# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2019

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

data_181009_yxf180912_1
_database_code_depnum_ccdc_archive 'CCDC 1894188'
loop_
_audit_author_name
_audit_author_address
'Wanzhi Chen'
;Zhejiang University
China
;
_audit_update_record             
;
2019-01-28 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H26 N2 O9 S'
_chemical_formula_weight         566.57

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.9913(8)
_cell_length_b                   20.6489(12)
_cell_length_c                   12.3839(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.075(6)
_cell_angle_gamma                90.00
_cell_volume                     2775.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2670
_cell_measurement_theta_min      3.5682
_cell_measurement_theta_max      29.5697

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9308
_exptl_absorpt_correction_T_max  0.9499
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10619
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4885
_reflns_number_gt                2783
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0972P)²+0.8401P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4885
_refine_ls_number_parameters     364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0663
_refine_ls_wR_factor_ref         0.2127
_refine_ls_wR_factor_gt          0.1751
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.50941(9) 0.14459(6) 0.01833(10) 0.1033(5) Uani 1 1 d . . .
C1 C 1.0301(3) 0.10105(15) 0.0390(3) 0.0714(9) Uani 1 1 d . . .
O5 O 0.4279(3) 0.19526(16) -0.0268(3) 0.1256(11) Uani 1 1 d . . .
C2 C 0.9780(3) 0.12940(17) 0.1312(3) 0.0755(9) Uani 1 1 d . . .
C3 C 0.8667(3) 0.17281(18) 0.1031(3) 0.0726(9) Uani 1 1 d . . .
C4 C 1.0028(3) 0.26616(16) 0.0917(3) 0.0714(9) Uani 1 1 d . . .
O7 O 1.0180(3) 0.11863(14) 0.2265(2) 0.1013(9) Uani 1 1 d . . .
C5 C 0.8788(3) 0.23584(17) 0.0836(2) 0.0708(9) Uani 1 1 d . . .
C6 C 0.6442(3) 0.17957(15) 0.0545(3) 0.0636(8) Uani 1 1 d . . .
H6 H 0.6670 0.1871 -0.0178 0.076 Uiso 1 1 calc R . .
C7 C 1.0718(3) 0.27731(19) 0.1918(3) 0.0777(10) Uani 1 1 d . . .
H7 H 1.0377 0.2682 0.2542 0.093 Uiso 1 1 calc R . .
C8 C 0.7463(3) 0.13862(19) 0.1020(3) 0.0881(11) Uani 1 1 d . . .
H8A H 0.7457 0.0990 0.0598 0.106 Uiso 1 1 calc R . .
H8B H 0.7368 0.1271 0.1761 0.106 Uiso 1 1 calc R . .
C9 C 1.1394(3) 0.06557(18) 0.0599(4) 0.0881(11) Uani 1 1 d . . .
H9 H 1.1788 0.0603 0.1315 0.106 Uiso 1 1 calc R . .
C10 C 0.7627(4) 0.27562(17) 0.0570(3) 0.0810(10) Uani 1 1 d . . .
O9 O 0.5322(3) 0.09064(15) -0.0475(3) 0.1199(11) Uani 1 1 d . . .
C11 C 1.1312(4) 0.04337(18) -0.1292(4) 0.0910(12) Uani 1 1 d . . .
O12 O 1.3584(3) 0.33598(17) 0.1146(3) 0.1245(11) Uani 1 1 d . . .
O11 O 1.1873(3) 0.01312(16) -0.2062(4) 0.1263(11) Uani 1 1 d . . .
C14 C 0.9745(3) 0.10653(18) -0.0674(3) 0.0850(11) Uani 1 1 d . . .
H14 H 0.9023 0.1306 -0.0832 0.102 Uiso 1 1 calc R . .
C15 C 1.1891(4) 0.30138(17) 0.2036(3) 0.0810(10) Uani 1 1 d . . .
H15 H 1.2329 0.3092 0.2730 0.097 Uiso 1 1 calc R . .
C16 C 1.0222(4) 0.07739(19) -0.1527(3) 0.0906(11) Uani 1 1 d . . .
H16 H 0.9815 0.0807 -0.2243 0.109 Uiso 1 1 calc R . .
