) . . ?
C26 O4 C27 109.4(3) . . ?
C1 N1 H1N1 111(2) . . ?
C1 N1 H1N2 111(2) . . ?
H1N1 N1 H1N2 107.4(14) . . ?
C1 N1 H1N3 113(2) . . ?
H1N1 N1 H1N3 107.0(14) . . ?
H1N2 N1 H1N3 107.8(14) . . ?
C8 C1 N1 108.0(2) . . ?
C8 C1 C2 110.5(2) . . ?
N1 C1 C2 107.11(18) . . ?
C8 C1 C14 111.8(2) . . ?
N1 C1 C14 107.5(2) . . ?
C2 C1 C14 111.6(2) . . ?
C3 C2 C7 118.5(3) . . ?
C3 C2 C1 121.6(2) . . ?
C7 C2 C1 119.8(2) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C5 C4 C3 120.6(4) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C4 C5 C6 120.2(3) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
C5 C6 C7 119.4(3) . . ?
C5 C6 H6A 120.3 . . ?
C7 C6 H6A 120.3 . . ?
C2 C7 C6 120.6(3) . . ?
C2 C7 H7A 119.7 . . ?
C6 C7 H7A 119.7 . . ?
C13 C8 C9 118.2(3) . . ?
C13 C8 C1 120.5(2) . . ?
C9 C8 C1 121.2(3) . . ?
C10 C9 C8 120.6(4) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C11 C10 C9 121.2(4) . . ?
C11 C10 H10A 119.4 . . ?
C9 C10 H10A 119.4 . . ?
C10 C11 C12 119.8(4) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C11 C12 C13 119.4(4) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C8 C13 C12 120.7(3) . . ?
C8 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
C15 C14 C19 117.7(3) . . ?
C15 C14 C1 120.1(3) . . ?
C19 C14 C1 122.2(3) . . ?
C14 C15 C16 121.0(4) . . ?
C14 C15 H15A 119.5 . . ?
C16 C15 H15A 119.5 . . ?
C17 C16 C15 120.2(4) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C18 C17 C16 119.4(4) . . ?
C18 C17 H17A 120.3 . . ?
C16 C17 H17A 120.3 . . ?
C17 C18 C19 121.0(4) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C14 C19 C18 120.5(4) . . ?
C14 C19 H19A 119.7 . . ?
C18 C19 H19A 119.7 . . ?
C21 C20 C25 118.6(2) . . ?
C21 C20 S1 120.86(19) . . ?
C25 C20 S1 120.5(2) . . ?
C20 C21 C22 120.4(2) . . ?
C20 C21 H21A 119.8 . . ?
C22 C21 H21A 119.8 . . ?
C23 C22 C21 122.8(3) . . ?
C23 C22 H22A 118.6 . . ?
C21 C22 H22A 118.6 . . ?
C22 C23 C24 115.9(2) . . ?
C22 C23 C23 121.9(3) . 2_568 ?
C24 C23 C23 122.2(3) . 2_568 ?
C23 C24 C25 121.9(3) . . ?
C23 C24 H24A 119.0 . . ?
C25 C24 H24A 119.0 . . ?
C20 C25 C24 120.4(3) . . ?
C20 C25 H25A 119.8 . . ?
C24 C25 H25A 119.8 . . ?
O4 C26 C27 110.5(4) . 2_567 ?
O4 C26 H26A 109.5 . . ?
C27 C26 H26A 109.5 2_567 . ?
O4 C26 H26B 109.5 . . ?
C27 C26 H26B 109.5 2_567 . ?
H26A C26 H26B 108.1 . . ?
O4 C27 C26 111.8(4) . 2_567 ?
O4 C27 H27A 109.3 . . ?
C26 C27 H27A 109.3 2_567 . ?
O4 C27 H27B 109.3 . . ?
C26 C27 H27B 109.3 2_567 . ?
H27A C27 H27B 107.9 . . ?

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
C8 C1 C2 C3 -112.6(3) . . . . ?
N1 C1 C2 C3 130.0(3) . . . . ?
C14 C1 C2 C3 12.5(4) . . . . ?
C8 C1 C2 C7 64.0(3) . . . . ?
N1 C1 C2 C7 -53.4(3) . . . . ?
C14 C1 C2 C7 -170.8(2) . . . . ?
C7 C2 C3 C4 -0.4(5) . . . . ?
C1 C2 C3 C4 176.3(3) . . . . ?
C2 C3 C4 C5 -0.9(6) . . . . ?
C3 C4 C5 C6 1.6(6) . . . . ?
C4 C5 C6 C7 -1.1(5) . . . . ?
C3 C2 C7 C6 1.0(4) . . . . ?
C1 C2 C7 C6 -175.8(2) . . . . ?
C5 C6 C7 C2 -0.2(4) . . . . ?
N1 C1 C8 C13 147.5(2) . . . . ?
C2 C1 C8 C13 30.6(3) . . . . ?
C14 C1 C8 C13 -94.4(3) . . . . ?
N1 C1 C8 C9 -35.3(3) . . . . ?
C2 C1 C8 C9 -152.2(2) . . . . ?
C14 C1 C8 C9 82.8(3) . . . . ?
C13 C8 C9 C10 -0.7(4) . . . . ?
C1 C8 C9 C10 -178.0(3) . . . . ?
C8 C9 C10 C11 1.3(5) . . . . ?
C9 C10 C11 C12 -0.5(6) . . . . ?
C10 C11 C12 C13 -0.9(5) . . . . ?
C9 C8 C13 C12 -0.7(4) . . . . ?
C1 C8 C13 C12 176.6(3) . . . . ?
C11 C12 C13 C8 1.5(5) . . . . ?
C8 C1 C14 C15 -165.7(3) . . . . ?
N1 C1 C14 C15 -47.3(3) . . . . ?
C2 C1 C14 C15 69.9(3) . . . . ?
C8 C1 C14 C19 16.3(3) . . . . ?
N1 C1 C14 C19 134.7(3) . . . . ?
C2 C1 C14 C19 -108.1(3) . . . . ?
C19 C14 C15 C16 0.3(5) . . . . ?
C1 C14 C15 C16 -177.7(3) . . . . ?
C14 C15 C16 C17 -0.2(6) . . . . ?
C15 C16 C17 C18 0.5(6) . . . . ?
C16 C17 C18 C19 -0.9(6) . . . . ?
C15 C14 C19 C18 -0.8(5) . . . . ?
C1 C14 C19 C18 177.3(3) . . . . ?
C17 C18 C19 C14 1.1(5) . . . . ?
O3 S1 C20 C21 -103.6(3) . . . . ?
O1 S1 C20 C21 137.5(3) . . . . ?
O2 S1 C20 C21 17.7(3) . . . . ?
O3 S1 C20 C25 76.7(4) . . . . ?
O1 S1 C20 C25 -42.1(4) . . . . ?
O2 S1 C20 C25 -162.0(3) . . . . ?
C25 C20 C21 C22 -0.3(6) . . . . ?
S1 C20 C21 C22 -180.0(3) . . . . ?
C20 C21 C22 C23 1.6(6) . . . . ?
C21 C22 C23 C24 -1.3(6) . . . . ?
C21 C22 C23 C23 179.1(4) . . . 2_568 ?
C22 C23 C24 C25 -0.2(7) . . . . ?
C23 C23 C24 C25 179.4(4) 2_568 . . . ?
C21 C20 C25 C24 -1.2(7) . . . . ?
S1 C20 C25 C24 178.5(4) . . . . ?
C23 C24 C25 C20 1.5(8) . . . . ?
C27 O4 C26 C27 56.5(5) . . . 2_567 ?
C26 O4 C27 C26 -57.2(5) . . . 2_567 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N1 O2 0.86(3) 1.923(11) 2.783(3) 172(3) .
N1 H1N2 O4 0.86(3) 2.044(12) 2.891(4) 168(2) .
N1 H1N3 O3 0.86(3) 2.320(15) 3.112(4) 153(2) 2_577
N1 H1N3 O1 0.86(3) 2.435(16) 3.190(4) 147(2) 2_577

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.052
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1044778'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C12 H8 O6 S2, 2(C19 H18 N), 2(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C52 H56 N2 O10 S2'
_chemical_formula_weight         933.11

