# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_complex8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(H3 O)'
_chemical_formula_sum            'C12 H14 O10 S2'
_chemical_formula_weight         382.35

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'


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

_cell_length_a                   29.188(7)
_cell_length_b                   5.7170(10)
_cell_length_c                   22.742(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.89(2)
_cell_angle_gamma                90.00
_cell_volume                     3256.6(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9940
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.46

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9250
_exptl_absorpt_correction_T_max  0.9456
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15272
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3725
_reflns_number_gt                2850
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97


_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)+(0.0813P)²+4.0863P] 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         3725
_refine_ls_number_parameters     241
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1518
_refine_ls_wR_factor_gt          0.1352
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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 0.67467(2) 0.46663(12) 0.53870(3) 0.03017(19) Uani 1 1 d . . .
S2 S 0.33857(2) 0.05458(12) 0.20888(3) 0.03005(19) Uani 1 1 d . . .
O1 O 0.66479(8) 0.2489(4) 0.56307(10) 0.0419(5) Uani 1 1 d . . .
O1W O 0.73781(7) 0.5305(3) 0.41956(9) 0.0321(4) Uani 1 1 d D . .
H1W1 H 0.7175(10) 0.622(4) 0.3872(9) 0.048 Uiso 1 1 d D . .
H1W2 H 0.7370(12) 0.397(2) 0.4024(12) 0.048 Uiso 1 1 d D . .
H1W3 H 0.7275(12) 0.519(4) 0.4480(11) 0.048 Uiso 1 1 d D . .
O2 O 0.68356(8) 0.6612(4) 0.58420(9) 0.0416(5) Uani 1 1 d . . .
O2W O 0.29392(10) -0.4883(5) 0.28677(13) 0.0579(6) Uani 1 1 d D . .
H2W3 H 0.2616(7) -0.454(7) 0.2760(17) 0.087 Uiso 1 1 d D . .
H2W1 H 0.2922(14) -0.596(5) 0.2592(14) 0.087 Uiso 1 1 d D . .
H2W2 H 0.3089(13) -0.551(6) 0.3274(9) 0.087 Uiso 1 1 d D . .
O3 O 0.71726(8) 0.4446(4) 0.52403(10) 0.0432(5) Uani 1 1 d . . .
O4 O 0.65657(8) 0.8453(4) 0.43865(10) 0.0433(5) Uani 1 1 d D . .
H4O H 0.6536(16) 0.944(5) 0.4091(15) 0.065 Uiso 1 1 d D . .
O5 O 0.33086(9) -0.1935(4) 0.20788(10) 0.0458(5) Uani 1 1 d . . .
O6 O 0.29081(7) 0.1838(4) 0.19528(9) 0.0388(5) Uani 1 1 d . . .
O7 O 0.35775(8) 0.1343(4) 0.16478(9) 0.0388(5) Uani 1 1 d . . .
O8 O 0.33444(8) -0.0332(4) 0.33351(9) 0.0389(5) Uani 1 1 d D . .
H8O H 0.3406(15) -0.080(6) 0.3719(10) 0.058 Uiso 1 1 d D . .
C1 C 0.61470(10) 0.5320(5) 0.46148(12) 0.0317(6) Uani 1 1 d . . .
C2 C 0.61163(11) 0.7191(5) 0.42029(13) 0.0359(6) Uani 1 1 d . . .
C3 C 0.56270(12) 0.7710(6) 0.36196(15) 0.0488(8) Uani 1 1 d . . .
H3 H 0.5601 0.8942 0.3337 0.059 Uiso 1 1 calc R . .
C4 C 0.51799(12) 0.6395(6) 0.34608(15) 0.0488(8) Uani 1 1 d . . .
H4 H 0.4855 0.6771 0.3072 0.059 Uiso 1 1 calc R . .
C5 C 0.52028(11) 0.4530(5) 0.38654(14) 0.0397(7) Uani 1 1 d . . .
C6 C 0.56964(11) 0.4015(5) 0.44443(14) 0.0369(6) Uani 1 1 d . . .
H6 H 0.5723 0.2766 0.4722 0.044 Uiso 1 1 calc R . .
C7 C 0.47245(11) 0.3173(5) 0.37249(13) 0.0379(6) Uani 1 1 d . . .
C8 C 0.43318(10) 0.2552(5) 0.30611(13) 0.0353(6) Uani 1 1 d . . .
H8 H 0.4373 0.2973 0.2696 0.042 Uiso 1 1 calc R . .
C9 C 0.38816(10) 0.1318(5) 0.29357(12) 0.0300(5) Uani 1 1 d . . .
C10 C 0.38094(10) 0.0726(5) 0.34803(13) 0.0316(6) Uani 1 1 d . . .
C11 C 0.41990(11) 0.1315(5) 0.41433(13) 0.0378(6) Uani 1 1 d . . .
H11 H 0.4157 0.0913 0.4509 0.045 Uiso 1 1 calc R . .
C12 C 0.46473(11) 0.2496(5) 0.42584(13) 0.0406(7) Uani 1 1 d . . .
H12 H 0.4908 0.2858 0.4707 0.049 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 1.448(2) . ?
S1 O2 1.449(2) . ?
S1 O1 1.451(2) . ?
S1 C1 1.770(3) . ?
S2 O5 1.435(2) . ?
S2 O7 1.4502(19) . ?
S2 O6 1.464(2) . ?
S2 C9 1.771(2) . ?
O1W H1W1 0.849(9) . ?
O1W H1W2 0.851(9) . ?
O1W H1W3 0.846(9) . ?
O2W H2W3 0.867(10) . ?
O2W H2W1 0.864(10) . ?
O2W H2W2 0.872(10) . ?
O4 C2 1.361(3) . ?
O4 H4O 0.845(10) . ?
O8 C10 1.363(3) . ?
O8 H8O 0.841(10) . ?
C1 C6 1.383(4) . ?
C1 C2 1.394(4) . ?
C2 C3 1.394(4) . ?
C3 C4 1.384(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(4) . ?
C5 C7 1.482(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.394(4) . ?
C7 C12 1.398(4) . ?
C8 C9 1.386(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.400(3) . ?
C10 C11 1.385(4) . ?
C11 C12 1.373(4) . ?
C11 H11 0.9300 . ?
C12 H12 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 O2 111.78(13) . . ?
O3 S1 O1 112.08(13) . . ?
O2 S1 O1 112.56(12) . . ?
O3 S1 C1 108.57(12) . . ?
O2 S1 C1 105.66(12) . . ?
O1 S1 C1 105.73(12) . . ?
O5 S2 O7 114.40(13) . . ?
O5 S2 O6 111.79(13) . . ?
O7 S2 O6 111.04(12) . . ?
O5 S2 C9 107.32(12) . . ?
O7 S2 C9 106.46(12) . . ?
O6 S2 C9 105.18(12) . . ?
H1W1 O1W H1W2 108.2(15) . . ?
H1W1 O1W H1W3 110.3(15) . . ?
H1W2 O1W H1W3 110.2(15) . . ?
H2W3 O2W H2W1 108.0(16) . . ?
H2W3 O2W H2W2 106.0(15) . . ?
H2W1 O2W H2W2 106.5(15) . . ?
C2 O4 H4O 115(3) . . ?
C10 O8 H8O 104(3) . . ?
C6 C1 C2 120.1(2) . . ?
C6 C1 S1 118.6(2) . . ?
C2 C1 S1 121.23(19) . . ?
O4 C2 C3 122.3(2) . . ?
O4 C2 C1 118.7(2) . . ?
C3 C2 C1 119.0(2) . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 121.8(3) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C4 C5 C6 117.5(3) . . ?
C4 C5 C7 122.7(2) . . ?
C6 C5 C7 119.7(3) . . ?
C1 C6 C5 121.6(3) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C8 C7 C12 117.4(2) . . ?
C8 C7 C5 121.8(2) . . ?
C12 C7 C5 120.8(2) . . ?
C9 C8 C7 121.2(2) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 119.9(2) . . ?
C8 C9 S2 120.65(19) . . ?
C10 C9 S2 119.43(19) . . ?
O8 C10 C11 122.0(2) . . ?
O8 C10 C9 118.5(2) . . ?
C11 C10 C9 119.5(2) . . ?
C12 C11 C10 119.8(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C7 122.2(2) . . ?
C11 C12 H12 118.9 . . ?
C7 C12 H12 118.9 . . ?

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
O3 S1 C1 C6 130.6(2) . . . . ?
O2 S1 C1 C6 -109.4(2) . . . . ?
O1 S1 C1 C6 10.1(3) . . . . ?
O3 S1 C1 C2 -53.1(3) . . . . ?
O2 S1 C1 C2 66.9(3) . . . . ?
O1 S1 C1 C2 -173.6(2) . . . . ?
C6 C1 C2 O4 179.5(3) . . . . ?
S1 C1 C2 O4 3.3(4) . . . . ?
C6 C1 C2 C3 -0.2(4) . . . . ?
S1 C1 C2 C3 -176.5(2) . . . . ?
O4 C2 C3 C4 -179.0(3) . . . . ?
C1 C2 C3 C4 0.7(5) . . . . ?
C2 C3 C4 C5 -0.6(6) . . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?
C3 C4 C5 C7 176.9(3) . . . . ?
C2 C1 C6 C5 -0.4(4) . . . . ?
S1 C1 C6 C5 176.0(2) . . . . ?
C4 C5 C6 C1 0.5(5) . . . . ?
C7 C5 C6 C1 -176.4(3) . . . . ?
C4 C5 C7 C8 41.0(5) . . . . ?
C6 C5 C7 C8 -142.3(3) . . . . ?
C4 C5 C7 C12 -138.0(3) . . . . ?
C6 C5 C7 C12 38.7(4) . . . . ?
C12 C7 C8 C9 0.2(4) . . . . ?
C5 C7 C8 C9 -178.8(3) . . . . ?
C7 C8 C9 C10 1.6(4) . . . . ?
C7 C8 C9 S2 179.9(2) . . . . ?
O5 S2 C9 C8 125.7(2) . . . . ?
O7 S2 C9 C8 2.8(3) . . . . ?
O6 S2 C9 C8 -115.1(2) . . . . ?
O5 S2 C9 C10 -56.0(3) . . . . ?
O7 S2 C9 C10 -178.9(2) . . . . ?
O6 S2 C9 C10 63.2(2) . . . . ?
C8 C9 C10 O8 175.2(3) . . . . ?
S2 C9 C10 O8 -3.2(4) . . . . ?
C8 C9 C10 C11 -2.1(4) . . . . ?
S2 C9 C10 C11 179.5(2) . . . . ?
O8 C10 C11 C12 -176.4(3) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 C7 1.1(5) . . . . ?
C8 C7 C12 C11 -1.6(5) . . . . ?
C5 C7 C12 C11 177.5(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 O5 0.849(9) 2.155(11) 2.990(3) 168(2) 2_665
O1W H1W2 O6 0.851(9) 2.286(17) 3.034(3) 147(2) 2_655
O1W H1W2 O3 0.851(9) 2.47(2) 3.003(3) 121(2) 7_656
O1W H1W3 O3 0.846(9) 1.945(10) 2.777(3) 167(3) .
O2W H2W3 O6 0.867(10) 2.101(19) 2.879(3) 149(3) 4_545
O2W H2W1 O6 0.864(10) 1.905(10) 2.767(3) 175(4) 1_545
O2W H2W2 O2 0.872(10) 2.007(17) 2.835(3) 158(3) 5_656
O4 H4O O7 0.845(10) 1.885(11) 2.726(3) 173(4) 2_665
O8 H8O O1 0.841(10) 1.838(16) 2.645(3) 161(4) 5_656

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.093
_database_code_depnum_ccdc_archive 'CCDC 1003905'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 4(H2 O)'
_chemical_formula_sum            'C50 H52 N2 O12 S2'
_chemical_formula_weight         937.06

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'
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                   12.9215(9)
_cell_length_b                   13.6231(8)
_cell_length_c                   14.7007(12)
_cell_angle_alpha                93.768(6)
_cell_angle_beta                 101.133(7)
_cell_angle_gamma                110.031(6)
_cell_volume                     2361.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3313
_cell_measurement_theta_min      3.07
_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          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             988
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9619
_exptl_absorpt_correction_T_max  0.9704
_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            14038
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.56
_reflns_number_total             10745
_reflns_number_gt                7197
_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)+(0.0557P)²+0.7760P] 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         10745
_refine_ls_number_parameters     643
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1475
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.38244(6) 0.22521(5) 0.22419(5) 0.04238(17) Uani 1 1 d . . .
S2 S 0.47785(5) 0.92100(4) 0.18643(4) 0.03586(15) Uani 1 1 d . . .
O1 O 0.45268(14) 0.23838(12) 0.15736(12) 0.0430(4) Uani 1 1 d . . .
O1W O 0.1043(5) 0.1596(5) 0.0160(3) 0.200(2) Uani 1 1 d D . .
H1W1 H 0.065(6) 0.097(4) 0.022(8) 0.300 Uiso 1 1 d D . .
H2W1 H 0.173(2) 0.173(7) 0.042(6) 0.300 Uiso 1 1 d D . .
O2 O 0.4253(2) 0.18174(16) 0.30515(15) 0.0735(7) Uani 1 1 d . . .
O2W O 0.1224(2) 0.8590(3) 0.05121(17) 0.0988(9) Uani 1 1 d D . .
H1W2 H 0.0507(12) 0.830(3) 0.025(3) 0.148 Uiso 1 1 d D . .
H2W2 H 0.148(3) 0.915(2) 0.027(3) 0.148 Uiso 1 1 d D . .
O3 O 0.26516(17) 0.16535(16) 0.18601(19) 0.0815(7) Uani 1 1 d . . .
O3W O 0.70460(17) 1.09728(15) 0.07218(13) 0.0559(5) Uani 1 1 d D . .
H1W3 H 0.661(2) 1.083(2) 0.0176(10) 0.084 Uiso 1 1 d D . .
H2W3 H 0.675(2) 1.054(2) 0.1067(15) 0.084 Uiso 1 1 d D . .
O4 O 0.36913(18) 0.30678(15) 0.42303(13) 0.0540(5) Uani 1 1 d D . .
HO4 H 0.380(3) 0.2529(17) 0.400(2) 0.081 Uiso 1 1 d D . .
O4W O 0.63814(18) 0.15661(16) 0.35615(15) 0.0633(6) Uani 1 1 d D . .
H1W4 H 0.5764(16) 0.167(2) 0.353(3) 0.095 Uiso 1 1 d D . .
H2W4 H 0.624(3) 0.0935(12) 0.333(2) 0.095 Uiso 1 1 d D . .
O5 O 0.39921(18) 0.94110(16) 0.11313(12) 0.0602(5) Uani 1 1 d . . .
O6 O 0.43711(14) 0.91097(13) 0.27245(11) 0.0410(4) Uani 1 1 d . . .
O7 O 0.59318(16) 0.99586(13) 0.20275(13) 0.0556(5) Uani 1 1 d . . .
O8 O 0.54904(18) 0.85942(13) 0.01799(12) 0.0529(5) Uani 1 1 d D . .
HO8 H 0.566(3) 0.840(2) -0.0307(14) 0.079 Uiso 1 1 d D . .
N1 N 0.69657(17) 0.25740(16) 0.20092(14) 0.0401(5) Uani 1 1 d D . .
H1N1 H 0.6396(16) 0.2755(19) 0.1788(14) 0.060 Uiso 1 1 d D . .
H1N2 H 0.699(2) 0.2115(16) 0.1592(11) 0.060 Uiso 1 1 d D . .
H1N3 H 0.682(2) 0.2270(17) 0.2491(11) 0.060 Uiso 1 1 d D . .
N2 N 0.22909(17) 0.94249(15) 0.24067(14) 0.0358(4) Uani 1 1 d D . .
H2N1 H 0.2938(11) 0.9347(16) 0.2527(16) 0.054 Uiso 1 1 d D . .
H2N2 H 0.2428(18) 1.0092(8) 0.2380(16) 0.054 Uiso 1 1 d D . .
H2N3 H 0.1927(16) 0.9098(15) 0.1851(10) 0.054 Uiso 1 1 d D . .
C1 C 0.16139(19) 0.90106(17) 0.31276(15) 0.0331(5) Uani 1 1 d . . .
C2 C 0.03913(19) 0.89034(18) 0.27245(16) 0.0367(5) Uani 1 1 d . . .
C3 C 0.0168(2) 0.9715(2) 0.2306(2) 0.0537(7) Uani 1 1 d . . .
H3A H 0.0766 1.0300 0.2236 0.064 Uiso 1 1 calc R . .
C4 C -0.0935(3) 0.9666(3) 0.1992(2) 0.0698(9) Uani 1 1 d . . .
H4A H -0.1073 1.0221 0.1722 0.084 Uiso 1 1 calc R . .
C5 C -0.1825(3) 0.8789(3) 0.2082(2) 0.0722(10) Uani 1 1 d . . .
H5A H -0.2566 0.8750 0.1869 0.087 Uiso 1 1 calc R . .
C6 C -0.1620(2) 0.7979(3) 0.2482(2) 0.0669(9) Uani 1 1 d . . .
H6A H -0.2223 0.7385 0.2532 0.080 Uiso 1 1 calc R . .
C7 C -0.0518(2) 0.8034(2) 0.2815(2) 0.0507(7) Uani 1 1 d . . .
H7A H -0.0387 0.7484 0.3100 0.061 Uiso 1 1 calc R . .
C8 C 0.2148(2) 0.98154(18) 0.40252(16) 0.0361(5) Uani 1 1 d . . .
C9 C 0.1495(2) 1.0130(3) 0.4528(2) 0.0627(8) Uani 1 1 d . . .
H9A H 0.0714 0.9885 0.4305 0.075 Uiso 1 1 calc R . .
C10 C 0.1992(3) 1.0810(3) 0.5366(2) 0.0845(12) Uani 1 1 d . . .
H10A H 0.1541 1.1024 0.5694 0.101 Uiso 1 1 calc R . .
C11 C 0.3130(3) 1.1166(3) 0.5712(2) 0.0707(9) Uani 1 1 d . . .
H11A H 0.3453 1.1609 0.6281 0.085 Uiso 1 1 calc R . .
C12 C 0.3799(2) 1.0870(2) 0.52209(19) 0.0541(7) Uani 1 1 d . . .
H12A H 0.4579 1.1121 0.5451 0.065 Uiso 1 1 calc R . .
C13 C 0.3314(2) 1.01959(19) 0.43807(17) 0.0424(6) Uani 1 1 d . . .
H13A H 0.3772 0.9996 0.4051 0.051 Uiso 1 1 calc R . .
C14 C 0.17255(19) 0.79435(18) 0.32895(17) 0.0360(5) Uani 1 1 d . . .
C15 C 0.2038(2) 0.7705(2) 0.41756(19) 0.0503(7) Uani 1 1 d . . .
H15A H 0.2206 0.8208 0.4696 0.060 Uiso 1 1 calc R . .
C16 C 0.2104(3) 0.6723(2) 0.4300(2) 0.0608(8) Uani 1 1 d . . .
H16A H 0.2321 0.6576 0.4900 0.073 Uiso 1 1 calc R . .
C17 C 0.1853(2) 0.5979(2) 0.3548(2) 0.0568(8) Uani 1 1 d . . .
H17A H 0.1890 0.5321 0.3633 0.068 Uiso 1 1 calc R . .
C18 C 0.1544(3) 0.6201(2) 0.2663(2) 0.0579(8) Uani 1 1 d . . .
H18A H 0.1379 0.5693 0.2148 0.070 Uiso 1 1 calc R . .
C19 C 0.1476(2) 0.71785(19) 0.25298(19) 0.0484(6) Uani 1 1 d . . .
H19A H 0.1261 0.7320 0.1927 0.058 Uiso 1 1 calc R . .
C20 C 0.80466(18) 0.35451(18) 0.22356(16) 0.0351(5) Uani 1 1 d . . .
C21 C 0.80045(19) 0.42789(19) 0.30545(15) 0.0355(5) Uani 1 1 d . . .
C22 C 0.8976(2) 0.4889(2) 0.37031(17) 0.0427(6) Uani 1 1 d . . .
H22A H 0.9650 0.4789 0.3689 0.051 Uiso 1 1 calc R . .
C23 C 0.8972(2) 0.5644(2) 0.43729(18) 0.0495(7) Uani 1 1 d . . .
H23A H 0.9641 0.6048 0.4802 0.059 Uiso 1 1 calc R . .
C24 C 0.7984(2) 0.5802(2) 0.44090(18) 0.0500(7) Uani 1 1 d . . .
H24A H 0.7978 0.6312 0.4859 0.060 Uiso 1 1 calc R . .
C25 C 0.7008(2) 0.5196(2) 0.3770(2) 0.0574(8) Uani 1 1 d . . .
H25A H 0.6333 0.5290 0.3791 0.069 Uiso 1 1 calc R . .
C26 C 0.7021(2) 0.4449(2) 0.30983(18) 0.0512(7) Uani 1 1 d . . .
H26A H 0.6354 0.4052 0.2665 0.061 Uiso 1 1 calc R . .
C27 C 0.8089(2) 0.4104(2) 0.13648(16) 0.0392(6) Uani 1 1 d . . .
C28 C 0.7833(3) 0.3537(2) 0.04795(18) 0.0582(8) Uani 1 1 d . . .
H28A H 0.7620 0.2806 0.0413 0.070 Uiso 1 1 calc R . .
C29 C 0.7891(3) 0.4038(3) -0.0300(2) 0.0702(9) Uani 1 1 d . . .
H29A H 0.7715 0.3641 -0.0885 0.084 Uiso 1 1 calc R . .
C30 C 0.8199(3) 0.5104(3) -0.0229(2) 0.0753(10) Uani 1 1 d . . .
H30A H 0.8235 0.5436 -0.0761 0.090 Uiso 1 1 calc R . .
C31 C 0.8458(4) 0.5684(3) 0.0637(3) 0.0964(14) Uani 1 1 d . . .
H31A H 0.8676 0.6415 0.0695 0.116 Uiso 1 1 calc R . .
C32 C 0.8393(3) 0.5182(2) 0.1422(2) 0.0723(10) Uani 1 1 d . . .
H32A H 0.8558 0.5583 0.2005 0.087 Uiso 1 1 calc R . .
C33 C 0.90157(19) 0.31396(19) 0.25039(17) 0.0384(5) Uani 1 1 d . . .
C34 C 0.9038(2) 0.2562(2) 0.32416(19) 0.0511(7) Uani 1 1 d . . .
H34A H 0.8452 0.2409 0.3554 0.061 Uiso 1 1 calc R . .
C35 C 0.9917(3) 0.2209(2) 0.3523(2) 0.0615(8) Uani 1 1 d . . .
H35A H 0.9913 0.1812 0.4015 0.074 Uiso 1 1 calc R . .
C36 C 1.0797(3) 0.2443(3) 0.3078(3) 0.0678(9) Uani 1 1 d . . .
H36A H 1.1396 0.2218 0.3274 0.081 Uiso 1 1 calc R . .
C37 C 1.0783(3) 0.3006(3) 0.2352(3) 0.0688(9) Uani 1 1 d . . .
H37A H 1.1375 0.3161 0.2046 0.083 Uiso 1 1 calc R . .
C38 C 0.9899(2) 0.3351(2) 0.2059(2) 0.0526(7) Uani 1 1 d . . .
H38A H 0.9901 0.3731 0.1555 0.063 Uiso 1 1 calc R . .
C39 C 0.43640(19) 0.53683(17) 0.24556(15) 0.0327(5) Uani 1 1 d . . .
C40 C 0.4262(2) 0.55770(19) 0.33717(16) 0.0375(5) Uani 1 1 d . . .
H40A H 0.4363 0.6262 0.3608 0.045 Uiso 1 1 calc R . .
C41 C 0.4017(2) 0.4804(2) 0.39294(16) 0.0402(6) Uani 1 1 d . . .
H41A H 0.3938 0.4969 0.4530 0.048 Uiso 1 1 calc R . .
C42 C 0.3885(2) 0.37726(19) 0.36128(16) 0.0365(5) Uani 1 1 d . . .
C43 C 0.39646(18) 0.35376(17) 0.27000(16) 0.0320(5) Uani 1 1 d . . .
C44 C 0.41822(19) 0.43251(17) 0.21318(15) 0.0333(5) Uani 1 1 d . . .
H44A H 0.4207 0.4151 0.1516 0.040 Uiso 1 1 calc R . .
C45 C 0.4678(2) 0.62097(17) 0.18590(16) 0.0356(5) Uani 1 1 d . . .
C46 C 0.5120(2) 0.60873(19) 0.10837(18) 0.0490(7) Uani 1 1 d . . .
H46A H 0.5239 0.5464 0.0945 0.059 Uiso 1 1 calc R . .
C47 C 0.5383(3) 0.6855(2) 0.05199(18) 0.0510(7) Uani 1 1 d . . .
H47A H 0.5660 0.6738 0.0001 0.061 Uiso 1 1 calc R . .
C48 C 0.5241(2) 0.78064(18) 0.07154(16) 0.0392(6) Uani 1 1 d . . .
C49 C 0.48527(19) 0.79697(16) 0.15123(15) 0.0315(5) Uani 1 1 d . . .
C50 C 0.45732(19) 0.71785(17) 0.20660(15) 0.0321(5) Uani 1 1 d . . .
H50A H 0.4307 0.7298 0.2591 0.039 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 1.429(2) . ?
S1 O1 1.4412(17) . ?
S1 O2 1.462(2) . ?
S1 C43 1.770(2) . ?
S2 O5 1.4406(19) . ?
S2 O7 1.4515(18) . ?
S2 O6 1.4579(16) . ?
S2 C49 1.774(2) . ?
O1W H1W1 0.85(5) . ?
O1W H2W1 0.85(5) . ?
O2W H1W2 0.86(5) . ?
O2W H2W2 0.86(5) . ?
O3W H1W3 0.85(5) . ?
O3W H2W3 0.85(5) . ?
O4 C42 1.359(3) . ?
O4 HO4 0.85(5) . ?
O4W H1W4 0.85(5) . ?
O4W H2W4 0.85(5) . ?
O8 C48 1.359(3) . ?
O8 HO8 0.85(5) . ?
N1 C20 1.519(3) . ?
N1 H1N1 0.87(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
N2 C1 1.518(3) . ?
N2 H2N1 0.87(3) . ?
N2 H2N2 0.87(3) . ?
N2 H2N3 0.86(3) . ?
C1 C2 1.529(3) . ?
C1 C8 1.536(3) . ?
C1 C14 1.538(3) . ?
C2 C3 1.386(4) . ?
C2 C7 1.389(3) . ?
C3 C4 1.388(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.381(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.363(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.388(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.374(4) . ?
C8 C13 1.391(3) . ?
C9 C10 1.387(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.359(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.367(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.385(3) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.381(3) . ?
C14 C19 1.384(3) . ?
C15 C16 1.391(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.358(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.370(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.388(4) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C33 1.530(3) . ?
C20 C27 1.533(3) . ?
C20 C21 1.535(3) . ?
C21 C22 1.376(3) . ?
C21 C26 1.380(3) . ?
C22 C23 1.379(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.376(4) . ?
C23 H23A 0.9300 . ?
C24 C25 1.372(4) . ?
C24 H24A 0.9300 . ?
C25 C26 1.377(4) . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9300 . ?
C27 C32 1.376(4) . ?
C27 C28 1.388(3) . ?
C28 C29 1.373(4) . ?
C28 H28A 0.9300 . ?
C29 C30 1.359(5) . ?
C29 H29A 0.9300 . ?
C30 C31 1.371(5) . ?
C30 H30A 0.9300 . ?
C31 C32 1.382(4) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
C33 C38 1.379(3) . ?
C33 C34 1.382(4) . ?
C34 C35 1.383(4) . ?
C34 H34A 0.9300 . ?
C35 C36 1.374(4) . ?
C35 H35A 0.9300 . ?
C36 C37 1.356(5) . ?
C36 H36A 0.9300 . ?
C37 C38 1.384(4) . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9300 . ?
C39 C44 1.393(3) . ?
C39 C40 1.399(3) . ?
C39 C45 1.483(3) . ?
C40 C41 1.367(3) . ?
C40 H40A 0.9300 . ?
C41 C42 1.392(3) . ?
C41 H41A 0.9300 . ?
C42 C43 1.390(3) . ?
C43 C44 1.389(3) . ?
C44 H44A 0.9300 . ?
C45 C50 1.392(3) . ?
C45 C46 1.394(3) . ?
C46 C47 1.369(3) . ?
C46 H46A 0.9300 . ?
C47 C48 1.390(3) . ?
C47 H47A 0.9300 . ?
C48 C49 1.394(3) . ?
C49 C50 1.385(3) . ?
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
O3 S1 O1 114.65(13) . . ?
O3 S1 O2 110.36(15) . . ?
O1 S1 O2 111.71(12) . . ?
O3 S1 C43 108.52(12) . . ?
O1 S1 C43 106.32(10) . . ?
O2 S1 C43 104.66(12) . . ?
O5 S2 O7 114.09(13) . . ?
O5 S2 O6 111.13(11) . . ?
O7 S2 O6 111.89(11) . . ?
O5 S2 C49 108.04(11) . . ?
O7 S2 C49 105.07(11) . . ?
O6 S2 C49 106.04(10) . . ?
H1W1 O1W H2W1 109.4(18) . . ?
H1W2 O2W H2W2 106.3(16) . . ?
H1W3 O3W H2W3 109.9(16) . . ?
C42 O4 HO4 107(2) . . ?
H1W4 O4W H2W4 109.4(16) . . ?
C48 O8 HO8 111(2) . . ?
C20 N1 H1N1 109.3(17) . . ?
C20 N1 H1N2 111.2(17) . . ?
H1N1 N1 H1N2 107.8(14) . . ?
C20 N1 H1N3 113.6(17) . . ?
H1N1 N1 H1N3 106.5(13) . . ?
H1N2 N1 H1N3 108.3(14) . . ?
C1 N2 H2N1 111.6(16) . . ?
C1 N2 H2N2 112.7(16) . . ?
H2N1 N2 H2N2 106.9(13) . . ?
C1 N2 H2N3 110.9(16) . . ?
H2N1 N2 H2N3 108.1(14) . . ?
H2N2 N2 H2N3 106.3(13) . . ?
N2 C1 C2 107.52(18) . . ?
N2 C1 C8 107.25(17) . . ?
C2 C1 C8 111.71(18) . . ?
N2 C1 C14 106.40(18) . . ?
C2 C1 C14 112.53(18) . . ?
C8 C1 C14 111.08(19) . . ?
C3 C2 C7 118.3(2) . . ?
C3 C2 C1 120.0(2) . . ?
C7 C2 C1 121.6(2) . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C7 120.5(3) . . ?
C5 C6 H6A 119.8 . . ?
C7 C6 H6A 119.8 . . ?
C6 C7 C2 120.4(3) . . ?
C6 C7 H7A 119.8 . . ?
C2 C7 H7A 119.8 . . ?
C9 C8 C13 118.2(2) . . ?
C9 C8 C1 121.5(2) . . ?
C13 C8 C1 120.2(2) . . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C10 C11 C12 119.8(3) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C11 C12 C13 120.0(3) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C12 C13 C8 120.7(3) . . ?
C12 C13 H13A 119.7 . . ?
C8 C13 H13A 119.7 . . ?
C15 C14 C19 118.3(2) . . ?
C15 C14 C1 122.2(2) . . ?
C19 C14 C1 119.5(2) . . ?
C14 C15 C16 120.8(3) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C17 C16 C15 120.3(3) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C16 C17 C18 119.9(3) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C17 C18 C19 120.4(3) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C14 C19 C18 120.4(3) . . ?
C14 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
N1 C20 C33 105.90(19) . . ?
N1 C20 C27 107.64(18) . . ?
C33 C20 C27 113.5(2) . . ?
N1 C20 C21 108.65(17) . . ?
C33 C20 C21 111.32(18) . . ?
C27 C20 C21 109.60(19) . . ?
C22 C21 C26 117.6(2) . . ?
C22 C21 C20 120.9(2) . . ?
C26 C21 C20 121.0(2) . . ?
C21 C22 C23 121.5(2) . . ?
C21 C22 H22A 119.3 . . ?
C23 C22 H22A 119.3 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23A 119.9 . . ?
C22 C23 H23A 119.9 . . ?
C25 C24 C23 118.9(2) . . ?
C25 C24 H24A 120.6 . . ?
C23 C24 H24A 120.6 . . ?
C24 C25 C26 120.4(2) . . ?
C24 C25 H25A 119.8 . . ?
C26 C25 H25A 119.8 . . ?
C25 C26 C21 121.4(2) . . ?
C25 C26 H26A 119.3 . . ?
C21 C26 H26A 119.3 . . ?
C32 C27 C28 117.1(2) . . ?
C32 C27 C20 122.0(2) . . ?
C28 C27 C20 120.9(2) . . ?
C29 C28 C27 121.0(3) . . ?
C29 C28 H28A 119.5 . . ?
C27 C28 H28A 119.5 . . ?
C30 C29 C28 121.1(3) . . ?
C30 C29 H29A 119.4 . . ?
C28 C29 H29A 119.4 . . ?
C29 C30 C31 119.2(3) . . ?
C29 C30 H30A 120.4 . . ?
C31 C30 H30A 120.4 . . ?
C30 C31 C32 119.9(3) . . ?
C30 C31 H31A 120.0 . . ?
C32 C31 H31A 120.0 . . ?
C27 C32 C31 121.7(3) . . ?
C27 C32 H32A 119.2 . . ?
C31 C32 H32A 119.2 . . ?
C38 C33 C34 117.8(2) . . ?
C38 C33 C20 122.8(2) . . ?
C34 C33 C20 119.3(2) . . ?
C33 C34 C35 121.1(3) . . ?
C33 C34 H34A 119.5 . . ?
C35 C34 H34A 119.5 . . ?
C36 C35 C34 120.1(3) . . ?
C36 C35 H35A 120.0 . . ?
C34 C35 H35A 120.0 . . ?
C37 C36 C35 119.4(3) . . ?
C37 C36 H36A 120.3 . . ?
C35 C36 H36A 120.3 . . ?
C36 C37 C38 120.8(3) . . ?
C36 C37 H37A 119.6 . . ?
C38 C37 H37A 119.6 . . ?
C33 C38 C37 120.8(3) . . ?
C33 C38 H38A 119.6 . . ?
C37 C38 H38A 119.6 . . ?
C44 C39 C40 116.6(2) . . ?
C44 C39 C45 121.0(2) . . ?
C40 C39 C45 122.4(2) . . ?
C41 C40 C39 121.9(2) . . ?
C41 C40 H40A 119.0 . . ?
C39 C40 H40A 119.0 . . ?
C40 C41 C42 121.0(2) . . ?
C40 C41 H41A 119.5 . . ?
C42 C41 H41A 119.5 . . ?
O4 C42 C43 124.8(2) . . ?
O4 C42 C41 116.8(2) . . ?
C43 C42 C41 118.3(2) . . ?
C44 C43 C42 120.0(2) . . ?
C44 C43 S1 118.50(17) . . ?
C42 C43 S1 121.48(17) . . ?
C43 C44 C39 122.0(2) . . ?
C43 C44 H44A 119.0 . . ?
C39 C44 H44A 119.0 . . ?
C50 C45 C46 116.7(2) . . ?
C50 C45 C39 121.1(2) . . ?
C46 C45 C39 122.2(2) . . ?
C47 C46 C45 122.1(2) . . ?
C47 C46 H46A 118.9 . . ?
C45 C46 H46A 118.9 . . ?
C46 C47 C48 120.7(2) . . ?
C46 C47 H47A 119.6 . . ?
C48 C47 H47A 119.6 . . ?
O8 C48 C47 123.1(2) . . ?
O8 C48 C49 118.6(2) . . ?
C47 C48 C49 118.3(2) . . ?
C50 C49 C48 120.1(2) . . ?
C50 C49 S2 119.09(17) . . ?
C48 C49 S2 120.69(17) . . ?
C49 C50 C45 121.9(2) . . ?
C49 C50 H50A 119.0 . . ?
C45 C50 H50A 119.0 . . ?