N1 N 0.7863(3) 0.34382(18) 0.1059(4) 0.0997(10) Uani 1 1 d . . .
C19 C 0.6520(3) 0.24553(18) 0.0967(3) 0.0854(11) Uani 1 1 d . . .
H19A H 0.6629 0.2454 0.1760 0.102 Uiso 1 1 calc R . .
H19B H 0.5776 0.2695 0.0691 0.102 Uiso 1 1 calc R . .
C20 C 0.4631(3) 0.1150(2) 0.1379(4) 0.0915(12) Uani 1 1 d . . .
C21 C 1.2413(4) 0.31381(19) 0.1132(4) 0.0906(12) Uani 1 1 d . . .
N2 N 0.7293(4) 0.2870(2) -0.0667(3) 0.1202(13) Uani 1 1 d . . .
C23 C 0.4852(4) 0.0521(2) 0.1685(5) 0.1160(16) Uani 1 1 d . . .
H23 H 0.5279 0.0250 0.1275 0.139 Uiso 1 1 calc R . .
C24 C 1.1890(4) 0.0386(2) -0.0233(5) 0.1000(13) Uani 1 1 d . . .
H24 H 1.2635 0.0165 -0.0080 0.120 Uiso 1 1 calc R . .
C26 C 0.3820(5) 0.0677(3) 0.3231(5) 0.1266(17) Uani 1 1 d . . .
C29 C 0.4017(4) 0.1545(2) 0.1979(5) 0.1218(17) Uani 1 1 d . . .
H29 H 0.3868 0.1973 0.1770 0.146 Uiso 1 1 calc R . .
C30 C 1.0552(5) 0.2808(3) 0.0020(3) 0.1274(19) Uani 1 1 d . . .
H30 H 1.0101 0.2752 -0.0674 0.153 Uiso 1 1 calc R . .
C31 C 1.1726(6) 0.3034(3) 0.0129(4) 0.151(3) Uani 1 1 d . . .
H31 H 1.2071 0.3120 -0.0496 0.181 Uiso 1 1 calc R . .
C32 C 0.3303(7) 0.0400(4) 0.4195(6) 0.189(3) Uani 1 1 d . . .
H32A H 0.2432 0.0479 0.4102 0.283 Uiso 1 1 calc R . .
H32B H 0.3696 0.0603 0.4856 0.283 Uiso 1 1 calc R . .
H32C H 0.3453 -0.0058 0.4238 0.283 Uiso 1 1 calc R . .
C33 C 0.4442(6) 0.0291(3) 0.2599(6) 0.1374(19) Uani 1 1 d . . .
H33 H 0.4590 -0.0139 0.2799 0.165 Uiso 1 1 calc R . .
C34 C 0.3622(6) 0.1314(3) 0.2881(6) 0.145(2) Uani 1 1 d . . .
H34 H 0.3202 0.1592 0.3286 0.174 Uiso 1 1 calc R . .
O10 O 0.7591(3) 0.35268(17) 0.1933(3) 0.1248(11) Uani 1 1 d . . .
O6 O 0.8363(5) 0.38270(18) 0.0549(4) 0.1630(16) Uani 1 1 d . . .
O4 O 0.7859(4) 0.2586(2) -0.1278(3) 0.1375(13) Uani 1 1 d . . .
O8 O 0.6445(5) 0.3237(3) -0.0948(3) 0.198(2) Uani 1 1 d . . .
C51 C 1.4273(4) 0.3532(3) 0.2162(5) 0.1277(18) Uani 1 1 d . . .
H51A H 1.3843 0.3863 0.2496 0.192 Uiso 1 1 calc R . .
H51B H 1.5064 0.3693 0.2053 0.192 Uiso 1 1 calc R . .
H51C H 1.4382 0.3159 0.2629 0.192 Uiso 1 1 calc R . .
C50 C 1.1268(6) 0.0117(3) -0.3159(5) 0.140(2) Uani 1 1 d . . .
H50A H 1.0485 -0.0095 -0.3193 0.210 Uiso 1 1 calc R . .
H50B H 1.1764 -0.0115 -0.3601 0.210 Uiso 1 1 calc R . .
H50C H 1.1143 0.0552 -0.3428 0.210 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 O9 1.426(3) . ?
S1 O5 1.432(3) . ?
S1 C6 1.646(3) . ?
S1 C20 1.750(5) . ?
C1 C14 1.367(5) . ?
C1 C9 1.396(5) . ?
C1 C2 1.476(5) . ?
C2 O7 1.213(4) . ?
C2 C3 1.512(5) . ?
C3 C5 1.334(5) . ?
C3 C8 1.498(5) . ?
C4 C30 1.363(5) . ?
C4 C7 1.367(5) . ?
C4 C5 1.489(5) . ?
C5 C10 1.509(5) . ?
C6 C8 1.453(4) . ?
C6 C19 1.456(5) . ?
C7 C15 1.368(5) . ?
C9 C24 1.359(6) . ?
C10 C19 1.516(5) . ?
C10 N2 1.536(5) . ?
C10 N1 1.539(5) . ?
C11 O11 1.366(5) . ?
C11 C24 1.367(6) . ?
C11 C16 1.380(5) . ?
O12 C21 1.364(5) . ?
O12 C51 1.408(6) . ?
O11 C50 1.416(6) . ?
C14 C16 1.388(5) . ?
C15 C21 1.361(5) . ?
N1 O10 1.182(4) . ?
N1 O6 1.206(5) . ?
C20 C29 1.352(6) . ?
C20 C23 1.365(6) . ?
C21 C31 1.365(6) . ?
N2 O4 1.205(5) . ?
N2 O8 1.210(5) . ?
C23 C33 1.367(7) . ?
C26 C33 1.372(7) . ?
C26 C34 1.392(8) . ?
C26 C32 1.513(8) . ?
C29 C34 1.347(8) . ?
C30 C31 1.359(7) . ?