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.8382(11)
_cell_length_b                   13.0040(10)
_cell_length_c                   17.5401(16)
_cell_angle_alpha                96.672(7)
_cell_angle_beta                 91.670(8)
_cell_angle_gamma                94.678(8)
_cell_volume                     2445.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3127
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             988
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9623
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14570
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.56
_reflns_number_total             11130
_reflns_number_gt                6724
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0640P)²+0.2309P] where P=(Fo²+2Fc²)/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         11130
_refine_ls_number_parameters     633
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1617
_refine_ls_wR_factor_gt          0.1348
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.3667(5) 0.5681(5) 0.1225(4) 0.0417(18) Uani 1 1 d . . .
S2 S -0.3969(6) 0.9062(6) 0.3777(4) 0.053(2) Uani 1 1 d . . .
O1 O 0.3468(16) 0.5826(15) 0.0418(10) 0.053(5) Uani 1 1 d . . .
O1W O 0.3027(15) 0.4311(15) -0.0851(10) 0.049(5) Uani 1 1 d D . .
H1W1 H 0.370(16) 0.42(2) -0.107(15) 0.073 Uiso 1 1 d D . .
H2W1 H 0.32(2) 0.482(17) -0.050(13) 0.073 Uiso 1 1 d D . .
O2 O 0.4790(15) 0.6249(16) 0.1568(12) 0.062(6) Uani 1 1 d . . .
O2W O -0.2841(16) 1.0766(16) 0.5778(12) 0.058(5) Uani 1 1 d D . .
H2W2 H -0.34(2) 1.10(2) 0.604(16) 0.086 Uiso 1 1 d D . .
H1W2 H -0.31(2) 1.020(16) 0.550(17) 0.086 Uiso 1 1 d D . .
O3 O 0.3577(17) 0.4587(14) 0.1334(11) 0.058(5) Uani 1 1 d . . .
O4 O -0.3816(18) 1.0062(15) 0.3498(12) 0.065(6) Uani 1 1 d . . .
O5 O -0.379(2) 0.9161(16) 0.4609(12) 0.070(6) Uani 1 1 d . . .
O6 O -0.5118(17) 0.8476(18) 0.3495(15) 0.088(8) Uani 1 1 d . . .
O7 O 0.554(2) 0.248(2) 0.0270(19) 0.098(9) Uani 1 1 d D . .
H7O H 0.59(4) 0.29(3) 0.00(2) 0.148 Uiso 1 1 d D . .
O8 O -0.573(2) 1.238(2) 0.4475(18) 0.092(8) Uani 1 1 d D . .
H8O H -0.60(4) 1.20(3) 0.48(2) 0.137 Uiso 1 1 d D . .
N1 N 0.3088(18) 0.2895(16) 0.0226(13) 0.042(5) Uani 1 1 d D . .
H1N1 H 0.383(13) 0.269(18) 0.020(12) 0.063 Uiso 1 1 d D . .
H1N3 H 0.30(2) 0.322(17) -0.018(8) 0.063 Uiso 1 1 d D . .
H1N2 H 0.31(2) 0.338(15) 0.062(9) 0.063 Uiso 1 1 d D . .
N2 N -0.3278(19) 1.1862(17) 0.4493(13) 0.044(5) Uani 1 1 d D . .
H2N1 H -0.400(14) 1.210(18) 0.452(12) 0.066 Uiso 1 1 d D . .
H2N2 H -0.33(2) 1.136(15) 0.413(9) 0.066 Uiso 1 1 d D . .
H2N3 H -0.31(2) 1.160(18) 0.492(8) 0.066 Uiso 1 1 d D . .
C1 C 0.212(2) 0.2006(18) 0.0296(14) 0.039(6) Uani 1 1 d . . .
C2 C 0.260(2) 0.138(2) 0.0918(15) 0.044(6) Uani 1 1 d . . .
C3 C 0.318(2) 0.189(3) 0.1594(18) 0.060(8) Uani 1 1 d . . .
H3A H 0.3289 0.2608 0.1668 0.072 Uiso 1 1 calc R . .
C4 C 0.359(3) 0.132(3) 0.216(2) 0.075(10) Uani 1 1 d . . .
H4A H 0.3979 0.1663 0.2608 0.090 Uiso 1 1 calc R . .
C5 C 0.344(3) 0.026(4) 0.207(2) 0.084(12) Uani 1 1 d . . .
H5A H 0.3732 -0.0116 0.2443 0.101 Uiso 1 1 calc R . .
C6 C 0.286(4) -0.024(3) 0.140(2) 0.089(12) Uani 1 1 d . . .
H6A H 0.2740 -0.0965 0.1339 0.107 Uiso 1 1 calc R . .
C7 C 0.244(3) 0.031(2) 0.0836(18) 0.062(8) Uani 1 1 d . . .
H7A H 0.2053 -0.0039 0.0391 0.075 Uiso 1 1 calc R . .
C8 C 0.195(2) 0.1346(19) -0.0492(15) 0.044(6) Uani 1 1 d . . .
C9 C 0.299(3) 0.103(2) -0.0870(17) 0.056(7) Uani 1 1 d . . .
H9A H 0.3777 0.1232 -0.0650 0.068 Uiso 1 1 calc R . .
C10 C 0.288(3) 0.041(2) -0.1567(18) 0.066(9) Uani 1 1 d . . .
H10A H 0.3583 0.0191 -0.1805 0.079 Uiso 1 1 calc R . .
C11 C 0.173(3) 0.010(2) -0.1913(19) 0.069(9) Uani 1 1 d . . .
H11A H 0.1651 -0.0307 -0.2386 0.082 Uiso 1 1 calc R . .
C12 C 0.069(3) 0.042(2) -0.155(2) 0.073(9) Uani 1 1 d . . .
H12A H -0.0087 0.0218 -0.1781 0.087 Uiso 1 1 calc R . .
C13 C 0.080(3) 0.103(2) -0.0846(18) 0.059(8) Uani 1 1 d . . .
H13A H 0.0092 0.1227 -0.0606 0.071 Uiso 1 1 calc R . .
C14 C 0.092(2) 0.2506(19) 0.0537(14) 0.039(6) Uani 1 1 d . . .
C15 C 0.046(2) 0.324(2) 0.0116(15) 0.046(6) Uani 1 1 d . . .
H15A H 0.0866 0.3426 -0.0313 0.055 Uiso 1 1 calc R . .
C16 C -0.061(2) 0.370(2) 0.0326(17) 0.051(7) Uani 1 1 d . . .
H16A H -0.0906 0.4189 0.0039 0.061 Uiso 1 1 calc R . .
C17 C -0.122(2) 0.344(2) 0.0953(18) 0.057(8) Uani 1 1 d . . .
H17A H -0.1934 0.3750 0.1098 0.068 Uiso 1 1 calc R . .
C18 C -0.078(3) 0.270(3) 0.1365(19) 0.069(9) Uani 1 1 d . . .
H18A H -0.1205 0.2515 0.1788 0.083 Uiso 1 1 calc R . .
C19 C 0.028(2) 0.224(2) 0.1159(17) 0.059(8) Uani 1 1 d . . .
H19A H 0.0568 0.1745 0.1445 0.071 Uiso 1 1 calc R . .
C20 C -0.230(2) 1.2726(19) 0.4372(14) 0.040(6) Uani 1 1 d . . .
C21 C -0.206(2) 1.3402(19) 0.5145(15) 0.045(6) Uani 1 1 d . . .
C22 C -0.303(3) 1.365(2) 0.5612(17) 0.060(8) Uani 1 1 d . . .
H22A H -0.3823 1.3345 0.5472 0.072 Uiso 1 1 calc R . .
C23 C -0.284(4) 1.432(3) 0.6279(19) 0.071(9) Uani 1 1 d . . .
H23A H -0.3506 1.4474 0.6584 0.085 Uiso 1 1 calc R . .
C24 C -0.168(4) 1.477(2) 0.649(2) 0.077(10) Uani 1 1 d . . .
H24A H -0.1552 1.5246 0.6932 0.092 Uiso 1 1 calc R . .
C25 C -0.069(4) 1.452(3) 0.605(2) 0.079(10) Uani 1 1 d . . .
H25A H 0.0104 1.4809 0.6200 0.095 Uiso 1 1 calc R . .
C26 C -0.088(3) 1.384(2) 0.5381(18) 0.060(8) Uani 1 1 d . . .
H26A H -0.0212 1.3670 0.5087 0.072 Uiso 1 1 calc R . .
C27 C -0.114(2) 1.222(2) 0.4091(14) 0.043(6) Uani 1 1 d . . .
C28 C -0.075(3) 1.136(2) 0.4396(17) 0.060(8) Uani 1 1 d . . .
H28A H -0.1209 1.1081 0.4774 0.072 Uiso 1 1 calc R . .
C29 C 0.031(3) 1.092(3) 0.4153(19) 0.066(9) Uani 1 1 d . . .
H29A H 0.0549 1.0341 0.4366 0.079 Uiso 1 1 calc R . .
C30 C 0.099(3) 1.132(3) 0.3603(19) 0.065(9) Uani 1 1 d . . .
H30A H 0.1702 1.1023 0.3437 0.079 Uiso 1 1 calc R . .
C31 C 0.062(3) 1.217(3) 0.3296(19) 0.071(9) Uani 1 1 d . . .
H31A H 0.1091 1.2457 0.2924 0.085 Uiso 1 1 calc R . .
C32 C -0.044(3) 1.261(2) 0.3533(17) 0.057(7) Uani 1 1 d . . .
H32A H -0.0682 1.3187 0.3312 0.068 Uiso 1 1 calc R . .
C33 C -0.285(2) 1.335(2) 0.3770(15) 0.047(7) Uani 1 1 d . . .
C34 C -0.335(3) 1.283(3) 0.3079(18) 0.066(9) Uani 1 1 d . . .
H34A H -0.3363 1.2112 0.2984 0.079 Uiso 1 1 calc R . .
C35 C -0.383(3) 1.340(4) 0.253(2) 0.088(12) Uani 1 1 d . . .
H35A H -0.4175 1.3049 0.2067 0.106 Uiso 1 1 calc R . .
C36 C -0.381(4) 1.445(4) 0.266(3) 0.099(15) Uani 1 1 d . . .
H36A H -0.4131 1.4825 0.2288 0.119 Uiso 1 1 calc R . .
C37 C -0.332(4) 1.496(3) 0.333(3) 0.096(13) Uani 1 1 d . . .
H37A H -0.3304 1.5677 0.3415 0.115 Uiso 1 1 calc R . .
C38 C -0.283(3) 1.442(3) 0.3889(19) 0.069(9) Uani 1 1 d . . .
H38A H -0.2496 1.4778 0.4347 0.082 Uiso 1 1 calc R . .
C39 C 0.154(2) 0.7547(19) 0.2509(15) 0.045(6) Uani 1 1 d . . .
H39A H 0.1646 0.8178 0.2822 0.054 Uiso 1 1 calc R . .
C40 C 0.256(2) 0.7143(19) 0.2168(15) 0.042(6) Uani 1 1 d . . .
H40A H 0.3343 0.7498 0.2254 0.051 Uiso 1 1 calc R . .
C41 C 0.241(2) 0.6209(18) 0.1700(13) 0.036(5) Uani 1 1 d . . .
C42 C 0.124(2) 0.567(2) 0.1586(14) 0.044(6) Uani 1 1 d . . .
H42A H 0.1149 0.5031 0.1279 0.053 Uiso 1 1 calc R . .
C43 C 0.023(2) 0.607(2) 0.1927(14) 0.045(6) Uani 1 1 d . . .
H43A H -0.0542 0.5705 0.1847 0.054 Uiso 1 1 calc R . .
C44 C 0.036(2) 0.7024(19) 0.2390(14) 0.039(6) Uani 1 1 d . . .
C45 C -0.073(2) 0.7456(19) 0.2757(14) 0.039(6) Uani 1 1 d . . .
C46 C -0.190(2) 0.7271(19) 0.2410(14) 0.040(6) Uani 1 1 d . . .
H46A H -0.2016 0.6835 0.1950 0.049 Uiso 1 1 calc R . .
C47 C -0.291(2) 0.7716(19) 0.2729(14) 0.041(6) Uani 1 1 d . . .
H47A H -0.3691 0.7581 0.2485 0.049 Uiso 1 1 calc R . .
C48 C -0.275(2) 0.8358(19) 0.3407(14) 0.042(6) Uani 1 1 d . . .
C49 C -0.160(3) 0.851(3) 0.3787(17) 0.066(9) Uani 1 1 d . . .
H49A H -0.1505 0.8910 0.4261 0.079 Uiso 1 1 calc R . .
C50 C -0.060(3) 0.806(2) 0.3468(17) 0.063(9) Uani 1 1 d . . .
H50A H 0.0163 0.8165 0.3729 0.076 Uiso 1 1 calc R . .
C51 C 0.610(4) 0.163(3) 0.042(3) 0.112(16) Uani 1 1 d D . .
H51A H 0.6399 0.1717 0.0943 0.168 Uiso 1 1 calc R . .
H51B H 0.6787 0.1548 0.0086 0.168 Uiso 1 1 calc R . .
H51C H 0.5520 0.1033 0.0323 0.168 Uiso 1 1 calc R . .
C52 C -0.630(4) 1.328(3) 0.448(3) 0.13(2) Uani 1 1 d D . .
H52A H -0.5761 1.3851 0.4716 0.197 Uiso 1 1 calc R . .
H52B H -0.7048 1.3221 0.4760 0.197 Uiso 1 1 calc R . .
H52C H -0.6511 1.3387 0.3959 0.197 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.447(18) . ?
S1 O3 1.454(19) . ?
S1 O1 1.462(18) . ?
S1 C41 1.76(2) . ?
S2 O4 1.44(2) . ?
S2 O6 1.45(2) . ?
S2 O5 1.46(2) . ?
S2 C48 1.76(2) . ?
O1W H1W1 0.85(2) . ?
O1W H2W1 0.85(2) . ?
O2W H2W2 0.85(2) . ?
O2W H1W2 0.85(2) . ?
O7 C51 1.35(4) . ?
O7 H7O 0.85(3) . ?
O8 C52 1.37(4) . ?
O8 H8O 0.85(3) . ?
N1 C1 1.52(3) . ?
N1 H1N1 0.86(3) . ?
N1 H1N3 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N2 C20 1.52(3) . ?
N2 H2N1 0.86(3) . ?
N2 H2N2 0.86(3) . ?
N2 H2N3 0.86(3) . ?
C1 C8 1.54(4) . ?
C1 C2 1.54(3) . ?
C1 C14 1.54(3) . ?
C2 C7 1.38(4) . ?
C2 C3 1.39(4) . ?
C3 C4 1.39(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.36(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.37(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.38(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.39(4) . ?
C8 C9 1.39(3) . ?
C9 C10 1.38(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.38(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.37(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.39(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C19 1.37(4) . ?
C14 C15 1.39(3) . ?
C15 C16 1.38(3) . ?
C15 H15A 0.9300 . ?
C16 C17 1.37(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.37(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.38(4) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.53(4) . ?
C20 C27 1.53(3) . ?
C20 C33 1.54(3) . ?
C21 C26 1.38(4) . ?
C21 C22 1.39(4) . ?
C22 C23 1.38(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.37(5) . ?
C23 H23A 0.9300 . ?
C24 C25 1.38(5) . ?
C24 H24A 0.9300 . ?
C25 C26 1.39(4) . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9300 . ?
C27 C32 1.38(4) . ?
C27 C28 1.38(4) . ?
C28 C29 1.38(4) . ?
C28 H28A 0.9300 . ?
C29 C30 1.36(4) . ?
C29 H29A 0.9300 . ?
C30 C31 1.37(4) . ?
C30 H30A 0.9300 . ?
C31 C32 1.38(4) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
C33 C38 1.38(4) . ?
C33 C34 1.39(4) . ?
C34 C35 1.39(4) . ?
C34 H34A 0.9300 . ?
C35 C36 1.37(6) . ?
C35 H35A 0.9300 . ?
C36 C37 1.35(6) . ?
C36 H36A 0.9300 . ?
C37 C38 1.39(5) . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9300 . ?
C39 C40 1.38(3) . ?
C39 C44 1.40(3) . ?
C39 H39A 0.9300 . ?
C40 C41 1.38(3) . ?
C40 H40A 0.9300 . ?
C41 C42 1.39(3) . ?
C42 C43 1.38(3) . ?
C42 H42A 0.9300 . ?
C43 C44 1.40(3) . ?
C43 H43A 0.9300 . ?
C44 C45 1.48(3) . ?
C45 C46 1.39(3) . ?
C45 C50 1.39(3) . ?
C46 C47 1.38(3) . ?
C46 H46A 0.9300 . ?
C47 C48 1.37(3) . ?
C47 H47A 0.9300 . ?
C48 C49 1.38(4) . ?
C49 C50 1.37(3) . ?
C49 H49A 0.9300 . ?
C50 H50A 0.9300 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?