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
N2 C1 C2 C3 -46.0(3) . . . . ?
C8 C1 C2 C3 71.4(3) . . . . ?
C14 C1 C2 C3 -162.8(2) . . . . ?
N2 C1 C2 C7 138.0(2) . . . . ?
C8 C1 C2 C7 -104.6(2) . . . . ?
C14 C1 C2 C7 21.1(3) . . . . ?
C7 C2 C3 C4 0.5(4) . . . . ?
C1 C2 C3 C4 -175.7(2) . . . . ?
C2 C3 C4 C5 -1.1(5) . . . . ?
C3 C4 C5 C6 0.3(5) . . . . ?
C4 C5 C6 C7 1.0(5) . . . . ?
C5 C6 C7 C2 -1.6(4) . . . . ?
C3 C2 C7 C6 0.8(4) . . . . ?
C1 C2 C7 C6 176.9(2) . . . . ?
N2 C1 C8 C9 135.7(3) . . . . ?
C2 C1 C8 C9 18.2(3) . . . . ?
C14 C1 C8 C9 -108.4(3) . . . . ?
N2 C1 C8 C13 -48.3(3) . . . . ?
C2 C1 C8 C13 -165.8(2) . . . . ?
C14 C1 C8 C13 67.6(3) . . . . ?
C13 C8 C9 C10 0.1(5) . . . . ?
C1 C8 C9 C10 176.2(3) . . . . ?
C8 C9 C10 C11 -0.9(6) . . . . ?
C9 C10 C11 C12 1.4(6) . . . . ?
C10 C11 C12 C13 -1.0(5) . . . . ?
C11 C12 C13 C8 0.2(4) . . . . ?
C9 C8 C13 C12 0.3(4) . . . . ?
C1 C8 C13 C12 -175.9(2) . . . . ?
N2 C1 C14 C15 129.6(2) . . . . ?
C2 C1 C14 C15 -112.9(3) . . . . ?
C8 C1 C14 C15 13.1(3) . . . . ?
N2 C1 C14 C19 -52.3(3) . . . . ?
C2 C1 C14 C19 65.2(3) . . . . ?
C8 C1 C14 C19 -168.7(2) . . . . ?
C19 C14 C15 C16 0.2(4) . . . . ?
C1 C14 C15 C16 178.4(2) . . . . ?
C14 C15 C16 C17 -0.5(4) . . . . ?
C15 C16 C17 C18 0.6(4) . . . . ?
C16 C17 C18 C19 -0.6(4) . . . . ?
C15 C14 C19 C18 -0.2(4) . . . . ?
C1 C14 C19 C18 -178.4(2) . . . . ?
C17 C18 C19 C14 0.4(4) . . . . ?
N1 C20 C21 C22 146.7(2) . . . . ?
C33 C20 C21 C22 30.5(3) . . . . ?
C27 C20 C21 C22 -95.9(3) . . . . ?
N1 C20 C21 C26 -41.6(3) . . . . ?
C33 C20 C21 C26 -157.8(2) . . . . ?
C27 C20 C21 C26 75.8(3) . . . . ?
C26 C21 C22 C23 -0.1(4) . . . . ?
C20 C21 C22 C23 171.9(2) . . . . ?
C21 C22 C23 C24 0.3(4) . . . . ?
C22 C23 C24 C25 0.1(4) . . . . ?
C23 C24 C25 C26 -0.7(5) . . . . ?
C24 C25 C26 C21 0.9(5) . . . . ?
C22 C21 C26 C25 -0.5(4) . . . . ?
C20 C21 C26 C25 -172.5(3) . . . . ?
N1 C20 C27 C32 136.0(3) . . . . ?
C33 C20 C27 C32 -107.2(3) . . . . ?
C21 C20 C27 C32 18.0(3) . . . . ?
N1 C20 C27 C28 -44.8(3) . . . . ?
C33 C20 C27 C28 72.0(3) . . . . ?
C21 C20 C27 C28 -162.8(2) . . . . ?
C32 C27 C28 C29 0.4(5) . . . . ?
C20 C27 C28 C29 -178.8(3) . . . . ?
C27 C28 C29 C30 0.0(5) . . . . ?
C28 C29 C30 C31 0.0(6) . . . . ?
C29 C30 C31 C32 -0.5(6) . . . . ?
C28 C27 C32 C31 -0.9(5) . . . . ?
C20 C27 C32 C31 178.3(3) . . . . ?
C30 C31 C32 C27 1.0(7) . . . . ?
N1 C20 C33 C38 123.9(2) . . . . ?
C27 C20 C33 C38 6.1(3) . . . . ?
C21 C20 C33 C38 -118.2(2) . . . . ?
N1 C20 C33 C34 -58.1(3) . . . . ?
C27 C20 C33 C34 -176.0(2) . . . . ?
C21 C20 C33 C34 59.8(3) . . . . ?
C38 C33 C34 C35 0.0(4) . . . . ?
C20 C33 C34 C35 -178.1(2) . . . . ?
C33 C34 C35 C36 1.0(4) . . . . ?
C34 C35 C36 C37 -1.2(5) . . . . ?
C35 C36 C37 C38 0.4(5) . . . . ?
C34 C33 C38 C37 -0.8(4) . . . . ?
C20 C33 C38 C37 177.2(2) . . . . ?
C36 C37 C38 C33 0.6(5) . . . . ?
C44 C39 C40 C41 1.2(3) . . . . ?
C45 C39 C40 C41 -177.2(2) . . . . ?
C39 C40 C41 C42 1.5(4) . . . . ?
C40 C41 C42 O4 177.2(2) . . . . ?
C40 C41 C42 C43 -2.4(4) . . . . ?
O4 C42 C43 C44 -179.0(2) . . . . ?
C41 C42 C43 C44 0.6(3) . . . . ?
O4 C42 C43 S1 -0.4(3) . . . . ?
C41 C42 C43 S1 179.24(18) . . . . ?
O3 S1 C43 C44 -94.0(2) . . . . ?
O1 S1 C43 C44 29.8(2) . . . . ?
O2 S1 C43 C44 148.18(19) . . . . ?
O3 S1 C43 C42 87.4(2) . . . . ?
O1 S1 C43 C42 -148.83(19) . . . . ?
O2 S1 C43 C42 -30.5(2) . . . . ?
C42 C43 C44 C39 2.2(3) . . . . ?
S1 C43 C44 C39 -176.49(17) . . . . ?
C40 C39 C44 C43 -3.0(3) . . . . ?
C45 C39 C44 C43 175.4(2) . . . . ?
C44 C39 C45 C50 163.0(2) . . . . ?
C40 C39 C45 C50 -18.6(4) . . . . ?
C44 C39 C45 C46 -18.8(4) . . . . ?
C40 C39 C45 C46 159.6(2) . . . . ?
C50 C45 C46 C47 -3.4(4) . . . . ?
C39 C45 C46 C47 178.3(3) . . . . ?
C45 C46 C47 C48 1.4(5) . . . . ?
C46 C47 C48 O8 179.9(3) . . . . ?
C46 C47 C48 C49 1.7(4) . . . . ?
O8 C48 C49 C50 179.0(2) . . . . ?
C47 C48 C49 C50 -2.7(4) . . . . ?
O8 C48 C49 S2 -4.3(3) . . . . ?
C47 C48 C49 S2 174.0(2) . . . . ?
O5 S2 C49 C50 -121.0(2) . . . . ?
O7 S2 C49 C50 116.88(19) . . . . ?
O6 S2 C49 C50 -1.7(2) . . . . ?
O5 S2 C49 C48 62.2(2) . . . . ?
O7 S2 C49 C48 -59.9(2) . . . . ?
O6 S2 C49 C48 -178.55(19) . . . . ?
C48 C49 C50 C45 0.7(4) . . . . ?
S2 C49 C50 C45 -176.10(17) . . . . ?
C46 C45 C50 C49 2.3(3) . . . . ?
C39 C45 C50 C49 -179.4(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 H2W1 O3 0.85(5) 2.24(7) 2.904(5) 135(8) .
O2W H1W2 O1W 0.86(5) 2.03(3) 2.822(6) 151(4) 2_565
O2W H2W2 O3W 0.86(5) 2.66(5) 3.072(4) 111(4) 2_675
O3W H1W3 O5 0.85(5) 1.891(11) 2.723(3) 165(3) 2_675
O3W H2W3 O7 0.85(5) 1.971(15) 2.778(3) 160(3) .
O4 HO4 O2 0.85(5) 1.944(19) 2.716(3) 151(3) .
O4W H1W4 O2 0.85(5) 2.025(15) 2.851(3) 164(4) .
O4W H2W4 O7 0.85(5) 2.15(2) 2.862(3) 142(3) 1_545
O8 HO8 O1 0.85(5) 2.010(15) 2.815(2) 159(3) 2_665
N1 H1N1 O1 0.87(3) 2.244(17) 3.008(3) 147(2) .
N1 H1N2 O3W 0.86(3) 1.979(10) 2.835(3) 175(2) 1_545
N1 H1N3 O4W 0.86(3) 1.971(10) 2.834(3) 176(2) .
N2 H2N1 O6 0.87(3) 1.958(9) 2.821(3) 176(2) .
N2 H2N2 O3 0.87(3) 2.252(12) 3.095(3) 163(2) 1_565
N2 H2N3 O2W 0.86(3) 1.970(11) 2.825(3) 170(2) .

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.049
_database_code_depnum_ccdc_archive 'CCDC 1025993'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 2(H2 O), H2 O'
_chemical_formula_sum            'C50 H50 N2 O11 S2'
_chemical_formula_weight         919.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   27.0976(12)
_cell_length_b                   12.9962(4)
_cell_length_c                   13.9750(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.679(5)
_cell_angle_gamma                90.00
_cell_volume                     4781.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1890
_cell_measurement_theta_min      3.47
_cell_measurement_theta_max      27.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9581
_exptl_absorpt_correction_T_max  0.9695
_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            8515
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.56
_reflns_number_total             5476
_reflns_number_gt                3677
_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)+(0.0852P)²+6.2570P] 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         5476
_refine_ls_number_parameters     313
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0660
_refine_ls_wR_factor_ref         0.1906
_refine_ls_wR_factor_gt          0.1652
_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 0.46286(3) 0.65582(5) 0.01555(6) 0.0420(2) Uani 1 1 d . . .
O1 O 0.48616(10) 0.62485(18) 0.11389(19) 0.0749(7) Uani 1 1 d . . .
O1W O 0.43872(10) 0.48262(19) 0.27638(16) 0.0638(6) Uani 1 1 d D . .
H1W H 0.4608(12) 0.531(2) 0.289(3) 0.096 Uiso 1 1 d D . .
H2W H 0.4468(14) 0.437(2) 0.322(2) 0.096 Uiso 1 1 d D . .
O2 O 0.49445(9) 0.64396(15) -0.0541(2) 0.0658(7) Uani 1 1 d . . .
O3 O 0.41344(7) 0.60587(14) -0.02082(17) 0.0527(5) Uani 1 1 d . . .
O4 O 0.36591(8) 0.76277(16) 0.0487(2) 0.0627(7) Uani 1 1 d D . .
H4O H 0.3703(16) 0.7043(16) 0.025(3) 0.094 Uiso 1 1 d D . .
N1 N 0.41121(8) 0.41795(16) 0.08343(17) 0.0372(5) Uani 1 1 d D . .
H1N1 H 0.4116(10) 0.4744(12) 0.0501(15) 0.056 Uiso 1 1 d D . .
H1N2 H 0.4182(10) 0.4367(18) 0.1453(8) 0.056 Uiso 1 1 d D . .
H1N3 H 0.4362(8) 0.3807(16) 0.0755(17) 0.056 Uiso 1 1 d D . .
C1 C 0.36091(10) 0.36077(19) 0.05609(19) 0.0375(6) Uani 1 1 d . . .
C2 C 0.35697(15) 0.2917(2) 0.1423(2) 0.0565(8) Uani 1 1 d . . .
C3 C 0.31130(19) 0.2855(4) 0.1724(3) 0.0937(15) Uani 1 1 d . . .
H3A H 0.2840 0.3272 0.1433 0.112 Uiso 1 1 calc R . .
C4 C 0.3071(4) 0.2168(6) 0.2459(5) 0.0977(15) Uani 1 1 d . . .
H4A H 0.2767 0.2128 0.2658 0.188 Uiso 1 1 calc R . .
C5 C 0.3463(5) 0.1554(6) 0.2894(5) 0.0837(6) Uani 1 1 d . . .
H5A H 0.3428 0.1088 0.3378 0.226 Uiso 1 1 calc R . .
C6 C 0.3906(4) 0.1623(4) 0.2617(4) 0.0815(5) Uani 1 1 d . . .
H6A H 0.4177 0.1210 0.2927 0.175 Uiso 1 1 calc R . .
C7 C 0.3970(2) 0.2310(3) 0.1868(3) 0.0864(13) Uani 1 1 d . . .
H7A H 0.4278 0.2347 0.1683 0.104 Uiso 1 1 calc R . .
C8 C 0.35995(10) 0.2956(2) -0.03574(19) 0.0389(6) Uani 1 1 d . . .
C9 C 0.38401(13) 0.3283(3) -0.1074(2) 0.0566(8) Uani 1 1 d . . .
H9A H 0.4018 0.3901 -0.0991 0.068 Uiso 1 1 calc R . .
C10 C 0.38199(16) 0.2703(3) -0.1914(3) 0.0738(11) Uani 1 1 d . . .
H10A H 0.3989 0.2925 -0.2383 0.089 Uiso 1 1 calc R . .
C11 C 0.35506(16) 0.1798(3) -0.2052(3) 0.0745(11) Uani 1 1 d . . .
H11A H 0.3534 0.1411 -0.2618 0.089 Uiso 1 1 calc R . .
C12 C 0.33074(16) 0.1467(3) -0.1356(3) 0.0717(10) Uani 1 1 d . . .
H12A H 0.3126 0.0854 -0.1451 0.086 Uiso 1 1 calc R . .
C13 C 0.33290(13) 0.2037(2) -0.0511(2) 0.0546(8) Uani 1 1 d . . .
H13A H 0.3162 0.1805 -0.0044 0.065 Uiso 1 1 calc R . .
C14 C 0.31974(10) 0.4445(2) 0.0367(2) 0.0459(7) Uani 1 1 d . . .
C15 C 0.31957(12) 0.5197(3) 0.1075(3) 0.0690(10) Uani 1 1 d . . .
H15A H 0.3442 0.5182 0.1664 0.083 Uiso 1 1 calc R . .
C16 C 0.28331(15) 0.5967(3) 0.0915(4) 0.0925(15) Uani 1 1 d . . .
H16A H 0.2840 0.6466 0.1394 0.111 Uiso 1 1 calc R . .
C17 C 0.24713(16) 0.5997(3) 0.0071(5) 0.1015(17) Uani 1 1 d . . .
H17A H 0.2229 0.6518 -0.0036 0.122 Uiso 1 1 calc R . .
C18 C 0.24617(16) 0.5266(4) -0.0625(4) 0.0968(15) Uani 1 1 d . . .
H18A H 0.2207 0.5281 -0.1202 0.116 Uiso 1 1 calc R . .
C19 C 0.28288(13) 0.4491(3) -0.0488(3) 0.0680(10) Uani 1 1 d . . .
H19A H 0.2822 0.4006 -0.0980 0.082 Uiso 1 1 calc R . .
C20 C 0.44963(10) 0.78852(18) 0.0177(2) 0.0378(6) Uani 1 1 d . . .
C21 C 0.40420(11) 0.8251(2) 0.0362(2) 0.0465(7) Uani 1 1 d . . .
C22 C 0.39742(12) 0.9302(2) 0.0410(3) 0.0629(10) Uani 1 1 d . . .
H22A H 0.3676 0.9558 0.0539 0.075 Uiso 1 1 calc R . .
C23 C 0.43430(12) 0.9974(2) 0.0269(3) 0.0577(9) Uani 1 1 d . . .
H23A H 0.4286 1.0678 0.0304 0.069 Uiso 1 1 calc R . .
C24 C 0.48006(10) 0.96389(19) 0.0075(2) 0.0419(6) Uani 1 1 d . . .
C25 C 0.48653(10) 0.85748(19) 0.0040(2) 0.0411(6) Uani 1 1 d . . .
H25A H 0.5166 0.8319 -0.0080 0.049 Uiso 1 1 calc R . .
O2W O 0.5000 -0.0947(19) 0.2500 0.209(7) Uani 0.50 2 d SP A 1
O2W' O 0.5000 0.0572(19) 0.2500 0.209(7) Uani 0.50 2 d SP 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 O1 1.428(2) . ?
S1 O2 1.448(2) . ?
S1 O3 1.467(2) . ?
S1 C20 1.763(2) . ?
O1W H1W 0.85(3) . ?
O1W H2W 0.85(3) . ?
O4 C21 1.360(3) . ?
O4 H4O 0.85(3) . ?
N1 C1 1.520(3) . ?
N1 H1N1 0.87(3) . ?
N1 H1N2 0.87(3) . ?
N1 H1N3 0.86(3) . ?
C1 C2 1.527(4) . ?
C1 C8 1.533(4) . ?
C1 C14 1.536(4) . ?
C2 C7 1.366(6) . ?
C2 C3 1.400(6) . ?
C3 C4 1.387(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.353(13) . ?
C4 H4A 0.9300 . ?
C5 C6 1.348(13) . ?
C5 H5A 0.9300 . ?
C6 C7 1.417(7) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.385(4) . ?
C8 C13 1.391(4) . ?
C9 C10 1.385(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.373(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.367(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.383(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C19 1.365(5) . ?
C14 C15 1.392(4) . ?
C15 C16 1.383(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.344(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.355(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.397(5) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C25 1.390(3) . ?
C20 C21 1.399(4) . ?
C21 C22 1.382(4) . ?
C22 C23 1.376(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.400(4) . ?
C23 H23A 0.9300 . ?
C24 C25 1.396(3) . ?
C24 C24 1.484(5) 5_675 ?
C25 H25A 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 114.81(16) . . ?
O1 S1 O3 111.62(14) . . ?
O2 S1 O3 110.88(14) . . ?
O1 S1 C20 107.73(14) . . ?
O2 S1 C20 105.70(12) . . ?
O3 S1 C20 105.43(12) . . ?
H1W O1W H2W 108.0(16) . . ?
C21 O4 H4O 108(3) . . ?
C1 N1 H1N1 113.7(18) . . ?
C1 N1 H1N2 110.9(18) . . ?
H1N1 N1 H1N2 105.5(14) . . ?
C1 N1 H1N3 112.3(19) . . ?
H1N1 N1 H1N3 107.2(14) . . ?
H1N2 N1 H1N3 106.9(14) . . ?
N1 C1 C2 108.4(2) . . ?
N1 C1 C8 108.5(2) . . ?
C2 C1 C8 110.2(2) . . ?
N1 C1 C14 105.6(2) . . ?
C2 C1 C14 111.9(2) . . ?
C8 C1 C14 112.1(2) . . ?
C7 C2 C3 119.6(4) . . ?
C7 C2 C1 120.1(3) . . ?
C3 C2 C1 120.2(3) . . ?
C4 C3 C2 119.5(6) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C5 C4 C3 121.2(8) . . ?
C5 C4 H4A 119.4 . . ?
C3 C4 H4A 119.4 . . ?
C6 C5 C4 119.4(6) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C5 C6 C7 121.8(7) . . ?
C5 C6 H6A 119.1 . . ?
C7 C6 H6A 119.1 . . ?
C2 C7 C6 118.5(6) . . ?
C2 C7 H7A 120.8 . . ?
C6 C7 H7A 120.8 . . ?
C9 C8 C13 118.2(3) . . ?
C9 C8 C1 121.2(2) . . ?
C13 C8 C1 120.5(2) . . ?
C10 C9 C8 121.0(3) . . ?
C10 C9 H9A 119.5 . . ?
C8 C9 H9A 119.5 . . ?
C11 C10 C9 119.9(3) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C12 C11 C10 119.9(3) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C12 C13 C8 120.4(3) . . ?
C12 C13 H13A 119.8 . . ?
C8 C13 H13A 119.8 . . ?
C19 C14 C15 117.8(3) . . ?
C19 C14 C1 122.4(3) . . ?
C15 C14 C1 119.8(3) . . ?
C16 C15 C14 121.0(4) . . ?
C16 C15 H15A 119.5 . . ?
C14 C15 H15A 119.5 . . ?
C17 C16 C15 120.4(4) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C16 C17 C18 119.7(4) . . ?
C16 C17 H17A 120.2 . . ?
C18 C17 H17A 120.2 . . ?
C17 C18 C19 121.0(4) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C14 C19 C18 120.1(4) . . ?
C14 C19 H19A 120.0 . . ?
C18 C19 H19A 120.0 . . ?
C25 C20 C21 120.0(2) . . ?
C25 C20 S1 118.20(19) . . ?
C21 C20 S1 121.80(19) . . ?
O4 C21 C22 117.9(2) . . ?
O4 C21 C20 123.5(2) . . ?
C22 C21 C20 118.5(2) . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 H22A 119.6 . . ?
C21 C22 H22A 119.6 . . ?
C22 C23 C24 122.4(3) . . ?
C22 C23 H23A 118.8 . . ?
C24 C23 H23A 118.8 . . ?
C25 C24 C23 116.1(2) . . ?
C25 C24 C24 121.3(3) . 5_675 ?
C23 C24 C24 122.6(3) . 5_675 ?
C20 C25 C24 122.2(2) . . ?
C20 C25 H25A 118.9 . . ?
C24 C25 H25A 118.9 . . ?

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
N1 C1 C2 C7 -47.1(4) . . . . ?
C8 C1 C2 C7 71.5(4) . . . . ?
C14 C1 C2 C7 -163.1(3) . . . . ?
N1 C1 C2 C3 136.8(3) . . . . ?
C8 C1 C2 C3 -104.6(3) . . . . ?
C14 C1 C2 C3 20.8(4) . . . . ?
C7 C2 C3 C4 -1.0(6) . . . . ?
C1 C2 C3 C4 175.2(4) . . . . ?
C2 C3 C4 C5 0.0(9) . . . . ?
C3 C4 C5 C6 1.1(12) . . . . ?
C4 C5 C6 C7 -1.3(11) . . . . ?
C3 C2 C7 C6 0.8(6) . . . . ?
C1 C2 C7 C6 -175.4(3) . . . . ?
C5 C6 C7 C2 0.3(8) . . . . ?
N1 C1 C8 C9 -33.0(3) . . . . ?
C2 C1 C8 C9 -151.5(3) . . . . ?
C14 C1 C8 C9 83.2(3) . . . . ?
N1 C1 C8 C13 149.8(3) . . . . ?
C2 C1 C8 C13 31.3(4) . . . . ?
C14 C1 C8 C13 -94.0(3) . . . . ?
C13 C8 C9 C10 -1.2(5) . . . . ?
C1 C8 C9 C10 -178.4(3) . . . . ?
C8 C9 C10 C11 1.2(6) . . . . ?
C9 C10 C11 C12 -0.7(6) . . . . ?
C10 C11 C12 C13 0.1(6) . . . . ?
C11 C12 C13 C8 -0.1(6) . . . . ?
C9 C8 C13 C12 0.6(5) . . . . ?
C1 C8 C13 C12 177.9(3) . . . . ?
N1 C1 C14 C19 126.3(3) . . . . ?
C2 C1 C14 C19 -116.0(3) . . . . ?
C8 C1 C14 C19 8.4(4) . . . . ?
N1 C1 C14 C15 -53.1(3) . . . . ?
C2 C1 C14 C15 64.6(3) . . . . ?
C8 C1 C14 C15 -171.1(3) . . . . ?
C19 C14 C15 C16 -0.2(5) . . . . ?
C1 C14 C15 C16 179.2(3) . . . . ?
C14 C15 C16 C17 0.5(6) . . . . ?
C15 C16 C17 C18 0.3(7) . . . . ?
C16 C17 C18 C19 -1.4(7) . . . . ?
C15 C14 C19 C18 -0.9(5) . . . . ?
C1 C14 C19 C18 179.7(3) . . . . ?
C17 C18 C19 C14 1.7(7) . . . . ?
O1 S1 C20 C25 90.2(3) . . . . ?
O2 S1 C20 C25 -33.0(3) . . . . ?
O3 S1 C20 C25 -150.5(2) . . . . ?
O1 S1 C20 C21 -87.6(3) . . . . ?
O2 S1 C20 C21 149.2(3) . . . . ?
O3 S1 C20 C21 31.7(3) . . . . ?
C25 C20 C21 O4 178.8(3) . . . . ?
S1 C20 C21 O4 -3.4(4) . . . . ?
C25 C20 C21 C22 -0.5(5) . . . . ?
S1 C20 C21 C22 177.2(3) . . . . ?
O4 C21 C22 C23 -178.7(3) . . . . ?
C20 C21 C22 C23 0.7(6) . . . . ?
C21 C22 C23 C24 -0.2(6) . . . . ?
C22 C23 C24 C25 -0.5(5) . . . . ?
C22 C23 C24 C24 -179.9(4) . . . 5_675 ?
C21 C20 C25 C24 -0.2(5) . . . . ?
S1 C20 C25 C24 -178.0(2) . . . . ?
C23 C24 C25 C20 0.7(5) . . . . ?
C24 C24 C25 C20 -179.9(3) 5_675 . . . ?

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 O1 0.85(3) 2.12(2) 2.904(3) 153(3) 2_655
O1W H2W O2 0.85(3) 2.176(18) 2.985(3) 158(3) 6_566
O4 H4O O3 0.85(3) 1.94(2) 2.712(3) 150(4) .
N1 H1N1 O3 0.87(3) 1.981(10) 2.852(3) 178(2) .
N1 H1N2 O1W 0.87(3) 1.882(11) 2.754(3) 175(3) .
N1 H1N3 O2 0.86(3) 1.997(16) 2.801(3) 155(2) 5_665

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.056
_database_code_depnum_ccdc_archive 'CCDC 1025994'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 2(C H4 O), H2 O'
_chemical_formula_sum            'C52 H54 N2 O11 S2'
_chemical_formula_weight         947.09