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 S1 O3 113.2(12) . . ?
O2 S1 O1 112.8(12) . . ?
O3 S1 O1 111.6(11) . . ?
O2 S1 C41 107.3(11) . . ?
O3 S1 C41 106.0(11) . . ?
O1 S1 C41 105.3(10) . . ?
O4 S2 O6 112.4(15) . . ?
O4 S2 O5 111.1(12) . . ?
O6 S2 O5 113.7(15) . . ?
O4 S2 C48 106.3(12) . . ?
O6 S2 C48 107.1(11) . . ?
O5 S2 C48 105.7(12) . . ?
H1W1 O1W H2W1 106.00 . . ?
H2W2 O2W H1W2 111.00 . . ?
C51 O7 H7O 119.00 . . ?
C52 O8 H8O 113.00 . . ?
C1 N1 H1N1 112(10) . . ?
C1 N1 H1N3 115(10) . . ?
H1N1 N1 H1N3 105.00 . . ?
C1 N1 H1N2 112(10) . . ?
H1N1 N1 H1N2 107.00 . . ?
H1N3 N1 H1N2 105(10) . . ?
C20 N2 H2N1 110(10) . . ?
C20 N2 H2N2 113(10) . . ?
H2N1 N2 H2N2 107(10) . . ?
C20 N2 H2N3 111(10) . . ?
H2N1 N2 H2N3 107(10) . . ?
H2N2 N2 H2N3 107.00 . . ?
N1 C1 C8 107.6(19) . . ?
N1 C1 C2 107.0(19) . . ?
C8 C1 C2 112(2) . . ?
N1 C1 C14 106.3(18) . . ?
C8 C1 C14 112.3(19) . . ?
C2 C1 C14 111.5(19) . . ?
C7 C2 C3 118(3) . . ?
C7 C2 C1 121(3) . . ?
C3 C2 C1 121(2) . . ?
C2 C3 C4 120(3) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
C5 C4 C3 121(4) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C4 C5 C6 119(3) . . ?
C4 C5 H5A 120.5 . . ?
C6 C5 H5A 120.5 . . ?
C5 C6 C7 121(4) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
C2 C7 C6 121(3) . . ?
C2 C7 H7A 119.5 . . ?
C6 C7 H7A 119.5 . . ?
C13 C8 C9 117(3) . . ?
C13 C8 C1 123(2) . . ?
C9 C8 C1 120(2) . . ?
C10 C9 C8 121(3) . . ?
C10 C9 H9A 119.4 . . ?
C8 C9 H9A 119.4 . . ?
C9 C10 C11 121(3) . . ?
C9 C10 H10A 119.7 . . ?
C11 C10 H10A 119.7 . . ?
C12 C11 C10 119(3) . . ?
C12 C11 H11A 120.5 . . ?
C10 C11 H11A 120.5 . . ?
C11 C12 C13 121(3) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C8 C13 C12 121(3) . . ?
C8 C13 H13A 119.4 . . ?
C12 C13 H13A 119.4 . . ?
C19 C14 C15 118(2) . . ?
C19 C14 C1 122(2) . . ?
C15 C14 C1 120(2) . . ?
C16 C15 C14 121(2) . . ?
C16 C15 H15A 119.6 . . ?
C14 C15 H15A 119.6 . . ?
C17 C16 C15 120(3) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C16 C17 C18 119(2) . . ?
C16 C17 H17A 120.4 . . ?
C18 C17 H17A 120.4 . . ?
C17 C18 C19 121(3) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C14 C19 C18 121(3) . . ?
C14 C19 H19A 119.6 . . ?
C18 C19 H19A 119.6 . . ?
N2 C20 C21 107(2) . . ?
N2 C20 C27 107.8(19) . . ?
C21 C20 C27 112(2) . . ?
N2 C20 C33 106.9(19) . . ?
C21 C20 C33 111(2) . . ?
C27 C20 C33 112(2) . . ?
C26 C21 C22 118(3) . . ?
C26 C21 C20 122(2) . . ?
C22 C21 C20 120(2) . . ?
C23 C22 C21 121(3) . . ?
C23 C22 H22A 119.3 . . ?
C21 C22 H22A 119.3 . . ?
C24 C23 C22 120(3) . . ?
C24 C23 H23A 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C23 C24 C25 120(3) . . ?
C23 C24 H24A 120.1 . . ?
C25 C24 H24A 120.1 . . ?
C24 C25 C26 120(3) . . ?
C24 C25 H25A 120.0 . . ?
C26 C25 H25A 120.0 . . ?
C21 C26 C25 121(3) . . ?
C21 C26 H26A 119.5 . . ?
C25 C26 H26A 119.5 . . ?
C32 C27 C28 117(2) . . ?
C32 C27 C20 121(2) . . ?
C28 C27 C20 121(2) . . ?
C29 C28 C27 121(3) . . ?
C29 C28 H28A 119.3 . . ?
C27 C28 H28A 119.3 . . ?
C30 C29 C28 120(3) . . ?
C30 C29 H29A 119.9 . . ?
C28 C29 H29A 119.9 . . ?
C29 C30 C31 119(3) . . ?
C29 C30 H30A 120.4 . . ?
C31 C30 H30A 120.4 . . ?
C30 C31 C32 121(3) . . ?
C30 C31 H31A 119.6 . . ?
C32 C31 H31A 119.6 . . ?
C27 C32 C31 121(3) . . ?
C27 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
C38 C33 C34 119(3) . . ?
C38 C33 C20 122(3) . . ?
C34 C33 C20 120(2) . . ?
C33 C34 C35 120(3) . . ?
C33 C34 H34A 120.1 . . ?
C35 C34 H34A 120.1 . . ?
C36 C35 C34 121(4) . . ?
C36 C35 H35A 119.7 . . ?
C34 C35 H35A 119.7 . . ?
C37 C36 C35 120(3) . . ?
C37 C36 H36A 120.1 . . ?
C35 C36 H36A 120.1 . . ?
C36 C37 C38 121(4) . . ?
C36 C37 H37A 119.5 . . ?
C38 C37 H37A 119.5 . . ?
C33 C38 C37 120(4) . . ?
C33 C38 H38A 119.9 . . ?
C37 C38 H38A 119.9 . . ?
C40 C39 C44 121(2) . . ?
C40 C39 H39A 119.4 . . ?
C44 C39 H39A 119.4 . . ?
C41 C40 C39 119(2) . . ?
C41 C40 H40A 120.3 . . ?
C39 C40 H40A 120.3 . . ?
C40 C41 C42 120(2) . . ?
C40 C41 S1 121.3(18) . . ?
C42 C41 S1 118.4(18) . . ?
C43 C42 C41 120(2) . . ?
C43 C42 H42A 119.9 . . ?
C41 C42 H42A 119.9 . . ?
C42 C43 C44 121(2) . . ?
C42 C43 H43A 119.7 . . ?
C44 C43 H43A 119.7 . . ?
C43 C44 C39 118(2) . . ?
C43 C44 C45 121(2) . . ?
C39 C44 C45 121(2) . . ?
C46 C45 C50 118(2) . . ?
C46 C45 C44 121(2) . . ?
C50 C45 C44 121(2) . . ?
C47 C46 C45 122(2) . . ?
C47 C46 H46A 119.1 . . ?
C45 C46 H46A 119.1 . . ?
C48 C47 C46 119(2) . . ?
C48 C47 H47A 120.3 . . ?
C46 C47 H47A 120.3 . . ?
C47 C48 C49 120(2) . . ?
C47 C48 S2 120.8(19) . . ?
C49 C48 S2 119.2(19) . . ?
C50 C49 C48 120(2) . . ?
C50 C49 H49A 119.8 . . ?
C48 C49 H49A 119.8 . . ?
C49 C50 C45 121(2) . . ?
C49 C50 H50A 119.6 . . ?
C45 C50 H50A 119.6 . . ?
O7 C51 H51A 109.5 . . ?
O7 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O7 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O8 C52 H52A 109.5 . . ?
O8 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O8 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C7 -140(2) . . . . ?
C8 C1 C2 C7 -23(3) . . . . ?
C14 C1 C2 C7 104(3) . . . . ?
N1 C1 C2 C3 42(3) . . . . ?
C8 C1 C2 C3 159(2) . . . . ?
C14 C1 C2 C3 -74(3) . . . . ?
C7 C2 C3 C4 1(4) . . . . ?
C1 C2 C3 C4 179(2) . . . . ?
C2 C3 C4 C5 0(5) . . . . ?
C3 C4 C5 C6 -1(5) . . . . ?
C4 C5 C6 C7 1(5) . . . . ?
C3 C2 C7 C6 -1(4) . . . . ?
C1 C2 C7 C6 -179(3) . . . . ?
C5 C6 C7 C2 0(5) . . . . ?
N1 C1 C8 C13 -132(2) . . . . ?
C2 C1 C8 C13 111(3) . . . . ?
C14 C1 C8 C13 -15(3) . . . . ?
N1 C1 C8 C9 50(3) . . . . ?
C2 C1 C8 C9 -68(3) . . . . ?
C14 C1 C8 C9 166(2) . . . . ?
C13 C8 C9 C10 -1(4) . . . . ?
C1 C8 C9 C10 178(3) . . . . ?
C8 C9 C10 C11 1(5) . . . . ?
C9 C10 C11 C12 -1(5) . . . . ?
C10 C11 C12 C13 0(5) . . . . ?
C9 C8 C13 C12 0(4) . . . . ?
C1 C8 C13 C12 -179(3) . . . . ?
C11 C12 C13 C8 1(5) . . . . ?
N1 C1 C14 C19 -128(3) . . . . ?
C8 C1 C14 C19 115(3) . . . . ?
C2 C1 C14 C19 -12(3) . . . . ?
N1 C1 C14 C15 53(3) . . . . ?
C8 C1 C14 C15 -65(3) . . . . ?
C2 C1 C14 C15 169(2) . . . . ?
C19 C14 C15 C16 1(4) . . . . ?
C1 C14 C15 C16 -180(2) . . . . ?
C14 C15 C16 C17 0(4) . . . . ?
C15 C16 C17 C18 -1(4) . . . . ?
C16 C17 C18 C19 1(5) . . . . ?
C15 C14 C19 C18 -1(4) . . . . ?
C1 C14 C19 C18 180(3) . . . . ?
C17 C18 C19 C14 0(5) . . . . ?
N2 C20 C21 C26 143(2) . . . . ?
C27 C20 C21 C26 25(3) . . . . ?
C33 C20 C21 C26 -101(3) . . . . ?
N2 C20 C21 C22 -41(3) . . . . ?
C27 C20 C21 C22 -159(2) . . . . ?
C33 C20 C21 C22 75(3) . . . . ?
C26 C21 C22 C23 2(4) . . . . ?
C20 C21 C22 C23 -174(3) . . . . ?
C21 C22 C23 C24 0(5) . . . . ?
C22 C23 C24 C25 -2(5) . . . . ?
C23 C24 C25 C26 2(5) . . . . ?
C22 C21 C26 C25 -2(4) . . . . ?
C20 C21 C26 C25 174(3) . . . . ?
C24 C25 C26 C21 0(5) . . . . ?
N2 C20 C27 C32 141(2) . . . . ?
C21 C20 C27 C32 -102(3) . . . . ?
C33 C20 C27 C32 24(3) . . . . ?
N2 C20 C27 C28 -40(3) . . . . ?
C21 C20 C27 C28 78(3) . . . . ?
C33 C20 C27 C28 -157(2) . . . . ?
C32 C27 C28 C29 0(4) . . . . ?
C20 C27 C28 C29 -179(3) . . . . ?
C27 C28 C29 C30 0(5) . . . . ?
C28 C29 C30 C31 0(5) . . . . ?
C29 C30 C31 C32 -1(5) . . . . ?
C28 C27 C32 C31 -1(4) . . . . ?
C20 C27 C32 C31 178(3) . . . . ?
C30 C31 C32 C27 1(5) . . . . ?
N2 C20 C33 C38 130(3) . . . . ?
C21 C20 C33 C38 13(3) . . . . ?
C27 C20 C33 C38 -112(3) . . . . ?
N2 C20 C33 C34 -52(3) . . . . ?
C21 C20 C33 C34 -168(2) . . . . ?
C27 C20 C33 C34 66(3) . . . . ?
C38 C33 C34 C35 -1(4) . . . . ?
C20 C33 C34 C35 -179(3) . . . . ?
C33 C34 C35 C36 1(5) . . . . ?
C34 C35 C36 C37 0(6) . . . . ?
C35 C36 C37 C38 0(6) . . . . ?
C34 C33 C38 C37 1(5) . . . . ?
C20 C33 C38 C37 179(3) . . . . ?
C36 C37 C38 C33 0(6) . . . . ?
C44 C39 C40 C41 0(4) . . . . ?
C39 C40 C41 C42 -1(4) . . . . ?
C39 C40 C41 S1 177.7(19) . . . . ?
O2 S1 C41 C40 14(3) . . . . ?
O3 S1 C41 C40 135(2) . . . . ?
O1 S1 C41 C40 -107(2) . . . . ?
O2 S1 C41 C42 -167(2) . . . . ?
O3 S1 C41 C42 -46(2) . . . . ?
O1 S1 C41 C42 72(2) . . . . ?
C40 C41 C42 C43 1(4) . . . . ?
S1 C41 C42 C43 -178(2) . . . . ?
C41 C42 C43 C44 0(4) . . . . ?
C42 C43 C44 C39 -1(4) . . . . ?
C42 C43 C44 C45 -180(2) . . . . ?
C40 C39 C44 C43 1(4) . . . . ?
C40 C39 C44 C45 180(2) . . . . ?
C43 C44 C45 C46 -32(4) . . . . ?
C39 C44 C45 C46 149(3) . . . . ?
C43 C44 C45 C50 148(3) . . . . ?
C39 C44 C45 C50 -31(4) . . . . ?
C50 C45 C46 C47 4(4) . . . . ?
C44 C45 C46 C47 -177(2) . . . . ?
C45 C46 C47 C48 0(4) . . . . ?
C46 C47 C48 C49 -4(4) . . . . ?
C46 C47 C48 S2 173(2) . . . . ?
O4 S2 C48 C47 -93(2) . . . . ?
O6 S2 C48 C47 27(3) . . . . ?
O5 S2 C48 C47 149(2) . . . . ?
O4 S2 C48 C49 83(3) . . . . ?
O6 S2 C48 C49 -156(3) . . . . ?
O5 S2 C48 C49 -35(3) . . . . ?
C47 C48 C49 C50 4(5) . . . . ?
S2 C48 C49 C50 -173(3) . . . . ?
C48 C49 C50 C45 0(5) . . . . ?
C46 C45 C50 C49 -4(5) . . . . ?
C44 C45 C50 C49 176(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O2 0.85(2) 1.97(10) 2.82(2) 173.00 2_665
O1W H2W1 O1 0.85(2) 1.95(11) 2.80(2) 170.00 .
O2W H2W2 O6 0.85(2) 1.93(11) 2.78(3) 172(33) 2_476
O2W H1W2 O5 0.85(2) 2.03(14) 2.86(3) 163.00 .
O7 H7O O1 0.85(3) 1.96(18) 2.78(3) 162(47) 2_665
O8 H8O O5 0.85(3) 1.90(15) 2.74(3) 161.00 2_476
N1 H1N1 O7 0.86(3) 1.90(11) 2.76(3) 169.00 .
N1 H1N3 O1W 0.86(3) 1.95(14) 2.79(3) 161(24) .
N1 H1N2 O3 0.86(3) 1.92(13) 2.77(3) 163(23) .
N2 H2N1 O8 0.86(3) 1.94(11) 2.79(3) 169.00 .
N2 H2N2 O4 0.86(3) 1.93(13) 2.76(3) 161.00 .
N2 H2N3 O2W 0.86(3) 1.99(11) 2.85(3) 169.00 .

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.045
####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 1044779'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), 2(C3 H8 O), H2 O'
_chemical_formula_sum            'C56 H62 N2 O9 S2'
_chemical_formula_weight         971.22

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           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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

_cell_length_a                   15.2948(7)
_cell_length_b                   18.2388(13)
_cell_length_c                   9.5627(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2667.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1096
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9665
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5017
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.1105
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3811
_reflns_number_gt                1967
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0272P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(13)
_refine_ls_number_reflns         3811
_refine_ls_number_parameters     330
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0884
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.036
_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
N1 N 0.0067(2) 0.8692(2) 0.6381(4) 0.0507(12) Uani 1 1 d D . .
C6 C 0.0596(4) 0.6880(4) 0.2826(7) 0.100(3) Uani 1 1 d . . .
H6A H 0.0563 0.6395 0.2531 0.119 Uiso 1 1 calc R . .
C15 C 0.0089(4) 0.6964(3) 0.8050(6) 0.0747(19) Uani 1 1 d . . .
H15A H 0.0658 0.6994 0.8390 0.090 Uiso 1 1 calc R . .
C19 C -0.1017(4) 0.7358(4) 0.6483(6) 0.087(2) Uani 1 1 d . . .
H19A H -0.1207 0.7670 0.5776 0.104 Uiso 1 1 calc R . .
C17 C -0.1291(8) 0.6409(5) 0.8143(10) 0.131(4) Uani 1 1 d . . .
H17A H -0.1661 0.6061 0.8537 0.157 Uiso 1 1 calc R . .
C18 C -0.1597(5) 0.6838(5) 0.7064(9) 0.112(3) Uani 1 1 d . . .
H18A H -0.2165 0.6787 0.6729 0.134 Uiso 1 1 calc R . .
C16 C -0.0490(6) 0.6478(5) 0.8633(8) 0.113(3) Uani 1 1 d . . .
H16A H -0.0315 0.6193 0.9388 0.135 Uiso 1 1 calc R . .
C2 C 0.0541(3) 0.7759(3) 0.4682(5) 0.0462(13) Uani 1 1 d . . .
C13 C 0.2033(3) 0.7529(3) 0.6467(5) 0.0732(19) Uani 1 1 d . . .
H13A H 0.1943 0.7236 0.5684 0.088 Uiso 1 1 calc R . .
C3 C 0.0718(3) 0.8303(3) 0.3719(6) 0.0659(17) Uani 1 1 d . . .
H3A H 0.0783 0.8786 0.4012 0.079 Uiso 1 1 calc R . .
C8 C 0.1375(3) 0.7964(3) 0.6947(5) 0.0479(13) Uani 1 1 d . . .
C10 C 0.2316(4) 0.8387(4) 0.8741(6) 0.095(2) Uani 1 1 d . . .
H10A H 0.2401 0.8682 0.9522 0.114 Uiso 1 1 calc R . .
C11 C 0.2999(4) 0.7960(4) 0.8263(7) 0.086(2) Uani 1 1 d . . .
H11A H 0.3546 0.7973 0.8690 0.103 Uiso 1 1 calc R . .
C14 C -0.0170(4) 0.7406(3) 0.6962(6) 0.0574(15) Uani 1 1 d . . .
C7 C 0.0483(4) 0.7053(4) 0.4220(6) 0.0798(18) Uani 1 1 d . . .
H7A H 0.0366 0.6680 0.4857 0.096 Uiso 1 1 calc R . .
C4 C 0.0800(4) 0.8129(4) 0.2315(6) 0.087(2) Uani 1 1 d . . .
H4A H 0.0887 0.8499 0.1661 0.105 Uiso 1 1 calc R . .
C12 C 0.2840(4) 0.7520(4) 0.7142(6) 0.082(2) Uani 1 1 d . . .
H12A H 0.3278 0.7208 0.6821 0.099 Uiso 1 1 calc R . .
C9 C 0.1528(4) 0.8387(3) 0.8107(6) 0.081(2) Uani 1 1 d . . .
H9A H 0.1082 0.8679 0.8462 0.097 Uiso 1 1 calc R . .
C1 C 0.0474(3) 0.7947(3) 0.6229(5) 0.0444(13) Uani 1 1 d . . .
C5 C 0.0753(4) 0.7420(5) 0.1895(7) 0.091(2) Uani 1 1 d . . .
H5A H 0.0831 0.7304 0.0955 0.109 Uiso 1 1 calc R . .
S1 S 0.34362(7) 0.52862(10) 0.54395(17) 0.0581(4) Uani 1 1 d . . .
O1 O 0.38185(16) 0.48535(19) 0.4313(4) 0.0598(10) Uani 1 1 d . . .
O2 O 0.35956(19) 0.6064(2) 0.5274(4) 0.0859(13) Uani 1 1 d . . .
O3 O 0.36556(18) 0.5023(2) 0.6823(4) 0.0912(14) Uani 1 1 d . . .
C25 C 0.1789(3) 0.5408(3) 0.6427(5) 0.0620(17) Uani 1 1 d . . .
H25A H 0.2052 0.5613 0.7212 0.074 Uiso 1 1 calc R . .
C20 C 0.2294(2) 0.5182(3) 0.5320(5) 0.0419(12) Uani 1 1 d . . .
C21 C 0.1916(3) 0.4877(4) 0.4182(5) 0.0733(19) Uani 1 1 d . . .
H21A H 0.2259 0.4712 0.3443 0.088 Uiso 1 1 calc R . .
C24 C 0.0895(3) 0.5330(3) 0.6374(6) 0.0653(17) Uani 1 1 d . . .
H24A H 0.0562 0.5480 0.7136 0.078 Uiso 1 1 calc R . .
C23 C 0.0477(2) 0.5035(3) 0.5225(5) 0.0494(15) Uani 1 1 d . . .
C22 C 0.0993(3) 0.4811(3) 0.4125(5) 0.0729(18) Uani 1 1 d . . .
H22A H 0.0732 0.4613 0.3332 0.087 Uiso 1 1 calc R . .
H1N1 H -0.013(3) 0.883(3) 0.719(2) 0.109 Uiso 1 1 d D . .
H1N2 H -0.0360(18) 0.877(3) 0.580(3) 0.109 Uiso 1 1 d D . .
H1N3 H 0.048(2) 0.900(2) 0.616(4) 0.109 Uiso 1 1 d D . .
O1W O 0.5000 0.5000 0.8741(5) 0.0703(17) Uani 1 2 d SD . .
H1W H 0.456(2) 0.495(4) 0.821(4) 0.105 Uiso 1 1 d D . .
O4 O 0.5458(3) 0.4022(3) 1.0833(4) 0.1020(16) Uani 1 1 d D . .
C26 C 0.6230(6) 0.3718(5) 1.0350(10) 0.173(4) Uani 0.50 1 d PD A 1
H26A H 0.6137 0.3502 0.9436 0.208 Uiso 0.50 1 calc PR A 1
H26B H 0.6422 0.3335 1.0983 0.208 Uiso 0.50 1 calc PR A 1
C27 C 0.6926(8) 0.4315(10) 1.026(2) 0.224(9) Uani 0.50 1 d PD A 1
H27A H 0.6860 0.4543 0.9346 0.269 Uiso 0.50 1 calc PR A 1
H27B H 0.6771 0.4684 1.0943 0.269 Uiso 0.50 1 calc PR A 1
C28 C 0.7826(8) 0.4174(11) 1.0431(13) 0.305(8) Uani 0.50 1 d PD A 1
H28A H 0.8145 0.4626 1.0379 0.458 Uiso 0.50 1 calc PR A 1
H28B H 0.8022 0.3849 0.9706 0.458 Uiso 0.50 1 calc PR A 1
H28C H 0.7922 0.3950 1.1326 0.458 Uiso 0.50 1 calc PR A 1
C26' C 0.6230(6) 0.3718(5) 1.0350(10) 0.173(4) Uani 0.50 1 d PD A 2
H26C H 0.6244 0.3723 0.9336 0.208 Uiso 0.50 1 calc PR A 2
H26D H 0.6286 0.3215 1.0669 0.208 Uiso 0.50 1 calc PR A 2
C27' C 0.6959(8) 0.4182(12) 1.0935(16) 0.224(9) Uani 0.50 1 d PD A 2
H27C H 0.6762 0.4687 1.0870 0.269 Uiso 0.50 1 calc PR A 2
H27D H 0.6993 0.4068 1.1924 0.269 Uiso 0.50 1 calc PR A 2
C28' C 0.7826(8) 0.4174(11) 1.0431(13) 0.305(8) Uani 0.50 1 d PD A 2
H28D H 0.8167 0.4530 1.0929 0.458 Uiso 0.50 1 calc PR A 2
H28E H 0.7828 0.4290 0.9452 0.458 Uiso 0.50 1 calc PR A 2
H28F H 0.8073 0.3695 1.0569 0.458 Uiso 0.50 1 calc PR A 2
H4O H 0.495(2) 0.408(6) 1.048(6) 0.458 Uiso 1 1 d 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
N1 C1 1.500(6) . ?
N1 H1N1 0.868(10) . ?
N1 H1N2 0.871(10) . ?
N1 H1N3 0.867(10) . ?
C6 C5 1.349(8) . ?
C6 C7 1.381(8) . ?
C6 H6A 0.9300 . ?
C15 C16 1.371(9) . ?
C15 C14 1.374(7) . ?
C15 H15A 0.9300 . ?
C19 C14 1.377(7) . ?
C19 C18 1.413(8) . ?
C19 H19A 0.9300 . ?
C17 C16 1.318(10) . ?
C17 C18 1.377(11) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C16 H16A 0.9300 . ?
C2 C7 1.365(7) . ?
C2 C3 1.380(7) . ?
C2 C1 1.522(6) . ?
C13 C8 1.362(6) . ?
C13 C12 1.394(7) . ?
C13 H13A 0.9300 . ?
C3 C4 1.384(7) . ?
C3 H3A 0.9300 . ?
C8 C9 1.372(7) . ?
C8 C1 1.540(6) . ?
C10 C9 1.349(7) . ?
C10 C11 1.381(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.361(8) . ?
C11 H11A 0.9300 . ?
C14 C1 1.561(7) . ?
C7 H7A 0.9300 . ?
C4 C5 1.357(8) . ?
C4 H4A 0.9300 . ?
C12 H12A 0.9300 . ?
C9 H9A 0.9300 . ?
C5 H5A 0.9300 . ?
S1 O2 1.447(4) . ?
S1 O3 1.447(4) . ?
S1 O1 1.458(3) . ?
S1 C20 1.761(4) . ?
C25 C24 1.376(6) . ?
C25 C20 1.373(6) . ?
C25 H25A 0.9300 . ?
C20 C21 1.352(6) . ?
C21 C22 1.418(6) . ?
C21 H21A 0.9300 . ?
C24 C23 1.381(6) . ?
C24 H24A 0.9300 . ?
C23 C22 1.378(6) . ?
C23 C23 1.464(8) 2_565 ?
C22 H22A 0.9300 . ?
O1W H1W 0.842(10) . ?
O4 C26 1.383(6) . ?
O4 H4O 0.854(11) . ?
C26 C27 1.525(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.410(10) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C27' H27C 0.9700 . ?
C27' H27D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 H1N1 119(4) . . ?
C1 N1 H1N2 114(3) . . ?
H1N1 N1 H1N2 105.2(16) . . ?
C1 N1 H1N3 105(3) . . ?
H1N1 N1 H1N3 106.2(16) . . ?
H1N2 N1 H1N3 105.8(16) . . ?
C5 C6 C7 119.6(7) . . ?
C5 C6 H6A 120.2 . . ?
C7 C6 H6A 120.2 . . ?
C16 C15 C14 120.0(7) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C14 C19 C18 120.2(7) . . ?
C14 C19 H19A 119.9 . . ?
C18 C19 H19A 119.9 . . ?
C16 C17 C18 121.9(10) . . ?
C16 C17 H17A 119.1 . . ?
C18 C17 H17A 119.1 . . ?
C17 C18 C19 117.6(8) . . ?
C17 C18 H18A 121.2 . . ?
C19 C18 H18A 121.2 . . ?
C17 C16 C15 121.2(10) . . ?
C17 C16 H16A 119.4 . . ?
C15 C16 H16A 119.4 . . ?
C7 C2 C3 118.3(5) . . ?
C7 C2 C1 121.5(5) . . ?
C3 C2 C1 120.0(5) . . ?
C8 C13 C12 120.4(5) . . ?
C8 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C4 C3 C2 120.1(6) . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C13 C8 C9 118.3(5) . . ?
C13 C8 C1 120.0(5) . . ?
C9 C8 C1 121.7(5) . . ?
C9 C10 C11 121.9(6) . . ?
C9 C10 H10A 119.1 . . ?
C11 C10 H10A 119.1 . . ?
C12 C11 C10 117.2(5) . . ?
C12 C11 H11A 121.4 . . ?
C10 C11 H11A 121.4 . . ?
C15 C14 C19 119.1(6) . . ?
C15 C14 C1 122.0(5) . . ?
C19 C14 C1 118.9(6) . . ?
C2 C7 C6 121.3(6) . . ?
C2 C7 H7A 119.4 . . ?
C6 C7 H7A 119.4 . . ?
C5 C4 C3 120.0(6) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C11 C12 C13 121.1(6) . . ?
C11 C12 H12A 119.4 . . ?
C13 C12 H12A 119.4 . . ?
C10 C9 C8 121.0(5) . . ?
C10 C9 H9A 119.5 . . ?
C8 C9 H9A 119.5 . . ?
N1 C1 C2 109.1(4) . . ?
N1 C1 C8 108.0(4) . . ?
C2 C1 C8 112.2(4) . . ?
N1 C1 C14 105.5(4) . . ?
C2 C1 C14 109.7(4) . . ?
C8 C1 C14 112.1(4) . . ?
C6 C5 C4 120.6(6) . . ?
C6 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
O2 S1 O3 112.7(3) . . ?
O2 S1 O1 112.4(2) . . ?
O3 S1 O1 113.8(2) . . ?
O2 S1 C20 105.4(2) . . ?
O3 S1 C20 104.7(2) . . ?
O1 S1 C20 106.9(2) . . ?
C24 C25 C20 120.0(4) . . ?
C24 C25 H25A 120.0 . . ?
C20 C25 H25A 120.0 . . ?
C21 C20 C25 120.2(4) . . ?
C21 C20 S1 121.4(4) . . ?
C25 C20 S1 118.4(4) . . ?
C20 C21 C22 119.5(5) . . ?
C20 C21 H21A 120.3 . . ?
C22 C21 H21A 120.3 . . ?
C25 C24 C23 122.0(5) . . ?
C25 C24 H24A 119.0 . . ?
C23 C24 H24A 119.0 . . ?
C24 C23 C22 117.2(4) . . ?
C24 C23 C23 119.7(3) . 2_565 ?
C22 C23 C23 123.0(4) . 2_565 ?
C23 C22 C21 121.1(5) . . ?
C23 C22 H22A 119.5 . . ?
C21 C22 H22A 119.5 . . ?
C26 O4 H4O 134(2) . . ?
O4 C26 C27 109.2(9) . . ?
O4 C26 H26A 109.8 . . ?
C27 C26 H26A 109.8 . . ?
O4 C26 H26B 109.8 . . ?
C27 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
C28 C27 C26 123.0(14) . . ?
C28 C27 H27A 106.6 . . ?
C26 C27 H27A 106.6 . . ?
C28 C27 H27B 106.6 . . ?
C26 C27 H27B 106.6 . . ?
H27A C27 H27B 106.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H27C C27' H27D 106.4 . . ?

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
C16 C17 C18 C19 0.4(13) . . . . ?
C14 C19 C18 C17 2.3(10) . . . . ?
C18 C17 C16 C15 -2.6(14) . . . . ?
C14 C15 C16 C17 2.1(11) . . . . ?
C7 C2 C3 C4 2.5(7) . . . . ?
C1 C2 C3 C4 178.5(5) . . . . ?
C12 C13 C8 C9 -0.3(9) . . . . ?
C12 C13 C8 C1 -177.6(5) . . . . ?
C9 C10 C11 C12 -1.8(10) . . . . ?
C16 C15 C14 C19 0.7(9) . . . . ?
C16 C15 C14 C1 -177.8(6) . . . . ?
C18 C19 C14 C15 -2.8(9) . . . . ?
C18 C19 C14 C1 175.7(5) . . . . ?
C3 C2 C7 C6 -0.2(8) . . . . ?
C1 C2 C7 C6 -176.1(5) . . . . ?
C5 C6 C7 C2 -1.0(10) . . . . ?
C2 C3 C4 C5 -3.6(9) . . . . ?
C10 C11 C12 C13 3.0(10) . . . . ?
C8 C13 C12 C11 -2.1(10) . . . . ?
C11 C10 C9 C8 -0.4(11) . . . . ?
C13 C8 C9 C10 1.5(9) . . . . ?
C1 C8 C9 C10 178.8(6) . . . . ?
C7 C2 C1 N1 -148.6(4) . . . . ?
C3 C2 C1 N1 35.5(6) . . . . ?
C7 C2 C1 C8 91.7(6) . . . . ?
C3 C2 C1 C8 -84.2(6) . . . . ?
C7 C2 C1 C14 -33.6(6) . . . . ?
C3 C2 C1 C14 150.6(5) . . . . ?
C13 C8 C1 N1 -149.8(5) . . . . ?
C9 C8 C1 N1 32.9(7) . . . . ?
C13 C8 C1 C2 -29.6(7) . . . . ?
C9 C8 C1 C2 153.2(5) . . . . ?
C13 C8 C1 C14 94.3(5) . . . . ?
C9 C8 C1 C14 -82.9(7) . . . . ?
C15 C14 C1 N1 -122.2(5) . . . . ?
C19 C14 C1 N1 59.3(6) . . . . ?
C15 C14 C1 C2 120.5(5) . . . . ?
C19 C14 C1 C2 -58.0(6) . . . . ?
C15 C14 C1 C8 -4.8(7) . . . . ?
C19 C14 C1 C8 176.7(5) . . . . ?
C7 C6 C5 C4 -0.2(11) . . . . ?
C3 C4 C5 C6 2.4(11) . . . . ?
C24 C25 C20 C21 -0.6(9) . . . . ?
C24 C25 C20 S1 -179.6(4) . . . . ?
O2 S1 C20 C21 107.6(5) . . . . ?
O3 S1 C20 C21 -133.3(5) . . . . ?
O1 S1 C20 C21 -12.3(5) . . . . ?
O2 S1 C20 C25 -73.5(5) . . . . ?
O3 S1 C20 C25 45.6(5) . . . . ?
O1 S1 C20 C25 166.7(4) . . . . ?
C25 C20 C21 C22 1.7(9) . . . . ?
S1 C20 C21 C22 -179.3(5) . . . . ?
C20 C25 C24 C23 -0.7(9) . . . . ?
C25 C24 C23 C22 0.8(9) . . . . ?
C25 C24 C23 C23 179.9(6) . . . 2_565 ?
C24 C23 C22 C21 0.4(9) . . . . ?
C23 C23 C22 C21 -178.7(6) 2_565 . . . ?
C20 C21 C22 C23 -1.7(10) . . . . ?
O4 C26 C27 C28 150.2(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N1 O4 0.868(10) 1.986(12) 2.847(5) 171(5) 4_557
N1 H1N2 O2 0.871(10) 1.921(13) 2.787(5) 172(4) 3_466
N1 H1N3 O1 0.867(10) 1.948(17) 2.800(5) 167(5) 4_556
O1W H1W O3 0.842(10) 1.926(17) 2.755(5) 168(6) .
O4 H4O O1W 0.854(11) 2.36(12) 2.771(6) 110(9) .

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.040
####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 1044780'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), 2(C4 H10 O), H2 O'
_chemical_formula_sum            'C58 H66 N2 O9 S2'
_chemical_formula_weight         999.25

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           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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