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                   13.0823(9)
_cell_length_b                   13.6545(8)
_cell_length_c                   14.8789(7)
_cell_angle_alpha                98.884(5)
_cell_angle_beta                 94.355(5)
_cell_angle_gamma                110.469(6)
_cell_volume                     2435.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3350
_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          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9632
_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            14501
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         27.56
_reflns_number_total             11090
_reflns_number_gt                7650
_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)+(0.0484P)²+0.8861P] 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         11090
_refine_ls_number_parameters     642
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1382
_refine_ls_wR_factor_gt          0.1208
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.024
_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 0.50919(5) 1.42870(4) 0.19352(4) 0.03678(15) Uani 1 1 d . . .
S2 S 0.37529(5) 0.73169(4) 0.20857(4) 0.03588(14) Uani 1 1 d . . .
O1 O 0.45914(14) 1.42272(13) 0.27745(11) 0.0443(4) Uani 1 1 d . . .
O1W O 0.32266(17) 1.39500(15) -0.05125(12) 0.0600(5) Uani 1 1 d D . .
H1W H 0.344(2) 1.4448(19) -0.0811(18) 0.090 Uiso 1 1 d D . .
H2W H 0.3717(19) 1.406(2) -0.0058(15) 0.090 Uiso 1 1 d D . .
O2 O 0.43694(17) 1.43671(16) 0.11948(12) 0.0632(5) Uani 1 1 d . . .
O3 O 0.61815(15) 1.50984(13) 0.20831(13) 0.0555(5) Uani 1 1 d . . .
O4 O 0.61097(18) 1.36303(14) 0.03379(12) 0.0573(5) Uani 1 1 d D . .
H4O H 0.633(3) 1.341(2) -0.0151(14) 0.086 Uiso 1 1 d D . .
O5 O 0.30853(15) 0.71260(14) 0.12144(12) 0.0525(5) Uani 1 1 d . . .
O6 O 0.48155(15) 0.72687(15) 0.19756(16) 0.0665(6) Uani 1 1 d . . .
O7 O 0.31732(16) 0.66455(13) 0.26994(12) 0.0565(5) Uani 1 1 d . . .
O8 O 0.35672(19) 0.81984(14) 0.41356(12) 0.0605(5) Uani 1 1 d D . .
H8O H 0.341(3) 0.7584(14) 0.3803(19) 0.091 Uiso 1 1 d D . .
O9 O 0.6790(2) 0.67276(16) 0.36906(15) 0.0718(6) Uani 1 1 d D . .
H9O H 0.661(3) 0.6085(12) 0.342(2) 0.108 Uiso 1 1 d D . .
O10 O 0.1587(2) 1.3734(2) 0.06184(15) 0.0854(7) Uani 1 1 d D . .
H10O H 0.212(2) 1.376(4) 0.031(3) 0.128 Uiso 1 1 d D . .
N1 N 0.25080(15) 1.44069(15) 0.24932(13) 0.0356(4) Uani 1 1 d D . .
H1N1 H 0.2208(16) 1.4154(15) 0.1926(8) 0.053 Uiso 1 1 d D . .
H1N2 H 0.3127(12) 1.4305(16) 0.2549(15) 0.053 Uiso 1 1 d D . .
H1N3 H 0.2679(17) 1.5092(8) 0.2580(14) 0.053 Uiso 1 1 d D . .
N2 N 0.70458(16) 0.76113(16) 0.21011(14) 0.0413(5) Uani 1 1 d D . .
H2N1 H 0.703(2) 0.7330(18) 0.2586(9) 0.062 Uiso 1 1 d D . .
H2N2 H 0.6439(14) 0.7735(19) 0.2031(14) 0.062 Uiso 1 1 d D . .
H2N3 H 0.701(2) 0.7135(16) 0.1635(10) 0.062 Uiso 1 1 d D . .
C1 C 0.52810(17) 1.30617(16) 0.16218(14) 0.0315(5) Uani 1 1 d . . .
C2 C 0.57875(19) 1.28698(17) 0.08544(15) 0.0374(5) Uani 1 1 d . . .
C3 C 0.5972(2) 1.19219(18) 0.06622(16) 0.0434(6) Uani 1 1 d . . .
H3 H 0.6322 1.1792 0.0161 0.052 Uiso 1 1 calc R . .
C4 C 0.5641(2) 1.11731(18) 0.12109(16) 0.0406(5) Uani 1 1 d . . .
H4 H 0.5786 1.0550 0.1080 0.049 Uiso 1 1 calc R . .
C5 C 0.50919(18) 1.13270(17) 0.19568(15) 0.0326(5) Uani 1 1 d . . .
C6 C 0.49275(17) 1.22916(16) 0.21534(14) 0.0313(5) Uani 1 1 d . . .
H6 H 0.4573 1.2419 0.2652 0.038 Uiso 1 1 calc R . .
C7 C 0.46762(18) 1.05003(17) 0.25176(15) 0.0336(5) Uani 1 1 d . . .
C8 C 0.43736(18) 0.94281(17) 0.21359(15) 0.0344(5) Uani 1 1 d . . .
H8 H 0.4424 0.9234 0.1518 0.041 Uiso 1 1 calc R . .
C9 C 0.39972(18) 0.86341(17) 0.26464(15) 0.0323(5) Uani 1 1 d . . .
C10 C 0.3906(2) 0.89122(18) 0.35723(16) 0.0389(5) Uani 1 1 d . . .
C11 C 0.4181(2) 0.99804(19) 0.39548(16) 0.0440(6) Uani 1 1 d . . .
H11 H 0.4104 1.0174 0.4566 0.053 Uiso 1 1 calc R . .
C12 C 0.4566(2) 1.07545(18) 0.34449(15) 0.0392(5) Uani 1 1 d . . .
H12 H 0.4759 1.1465 0.3721 0.047 Uiso 1 1 calc R . .
C13 C 0.17430(18) 1.39052(17) 0.31518(15) 0.0334(5) Uani 1 1 d . . .
C14 C 0.18267(18) 1.28183(18) 0.31782(18) 0.0410(6) Uani 1 1 d . . .
C15 C 0.1782(2) 1.2138(2) 0.2368(2) 0.0594(7) Uani 1 1 d . . .
H15 H 0.1721 1.2351 0.1809 0.071 Uiso 1 1 calc R . .
C16 C 0.1828(3) 1.1137(2) 0.2388(3) 0.0801(11) Uani 1 1 d . . .
H16 H 0.1800 1.0687 0.1842 0.096 Uiso 1 1 calc R . .
C17 C 0.1914(3) 1.0813(3) 0.3206(4) 0.0871(13) Uani 1 1 d . . .
H17 H 0.1943 1.0144 0.3217 0.104 Uiso 1 1 calc R . .
C18 C 0.1957(3) 1.1469(3) 0.3994(3) 0.0853(12) Uani 1 1 d . . .
H18 H 0.2013 1.1246 0.4549 0.102 Uiso 1 1 calc R . .
C19 C 0.1918(2) 1.2470(2) 0.3994(2) 0.0615(8) Uani 1 1 d . . .
H19 H 0.1953 1.2911 0.4547 0.074 Uiso 1 1 calc R . .
C20 C 0.21458(19) 1.46573(18) 0.40914(15) 0.0380(5) Uani 1 1 d . . .
C21 C 0.3242(2) 1.5041(2) 0.44606(17) 0.0479(6) Uani 1 1 d . . .
H21 H 0.3743 1.4859 0.4126 0.057 Uiso 1 1 calc R . .
C22 C 0.3609(2) 1.5694(2) 0.53230(19) 0.0616(8) Uani 1 1 d . . .
H22 H 0.4353 1.5945 0.5558 0.074 Uiso 1 1 calc R . .
C23 C 0.2908(3) 1.5964(4) 0.5818(2) 0.0985(14) Uani 1 1 d . . .
H23 H 0.3158 1.6400 0.6396 0.118 Uiso 1 1 calc R . .
C24 C 0.1827(3) 1.5595(5) 0.5469(3) 0.104(3) Uani 1 1 d . . .
H24 H 0.1333 1.5777 0.5813 0.182 Uiso 1 1 calc R . .
C25 C 0.1446(3) 1.4948(4) 0.4606(2) 0.1018(15) Uani 1 1 d . . .
H25 H 0.0701 1.4710 0.4375 0.122 Uiso 1 1 calc R . .
C26 C 0.05790(19) 1.38005(19) 0.27795(15) 0.0378(5) Uani 1 1 d . . .
C27 C -0.0324(2) 1.2897(2) 0.27772(19) 0.0536(7) Uani 1 1 d . . .
H27 H -0.0229 1.2324 0.2989 0.064 Uiso 1 1 calc R . .
C28 C -0.1373(2) 1.2835(3) 0.2461(2) 0.0720(9) Uani 1 1 d . . .
H28 H -0.1974 1.2218 0.2459 0.086 Uiso 1 1 calc R . .
C29 C -0.1533(2) 1.3662(3) 0.2154(2) 0.0717(9) Uani 1 1 d . . .
H29 H -0.2239 1.3612 0.1940 0.086 Uiso 1 1 calc R . .
C30 C -0.0648(3) 1.4568(3) 0.2163(2) 0.0743(9) Uani 1 1 d . . .
H30 H -0.0753 1.5141 0.1958 0.089 Uiso 1 1 calc R . .
C31 C 0.0404(2) 1.4640(2) 0.2476(2) 0.0576(7) Uani 1 1 d . . .
H31 H 0.1001 1.5263 0.2481 0.069 Uiso 1 1 calc R . .
C32 C 0.80700(17) 0.85954(18) 0.21929(15) 0.0353(5) Uani 1 1 d . . .
C33 C 0.90339(19) 0.82089(19) 0.22510(17) 0.0422(6) Uani 1 1 d . . .
C34 C 0.9734(2) 0.8288(2) 0.1597(2) 0.0646(8) Uani 1 1 d . . .
H34 H 0.9625 0.8582 0.1091 0.078 Uiso 1 1 calc R . .
C35 C 1.0604(3) 0.7933(3) 0.1688(3) 0.0938(13) Uani 1 1 d . . .
H35 H 1.1074 0.7994 0.1244 0.113 Uiso 1 1 calc R . .
C36 C 1.0773(3) 0.7500(3) 0.2415(4) 0.0931(14) Uani 1 1 d . . .
H36 H 1.1364 0.7273 0.2472 0.112 Uiso 1 1 calc R . .
C37 C 1.0084(3) 0.7392(3) 0.3066(3) 0.0803(11) Uani 1 1 d . . .
H37 H 1.0195 0.7082 0.3561 0.096 Uiso 1 1 calc R . .
C38 C 0.9212(2) 0.7747(2) 0.2986(2) 0.0606(8) Uani 1 1 d . . .
H38 H 0.8743 0.7675 0.3431 0.073 Uiso 1 1 calc R . .
C39 C 0.80920(18) 0.93820(18) 0.30668(15) 0.0354(5) Uani 1 1 d . . .
C40 C 0.9036(2) 0.9928(2) 0.36875(17) 0.0493(6) Uani 1 1 d . . .
H40 H 0.9670 0.9781 0.3608 0.059 Uiso 1 1 calc R . .
C41 C 0.9057(2) 1.0689(2) 0.44257(19) 0.0595(7) Uani 1 1 d . . .
H41 H 0.9700 1.1046 0.4838 0.071 Uiso 1 1 calc R . .
C42 C 0.8132(3) 1.0919(2) 0.45514(19) 0.0595(7) Uani 1 1 d . . .
H42 H 0.8142 1.1424 0.5052 0.071 Uiso 1 1 calc R . .
C43 C 0.7192(2) 1.0399(2) 0.39326(19) 0.0590(7) Uani 1 1 d . . .
H43 H 0.6566 1.0560 0.4008 0.071 Uiso 1 1 calc R . .
C44 C 0.7173(2) 0.9635(2) 0.31961(18) 0.0498(6) Uani 1 1 d . . .
H44 H 0.6531 0.9287 0.2781 0.060 Uiso 1 1 calc R . .
C45 C 0.79930(19) 0.91312(19) 0.13723(16) 0.0401(5) Uani 1 1 d . . .
C46 C 0.7183(2) 0.8691(2) 0.06292(18) 0.0605(8) Uani 1 1 d . . .
H46 H 0.6662 0.8012 0.0593 0.073 Uiso 1 1 calc R . .
C47 C 0.7127(3) 0.9240(3) -0.0065(2) 0.0773(10) Uani 1 1 d . . .
H47 H 0.6566 0.8928 -0.0559 0.093 Uiso 1 1 calc R . .
C48 C 0.7880(3) 1.0230(3) -0.0037(2) 0.0744(9) Uani 1 1 d . . .
H48 H 0.7832 1.0598 -0.0505 0.089 Uiso 1 1 calc R . .
C49 C 0.8712(3) 1.0680(3) 0.0690(2) 0.0774(10) Uani 1 1 d . . .
H49 H 0.9240 1.1351 0.0710 0.093 Uiso 1 1 calc R . .
C50 C 0.8767(3) 1.0138(2) 0.13926(19) 0.0636(8) Uani 1 1 d . . .
H50 H 0.9331 1.0453 0.1885 0.076 Uiso 1 1 calc R . .
C51 C 0.5926(3) 0.6888(3) 0.4095(3) 0.0877(11) Uani 1 1 d . . .
H51A H 0.5258 0.6556 0.3669 0.131 Uiso 1 1 calc R . .
H51B H 0.6080 0.7638 0.4260 0.131 Uiso 1 1 calc R . .
H51C H 0.5843 0.6581 0.4636 0.131 Uiso 1 1 calc R . .
C52 C 0.0993(4) 1.4300(5) 0.0238(3) 0.137(2) Uani 1 1 d . . .
H52C H 0.1238 1.5012 0.0588 0.205 Uiso 1 1 calc R . .
H52A H 0.0221 1.3947 0.0254 0.205 Uiso 1 1 calc R . .
H52B H 0.1120 1.4323 -0.0387 0.205 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 1.4388(18) . ?
S1 O3 1.4424(18) . ?
S1 O1 1.4537(16) . ?
S1 C1 1.773(2) . ?
S2 O6 1.4349(18) . ?
S2 O5 1.4407(18) . ?
S2 O7 1.4584(17) . ?
S2 C9 1.768(2) . ?
O1W H1W 0.85(3) . ?
O1W H2W 0.85(3) . ?
O4 C2 1.355(3) . ?
O4 H4O 0.85(3) . ?
O8 C10 1.362(3) . ?
O8 H8O 0.85(3) . ?
O9 C51 1.387(4) . ?
O9 H9O 0.85(3) . ?
O10 C52 1.417(5) . ?
O10 H10O 0.85(3) . ?
N1 C13 1.519(3) . ?
N1 H1N1 0.87(3) . ?
N1 H1N2 0.87(3) . ?
N1 H1N3 0.87(3) . ?
N2 C32 1.509(3) . ?
N2 H2N1 0.87(3) . ?
N2 H2N2 0.87(3) . ?
N2 H2N3 0.86(3) . ?
C1 C6 1.385(3) . ?
C1 C2 1.398(3) . ?
C2 C3 1.390(3) . ?
C3 C4 1.379(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(3) . ?
C5 C7 1.482(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.388(3) . ?
C7 C12 1.401(3) . ?
C8 C9 1.390(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.397(3) . ?
C10 C11 1.388(3) . ?
C11 C12 1.371(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C26 1.530(3) . ?
C13 C14 1.532(3) . ?
C13 C20 1.534(3) . ?
C14 C19 1.382(4) . ?
C14 C15 1.387(4) . ?
C15 C16 1.393(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.367(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.345(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.386(4) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C25 1.360(4) . ?
C20 C21 1.378(3) . ?
C21 C22 1.388(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.333(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.354(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.387(4) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.377(3) . ?
C26 C31 1.378(3) . ?
C27 C28 1.386(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.355(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.365(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.384(4) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C33 1.529(3) . ?
C32 C45 1.531(3) . ?
C32 C39 1.545(3) . ?
C33 C34 1.378(4) . ?
C33 C38 1.387(4) . ?
C34 C35 1.390(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.350(6) . ?
C35 H35 0.9300 . ?
C36 C37 1.364(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.391(4) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C40 1.380(3) . ?
C39 C44 1.381(3) . ?
C40 C41 1.382(4) . ?
C40 H40 0.9300 . ?
C41 C42 1.371(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.371(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.383(4) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 C46 1.371(3) . ?
C45 C50 1.388(3) . ?
C46 C47 1.377(4) . ?
C46 H46 0.9300 . ?
C47 C48 1.358(4) . ?
C47 H47 0.9300 . ?
C48 C49 1.371(4) . ?
C48 H48 0.9300 . ?
C49 C50 1.382(4) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 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 113.79(12) . . ?
O2 S1 O1 111.54(11) . . ?
O3 S1 O1 112.13(11) . . ?
O2 S1 C1 107.22(11) . . ?
O3 S1 C1 105.48(11) . . ?
O1 S1 C1 106.07(10) . . ?
O6 S2 O5 111.92(12) . . ?
O6 S2 O7 113.52(12) . . ?
O5 S2 O7 112.16(11) . . ?
O6 S2 C9 106.20(11) . . ?
O5 S2 C9 107.61(10) . . ?
O7 S2 C9 104.82(10) . . ?
H1W O1W H2W 109.3(16) . . ?
C2 O4 H4O 112(2) . . ?
C10 O8 H8O 106(2) . . ?
C51 O9 H9O 111(3) . . ?
C52 O10 H10O 108(3) . . ?
C13 N1 H1N1 111.6(16) . . ?
C13 N1 H1N2 112.9(16) . . ?
H1N1 N1 H1N2 107.1(13) . . ?
C13 N1 H1N3 111.9(15) . . ?
H1N1 N1 H1N3 106.7(13) . . ?
H1N2 N1 H1N3 106.2(13) . . ?
C32 N2 H2N1 111.2(17) . . ?
C32 N2 H2N2 113.3(17) . . ?
H2N1 N2 H2N2 106.1(13) . . ?
C32 N2 H2N3 111.4(17) . . ?
H2N1 N2 H2N3 107.8(14) . . ?
H2N2 N2 H2N3 106.7(13) . . ?
C6 C1 C2 119.92(19) . . ?
C6 C1 S1 119.09(16) . . ?
C2 C1 S1 120.98(16) . . ?
O4 C2 C3 122.2(2) . . ?
O4 C2 C1 118.7(2) . . ?
C3 C2 C1 119.1(2) . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 121.6(2) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 117.5(2) . . ?
C4 C5 C7 121.93(19) . . ?
C6 C5 C7 120.5(2) . . ?
C1 C6 C5 121.5(2) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C8 C7 C12 117.0(2) . . ?
C8 C7 C5 120.72(19) . . ?
C12 C7 C5 122.3(2) . . ?
C7 C8 C9 122.2(2) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C10 119.6(2) . . ?
C8 C9 S2 116.61(16) . . ?
C10 C9 S2 123.67(16) . . ?
O8 C10 C11 117.1(2) . . ?
O8 C10 C9 124.1(2) . . ?
C11 C10 C9 118.7(2) . . ?
C12 C11 C10 120.9(2) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C7 121.6(2) . . ?
C11 C12 H12 119.2 . . ?
C7 C12 H12 119.2 . . ?
N1 C13 C26 107.49(17) . . ?
N1 C13 C14 106.88(17) . . ?
C26 C13 C14 112.00(18) . . ?
N1 C13 C20 107.08(17) . . ?
C26 C13 C20 111.18(18) . . ?
C14 C13 C20 111.90(18) . . ?
C19 C14 C15 117.9(2) . . ?
C19 C14 C13 121.8(2) . . ?
C15 C14 C13 120.2(2) . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 119.5(3) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 121.2(3) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C14 C19 C18 120.6(3) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C25 C20 C21 117.2(2) . . ?
C25 C20 C13 122.2(2) . . ?
C21 C20 C13 120.6(2) . . ?
C20 C21 C22 121.1(2) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 119.2(3) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C23 C24 C25 120.9(3) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C20 C25 C24 120.9(3) . . ?
C20 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C27 C26 C31 118.1(2) . . ?
C27 C26 C13 121.6(2) . . ?
C31 C26 C13 120.2(2) . . ?
C26 C27 C28 120.4(3) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C29 C28 C27 120.9(3) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 119.4(3) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C29 C30 C31 120.4(3) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C26 C31 C30 120.8(3) . . ?
C26 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
N2 C32 C33 105.54(18) . . ?
N2 C32 C45 108.92(17) . . ?
C33 C32 C45 113.98(19) . . ?
N2 C32 C39 107.93(18) . . ?
C33 C32 C39 112.90(18) . . ?
C45 C32 C39 107.37(18) . . ?
C34 C33 C38 118.0(2) . . ?
C34 C33 C32 122.8(2) . . ?
C38 C33 C32 119.1(2) . . ?
C33 C34 C35 120.4(3) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C36 C35 C34 120.6(3) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C37 120.4(3) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C36 C37 C38 119.6(4) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 H37 120.2 . . ?
C33 C38 C37 120.9(3) . . ?
C33 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C40 C39 C44 117.8(2) . . ?
C40 C39 C32 122.3(2) . . ?
C44 C39 C32 119.6(2) . . ?
C39 C40 C41 121.2(2) . . ?
C39 C40 H40 119.4 . . ?
C41 C40 H40 119.4 . . ?
C42 C41 C40 120.2(3) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C43 119.5(3) . . ?
C41 C42 H42 120.3 . . ?
C43 C42 H42 120.3 . . ?
C42 C43 C44 120.2(3) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C39 C44 C43 121.1(2) . . ?
C39 C44 H44 119.4 . . ?
C43 C44 H44 119.4 . . ?
C46 C45 C50 117.7(2) . . ?
C46 C45 C32 124.0(2) . . ?
C50 C45 C32 118.3(2) . . ?
C45 C46 C47 121.0(3) . . ?
C45 C46 H46 119.5 . . ?
C47 C46 H46 119.5 . . ?
C48 C47 C46 121.0(3) . . ?
C48 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C47 C48 C49 119.2(3) . . ?
C47 C48 H48 120.4 . . ?
C49 C48 H48 120.4 . . ?
C48 C49 C50 120.2(3) . . ?
C48 C49 H49 119.9 . . ?
C50 C49 H49 119.9 . . ?
C49 C50 C45 120.8(3) . . ?
C49 C50 H50 119.6 . . ?
C45 C50 H50 119.6 . . ?
O9 C51 H51A 109.5 . . ?
O9 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O9 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O10 C52 H52C 109.5 . . ?
O10 C52 H52A 109.5 . . ?
H52C C52 H52A 109.5 . . ?
O10 C52 H52B 109.5 . . ?
H52C C52 H52B 109.5 . . ?
H52A C52 H52B 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
O2 S1 C1 C6 -117.44(19) . . . . ?
O3 S1 C1 C6 120.96(18) . . . . ?
O1 S1 C1 C6 1.9(2) . . . . ?
O2 S1 C1 C2 63.1(2) . . . . ?
O3 S1 C1 C2 -58.5(2) . . . . ?
O1 S1 C1 C2 -177.62(18) . . . . ?
C6 C1 C2 O4 179.0(2) . . . . ?
S1 C1 C2 O4 -1.6(3) . . . . ?
C6 C1 C2 C3 -2.9(3) . . . . ?
S1 C1 C2 C3 176.57(18) . . . . ?
O4 C2 C3 C4 179.4(2) . . . . ?
C1 C2 C3 C4 1.3(4) . . . . ?
C2 C3 C4 C5 1.5(4) . . . . ?
C3 C4 C5 C6 -2.5(3) . . . . ?
C3 C4 C5 C7 176.4(2) . . . . ?
C2 C1 C6 C5 1.8(3) . . . . ?
S1 C1 C6 C5 -177.66(16) . . . . ?
C4 C5 C6 C1 0.9(3) . . . . ?
C7 C5 C6 C1 -178.10(19) . . . . ?
C4 C5 C7 C8 -28.3(3) . . . . ?
C6 C5 C7 C8 150.6(2) . . . . ?
C4 C5 C7 C12 151.9(2) . . . . ?
C6 C5 C7 C12 -29.2(3) . . . . ?
C12 C7 C8 C9 -1.2(3) . . . . ?
C5 C7 C8 C9 179.0(2) . . . . ?
C7 C8 C9 C10 0.7(3) . . . . ?
C7 C8 C9 S2 -174.95(17) . . . . ?
O6 S2 C9 C8 70.3(2) . . . . ?
O5 S2 C9 C8 -49.7(2) . . . . ?
O7 S2 C9 C8 -169.25(17) . . . . ?
O6 S2 C9 C10 -105.1(2) . . . . ?
O5 S2 C9 C10 134.9(2) . . . . ?
O7 S2 C9 C10 15.3(2) . . . . ?
C8 C9 C10 O8 -178.7(2) . . . . ?
S2 C9 C10 O8 -3.4(3) . . . . ?
C8 C9 C10 C11 0.9(3) . . . . ?
S2 C9 C10 C11 176.16(18) . . . . ?
O8 C10 C11 C12 177.8(2) . . . . ?
C9 C10 C11 C12 -1.8(4) . . . . ?
C10 C11 C12 C7 1.3(4) . . . . ?
C8 C7 C12 C11 0.3(3) . . . . ?
C5 C7 C12 C11 -179.9(2) . . . . ?
N1 C13 C14 C19 135.7(2) . . . . ?
C26 C13 C14 C19 -106.9(3) . . . . ?
C20 C13 C14 C19 18.7(3) . . . . ?
N1 C13 C14 C15 -46.1(3) . . . . ?
C26 C13 C14 C15 71.3(3) . . . . ?
C20 C13 C14 C15 -163.1(2) . . . . ?
C19 C14 C15 C16 0.0(4) . . . . ?
C13 C14 C15 C16 -178.3(2) . . . . ?
C14 C15 C16 C17 0.2(5) . . . . ?
C15 C16 C17 C18 -0.1(5) . . . . ?
C16 C17 C18 C19 -0.2(5) . . . . ?
C15 C14 C19 C18 -0.3(4) . . . . ?
C13 C14 C19 C18 177.9(3) . . . . ?
C17 C18 C19 C14 0.4(5) . . . . ?
N1 C13 C20 C25 132.9(3) . . . . ?
C26 C13 C20 C25 15.8(4) . . . . ?
C14 C13 C20 C25 -110.3(3) . . . . ?
N1 C13 C20 C21 -49.1(3) . . . . ?
C26 C13 C20 C21 -166.2(2) . . . . ?
C14 C13 C20 C21 67.7(3) . . . . ?
C25 C20 C21 C22 0.2(4) . . . . ?
C13 C20 C21 C22 -177.9(2) . . . . ?
C20 C21 C22 C23 0.2(5) . . . . ?
C21 C22 C23 C24 -0.1(7) . . . . ?
C22 C23 C24 C25 -0.4(9) . . . . ?
C21 C20 C25 C24 -0.7(6) . . . . ?
C13 C20 C25 C24 177.4(4) . . . . ?
C23 C24 C25 C20 0.8(9) . . . . ?
N1 C13 C26 C27 137.5(2) . . . . ?
C14 C13 C26 C27 20.4(3) . . . . ?
C20 C13 C26 C27 -105.6(3) . . . . ?
N1 C13 C26 C31 -45.6(3) . . . . ?
C14 C13 C26 C31 -162.7(2) . . . . ?
C20 C13 C26 C31 71.3(3) . . . . ?
C31 C26 C27 C28 1.2(4) . . . . ?
C13 C26 C27 C28 178.1(2) . . . . ?
C26 C27 C28 C29 -0.5(5) . . . . ?
C27 C28 C29 C30 -0.3(5) . . . . ?
C28 C29 C30 C31 0.4(5) . . . . ?
C27 C26 C31 C30 -1.1(4) . . . . ?
C13 C26 C31 C30 -178.1(3) . . . . ?
C29 C30 C31 C26 0.3(5) . . . . ?
N2 C32 C33 C34 116.4(3) . . . . ?
C45 C32 C33 C34 -3.1(3) . . . . ?
C39 C32 C33 C34 -126.0(3) . . . . ?
N2 C32 C33 C38 -63.0(3) . . . . ?
C45 C32 C33 C38 177.5(2) . . . . ?
C39 C32 C33 C38 54.7(3) . . . . ?
C38 C33 C34 C35 -1.2(4) . . . . ?
C32 C33 C34 C35 179.4(3) . . . . ?
C33 C34 C35 C36 0.3(5) . . . . ?
C34 C35 C36 C37 0.8(6) . . . . ?
C35 C36 C37 C38 -1.1(5) . . . . ?
C34 C33 C38 C37 1.0(4) . . . . ?
C32 C33 C38 C37 -179.6(3) . . . . ?
C36 C37 C38 C33 0.1(5) . . . . ?
N2 C32 C39 C40 135.6(2) . . . . ?
C33 C32 C39 C40 19.4(3) . . . . ?
C45 C32 C39 C40 -107.1(2) . . . . ?
N2 C32 C39 C44 -50.9(3) . . . . ?
C33 C32 C39 C44 -167.2(2) . . . . ?
C45 C32 C39 C44 66.4(3) . . . . ?
C44 C39 C40 C41 1.3(4) . . . . ?
C32 C39 C40 C41 174.8(2) . . . . ?
C39 C40 C41 C42 -0.3(4) . . . . ?
C40 C41 C42 C43 -0.9(5) . . . . ?
C41 C42 C43 C44 1.1(5) . . . . ?
C40 C39 C44 C43 -1.1(4) . . . . ?
C32 C39 C44 C43 -174.8(2) . . . . ?
C42 C43 C44 C39 -0.1(4) . . . . ?
N2 C32 C45 C46 -7.7(3) . . . . ?
C33 C32 C45 C46 109.9(3) . . . . ?
C39 C32 C45 C46 -124.3(3) . . . . ?
N2 C32 C45 C50 170.1(2) . . . . ?
C33 C32 C45 C50 -72.4(3) . . . . ?
C39 C32 C45 C50 53.5(3) . . . . ?
C50 C45 C46 C47 -1.3(5) . . . . ?
C32 C45 C46 C47 176.5(3) . . . . ?
C45 C46 C47 C48 0.6(5) . . . . ?
C46 C47 C48 C49 0.7(6) . . . . ?
C47 C48 C49 C50 -1.3(6) . . . . ?
C48 C49 C50 C45 0.6(5) . . . . ?
C46 C45 C50 C49 0.7(5) . . . . ?
C32 C45 C50 C49 -177.3(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 H1W O3 0.85(3) 2.121(19) 2.874(3) 148(3) 2_685
O1W H1W O4 0.85(3) 2.45(3) 3.071(3) 130(3) 2_685
O1W H2W O2 0.85(3) 1.910(15) 2.719(3) 158(3) .
O4 H4O O5 0.85(3) 1.961(11) 2.811(2) 176(3) 2_675
O8 H8O O7 0.85(3) 1.853(17) 2.645(3) 154(3) .
O9 H9O O3 0.85(3) 2.13(2) 2.852(3) 142(3) 1_545
O10 H10O O1W 0.85(3) 1.942(13) 2.789(3) 171(4) .
N1 H1N1 O10 0.87(3) 1.966(10) 2.828(3) 174(2) .
N1 H1N2 O1 0.87(3) 1.962(9) 2.827(2) 173.6(19) .
N1 H1N3 O7 0.87(3) 1.963(10) 2.829(2) 175(2) 1_565
N2 H2N1 O9 0.87(3) 1.947(10) 2.807(3) 172(2) .
N2 H2N2 O6 0.87(3) 1.984(16) 2.775(3) 151(2) .
N2 H2N3 O1W 0.86(3) 1.978(10) 2.836(3) 174(2) 2_675

_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         -0.357
_refine_diff_density_rms         0.044
_database_code_depnum_ccdc_archive 'CCDC 1025995'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 4(C H4 O)'
_chemical_formula_sum            'C54 H60 N2 O12 S2'
_chemical_formula_weight         993.16

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                   10.0429(6)
_cell_length_b                   12.1542(7)
_cell_length_c                   12.5456(8)
_cell_angle_alpha                67.646(6)
_cell_angle_beta                 67.742(6)
_cell_angle_gamma                80.119(5)
_cell_volume                     1310.07(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1614
_cell_measurement_theta_min      3.34
_cell_measurement_theta_max      27.52

_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    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             526
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9632
_exptl_absorpt_correction_T_max  0.9695
_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            7751
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         27.56
_reflns_number_total             5968
_reflns_number_gt                3885
_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)+(0.0622P)²+0.1468P] 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         5968
_refine_ls_number_parameters     336
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0580
_refine_ls_wR_factor_ref         0.1549
_refine_ls_wR_factor_gt          0.1308
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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 -0.19870(6) 0.63354(5) 0.13394(5) 0.04339(18) Uani 1 1 d . . .
O1 O -0.07967(18) 0.61541(13) 0.03073(13) 0.0526(4) Uani 1 1 d . . .
O2 O -0.1789(2) 0.56235(14) 0.24979(14) 0.0593(5) Uani 1 1 d . . .
O3 O -0.3392(2) 0.61787(16) 0.13404(19) 0.0725(5) Uani 1 1 d . . .
O4 O -0.4482(2) 0.78041(17) 0.2555(2) 0.0771(6) Uani 1 1 d D . .
H4O H -0.444(4) 0.720(2) 0.236(3) 0.116 Uiso 1 1 d D . .
O5 O 0.2669(3) 0.5032(3) 0.1766(2) 0.1137(9) Uani 1 1 d D . .
H5O H 0.312(5) 0.480(4) 0.227(4) 0.171 Uiso 1 1 d D . .
O6 O 0.4313(3) 0.4804(4) 0.3037(3) 0.1481(13) Uani 1 1 d D . .
H6O H 0.515(3) 0.503(6) 0.253(5) 0.222 Uiso 1 1 d D . .
N1 N 0.0397(2) 0.38509(15) 0.20445(15) 0.0406(4) Uani 1 1 d D . .
H1N1 H -0.0299(15) 0.4362(17) 0.2208(19) 0.061 Uiso 1 1 d D . .
H1N2 H 0.1169(14) 0.4155(19) 0.1980(19) 0.061 Uiso 1 1 d D . .
H1N3 H 0.054(2) 0.3870(19) 0.1310(12) 0.061 Uiso 1 1 d D . .
C1 C 0.0148(2) 0.26038(18) 0.29791(18) 0.0393(5) Uani 1 1 d . . .
C2 C 0.1246(2) 0.17612(19) 0.24067(19) 0.0419(5) Uani 1 1 d . . .
C3 C 0.0884(3) 0.0630(2) 0.2619(2) 0.0524(6) Uani 1 1 d . . .
H3A H -0.0055 0.0388 0.3083 0.063 Uiso 1 1 calc R . .
C4 C 0.1901(3) -0.0147(2) 0.2151(3) 0.0656(7) Uani 1 1 d . . .
H4A H 0.1641 -0.0907 0.2309 0.079 Uiso 1 1 calc R . .
C5 C 0.3285(3) 0.0196(3) 0.1456(3) 0.0718(8) Uani 1 1 d . . .
H5A H 0.3968 -0.0332 0.1151 0.086 Uiso 1 1 calc R . .
C6 C 0.3657(3) 0.1316(3) 0.1213(3) 0.0766(9) Uani 1 1 d . . .
H6A H 0.4592 0.1557 0.0724 0.092 Uiso 1 1 calc R . .
C7 C 0.2655(3) 0.2098(2) 0.1688(2) 0.0608(7) Uani 1 1 d . . .
H7A H 0.2927 0.2856 0.1525 0.073 Uiso 1 1 calc R . .
C8 C -0.1402(2) 0.22974(19) 0.32797(19) 0.0426(5) Uani 1 1 d . . .
C9 C -0.2192(3) 0.1593(2) 0.4459(2) 0.0637(7) Uani 1 1 d . . .
H9A H -0.1792 0.1332 0.5075 0.076 Uiso 1 1 calc R . .
C10 C -0.3571(4) 0.1279(3) 0.4720(3) 0.0854(10) Uani 1 1 d . . .
H10A H -0.4090 0.0806 0.5511 0.103 Uiso 1 1 calc R . .
C11 C -0.4178(3) 0.1655(3) 0.3831(4) 0.0847(10) Uani 1 1 d . . .
H11A H -0.5105 0.1437 0.4016 0.102 Uiso 1 1 calc R . .
C12 C -0.3421(3) 0.2353(3) 0.2667(3) 0.0714(8) Uani 1 1 d . . .
H12A H -0.3836 0.2616 0.2060 0.086 Uiso 1 1 calc R . .
C13 C -0.2035(3) 0.2670(2) 0.2389(2) 0.0533(6) Uani 1 1 d . . .
H13A H -0.1524 0.3140 0.1593 0.064 Uiso 1 1 calc R . .
C14 C 0.0378(3) 0.26345(19) 0.41115(19) 0.0477(6) Uani 1 1 d . . .
C15 C 0.1334(3) 0.1866(3) 0.4621(2) 0.0617(7) Uani 1 1 d . . .
H15A H 0.1884 0.1318 0.4262 0.074 Uiso 1 1 calc R . .
C16 C 0.1483(4) 0.1900(3) 0.5659(3) 0.0828(10) Uani 1 1 d . . .
H16A H 0.2131 0.1375 0.5991 0.099 Uiso 1 1 calc R . .
C17 C 0.0697(5) 0.2691(4) 0.6196(3) 0.0922(12) Uani 1 1 d . . .
H17A H 0.0809 0.2714 0.6890 0.111 Uiso 1 1 calc R . .
C18 C -0.0267(5) 0.3462(3) 0.5710(3) 0.0907(11) Uani 1 1 d . . .
H18A H -0.0812 0.4003 0.6081 0.109 Uiso 1 1 calc R . .
C19 C -0.0436(4) 0.3438(2) 0.4665(2) 0.0733(9) Uani 1 1 d . . .
H19A H -0.1092 0.3960 0.4342 0.088 Uiso 1 1 calc R . .
C20 C -0.1992(2) 0.78441(18) 0.11970(19) 0.0378(5) Uani 1 1 d . . .
C21 C -0.3210(2) 0.8362(2) 0.1859(2) 0.0481(6) Uani 1 1 d . . .
C22 C -0.3131(3) 0.9497(2) 0.1815(2) 0.0580(7) Uani 1 1 d . . .
H22A H -0.3926 0.9846 0.2268 0.070 Uiso 1 1 calc R . .
C23 C -0.1887(3) 1.0124(2) 0.1106(2) 0.0521(6) Uani 1 1 d . . .
H23A H -0.1863 1.0887 0.1101 0.062 Uiso 1 1 calc R . .
C24 C -0.0660(2) 0.96533(18) 0.03935(19) 0.0383(5) Uani 1 1 d . . .
C25 C -0.0751(2) 0.84870(18) 0.04772(18) 0.0384(5) Uani 1 1 d . . .
H25A H 0.0048 0.8130 0.0036 0.046 Uiso 1 1 calc R . .
C26 C 0.2977(8) 0.6101(6) 0.0811(6) 0.225(4) Uani 1 1 d . . .
H26A H 0.2999 0.6710 0.1116 0.338 Uiso 1 1 calc R . .
H26B H 0.2249 0.6306 0.0440 0.338 Uiso 1 1 calc R . .
H26C H 0.3897 0.6034 0.0211 0.338 Uiso 1 1 calc R . .
C27 C 0.4098(6) 0.4484(5) 0.4247(5) 0.1407(17) Uani 1 1 d . . .
H27A H 0.3821 0.5174 0.4487 0.211 Uiso 1 1 calc R . .
H27B H 0.4971 0.4133 0.4396 0.211 Uiso 1 1 calc R . .
H27C H 0.3349 0.3916 0.4716 0.211 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 1.4503(16) . ?
S1 O1 1.4519(16) . ?
S1 O3 1.4554(19) . ?
S1 C20 1.773(2) . ?
O4 C21 1.362(3) . ?
O4 H4O 0.85(3) . ?
O5 C26 1.376(5) . ?
O5 H5O 0.85(3) . ?
O6 C27 1.354(5) . ?
O6 H6O 0.85(3) . ?
N1 C1 1.514(3) . ?
N1 H1N1 0.87(2) . ?
N1 H1N2 0.87(2) . ?
N1 H1N3 0.87(2) . ?
C1 C8 1.533(3) . ?
C1 C2 1.534(3) . ?
C1 C14 1.538(3) . ?
C2 C3 1.384(3) . ?
C2 C7 1.391(3) . ?
C3 C4 1.384(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.367(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.364(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.385(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.382(3) . ?
C8 C9 1.390(3) . ?
C9 C10 1.384(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.362(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.367(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.387(3) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.380(3) . ?
C14 C19 1.385(3) . ?
C15 C16 1.382(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.353(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.374(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.395(4) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C25 1.387(3) . ?
C20 C21 1.395(3) . ?
C21 C22 1.374(3) . ?
C22 C23 1.379(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.399(3) . ?
C23 H23A 0.9300 . ?
C24 C25 1.397(3) . ?
C24 C24 1.484(4) 2_575 ?
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 . ?