_cell_length_a                   18.878(3)
_cell_length_b                   15.3625(17)
_cell_length_c                   9.4488(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2740.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1043
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9670
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6756
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         27.56
_reflns_number_total             5342
_reflns_number_gt                3425
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0560P)²+0.5941P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(13)
_refine_ls_number_reflns         5342
_refine_ls_number_parameters     378
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.1562
_refine_ls_wR_factor_gt          0.1349
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.02395(7) 0.15703(6) 1.06083(11) 0.0602(3) Uani 1 1 d . A .
O1 O -0.01500(16) 0.11827(15) 0.9445(3) 0.0666(8) Uani 1 1 d . . .
O1W O 0.0000 0.0000 1.3865(4) 0.0697(12) Uani 1 2 d SD . .
H1W H 0.005(3) 0.044(2) 1.333(4) 0.104 Uiso 1 1 d D . .
O2 O -0.0061(2) 0.13771(19) 1.1979(3) 0.0904(11) Uani 1 1 d . . .
O3 O 0.09910(17) 0.13872(18) 1.0521(4) 0.0866(10) Uani 1 1 d . . .
O4 O 0.0957(2) 0.0534(2) 1.5945(3) 0.0916(11) Uani 1 1 d D . .
H4O H 0.067(3) 0.021(3) 1.550(6) 0.137 Uiso 1 1 d D . .
N1 N 0.12574(19) -0.0028(2) 0.8733(3) 0.0523(8) Uani 1 1 d D . .
H1N2 H 0.1156(19) 0.016(2) 0.7893(16) 0.078 Uiso 1 1 d D . .
H1N1 H 0.0901(14) -0.0350(19) 0.900(3) 0.078 Uiso 1 1 d D . .
H1N3 H 0.1242(19) 0.0424(14) 0.929(3) 0.078 Uiso 1 1 d D . .
C1 C 0.0161(2) 0.2715(2) 1.0421(4) 0.0453(9) Uani 1 1 d D . .
C4 C 0.0033(2) 0.4517(2) 1.0287(4) 0.0490(9) Uani 1 1 d . . .
C2 C 0.0385(10) 0.3251(11) 1.1521(12) 0.062(5) Uani 0.50 1 d P A 1
H2A H 0.0581 0.2994 1.2322 0.074 Uiso 0.50 1 calc PR A 1
C3 C 0.0329(12) 0.4120(10) 1.1479(14) 0.067(5) Uani 0.50 1 d P A 1
H3A H 0.0486 0.4456 1.2235 0.081 Uiso 0.50 1 calc PR A 1
C5 C -0.0183(13) 0.4010(12) 0.9274(17) 0.096(9) Uani 0.50 1 d P A 1
H5A H -0.0393 0.4261 0.8482 0.115 Uiso 0.50 1 calc PR A 1
C6 C -0.0113(8) 0.3102(12) 0.9324(14) 0.063(5) Uani 0.50 1 d P A 1
H6A H -0.0266 0.2770 0.8560 0.076 Uiso 0.50 1 calc PR A 1
C2' C 0.0625(14) 0.3186(15) 1.103(3) 0.154(13) Uani 0.50 1 d P A 2
H2'A H 0.1000 0.2941 1.1531 0.185 Uiso 0.50 1 calc PR A 2
C3' C 0.0541(15) 0.4133(15) 1.091(3) 0.176(14) Uani 0.50 1 d P A 2
H3'A H 0.0887 0.4480 1.1332 0.211 Uiso 0.50 1 calc PR A 2
C5' C -0.0407(13) 0.3990(16) 0.961(2) 0.113(9) Uani 0.50 1 d P A 2
H5'A H -0.0752 0.4246 0.9042 0.135 Uiso 0.50 1 calc PR A 2
C6' C -0.0396(8) 0.3080(12) 0.9671(19) 0.091(7) Uani 0.50 1 d PD A 2
H6'A H -0.0741 0.2741 0.9237 0.109 Uiso 0.50 1 calc PR A 2
C7 C 0.1280(4) 0.1268(4) 1.5368(7) 0.126(2) Uani 0.50 1 d PD B 3
H7A H 0.1416 0.1165 1.4392 0.151 Uiso 0.50 1 calc PR B 3
H7B H 0.1698 0.1428 1.5905 0.151 Uiso 0.50 1 calc PR B 3
C8 C 0.0725(7) 0.1966(7) 1.546(2) 0.154(5) Uani 0.50 1 d PD B 3
H8A H 0.0376 0.1862 1.4728 0.185 Uiso 0.50 1 calc PR B 3
H8B H 0.0486 0.1912 1.6366 0.185 Uiso 0.50 1 calc PR B 3
C9 C 0.0989(7) 0.2877(8) 1.532(2) 0.165(5) Uani 0.50 1 d PD B 3
H9A H 0.1339 0.3003 1.6040 0.198 Uiso 0.50 1 calc PR B 3
H9B H 0.1204 0.2963 1.4395 0.198 Uiso 0.50 1 calc PR B 3
C10 C 0.0359(5) 0.3456(6) 1.5485(12) 0.200(4) Uani 0.50 1 d PD B 3
H10A H 0.0504 0.4052 1.5405 0.300 Uiso 0.50 1 calc PR B 3
H10B H 0.0150 0.3360 1.6398 0.300 Uiso 0.50 1 calc PR B 3
H10C H 0.0019 0.3325 1.4761 0.300 Uiso 0.50 1 calc PR B 3
C7' C 0.1280(4) 0.1268(4) 1.5368(7) 0.126(2) Uani 0.50 1 d P B 4
H7'A H 0.1167 0.1255 1.4367 0.151 Uiso 0.50 1 calc PR B 4
H7'B H 0.1785 0.1162 1.5435 0.151 Uiso 0.50 1 calc PR B 4
C8' C 0.1179(8) 0.2164(7) 1.581(2) 0.154(5) Uani 0.50 1 d PD B 4
H8'A H 0.1304 0.2217 1.6800 0.185 Uiso 0.50 1 calc PR B 4
H8'B H 0.1497 0.2534 1.5272 0.185 Uiso 0.50 1 calc PR B 4
C9' C 0.0464(7) 0.2467(8) 1.561(3) 0.165(5) Uani 0.50 1 d PD B 4
H9'A H 0.0182 0.2263 1.6406 0.198 Uiso 0.50 1 calc PR B 4
H9'B H 0.0275 0.2197 1.4767 0.198 Uiso 0.50 1 calc PR B 4
C10' C 0.0359(5) 0.3456(6) 1.5485(12) 0.200(4) Uani 0.50 1 d P B 4
H10D H -0.0136 0.3582 1.5381 0.300 Uiso 0.50 1 calc PR B 4
H10E H 0.0612 0.3666 1.4673 0.300 Uiso 0.50 1 calc PR B 4
H10F H 0.0537 0.3736 1.6322 0.300 Uiso 0.50 1 calc PR B 4
C11 C 0.1996(2) -0.0389(3) 0.8850(3) 0.0504(10) Uani 1 1 d . . .
C12 C 0.2182(3) -0.0468(2) 1.0436(4) 0.0554(10) Uani 1 1 d . . .
C13 C 0.2861(3) -0.0338(4) 1.0902(5) 0.108(2) Uani 1 1 d . . .
H13A H 0.3211 -0.0167 1.0268 0.129 Uiso 1 1 calc R . .
C14 C 0.3028(4) -0.0460(5) 1.2318(7) 0.134(3) Uani 1 1 d . . .
H14A H 0.3494 -0.0398 1.2620 0.160 Uiso 1 1 calc R . .
C15 C 0.2517(5) -0.0669(4) 1.3261(6) 0.113(2) Uani 1 1 d . . .
H15A H 0.2627 -0.0723 1.4216 0.136 Uiso 1 1 calc R . .
C16 C 0.1849(4) -0.0797(4) 1.2814(5) 0.100(2) Uani 1 1 d . . .
H16A H 0.1499 -0.0953 1.3458 0.120 Uiso 1 1 calc R . .
C17 C 0.1681(3) -0.0697(3) 1.1389(4) 0.0764(15) Uani 1 1 d . . .
H17A H 0.1218 -0.0789 1.1088 0.092 Uiso 1 1 calc R . .
C18 C 0.2006(2) -0.1281(3) 0.8124(4) 0.0517(10) Uani 1 1 d . . .
C19 C 0.1565(3) -0.1459(3) 0.6999(4) 0.0747(13) Uani 1 1 d . . .
H19A H 0.1249 -0.1039 0.6679 0.090 Uiso 1 1 calc R . .
C20 C 0.1593(3) -0.2267(4) 0.6343(5) 0.0931(17) Uani 1 1 d . . .
H20A H 0.1285 -0.2384 0.5599 0.112 Uiso 1 1 calc R . .
C21 C 0.2057(3) -0.2889(4) 0.6760(5) 0.0851(15) Uani 1 1 d . . .
H21A H 0.2074 -0.3423 0.6297 0.102 Uiso 1 1 calc R . .
C22 C 0.2496(3) -0.2722(3) 0.7855(5) 0.0912(17) Uani 1 1 d . . .
H22A H 0.2819 -0.3141 0.8151 0.109 Uiso 1 1 calc R . .
C23 C 0.2463(3) -0.1929(3) 0.8534(5) 0.0820(16) Uani 1 1 d . . .
H23A H 0.2763 -0.1829 0.9299 0.098 Uiso 1 1 calc R . .
C24 C 0.2497(2) 0.0269(3) 0.8140(4) 0.0582(11) Uani 1 1 d . . .
C25 C 0.2490(3) 0.1127(3) 0.8596(5) 0.0915(17) Uani 1 1 d . . .
H25A H 0.2165 0.1302 0.9279 0.110 Uiso 1 1 calc R . .
C26 C 0.2965(4) 0.1727(4) 0.8042(7) 0.113(2) Uani 1 1 d . . .
H26A H 0.2960 0.2300 0.8358 0.136 Uiso 1 1 calc R . .
C27 C 0.3434(3) 0.1478(5) 0.7046(7) 0.102(2) Uani 1 1 d . . .
H27A H 0.3757 0.1881 0.6693 0.122 Uiso 1 1 calc R . .
C28 C 0.3443(3) 0.0649(5) 0.6550(6) 0.0965(18) Uani 1 1 d . . .
H28A H 0.3763 0.0488 0.5849 0.116 Uiso 1 1 calc R . .
C29 C 0.2971(3) 0.0039(3) 0.7098(5) 0.0722(13) Uani 1 1 d . . .
H29A H 0.2977 -0.0529 0.6756 0.087 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.445(3) . ?
S1 O3 1.449(3) . ?
S1 O1 1.451(3) . ?
S1 C1 1.773(3) . ?
O1W H1W 0.85(4) . ?
O4 C7 1.393(6) . ?
O4 H4O 0.85(4) . ?
N1 C11 1.504(5) . ?
N1 H1N2 0.86(4) . ?
N1 H1N1 0.86(4) . ?
N1 H1N3 0.86(4) . ?
C1 C2' 1.27(3) . ?
C1 C6 1.303(12) . ?
C1 C6' 1.386(9) . ?
C1 C2 1.392(15) . ?
C4 C3' 1.27(3) . ?
C4 C5 1.30(2) . ?
C4 C5' 1.32(2) . ?
C4 C3 1.397(18) . ?
C4 C4 1.490(6) 2_565 ?
C2 C3 1.34(2) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C5 C6 1.40(3) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C2' C3' 1.47(3) . ?
C2' H2'A 0.9300 . ?
C3' H3'A 0.9300 . ?
C5' C6' 1.40(3) . ?
C5' H5'A 0.9300 . ?
C6' H6'A 0.9300 . ?
C7 C8 1.501(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.493(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.492(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C8' C9' 1.440(9) . ?
C8' H8'A 0.9700 . ?
C8' H8'B 0.9700 . ?
C9' H9'A 0.9700 . ?
C9' H9'B 0.9700 . ?
C11 C18 1.532(5) . ?
C11 C24 1.538(6) . ?
C11 C12 1.544(5) . ?
C12 C17 1.353(6) . ?
C12 C13 1.370(7) . ?
C13 C14 1.387(7) . ?
C13 H13A 0.9300 . ?
C14 C15 1.352(9) . ?
C14 H14A 0.9300 . ?
C15 C16 1.344(8) . ?
C15 H15A 0.9300 . ?
C16 C17 1.392(7) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C18 C23 1.374(6) . ?
C18 C19 1.378(5) . ?
C19 C20 1.388(6) . ?
C19 H19A 0.9300 . ?
C20 C21 1.355(7) . ?
C20 H20A 0.9300 . ?
C21 C22 1.350(7) . ?
C21 H21A 0.9300 . ?
C22 C23 1.378(7) . ?
C22 H22A 0.9300 . ?
C23 H23A 0.9300 . ?
C24 C29 1.378(6) . ?
C24 C25 1.387(6) . ?
C25 C26 1.389(7) . ?
C25 H25A 0.9300 . ?
C26 C27 1.348(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.358(8) . ?
C27 H27A 0.9300 . ?
C28 C29 1.392(7) . ?
C28 H28A 0.9300 . ?
C29 H29A 0.9300 . ?

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 S1 O3 113.3(2) . . ?
O2 S1 O1 113.32(19) . . ?
O3 S1 O1 111.93(19) . . ?
O2 S1 C1 105.10(18) . . ?
O3 S1 C1 105.58(18) . . ?
O1 S1 C1 106.80(17) . . ?
C7 O4 H4O 124(4) . . ?
C11 N1 H1N2 113(3) . . ?
C11 N1 H1N1 119(2) . . ?
H1N2 N1 H1N1 106.4(15) . . ?
C11 N1 H1N3 106(2) . . ?
H1N2 N1 H1N3 106.5(15) . . ?
H1N1 N1 H1N3 104.5(15) . . ?
C2' C1 C6 112.0(15) . . ?
C2' C1 C6' 121.5(13) . . ?
C6 C1 C2 116.4(10) . . ?
C6' C1 C2 111.8(11) . . ?
C2' C1 S1 117.5(11) . . ?
C6 C1 S1 124.4(8) . . ?
C6' C1 S1 121.0(9) . . ?
C2 C1 S1 119.1(6) . . ?
C3' C4 C5 107.6(14) . . ?
C3' C4 C5' 114.5(14) . . ?
C5 C4 C3 117.3(9) . . ?
C5' C4 C3 112.0(12) . . ?
C3' C4 C4 121.6(10) . 2_565 ?
C5 C4 C4 124.8(7) . 2_565 ?
C5' C4 C4 123.8(10) . 2_565 ?
C3 C4 C4 117.9(6) . 2_565 ?
C3 C2 C1 122.9(11) . . ?
C3 C2 H2A 118.5 . . ?
C1 C2 H2A 118.5 . . ?
C2 C3 C4 119.3(12) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C4 C5 C6 122.8(13) . . ?
C4 C5 H5A 118.6 . . ?
C6 C5 H5A 118.6 . . ?
C1 C6 C5 121.2(14) . . ?
C1 C6 H6A 119.4 . . ?
C5 C6 H6A 119.4 . . ?
C1 C2' C3' 117(2) . . ?
C1 C2' H2'A 121.4 . . ?
C3' C2' H2'A 121.4 . . ?
C4 C3' C2' 125.1(19) . . ?
C4 C3' H3'A 117.4 . . ?
C2' C3' H3'A 117.4 . . ?
C4 C5' C6' 125.5(16) . . ?
C4 C5' H5'A 117.3 . . ?
C6' C5' H5'A 117.3 . . ?
C1 C6' C5' 116.0(15) . . ?
C1 C6' H6'A 122.0 . . ?
C5' C6' H6'A 122.0 . . ?
O4 C7 C8 104.4(8) . . ?
O4 C7 H7A 110.9 . . ?
C8 C7 H7A 110.9 . . ?
O4 C7 H7B 110.9 . . ?
C8 C7 H7B 110.9 . . ?
H7A C7 H7B 108.9 . . ?
C9 C8 C7 115.6(10) . . ?
C9 C8 H8A 108.4 . . ?
C7 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
C7 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
C10 C9 C8 106.4(9) . . ?
C10 C9 H9A 110.4 . . ?
C8 C9 H9A 110.4 . . ?
C10 C9 H9B 110.4 . . ?
C8 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9' C8' H8'A 108.9 . . ?
C9' C8' H8'B 108.9 . . ?
H8'A C8' H8'B 107.8 . . ?
C8' C9' H9'A 108.1 . . ?
C8' C9' H9'B 108.1 . . ?
H9'A C9' H9'B 107.3 . . ?
N1 C11 C18 107.9(3) . . ?
N1 C11 C24 107.2(3) . . ?
C18 C11 C24 112.6(3) . . ?
N1 C11 C12 108.2(3) . . ?
C18 C11 C12 111.2(3) . . ?
C24 C11 C12 109.6(3) . . ?
C17 C12 C13 118.5(4) . . ?
C17 C12 C11 120.5(4) . . ?
C13 C12 C11 120.9(4) . . ?
C12 C13 C14 120.2(6) . . ?
C12 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
C15 C14 C13 120.4(7) . . ?
C15 C14 H14A 119.8 . . ?
C13 C14 H14A 119.8 . . ?
C16 C15 C14 119.8(5) . . ?
C16 C15 H15A 120.1 . . ?
C14 C15 H15A 120.1 . . ?
C15 C16 C17 120.1(6) . . ?
C15 C16 H16A 120.0 . . ?
C17 C16 H16A 120.0 . . ?
C12 C17 C16 120.9(5) . . ?
C12 C17 H17A 119.5 . . ?
C16 C17 H17A 119.5 . . ?
C23 C18 C19 116.9(4) . . ?
C23 C18 C11 122.0(4) . . ?
C19 C18 C11 121.0(4) . . ?
C18 C19 C20 120.0(5) . . ?
C18 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C21 C20 C19 121.6(5) . . ?
C21 C20 H20A 119.2 . . ?
C19 C20 H20A 119.2 . . ?
C22 C21 C20 119.1(5) . . ?
C22 C21 H21A 120.4 . . ?
C20 C21 H21A 120.4 . . ?
C21 C22 C23 119.8(5) . . ?
C21 C22 H22A 120.1 . . ?
C23 C22 H22A 120.1 . . ?
C18 C23 C22 122.5(5) . . ?
C18 C23 H23A 118.7 . . ?
C22 C23 H23A 118.7 . . ?
C29 C24 C25 118.2(4) . . ?
C29 C24 C11 122.9(4) . . ?
C25 C24 C11 118.9(4) . . ?
C24 C25 C26 120.5(5) . . ?
C24 C25 H25A 119.8 . . ?
C26 C25 H25A 119.8 . . ?
C27 C26 C25 120.0(6) . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C26 C27 C28 121.0(6) . . ?
C26 C27 H27A 119.5 . . ?
C28 C27 H27A 119.5 . . ?
C27 C28 C29 119.7(6) . . ?
C27 C28 H28A 120.2 . . ?
C29 C28 H28A 120.2 . . ?
C24 C29 C28 120.6(5) . . ?
C24 C29 H29A 119.7 . . ?
C28 C29 H29A 119.7 . . ?

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
O2 S1 C1 C2' 80.6(14) . . . . ?
O3 S1 C1 C2' -39.5(14) . . . . ?
O1 S1 C1 C2' -158.7(14) . . . . ?
O2 S1 C1 C6 -129.2(10) . . . . ?
O3 S1 C1 C6 110.7(10) . . . . ?
O1 S1 C1 C6 -8.6(10) . . . . ?
O2 S1 C1 C6' -97.6(10) . . . . ?
O3 S1 C1 C6' 142.4(10) . . . . ?
O1 S1 C1 C6' 23.1(10) . . . . ?
O2 S1 C1 C2 48.8(10) . . . . ?
O3 S1 C1 C2 -71.3(10) . . . . ?
O1 S1 C1 C2 169.4(10) . . . . ?
C2' C1 C2 C3 87(4) . . . . ?
C6 C1 C2 C3 0(3) . . . . ?
C6' C1 C2 C3 -29(3) . . . . ?
S1 C1 C2 C3 -178.4(16) . . . . ?
C1 C2 C3 C4 0(3) . . . . ?
C3' C4 C3 C2 -76(3) . . . . ?
C5 C4 C3 C2 1(3) . . . . ?
C5' C4 C3 C2 26(3) . . . . ?
C4 C4 C3 C2 178.9(15) 2_565 . . . ?
C3' C4 C5 C6 27(3) . . . . ?
C5' C4 C5 C6 -84(4) . . . . ?
C3 C4 C5 C6 -2(3) . . . . ?
C4 C4 C5 C6 -179.7(15) 2_565 . . . ?
C2' C1 C6 C5 -31(2) . . . . ?
C6' C1 C6 C5 86(4) . . . . ?
C2 C1 C6 C5 -1(2) . . . . ?
S1 C1 C6 C5 177.5(15) . . . . ?
C4 C5 C6 C1 2(3) . . . . ?
C6 C1 C2' C3' 28(3) . . . . ?
C6' C1 C2' C3' 0(3) . . . . ?
C2 C1 C2' C3' -77(3) . . . . ?
S1 C1 C2' C3' -177.8(18) . . . . ?
C5 C4 C3' C2' -30(3) . . . . ?
C5' C4 C3' C2' -6(4) . . . . ?
C3 C4 C3' C2' 86(4) . . . . ?
C4 C4 C3' C2' 177(2) 2_565 . . . ?
C1 C2' C3' C4 2(4) . . . . ?
C3' C4 C5' C6' 8(3) . . . . ?
C5 C4 C5' C6' 85(4) . . . . ?
C3 C4 C5' C6' -23(3) . . . . ?
C4 C4 C5' C6' -174.8(18) 2_565 . . . ?
C2' C1 C6' C5' 1(3) . . . . ?
C6 C1 C6' C5' -75(4) . . . . ?
C2 C1 C6' C5' 31(2) . . . . ?
S1 C1 C6' C5' 179.3(15) . . . . ?
C4 C5' C6' C1 -5(3) . . . . ?
O4 C7 C8 C9 162.6(15) . . . . ?
C7 C8 C9 C10 -178.3(15) . . . . ?
N1 C11 C12 C17 36.2(5) . . . . ?
C18 C11 C12 C17 -82.2(5) . . . . ?
C24 C11 C12 C17 152.7(4) . . . . ?
N1 C11 C12 C13 -146.1(4) . . . . ?
C18 C11 C12 C13 95.5(5) . . . . ?
C24 C11 C12 C13 -29.6(6) . . . . ?
C17 C12 C13 C14 1.5(8) . . . . ?
C11 C12 C13 C14 -176.3(6) . . . . ?
C12 C13 C14 C15 -3.1(11) . . . . ?
C13 C14 C15 C16 3.0(12) . . . . ?
C14 C15 C16 C17 -1.4(10) . . . . ?
C13 C12 C17 C16 0.1(7) . . . . ?
C11 C12 C17 C16 177.9(5) . . . . ?
C15 C16 C17 C12 -0.2(8) . . . . ?
N1 C11 C18 C23 -151.2(4) . . . . ?
C24 C11 C18 C23 90.7(5) . . . . ?
C12 C11 C18 C23 -32.7(6) . . . . ?
N1 C11 C18 C19 30.5(5) . . . . ?
C24 C11 C18 C19 -87.6(5) . . . . ?
C12 C11 C18 C19 149.0(4) . . . . ?
C23 C18 C19 C20 0.5(7) . . . . ?
C11 C18 C19 C20 178.9(5) . . . . ?
C18 C19 C20 C21 -1.5(9) . . . . ?
C19 C20 C21 C22 1.1(9) . . . . ?
C20 C21 C22 C23 0.3(8) . . . . ?
C19 C18 C23 C22 0.9(7) . . . . ?
C11 C18 C23 C22 -177.5(5) . . . . ?
C21 C22 C23 C18 -1.3(9) . . . . ?
N1 C11 C24 C29 -127.1(4) . . . . ?
C18 C11 C24 C29 -8.6(5) . . . . ?
C12 C11 C24 C29 115.7(4) . . . . ?
N1 C11 C24 C25 55.1(5) . . . . ?
C18 C11 C24 C25 173.7(4) . . . . ?
C12 C11 C24 C25 -62.0(5) . . . . ?
C29 C24 C25 C26 -1.9(8) . . . . ?
C11 C24 C25 C26 175.9(5) . . . . ?
C24 C25 C26 C27 0.4(9) . . . . ?
C25 C26 C27 C28 1.2(9) . . . . ?
C26 C27 C28 C29 -1.4(9) . . . . ?
C25 C24 C29 C28 1.8(7) . . . . ?
C11 C24 C29 C28 -176.0(4) . . . . ?
C27 C28 C29 C24 -0.2(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W O2 0.85(4) 1.934(16) 2.769(4) 167(5) .
O4 H4O O1W 0.85(4) 2.03(3) 2.793(4) 150(6) .
N1 H1N2 O4 0.86(4) 1.965(10) 2.829(4) 177(4) 1_554
N1 H1N1 O1 0.86(4) 1.955(11) 2.823(4) 173(3) 2
N1 H1N3 O3 0.86(4) 1.939(14) 2.799(4) 168(3) .

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_13
_database_code_depnum_ccdc_archive 'CCDC 1044781'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O6 S2, 2(C19 H18 N), 2(C5 H12 O), H2 O'
_chemical_formula_sum            'C60 H70 N2 O9 S2'
_chemical_formula_weight         1027.30

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           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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

_cell_length_a                   19.8998(9)
_cell_length_b                   15.4214(6)
_cell_length_c                   9.2206(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2829.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1278
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9676
_exptl_absorpt_correction_T_max  0.9763
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7066
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         27.56
_reflns_number_total             5740
_reflns_number_gt                4040
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0489P)²+0.4599P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(11)
_refine_ls_number_reflns         5740
_refine_ls_number_parameters     360
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.1395
_refine_ls_wR_factor_gt          0.1210
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.47611(4) 0.34125(5) 1.06049(10) 0.0428(2) Uani 1 1 d . . .
O1 O 0.51332(12) 0.38264(14) 0.9440(3) 0.0528(6) Uani 1 1 d . . .
O1W O 0.5000 0.5000 1.3851(4) 0.0598(10) Uani 1 2 d SD . .
H1W H 0.499(3) 0.4521(16) 1.339(4) 0.090 Uiso 1 1 d D . .
O2 O 0.50514(14) 0.35669(16) 1.2024(3) 0.0607(7) Uani 1 1 d . . .
O3 O 0.40458(11) 0.36096(14) 1.0547(3) 0.0588(7) Uani 1 1 d . . .
O4 O 0.09823(17) 0.9530(2) 1.4144(3) 0.0809(9) Uani 1 1 d D . .
H4O H 0.0647(18) 0.968(4) 1.465(5) 0.121 Uiso 1 1 d D . .
N1 N 0.37939(14) 0.50347(18) 0.8741(3) 0.0385(7) Uani 1 1 d D . .
H1N1 H 0.3837(15) 0.4578(12) 0.929(2) 0.058 Uiso 1 1 d D . .
H1N2 H 0.4125(12) 0.5374(15) 0.899(3) 0.058 Uiso 1 1 d D . .
H1N3 H 0.3884(15) 0.4855(17) 0.7869(14) 0.058 Uiso 1 1 d D . .
C1 C 0.30871(16) 0.5393(2) 0.8905(3) 0.0367(8) Uani 1 1 d . . .
C2 C 0.30694(17) 0.6287(2) 0.8196(3) 0.0388(8) Uani 1 1 d . . .
C3 C 0.3484(2) 0.6510(3) 0.7075(4) 0.0633(11) Uani 1 1 d . . .
H3A H 0.3805 0.6114 0.6758 0.076 Uiso 1 1 calc R . .
C4 C 0.3438(3) 0.7316(3) 0.6394(5) 0.0793(14) Uani 1 1 d . . .
H4A H 0.3730 0.7458 0.5643 0.095 Uiso 1 1 calc R . .
C5 C 0.2964(3) 0.7892(3) 0.6834(5) 0.0779(14) Uani 1 1 d . . .
H5A H 0.2928 0.8428 0.6377 0.093 Uiso 1 1 calc R . .
C6 C 0.2542(3) 0.7689(3) 0.7943(5) 0.0788(15) Uani 1 1 d . . .
H6A H 0.2214 0.8081 0.8238 0.095 Uiso 1 1 calc R . .
C7 C 0.2602(2) 0.6900(3) 0.8624(5) 0.0629(12) Uani 1 1 d . . .
H7A H 0.2318 0.6773 0.9398 0.075 Uiso 1 1 calc R . .
C8 C 0.29433(16) 0.5464(2) 1.0534(4) 0.0387(7) Uani 1 1 d . . .
C9 C 0.3417(2) 0.5799(3) 1.1467(4) 0.0516(10) Uani 1 1 d . . .
H9A H 0.3838 0.5948 1.1108 0.062 Uiso 1 1 calc R . .
C10 C 0.3283(2) 0.5919(3) 1.2916(4) 0.0676(13) Uani 1 1 d . . .
H10A H 0.3611 0.6150 1.3522 0.081 Uiso 1 1 calc R . .
C11 C 0.2673(3) 0.5700(3) 1.3461(5) 0.0815(16) Uani 1 1 d . . .
H11A H 0.2579 0.5784 1.4438 0.098 Uiso 1 1 calc R . .
C12 C 0.2199(3) 0.5356(4) 1.2564(5) 0.0862(16) Uani 1 1 d . . .
H12A H 0.1783 0.5197 1.2939 0.103 Uiso 1 1 calc R . .
C13 C 0.2328(2) 0.5238(3) 1.1103(4) 0.0690(13) Uani 1 1 d . . .
H13A H 0.1998 0.5006 1.0503 0.083 Uiso 1 1 calc R . .
C14 C 0.26083(18) 0.4747(2) 0.8181(4) 0.0439(9) Uani 1 1 d . . .
C15 C 0.2653(2) 0.3868(3) 0.8524(5) 0.0607(11) Uani 1 1 d . . .
H15A H 0.2996 0.3677 0.9130 0.073 Uiso 1 1 calc R . .
C16 C 0.2196(3) 0.3275(3) 0.7979(5) 0.0770(14) Uani 1 1 d . . .
H16A H 0.2233 0.2690 0.8213 0.092 Uiso 1 1 calc R . .
C17 C 0.1687(3) 0.3557(4) 0.7091(5) 0.0830(15) Uani 1 1 d . . .
H17A H 0.1368 0.3166 0.6750 0.100 Uiso 1 1 calc R . .
C18 C 0.1650(2) 0.4413(4) 0.6710(5) 0.0820(15) Uani 1 1 d . . .
H18A H 0.1315 0.4597 0.6078 0.098 Uiso 1 1 calc R . .
C19 C 0.2102(2) 0.5004(3) 0.7252(4) 0.0575(10) Uani 1 1 d . . .
H19A H 0.2066 0.5585 0.6990 0.069 Uiso 1 1 calc R . .
C20 C 0.48336(16) 0.22766(18) 1.0336(4) 0.0389(8) Uani 1 1 d . . .
C21 C 0.4314(2) 0.1747(2) 1.0720(6) 0.0807(15) Uani 1 1 d . . .
H21A H 0.3911 0.1984 1.1046 0.097 Uiso 1 1 calc R . .
C22 C 0.4388(2) 0.0855(2) 1.0624(7) 0.0851(16) Uani 1 1 d . . .
H22A H 0.4032 0.0501 1.0901 0.102 Uiso 1 1 calc R . .
C23 C 0.49638(17) 0.0482(2) 1.0135(4) 0.0448(9) Uani 1 1 d . . .
C24 C 0.5472(2) 0.1024(3) 0.9724(6) 0.0815(16) Uani 1 1 d . . .
H24A H 0.5869 0.0788 0.9372 0.098 Uiso 1 1 calc R . .
C25 C 0.54103(19) 0.1919(2) 0.9818(5) 0.0722(15) Uani 1 1 d . . .
H25A H 0.5763 0.2273 0.9526 0.087 Uiso 1 1 calc R . .
C26 C 0.1290(15) 0.8754(7) 1.464(4) 0.100(4) Uani 0.50 1 d PD A 1
H26A H 0.1344 0.8761 1.5686 0.120 Uiso 0.50 1 calc PR A 1
H26B H 0.1727 0.8672 1.4193 0.120 Uiso 0.50 1 calc PR A 1
C27 C 0.0815(9) 0.8067(10) 1.419(3) 0.158(5) Uani 0.50 1 d PD A 1
H27A H 0.0791 0.8042 1.3137 0.190 Uiso 0.50 1 calc PR A 1
H27B H 0.0369 0.8192 1.4558 0.190 Uiso 0.50 1 calc PR A 1
C28 C 0.1059(10) 0.7224(10) 1.477(3) 0.183(6) Uani 0.50 1 d PD A 1
H28A H 0.1036 0.7236 1.5825 0.219 Uiso 0.50 1 calc PR A 1
H28B H 0.1525 0.7141 1.4498 0.219 Uiso 0.50 1 calc PR A 1
C29 C 0.0643(13) 0.6468(18) 1.421(3) 0.245(7) Uani 0.50 1 d PD A 1
H29A H 0.0431 0.6598 1.3292 0.294 Uiso 0.50 1 calc PR A 1
H29B H 0.0906 0.5941 1.4129 0.294 Uiso 0.50 1 calc PR A 1
C30 C 0.0147(11) 0.6420(18) 1.542(2) 0.191(7) Uani 0.50 1 d PD A 1
H30A H -0.0154 0.5944 1.5257 0.286 Uiso 0.50 1 calc PR A 1
H30B H -0.0105 0.6951 1.5462 0.286 Uiso 0.50 1 calc PR A 1
H30C H 0.0380 0.6336 1.6322 0.286 Uiso 0.50 1 calc PR A 1
C26' C 0.1315(17) 0.8886(9) 1.495(4) 0.100(4) Uani 0.50 1 d PD A 2
H26C H 0.1170 0.8943 1.5949 0.120 Uiso 0.50 1 calc PR A 2
H26D H 0.1791 0.9022 1.4928 0.120 Uiso 0.50 1 calc PR A 2
C27' C 0.1243(7) 0.7969(10) 1.454(3) 0.158(5) Uani 0.50 1 d PD A 2
H27C H 0.1485 0.7877 1.3644 0.190 Uiso 0.50 1 calc PR A 2
H27D H 0.1462 0.7621 1.5283 0.190 Uiso 0.50 1 calc PR A 2
C28' C 0.0563(7) 0.7642(12) 1.436(3) 0.183(6) Uani 0.50 1 d PD A 2
H28C H 0.0393 0.7767 1.3394 0.219 Uiso 0.50 1 calc PR A 2
H28D H 0.0259 0.7886 1.5073 0.219 Uiso 0.50 1 calc PR A 2
C29' C 0.0654(13) 0.6682(13) 1.458(4) 0.245(7) Uani 0.50 1 d PD A 2
H29C H 0.1001 0.6462 1.3939 0.294 Uiso 0.50 1 calc PR A 2
H29D H 0.0786 0.6564 1.5574 0.294 Uiso 0.50 1 calc PR A 2
C30' C 0.0003(11) 0.6265(18) 1.426(2) 0.191(7) Uani 0.50 1 d PD A 2
H30D H 0.0056 0.5646 1.4276 0.286 Uiso 0.50 1 calc PR A 2
H30E H -0.0147 0.6441 1.3311 0.286 Uiso 0.50 1 calc PR A 2
H30F H -0.0322 0.6436 1.4969 0.286 Uiso 0.50 1 calc PR A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.450(3) . ?
S1 O1 1.452(2) . ?
S1 O3 1.456(2) . ?
S1 C20 1.775(3) . ?
O1W H1W 0.85(3) . ?
O4 C26' 1.405(9) . ?
O4 C26 1.420(9) . ?
O4 H4O 0.85(3) . ?
N1 C1 1.519(4) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
C1 C2 1.525(4) . ?
C1 C14 1.532(5) . ?
C1 C8 1.533(5) . ?
C2 C3 1.367(5) . ?
C2 C7 1.384(5) . ?
C3 C4 1.397(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.358(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.360(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.375(6) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.377(5) . ?
C8 C9 1.377(5) . ?
C9 C10 1.375(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.358(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.361(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.383(6) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C19 1.381(5) . ?
C14 C15 1.394(6) . ?
C15 C16 1.385(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.372(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.368(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.375(6) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C25 1.360(5) . ?
C20 C21 1.365(5) . ?
C21 C22 1.386(5) . ?
C21 H21A 0.9300 . ?
C22 C23 1.360(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.365(5) . ?
C23 C23 1.493(6) 2_655 ?
C24 C25 1.387(5) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.480(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.490(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.520(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.490(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C26' C27' 1.470(10) . ?
C26' H26C 0.9700 . ?
C26' H26D 0.9700 . ?
C27' C28' 1.455(9) . ?
C27' H27C 0.9700 . ?
C27' H27D 0.9700 . ?
C28' C29' 1.505(10) . ?
C28' H28C 0.9700 . ?
C28' H28D 0.9700 . ?
C29' C30' 1.478(10) . ?
C29' H29C 0.9700 . ?
C29' H29D 0.9700 . ?
C30' H30D 0.9600 . ?
C30' H30E 0.9600 . ?
C30' H30F 0.9600 . ?