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 111.57(10) . . ?
O2 S1 O3 112.06(11) . . ?
O1 S1 O3 113.59(11) . . ?
O2 S1 C20 106.44(10) . . ?
O1 S1 C20 107.38(10) . . ?
O3 S1 C20 105.22(10) . . ?
C21 O4 H4O 107(3) . . ?
C26 O5 H5O 120(4) . . ?
C27 O6 H6O 117(4) . . ?
C1 N1 H1N1 114.3(15) . . ?
C1 N1 H1N2 112.2(15) . . ?
H1N1 N1 H1N2 105.1(13) . . ?
C1 N1 H1N3 112.2(15) . . ?
H1N1 N1 H1N3 107.1(13) . . ?
H1N2 N1 H1N3 105.3(12) . . ?
N1 C1 C8 107.72(17) . . ?
N1 C1 C2 107.72(16) . . ?
C8 C1 C2 111.63(17) . . ?
N1 C1 C14 106.35(16) . . ?
C8 C1 C14 111.47(17) . . ?
C2 C1 C14 111.65(18) . . ?
C3 C2 C7 117.8(2) . . ?
C3 C2 C1 121.3(2) . . ?
C7 C2 C1 120.9(2) . . ?
C2 C3 C4 120.9(2) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C7 120.6(3) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
C6 C7 C2 120.6(3) . . ?
C6 C7 H7A 119.7 . . ?
C2 C7 H7A 119.7 . . ?
C13 C8 C9 118.2(2) . . ?
C13 C8 C1 121.58(19) . . ?
C9 C8 C1 120.2(2) . . ?
C10 C9 C8 120.3(3) . . ?
C10 C9 H9A 119.9 . . ?
C8 C9 H9A 119.9 . . ?
C11 C10 C9 120.8(3) . . ?
C11 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C10 C11 C12 119.8(3) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C11 C12 C13 120.1(3) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C8 C13 C12 120.9(2) . . ?
C8 C13 H13A 119.6 . . ?
C12 C13 H13A 119.6 . . ?
C15 C14 C19 118.6(2) . . ?
C15 C14 C1 122.5(2) . . ?
C19 C14 C1 118.8(2) . . ?
C14 C15 C16 120.8(3) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C17 C16 C15 120.6(3) . . ?
C17 C16 H16A 119.7 . . ?
C15 C16 H16A 119.7 . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 H17A 120.2 . . ?
C18 C17 H17A 120.2 . . ?
C17 C18 C19 120.5(3) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
C14 C19 C18 119.7(3) . . ?
C14 C19 H19A 120.1 . . ?
C18 C19 H19A 120.1 . . ?
C25 C20 C21 120.14(19) . . ?
C25 C20 S1 119.59(16) . . ?
C21 C20 S1 120.17(17) . . ?
O4 C21 C22 117.7(2) . . ?
O4 C21 C20 123.7(2) . . ?
C22 C21 C20 118.6(2) . . ?
C21 C22 C23 120.8(2) . . ?
C21 C22 H22A 119.6 . . ?
C23 C22 H22A 119.6 . . ?
C22 C23 C24 122.4(2) . . ?
C22 C23 H23A 118.8 . . ?
C24 C23 H23A 118.8 . . ?
C25 C24 C23 115.84(19) . . ?
C25 C24 C24 122.1(2) . 2_575 ?
C23 C24 C24 122.1(2) . 2_575 ?
C20 C25 C24 122.19(19) . . ?
C20 C25 H25A 118.9 . . ?
C24 C25 H25A 118.9 . . ?
O5 C26 H26A 109.5 . . ?
O5 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O5 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O6 C27 H27A 109.5 . . ?
O6 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O6 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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 -142.7(2) . . . . ?
C8 C1 C2 C3 -24.7(3) . . . . ?
C14 C1 C2 C3 100.8(2) . . . . ?
N1 C1 C2 C7 39.4(3) . . . . ?
C8 C1 C2 C7 157.4(2) . . . . ?
C14 C1 C2 C7 -77.0(3) . . . . ?
C7 C2 C3 C4 1.3(4) . . . . ?
C1 C2 C3 C4 -176.7(2) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
C3 C4 C5 C6 -0.8(4) . . . . ?
C4 C5 C6 C7 1.6(5) . . . . ?
C5 C6 C7 C2 -0.9(5) . . . . ?
C3 C2 C7 C6 -0.5(4) . . . . ?
C1 C2 C7 C6 177.5(2) . . . . ?
N1 C1 C8 C13 37.0(3) . . . . ?
C2 C1 C8 C13 -81.0(2) . . . . ?
C14 C1 C8 C13 153.3(2) . . . . ?
N1 C1 C8 C9 -145.4(2) . . . . ?
C2 C1 C8 C9 96.6(2) . . . . ?
C14 C1 C8 C9 -29.0(3) . . . . ?
C13 C8 C9 C10 0.1(4) . . . . ?
C1 C8 C9 C10 -177.6(2) . . . . ?
C8 C9 C10 C11 -0.2(5) . . . . ?
C9 C10 C11 C12 -0.2(5) . . . . ?
C10 C11 C12 C13 0.5(5) . . . . ?
C9 C8 C13 C12 0.2(4) . . . . ?
C1 C8 C13 C12 177.9(2) . . . . ?
C11 C12 C13 C8 -0.5(4) . . . . ?
N1 C1 C14 C15 -125.4(2) . . . . ?
C8 C1 C14 C15 117.4(2) . . . . ?
C2 C1 C14 C15 -8.2(3) . . . . ?
N1 C1 C14 C19 56.6(3) . . . . ?
C8 C1 C14 C19 -60.5(3) . . . . ?
C2 C1 C14 C19 173.9(2) . . . . ?
C19 C14 C15 C16 -0.4(4) . . . . ?
C1 C14 C15 C16 -178.3(2) . . . . ?
C14 C15 C16 C17 -0.2(5) . . . . ?
C15 C16 C17 C18 0.5(5) . . . . ?
C16 C17 C18 C19 -0.3(5) . . . . ?
C15 C14 C19 C18 0.5(4) . . . . ?
C1 C14 C19 C18 178.5(2) . . . . ?
C17 C18 C19 C14 -0.2(5) . . . . ?
O2 S1 C20 C25 99.30(18) . . . . ?
O1 S1 C20 C25 -20.3(2) . . . . ?
O3 S1 C20 C25 -141.61(18) . . . . ?
O2 S1 C20 C21 -77.1(2) . . . . ?
O1 S1 C20 C21 163.29(18) . . . . ?
O3 S1 C20 C21 42.0(2) . . . . ?
C25 C20 C21 O4 177.8(2) . . . . ?
S1 C20 C21 O4 -5.8(3) . . . . ?
C25 C20 C21 C22 -2.3(3) . . . . ?
S1 C20 C21 C22 174.07(19) . . . . ?
O4 C21 C22 C23 -178.5(2) . . . . ?
C20 C21 C22 C23 1.7(4) . . . . ?
C21 C22 C23 C24 0.7(4) . . . . ?
C22 C23 C24 C25 -2.3(4) . . . . ?
C22 C23 C24 C24 178.2(3) . . . 2_575 ?
C21 C20 C25 C24 0.7(3) . . . . ?
S1 C20 C25 C24 -175.74(16) . . . . ?
C23 C24 C25 C20 1.6(3) . . . . ?
C24 C24 C25 C20 -178.9(2) 2_575 . . . ?

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 O3 0.85(3) 2.00(2) 2.776(3) 151(3) .
O5 H5O O6 0.85(3) 1.80(2) 2.616(4) 161(5) .
O6 H6O O3 0.85(3) 1.95(3) 2.745(4) 155(6) 1_655
N1 H1N1 O2 0.87(2) 1.986(10) 2.855(2) 176(2) .
N1 H1N2 O5 0.87(2) 1.873(10) 2.744(3) 171(2) .
N1 H1N3 O1 0.87(2) 1.957(9) 2.825(2) 177(2) 2_565

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.043
_database_code_depnum_ccdc_archive 'CCDC 1025996'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), C H4 O'
_chemical_formula_sum            'C51 H48 N2 O9 S2'
_chemical_formula_weight         897.03

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           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                   12.9200(7)
_cell_length_b                   13.9363(6)
_cell_length_c                   13.9627(6)
_cell_angle_alpha                87.493(4)
_cell_angle_beta                 85.351(4)
_cell_angle_gamma                63.093(5)
_cell_volume                     2234.47(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3483
_cell_measurement_theta_min      3.16
_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          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9615
_exptl_absorpt_correction_T_max  0.9683
_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            13260
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         27.56
_reflns_number_total             10178
_reflns_number_gt                6472
_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)+(0.0564P)²+0.9768P] 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         10178
_refine_ls_number_parameters     605
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0625
_refine_ls_wR_factor_ref         0.1580
_refine_ls_wR_factor_gt          0.1349
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.035
_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 0.33933(6) -0.07636(6) 0.51221(5) 0.04175(18) Uani 1 1 d . . .
S2 S 0.26477(7) 0.06974(6) 1.02596(5) 0.0472(2) Uani 1 1 d . . .
O1 O 0.3533(2) 0.01601(19) 0.53237(17) 0.0744(7) Uani 1 1 d . . .
O2 O 0.3221(2) -0.0827(2) 0.41237(14) 0.0788(8) Uani 1 1 d . . .
O3 O 0.4326(2) -0.1739(2) 0.54491(18) 0.0867(9) Uani 1 1 d . . .
O4 O 0.1644(3) -0.1553(2) 0.45943(17) 0.0856(8) Uani 1 1 d D . .
H4O H 0.204(4) -0.127(4) 0.429(3) 0.128 Uiso 1 1 d D . .
O5 O 0.2622(2) 0.17317(17) 1.0136(2) 0.0752(7) Uani 1 1 d . . .
O6 O 0.3688(2) -0.01543(18) 0.98433(17) 0.0748(7) Uani 1 1 d . . .
O7 O 0.2405(3) 0.0501(2) 1.12622(16) 0.0891(9) Uani 1 1 d . . .
O8 O 0.0077(2) 0.17968(18) 1.09380(16) 0.0704(7) Uani 1 1 d D . .
H8O H 0.0765(17) 0.148(3) 1.113(3) 0.106 Uiso 1 1 d D . .
O9 O 0.52143(18) -0.13546(17) 0.27339(14) 0.0529(5) Uani 1 1 d D . .
H9O H 0.4595(18) -0.129(3) 0.304(2) 0.079 Uiso 1 1 d D . .
N1 N 0.64325(19) -0.21237(18) 0.45228(16) 0.0416(5) Uani 1 1 d D . .
H1N1 H 0.5860(18) -0.211(2) 0.4901(14) 0.062 Uiso 1 1 d D . .
H1N2 H 0.623(2) -0.208(2) 0.3942(8) 0.062 Uiso 1 1 d D . .
H1N3 H 0.650(2) -0.1547(15) 0.4630(16) 0.062 Uiso 1 1 d D . .
N2 N 0.4573(2) 0.19543(17) 0.93210(16) 0.0396(5) Uani 1 1 d D . .
H2N1 H 0.3963(13) 0.192(2) 0.9587(15) 0.059 Uiso 1 1 d D . .
H2N2 H 0.5174(13) 0.1398(16) 0.9512(16) 0.059 Uiso 1 1 d D . .
H2N3 H 0.4563(19) 0.191(2) 0.8709(7) 0.059 Uiso 1 1 d D . .
C1 C 0.7561(2) -0.3125(2) 0.46645(17) 0.0356(6) Uani 1 1 d . . .
C2 C 0.8492(2) -0.29660(19) 0.40318(18) 0.0354(6) Uani 1 1 d . . .
C3 C 0.8371(3) -0.2805(2) 0.3048(2) 0.0494(7) Uani 1 1 d . . .
H3A H 0.7709 -0.2768 0.2795 0.059 Uiso 1 1 calc R . .
C4 C 0.9205(3) -0.2700(2) 0.2441(2) 0.0580(8) Uani 1 1 d . . .
H4A H 0.9114 -0.2604 0.1785 0.070 Uiso 1 1 calc R . .
C5 C 1.0173(3) -0.2738(2) 0.2812(3) 0.0628(9) Uani 1 1 d . . .
H5A H 1.0744 -0.2671 0.2405 0.075 Uiso 1 1 calc R . .
C6 C 1.0302(3) -0.2873(3) 0.3774(3) 0.0604(9) Uani 1 1 d . . .
H6A H 1.0955 -0.2886 0.4022 0.072 Uiso 1 1 calc R . .
C7 C 0.9466(2) -0.2992(2) 0.4389(2) 0.0459(7) Uani 1 1 d . . .
H7A H 0.9565 -0.3089 0.5044 0.055 Uiso 1 1 calc R . .
C8 C 0.7768(2) -0.3195(2) 0.57399(18) 0.0391(6) Uani 1 1 d . . .
C9 C 0.7644(3) -0.2300(3) 0.6225(2) 0.0555(8) Uani 1 1 d . . .
H9A H 0.7397 -0.1642 0.5904 0.067 Uiso 1 1 calc R . .
C10 C 0.7882(3) -0.2371(3) 0.7181(2) 0.0680(10) Uani 1 1 d . . .
H10A H 0.7789 -0.1761 0.7499 0.082 Uiso 1 1 calc R . .
C11 C 0.8254(3) -0.3331(3) 0.7661(2) 0.0709(10) Uani 1 1 d . . .
H11A H 0.8422 -0.3379 0.8302 0.085 Uiso 1 1 calc R . .
C12 C 0.8378(3) -0.4219(3) 0.7194(2) 0.0724(10) Uani 1 1 d . . .
H12A H 0.8624 -0.4873 0.7521 0.087 Uiso 1 1 calc R . .
C13 C 0.8140(3) -0.4157(2) 0.6236(2) 0.0551(8) Uani 1 1 d . . .
H13A H 0.8232 -0.4771 0.5926 0.066 Uiso 1 1 calc R . .
C14 C 0.7434(2) -0.4095(2) 0.43341(19) 0.0430(6) Uani 1 1 d . . .
C15 C 0.8395(3) -0.4961(2) 0.3925(2) 0.0566(8) Uani 1 1 d . . .
H15A H 0.9098 -0.4926 0.3822 0.068 Uiso 1 1 calc R . .
C16 C 0.8328(4) -0.5874(3) 0.3668(3) 0.0776(11) Uani 1 1 d . . .
H16A H 0.8986 -0.6450 0.3398 0.093 Uiso 1 1 calc R . .
C17 C 0.7317(5) -0.5938(4) 0.3805(4) 0.1004(15) Uani 1 1 d . . .
H17A H 0.7277 -0.6559 0.3639 0.120 Uiso 1 1 calc R . .
C18 C 0.6354(5) -0.5086(4) 0.4186(4) 0.1134(17) Uani 1 1 d . . .
H18A H 0.5651 -0.5122 0.4265 0.136 Uiso 1 1 calc R . .
C19 C 0.6408(3) -0.4156(3) 0.4464(3) 0.0799(11) Uani 1 1 d . . .
H19A H 0.5747 -0.3584 0.4734 0.096 Uiso 1 1 calc R . .
C20 C 0.4606(2) 0.30045(19) 0.95375(17) 0.0339(5) Uani 1 1 d . . .
C21 C 0.3353(2) 0.3894(2) 0.96054(18) 0.0379(6) Uani 1 1 d . . .
C22 C 0.2590(3) 0.3958(3) 0.8944(3) 0.0687(10) Uani 1 1 d . . .
H22A H 0.2834 0.3435 0.8472 0.082 Uiso 1 1 calc R . .
C23 C 0.1470(3) 0.4782(3) 0.8966(3) 0.0888(13) Uani 1 1 d . . .
H23A H 0.0969 0.4805 0.8514 0.107 Uiso 1 1 calc R . .
C24 C 0.1095(3) 0.5562(3) 0.9644(3) 0.0774(11) Uani 1 1 d . . .
H24A H 0.0338 0.6114 0.9663 0.093 Uiso 1 1 calc R . .
C25 C 0.1846(3) 0.5523(3) 1.0295(3) 0.0710(10) Uani 1 1 d . . .
H25A H 0.1602 0.6061 1.0752 0.085 Uiso 1 1 calc R . .
C26 C 0.2968(3) 0.4691(2) 1.0283(2) 0.0522(7) Uani 1 1 d . . .
H26A H 0.3465 0.4671 1.0738 0.063 Uiso 1 1 calc R . .
C27 C 0.5320(2) 0.3223(2) 0.87064(17) 0.0360(6) Uani 1 1 d . . .
C28 C 0.5021(3) 0.4260(2) 0.8388(2) 0.0539(8) Uani 1 1 d . . .
H28A H 0.4365 0.4827 0.8669 0.065 Uiso 1 1 calc R . .
C29 C 0.5681(3) 0.4467(3) 0.7658(3) 0.0707(10) Uani 1 1 d . . .
H29A H 0.5474 0.5173 0.7460 0.085 Uiso 1 1 calc R . .
C30 C 0.6632(3) 0.3645(3) 0.7225(2) 0.0673(10) Uani 1 1 d . . .
H30A H 0.7059 0.3785 0.6719 0.081 Uiso 1 1 calc R . .
C31 C 0.6957(3) 0.2610(3) 0.7541(2) 0.0559(8) Uani 1 1 d . . .
H31A H 0.7614 0.2049 0.7252 0.067 Uiso 1 1 calc R . .
C32 C 0.6319(2) 0.2395(2) 0.82818(19) 0.0439(6) Uani 1 1 d . . .
H32A H 0.6558 0.1691 0.8500 0.053 Uiso 1 1 calc R . .
C33 C 0.5168(2) 0.28254(19) 1.04946(18) 0.0350(6) Uani 1 1 d . . .
C34 C 0.6135(2) 0.2984(2) 1.05948(19) 0.0432(6) Uani 1 1 d . . .
H34A H 0.6466 0.3204 1.0068 0.052 Uiso 1 1 calc R . .
C35 C 0.6618(3) 0.2816(2) 1.1484(2) 0.0544(8) Uani 1 1 d . . .
H35A H 0.7275 0.2914 1.1547 0.065 Uiso 1 1 calc R . .
C36 C 0.6119(3) 0.2507(2) 1.2264(2) 0.0561(8) Uani 1 1 d . . .
H36A H 0.6433 0.2406 1.2858 0.067 Uiso 1 1 calc R . .
C37 C 0.5166(3) 0.2346(2) 1.2172(2) 0.0565(8) Uani 1 1 d . . .
H37A H 0.4836 0.2132 1.2703 0.068 Uiso 1 1 calc R . .
C38 C 0.4691(3) 0.2499(2) 1.12950(19) 0.0468(7) Uani 1 1 d . . .
H38A H 0.4045 0.2383 1.1238 0.056 Uiso 1 1 calc R . .
C39 C 0.2136(2) -0.0665(2) 0.57944(18) 0.0367(6) Uani 1 1 d . . .
C40 C 0.1450(3) -0.1084(2) 0.5465(2) 0.0513(7) Uani 1 1 d . . .
C41 C 0.0507(3) -0.1034(3) 0.6064(2) 0.0638(9) Uani 1 1 d . . .
H41A H 0.0018 -0.1292 0.5848 0.077 Uiso 1 1 calc R . .
C42 C 0.0298(3) -0.0611(3) 0.6964(2) 0.0537(8) Uani 1 1 d . . .
H42A H -0.0322 -0.0605 0.7355 0.064 Uiso 1 1 calc R . .
C43 C 0.0981(2) -0.0189(2) 0.73141(18) 0.0389(6) Uani 1 1 d . . .
C44 C 0.1888(2) -0.0209(2) 0.67027(17) 0.0366(6) Uani 1 1 d . . .
H44A H 0.2346 0.0090 0.6905 0.044 Uiso 1 1 calc R . .
C45 C 0.0761(2) 0.0281(2) 0.82827(18) 0.0376(6) Uani 1 1 d . . .
C46 C 0.1674(2) 0.0237(2) 0.87852(18) 0.0384(6) Uani 1 1 d . . .
H46A H 0.2434 -0.0140 0.8524 0.046 Uiso 1 1 calc R . .
C47 C 0.1476(2) 0.0740(2) 0.96607(18) 0.0402(6) Uani 1 1 d . . .
C48 C 0.0342(3) 0.1288(2) 1.00736(19) 0.0465(7) Uani 1 1 d . . .
C49 C -0.0563(3) 0.1312(2) 0.9602(2) 0.0541(8) Uani 1 1 d . . .
H49A H -0.1319 0.1663 0.9878 0.065 Uiso 1 1 calc R . .
C50 C -0.0357(2) 0.0817(2) 0.8721(2) 0.0476(7) Uani 1 1 d . . .
H50A H -0.0982 0.0844 0.8414 0.057 Uiso 1 1 calc R . .
C51 C 0.5143(4) -0.0308(3) 0.2576(3) 0.0747(10) Uani 1 1 d . . .
H51A H 0.4433 0.0149 0.2285 0.112 Uiso 1 1 calc R . .
H51B H 0.5794 -0.0360 0.2158 0.112 Uiso 1 1 calc R . .
H51C H 0.5155 -0.0009 0.3179 0.112 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 1.421(2) . ?
S1 O3 1.435(2) . ?
S1 O2 1.442(2) . ?
S1 C39 1.761(3) . ?
S2 O6 1.429(2) . ?
S2 O5 1.430(2) . ?
S2 O7 1.451(2) . ?
S2 C47 1.764(3) . ?
O4 C40 1.357(3) . ?
O4 H4O 0.85(2) . ?
O8 C48 1.366(3) . ?
O8 H8O 0.85(2) . ?
O9 C51 1.428(4) . ?
O9 H9O 0.85(2) . ?
N1 C1 1.514(3) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
N2 C20 1.527(3) . ?
N2 H2N1 0.86(3) . ?
N2 H2N2 0.86(3) . ?
N2 H2N3 0.86(3) . ?
C1 C2 1.525(3) . ?
C1 C14 1.528(3) . ?
C1 C8 1.537(3) . ?
C2 C7 1.376(4) . ?
C2 C3 1.392(4) . ?
C3 C4 1.373(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.362(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.389(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.378(4) . ?
C8 C9 1.385(4) . ?
C9 C10 1.384(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.364(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.363(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.387(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C19 1.365(4) . ?
C14 C15 1.383(4) . ?
C15 C16 1.378(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.348(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.360(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.402(5) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.528(3) . ?
C20 C33 1.530(3) . ?
C20 C27 1.530(3) . ?
C21 C26 1.376(4) . ?
C21 C22 1.376(4) . ?
C22 C23 1.380(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.361(5) . ?
C23 H23A 0.9300 . ?
C24 C25 1.364(5) . ?
C24 H24A 0.9300 . ?
C25 C26 1.387(4) . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9300 . ?
C27 C28 1.378(4) . ?
C27 C32 1.392(4) . ?
C28 C29 1.380(4) . ?
C28 H28A 0.9300 . ?
C29 C30 1.361(5) . ?
C29 H29A 0.9300 . ?
C30 C31 1.370(5) . ?
C30 H30A 0.9300 . ?
C31 C32 1.378(4) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
C33 C34 1.383(4) . ?
C33 C38 1.390(4) . ?
C34 C35 1.398(4) . ?
C34 H34A 0.9300 . ?
C35 C36 1.372(4) . ?
C35 H35A 0.9300 . ?
C36 C37 1.364(4) . ?
C36 H36A 0.9300 . ?
C37 C38 1.380(4) . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9300 . ?
C39 C40 1.377(4) . ?
C39 C44 1.391(3) . ?
C40 C41 1.396(4) . ?
C41 C42 1.365(4) . ?
C41 H41A 0.9300 . ?
C42 C43 1.388(4) . ?
C42 H42A 0.9300 . ?
C43 C44 1.384(3) . ?
C43 C45 1.479(4) . ?
C44 H44A 0.9300 . ?
C45 C50 1.393(3) . ?
C45 C46 1.396(4) . ?
C46 C47 1.383(3) . ?
C46 H46A 0.9300 . ?
C47 C48 1.397(4) . ?
C48 C49 1.375(4) . ?
C49 C50 1.383(4) . ?
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
O1 S1 O3 112.15(18) . . ?
O1 S1 O2 112.62(16) . . ?
O3 S1 O2 111.52(16) . . ?
O1 S1 C39 107.58(12) . . ?
O3 S1 C39 105.23(13) . . ?
O2 S1 C39 107.26(13) . . ?
O6 S2 O5 113.22(16) . . ?
O6 S2 O7 112.87(17) . . ?
O5 S2 O7 110.79(16) . . ?
O6 S2 C47 107.24(13) . . ?
O5 S2 C47 106.98(14) . . ?
O7 S2 C47 105.17(14) . . ?
C40 O4 H4O 101(3) . . ?
C48 O8 H8O 96(3) . . ?
C51 O9 H9O 108(2) . . ?
C1 N1 H1N1 112.5(18) . . ?
C1 N1 H1N2 111.4(19) . . ?
H1N1 N1 H1N2 106.7(14) . . ?
C1 N1 H1N3 111.4(19) . . ?
H1N1 N1 H1N3 107.2(14) . . ?
H1N2 N1 H1N3 107.4(14) . . ?
C20 N2 H2N1 112.5(18) . . ?
C20 N2 H2N2 112.1(18) . . ?
H2N1 N2 H2N2 107.5(14) . . ?
C20 N2 H2N3 108.9(18) . . ?
H2N1 N2 H2N3 107.5(14) . . ?
H2N2 N2 H2N3 108.1(14) . . ?
N1 C1 C2 105.8(2) . . ?
N1 C1 C14 108.3(2) . . ?
C2 C1 C14 110.7(2) . . ?
N1 C1 C8 106.97(19) . . ?
C2 C1 C8 112.8(2) . . ?
C14 C1 C8 111.9(2) . . ?
C7 C2 C3 118.0(3) . . ?
C7 C2 C1 122.8(2) . . ?
C3 C2 C1 119.2(2) . . ?
C4 C3 C2 121.6(3) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C7 120.5(3) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
C2 C7 C6 120.3(3) . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C13 C8 C9 118.1(3) . . ?
C13 C8 C1 121.2(2) . . ?
C9 C8 C1 120.6(2) . . ?
C10 C9 C8 120.8(3) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C11 C10 C9 120.4(3) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C12 C11 C10 119.4(3) . . ?
C12 C11 H11A 120.3 . . ?
C10 C11 H11A 120.3 . . ?
C11 C12 C13 120.7(3) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C8 C13 C12 120.6(3) . . ?
C8 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
C19 C14 C15 118.4(3) . . ?
C19 C14 C1 122.0(3) . . ?
C15 C14 C1 119.5(2) . . ?
C16 C15 C14 121.1(3) . . ?
C16 C15 H15A 119.5 . . ?
C14 C15 H15A 119.5 . . ?
C17 C16 C15 120.4(4) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C16 C17 C18 119.5(4) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
C17 C18 C19 120.9(4) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C14 C19 C18 119.6(4) . . ?
C14 C19 H19A 120.2 . . ?
C18 C19 H19A 120.2 . . ?
N2 C20 C21 107.73(19) . . ?
N2 C20 C33 106.15(19) . . ?
C21 C20 C33 111.8(2) . . ?
N2 C20 C27 107.42(19) . . ?
C21 C20 C27 110.9(2) . . ?
C33 C20 C27 112.6(2) . . ?
C26 C21 C22 117.7(3) . . ?
C26 C21 C20 121.8(2) . . ?
C22 C21 C20 120.4(2) . . ?
C21 C22 C23 121.4(3) . . ?
C21 C22 H22A 119.3 . . ?
C23 C22 H22A 119.3 . . ?
C24 C23 C22 120.4(4) . . ?
C24 C23 H23A 119.8 . . ?
C22 C23 H23A 119.8 . . ?
C23 C24 C25 119.0(3) . . ?
C23 C24 H24A 120.5 . . ?
C25 C24 H24A 120.5 . . ?
C24 C25 C26 120.9(3) . . ?
C24 C25 H25A 119.6 . . ?
C26 C25 H25A 119.6 . . ?
C21 C26 C25 120.6(3) . . ?
C21 C26 H26A 119.7 . . ?
C25 C26 H26A 119.7 . . ?
C28 C27 C32 117.9(3) . . ?
C28 C27 C20 120.6(2) . . ?
C32 C27 C20 121.4(2) . . ?
C27 C28 C29 121.0(3) . . ?
C27 C28 H28A 119.5 . . ?
C29 C28 H28A 119.5 . . ?
C30 C29 C28 120.4(3) . . ?
C30 C29 H29A 119.8 . . ?
C28 C29 H29A 119.8 . . ?
C29 C30 C31 119.6(3) . . ?
C29 C30 H30A 120.2 . . ?
C31 C30 H30A 120.2 . . ?
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 118.5(2) . . ?
C34 C33 C20 122.2(2) . . ?
C38 C33 C20 119.3(2) . . ?
C33 C34 C35 120.3(3) . . ?
C33 C34 H34A 119.8 . . ?
C35 C34 H34A 119.8 . . ?
C36 C35 C34 119.8(3) . . ?
C36 C35 H35A 120.1 . . ?
C34 C35 H35A 120.1 . . ?
C37 C36 C35 120.4(3) . . ?
C37 C36 H36A 119.8 . . ?
C35 C36 H36A 119.8 . . ?
C36 C37 C38 120.2(3) . . ?
C36 C37 H37A 119.9 . . ?
C38 C37 H37A 119.9 . . ?
C37 C38 C33 120.8(3) . . ?
C37 C38 H38A 119.6 . . ?
C33 C38 H38A 119.6 . . ?
C40 C39 C44 120.2(2) . . ?
C40 C39 S1 121.5(2) . . ?
C44 C39 S1 118.09(19) . . ?
O4 C40 C39 123.7(3) . . ?
O4 C40 C41 118.0(3) . . ?
C39 C40 C41 118.3(3) . . ?
C42 C41 C40 120.6(3) . . ?
C42 C41 H41A 119.7 . . ?
C40 C41 H41A 119.7 . . ?
C41 C42 C43 122.2(3) . . ?
C41 C42 H42A 118.9 . . ?
C43 C42 H42A 118.9 . . ?
C44 C43 C42 116.7(2) . . ?
C44 C43 C45 120.3(2) . . ?
C42 C43 C45 123.0(2) . . ?
C43 C44 C39 121.9(2) . . ?
C43 C44 H44A 119.0 . . ?
C39 C44 H44A 119.0 . . ?
C50 C45 C46 117.0(2) . . ?
C50 C45 C43 122.0(2) . . ?
C46 C45 C43 121.0(2) . . ?
C47 C46 C45 121.7(2) . . ?
C47 C46 H46A 119.1 . . ?
C45 C46 H46A 119.1 . . ?
C46 C47 C48 119.9(3) . . ?
C46 C47 S2 120.5(2) . . ?
C48 C47 S2 119.7(2) . . ?
O8 C48 C49 117.5(3) . . ?
O8 C48 C47 123.4(3) . . ?
C49 C48 C47 119.2(3) . . ?
C48 C49 C50 120.5(3) . . ?
C48 C49 H49A 119.7 . . ?
C50 C49 H49A 119.7 . . ?
C49 C50 C45 121.7(3) . . ?
C49 C50 H50A 119.1 . . ?
C45 C50 H50A 119.1 . . ?
O9 C51 H51A 109.5 . . ?
O9 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O9 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 122.6(3) . . . . ?
C14 C1 C2 C7 -120.3(3) . . . . ?
C8 C1 C2 C7 6.0(3) . . . . ?
N1 C1 C2 C3 -58.5(3) . . . . ?
C14 C1 C2 C3 58.6(3) . . . . ?
C8 C1 C2 C3 -175.1(2) . . . . ?
C7 C2 C3 C4 1.6(4) . . . . ?
C1 C2 C3 C4 -177.4(3) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C3 C4 C5 C6 -0.3(5) . . . . ?
C4 C5 C6 C7 1.1(5) . . . . ?
C3 C2 C7 C6 -0.8(4) . . . . ?
C1 C2 C7 C6 178.1(2) . . . . ?
C5 C6 C7 C2 -0.5(5) . . . . ?
N1 C1 C8 C13 136.6(3) . . . . ?
C2 C1 C8 C13 -107.5(3) . . . . ?
C14 C1 C8 C13 18.2(3) . . . . ?
N1 C1 C8 C9 -46.8(3) . . . . ?
C2 C1 C8 C9 69.0(3) . . . . ?
C14 C1 C8 C9 -165.3(2) . . . . ?
C13 C8 C9 C10 -0.3(4) . . . . ?
C1 C8 C9 C10 -176.9(3) . . . . ?
C8 C9 C10 C11 0.5(5) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
C10 C11 C12 C13 0.6(6) . . . . ?
C9 C8 C13 C12 0.1(4) . . . . ?
C1 C8 C13 C12 176.8(3) . . . . ?
C11 C12 C13 C8 -0.3(5) . . . . ?
N1 C1 C14 C19 -35.5(4) . . . . ?
C2 C1 C14 C19 -151.1(3) . . . . ?
C8 C1 C14 C19 82.1(4) . . . . ?
N1 C1 C14 C15 147.1(3) . . . . ?
C2 C1 C14 C15 31.6(3) . . . . ?
C8 C1 C14 C15 -95.2(3) . . . . ?
C19 C14 C15 C16 -1.1(5) . . . . ?
C1 C14 C15 C16 176.3(3) . . . . ?
C14 C15 C16 C17 0.5(6) . . . . ?
C15 C16 C17 C18 0.9(7) . . . . ?
C16 C17 C18 C19 -1.8(8) . . . . ?
C15 C14 C19 C18 0.3(6) . . . . ?
C1 C14 C19 C18 -177.1(4) . . . . ?
C17 C18 C19 C14 1.1(8) . . . . ?
N2 C20 C21 C26 140.5(2) . . . . ?
C33 C20 C21 C26 24.2(3) . . . . ?
C27 C20 C21 C26 -102.3(3) . . . . ?
N2 C20 C21 C22 -43.6(3) . . . . ?
C33 C20 C21 C22 -159.8(3) . . . . ?
C27 C20 C21 C22 73.7(3) . . . . ?
C26 C21 C22 C23 -1.0(5) . . . . ?
C20 C21 C22 C23 -177.1(3) . . . . ?
C21 C22 C23 C24 0.5(7) . . . . ?
C22 C23 C24 C25 0.7(6) . . . . ?
C23 C24 C25 C26 -1.4(6) . . . . ?
C22 C21 C26 C25 0.3(5) . . . . ?
C20 C21 C26 C25 176.3(3) . . . . ?
C24 C25 C26 C21 0.9(5) . . . . ?
N2 C20 C27 C28 143.8(2) . . . . ?
C21 C20 C27 C28 26.3(3) . . . . ?
C33 C20 C27 C28 -99.7(3) . . . . ?
N2 C20 C27 C32 -39.5(3) . . . . ?
C21 C20 C27 C32 -157.0(2) . . . . ?
C33 C20 C27 C32 77.0(3) . . . . ?
C32 C27 C28 C29 1.2(4) . . . . ?
C20 C27 C28 C29 178.0(3) . . . . ?
C27 C28 C29 C30 1.2(5) . . . . ?
C28 C29 C30 C31 -2.3(6) . . . . ?
C29 C30 C31 C32 0.9(5) . . . . ?
C30 C31 C32 C27 1.5(4) . . . . ?
C28 C27 C32 C31 -2.5(4) . . . . ?
C20 C27 C32 C31 -179.3(2) . . . . ?
N2 C20 C33 C34 124.8(2) . . . . ?
C21 C20 C33 C34 -118.0(3) . . . . ?
C27 C20 C33 C34 7.6(3) . . . . ?
N2 C20 C33 C38 -55.6(3) . . . . ?
C21 C20 C33 C38 61.6(3) . . . . ?
C27 C20 C33 C38 -172.9(2) . . . . ?
C38 C33 C34 C35 0.1(4) . . . . ?
C20 C33 C34 C35 179.7(2) . . . . ?
C33 C34 C35 C36 -0.9(4) . . . . ?
C34 C35 C36 C37 1.0(5) . . . . ?
C35 C36 C37 C38 -0.4(5) . . . . ?
C36 C37 C38 C33 -0.4(4) . . . . ?
C34 C33 C38 C37 0.5(4) . . . . ?
C20 C33 C38 C37 -179.0(2) . . . . ?
O1 S1 C39 C40 148.6(2) . . . . ?
O3 S1 C39 C40 -91.7(3) . . . . ?
O2 S1 C39 C40 27.2(3) . . . . ?
O1 S1 C39 C44 -35.5(3) . . . . ?
O3 S1 C39 C44 84.2(2) . . . . ?
O2 S1 C39 C44 -156.9(2) . . . . ?
C44 C39 C40 O4 -179.2(3) . . . . ?
S1 C39 C40 O4 -3.3(4) . . . . ?
C44 C39 C40 C41 0.2(4) . . . . ?
S1 C39 C40 C41 176.1(2) . . . . ?
O4 C40 C41 C42 177.4(3) . . . . ?
C39 C40 C41 C42 -2.1(5) . . . . ?
C40 C41 C42 C43 1.8(5) . . . . ?
C41 C42 C43 C44 0.5(5) . . . . ?
C41 C42 C43 C45 179.4(3) . . . . ?
C42 C43 C44 C39 -2.3(4) . . . . ?
C45 C43 C44 C39 178.7(2) . . . . ?
C40 C39 C44 C43 2.0(4) . . . . ?
S1 C39 C44 C43 -174.0(2) . . . . ?
C44 C43 C45 C50 146.6(3) . . . . ?
C42 C43 C45 C50 -32.4(4) . . . . ?
C44 C43 C45 C46 -31.1(4) . . . . ?
C42 C43 C45 C46 149.9(3) . . . . ?
C50 C45 C46 C47 -2.6(4) . . . . ?
C43 C45 C46 C47 175.2(2) . . . . ?
C45 C46 C47 C48 1.6(4) . . . . ?
C45 C46 C47 S2 -178.32(19) . . . . ?
O6 S2 C47 C46 -17.2(3) . . . . ?
O5 S2 C47 C46 104.6(2) . . . . ?
O7 S2 C47 C46 -137.6(2) . . . . ?
O6 S2 C47 C48 162.9(2) . . . . ?
O5 S2 C47 C48 -75.3(2) . . . . ?
O7 S2 C47 C48 42.5(3) . . . . ?
C46 C47 C48 O8 179.5(2) . . . . ?
S2 C47 C48 O8 -0.7(4) . . . . ?
C46 C47 C48 C49 0.4(4) . . . . ?
S2 C47 C48 C49 -179.7(2) . . . . ?
O8 C48 C49 C50 179.7(3) . . . . ?
C47 C48 C49 C50 -1.2(4) . . . . ?
C48 C49 C50 C45 0.1(4) . . . . ?
C46 C45 C50 C49 1.8(4) . . . . ?
C43 C45 C50 C49 -176.0(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
O4 H4O O2 0.85(2) 1.88(2) 2.683(3) 155(5) .
O8 H8O O7 0.85(2) 1.951(16) 2.783(4) 164(4) .
O9 H9O O2 0.85(2) 2.112(16) 2.922(3) 160(3) .
N1 H1N1 O3 0.86(3) 1.908(14) 2.745(3) 162(3) .
N1 H1N2 O9 0.86(3) 2.142(16) 2.957(3) 157(3) .
N1 H1N3 O1 0.86(3) 1.920(11) 2.775(3) 170(2) 2_656
N2 H2N1 O5 0.86(3) 1.961(10) 2.821(3) 175(3) .
N2 H2N2 O6 0.86(3) 1.937(11) 2.787(3) 168(2) 2_657
N2 H2N3 O9 0.86(3) 2.139(12) 2.980(3) 165(2) 2_656

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.048
_database_code_depnum_ccdc_archive 'CCDC 1025997'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C12 H8 O8 S2, 2(C19 H18 N), 2(C2 H6 O), 2(H2 O)'
_chemical_formula_sum            'C54 H60 N2 O12 S2'
_chemical_formula_weight         993.16

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                   9.6061(19)
_cell_length_b                   12.081(2)
_cell_length_c                   12.588(3)
_cell_angle_alpha                68.92(3)
_cell_angle_beta                 72.30(3)
_cell_angle_gamma                82.30(3)
_cell_volume                     1298.1(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    6191
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      25.00

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             526
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9644
_exptl_absorpt_correction_T_max  0.9756
_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            10052
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4514
_reflns_number_gt                2804
_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)+(0.1148P)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         4514
_refine_ls_number_parameters     332
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.2058
_refine_ls_wR_factor_gt          0.1805
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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 0.19096(10) 0.87075(6) 0.37331(7) 0.0660(3) Uani 1 1 d . . .
O1 O 0.1574(3) 0.93848(18) 0.26279(17) 0.0825(7) Uani 1 1 d . . .
O1W O 0.4597(10) 0.9905(8) 0.8327(7) 0.172(2) Uani 0.50 1 d P A 1
O1W' O 0.4493(10) 0.9793(8) 0.9751(7) 0.172(2) Uani 0.50 1 d P . 2
O2 O 0.3345(3) 0.8922(2) 0.3710(3) 0.1089(9) Uani 1 1 d . . .
O3 O 0.0762(3) 0.88664(18) 0.47279(18) 0.0820(7) Uani 1 1 d . . .
O4 O 0.4396(3) 0.7301(2) 0.2530(3) 0.0915(8) Uani 1 1 d D . .
H4O H 0.439(5) 0.790(3) 0.274(4) 0.137 Uiso 1 1 d D . .
O5 O 0.3064(5) 0.9794(4) 0.6861(4) 0.1503(14) Uani 1 1 d D . .
H5O H 0.3499 0.9780 0.7334 0.225 Uiso 1 1 calc RD . .
N1 N 0.0526(3) 0.88095(18) 0.70204(19) 0.0565(6) Uani 1 1 d D . .
H1N1 H -0.013(2) 0.936(2) 0.713(2) 0.085 Uiso 1 1 d D . .
H1N2 H 0.066(3) 0.883(3) 0.6302(14) 0.085 Uiso 1 1 d D . .
H1N3 H 0.1322(16) 0.902(3) 0.707(3) 0.085 Uiso 1 1 d D . .
C1 C 0.0215(3) 0.7564(2) 0.7918(2) 0.0529(7) Uani 1 1 d . . .
C2 C 0.1239(3) 0.6695(2) 0.7394(2) 0.0524(7) Uani 1 1 d . . .
C3 C 0.2648(4) 0.6991(3) 0.6696(3) 0.0664(8) Uani 1 1 d . . .
H3A H 0.2974 0.7746 0.6512 0.080 Uiso 1 1 calc R . .
C4 C 0.3575(4) 0.6176(3) 0.6268(3) 0.0766(9) Uani 1 1 d . . .
H4A H 0.4514 0.6390 0.5786 0.092 Uiso 1 1 calc R . .
C5 C 0.3115(4) 0.5052(3) 0.6552(3) 0.0803(10) Uani 1 1 d . . .
H5A H 0.3746 0.4501 0.6272 0.096 Uiso 1 1 calc R . .
C6 C 0.1759(4) 0.4748(3) 0.7232(3) 0.0768(10) Uani 1 1 d . . .
H6A H 0.1456 0.3984 0.7420 0.092 Uiso 1 1 calc R . .
C7 C 0.0788(4) 0.5558(2) 0.7664(3) 0.0645(8) Uani 1 1 d . . .
H7A H -0.0154 0.5336 0.8129 0.077 Uiso 1 1 calc R . .
C8 C -0.1380(3) 0.7330(2) 0.8153(3) 0.0566(7) Uani 1 1 d . . .
C9 C -0.2066(4) 0.7734(3) 0.7245(3) 0.0708(9) Uani 1 1 d . . .
H9A H -0.1545 0.8174 0.6483 0.085 Uiso 1 1 calc R . .
C10 C -0.3502(4) 0.7488(4) 0.7467(4) 0.0907(11) Uani 1 1 d . . .
H10A H -0.3949 0.7781 0.6857 0.109 Uiso 1 1 calc R . .
C11 C -0.4278(5) 0.6827(5) 0.8558(5) 0.1077(14) Uani 1 1 d . . .
H11A H -0.5246 0.6659 0.8692 0.129 Uiso 1 1 calc R . .
C12 C -0.3635(5) 0.6409(4) 0.9459(4) 0.1088(14) Uani 1 1 d . . .
H12A H -0.4167 0.5952 1.0209 0.131 Uiso 1 1 calc R . .
C13 C -0.2189(4) 0.6657(3) 0.9268(3) 0.0812(10) Uani 1 1 d . . .
H13A H -0.1764 0.6371 0.9892 0.097 Uiso 1 1 calc R . .
C14 C 0.0531(3) 0.7586(2) 0.9031(2) 0.0578(7) Uani 1 1 d . . .
C15 C -0.0180(5) 0.8409(3) 0.9553(3) 0.0861(11) Uani 1 1 d . . .
H15A H -0.0838 0.8953 0.9213 0.103 Uiso 1 1 calc R . .
C16 C 0.0057(6) 0.8446(3) 1.0563(3) 0.1027(14) Uani 1 1 d . . .
H16A H -0.0448 0.8996 1.0914 0.123 Uiso 1 1 calc R . .
C17 C 0.1060(5) 0.7650(4) 1.1048(3) 0.1000(13) Uani 1 1 d . . .
H17A H 0.1254 0.7683 1.1716 0.120 Uiso 1 1 calc R . .
C18 C 0.1768(4) 0.6818(4) 1.0559(3) 0.0873(11) Uani 1 1 d . . .
H18A H 0.2423 0.6276 1.0903 0.105 Uiso 1 1 calc R . .
C19 C 0.1507(4) 0.6784(3) 0.9550(3) 0.0674(8) Uani 1 1 d . . .
H19A H 0.1992 0.6217 0.9216 0.081 Uiso 1 1 calc R . .
C20 C 0.1945(3) 0.7206(2) 0.3858(2) 0.0576(8) Uani 1 1 d . . .
C21 C 0.0737(3) 0.6527(2) 0.4547(2) 0.0582(8) Uani 1 1 d . . .
H21A H -0.0050 0.6865 0.4982 0.070 Uiso 1 1 calc R . .
C22 C 0.0636(3) 0.5354(2) 0.4622(2) 0.0571(7) Uani 1 1 d . . .
C23 C 0.1854(4) 0.4923(3) 0.3916(3) 0.0667(8) Uani 1 1 d . . .
H23A H 0.1833 0.4160 0.3905 0.080 Uiso 1 1 calc R . .
C24 C 0.3063(4) 0.5570(3) 0.3246(3) 0.0705(9) Uani 1 1 d . . .
H24A H 0.3844 0.5236 0.2802 0.085 Uiso 1 1 calc R . .
C25 C 0.3154(4) 0.6722(3) 0.3212(3) 0.0656(8) Uani 1 1 d . . .
C26 C 0.3371(8) 1.0860(7) 0.5874(7) 0.163(2) Uani 1 1 d . . .
H26A H 0.4418 1.0963 0.5552 0.195 Uiso 1 1 calc R . .
H26B H 0.2978 1.0839 0.5257 0.195 Uiso 1 1 calc R . .
C27 C 0.2701(8) 1.1805(7) 0.6290(7) 0.185(3) Uani 1 1 d . . .
H27A H 0.2945 1.2548 0.5660 0.278 Uiso 1 1 calc R . .
H27B H 0.3045 1.1779 0.6939 0.278 Uiso 1 1 calc R . .
H27C H 0.1659 1.1725 0.6551 0.278 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 1.426(3) . ?
S1 O1 1.446(2) . ?
S1 O3 1.448(2) . ?
S1 C20 1.760(3) . ?
O4 C25 1.348(4) . ?
O4 H4O 0.85(3) . ?
O5 C26 1.421(7) . ?
O5 H5O 0.8200 . ?
N1 C1 1.524(3) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
C1 C8 1.515(4) . ?
C1 C2 1.527(4) . ?
C1 C14 1.531(4) . ?
C2 C3 1.384(4) . ?
C2 C7 1.387(4) . ?
C3 C4 1.381(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.373(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.338(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.398(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.386(5) . ?
C8 C9 1.396(4) . ?
C9 C10 1.374(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.351(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.361(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.390(6) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.379(4) . ?
C14 C19 1.385(4) . ?
C15 C16 1.375(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.383(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.364(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.382(4) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.380(4) . ?
C20 C25 1.392(4) . ?
C21 C22 1.400(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.403(4) . ?
C22 C22 1.456(6) 2_566 ?
C23 C24 1.357(5) . ?
C23 H23A 0.9300 . ?
C24 C25 1.390(4) . ?
C24 H24A 0.9300 . ?
C26 C27 1.420(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 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 111.93(18) . . ?
O2 S1 O3 114.62(17) . . ?
O1 S1 O3 110.77(13) . . ?
O2 S1 C20 105.28(15) . . ?
O1 S1 C20 106.15(12) . . ?
O3 S1 C20 107.49(15) . . ?
C25 O4 H4O 106(3) . . ?
C26 O5 H5O 109.5 . . ?
C1 N1 H1N1 116(2) . . ?
C1 N1 H1N2 112(2) . . ?
H1N1 N1 H1N2 106.1(14) . . ?
C1 N1 H1N3 107(2) . . ?
H1N1 N1 H1N3 106.8(15) . . ?
H1N2 N1 H1N3 107.9(15) . . ?
C8 C1 N1 107.9(2) . . ?
C8 C1 C2 112.2(2) . . ?
N1 C1 C2 107.8(2) . . ?
C8 C1 C14 111.3(2) . . ?
N1 C1 C14 105.4(2) . . ?
C2 C1 C14 111.9(2) . . ?
C3 C2 C7 118.4(2) . . ?
C3 C2 C1 121.6(3) . . ?
C7 C2 C1 120.0(3) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
C6 C5 C4 120.0(3) . . ?
C6 C5 H5A 120.0 . . ?
C4 C5 H5A 120.0 . . ?
C5 C6 C7 121.1(3) . . ?
C5 C6 H6A 119.4 . . ?
C7 C6 H6A 119.4 . . ?
C2 C7 C6 119.6(3) . . ?
C2 C7 H7A 120.2 . . ?
C6 C7 H7A 120.2 . . ?
C13 C8 C9 117.7(3) . . ?
C13 C8 C1 120.9(3) . . ?
C9 C8 C1 121.3(3) . . ?
C10 C9 C8 120.6(3) . . ?
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 119.6(4) . . ?
C10 C11 H11A 120.2 . . ?
C12 C11 H11A 120.2 . . ?
C11 C12 C13 120.7(4) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C8 C13 C12 120.3(4) . . ?
C8 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C15 C14 C19 118.4(3) . . ?
C15 C14 C1 119.9(3) . . ?
C19 C14 C1 121.7(2) . . ?
C16 C15 C14 121.7(3) . . ?
C16 C15 H15A 119.1 . . ?
C14 C15 H15A 119.1 . . ?
C15 C16 C17 118.7(4) . . ?
C15 C16 H16A 120.7 . . ?
C17 C16 H16A 120.7 . . ?
C18 C17 C16 120.9(3) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 119.8(4) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C18 C19 C14 120.6(3) . . ?
C18 C19 H19A 119.7 . . ?
C14 C19 H19A 119.7 . . ?
C21 C20 C25 120.0(3) . . ?
C21 C20 S1 119.7(2) . . ?
C25 C20 S1 120.2(3) . . ?
C20 C21 C22 123.2(2) . . ?
C20 C21 H21A 118.4 . . ?
C22 C21 H21A 118.4 . . ?
C21 C22 C23 114.7(3) . . ?
C21 C22 C22 122.2(3) . 2_566 ?
C23 C22 C22 123.1(3) . 2_566 ?
C24 C23 C22 123.0(3) . . ?
C24 C23 H23A 118.5 . . ?
C22 C23 H23A 118.5 . . ?
C23 C24 C25 121.3(3) . . ?
C23 C24 H24A 119.4 . . ?
C25 C24 H24A 119.4 . . ?
O4 C25 C24 117.6(3) . . ?
O4 C25 C20 124.7(3) . . ?
C24 C25 C20 117.8(3) . . ?
C27 C26 O5 106.9(6) . . ?
C27 C26 H26A 110.3 . . ?
O5 C26 H26A 110.3 . . ?
C27 C26 H26B 110.3 . . ?
O5 C26 H26B 110.3 . . ?
H26A C26 H26B 108.6 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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
C8 C1 C2 C3 154.0(2) . . . . ?
N1 C1 C2 C3 35.4(3) . . . . ?
C14 C1 C2 C3 -80.1(3) . . . . ?
C8 C1 C2 C7 -29.3(3) . . . . ?
N1 C1 C2 C7 -147.9(3) . . . . ?
C14 C1 C2 C7 96.6(3) . . . . ?
C7 C2 C3 C4 0.7(4) . . . . ?
C1 C2 C3 C4 177.5(3) . . . . ?
C2 C3 C4 C5 -1.3(5) . . . . ?
C3 C4 C5 C6 0.9(5) . . . . ?
C4 C5 C6 C7 0.0(5) . . . . ?
C3 C2 C7 C6 0.2(4) . . . . ?
C1 C2 C7 C6 -176.6(3) . . . . ?
C5 C6 C7 C2 -0.6(5) . . . . ?
N1 C1 C8 C13 -145.0(3) . . . . ?
C2 C1 C8 C13 96.3(3) . . . . ?
C14 C1 C8 C13 -29.9(3) . . . . ?
N1 C1 C8 C9 38.1(3) . . . . ?
C2 C1 C8 C9 -80.6(3) . . . . ?
C14 C1 C8 C9 153.2(2) . . . . ?
C13 C8 C9 C10 1.3(4) . . . . ?
C1 C8 C9 C10 178.3(3) . . . . ?
C8 C9 C10 C11 -1.6(5) . . . . ?
C9 C10 C11 C12 0.9(6) . . . . ?
C10 C11 C12 C13 0.2(6) . . . . ?
C9 C8 C13 C12 -0.3(5) . . . . ?
C1 C8 C13 C12 -177.3(3) . . . . ?
C11 C12 C13 C8 -0.4(6) . . . . ?
C8 C1 C14 C15 -60.4(4) . . . . ?
N1 C1 C14 C15 56.2(4) . . . . ?
C2 C1 C14 C15 173.1(3) . . . . ?
C8 C1 C14 C19 118.6(3) . . . . ?
N1 C1 C14 C19 -124.8(3) . . . . ?
C2 C1 C14 C19 -7.8(4) . . . . ?
C19 C14 C15 C16 -0.1(6) . . . . ?
C1 C14 C15 C16 179.0(3) . . . . ?
C14 C15 C16 C17 1.4(6) . . . . ?
C15 C16 C17 C18 -2.1(7) . . . . ?
C16 C17 C18 C19 1.5(6) . . . . ?
C17 C18 C19 C14 -0.1(6) . . . . ?
C15 C14 C19 C18 -0.6(5) . . . . ?
C1 C14 C19 C18 -179.6(3) . . . . ?
O2 S1 C20 C21 142.6(2) . . . . ?
O1 S1 C20 C21 -98.6(2) . . . . ?
O3 S1 C20 C21 20.0(3) . . . . ?
O2 S1 C20 C25 -41.1(3) . . . . ?
O1 S1 C20 C25 77.7(3) . . . . ?
O3 S1 C20 C25 -163.7(2) . . . . ?
C25 C20 C21 C22 -1.2(4) . . . . ?
S1 C20 C21 C22 175.1(2) . . . . ?
C20 C21 C22 C23 -1.5(4) . . . . ?
C20 C21 C22 C22 178.4(3) . . . 2_566 ?
C21 C22 C23 C24 2.5(4) . . . . ?
C22 C22 C23 C24 -177.4(3) 2_566 . . . ?
C22 C23 C24 C25 -0.8(5) . . . . ?
C23 C24 C25 O4 179.7(3) . . . . ?
C23 C24 C25 C20 -2.0(5) . . . . ?
C21 C20 C25 O4 -178.8(3) . . . . ?
S1 C20 C25 O4 4.9(4) . . . . ?
C21 C20 C25 C24 3.0(4) . . . . ?
S1 C20 C25 C24 -173.3(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
O4 H4O O2 0.85(3) 2.00(3) 2.777(4) 150(5) .
O5 H5O O1W 0.82 1.92 2.734(11) 174.0 .
N1 H1N1 O1 0.86(3) 1.960(10) 2.828(3) 178(2) 2_576
N1 H1N2 O3 0.86(3) 1.940(10) 2.801(3) 175(2) .
N1 H1N3 O5 0.86(3) 1.929(14) 2.776(4) 167(3) .

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.070
_database_code_depnum_ccdc_archive 'CCDC 1025998'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 2(C3 H8 O)'
_chemical_formula_sum            'C56 H60 N2 O10 S2'
_chemical_formula_weight         985.18

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   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   25.2368(15)
_cell_length_b                   7.9675(4)
_cell_length_c                   28.3845(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.958(7)
_cell_angle_gamma                90.00
_cell_volume                     5293.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2551
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      27.49

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2088
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9673
_exptl_absorpt_correction_T_max  0.9780
_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            9921
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6065
_reflns_number_gt                4120
_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)+(0.0871P)²+6.7076P] 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         6065
_refine_ls_number_parameters     347
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1983
_refine_ls_wR_factor_gt          0.1755
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.029
_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 0.30415(2) 0.19396(9) 0.20291(2) 0.0414(2) Uani 1 1 d . . .
O1 O 0.28663(16) 0.0168(5) 0.19624(15) 0.0766(10) Uani 0.662(2) 1 d P A 1
O2 O 0.31547(12) 0.2399(5) 0.25549(11) 0.0577(8) Uani 0.662(2) 1 d P A 1
O3 O 0.26525(13) 0.3027(6) 0.16688(14) 0.0772(11) Uani 0.662(2) 1 d P A 1
O1' O 0.2634(3) 0.1216(10) 0.1550(3) 0.0766(10) Uani 0.338(2) 1 d P A 2
O2' O 0.3148(2) 0.0910(10) 0.2430(2) 0.0577(8) Uani 0.338(2) 1 d P A 2
O3' O 0.2874(3) 0.3687(11) 0.2054(3) 0.0772(11) Uani 0.338(2) 1 d P A 2
O4 O 0.31880(9) 0.2510(4) 0.10137(7) 0.0707(7) Uani 1 1 d D A .
H4O H 0.2937(14) 0.246(6) 0.1143(16) 0.106 Uiso 1 1 d D . .
O5 O 0.24363(15) 0.7887(4) 0.12265(13) 0.0984(10) Uani 1 1 d D . .
H5O H 0.252(2) 0.874(4) 0.1422(17) 0.148 Uiso 1 1 d D . .
N1 N 0.18753(9) 0.5554(3) 0.16039(8) 0.0475(6) Uani 1 1 d D . .
H1N1 H 0.2117(11) 0.474(2) 0.1682(10) 0.071 Uiso 1 1 d D . .
H1N2 H 0.2000(12) 0.632(2) 0.1458(10) 0.071 Uiso 1 1 d D . .
H1N3 H 0.1872(13) 0.597(3) 0.1883(7) 0.071 Uiso 1 1 d D . .
C1 C 0.36871(10) 0.2128(3) 0.19251(9) 0.0361(5) Uani 1 1 d . A .
C2 C 0.36743(11) 0.2399(4) 0.14374(10) 0.0494(7) Uani 1 1 d . . .
C3 C 0.41922(13) 0.2570(5) 0.13750(12) 0.0708(11) Uani 1 1 d . A .
H3A H 0.4194 0.2725 0.1051 0.085 Uiso 1 1 calc R . .
C4 C 0.47009(12) 0.2513(5) 0.17849(11) 0.0626(9) Uani 1 1 d . . .
H4A H 0.5040 0.2653 0.1732 0.075 Uiso 1 1 calc R A .
C5 C 0.47244(10) 0.2251(3) 0.22776(9) 0.0399(6) Uani 1 1 d . . .
C6 C 0.42021(10) 0.2042(3) 0.23354(9) 0.0386(5) Uani 1 1 d . . .
H6A H 0.4200 0.1839 0.2658 0.046 Uiso 1 1 calc R A .
C7 C 0.12997(10) 0.4860(3) 0.12604(9) 0.0412(6) Uani 1 1 d . . .
C8 C 0.10728(11) 0.3799(4) 0.15959(10) 0.0449(6) Uani 1 1 d . . .
C9 C 0.05066(13) 0.3894(4) 0.15508(14) 0.0645(9) Uani 1 1 d . . .
H9A H 0.0254 0.4591 0.1307 0.077 Uiso 1 1 calc R . .
C10 C 0.03147(18) 0.2957(5) 0.1867(2) 0.0875(13) Uani 1 1 d . . .
H10A H -0.0065 0.3045 0.1834 0.105 Uiso 1 1 calc R . .
C11 C 0.06734(19) 0.1907(6) 0.22242(16) 0.0807(11) Uani 1 1 d . . .
H11A H 0.0541 0.1291 0.2436 0.097 Uiso 1 1 calc R . .
C12 C 0.12297(17) 0.1768(6) 0.22679(14) 0.0816(11) Uani 1 1 d . . .
H12A H 0.1476 0.1042 0.2507 0.098 Uiso 1 1 calc R . .
C13 C 0.14269(14) 0.2705(5) 0.19584(12) 0.0672(10) Uani 1 1 d . . .
H13A H 0.1807 0.2602 0.1993 0.081 Uiso 1 1 calc R . .
C14 C 0.09032(12) 0.6345(3) 0.10285(11) 0.0478(6) Uani 1 1 d . . .
C15 C 0.09132(13) 0.7800(4) 0.12895(12) 0.0508(7) Uani 1 1 d . . .
H15A H 0.1195 0.7956 0.1610 0.061 Uiso 1 1 calc R . .
C16 C 0.05059(15) 0.9047(4) 0.10801(14) 0.0610(8) Uani 1 1 d . . .
H16A H 0.0519 1.0017 0.1266 0.073 Uiso 1 1 calc R . .
C17 C 0.00945(17) 0.8886(5) 0.06157(16) 0.0803(11) Uani 1 1 d . . .
H17A H -0.0175 0.9729 0.0481 0.096 Uiso 1 1 calc R . .
C18 C 0.0081(2) 0.7484(6) 0.03516(19) 0.120(2) Uani 1 1 d . . .
H18A H -0.0203 0.7356 0.0031 0.144 Uiso 1 1 calc R . .
C19 C 0.04822(18) 0.6216(5) 0.05453(16) 0.1023(17) Uani 1 1 d . . .
H19A H 0.0469 0.5270 0.0349 0.123 Uiso 1 1 calc R . .
C20 C 0.14218(11) 0.3818(3) 0.08553(9) 0.0408(6) Uani 1 1 d . . .
C21 C 0.13403(13) 0.2115(4) 0.08054(10) 0.0495(7) Uani 1 1 d . . .
H21A H 0.1194 0.1556 0.1018 0.059 Uiso 1 1 calc R . .
C22 C 0.14709(15) 0.1210(4) 0.04476(12) 0.0638(8) Uani 1 1 d . . .
H22A H 0.1408 0.0058 0.0420 0.077 Uiso 1 1 calc R . .
C23 C 0.16919(15) 0.2001(5) 0.01330(12) 0.0675(9) Uani 1 1 d . . .
H23A H 0.1781 0.1394 -0.0107 0.081 Uiso 1 1 calc R . .
C24 C 0.17789(18) 0.3697(5) 0.01779(12) 0.0788(11) Uani 1 1 d . . .
H24A H 0.1932 0.4245 -0.0032 0.095 Uiso 1 1 calc R . .
C25 C 0.16420(16) 0.4605(4) 0.05314(11) 0.0672(9) Uani 1 1 d . . .
H25A H 0.1698 0.5761 0.0553 0.081 Uiso 1 1 calc R . .
C26 C 0.2966(4) 0.7315(14) 0.1251(4) 0.104(2) Uani 0.50 1 d PD B 3
H26A H 0.2984 0.6108 0.1298 0.125 Uiso 0.50 1 calc PR B 3
H26B H 0.3262 0.7812 0.1544 0.125 Uiso 0.50 1 calc PR B 3
C27 C 0.3081(5) 0.773(2) 0.0785(5) 0.136(3) Uani 0.50 1 d PD B 3
H27A H 0.2802 0.7149 0.0499 0.163 Uiso 0.50 1 calc PR B 3
H27B H 0.3022 0.8926 0.0721 0.163 Uiso 0.50 1 calc PR B 3
C28 C 0.3663(4) 0.7294(10) 0.0805(3) 0.178(3) Uani 0.50 1 d PD B 3
H28A H 0.3932 0.8113 0.1006 0.268 Uiso 0.50 1 calc PR B 3
H28B H 0.3664 0.7283 0.0467 0.268 Uiso 0.50 1 calc PR B 3
H28C H 0.3768 0.6205 0.0956 0.268 Uiso 0.50 1 calc PR B 3
C26' C 0.2762(4) 0.7903(14) 0.0886(4) 0.104(2) Uani 0.50 1 d PD B 4
H26C H 0.2753 0.9019 0.0747 0.125 Uiso 0.50 1 calc PR B 4
H26D H 0.2588 0.7132 0.0606 0.125 Uiso 0.50 1 calc PR B 4
C27' C 0.3367(5) 0.7393(19) 0.1179(4) 0.136(3) Uani 0.50 1 d PD B 4
H27C H 0.3378 0.6312 0.1339 0.163 Uiso 0.50 1 calc PR B 4
H27D H 0.3554 0.8213 0.1441 0.163 Uiso 0.50 1 calc PR B 4
C28' C 0.3663(4) 0.7294(10) 0.0805(3) 0.178(3) Uani 0.50 1 d PD B 4
H28D H 0.3440 0.6617 0.0520 0.268 Uiso 0.50 1 calc PR B 4
H28E H 0.4034 0.6799 0.0968 0.268 Uiso 0.50 1 calc PR B 4
H28F H 0.3703 0.8403 0.0690 0.268 Uiso 0.50 1 calc PR B 4


_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' 1.346(6) . ?
S1 O3 1.418(3) . ?
S1 O2 1.457(3) . ?
S1 O3' 1.464(9) . ?
S1 O1 1.470(4) . ?
S1 O1' 1.480(7) . ?
S1 C1 1.767(2) . ?
O4 C2 1.363(3) . ?
O4 H4O 0.85(4) . ?
O5 C26 1.390(8) . ?
O5 C26' 1.484(12) . ?
O5 H5O 0.85(4) . ?
N1 C7 1.519(3) . ?
N1 H1N1 0.86(4) . ?
N1 H1N2 0.86(4) . ?
N1 H1N3 0.86(4) . ?
C1 C6 1.385(3) . ?
C1 C2 1.389(3) . ?
C2 C3 1.390(4) . ?
C3 C4 1.374(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.393(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.398(3) . ?
C5 C5 1.489(5) 2_655 ?
C6 H6A 0.9300 . ?
C7 C14 1.530(4) . ?
C7 C8 1.535(4) . ?
C7 C20 1.540(3) . ?
C8 C9 1.388(4) . ?
C8 C13 1.389(4) . ?
C9 C10 1.386(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.365(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.367(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.380(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.371(4) . ?
C14 C19 1.390(4) . ?
C15 C16 1.393(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.345(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.339(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.390(5) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.372(4) . ?
C20 C25 1.389(4) . ?
C21 C22 1.382(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.370(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.367(5) . ?
C23 H23A 0.9300 . ?
C24 C25 1.382(5) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.493(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.490(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C26' C27' 1.496(9) . ?
C26' H26C 0.9700 . ?
C26' H26D 0.9700 . ?
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
O2' S1 O3 148.0(3) . . ?
O2' S1 O2 52.2(3) . . ?
O3 S1 O2 113.8(2) . . ?
O2' S1 O3' 120.6(4) . . ?
O3 S1 O3' 47.1(3) . . ?
O2 S1 O3' 70.2(3) . . ?
O2' S1 O1 58.6(3) . . ?
O3 S1 O1 113.6(2) . . ?
O2 S1 O1 107.9(2) . . ?
O3' S1 O1 147.2(3) . . ?
O2' S1 O1' 112.9(4) . . ?
O3 S1 O1' 61.3(4) . . ?
O2 S1 O1' 147.2(3) . . ?
O3' S1 O1' 107.5(4) . . ?
O1 S1 O1' 55.6(3) . . ?
O2' S1 C1 106.7(2) . . ?
O3 S1 C1 105.10(16) . . ?
O2 S1 C1 108.05(14) . . ?
O3' S1 C1 103.2(3) . . ?
O1 S1 C1 108.16(17) . . ?
O1' S1 C1 104.3(3) . . ?
C2 O4 H4O 101(3) . . ?
C26 O5 H5O 103(4) . . ?
C26' O5 H5O 111(4) . . ?
C7 N1 H1N1 108(2) . . ?
C7 N1 H1N2 113(2) . . ?
H1N1 N1 H1N2 107.9(15) . . ?
C7 N1 H1N3 113(2) . . ?
H1N1 N1 H1N3 107.7(15) . . ?
H1N2 N1 H1N3 107.6(15) . . ?
C6 C1 C2 120.7(2) . . ?
C6 C1 S1 119.27(18) . . ?
C2 C1 S1 120.01(18) . . ?
O4 C2 C1 124.6(2) . . ?
O4 C2 C3 117.4(2) . . ?
C1 C2 C3 118.0(2) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C3 C4 C5 122.0(3) . . ?
C3 C4 H4A 119.0 . . ?
C5 C4 H4A 119.0 . . ?
C4 C5 C6 116.6(2) . . ?
C4 C5 C5 121.8(3) . 2_655 ?
C6 C5 C5 121.6(3) . 2_655 ?
C1 C6 C5 121.7(2) . . ?
C1 C6 H6A 119.2 . . ?
C5 C6 H6A 119.2 . . ?
N1 C7 C14 108.0(2) . . ?
N1 C7 C8 106.9(2) . . ?
C14 C7 C8 110.9(2) . . ?
N1 C7 C20 105.4(2) . . ?
C14 C7 C20 112.1(2) . . ?
C8 C7 C20 113.0(2) . . ?
C9 C8 C13 117.2(3) . . ?
C9 C8 C7 121.5(3) . . ?
C13 C8 C7 121.3(2) . . ?
C10 C9 C8 120.5(3) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C10 C11 C12 119.3(4) . . ?
C10 C11 H11A 120.3 . . ?
C12 C11 H11A 120.3 . . ?
C11 C12 C13 120.1(4) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C12 C13 C8 121.7(3) . . ?
C12 C13 H13A 119.1 . . ?
C8 C13 H13A 119.1 . . ?
C15 C14 C19 116.6(3) . . ?
C15 C14 C7 123.0(2) . . ?
C19 C14 C7 120.2(3) . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C17 C16 C15 121.7(3) . . ?
C17 C16 H16A 119.1 . . ?
C15 C16 H16A 119.1 . . ?
C18 C17 C16 118.5(3) . . ?
C18 C17 H17A 120.8 . . ?
C16 C17 H17A 120.8 . . ?
C17 C18 C19 121.5(4) . . ?
C17 C18 H18A 119.2 . . ?
C19 C18 H18A 119.2 . . ?
C14 C19 C18 120.8(4) . . ?
C14 C19 H19A 119.6 . . ?
C18 C19 H19A 119.6 . . ?
C21 C20 C25 117.4(3) . . ?
C21 C20 C7 123.1(2) . . ?
C25 C20 C7 119.5(3) . . ?
C20 C21 C22 121.6(3) . . ?
C20 C21 H21A 119.2 . . ?
C22 C21 H21A 119.2 . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H22A 119.8 . . ?
C21 C22 H22A 119.8 . . ?
C24 C23 C22 118.9(3) . . ?
C24 C23 H23A 120.5 . . ?
C22 C23 H23A 120.5 . . ?
C23 C24 C25 120.7(3) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
C24 C25 C20 121.0(3) . . ?
C24 C25 H25A 119.5 . . ?
C20 C25 H25A 119.5 . . ?
O5 C26 C27 112.6(8) . . ?
O5 C26 H26A 109.1 . . ?
C27 C26 H26A 109.1 . . ?
O5 C26 H26B 109.1 . . ?
C27 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
C28 C27 C26 115.3(8) . . ?
C28 C27 H27A 108.4 . . ?
C26 C27 H27A 108.4 . . ?
C28 C27 H27B 108.4 . . ?
C26 C27 H27B 108.4 . . ?
H27A C27 H27B 107.5 . . ?
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 . . ?
O5 C26' C27' 109.5(8) . . ?
O5 C26' H26C 109.8 . . ?
C27' C26' H26C 109.8 . . ?
O5 C26' H26D 109.8 . . ?
C27' C26' H26D 109.8 . . ?
H26C C26' H26D 108.2 . . ?
C26' C27' H27C 110.3 . . ?
C26' C27' H27D 110.3 . . ?
H27C C27' H27D 108.5 . . ?