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 S1 O1 113.09(15) . . ?
O2 S1 O3 112.82(18) . . ?
O1 S1 O3 112.31(16) . . ?
O2 S1 C20 104.82(15) . . ?
O1 S1 C20 106.79(15) . . ?
O3 S1 C20 106.28(14) . . ?
C26' O4 H4O 106(4) . . ?
C26 O4 H4O 113(5) . . ?
C1 N1 H1N1 109(2) . . ?
C1 N1 H1N2 117(2) . . ?
H1N1 N1 H1N2 104.7(14) . . ?
C1 N1 H1N3 114(2) . . ?
H1N1 N1 H1N3 105.2(14) . . ?
H1N2 N1 H1N3 106.4(15) . . ?
N1 C1 C2 107.9(3) . . ?
N1 C1 C14 107.2(3) . . ?
C2 C1 C14 112.8(3) . . ?
N1 C1 C8 107.2(2) . . ?
C2 C1 C8 110.6(3) . . ?
C14 C1 C8 110.9(3) . . ?
C3 C2 C7 116.7(4) . . ?
C3 C2 C1 122.5(3) . . ?
C7 C2 C1 120.7(3) . . ?
C2 C3 C4 121.6(4) . . ?
C2 C3 H3A 119.2 . . ?
C4 C3 H3A 119.2 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
C5 C6 C7 119.6(4) . . ?
C5 C6 H6A 120.2 . . ?
C7 C6 H6A 120.2 . . ?
C6 C7 C2 122.2(4) . . ?
C6 C7 H7A 118.9 . . ?
C2 C7 H7A 118.9 . . ?
C13 C8 C9 117.8(3) . . ?
C13 C8 C1 121.4(3) . . ?
C9 C8 C1 120.7(3) . . ?
C10 C9 C8 121.6(4) . . ?
C10 C9 H9A 119.2 . . ?
C8 C9 H9A 119.2 . . ?
C11 C10 C9 120.0(4) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 119.4(4) . . ?
C10 C11 H11A 120.3 . . ?
C12 C11 H11A 120.3 . . ?
C11 C12 C13 121.0(4) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C8 C13 C12 120.1(4) . . ?
C8 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C19 C14 C15 117.8(4) . . ?
C19 C14 C1 122.5(4) . . ?
C15 C14 C1 119.6(3) . . ?
C16 C15 C14 121.2(4) . . ?
C16 C15 H15A 119.4 . . ?
C14 C15 H15A 119.4 . . ?
C17 C16 C15 119.5(5) . . ?
C17 C16 H16A 120.3 . . ?
C15 C16 H16A 120.3 . . ?
C18 C17 C16 119.9(4) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C19 120.7(5) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C18 C19 C14 120.8(5) . . ?
C18 C19 H19A 119.6 . . ?
C14 C19 H19A 119.6 . . ?
C25 C20 C21 119.2(3) . . ?
C25 C20 S1 121.2(2) . . ?
C21 C20 S1 119.5(3) . . ?
C20 C21 C22 119.7(4) . . ?
C20 C21 H21A 120.1 . . ?
C22 C21 H21A 120.1 . . ?
C23 C22 C21 122.1(4) . . ?
C23 C22 H22A 119.0 . . ?
C21 C22 H22A 119.0 . . ?
C22 C23 C24 117.2(3) . . ?
C22 C23 C23 120.2(4) . 2_655 ?
C24 C23 C23 122.6(4) . 2_655 ?
C23 C24 C25 121.8(4) . . ?
C23 C24 H24A 119.1 . . ?
C25 C24 H24A 119.1 . . ?
C20 C25 C24 120.0(3) . . ?
C20 C25 H25A 120.0 . . ?
C24 C25 H25A 120.0 . . ?
O4 C26 C27 103.7(11) . . ?
O4 C26 H26A 111.0 . . ?
C27 C26 H26A 111.0 . . ?
O4 C26 H26B 111.0 . . ?
C27 C26 H26B 111.0 . . ?
H26A C26 H26B 109.0 . . ?
C26 C27 C28 108.3(13) . . ?
C26 C27 H27A 110.0 . . ?
C28 C27 H27A 110.0 . . ?
C26 C27 H27B 110.0 . . ?
C28 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
C27 C28 C29 112(2) . . ?
C27 C28 H28A 109.3 . . ?
C29 C28 H28A 109.3 . . ?
C27 C28 H28B 109.3 . . ?
C29 C28 H28B 109.3 . . ?
H28A C28 H28B 107.9 . . ?
C30 C29 C28 98.3(18) . . ?
C30 C29 H29A 112.1 . . ?
C28 C29 H29A 112.1 . . ?
C30 C29 H29B 112.1 . . ?
C28 C29 H29B 112.1 . . ?
H29A C29 H29B 109.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O4 C26' C27' 119.9(16) . . ?
O4 C26' H26C 107.3 . . ?
C27' C26' H26C 107.3 . . ?
O4 C26' H26D 107.3 . . ?
C27' C26' H26D 107.3 . . ?
H26C C26' H26D 106.9 . . ?
C28' C27' C26' 117(2) . . ?
C28' C27' H27C 108.0 . . ?
C26' C27' H27C 108.0 . . ?
C28' C27' H27D 108.0 . . ?
C26' C27' H27D 108.0 . . ?
H27C C27' H27D 107.3 . . ?
C27' C28' C29' 102.2(15) . . ?
C27' C28' H28C 111.3 . . ?
C29' C28' H28C 111.3 . . ?
C27' C28' H28D 111.3 . . ?
C29' C28' H28D 111.3 . . ?
H28C C28' H28D 109.2 . . ?
C30' C29' C28' 107(2) . . ?
C30' C29' H29C 110.3 . . ?
C28' C29' H29C 110.3 . . ?
C30' C29' H29D 110.3 . . ?
C28' C29' H29D 110.3 . . ?
H29C C29' H29D 108.5 . . ?
C29' C30' H30D 109.5 . . ?
C29' C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C29' C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 28.1(4) . . . . ?
C14 C1 C2 C3 -90.2(4) . . . . ?
C8 C1 C2 C3 145.0(3) . . . . ?
N1 C1 C2 C7 -155.2(3) . . . . ?
C14 C1 C2 C7 86.6(4) . . . . ?
C8 C1 C2 C7 -38.2(4) . . . . ?
C7 C2 C3 C4 0.0(6) . . . . ?
C1 C2 C3 C4 176.8(4) . . . . ?
C2 C3 C4 C5 -1.0(7) . . . . ?
C3 C4 C5 C6 0.7(8) . . . . ?
C4 C5 C6 C7 0.6(8) . . . . ?
C5 C6 C7 C2 -1.8(7) . . . . ?
C3 C2 C7 C6 1.4(6) . . . . ?
C1 C2 C7 C6 -175.5(4) . . . . ?
N1 C1 C8 C13 -139.0(3) . . . . ?
C2 C1 C8 C13 103.6(4) . . . . ?
C14 C1 C8 C13 -22.3(5) . . . . ?
N1 C1 C8 C9 44.4(4) . . . . ?
C2 C1 C8 C9 -73.0(4) . . . . ?
C14 C1 C8 C9 161.2(3) . . . . ?
C13 C8 C9 C10 -0.9(6) . . . . ?
C1 C8 C9 C10 175.8(4) . . . . ?
C8 C9 C10 C11 0.4(7) . . . . ?
C9 C10 C11 C12 0.5(8) . . . . ?
C10 C11 C12 C13 -1.0(9) . . . . ?
C9 C8 C13 C12 0.5(7) . . . . ?
C1 C8 C13 C12 -176.2(4) . . . . ?
C11 C12 C13 C8 0.5(8) . . . . ?
N1 C1 C14 C19 -134.0(3) . . . . ?
C2 C1 C14 C19 -15.4(4) . . . . ?
C8 C1 C14 C19 109.3(4) . . . . ?
N1 C1 C14 C15 49.8(4) . . . . ?
C2 C1 C14 C15 168.4(3) . . . . ?
C8 C1 C14 C15 -67.0(4) . . . . ?
C19 C14 C15 C16 -1.5(6) . . . . ?
C1 C14 C15 C16 174.9(4) . . . . ?
C14 C15 C16 C17 -0.4(7) . . . . ?
C15 C16 C17 C18 2.4(7) . . . . ?
C16 C17 C18 C19 -2.6(8) . . . . ?
C17 C18 C19 C14 0.7(7) . . . . ?
C15 C14 C19 C18 1.3(6) . . . . ?
C1 C14 C19 C18 -175.0(4) . . . . ?
O2 S1 C20 C25 -84.1(4) . . . . ?
O1 S1 C20 C25 36.1(4) . . . . ?
O3 S1 C20 C25 156.2(3) . . . . ?
O2 S1 C20 C21 92.7(4) . . . . ?
O1 S1 C20 C21 -147.1(4) . . . . ?
O3 S1 C20 C21 -27.0(4) . . . . ?
C25 C20 C21 C22 2.1(8) . . . . ?
S1 C20 C21 C22 -174.8(4) . . . . ?
C20 C21 C22 C23 -0.9(9) . . . . ?
C21 C22 C23 C24 -0.6(8) . . . . ?
C21 C22 C23 C23 176.2(5) . . . 2_655 ?
C22 C23 C24 C25 0.9(8) . . . . ?
C23 C23 C24 C25 -175.9(4) 2_655 . . . ?
C21 C20 C25 C24 -1.8(7) . . . . ?
S1 C20 C25 C24 175.0(4) . . . . ?
C23 C24 C25 C20 0.3(8) . . . . ?
C26' O4 C26 C27 136(15) . . . . ?
O4 C26 C27 C28 -175(2) . . . . ?
C26 C27 C28 C29 -173(3) . . . . ?
C27 C28 C29 C30 -93(2) . . . . ?
C26 O4 C26' C27' -19(10) . . . . ?
O4 C26' C27' C28' -51(4) . . . . ?
C26' C27' C28' C29' -157(2) . . . . ?
C27' C28' C29' C30' -174(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W O2 0.85(3) 1.940(13) 2.781(3) 168(4) .
O4 H4O O1W 0.85(3) 1.955(16) 2.786(4) 168(5) 3_468
N1 H1N1 O3 0.86(3) 1.932(11) 2.803(4) 173(3) .
N1 H1N2 O1 0.86(3) 1.967(10) 2.839(4) 176(3) 2_665
N1 H1N3 O4 0.86(3) 1.941(10) 2.807(4) 174(3) 4_547

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.040
####################################################################### 
# 
# 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_14
_database_code_depnum_ccdc_archive 'CCDC 1044782'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C12 H8 O6 S2, 2(C19 H18 N), 2(C3 H7 N O), 3(H2 O)'
_chemical_formula_sum            'C56 H64 N4 O11 S2'
_chemical_formula_weight         1033.25