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
O2' S1 C1 C6 -31.8(4) . . . . ?
O3 S1 C1 C6 144.9(3) . . . . ?
O2 S1 C1 C6 23.1(3) . . . . ?
O3' S1 C1 C6 96.2(4) . . . . ?
O1 S1 C1 C6 -93.5(3) . . . . ?
O1' S1 C1 C6 -151.5(4) . . . . ?
O2' S1 C1 C2 149.7(4) . . . . ?
O3 S1 C1 C2 -33.7(3) . . . . ?
O2 S1 C1 C2 -155.5(3) . . . . ?
O3' S1 C1 C2 -82.3(4) . . . . ?
O1 S1 C1 C2 88.0(3) . . . . ?
O1' S1 C1 C2 29.9(4) . . . . ?
C6 C1 C2 O4 -179.6(3) . . . . ?
S1 C1 C2 O4 -1.1(4) . . . . ?
C6 C1 C2 C3 0.3(5) . . . . ?
S1 C1 C2 C3 178.9(3) . . . . ?
O4 C2 C3 C4 178.4(3) . . . . ?
C1 C2 C3 C4 -1.5(6) . . . . ?
C2 C3 C4 C5 1.3(6) . . . . ?
C3 C4 C5 C6 0.2(5) . . . . ?
C3 C4 C5 C5 -177.8(3) . . . 2_655 ?
C2 C1 C6 C5 1.1(4) . . . . ?
S1 C1 C6 C5 -177.4(2) . . . . ?
C4 C5 C6 C1 -1.4(4) . . . . ?
C5 C5 C6 C1 176.59(18) 2_655 . . . ?
N1 C7 C8 C9 136.5(3) . . . . ?
C14 C7 C8 C9 18.9(4) . . . . ?
C20 C7 C8 C9 -108.0(3) . . . . ?
N1 C7 C8 C13 -43.4(3) . . . . ?
C14 C7 C8 C13 -160.9(3) . . . . ?
C20 C7 C8 C13 72.1(3) . . . . ?
C13 C8 C9 C10 1.6(5) . . . . ?
C7 C8 C9 C10 -178.3(3) . . . . ?
C8 C9 C10 C11 -0.8(6) . . . . ?
C9 C10 C11 C12 -0.6(7) . . . . ?
C10 C11 C12 C13 1.1(6) . . . . ?
C11 C12 C13 C8 -0.3(6) . . . . ?
C9 C8 C13 C12 -1.0(5) . . . . ?
C7 C8 C13 C12 178.8(3) . . . . ?
N1 C7 C14 C15 -36.3(3) . . . . ?
C8 C7 C14 C15 80.6(3) . . . . ?
C20 C7 C14 C15 -152.0(3) . . . . ?
N1 C7 C14 C19 148.3(3) . . . . ?
C8 C7 C14 C19 -94.8(4) . . . . ?
C20 C7 C14 C19 32.7(4) . . . . ?
C19 C14 C15 C16 2.0(5) . . . . ?
C7 C14 C15 C16 -173.5(3) . . . . ?
C14 C15 C16 C17 -0.8(5) . . . . ?
C15 C16 C17 C18 -0.1(6) . . . . ?
C16 C17 C18 C19 -0.4(9) . . . . ?
C15 C14 C19 C18 -2.5(7) . . . . ?
C7 C14 C19 C18 173.1(5) . . . . ?
C17 C18 C19 C14 1.8(9) . . . . ?
N1 C7 C20 C21 115.8(3) . . . . ?
C14 C7 C20 C21 -126.9(3) . . . . ?
C8 C7 C20 C21 -0.6(3) . . . . ?
N1 C7 C20 C25 -62.1(3) . . . . ?
C14 C7 C20 C25 55.2(3) . . . . ?
C8 C7 C20 C25 -178.5(3) . . . . ?
C25 C20 C21 C22 0.0(4) . . . . ?
C7 C20 C21 C22 -178.0(3) . . . . ?
C20 C21 C22 C23 0.5(5) . . . . ?
C21 C22 C23 C24 -0.2(5) . . . . ?
C22 C23 C24 C25 -0.6(6) . . . . ?
C23 C24 C25 C20 1.1(6) . . . . ?
C21 C20 C25 C24 -0.7(5) . . . . ?
C7 C20 C25 C24 177.3(3) . . . . ?
C26' O5 C26 C27 1.5(11) . . . . ?
O5 C26 C27 C28 174.6(10) . . . . ?
C26 O5 C26' C27' -11.9(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
O4 H4O O3 0.85(4) 1.93(2) 2.708(4) 152(4) .
O5 H5O O1 0.85(4) 1.85(2) 2.674(5) 163(6) 1_565
N1 H1N1 O3 0.86(4) 1.929(12) 2.769(4) 164(2) .
N1 H1N2 O5 0.86(4) 1.933(13) 2.782(4) 168(3) .
N1 H1N3 O2 0.86(4) 1.981(11) 2.829(4) 167(2) 4

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.050
_database_code_depnum_ccdc_archive 'CCDC 1025999'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 2(C4 H10 O)'
_chemical_formula_sum            'C58 H64 N2 O10 S2'
_chemical_formula_weight         1013.23

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           monoclinic
_symmetry_space_group_name_H-M   'C 2'
_symmetry_space_group_name_Hall  'C 2y'

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                   25.3691(12)
_cell_length_b                   8.0242(5)
_cell_length_c                   15.2135(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.171(3)
_cell_angle_gamma                90.00
_cell_volume                     2704.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1371
_cell_measurement_theta_min      3.74
_cell_measurement_theta_max      25.76

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_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             1076
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9676
_exptl_absorpt_correction_T_max  0.9767
_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            5270
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4702
_reflns_number_gt                3594
_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)+(0.1499P)²+0.9913P] 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   0.25(15)
_refine_ls_number_reflns         4702
_refine_ls_number_parameters     353
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0805
_refine_ls_wR_factor_ref         0.2352
_refine_ls_wR_factor_gt          0.2122
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.051
_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 0.64688(4) 0.37527(17) 0.90459(8) 0.0441(3) Uani 1 1 d . . .
O1 O 0.6885(2) 0.4197(9) 1.0104(4) 0.0594(16) Uani 0.606(4) 1 d P A 1
O2 O 0.6572(3) 0.2065(10) 0.8898(6) 0.0749(17) Uani 0.606(4) 1 d P A 1
O3 O 0.6496(3) 0.4885(11) 0.8339(6) 0.0753(19) Uani 0.606(4) 1 d P A 1
O1' O 0.6761(4) 0.2637(15) 0.9829(7) 0.0594(16) Uani 0.394(4) 1 d P A 2
O2' O 0.6395(5) 0.2998(17) 0.8101(10) 0.0749(17) Uani 0.394(4) 1 d P A 2
O3' O 0.6677(5) 0.5405(18) 0.9129(9) 0.0753(19) Uani 0.394(4) 1 d P A 2
O4 O 0.53096(15) 0.4418(7) 0.7044(2) 0.0670(12) Uani 1 1 d D A .
H4O H 0.5678(12) 0.470(11) 0.733(5) 0.100 Uiso 1 1 d D . .
N1 N 0.72592(17) 0.7305(6) 0.8267(3) 0.0472(10) Uani 1 1 d D . .
H1N1 H 0.7119(18) 0.654(5) 0.849(3) 0.071 Uiso 1 1 d D . .
H1N2 H 0.7002(15) 0.808(4) 0.799(4) 0.071 Uiso 1 1 d D . .
H1N3 H 0.7579(13) 0.771(5) 0.876(2) 0.071 Uiso 1 1 d D . .
C1 C 0.74842(19) 0.6560(6) 0.7589(3) 0.0415(10) Uani 1 1 d . . .
C2 C 0.8028(2) 0.5489(7) 0.8257(3) 0.0447(11) Uani 1 1 d . . .
C3 C 0.8576(2) 0.5634(8) 0.8251(5) 0.0603(14) Uani 1 1 d . . .
H3A H 0.8608 0.6365 0.7805 0.072 Uiso 1 1 calc R . .
C4 C 0.9073(3) 0.4689(10) 0.8910(6) 0.082(2) Uani 1 1 d . . .
H4A H 0.9438 0.4831 0.8915 0.098 Uiso 1 1 calc R . .
C5 C 0.9037(3) 0.3575(10) 0.9541(5) 0.0744(18) Uani 1 1 d . . .
H5A H 0.9370 0.2925 0.9957 0.089 Uiso 1 1 calc R . .
C6 C 0.8502(3) 0.3400(9) 0.9566(4) 0.076(2) Uani 1 1 d . . .
H6A H 0.8479 0.2672 1.0022 0.091 Uiso 1 1 calc R . .
C7 C 0.8004(2) 0.4317(9) 0.8908(4) 0.0632(16) Uani 1 1 d . . .
H7A H 0.7639 0.4144 0.8901 0.076 Uiso 1 1 calc R . .
C8 C 0.7655(2) 0.8012(7) 0.7111(4) 0.0455(11) Uani 1 1 d . . .
C9 C 0.7861(2) 0.9527(8) 0.7569(4) 0.0532(12) Uani 1 1 d . . .
H9A H 0.7864 0.9756 0.8171 0.064 Uiso 1 1 calc R . .
C10 C 0.8065(2) 1.0719(8) 0.7149(5) 0.0652(16) Uani 1 1 d . . .
H10A H 0.8211 1.1724 0.7486 0.078 Uiso 1 1 calc R . .
C11 C 0.8059(3) 1.0473(10) 0.6267(5) 0.0780(19) Uani 1 1 d . . .
H11A H 0.8190 1.1294 0.5987 0.094 Uiso 1 1 calc R . .
C12 C 0.7851(3) 0.8957(11) 0.5795(5) 0.083(2) Uani 1 1 d . . .
H12A H 0.7837 0.8758 0.5182 0.100 Uiso 1 1 calc R . .
C13 C 0.7665(3) 0.7744(9) 0.6212(4) 0.0707(17) Uani 1 1 d . . .
H13A H 0.7542 0.6719 0.5891 0.085 Uiso 1 1 calc R . .
C14 C 0.6942(2) 0.5575(7) 0.6765(3) 0.0455(11) Uani 1 1 d . . .
C15 C 0.6422(3) 0.6407(9) 0.6146(5) 0.0708(17) Uani 1 1 d . . .
H15A H 0.6399 0.7555 0.6204 0.085 Uiso 1 1 calc R . .
C16 C 0.5920(3) 0.5517(11) 0.5422(5) 0.084(2) Uani 1 1 d . . .
H16A H 0.5569 0.6091 0.4995 0.101 Uiso 1 1 calc R . .
C17 C 0.5938(3) 0.3883(12) 0.5334(4) 0.0765(18) Uani 1 1 d . . .
H17A H 0.5599 0.3306 0.4866 0.092 Uiso 1 1 calc R . .
C18 C 0.6465(3) 0.3045(10) 0.5944(5) 0.080(2) Uani 1 1 d . . .
H18A H 0.6489 0.1899 0.5878 0.096 Uiso 1 1 calc R . .
C19 C 0.6962(2) 0.3918(8) 0.6657(4) 0.0579(13) Uani 1 1 d . . .
H19A H 0.7316 0.3344 0.7069 0.070 Uiso 1 1 calc R . .
C20 C 0.57256(17) 0.3981(6) 0.8849(3) 0.0377(9) Uani 1 1 d . A .
C21 C 0.5246(2) 0.4299(7) 0.7877(3) 0.0486(13) Uani 1 1 d . . .
C22 C 0.4678(2) 0.4492(10) 0.7778(4) 0.0701(19) Uani 1 1 d . A .
H22A H 0.4351 0.4674 0.7140 0.084 Uiso 1 1 calc R . .
C23 C 0.45809(19) 0.4426(8) 0.8582(3) 0.0579(16) Uani 1 1 d . . .
H23A H 0.4191 0.4573 0.8479 0.069 Uiso 1 1 calc R A .
C24 C 0.50550(17) 0.4141(5) 0.9566(3) 0.0385(10) Uani 1 1 d . . .
C25 C 0.56243(17) 0.3901(7) 0.9667(3) 0.0403(9) Uani 1 1 d . . .
H25A H 0.5948 0.3679 1.0301 0.048 Uiso 1 1 calc R A .
O5 O 0.6333(2) 0.9666(7) 0.7495(4) 0.0924(16) Uani 0.50 1 d PD B 3
H5O H 0.6482 1.0458 0.7879 0.139 Uiso 0.50 1 calc PRD B 3
C26 C 0.5839(6) 0.905(2) 0.7576(13) 0.105(4) Uani 0.50 1 d PD B 3
H26A H 0.5909 0.9287 0.8250 0.126 Uiso 0.50 1 calc PR B 3
H26B H 0.5834 0.7843 0.7509 0.126 Uiso 0.50 1 calc PR B 3
C27 C 0.5231(5) 0.9679(15) 0.6850(9) 0.140(4) Uani 0.50 1 d PD B 3
H27A H 0.5147 0.9377 0.6176 0.168 Uiso 0.50 1 calc PR B 3
H27B H 0.5238 1.0886 0.6888 0.168 Uiso 0.50 1 calc PR B 3
C28 C 0.4725(6) 0.906(4) 0.7000(18) 0.159(7) Uani 0.50 1 d PD B 3
H28A H 0.4704 0.7858 0.6935 0.191 Uiso 0.50 1 calc PR B 3
H28B H 0.4811 0.9332 0.7679 0.191 Uiso 0.50 1 calc PR B 3
C29 C 0.4128(6) 0.978(2) 0.6275(11) 0.164(5) Uani 0.50 1 d PD B 3
H29A H 0.3822 0.9316 0.6404 0.246 Uiso 0.50 1 calc PR B 3
H29B H 0.4036 0.9506 0.5601 0.246 Uiso 0.50 1 calc PR B 3
H29C H 0.4139 1.0964 0.6354 0.246 Uiso 0.50 1 calc PR B 3
O5' O 0.6333(2) 0.9666(7) 0.7495(4) 0.0924(16) Uani 0.50 1 d P C 4
H5'O H 0.6437 1.0375 0.7937 0.139 Uiso 0.50 1 calc PR C 4
C26' C 0.5787(7) 0.996(3) 0.6804(16) 0.105(4) Uani 0.50 1 d PD C 4
H26C H 0.5737 0.9341 0.6220 0.126 Uiso 0.50 1 calc PR C 4
H26D H 0.5780 1.1127 0.6637 0.126 Uiso 0.50 1 calc PR C 4
C27' C 0.5231(5) 0.9679(15) 0.6850(9) 0.140(4) Uani 0.50 1 d PD C 4
H27C H 0.5219 1.0553 0.7281 0.168 Uiso 0.50 1 calc PR C 4
H27D H 0.5293 0.8646 0.7219 0.168 Uiso 0.50 1 calc PR C 4
C28' C 0.4607(5) 0.958(4) 0.5984(13) 0.159(7) Uani 0.50 1 d PD C 4
H28C H 0.4556 0.8506 0.5655 0.191 Uiso 0.50 1 calc PR C 4
H28D H 0.4556 1.0436 0.5501 0.191 Uiso 0.50 1 calc PR C 4
C29' C 0.4128(6) 0.978(2) 0.6275(11) 0.164(5) Uani 0.50 1 d PD C 4
H29D H 0.3738 0.9691 0.5686 0.246 Uiso 0.50 1 calc PR C 4
H29E H 0.4167 1.0846 0.6583 0.246 Uiso 0.50 1 calc PR C 4
H29F H 0.4169 0.8916 0.6744 0.246 Uiso 0.50 1 calc PR C 4


_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' 1.382(10) . ?
S1 O3' 1.410(14) . ?
S1 O2 1.418(8) . ?
S1 O3 1.435(7) . ?
S1 O1 1.475(6) . ?
S1 O2' 1.486(12) . ?
S1 C20 1.769(4) . ?
O4 C21 1.356(5) . ?
O4 H4O 0.85(3) . ?
N1 C1 1.524(6) . ?
N1 H1N1 0.85(2) . ?
N1 H1N2 0.85(2) . ?
N1 H1N3 0.86(2) . ?
C1 C2 1.519(7) . ?
C1 C8 1.542(7) . ?
C1 C14 1.550(7) . ?
C2 C7 1.389(8) . ?
C2 C3 1.399(7) . ?
C3 C4 1.393(8) . ?
C3 H3A 0.9300 . ?
C4 C5 1.347(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.383(9) . ?
C5 H5A 0.9300 . ?
C6 C7 1.382(8) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.372(8) . ?
C8 C13 1.397(7) . ?
C9 C10 1.382(8) . ?
C9 H9A 0.9300 . ?
C10 C11 1.349(10) . ?
C10 H10A 0.9300 . ?
C11 C12 1.379(11) . ?
C11 H11A 0.9300 . ?
C12 C13 1.366(10) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C19 1.343(8) . ?
C14 C15 1.366(8) . ?
C15 C16 1.405(9) . ?
C15 H15A 0.9300 . ?
C16 C17 1.321(11) . ?
C16 H16A 0.9300 . ?
C17 C18 1.375(11) . ?
C17 H17A 0.9300 . ?
C18 C19 1.386(8) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C25 1.389(5) . ?
C20 C21 1.406(6) . ?
C21 C22 1.384(7) . ?
C22 C23 1.362(7) . ?
C22 H22A 0.9300 . ?
C23 C24 1.409(6) . ?
C23 H23A 0.9300 . ?
C24 C25 1.390(5) . ?
C24 C24 1.476(8) 2_657 ?
C25 H25A 0.9300 . ?
O5 C26 1.408(18) . ?
O5 H5O 0.8200 . ?
C26 C27 1.482(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.493(10) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.487(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C26' H26C 0.9700 . ?
C26' H26D 0.9700 . ?
C28' H28C 0.9700 . ?
C28' H28D 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
O1' S1 O3' 120.8(7) . . ?
O1' S1 O2 57.0(6) . . ?
O3' S1 O2 145.3(5) . . ?
O1' S1 O3 148.7(5) . . ?
O3' S1 O3 47.1(5) . . ?
O2 S1 O3 113.9(5) . . ?
O1' S1 O1 54.4(6) . . ?
O3' S1 O1 68.7(6) . . ?
O2 S1 O1 108.3(4) . . ?
O3 S1 O1 113.2(4) . . ?
O1' S1 O2' 109.4(7) . . ?
O3' S1 O2' 109.6(7) . . ?
O2 S1 O2' 53.3(6) . . ?
O3 S1 O2' 64.0(6) . . ?
O1 S1 O2' 147.2(5) . . ?
O1' S1 C20 107.0(4) . . ?
O3' S1 C20 103.9(5) . . ?
O2 S1 C20 109.7(4) . . ?
O3 S1 C20 104.1(3) . . ?
O1 S1 C20 107.2(3) . . ?
O2' S1 C20 104.9(5) . . ?
C21 O4 H4O 98(6) . . ?
C1 N1 H1N1 110(4) . . ?
C1 N1 H1N2 114(4) . . ?
H1N1 N1 H1N2 110.6(18) . . ?
C1 N1 H1N3 104(4) . . ?
H1N1 N1 H1N3 109.3(17) . . ?
H1N2 N1 H1N3 108.8(17) . . ?
C2 C1 N1 106.6(3) . . ?
C2 C1 C8 111.8(4) . . ?
N1 C1 C8 107.8(4) . . ?
C2 C1 C14 114.2(4) . . ?
N1 C1 C14 105.7(4) . . ?
C8 C1 C14 110.3(4) . . ?
C7 C2 C3 116.8(5) . . ?
C7 C2 C1 121.2(4) . . ?
C3 C2 C1 122.0(4) . . ?
C4 C3 C2 120.3(6) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C5 C4 C3 121.5(6) . . ?
C5 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
C4 C5 C6 119.7(5) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
C7 C6 C5 119.3(6) . . ?
C7 C6 H6A 120.3 . . ?
C5 C6 H6A 120.3 . . ?
C6 C7 C2 122.3(5) . . ?
C6 C7 H7A 118.9 . . ?
C2 C7 H7A 118.9 . . ?
C9 C8 C13 116.6(5) . . ?
C9 C8 C1 123.8(4) . . ?
C13 C8 C1 119.2(5) . . ?
C8 C9 C10 121.0(6) . . ?
C8 C9 H9A 119.5 . . ?
C10 C9 H9A 119.5 . . ?
C11 C10 C9 122.2(7) . . ?
C11 C10 H10A 118.9 . . ?
C9 C10 H10A 118.9 . . ?
C10 C11 C12 117.6(6) . . ?
C10 C11 H11A 121.2 . . ?
C12 C11 H11A 121.2 . . ?
C13 C12 C11 121.1(6) . . ?
C13 C12 H12A 119.4 . . ?
C11 C12 H12A 119.4 . . ?
C12 C13 C8 121.4(6) . . ?
C12 C13 H13A 119.3 . . ?
C8 C13 H13A 119.3 . . ?
C19 C14 C15 118.7(5) . . ?
C19 C14 C1 122.2(5) . . ?
C15 C14 C1 119.1(5) . . ?
C14 C15 C16 119.6(7) . . ?
C14 C15 H15A 120.2 . . ?
C16 C15 H15A 120.2 . . ?
C17 C16 C15 121.4(7) . . ?
C17 C16 H16A 119.3 . . ?
C15 C16 H16A 119.3 . . ?
C16 C17 C18 119.1(7) . . ?
C16 C17 H17A 120.4 . . ?
C18 C17 H17A 120.4 . . ?
C17 C18 C19 119.7(7) . . ?
C17 C18 H18A 120.2 . . ?
C19 C18 H18A 120.2 . . ?
C14 C19 C18 121.5(6) . . ?
C14 C19 H19A 119.3 . . ?
C18 C19 H19A 119.3 . . ?
C25 C20 C21 120.5(4) . . ?
C25 C20 S1 119.4(3) . . ?
C21 C20 S1 120.0(3) . . ?
O4 C21 C22 118.8(4) . . ?
O4 C21 C20 124.1(4) . . ?
C22 C21 C20 117.1(4) . . ?
C23 C22 C21 122.2(4) . . ?
C23 C22 H22A 118.9 . . ?
C21 C22 H22A 118.9 . . ?
C22 C23 C24 121.8(4) . . ?
C22 C23 H23A 119.1 . . ?
C24 C23 H23A 119.1 . . ?
C25 C24 C23 116.3(4) . . ?
C25 C24 C24 122.7(4) . 2_657 ?
C23 C24 C24 121.0(4) . 2_657 ?
C20 C25 C24 122.1(4) . . ?
C20 C25 H25A 119.0 . . ?
C24 C25 H25A 119.0 . . ?
C26 O5 H5O 109.5 . . ?
O5 C26 C27 117.5(13) . . ?
O5 C26 H26A 107.9 . . ?
C27 C26 H26A 107.9 . . ?
O5 C26 H26B 107.9 . . ?
C27 C26 H26B 107.9 . . ?
H26A C26 H26B 107.2 . . ?
C26 C27 C28 115.6(12) . . ?
C26 C27 H27A 108.4 . . ?
C28 C27 H27A 108.4 . . ?
C26 C27 H27B 108.4 . . ?
C28 C27 H27B 108.4 . . ?
H27A C27 H27B 107.4 . . ?
C29 C28 C27 113.6(13) . . ?
C29 C28 H28A 108.8 . . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 . . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
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 . . ?
H26C C26' H26D 106.0 . . ?
H28C C28' H28D 107.7 . . ?

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 C7 49.9(6) . . . . ?
C8 C1 C2 C7 167.5(5) . . . . ?
C14 C1 C2 C7 -66.4(6) . . . . ?
N1 C1 C2 C3 -129.9(5) . . . . ?
C8 C1 C2 C3 -12.3(7) . . . . ?
C14 C1 C2 C3 113.8(5) . . . . ?
C7 C2 C3 C4 -3.0(9) . . . . ?
C1 C2 C3 C4 176.8(6) . . . . ?
C2 C3 C4 C5 2.4(11) . . . . ?
C3 C4 C5 C6 -2.4(11) . . . . ?
C4 C5 C6 C7 3.1(11) . . . . ?
C5 C6 C7 C2 -3.9(10) . . . . ?
C3 C2 C7 C6 3.8(9) . . . . ?
C1 C2 C7 C6 -176.0(6) . . . . ?
C2 C1 C8 C9 -86.9(6) . . . . ?
N1 C1 C8 C9 30.0(6) . . . . ?
C14 C1 C8 C9 144.9(5) . . . . ?
C2 C1 C8 C13 86.0(6) . . . . ?
N1 C1 C8 C13 -157.1(5) . . . . ?
C14 C1 C8 C13 -42.2(6) . . . . ?
C13 C8 C9 C10 0.3(8) . . . . ?
C1 C8 C9 C10 173.3(5) . . . . ?
C8 C9 C10 C11 1.5(9) . . . . ?
C9 C10 C11 C12 -1.3(10) . . . . ?
C10 C11 C12 C13 -0.7(11) . . . . ?
C11 C12 C13 C8 2.6(12) . . . . ?
C9 C8 C13 C12 -2.3(9) . . . . ?
C1 C8 C13 C12 -175.6(6) . . . . ?
C2 C1 C14 C19 -0.6(6) . . . . ?
N1 C1 C14 C19 -117.5(5) . . . . ?
C8 C1 C14 C19 126.3(5) . . . . ?
C2 C1 C14 C15 177.6(5) . . . . ?
N1 C1 C14 C15 60.7(6) . . . . ?
C8 C1 C14 C15 -55.6(6) . . . . ?
C19 C14 C15 C16 0.5(10) . . . . ?
C1 C14 C15 C16 -177.7(6) . . . . ?
C14 C15 C16 C17 1.0(12) . . . . ?
C15 C16 C17 C18 -2.1(12) . . . . ?
C16 C17 C18 C19 1.8(11) . . . . ?
C15 C14 C19 C18 -0.8(9) . . . . ?
C1 C14 C19 C18 177.3(5) . . . . ?
C17 C18 C19 C14 -0.3(10) . . . . ?
O1' S1 C20 C25 34.0(7) . . . . ?
O3' S1 C20 C25 -94.8(7) . . . . ?
O2 S1 C20 C25 94.3(6) . . . . ?
O3 S1 C20 C25 -143.4(5) . . . . ?
O1 S1 C20 C25 -23.1(6) . . . . ?
O2' S1 C20 C25 150.2(7) . . . . ?
O1' S1 C20 C21 -148.2(6) . . . . ?
O3' S1 C20 C21 83.0(6) . . . . ?
O2 S1 C20 C21 -87.9(6) . . . . ?
O3 S1 C20 C21 34.4(6) . . . . ?
O1 S1 C20 C21 154.7(5) . . . . ?
O2' S1 C20 C21 -32.0(7) . . . . ?
C25 C20 C21 O4 179.1(5) . . . . ?
S1 C20 C21 O4 1.3(7) . . . . ?
C25 C20 C21 C22 -1.2(8) . . . . ?
S1 C20 C21 C22 -178.9(5) . . . . ?
O4 C21 C22 C23 -178.6(6) . . . . ?
C20 C21 C22 C23 1.7(10) . . . . ?
C21 C22 C23 C24 -0.6(11) . . . . ?
C22 C23 C24 C25 -1.1(9) . . . . ?
C22 C23 C24 C24 177.5(5) . . . 2_657 ?
C21 C20 C25 C24 -0.6(8) . . . . ?
S1 C20 C25 C24 177.2(4) . . . . ?
C23 C24 C25 C20 1.7(8) . . . . ?
C24 C24 C25 C20 -176.9(4) 2_657 . . . ?
O5 C26 C27 C28 -176.7(18) . . . . ?
C26 C27 C28 C29 178.0(18) . . . . ?

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 O3 0.85(3) 1.89(3) 2.702(8) 160(8) .
O5 H5O O2 0.82 1.94 2.714(9) 156.4 1_565
N1 H1N1 O3 0.85(2) 1.99(2) 2.782(8) 153(4) .
N1 H1N2 O5 0.85(2) 1.955(17) 2.793(7) 169(5) .
N1 H1N3 O1 0.86(2) 1.99(2) 2.813(7) 161(5) 4_657

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.079
_database_code_depnum_ccdc_archive 'CCDC 1026000'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_9

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 2(C5 H12 O)'
_chemical_formula_sum            'C60 H68 N2 O10 S2'
_chemical_formula_weight         1041.28

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           monoclinic
_symmetry_space_group_name_H-M   'C 2'
_symmetry_space_group_name_Hall  'C 2y'

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                   25.6094(14)
_cell_length_b                   8.1885(3)
_cell_length_c                   15.2041(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.790(4)
_cell_angle_gamma                90.00
_cell_volume                     2794.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1304
_cell_measurement_theta_min      3.68
_cell_measurement_theta_max      26.04

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1108
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9682
_exptl_absorpt_correction_T_max  0.9772
_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            5178
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4586
_reflns_number_gt                3386
_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)+(0.0891P)²+1.5638P] 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   0.27(13)
_refine_ls_number_reflns         4586
_refine_ls_number_parameters     374
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1685
_refine_ls_wR_factor_gt          0.1504
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.026
_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 0.35439(4) 0.90552(14) 0.59580(7) 0.0459(3) Uani 1 1 d . . .
O1 O 0.3126(2) 0.8595(9) 0.4883(4) 0.0644(15) Uani 0.533(3) 1 d P A 1
O2 O 0.3446(3) 1.0738(9) 0.6073(6) 0.0764(15) Uani 0.533(3) 1 d P A 1
O3 O 0.3499(3) 0.7953(11) 0.6654(6) 0.0788(18) Uani 0.533(3) 1 d P A 1
O1' O 0.3274(3) 1.0175(11) 0.5200(5) 0.0644(15) Uani 0.467(3) 1 d P A 2
O2' O 0.3621(4) 0.9836(11) 0.6913(7) 0.0764(15) Uani 0.467(3) 1 d P A 2
O3' O 0.3308(4) 0.7481(12) 0.5877(7) 0.0788(18) Uani 0.467(3) 1 d P A 2
O4 O 0.46865(13) 0.8380(6) 0.7954(2) 0.0726(11) Uani 1 1 d D A .
H4O H 0.4316(7) 0.829(9) 0.774(5) 0.109 Uiso 1 1 d D . .
O5 O 0.3559(2) 0.3122(6) 0.7363(4) 0.1012(14) Uani 1 1 d D . .
H5O H 0.343(4) 0.218(5) 0.710(6) 0.152 Uiso 1 1 d D . .
N1 N 0.27134(15) 0.5586(5) 0.6673(3) 0.0492(9) Uani 1 1 d D . .
H1N1 H 0.2866(15) 0.636(4) 0.648(3) 0.074 Uiso 1 1 d D . .
H1N2 H 0.2968(13) 0.480(3) 0.691(3) 0.074 Uiso 1 1 d D . .
H1N3 H 0.2407(11) 0.522(4) 0.6142(19) 0.074 Uiso 1 1 d D . .
C1 C 0.24985(16) 0.6330(5) 0.7369(3) 0.0417(9) Uani 1 1 d . . .
C2 C 0.23275(17) 0.4917(6) 0.7843(3) 0.0440(9) Uani 1 1 d . . .
C3 C 0.21448(19) 0.3410(6) 0.7418(4) 0.0548(11) Uani 1 1 d . . .
H3A H 0.2144 0.3154 0.6822 0.066 Uiso 1 1 calc R . .
C4 C 0.1958(2) 0.2252(7) 0.7887(5) 0.0720(15) Uani 1 1 d . . .
H4A H 0.1832 0.1232 0.7590 0.086 Uiso 1 1 calc R . .
C5 C 0.1956(2) 0.2570(8) 0.8757(5) 0.0767(17) Uani 1 1 d . . .
H5A H 0.1833 0.1781 0.9059 0.092 Uiso 1 1 calc R . .
C6 C 0.2134(2) 0.4053(10) 0.9179(4) 0.0783(15) Uani 1 1 d . . .
H6A H 0.2134 0.4281 0.9777 0.094 Uiso 1 1 calc R . .
C7 C 0.2319(2) 0.5250(7) 0.8742(3) 0.0589(12) Uani 1 1 d . . .
H7A H 0.2437 0.6270 0.9044 0.071 Uiso 1 1 calc R . .
C8 C 0.19601(17) 0.7389(5) 0.6702(3) 0.0432(9) Uani 1 1 d . . .
C9 C 0.1998(2) 0.8592(7) 0.6080(3) 0.0652(14) Uani 1 1 d . . .
H9A H 0.2361 0.8759 0.6092 0.078 Uiso 1 1 calc R . .
C10 C 0.1516(3) 0.9535(7) 0.5453(4) 0.0791(17) Uani 1 1 d . . .
H10A H 0.1553 1.0327 0.5047 0.095 Uiso 1 1 calc R . .
C11 C 0.0969(2) 0.9282(8) 0.5434(4) 0.0786(16) Uani 1 1 d . . .
H11A H 0.0639 0.9910 0.5015 0.094 Uiso 1 1 calc R . .
C12 C 0.0923(2) 0.8130(8) 0.6024(4) 0.0766(16) Uani 1 1 d . . .
H12A H 0.0558 0.7962 0.6004 0.092 Uiso 1 1 calc R . .
C13 C 0.14083(19) 0.7189(6) 0.6660(4) 0.0582(12) Uani 1 1 d . . .
H13A H 0.1365 0.6409 0.7065 0.070 Uiso 1 1 calc R . .
C14 C 0.30312(18) 0.7288(6) 0.8164(3) 0.0443(10) Uani 1 1 d . . .
C15 C 0.3559(2) 0.6454(7) 0.8763(4) 0.0649(13) Uani 1 1 d . . .
H15A H 0.3580 0.5335 0.8682 0.078 Uiso 1 1 calc R . .
C16 C 0.4057(2) 0.7284(9) 0.9484(4) 0.0796(16) Uani 1 1 d . . .
H16A H 0.4406 0.6711 0.9880 0.095 Uiso 1 1 calc R . .
C17 C 0.4037(2) 0.8915(10) 0.9614(4) 0.0802(17) Uani 1 1 d . . .
H17A H 0.4372 0.9469 1.0087 0.096 Uiso 1 1 calc R . .
C18 C 0.3517(3) 0.9728(8) 0.9038(4) 0.0814(17) Uani 1 1 d . . .
H18A H 0.3496 1.0845 0.9130 0.098 Uiso 1 1 calc R . .
C19 C 0.3020(2) 0.8921(7) 0.8320(3) 0.0592(11) Uani 1 1 d . . .
H19A H 0.2671 0.9505 0.7935 0.071 Uiso 1 1 calc R . .
C20 C 0.42806(15) 0.8796(5) 0.6151(3) 0.0403(9) Uani 1 1 d . A .
C21 C 0.47502(18) 0.8500(6) 0.7116(3) 0.0525(11) Uani 1 1 d . . .
C22 C 0.5314(2) 0.8269(8) 0.7222(3) 0.0730(16) Uani 1 1 d . A .
H22A H 0.5634 0.8073 0.7856 0.088 Uiso 1 1 calc R . .
C23 C 0.54095(18) 0.8324(7) 0.6414(3) 0.0623(14) Uani 1 1 d . . .
H23A H 0.5793 0.8154 0.6512 0.075 Uiso 1 1 calc R A .
C24 C 0.49479(15) 0.8629(5) 0.5440(3) 0.0415(9) Uani 1 1 d . . .
C25 C 0.43823(15) 0.8875(6) 0.5342(3) 0.0425(9) Uani 1 1 d . . .
H25A H 0.4065 0.9099 0.4710 0.051 Uiso 1 1 calc R A .
C26 C 0.4048(6) 0.369(2) 0.7279(12) 0.115(4) Uani 0.50 1 d PD B 3
H26A H 0.4056 0.4871 0.7268 0.139 Uiso 0.50 1 calc PR B 3
H26B H 0.4042 0.3267 0.6678 0.139 Uiso 0.50 1 calc PR B 3
C27 C 0.4565(7) 0.302(3) 0.8204(17) 0.168(8) Uani 0.50 1 d PD B 3
H27A H 0.4524 0.1856 0.8255 0.201 Uiso 0.50 1 calc PR B 3
H27B H 0.4594 0.3546 0.8799 0.201 Uiso 0.50 1 calc PR B 3
C28 C 0.5109(10) 0.340(3) 0.809(3) 0.268(12) Uani 0.50 1 d PD B 3
H28A H 0.5072 0.2836 0.7506 0.322 Uiso 0.50 1 calc PR B 3
H28D H 0.5113 0.4565 0.7972 0.322 Uiso 0.50 1 calc PR B 3
C29 C 0.5686(14) 0.295(5) 0.896(2) 0.203(11) Uani 0.50 1 d PD B 3
H29A H 0.5722 0.1775 0.9013 0.244 Uiso 0.50 1 calc PR B 3
H29D H 0.5702 0.3364 0.9575 0.244 Uiso 0.50 1 calc PR B 3
C30 C 0.6191(16) 0.365(6) 0.885(3) 0.135(9) Uani 0.50 1 d PD B 3
H30A H 0.6561 0.3234 0.9379 0.202 Uiso 0.50 1 calc PR B 3
H30B H 0.6188 0.4819 0.8901 0.202 Uiso 0.50 1 calc PR B 3
H30C H 0.6149 0.3345 0.8214 0.202 Uiso 0.50 1 calc PR B 3
C26' C 0.4158(4) 0.298(2) 0.8053(10) 0.115(4) Uani 0.50 1 d PD B 4
H26C H 0.4236 0.1857 0.8277 0.139 Uiso 0.50 1 calc PR B 4
H26D H 0.4235 0.3648 0.8632 0.139 Uiso 0.50 1 calc PR B 4
C27' C 0.4586(9) 0.345(3) 0.771(2) 0.168(8) Uani 0.50 1 d PD B 4
H27C H 0.4355 0.4199 0.7167 0.201 Uiso 0.50 1 calc PR B 4
H27D H 0.4616 0.2463 0.7390 0.201 Uiso 0.50 1 calc PR B 4
C28' C 0.5203(10) 0.415(4) 0.814(4) 0.268(12) Uani 0.50 1 d PD B 4
H28B H 0.5222 0.4922 0.7676 0.322 Uiso 0.50 1 calc PR B 4
H28C H 0.5308 0.4714 0.8766 0.322 Uiso 0.50 1 calc PR B 4
C29' C 0.5620(14) 0.279(4) 0.832(2) 0.203(11) Uani 0.50 1 d PD B 4
H29B H 0.5596 0.2487 0.7688 0.244 Uiso 0.50 1 calc PR B 4
H29C H 0.5485 0.1853 0.8554 0.244 Uiso 0.50 1 calc PR B 4
C30' C 0.6258(16) 0.309(6) 0.906(3) 0.135(9) Uani 0.50 1 d PD B 4
H30D H 0.6476 0.2086 0.9212 0.202 Uiso 0.50 1 calc PR B 4
H30E H 0.6286 0.3539 0.9668 0.202 Uiso 0.50 1 calc PR B 4
H30F H 0.6424 0.3855 0.8784 0.202 Uiso 0.50 1 calc PR B 4


_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' 1.371(7) . ?
S1 O3' 1.403(9) . ?
S1 O2 1.426(7) . ?
S1 O3 1.437(7) . ?
S1 O1 1.508(6) . ?
S1 O2' 1.510(9) . ?
S1 C20 1.777(3) . ?
O4 C21 1.363(5) . ?
O4 H4O 0.85(3) . ?
O5 C26' 1.384(9) . ?
O5 C26 1.397(9) . ?
O5 H5O 0.85(3) . ?
N1 C1 1.535(5) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
C1 C8 1.528(6) . ?
C1 C14 1.532(6) . ?
C1 C2 1.534(6) . ?
C2 C3 1.366(6) . ?
C2 C7 1.405(6) . ?
C3 C4 1.401(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.352(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.346(10) . ?
C5 H5A 0.9300 . ?
C6 C7 1.388(7) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.393(6) . ?
C8 C9 1.401(6) . ?
C9 C10 1.376(7) . ?
C9 H9A 0.9300 . ?
C10 C11 1.403(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.346(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.384(7) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C19 1.361(7) . ?
C14 C15 1.392(6) . ?
C15 C16 1.393(7) . ?
C15 H15A 0.9300 . ?
C16 C17 1.354(10) . ?
C16 H16A 0.9300 . ?
C17 C18 1.365(9) . ?
C17 H17A 0.9300 . ?
C18 C19 1.382(7) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C25 1.377(5) . ?
C20 C21 1.399(5) . ?
C21 C22 1.387(6) . ?
C22 C23 1.363(6) . ?
C22 H22A 0.9300 . ?
C23 C24 1.402(5) . ?
C23 H23A 0.9300 . ?
C24 C25 1.397(5) . ?
C24 C24 1.486(7) 2_656 ?
C25 H25A 0.9300 . ?
C26 C27 1.494(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.513(10) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.478(10) . ?
C28 H28A 0.9700 . ?
C28 H28D 0.9700 . ?
C29 C30 1.493(10) . ?
C29 H29A 0.9700 . ?
C29 H29D 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C26' C27' 1.471(9) . ?
C26' H26C 0.9700 . ?
C26' H26D 0.9700 . ?
C27' C28' 1.500(10) . ?
C27' H27C 0.9700 . ?
C27' H27D 0.9700 . ?
C28' C29' 1.475(10) . ?
C28' H28B 0.9700 . ?
C28' H28C 0.9700 . ?
C29' C30' 1.494(10) . ?
C29' H29B 0.9700 . ?
C29' H29C 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
O1' S1 O3' 121.3(5) . . ?
O1' S1 O2 53.8(4) . . ?
O3' S1 O2 143.6(4) . . ?
O1' S1 O3 148.5(4) . . ?
O3' S1 O3 45.9(4) . . ?
O2 S1 O3 115.8(5) . . ?
O1' S1 O1 56.5(5) . . ?
O3' S1 O1 67.9(5) . . ?
O2 S1 O1 107.4(4) . . ?
O3 S1 O1 112.0(4) . . ?
O1' S1 O2' 107.7(5) . . ?
O3' S1 O2' 109.0(5) . . ?
O2 S1 O2' 54.7(5) . . ?
O3 S1 O2' 65.0(5) . . ?
O1 S1 O2' 147.6(4) . . ?
O1' S1 C20 106.5(3) . . ?
O3' S1 C20 106.4(4) . . ?
O2 S1 C20 109.3(3) . . ?
O3 S1 C20 105.0(3) . . ?
O1 S1 C20 107.0(2) . . ?
O2' S1 C20 104.7(3) . . ?
C21 O4 H4O 106(4) . . ?
C26' O5 C26 51.8(9) . . ?
C26' O5 H5O 108(7) . . ?
C26 O5 H5O 114(6) . . ?
C1 N1 H1N1 108(3) . . ?
C1 N1 H1N2 117(3) . . ?
H1N1 N1 H1N2 108.4(16) . . ?
C1 N1 H1N3 108(3) . . ?
H1N1 N1 H1N3 107.1(16) . . ?
H1N2 N1 H1N3 107.4(16) . . ?
C8 C1 C14 114.1(3) . . ?
C8 C1 C2 111.7(3) . . ?
C14 C1 C2 111.3(3) . . ?
C8 C1 N1 106.0(3) . . ?
C14 C1 N1 105.6(3) . . ?
C2 C1 N1 107.6(3) . . ?
C3 C2 C7 118.2(4) . . ?
C3 C2 C1 124.7(4) . . ?
C7 C2 C1 116.9(4) . . ?
C2 C3 C4 119.6(5) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C5 C4 C3 122.1(6) . . ?
C5 C4 H4A 119.0 . . ?
C3 C4 H4A 119.0 . . ?
C6 C5 C4 118.6(5) . . ?
C6 C5 H5A 120.7 . . ?
C4 C5 H5A 120.7 . . ?
C5 C6 C7 121.7(5) . . ?
C5 C6 H6A 119.1 . . ?
C7 C6 H6A 119.1 . . ?
C6 C7 C2 119.7(5) . . ?
C6 C7 H7A 120.1 . . ?
C2 C7 H7A 120.1 . . ?
C13 C8 C9 116.8(4) . . ?
C13 C8 C1 122.3(4) . . ?
C9 C8 C1 120.9(4) . . ?
C10 C9 C8 122.1(4) . . ?
C10 C9 H9A 118.9 . . ?
C8 C9 H9A 118.9 . . ?
C9 C10 C11 119.0(5) . . ?
C9 C10 H10A 120.5 . . ?
C11 C10 H10A 120.5 . . ?
C12 C11 C10 119.9(5) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 121.1(5) . . ?
C11 C12 H12A 119.4 . . ?
C13 C12 H12A 119.4 . . ?
C12 C13 C8 121.1(5) . . ?
C12 C13 H13A 119.4 . . ?
C8 C13 H13A 119.4 . . ?
C19 C14 C15 117.6(4) . . ?
C19 C14 C1 123.7(4) . . ?
C15 C14 C1 118.7(4) . . ?
C14 C15 C16 120.5(5) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
C17 C16 C15 120.8(6) . . ?
C17 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
C16 C17 C18 118.7(5) . . ?
C16 C17 H17A 120.6 . . ?
C18 C17 H17A 120.6 . . ?
C17 C18 C19 121.1(6) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C14 C19 C18 121.3(5) . . ?
C14 C19 H19A 119.4 . . ?
C18 C19 H19A 119.4 . . ?
C25 C20 C21 120.5(3) . . ?
C25 C20 S1 119.3(3) . . ?
C21 C20 S1 120.2(3) . . ?
O4 C21 C22 117.9(4) . . ?
O4 C21 C20 124.2(3) . . ?
C22 C21 C20 117.8(3) . . ?
C23 C22 C21 121.3(4) . . ?
C23 C22 H22A 119.4 . . ?
C21 C22 H22A 119.4 . . ?
C22 C23 C24 122.1(4) . . ?
C22 C23 H23A 118.9 . . ?
C24 C23 H23A 118.9 . . ?
C25 C24 C23 116.2(3) . . ?
C25 C24 C24 122.0(4) . 2_656 ?
C23 C24 C24 121.7(4) . 2_656 ?
C20 C25 C24 122.0(3) . . ?
C20 C25 H25A 119.0 . . ?
C24 C25 H25A 119.0 . . ?
O5 C26 C27 102.8(11) . . ?
O5 C26 H26A 111.2 . . ?
C27 C26 H26A 111.2 . . ?
O5 C26 H26B 111.2 . . ?
C27 C26 H26B 111.2 . . ?
H26A C26 H26B 109.1 . . ?
C26 C27 C28 105.5(16) . . ?
C26 C27 H27A 110.6 . . ?
C28 C27 H27A 110.6 . . ?
C26 C27 H27B 110.6 . . ?
C28 C27 H27B 110.6 . . ?
H27A C27 H27B 108.8 . . ?
C29 C28 C27 115(3) . . ?
C29 C28 H28A 108.4 . . ?
C27 C28 H28A 108.4 . . ?
C29 C28 H28D 108.4 . . ?
C27 C28 H28D 108.4 . . ?
H28A C28 H28D 107.5 . . ?
C28 C29 C30 111(3) . . ?
C28 C29 H29A 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C28 C29 H29D 109.5 . . ?
C30 C29 H29D 109.5 . . ?
H29A C29 H29D 108.1 . . ?
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 . . ?
O5 C26' C27' 117.1(14) . . ?
O5 C26' H26C 108.0 . . ?
C27' C26' H26C 108.0 . . ?
O5 C26' H26D 108.0 . . ?
C27' C26' H26D 108.0 . . ?
H26C C26' H26D 107.3 . . ?
C26' C27' C28' 139(3) . . ?
C26' C27' H27C 102.3 . . ?
C28' C27' H27C 102.3 . . ?
C26' C27' H27D 102.3 . . ?
C28' C27' H27D 102.3 . . ?
H27C C27' H27D 104.9 . . ?
C29' C28' C27' 108(2) . . ?
C29' C28' H28B 110.1 . . ?
C27' C28' H28B 110.1 . . ?
C29' C28' H28C 110.1 . . ?
C27' C28' H28C 110.1 . . ?
H28B C28' H28C 108.4 . . ?
C28' C29' C30' 116(3) . . ?
C28' C29' H29B 108.2 . . ?
C30' C29' H29B 108.2 . . ?
C28' C29' H29C 108.2 . . ?
C30' C29' H29C 108.2 . . ?
H29B C29' H29C 107.3 . . ?
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
C8 C1 C2 C3 89.6(5) . . . . ?
C14 C1 C2 C3 -141.6(4) . . . . ?
N1 C1 C2 C3 -26.4(5) . . . . ?
C8 C1 C2 C7 -85.6(4) . . . . ?
C14 C1 C2 C7 43.2(5) . . . . ?
N1 C1 C2 C7 158.4(4) . . . . ?
C7 C2 C3 C4 -0.2(6) . . . . ?
C1 C2 C3 C4 -175.3(4) . . . . ?
C2 C3 C4 C5 -0.4(7) . . . . ?
C3 C4 C5 C6 0.5(8) . . . . ?
C4 C5 C6 C7 0.0(9) . . . . ?
C5 C6 C7 C2 -0.6(8) . . . . ?
C3 C2 C7 C6 0.7(7) . . . . ?
C1 C2 C7 C6 176.2(4) . . . . ?
C14 C1 C8 C13 -119.2(4) . . . . ?
C2 C1 C8 C13 8.1(5) . . . . ?
N1 C1 C8 C13 125.0(4) . . . . ?
C14 C1 C8 C9 62.4(5) . . . . ?
C2 C1 C8 C9 -170.2(4) . . . . ?
N1 C1 C8 C9 -53.3(5) . . . . ?
C13 C8 C9 C10 -0.2(7) . . . . ?
C1 C8 C9 C10 178.3(5) . . . . ?
C8 C9 C10 C11 -0.1(9) . . . . ?
C9 C10 C11 C12 -0.1(9) . . . . ?
C10 C11 C12 C13 0.5(9) . . . . ?
C11 C12 C13 C8 -0.8(8) . . . . ?
C9 C8 C13 C12 0.6(7) . . . . ?
C1 C8 C13 C12 -177.9(4) . . . . ?
C8 C1 C14 C19 4.4(5) . . . . ?
C2 C1 C14 C19 -123.1(4) . . . . ?
N1 C1 C14 C19 120.4(4) . . . . ?
C8 C1 C14 C15 -175.4(4) . . . . ?
C2 C1 C14 C15 57.0(5) . . . . ?
N1 C1 C14 C15 -59.4(5) . . . . ?
C19 C14 C15 C16 -0.9(7) . . . . ?
C1 C14 C15 C16 179.0(5) . . . . ?
C14 C15 C16 C17 -0.1(9) . . . . ?
C15 C16 C17 C18 1.2(9) . . . . ?
C16 C17 C18 C19 -1.2(8) . . . . ?
C15 C14 C19 C18 0.8(7) . . . . ?
C1 C14 C19 C18 -179.0(4) . . . . ?
C17 C18 C19 C14 0.2(8) . . . . ?
O1' S1 C20 C25 -34.9(5) . . . . ?
O3' S1 C20 C25 95.8(5) . . . . ?
O2 S1 C20 C25 -91.6(5) . . . . ?
O3 S1 C20 C25 143.6(5) . . . . ?
O1 S1 C20 C25 24.4(5) . . . . ?
O2' S1 C20 C25 -148.8(5) . . . . ?
O1' S1 C20 C21 145.8(5) . . . . ?
O3' S1 C20 C21 -83.6(5) . . . . ?
O2 S1 C20 C21 89.1(5) . . . . ?
O3 S1 C20 C21 -35.8(5) . . . . ?
O1 S1 C20 C21 -155.0(4) . . . . ?
O2' S1 C20 C21 31.8(5) . . . . ?
C25 C20 C21 O4 -179.0(5) . . . . ?
S1 C20 C21 O4 0.4(6) . . . . ?
C25 C20 C21 C22 -0.9(7) . . . . ?
S1 C20 C21 C22 178.5(4) . . . . ?
O4 C21 C22 C23 178.1(5) . . . . ?
C20 C21 C22 C23 -0.2(9) . . . . ?
C21 C22 C23 C24 0.6(10) . . . . ?
C22 C23 C24 C25 0.0(8) . . . . ?
C22 C23 C24 C24 -177.8(4) . . . 2_656 ?
C21 C20 C25 C24 1.5(7) . . . . ?
S1 C20 C25 C24 -177.9(3) . . . . ?
C23 C24 C25 C20 -1.0(7) . . . . ?
C24 C24 C25 C20 176.8(3) 2_656 . . . ?
C26' O5 C26 C27 5.5(16) . . . . ?
O5 C26 C27 C28 172.7(18) . . . . ?
C26 C27 C28 C29 176(2) . . . . ?
C27 C28 C29 C30 -170(3) . . . . ?
C26 O5 C26' C27' -9.5(17) . . . . ?
O5 C26' C27' C28' 150(3) . . . . ?
C26' C27' C28' C29' 99(4) . . . . ?
C27' C28' C29' C30' -159(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
O4 H4O O3 0.85(3) 1.96(3) 2.736(8) 151(6) .
O5 H5O O2 0.85(3) 1.98(6) 2.683(9) 139(8) 1_545
N1 H1N1 O3 0.86(3) 1.999(19) 2.804(8) 155(3) .
N1 H1N2 O5 0.86(3) 1.912(13) 2.769(6) 175(4) .
N1 H1N3 O1 0.86(3) 2.004(19) 2.824(7) 158(4) 4_546

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.047
_database_code_depnum_ccdc_archive 'CCDC 1026001'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_10

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 2(C4 H8 O2)'
_chemical_formula_sum            'C58 H60 N2 O12 S2'
_chemical_formula_weight         1041.20

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                   9.0753(8)
_cell_length_b                   13.0083(9)
_cell_length_c                   13.1464(12)
_cell_angle_alpha                63.421(8)
_cell_angle_beta                 75.925(8)
_cell_angle_gamma                72.752(7)
_cell_volume                     1314.42(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1885
_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          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             550
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9641
_exptl_absorpt_correction_T_max  0.9705
_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            7815
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6004
_reflns_number_gt                4162
_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)+(0.0811P)²+0.5648P] 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         6004
_refine_ls_number_parameters     346
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0663
_refine_ls_wR_factor_ref         0.1848
_refine_ls_wR_factor_gt          0.1626
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_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 0.61267(8) -0.13502(5) 0.35391(6) 0.0433(2) Uani 1 1 d . . .
O1 O 0.5517(3) -0.10820(17) 0.45417(18) 0.0588(6) Uani 1 1 d . . .
O2 O 0.5711(3) -0.02951(15) 0.25101(17) 0.0574(6) Uani 1 1 d . . .
O3 O 0.7745(2) -0.19247(17) 0.3509(2) 0.0660(6) Uani 1 1 d . . .
O4 O 0.3251(3) -0.08907(18) 0.2355(2) 0.0756(7) Uani 1 1 d D . .
H4O H 0.397(4) -0.055(4) 0.225(4) 0.113 Uiso 1 1 d D . .
O5 O 0.1072(2) 0.07154(19) 0.4344(2) 0.0684(6) Uani 1 1 d . . .
O6 O 0.9429(4) 0.0889(4) 0.0363(4) 0.1336(15) Uani 1 1 d . . .
N1 N 0.3871(2) 0.15754(17) 0.33185(18) 0.0363(5) Uani 1 1 d D . .
H1N1 H 0.2940(13) 0.144(2) 0.350(2) 0.054 Uiso 1 1 d D . .
H1N2 H 0.448(2) 0.1025(18) 0.313(2) 0.054 Uiso 1 1 d D . .
H1N3 H 0.413(2) 0.149(2) 0.3947(14) 0.054 Uiso 1 1 d D . .
C1 C 0.3913(3) 0.27673(19) 0.2315(2) 0.0336(5) Uani 1 1 d . . .
C2 C 0.3763(3) 0.2631(2) 0.1247(2) 0.0360(5) Uani 1 1 d . . .
C3 C 0.4682(4) 0.3066(3) 0.0217(3) 0.0603(8) Uani 1 1 d . . .
H3A H 0.5429 0.3458 0.0152 0.072 Uiso 1 1 calc R . .
C4 C 0.4498(5) 0.2921(4) -0.0730(3) 0.0806(11) Uani 1 1 d . . .
H4A H 0.5130 0.3212 -0.1421 0.097 Uiso 1 1 calc R . .
C5 C 0.3399(5) 0.2355(3) -0.0656(3) 0.0731(10) Uani 1 1 d . . .
H5A H 0.3292 0.2252 -0.1288 0.088 Uiso 1 1 calc R . .
C6 C 0.2465(4) 0.1946(3) 0.0351(3) 0.0617(8) Uani 1 1 d . . .
H6A H 0.1708 0.1568 0.0405 0.074 Uiso 1 1 calc R . .
C7 C 0.2633(3) 0.2087(2) 0.1295(2) 0.0457(6) Uani 1 1 d . . .
H7A H 0.1974 0.1811 0.1975 0.055 Uiso 1 1 calc R . .
C8 C 0.5481(3) 0.3024(2) 0.2261(2) 0.0376(5) Uani 1 1 d . . .
C9 C 0.5588(3) 0.3934(3) 0.2496(3) 0.0555(8) Uani 1 1 d . . .
H9A H 0.4687 0.4415 0.2691 0.067 Uiso 1 1 calc R . .
C10 C 0.7030(4) 0.4133(3) 0.2441(4) 0.0733(10) Uani 1 1 d . . .
H10A H 0.7088 0.4733 0.2623 0.088 Uiso 1 1 calc R . .
C11 C 0.8367(4) 0.3458(3) 0.2124(3) 0.0729(10) Uani 1 1 d . . .
H11A H 0.9329 0.3618 0.2056 0.087 Uiso 1 1 calc R . .
C12 C 0.8274(4) 0.2538(3) 0.1907(4) 0.0741(11) Uani 1 1 d . . .
H12A H 0.9179 0.2064 0.1705 0.089 Uiso 1 1 calc R . .
C13 C 0.6854(3) 0.2315(3) 0.1986(3) 0.0586(8) Uani 1 1 d . . .
H13A H 0.6810 0.1680 0.1853 0.070 Uiso 1 1 calc R . .
C14 C 0.2534(3) 0.3689(2) 0.2545(2) 0.0370(5) Uani 1 1 d . . .
C15 C 0.1748(3) 0.3534(2) 0.3620(2) 0.0455(6) Uani 1 1 d . . .
H15A H 0.2027 0.2833 0.4244 0.055 Uiso 1 1 calc R . .
C16 C 0.0535(4) 0.4423(3) 0.3781(3) 0.0616(8) Uani 1 1 d . . .
H16A H -0.0002 0.4303 0.4510 0.074 Uiso 1 1 calc R . .
C17 C 0.0127(4) 0.5466(3) 0.2877(4) 0.0703(10) Uani 1 1 d . . .
H17A H -0.0668 0.6062 0.2992 0.084 Uiso 1 1 calc R . .
C18 C 0.0899(4) 0.5631(3) 0.1797(4) 0.0686(10) Uani 1 1 d . . .
H18A H 0.0621 0.6341 0.1180 0.082 Uiso 1 1 calc R . .
C19 C 0.2083(3) 0.4753(2) 0.1620(3) 0.0533(7) Uani 1 1 d . . .
H19A H 0.2585 0.4868 0.0883 0.064 Uiso 1 1 calc R . .
C20 C 0.5069(3) -0.2353(2) 0.3654(2) 0.0380(5) Uani 1 1 d . . .
C21 C 0.5542(3) -0.3526(2) 0.4388(2) 0.0403(6) Uani 1 1 d . . .
H21A H 0.6424 -0.3747 0.4742 0.048 Uiso 1 1 calc R . .
C22 C 0.4737(3) -0.43770(19) 0.4609(2) 0.0372(5) Uani 1 1 d . . .
C23 C 0.3410(3) -0.3991(2) 0.4069(3) 0.0496(7) Uani 1 1 d . . .
H23A H 0.2829 -0.4532 0.4209 0.060 Uiso 1 1 calc R . .
C24 C 0.2934(4) -0.2844(2) 0.3341(3) 0.0582(8) Uani 1 1 d . . .
H24A H 0.2043 -0.2621 0.2996 0.070 Uiso 1 1 calc R . .
C25 C 0.3769(3) -0.2006(2) 0.3111(2) 0.0476(7) Uani 1 1 d . . .
C26 C -0.0330(5) 0.1131(3) 0.4904(4) 0.0912(13) Uani 1 1 d . . .
H26A H -0.0671 0.1972 0.4483 0.109 Uiso 1 1 calc R . .
H26B H -0.0186 0.0989 0.5667 0.109 Uiso 1 1 calc R . .
C27 C 0.1527(5) -0.0517(4) 0.5015(5) 0.123(2) Uani 1 1 d . . .
H27A H 0.1652 -0.0646 0.5778 0.147 Uiso 1 1 calc R . .
H27B H 0.2518 -0.0836 0.4665 0.147 Uiso 1 1 calc R . .
C28 C 0.8867(10) 0.0900(6) -0.0402(7) 0.189(4) Uani 1 1 d . . .
H28A H 0.8373 0.1699 -0.0863 0.227 Uiso 1 1 calc R . .
H28B H 0.8085 0.0426 -0.0072 0.227 Uiso 1 1 calc R . .
C29 C 0.9870(9) -0.0417(7) 0.1127(4) 0.151(3) Uani 1 1 d . . .
H29A H 1.0232 -0.0534 0.1814 0.181 Uiso 1 1 calc R . .
H29B H 0.8990 -0.0785 0.1345 0.181 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 1.437(2) . ?
S1 O1 1.452(2) . ?
S1 O2 1.4614(19) . ?
S1 C20 1.773(2) . ?
O4 C25 1.358(3) . ?
O4 H4O 0.85(3) . ?
O5 C26 1.395(4) . ?
O5 C27 1.428(5) . ?
O6 C28 1.227(6) . ?
O6 C29 1.522(7) . ?
N1 C1 1.525(3) . ?
N1 H1N1 0.87(3) . ?
N1 H1N2 0.87(3) . ?
N1 H1N3 0.87(3) . ?
C1 C14 1.532(3) . ?
C1 C2 1.533(3) . ?
C1 C8 1.534(3) . ?
C2 C3 1.376(4) . ?
C2 C7 1.384(3) . ?
C3 C4 1.394(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.367(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.358(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.383(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.383(3) . ?
C8 C13 1.390(4) . ?
C9 C10 1.388(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.366(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.379(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.372(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.374(4) . ?
C14 C19 1.400(4) . ?
C15 C16 1.394(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.366(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.373(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.379(4) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C25 1.383(4) . ?
C20 C21 1.393(3) . ?
C21 C22 1.390(3) . ?
C21 H21A 0.9300 . ?
C22 C23 1.394(4) . ?
C22 C22 1.483(5) 2_646 ?
C23 C24 1.368(4) . ?
C23 H23A 0.9300 . ?
C24 C25 1.392(4) . ?
C24 H24A 0.9300 . ?
C26 C27 1.487(6) 2_556 ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C26 1.487(6) 2_556 ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.481(9) 2_755 ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C28 1.481(9) 2_755 ?
C29 H29A 0.9700 . ?
C29 H29B 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 113.20(14) . . ?
O3 S1 O2 115.27(13) . . ?
O1 S1 O2 109.28(12) . . ?
O3 S1 C20 107.36(12) . . ?
O1 S1 C20 105.42(12) . . ?
O2 S1 C20 105.53(12) . . ?
C25 O4 H4O 103(3) . . ?
C26 O5 C27 107.1(3) . . ?
C28 O6 C29 103.4(5) . . ?
C1 N1 H1N1 110.9(18) . . ?
C1 N1 H1N2 109.8(18) . . ?
H1N1 N1 H1N2 107.2(14) . . ?
C1 N1 H1N3 115.4(17) . . ?
H1N1 N1 H1N3 105.8(13) . . ?
H1N2 N1 H1N3 107.3(14) . . ?
N1 C1 C14 108.89(19) . . ?
N1 C1 C2 106.63(17) . . ?
C14 C1 C2 110.16(19) . . ?
N1 C1 C8 105.35(18) . . ?
C14 C1 C8 112.15(18) . . ?
C2 C1 C8 113.3(2) . . ?
C3 C2 C7 118.0(2) . . ?
C3 C2 C1 122.5(2) . . ?
C7 C2 C1 119.5(2) . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 120.8(3) . . ?
C5 C4 H4A 119.6 . . ?
C3 C4 H4A 119.6 . . ?
C6 C5 C4 119.3(3) . . ?
C6 C5 H5A 120.4 . . ?
C4 C5 H5A 120.4 . . ?
C5 C6 C7 120.5(3) . . ?
C5 C6 H6A 119.8 . . ?
C7 C6 H6A 119.8 . . ?
C6 C7 C2 121.1(3) . . ?
C6 C7 H7A 119.4 . . ?
C2 C7 H7A 119.4 . . ?
C9 C8 C13 118.1(2) . . ?
C9 C8 C1 122.3(2) . . ?
C13 C8 C1 119.6(2) . . ?
C8 C9 C10 120.4(3) . . ?
C8 C9 H9A 119.8 . . ?
C10 C9 H9A 119.8 . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C10 C11 C12 119.2(3) . . ?
C10 C11 H11A 120.4 . . ?
C12 C11 H11A 120.4 . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C12 C13 C8 121.0(3) . . ?
C12 C13 H13A 119.5 . . ?
C8 C13 H13A 119.5 . . ?
C15 C14 C19 118.5(2) . . ?
C15 C14 C1 123.1(2) . . ?
C19 C14 C1 118.4(2) . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 H16A 119.7 . . ?
C15 C16 H16A 119.7 . . ?
C16 C17 C18 119.6(3) . . ?
C16 C17 H17A 120.2 . . ?
C18 C17 H17A 120.2 . . ?
C17 C18 C19 120.5(3) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
C18 C19 C14 120.4(3) . . ?
C18 C19 H19A 119.8 . . ?
C14 C19 H19A 119.8 . . ?
C25 C20 C21 120.0(2) . . ?
C25 C20 S1 122.95(18) . . ?
C21 C20 S1 116.9(2) . . ?
C22 C21 C20 122.1(2) . . ?
C22 C21 H21A 119.0 . . ?
C20 C21 H21A 119.0 . . ?
C21 C22 C23 116.4(2) . . ?
C21 C22 C22 121.3(3) . 2_646 ?
C23 C22 C22 122.3(3) . 2_646 ?
C24 C23 C22 122.3(2) . . ?
C24 C23 H23A 118.9 . . ?
C22 C23 H23A 118.9 . . ?
C23 C24 C25 120.7(3) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
O4 C25 C20 124.1(2) . . ?
O4 C25 C24 117.4(3) . . ?
C20 C25 C24 118.5(2) . . ?
O5 C26 C27 109.5(3) . 2_556 ?
O5 C26 H26A 109.8 . . ?
C27 C26 H26A 109.8 2_556 . ?
O5 C26 H26B 109.8 . . ?
C27 C26 H26B 109.8 2_556 . ?
H26A C26 H26B 108.2 . . ?
O5 C27 C26 110.1(4) . 2_556 ?
O5 C27 H27A 109.6 . . ?
C26 C27 H27A 109.6 2_556 . ?
O5 C27 H27B 109.6 . . ?
C26 C27 H27B 109.6 2_556 . ?
H27A C27 H27B 108.2 . . ?
O6 C28 C29 108.5(6) . 2_755 ?
O6 C28 H28A 110.0 . . ?
C29 C28 H28A 110.0 2_755 . ?
O6 C28 H28B 110.0 . . ?
C29 C28 H28B 110.0 2_755 . ?
H28A C28 H28B 108.4 . . ?
C28 C29 O6 104.0(5) 2_755 . ?
C28 C29 H29A 111.0 2_755 . ?
O6 C29 H29A 111.0 . . ?
C28 C29 H29B 111.0 2_755 . ?
O6 C29 H29B 111.0 . . ?
H29A C29 H29B 109.0 . . ?

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 -135.5(3) . . . . ?
C14 C1 C2 C3 106.5(3) . . . . ?
C8 C1 C2 C3 -20.0(3) . . . . ?
N1 C1 C2 C7 46.7(3) . . . . ?
C14 C1 C2 C7 -71.3(3) . . . . ?
C8 C1 C2 C7 162.2(2) . . . . ?
C7 C2 C3 C4 -2.1(5) . . . . ?
C1 C2 C3 C4 -179.9(3) . . . . ?
C2 C3 C4 C5 0.5(6) . . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
C4 C5 C6 C7 -0.7(6) . . . . ?
C5 C6 C7 C2 -0.9(5) . . . . ?
C3 C2 C7 C6 2.3(4) . . . . ?
C1 C2 C7 C6 -179.9(3) . . . . ?
N1 C1 C8 C9 -113.2(3) . . . . ?
C14 C1 C8 C9 5.1(4) . . . . ?
C2 C1 C8 C9 130.6(3) . . . . ?
N1 C1 C8 C13 65.8(3) . . . . ?
C14 C1 C8 C13 -175.9(3) . . . . ?
C2 C1 C8 C13 -50.4(3) . . . . ?
C13 C8 C9 C10 0.7(5) . . . . ?
C1 C8 C9 C10 179.8(3) . . . . ?
C8 C9 C10 C11 1.9(6) . . . . ?
C9 C10 C11 C12 -2.9(6) . . . . ?
C10 C11 C12 C13 1.3(6) . . . . ?
C11 C12 C13 C8 1.4(6) . . . . ?
C9 C8 C13 C12 -2.4(5) . . . . ?
C1 C8 C13 C12 178.5(3) . . . . ?
N1 C1 C14 C15 19.7(3) . . . . ?
C2 C1 C14 C15 136.3(2) . . . . ?
C8 C1 C14 C15 -96.5(3) . . . . ?
N1 C1 C14 C19 -162.2(2) . . . . ?
C2 C1 C14 C19 -45.6(3) . . . . ?
C8 C1 C14 C19 81.6(3) . . . . ?
C19 C14 C15 C16 -0.3(4) . . . . ?
C1 C14 C15 C16 177.8(2) . . . . ?
C14 C15 C16 C17 -1.1(4) . . . . ?
C15 C16 C17 C18 1.4(5) . . . . ?
C16 C17 C18 C19 -0.2(5) . . . . ?
C17 C18 C19 C14 -1.3(5) . . . . ?
C15 C14 C19 C18 1.5(4) . . . . ?
C1 C14 C19 C18 -176.7(3) . . . . ?
O3 S1 C20 C25 -143.3(2) . . . . ?
O1 S1 C20 C25 95.8(2) . . . . ?
O2 S1 C20 C25 -19.8(3) . . . . ?
O3 S1 C20 C21 40.9(2) . . . . ?
O1 S1 C20 C21 -80.1(2) . . . . ?
O2 S1 C20 C21 164.3(2) . . . . ?
C25 C20 C21 C22 -0.5(4) . . . . ?
S1 C20 C21 C22 175.45(19) . . . . ?
C20 C21 C22 C23 -1.0(4) . . . . ?
C20 C21 C22 C22 179.7(3) . . . 2_646 ?
C21 C22 C23 C24 1.3(4) . . . . ?
C22 C22 C23 C24 -179.4(3) 2_646 . . . ?
C22 C23 C24 C25 -0.1(5) . . . . ?
C21 C20 C25 O4 -177.9(3) . . . . ?
S1 C20 C25 O4 6.4(4) . . . . ?
C21 C20 C25 C24 1.7(4) . . . . ?
S1 C20 C25 C24 -174.0(2) . . . . ?
C23 C24 C25 O4 178.3(3) . . . . ?
C23 C24 C25 C20 -1.4(5) . . . . ?
C27 O5 C26 C27 -60.6(6) . . . 2_556 ?
C26 O5 C27 C26 61.1(6) . . . 2_556 ?
C29 O6 C28 C29 -70.0(8) . . . 2_755 ?
C28 O6 C29 C28 66.7(9) . . . 2_755 ?