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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   13.8413(12)
_cell_length_b                   12.9378(8)
_cell_length_c                   18.2777(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.265(6)
_cell_angle_gamma                90.00
_cell_volume                     2672.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2196
_cell_measurement_theta_min      3.23
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9634
_exptl_absorpt_correction_T_max  0.9759
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10086
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6111
_reflns_number_gt                4200
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0683P)²+0.8082P] where P=(Fo²+2Fc²)/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         6111
_refine_ls_number_parameters     346
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1610
_refine_ls_wR_factor_gt          0.1398
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.14527(5) 0.57380(5) 0.16130(4) 0.03627(17) Uani 1 1 d . . .
O1 O 0.11395(15) 0.47578(13) 0.11360(11) 0.0469(4) Uani 1 1 d . . .
O1W O -0.1822(4) 0.2144(2) -0.0032(2) 0.1123(11) Uani 1 1 d D . .
H1W1 H -0.164(5) 0.250(3) -0.032(3) 0.168 Uiso 1 1 d D . .
H1W2 H -0.225(4) 0.251(3) 0.006(4) 0.168 Uiso 1 1 d D . .
O2 O 0.04850(14) 0.61609(15) 0.16227(11) 0.0528(5) Uani 1 1 d . . .
O2W O 0.0448(8) 0.6195(7) 0.3339(6) 0.178(3) Uani 0.50 1 d P . .
H2W1 H 0.0594 0.6276 0.2950 0.214 Uiso 0.50 1 d PR . .
H2W2 H 0.0951 0.6536 0.3806 0.214 Uiso 0.50 1 d PR . .
O3 O 0.19383(17) 0.64732(16) 0.13119(12) 0.0622(6) Uani 1 1 d . . .
O4 O -0.24476(19) 0.39208(15) 0.06285(13) 0.0605(5) Uani 1 1 d . . .
N1 N -0.17625(16) 0.56651(14) 0.00644(12) 0.0308(4) Uani 1 1 d D . .
H1N3 H -0.1095(13) 0.5864(16) 0.0539(9) 0.046 Uiso 1 1 d D . .
H1N2 H -0.1637(19) 0.5540(17) -0.0340(10) 0.046 Uiso 1 1 d D . .
H1N1 H -0.1974(18) 0.5100(12) 0.0179(13) 0.046 Uiso 1 1 d D . .
N2 N -0.1352(2) 0.38655(17) 0.21457(16) 0.0526(6) Uani 1 1 d . . .
C1 C -0.26917(18) 0.64883(16) -0.02147(14) 0.0279(4) Uani 1 1 d . . .
C2 C -0.21631(18) 0.75435(16) -0.01929(14) 0.0290(5) Uani 1 1 d . . .
C3 C -0.14476(15) 0.76502(14) -0.04923(11) 0.0380(5) Uani 1 1 d . . .
H3A H -0.1231 0.7069 -0.0665 0.046 Uiso 1 1 calc R . .
C4 C -0.10538(15) 0.86222(14) -0.05345(11) 0.0457(6) Uani 1 1 d . . .
H4A H -0.0542 0.8687 -0.0728 0.055 Uiso 1 1 d R . .
C5 C -0.1392(2) 0.9490(2) -0.03030(17) 0.0473(6) Uani 1 1 d . . .
H5A H -0.1147 1.0140 -0.0353 0.057 Uiso 1 1 calc R . .
C6 C -0.2095(2) 0.93960(19) 0.00032(18) 0.0470(6) Uani 1 1 d . . .
H6A H -0.2314 0.9981 0.0170 0.056 Uiso 1 1 calc R . .
C7 C -0.2473(2) 0.84258(18) 0.00613(16) 0.0391(5) Uani 1 1 d . . .
H7A H -0.2940 0.8365 0.0273 0.047 Uiso 1 1 calc R . .
C8 C -0.2990(2) 0.64523(16) 0.04789(15) 0.0314(5) Uani 1 1 d . . .
C9 C -0.2091(2) 0.66092(19) 0.13735(16) 0.0411(6) Uani 1 1 d . . .
H9A H -0.1319 0.6703 0.1548 0.049 Uiso 1 1 calc R . .
C10 C -0.2333(3) 0.6628(2) 0.20146(19) 0.0552(7) Uani 1 1 d . . .
H10A H -0.1723 0.6736 0.2614 0.066 Uiso 1 1 calc R . .
C11 C -0.3474(3) 0.6487(2) 0.1763(2) 0.0660(9) Uani 1 1 d . . .
H11A H -0.3637 0.6509 0.2190 0.079 Uiso 1 1 calc R . .
C12 C -0.4364(3) 0.6315(2) 0.0884(2) 0.0606(8) Uani 1 1 d . . .
H12A H -0.5132 0.6209 0.0716 0.073 Uiso 1 1 calc R . .
C13 C -0.4130(2) 0.62983(19) 0.02379(18) 0.0440(6) Uani 1 1 d . . .
H13A H -0.4744 0.6183 -0.0359 0.053 Uiso 1 1 calc R . .
C14 C -0.37637(19) 0.62630(17) -0.11704(15) 0.0328(5) Uani 1 1 d . . .
C15 C -0.4532(2) 0.7057(2) -0.16848(19) 0.0582(8) Uani 1 1 d . . .
H15A H -0.4378 0.7721 -0.1447 0.070 Uiso 1 1 calc R . .
C16 C -0.5522(3) 0.6886(3) -0.2542(2) 0.0713(9) Uani 1 1 d . . .
H16A H -0.6038 0.7427 -0.2871 0.086 Uiso 1 1 calc R . .
C17 C -0.5741(3) 0.5918(3) -0.29082(19) 0.0643(9) Uani 1 1 d . . .
H17A H -0.6398 0.5801 -0.3491 0.077 Uiso 1 1 calc R . .
C18 C -0.4990(2) 0.5121(2) -0.24139(19) 0.0557(7) Uani 1 1 d . . .
H18A H -0.5138 0.4464 -0.2664 0.067 Uiso 1 1 calc R . .
C19 C -0.4010(2) 0.52857(19) -0.15438(16) 0.0422(6) Uani 1 1 d . . .
H19A H -0.3515 0.4736 -0.1210 0.051 Uiso 1 1 calc R . .
C20 C -0.1313(4) 0.3945(3) 0.2956(2) 0.0849(11) Uani 1 1 d . . .
H20A H -0.2098 0.4050 0.2798 0.127 Uiso 1 1 calc R . .
H20B H -0.0822 0.4519 0.3308 0.127 Uiso 1 1 calc R . .
H20C H -0.0992 0.3320 0.3298 0.127 Uiso 1 1 calc R . .
C21 C -0.2334(3) 0.3968(2) 0.1349(2) 0.0518(7) Uani 1 1 d . . .
H21A H -0.3017 0.4090 0.1321 0.062 Uiso 1 1 calc R . .
C22 C -0.0254(3) 0.3710(4) 0.2239(3) 0.1159(17) Uani 1 1 d . . .
H22A H -0.0409 0.3661 0.1656 0.174 Uiso 1 1 calc R . .
H22B H 0.0111 0.3083 0.2565 0.174 Uiso 1 1 calc R . .
H22C H 0.0265 0.4282 0.2558 0.174 Uiso 1 1 calc R . .
C23 C 0.25999(19) 0.54638(17) 0.27445(14) 0.0332(5) Uani 1 1 d . . .
C24 C 0.3080(2) 0.45051(19) 0.30147(16) 0.0459(6) Uani 1 1 d . . .
H24A H 0.2776 0.3964 0.2605 0.055 Uiso 1 1 calc R . .
C25 C 0.4017(2) 0.43278(19) 0.38936(15) 0.0452(6) Uani 1 1 d . . .
H25A H 0.4334 0.3666 0.4061 0.054 Uiso 1 1 calc R . .
C26 C 0.44951(18) 0.50983(18) 0.45278(14) 0.0348(5) Uani 1 1 d . . .
C27 C 0.3982(3) 0.6060(2) 0.4244(2) 0.0979(15) Uani 1 1 d . . .
H27A H 0.4271 0.6601 0.4653 0.117 Uiso 1 1 calc R . .
C28 C 0.3046(3) 0.6240(2) 0.3364(2) 0.0943(14) Uani 1 1 d . . .
H28A H 0.2717 0.6898 0.3192 0.113 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.4446(19) . ?
S1 O1 1.4559(17) . ?
S1 O2 1.4564(17) . ?
S1 C23 1.770(2) . ?
O1W H1W1 0.85(2) . ?
O1W H1W2 0.85(2) . ?
O2W H2W1 0.8500 . ?
O2W H2W2 0.8500 . ?
O4 C21 1.235(3) . ?
N1 C1 1.514(3) . ?
N1 H1N3 0.86(2) . ?
N1 H1N2 0.86(2) . ?
N1 H1N1 0.86(2) . ?
N2 C21 1.303(3) . ?
N2 C22 1.442(4) . ?
N2 C20 1.454(4) . ?
C1 C14 1.531(3) . ?
C1 C2 1.539(3) . ?
C1 C8 1.544(3) . ?
C2 C3 1.387(3) . ?
C2 C7 1.390(3) . ?
C3 C4 1.390(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.374(3) . ?
C4 H4A 0.9601 . ?
C5 C6 1.379(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.387(3) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.383(3) . ?
C8 C13 1.386(3) . ?
C9 C10 1.392(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.378(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.364(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.394(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C19 1.383(3) . ?
C14 C15 1.385(3) . ?
C15 C16 1.379(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.369(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.369(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.387(3) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.358(3) . ?
C23 C28 1.365(4) . ?
C24 C25 1.382(3) . ?
C24 H24A 0.9300 . ?
C25 C26 1.375(3) . ?
C25 H25A 0.9300 . ?
C26 C27 1.377(4) . ?
C26 C26 1.487(4) 3_666 ?
C27 C28 1.383(4) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?

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
O3 S1 O1 112.86(12) . . ?
O3 S1 O2 113.01(13) . . ?
O1 S1 O2 112.12(11) . . ?
O3 S1 C23 106.04(11) . . ?
O1 S1 C23 106.33(10) . . ?
O2 S1 C23 105.79(10) . . ?
H1W1 O1W H1W2 108.7(17) . . ?
H2W1 O2W H2W2 108.8 . . ?
C1 N1 H1N3 109.7(15) . . ?
C1 N1 H1N2 113.2(16) . . ?
H1N3 N1 H1N2 106.7(13) . . ?
C1 N1 H1N1 109.8(16) . . ?
H1N3 N1 H1N1 109.0(13) . . ?
H1N2 N1 H1N1 108.4(13) . . ?
C21 N2 C22 119.6(3) . . ?
C21 N2 C20 122.2(3) . . ?
C22 N2 C20 118.1(3) . . ?
N1 C1 C14 109.00(17) . . ?
N1 C1 C2 108.47(16) . . ?
C14 C1 C2 109.36(17) . . ?
N1 C1 C8 106.26(16) . . ?
C14 C1 C8 112.86(17) . . ?
C2 C1 C8 110.74(17) . . ?
C3 C2 C7 118.56(19) . . ?
C3 C2 C1 121.00(18) . . ?
C7 C2 C1 120.23(18) . . ?
C2 C3 C4 120.25(11) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 120.52(12) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.7 . . ?
C4 C5 C6 119.9(2) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
C5 C6 C7 119.7(2) . . ?
C5 C6 H6A 120.1 . . ?
C7 C6 H6A 120.1 . . ?
C6 C7 C2 121.0(2) . . ?
C6 C7 H7A 119.5 . . ?
C2 C7 H7A 119.5 . . ?
C9 C8 C13 118.6(2) . . ?
C9 C8 C1 118.79(19) . . ?
C13 C8 C1 122.6(2) . . ?
C8 C9 C10 120.5(2) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 120.4(3) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C8 C13 C12 120.5(3) . . ?
C8 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C19 C14 C15 118.0(2) . . ?
C19 C14 C1 122.5(2) . . ?
C15 C14 C1 119.5(2) . . ?
C16 C15 C14 121.5(3) . . ?
C16 C15 H15A 119.3 . . ?
C14 C15 H15A 119.3 . . ?
C17 C16 C15 119.8(3) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C18 C17 C16 119.8(3) . . ?
C18 C17 H17A 120.1 . . ?
C16 C17 H17A 120.1 . . ?
C17 C18 C19 120.5(3) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
C14 C19 C18 120.4(2) . . ?
C14 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 N2 126.6(3) . . ?
O4 C21 H21A 116.7 . . ?
N2 C21 H21A 116.7 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 118.6(2) . . ?
C24 C23 S1 121.90(18) . . ?
C28 C23 S1 119.51(19) . . ?
C23 C24 C25 120.5(2) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
C26 C25 C24 122.1(2) . . ?
C26 C25 H25A 118.9 . . ?
C24 C25 H25A 118.9 . . ?
C25 C26 C27 116.4(2) . . ?
C25 C26 C26 121.8(3) . 3_666 ?
C27 C26 C26 121.8(3) . 3_666 ?
C26 C27 C28 121.5(3) . . ?
C26 C27 H27A 119.2 . . ?
C28 C27 H27A 119.2 . . ?
C23 C28 C27 120.8(3) . . ?
C23 C28 H28A 119.6 . . ?
C27 C28 H28A 119.6 . . ?

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
N1 C1 C2 C3 40.2(2) . . . . ?
C14 C1 C2 C3 -78.6(2) . . . . ?
C8 C1 C2 C3 156.40(18) . . . . ?
N1 C1 C2 C7 -145.0(2) . . . . ?
C14 C1 C2 C7 96.2(2) . . . . ?
C8 C1 C2 C7 -28.8(3) . . . . ?
C7 C2 C3 C4 0.0(2) . . . . ?
C1 C2 C3 C4 174.90(13) . . . . ?
C2 C3 C4 C5 -1.68(16) . . . . ?
C3 C4 C5 C6 2.2(3) . . . . ?
C4 C5 C6 C7 -1.1(4) . . . . ?
C5 C6 C7 C2 -0.6(4) . . . . ?
C3 C2 C7 C6 1.1(3) . . . . ?
C1 C2 C7 C6 -173.8(2) . . . . ?
N1 C1 C8 C9 58.5(2) . . . . ?
C14 C1 C8 C9 177.9(2) . . . . ?
C2 C1 C8 C9 -59.1(3) . . . . ?
N1 C1 C8 C13 -123.4(2) . . . . ?
C14 C1 C8 C13 -4.0(3) . . . . ?
C2 C1 C8 C13 119.0(2) . . . . ?
C13 C8 C9 C10 -1.0(3) . . . . ?
C1 C8 C9 C10 177.2(2) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C9 C10 C11 C12 0.9(5) . . . . ?
C10 C11 C12 C13 -1.0(5) . . . . ?
C9 C8 C13 C12 0.8(4) . . . . ?
C1 C8 C13 C12 -177.3(2) . . . . ?
C11 C12 C13 C8 0.2(4) . . . . ?
N1 C1 C14 C19 23.2(3) . . . . ?
C2 C1 C14 C19 141.6(2) . . . . ?
C8 C1 C14 C19 -94.6(2) . . . . ?
N1 C1 C14 C15 -157.6(2) . . . . ?
C2 C1 C14 C15 -39.2(3) . . . . ?
C8 C1 C14 C15 84.6(3) . . . . ?
C19 C14 C15 C16 0.5(4) . . . . ?
C1 C14 C15 C16 -178.7(3) . . . . ?
C14 C15 C16 C17 -1.7(5) . . . . ?
C15 C16 C17 C18 1.3(5) . . . . ?
C16 C17 C18 C19 0.2(5) . . . . ?
C15 C14 C19 C18 1.1(4) . . . . ?
C1 C14 C19 C18 -179.8(2) . . . . ?
C17 C18 C19 C14 -1.4(4) . . . . ?
C22 N2 C21 O4 2.1(5) . . . . ?
C20 N2 C21 O4 179.4(3) . . . . ?
O3 S1 C23 C24 -115.9(2) . . . . ?
O1 S1 C23 C24 4.5(2) . . . . ?
O2 S1 C23 C24 123.9(2) . . . . ?
O3 S1 C23 C28 62.1(3) . . . . ?
O1 S1 C23 C28 -177.6(3) . . . . ?
O2 S1 C23 C28 -58.2(3) . . . . ?
C28 C23 C24 C25 -1.4(4) . . . . ?
S1 C23 C24 C25 176.6(2) . . . . ?
C23 C24 C25 C26 0.4(4) . . . . ?
C24 C25 C26 C27 0.7(4) . . . . ?
C24 C25 C26 C26 -179.9(3) . . . 3_666 ?
C25 C26 C27 C28 -0.9(6) . . . . ?
C26 C26 C27 C28 179.7(4) 3_666 . . . ?
C24 C23 C28 C27 1.2(6) . . . . ?
S1 C23 C28 C27 -176.8(3) . . . . ?
C26 C27 C28 C23 -0.1(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O3 0.85(2) 2.08(2) 2.874(3) 156(5) 3_565
O1W H1W2 O4 0.85(2) 2.19(3) 2.949(4) 148(5) .
O2W H2W1 O2 0.85 2.35 3.167(8) 162.2 .
O2W H2W2 O1W 0.85 1.99 2.812(9) 161.3 2
N1 H1N3 O2 0.86(2) 1.963(10) 2.823(2) 174(2) .
N1 H1N2 O1 0.86(2) 1.975(10) 2.836(2) 173(2) 3_565
N1 H1N1 O4 0.86(2) 2.013(9) 2.861(3) 169.6(19) .

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.051