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) 1.84(2) 2.649(3) 158(5) .
N1 H1N1 O5 0.87(3) 2.019(13) 2.862(3) 163(2) .
N1 H1N2 O2 0.87(3) 2.127(10) 2.980(3) 171(2) .
N1 H1N2 O1 0.87(3) 2.57(2) 3.146(3) 125(2) .
N1 H1N3 O1 0.87(3) 1.894(11) 2.751(3) 169(2) 2_656

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.053
_database_code_depnum_ccdc_archive 'CCDC 1026002'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_11

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 2(C3 H7 N O)'
_chemical_formula_sum            'C56 H58 N4 O10 S2'
_chemical_formula_weight         1011.18

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                   10.6098(10)
_cell_length_b                   12.0437(9)
_cell_length_c                   12.3814(8)
_cell_angle_alpha                64.981(7)
_cell_angle_beta                 78.038(7)
_cell_angle_gamma                66.971(8)
_cell_volume                     1317.73(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2391
_cell_measurement_theta_min      3.42
_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    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             534
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9650
_exptl_absorpt_correction_T_max  0.9744
_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            7789
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6013
_reflns_number_gt                4463
_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)+(0.0578P)²+0.3274P] 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         6013
_refine_ls_number_parameters     339
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1372
_refine_ls_wR_factor_gt          0.1228
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.81188(5) 0.05659(5) 1.18216(4) 0.03702(15) Uani 1 1 d . . .
O1 O 0.87558(16) 0.09741(17) 1.24309(15) 0.0600(4) Uani 1 1 d . . .
O2 O 0.91013(13) -0.03704(14) 1.13165(13) 0.0463(4) Uani 1 1 d . . .
O3 O 0.71977(15) 0.16430(14) 1.09246(12) 0.0520(4) Uani 1 1 d . . .
O4 O 0.7565(2) -0.1885(2) 1.20216(18) 0.0810(6) Uani 1 1 d D . .
H4O H 0.813(3) -0.148(3) 1.166(3) 0.121 Uiso 1 1 d D . .
O5 O 0.6568(2) 0.01091(19) 0.8888(2) 0.0988(8) Uani 1 1 d . . .
N1 N 0.79778(15) 0.17072(14) 0.86303(13) 0.0326(3) Uani 1 1 d D . .
H1N1 H 0.7742(17) 0.1725(19) 0.9344(11) 0.049 Uiso 1 1 d D . .
H1N2 H 0.8848(9) 0.1293(17) 0.8617(16) 0.049 Uiso 1 1 d D . .
H1N3 H 0.7570(16) 0.1244(17) 0.8556(17) 0.049 Uiso 1 1 d D . .
N2 N 0.6959(2) -0.1467(2) 0.8199(2) 0.0747(7) Uani 1 1 d . . .
C1 C 0.75523(17) 0.30660(16) 0.76704(16) 0.0304(4) Uani 1 1 d . . .
C2 C 0.60666(18) 0.37687(17) 0.80184(15) 0.0313(4) Uani 1 1 d . . .
C3 C 0.5070(2) 0.3211(2) 0.8240(2) 0.0456(5) Uani 1 1 d . . .
H3A H 0.5301 0.2421 0.8158 0.055 Uiso 1 1 calc R . .
C4 C 0.3734(2) 0.3815(2) 0.8581(2) 0.0560(6) Uani 1 1 d . . .
H4A H 0.3076 0.3432 0.8723 0.067 Uiso 1 1 calc R . .
C5 C 0.3384(2) 0.4977(2) 0.8709(2) 0.0542(6) Uani 1 1 d . . .
H5A H 0.2492 0.5373 0.8953 0.065 Uiso 1 1 calc R . .
C6 C 0.4341(2) 0.5549(2) 0.8480(2) 0.0575(6) Uani 1 1 d . . .
H6A H 0.4099 0.6343 0.8558 0.069 Uiso 1 1 calc R . .
C7 C 0.5678(2) 0.4955(2) 0.8129(2) 0.0478(5) Uani 1 1 d . . .
H7A H 0.6322 0.5360 0.7967 0.057 Uiso 1 1 calc R . .
C8 C 0.85241(18) 0.37359(18) 0.76632(17) 0.0344(4) Uani 1 1 d . . .
C9 C 0.9004(2) 0.3537(2) 0.8710(2) 0.0460(5) Uani 1 1 d . . .
H9A H 0.8774 0.2950 0.9430 0.055 Uiso 1 1 calc R . .
C10 C 0.9826(2) 0.4199(2) 0.8704(2) 0.0581(6) Uani 1 1 d . . .
H10A H 1.0146 0.4048 0.9415 0.070 Uiso 1 1 calc R . .
C11 C 1.0162(2) 0.5070(3) 0.7658(3) 0.0643(7) Uani 1 1 d . . .
H11A H 1.0719 0.5508 0.7651 0.077 Uiso 1 1 calc R . .
C12 C 0.9676(3) 0.5294(3) 0.6620(3) 0.0741(8) Uani 1 1 d . . .
H12A H 0.9889 0.5901 0.5907 0.089 Uiso 1 1 calc R . .
C13 C 0.8870(3) 0.4630(2) 0.6615(2) 0.0575(6) Uani 1 1 d . . .
H13A H 0.8556 0.4788 0.5899 0.069 Uiso 1 1 calc R . .
C14 C 0.76726(18) 0.29122(18) 0.64799(16) 0.0337(4) Uani 1 1 d . . .
C15 C 0.6736(2) 0.3731(2) 0.56177(19) 0.0560(6) Uani 1 1 d . . .
H15A H 0.5982 0.4390 0.5762 0.067 Uiso 1 1 calc R . .
C16 C 0.6890(3) 0.3597(3) 0.4540(2) 0.0677(7) Uani 1 1 d . . .
H16A H 0.6250 0.4175 0.3964 0.081 Uiso 1 1 calc R . .
C17 C 0.7965(3) 0.2631(3) 0.4308(2) 0.0576(6) Uani 1 1 d . . .
H17A H 0.8049 0.2528 0.3590 0.069 Uiso 1 1 calc R . .
C18 C 0.8911(3) 0.1821(2) 0.5140(2) 0.0662(7) Uani 1 1 d . . .
H18A H 0.9660 0.1166 0.4985 0.079 Uiso 1 1 calc R . .
C19 C 0.8777(2) 0.1958(2) 0.6220(2) 0.0549(6) Uani 1 1 d . . .
H19A H 0.9442 0.1397 0.6778 0.066 Uiso 1 1 calc R . .
C20 C 0.70787(19) -0.02773(18) 1.28863(16) 0.0361(4) Uani 1 1 d . . .
C21 C 0.6924(2) -0.1349(2) 1.2842(2) 0.0549(6) Uani 1 1 d . . .
C22 C 0.6029(3) -0.1903(3) 1.3679(3) 0.0840(10) Uani 1 1 d . . .
H22A H 0.5927 -0.2636 1.3680 0.101 Uiso 1 1 calc R . .
C23 C 0.5292(3) -0.1382(3) 1.4507(3) 0.0828(10) Uani 1 1 d . . .
H23A H 0.4694 -0.1769 1.5054 0.099 Uiso 1 1 calc R . .
C24 C 0.5410(2) -0.0289(2) 1.45572(19) 0.0479(5) Uani 1 1 d . . .
C25 C 0.63403(19) 0.02254(19) 1.37429(16) 0.0385(4) Uani 1 1 d . . .
H25A H 0.6477 0.0931 1.3769 0.046 Uiso 1 1 calc R . .
C26 C 0.6257(3) -0.0723(2) 0.8799(3) 0.0734(8) Uani 1 1 d . . .
H26 H 0.5444 -0.0839 0.9194 0.088 Uiso 1 1 calc R . .
C27 C 0.8202(5) -0.1320(5) 0.7543(6) 0.182(3) Uani 1 1 d . . .
H27A H 0.7989 -0.0525 0.6849 0.272 Uiso 1 1 calc R . .
H27B H 0.8685 -0.2046 0.7303 0.272 Uiso 1 1 calc R . .
H27C H 0.8766 -0.1291 0.8038 0.272 Uiso 1 1 calc R . .
C28 C 0.6487(3) -0.2423(3) 0.8148(3) 0.0800(9) Uani 1 1 d . . .
H28A H 0.5628 -0.2393 0.8597 0.120 Uiso 1 1 calc R . .
H28B H 0.7153 -0.3278 0.8480 0.120 Uiso 1 1 calc R . .
H28C H 0.6367 -0.2231 0.7332 0.120 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 1.4327(16) . ?
S1 O3 1.4529(15) . ?
S1 O2 1.4684(13) . ?
S1 C20 1.7687(18) . ?
O4 C21 1.355(3) . ?
O4 H4O 0.85(2) . ?
O5 C26 1.221(3) . ?
N1 C1 1.514(2) . ?
N1 H1N1 0.87(2) . ?
N1 H1N2 0.86(2) . ?
N1 H1N3 0.87(2) . ?
N2 C26 1.312(3) . ?
N2 C27 1.431(4) . ?
N2 C28 1.452(3) . ?
C1 C8 1.535(2) . ?
C1 C14 1.536(2) . ?
C1 C2 1.539(2) . ?
C2 C7 1.383(3) . ?
C2 C3 1.387(3) . ?
C3 C4 1.386(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.369(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.360(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.388(3) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.381(3) . ?
C8 C9 1.383(3) . ?
C9 C10 1.390(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.363(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.365(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(3) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.372(3) . ?
C14 C19 1.379(3) . ?
C15 C16 1.381(3) . ?
C15 H15A 0.9300 . ?
C16 C17 1.357(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.354(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.388(3) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.388(3) . ?
C20 C25 1.390(2) . ?
C21 C22 1.387(3) . ?
C22 C23 1.372(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.397(3) . ?
C23 H23A 0.9300 . ?
C24 C25 1.383(3) . ?
C24 C24 1.489(4) 2_658 ?
C25 H25A 0.9300 . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 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 113.53(10) . . ?
O1 S1 O2 113.35(9) . . ?
O3 S1 O2 110.69(9) . . ?
O1 S1 C20 107.67(9) . . ?
O3 S1 C20 105.52(9) . . ?
O2 S1 C20 105.39(9) . . ?
C21 O4 H4O 102(2) . . ?
C1 N1 H1N1 111.6(13) . . ?
C1 N1 H1N2 113.6(13) . . ?
H1N1 N1 H1N2 106.7(12) . . ?
C1 N1 H1N3 110.2(13) . . ?
H1N1 N1 H1N3 106.6(12) . . ?
H1N2 N1 H1N3 107.9(12) . . ?
C26 N2 C27 120.1(3) . . ?
C26 N2 C28 121.6(2) . . ?
C27 N2 C28 118.3(3) . . ?
N1 C1 C8 108.00(14) . . ?
N1 C1 C14 107.13(14) . . ?
C8 C1 C14 111.32(14) . . ?
N1 C1 C2 106.10(13) . . ?
C8 C1 C2 111.45(14) . . ?
C14 C1 C2 112.51(15) . . ?
C7 C2 C3 117.83(17) . . ?
C7 C2 C1 122.01(16) . . ?
C3 C2 C1 120.16(16) . . ?
C4 C3 C2 120.9(2) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C5 C4 C3 120.0(2) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C6 C5 C4 120.0(2) . . ?
C6 C5 H5A 120.0 . . ?
C4 C5 H5A 120.0 . . ?
C5 C6 C7 120.3(2) . . ?
C5 C6 H6A 119.8 . . ?
C7 C6 H6A 119.8 . . ?
C2 C7 C6 120.9(2) . . ?
C2 C7 H7A 119.6 . . ?
C6 C7 H7A 119.6 . . ?
C13 C8 C9 117.74(19) . . ?
C13 C8 C1 120.77(18) . . ?
C9 C8 C1 121.33(17) . . ?
C8 C9 C10 121.0(2) . . ?
C8 C9 H9A 119.5 . . ?
C10 C9 H9A 119.5 . . ?
C11 C10 C9 120.2(2) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 119.4(2) . . ?
C10 C11 H11A 120.3 . . ?
C12 C11 H11A 120.3 . . ?
C11 C12 C13 120.8(2) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C8 C13 C12 120.8(2) . . ?
C8 C13 H13A 119.6 . . ?
C12 C13 H13A 119.6 . . ?
C15 C14 C19 117.19(19) . . ?
C15 C14 C1 122.41(17) . . ?
C19 C14 C1 120.35(18) . . ?
C14 C15 C16 121.2(2) . . ?
C14 C15 H15A 119.4 . . ?
C16 C15 H15A 119.4 . . ?
C17 C16 C15 120.9(2) . . ?
C17 C16 H16A 119.5 . . ?
C15 C16 H16A 119.5 . . ?
C18 C17 C16 118.8(2) . . ?
C18 C17 H17A 120.6 . . ?
C16 C17 H17A 120.6 . . ?
C17 C18 C19 120.8(2) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C14 C19 C18 121.0(2) . . ?
C14 C19 H19A 119.5 . . ?
C18 C19 H19A 119.5 . . ?
C21 C20 C25 120.35(17) . . ?
C21 C20 S1 122.35(14) . . ?
C25 C20 S1 117.18(15) . . ?
O4 C21 C22 117.2(2) . . ?
O4 C21 C20 124.74(19) . . ?
C22 C21 C20 118.10(19) . . ?
C23 C22 C21 120.8(2) . . ?
C23 C22 H22A 119.6 . . ?
C21 C22 H22A 119.6 . . ?
C22 C23 C24 122.2(2) . . ?
C22 C23 H23A 118.9 . . ?
C24 C23 H23A 118.9 . . ?
C25 C24 C23 116.30(18) . . ?
C25 C24 C24 121.6(2) . 2_658 ?
C23 C24 C24 122.1(2) . 2_658 ?
C24 C25 C20 122.16(19) . . ?
C24 C25 H25A 118.9 . . ?
C20 C25 H25A 118.9 . . ?
O5 C26 N2 126.3(3) . . ?
O5 C26 H26 116.9 . . ?
N2 C26 H26 116.9 . . ?
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 . . ?
N2 C28 H28A 109.5 . . ?
N2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 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 125.98(19) . . . . ?
C8 C1 C2 C7 8.7(2) . . . . ?
C14 C1 C2 C7 -117.2(2) . . . . ?
N1 C1 C2 C3 -53.6(2) . . . . ?
C8 C1 C2 C3 -170.90(17) . . . . ?
C14 C1 C2 C3 63.3(2) . . . . ?
C7 C2 C3 C4 -1.1(3) . . . . ?
C1 C2 C3 C4 178.49(19) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C3 C4 C5 C6 1.2(4) . . . . ?
C4 C5 C6 C7 -0.8(4) . . . . ?
C3 C2 C7 C6 1.5(3) . . . . ?
C1 C2 C7 C6 -178.0(2) . . . . ?
C5 C6 C7 C2 -0.6(4) . . . . ?
N1 C1 C8 C13 147.70(18) . . . . ?
C14 C1 C8 C13 30.4(2) . . . . ?
C2 C1 C8 C13 -96.1(2) . . . . ?
N1 C1 C8 C9 -36.9(2) . . . . ?
C14 C1 C8 C9 -154.26(18) . . . . ?
C2 C1 C8 C9 79.2(2) . . . . ?
C13 C8 C9 C10 -1.0(3) . . . . ?
C1 C8 C9 C10 -176.55(19) . . . . ?
C8 C9 C10 C11 0.5(4) . . . . ?
C9 C10 C11 C12 0.6(4) . . . . ?
C10 C11 C12 C13 -1.3(4) . . . . ?
C9 C8 C13 C12 0.4(3) . . . . ?
C1 C8 C13 C12 175.9(2) . . . . ?
C11 C12 C13 C8 0.8(4) . . . . ?
N1 C1 C14 C15 141.01(19) . . . . ?
C8 C1 C14 C15 -101.1(2) . . . . ?
C2 C1 C14 C15 24.8(2) . . . . ?
N1 C1 C14 C19 -41.5(2) . . . . ?
C8 C1 C14 C19 76.3(2) . . . . ?
C2 C1 C14 C19 -157.75(18) . . . . ?
C19 C14 C15 C16 0.4(4) . . . . ?
C1 C14 C15 C16 178.0(2) . . . . ?
C14 C15 C16 C17 1.2(4) . . . . ?
C15 C16 C17 C18 -2.0(4) . . . . ?
C16 C17 C18 C19 1.1(4) . . . . ?
C15 C14 C19 C18 -1.3(3) . . . . ?
C1 C14 C19 C18 -178.9(2) . . . . ?
C17 C18 C19 C14 0.6(4) . . . . ?
O1 S1 C20 C21 -143.95(19) . . . . ?
O3 S1 C20 C21 94.5(2) . . . . ?
O2 S1 C20 C21 -22.7(2) . . . . ?
O1 S1 C20 C25 39.99(19) . . . . ?
O3 S1 C20 C25 -81.57(17) . . . . ?
O2 S1 C20 C25 161.26(16) . . . . ?
C25 C20 C21 O4 178.0(2) . . . . ?
S1 C20 C21 O4 2.0(4) . . . . ?
C25 C20 C21 C22 -0.7(4) . . . . ?
S1 C20 C21 C22 -176.6(2) . . . . ?
O4 C21 C22 C23 -177.1(3) . . . . ?
C20 C21 C22 C23 1.7(5) . . . . ?
C21 C22 C23 C24 -0.6(6) . . . . ?
C22 C23 C24 C25 -1.6(5) . . . . ?
C22 C23 C24 C24 178.9(3) . . . 2_658 ?
C23 C24 C25 C20 2.7(4) . . . . ?
C24 C24 C25 C20 -177.9(3) 2_658 . . . ?
C21 C20 C25 C24 -1.6(3) . . . . ?
S1 C20 C25 C24 174.57(18) . . . . ?
C27 N2 C26 O5 -1.6(6) . . . . ?
C28 N2 C26 O5 -179.6(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
O4 H4O O2 0.85(2) 1.854(16) 2.671(2) 160(3) .
N1 H1N1 O3 0.87(2) 1.893(9) 2.766(2) 175.5(18) .
N1 H1N2 O2 0.86(2) 2.020(9) 2.879(2) 175.5(16) 2_757
N1 H1N3 O5 0.87(2) 1.910(11) 2.753(2) 163.0(17) .

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.043
_database_code_depnum_ccdc_archive 'CCDC 1026003'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_12

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 O8 S2, 2(C19 H18 N), 2(C2 H6 O S)'
_chemical_formula_sum            'C54 H56 N2 O10 S4'
_chemical_formula_weight         1021.25

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           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                   8.9446(8)
_cell_length_b                   11.9700(10)
_cell_length_c                   12.7475(8)
_cell_angle_alpha                103.421(6)
_cell_angle_beta                 107.836(7)
_cell_angle_gamma                94.705(7)
_cell_volume                     1246.36(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1979
_cell_measurement_theta_min      3.43
_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          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             538
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9465
_exptl_absorpt_correction_T_max  0.9631
_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            7453
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         27.56
_reflns_number_total             5697
_reflns_number_gt                4365
_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)+(0.0698P)²+0.7940P] 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         5697
_refine_ls_number_parameters     330
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1560
_refine_ls_wR_factor_gt          0.1404
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.40841(7) 0.64947(5) 0.33475(4) 0.02717(16) Uani 1 1 d . . .
S2 S 0.94038(10) 0.68073(7) 0.47214(7) 0.0517(2) Uani 1 1 d . . .
O1 O 0.4836(2) 0.75378(14) 0.43035(13) 0.0349(4) Uani 1 1 d . . .
O2 O 0.4499(2) 0.54589(15) 0.36996(15) 0.0416(5) Uani 1 1 d . . .
O3 O 0.2405(2) 0.64440(19) 0.28224(15) 0.0466(5) Uani 1 1 d . . .
O4 O 0.6539(3) 0.85107(17) 0.32730(17) 0.0531(6) Uani 1 1 d D . .
H4O H 0.610(4) 0.838(3) 0.375(3) 0.080 Uiso 1 1 d D . .
O5 O 0.8882(3) 0.61856(19) 0.5461(2) 0.0562(6) Uani 1 1 d . . .
N1 N 0.6588(2) 0.68325(16) 0.63215(15) 0.0250(4) Uani 1 1 d D . .
H1N1 H 0.7379(18) 0.667(2) 0.609(2) 0.037 Uiso 1 1 d D . .
H1N2 H 0.5891(19) 0.701(2) 0.5781(16) 0.037 Uiso 1 1 d D . .
H1N3 H 0.618(2) 0.6214(14) 0.643(2) 0.037 Uiso 1 1 d D . .
C1 C 0.7124(3) 0.78412(19) 0.73877(18) 0.0242(4) Uani 1 1 d . . .
C2 C 0.8351(3) 0.7521(2) 0.83646(18) 0.0261(5) Uani 1 1 d . . .
C3 C 0.8962(3) 0.8346(2) 0.9430(2) 0.0366(6) Uani 1 1 d . . .
H3A H 0.8630 0.9067 0.9522 0.044 Uiso 1 1 calc R . .
C4 C 1.0049(3) 0.8107(3) 1.0345(2) 0.0455(7) Uani 1 1 d . . .
H4A H 1.0453 0.8667 1.1047 0.055 Uiso 1 1 calc R . .
C5 C 1.0541(3) 0.7033(3) 1.0221(2) 0.0502(7) Uani 1 1 d . . .
H5A H 1.1268 0.6866 1.0840 0.060 Uiso 1 1 calc R . .
C6 C 0.9957(3) 0.6216(3) 0.9184(3) 0.0457(7) Uani 1 1 d . . .
H6A H 1.0289 0.5495 0.9102 0.055 Uiso 1 1 calc R . .
C7 C 0.8870(3) 0.6453(2) 0.8250(2) 0.0338(5) Uani 1 1 d . . .
H7A H 0.8491 0.5894 0.7547 0.041 Uiso 1 1 calc R . .
C8 C 0.7858(3) 0.88309(19) 0.70271(19) 0.0278(5) Uani 1 1 d . . .
C9 C 0.9474(3) 0.8983(2) 0.7191(2) 0.0346(5) Uani 1 1 d . . .
H9A H 1.0112 0.8534 0.7583 0.042 Uiso 1 1 calc R . .
C10 C 1.0154(4) 0.9792(2) 0.6779(2) 0.0443(7) Uani 1 1 d . . .
H10A H 1.1238 0.9876 0.6887 0.053 Uiso 1 1 calc R . .
C11 C 0.9230(4) 1.0469(2) 0.6213(3) 0.0523(8) Uani 1 1 d . . .
H11A H 0.9688 1.1025 0.5952 0.063 Uiso 1 1 calc R . .
C12 C 0.7623(4) 1.0321(2) 0.6032(3) 0.0504(7) Uani 1 1 d . . .
H12A H 0.6994 1.0777 0.5643 0.061 Uiso 1 1 calc R . .
C13 C 0.6935(3) 0.9500(2) 0.6423(2) 0.0383(6) Uani 1 1 d . . .
H13A H 0.5842 0.9395 0.6279 0.046 Uiso 1 1 calc R . .
C14 C 0.5684(3) 0.8065(2) 0.77773(19) 0.0305(5) Uani 1 1 d . . .
C15 C 0.5403(4) 0.9175(3) 0.8196(2) 0.0451(7) Uani 1 1 d . . .
H15A H 0.6030 0.9821 0.8173 0.054 Uiso 1 1 calc R . .
C16 C 0.4181(4) 0.9322(3) 0.8653(3) 0.0592(9) Uani 1 1 d . . .
H16A H 0.3975 1.0068 0.8907 0.071 Uiso 1 1 calc R . .
C17 C 0.3275(4) 0.8384(4) 0.8733(3) 0.0604(10) Uani 1 1 d . . .
H17A H 0.2486 0.8495 0.9064 0.073 Uiso 1 1 calc R . .
C18 C 0.3544(3) 0.7283(3) 0.8324(3) 0.0535(8) Uani 1 1 d . . .
H18A H 0.2929 0.6642 0.8369 0.064 Uiso 1 1 calc R . .
C19 C 0.4732(3) 0.7125(3) 0.7842(2) 0.0403(6) Uani 1 1 d . . .
H19A H 0.4895 0.6374 0.7557 0.048 Uiso 1 1 calc R . .
C20 C 0.4979(3) 0.65766(19) 0.23023(18) 0.0258(5) Uani 1 1 d . . .
C21 C 0.6070(3) 0.7520(2) 0.2396(2) 0.0341(5) Uani 1 1 d . . .
C22 C 0.6744(4) 0.7449(2) 0.1539(2) 0.0447(7) Uani 1 1 d . . .
H22A H 0.7479 0.8071 0.1586 0.054 Uiso 1 1 calc R . .
C23 C 0.6346(3) 0.6476(2) 0.0624(2) 0.0404(6) Uani 1 1 d . . .
H23A H 0.6836 0.6450 0.0074 0.048 Uiso 1 1 calc R . .
C24 C 0.5225(3) 0.5525(2) 0.04966(18) 0.0289(5) Uani 1 1 d . . .
C25 C 0.4558(3) 0.5610(2) 0.13554(18) 0.0284(5) Uani 1 1 d . . .
H25A H 0.3800 0.4998 0.1297 0.034 Uiso 1 1 calc R . .
C26 C 0.9045(4) 0.5768(3) 0.3409(3) 0.0589(8) Uani 1 1 d . . .
H26A H 0.9548 0.5112 0.3545 0.088 Uiso 1 1 calc R . .
H26B H 0.9472 0.6108 0.2928 0.088 Uiso 1 1 calc R . .
H26C H 0.7919 0.5515 0.3039 0.088 Uiso 1 1 calc R . .
C27 C 1.1503(4) 0.6964(3) 0.5232(3) 0.0558(8) Uani 1 1 d . . .
H27A H 1.1909 0.7464 0.5999 0.084 Uiso 1 1 calc R . .
H27B H 1.1928 0.7300 0.4747 0.084 Uiso 1 1 calc R . .
H27C H 1.1812 0.6214 0.5227 0.084 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 1.4346(19) . ?
S1 O2 1.4521(18) . ?
S1 O1 1.4664(17) . ?
S1 C20 1.768(2) . ?
S2 O5 1.482(2) . ?
S2 C26 1.757(3) . ?
S2 C27 1.767(3) . ?
O4 C21 1.360(3) . ?
O4 H4O 0.85(3) . ?
N1 C1 1.510(3) . ?
N1 H1N1 0.86(3) . ?
N1 H1N2 0.86(3) . ?
N1 H1N3 0.86(3) . ?
C1 C8 1.535(3) . ?
C1 C2 1.535(3) . ?
C1 C14 1.537(3) . ?
C2 C7 1.386(3) . ?
C2 C3 1.397(3) . ?
C3 C4 1.376(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.383(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.366(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.391(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.386(3) . ?
C8 C13 1.386(3) . ?
C9 C10 1.385(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.370(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.373(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.387(4) . ?
C14 C19 1.388(4) . ?
C15 C16 1.392(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.371(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.370(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.386(4) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.388(3) . ?
C20 C25 1.392(3) . ?
C21 C22 1.389(3) . ?
C22 C23 1.375(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.398(3) . ?
C23 H23A 0.9300 . ?
C24 C25 1.386(3) . ?
C24 C24 1.487(4) 2_665 ?
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 . ?

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 113.71(12) . . ?
O3 S1 O1 113.39(11) . . ?
O2 S1 O1 110.09(10) . . ?
O3 S1 C20 107.26(11) . . ?
O2 S1 C20 105.73(11) . . ?
O1 S1 C20 106.03(10) . . ?
O5 S2 C26 106.28(16) . . ?
O5 S2 C27 104.56(15) . . ?
C26 S2 C27 98.17(16) . . ?
C21 O4 H4O 105(3) . . ?
C1 N1 H1N1 110.8(17) . . ?
C1 N1 H1N2 109.8(17) . . ?
H1N1 N1 H1N2 108.1(14) . . ?
C1 N1 H1N3 112.1(17) . . ?
H1N1 N1 H1N3 107.5(14) . . ?
H1N2 N1 H1N3 108.5(14) . . ?
N1 C1 C8 103.93(17) . . ?
N1 C1 C2 110.04(17) . . ?
C8 C1 C2 111.71(18) . . ?
N1 C1 C14 108.53(17) . . ?
C8 C1 C14 116.03(19) . . ?
C2 C1 C14 106.52(17) . . ?
C7 C2 C3 118.3(2) . . ?
C7 C2 C1 123.6(2) . . ?
C3 C2 C1 118.1(2) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C5 C6 C7 120.7(3) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C2 C7 C6 120.2(2) . . ?
C2 C7 H7A 119.9 . . ?
C6 C7 H7A 119.9 . . ?
C9 C8 C13 118.1(2) . . ?
C9 C8 C1 119.3(2) . . ?
C13 C8 C1 122.2(2) . . ?
C10 C9 C8 121.1(2) . . ?
C10 C9 H9A 119.5 . . ?
C8 C9 H9A 119.5 . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C11 C12 C13 120.5(3) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C12 C13 C8 120.7(3) . . ?
C12 C13 H13A 119.7 . . ?
C8 C13 H13A 119.7 . . ?
C15 C14 C19 118.1(2) . . ?
C15 C14 C1 122.8(2) . . ?
C19 C14 C1 118.7(2) . . ?
C14 C15 C16 120.0(3) . . ?
C14 C15 H15A 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C17 C16 C15 121.0(3) . . ?
C17 C16 H16A 119.5 . . ?
C15 C16 H16A 119.5 . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 H17A 120.3 . . ?
C16 C17 H17A 120.3 . . ?
C17 C18 C19 120.0(3) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C18 C19 C14 121.4(3) . . ?
C18 C19 H19A 119.3 . . ?
C14 C19 H19A 119.3 . . ?
C21 C20 C25 120.0(2) . . ?
C21 C20 S1 123.86(17) . . ?
C25 C20 S1 116.15(17) . . ?
O4 C21 C20 124.6(2) . . ?
O4 C21 C22 117.4(2) . . ?
C20 C21 C22 118.0(2) . . ?
C23 C22 C21 121.3(2) . . ?
C23 C22 H22A 119.4 . . ?
C21 C22 H22A 119.4 . . ?
C22 C23 C24 121.8(2) . . ?
C22 C23 H23A 119.1 . . ?
C24 C23 H23A 119.1 . . ?
C25 C24 C23 116.2(2) . . ?
C25 C24 C24 121.6(3) . 2_665 ?
C23 C24 C24 122.2(3) . 2_665 ?
C24 C25 C20 122.6(2) . . ?
C24 C25 H25A 118.7 . . ?
C20 C25 H25A 118.7 . . ?
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 . . ?

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 0.4(3) . . . . ?
C8 C1 C2 C7 -114.5(2) . . . . ?
C14 C1 C2 C7 117.8(2) . . . . ?
N1 C1 C2 C3 -178.87(19) . . . . ?
C8 C1 C2 C3 66.2(3) . . . . ?
C14 C1 C2 C3 -61.4(3) . . . . ?
C7 C2 C3 C4 -0.2(4) . . . . ?
C1 C2 C3 C4 179.1(2) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C4 C5 C6 C7 0.0(5) . . . . ?
C3 C2 C7 C6 0.9(4) . . . . ?
C1 C2 C7 C6 -178.4(2) . . . . ?
C5 C6 C7 C2 -0.8(4) . . . . ?
N1 C1 C8 C9 -91.6(2) . . . . ?
C2 C1 C8 C9 27.0(3) . . . . ?
C14 C1 C8 C9 149.3(2) . . . . ?
N1 C1 C8 C13 80.8(3) . . . . ?
C2 C1 C8 C13 -160.6(2) . . . . ?
C14 C1 C8 C13 -38.2(3) . . . . ?
C13 C8 C9 C10 1.0(4) . . . . ?
C1 C8 C9 C10 173.8(2) . . . . ?
C8 C9 C10 C11 0.9(4) . . . . ?
C9 C10 C11 C12 -1.6(4) . . . . ?
C10 C11 C12 C13 0.4(5) . . . . ?
C11 C12 C13 C8 1.5(4) . . . . ?
C9 C8 C13 C12 -2.2(4) . . . . ?
C1 C8 C13 C12 -174.7(2) . . . . ?
N1 C1 C14 C15 -140.1(2) . . . . ?
C8 C1 C14 C15 -23.6(3) . . . . ?
C2 C1 C14 C15 101.5(3) . . . . ?
N1 C1 C14 C19 47.8(3) . . . . ?
C8 C1 C14 C19 164.3(2) . . . . ?
C2 C1 C14 C19 -70.6(3) . . . . ?
C19 C14 C15 C16 -0.8(4) . . . . ?
C1 C14 C15 C16 -172.9(2) . . . . ?
C14 C15 C16 C17 2.3(5) . . . . ?
C15 C16 C17 C18 -2.2(5) . . . . ?
C16 C17 C18 C19 0.6(5) . . . . ?
C17 C18 C19 C14 0.9(4) . . . . ?
C15 C14 C19 C18 -0.8(4) . . . . ?
C1 C14 C19 C18 171.7(2) . . . . ?
O3 S1 C20 C21 116.7(2) . . . . ?
O2 S1 C20 C21 -121.6(2) . . . . ?
O1 S1 C20 C21 -4.7(2) . . . . ?
O3 S1 C20 C25 -64.7(2) . . . . ?
O2 S1 C20 C25 56.9(2) . . . . ?
O1 S1 C20 C25 173.82(18) . . . . ?
C25 C20 C21 O4 178.8(2) . . . . ?
S1 C20 C21 O4 -2.7(4) . . . . ?
C25 C20 C21 C22 -1.7(4) . . . . ?
S1 C20 C21 C22 176.8(2) . . . . ?
O4 C21 C22 C23 179.6(3) . . . . ?
C20 C21 C22 C23 0.1(4) . . . . ?
C21 C22 C23 C24 1.3(5) . . . . ?
C22 C23 C24 C25 -1.1(4) . . . . ?
C22 C23 C24 C24 179.4(3) . . . 2_665 ?
C23 C24 C25 C20 -0.6(4) . . . . ?
C24 C24 C25 C20 178.9(3) 2_665 . . . ?
C21 C20 C25 C24 2.0(4) . . . . ?
S1 C20 C25 C24 -176.63(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 O1 0.85(3) 1.853(18) 2.654(3) 156(4) .
N1 H1N1 O5 0.86(3) 1.836(10) 2.695(3) 173(2) .
N1 H1N2 O1 0.86(3) 2.097(11) 2.923(3) 161.4(19) .
N1 H1N3 O2 0.86(3) 1.997(13) 2.825(3) 162(2) 2_666

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.061


_database_code_depnum_ccdc_archive 'CCDC 1026004'