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
O9 S1 O5 120.21(19) . . ?
O9 S1 C6 105.47(17) . . ?
O5 S1 C6 105.44(18) . . ?
O9 S1 C20 108.2(2) . . ?
O5 S1 C20 109.7(2) . . ?
C6 S1 C20 106.99(17) . . ?
C14 C1 C9 117.6(4) . . ?
C14 C1 C2 122.9(3) . . ?
C9 C1 C2 119.5(3) . . ?
O7 C2 C1 123.7(3) . . ?
O7 C2 C3 119.2(3) . . ?
C1 C2 C3 117.1(3) . . ?
C5 C3 C8 124.8(3) . . ?
C5 C3 C2 121.3(3) . . ?
C8 C3 C2 113.8(3) . . ?
C30 C4 C7 117.1(4) . . ?
C30 C4 C5 122.6(3) . . ?
C7 C4 C5 120.2(3) . . ?
C3 C5 C4 120.9(3) . . ?
C3 C5 C10 117.8(3) . . ?
C4 C5 C10 121.3(3) . . ?
C8 C6 C19 113.7(3) . . ?
C8 C6 S1 117.3(3) . . ?
C19 C6 S1 120.5(2) . . ?
C4 C7 C15 122.5(3) . . ?
C6 C8 C3 110.8(3) . . ?
C24 C9 C1 120.7(4) . . ?
C5 C10 C19 113.6(3) . . ?
C5 C10 N2 111.3(3) . . ?
C19 C10 N2 107.9(3) . . ?
C5 C10 N1 109.1(3) . . ?
C19 C10 N1 109.9(3) . . ?
N2 C10 N1 104.6(3) . . ?
O11 C11 C24 116.3(4) . . ?
O11 C11 C16 123.9(5) . . ?
C24 C11 C16 119.8(4) . . ?
C21 O12 C51 118.0(4) . . ?
C11 O11 C50 118.9(4) . . ?
C1 C14 C16 122.2(4) . . ?
C21 C15 C7 119.5(4) . . ?
C11 C16 C14 118.6(4) . . ?
O10 N1 O6 125.3(4) . . ?
O10 N1 C10 116.8(4) . . ?
O6 N1 C10 117.7(4) . . ?
C6 C19 C10 105.8(3) . . ?
C29 C20 C23 120.2(5) . . ?
C29 C20 S1 119.5(4) . . ?
C23 C20 S1 120.3(4) . . ?
C15 C21 O12 124.9(4) . . ?
C15 C21 C31 118.4(4) . . ?
O12 C21 C31 116.7(4) . . ?
O4 N2 O8 125.1(4) . . ?
O4 N2 C10 119.0(4) . . ?
O8 N2 C10 115.8(4) . . ?
C20 C23 C33 119.5(5) . . ?
C9 C24 C11 121.1(4) . . ?
C33 C26 C34 116.0(6) . . ?
C33 C26 C32 120.9(6) . . ?
C34 C26 C32 122.9(6) . . ?
C34 C29 C20 119.8(5) . . ?
C31 C30 C4 120.8(4) . . ?
C30 C31 C21 121.6(4) . . ?
C23 C33 C26 122.0(6) . . ?
C29 C34 C26 122.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.053
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_x
_database_code_depnum_ccdc_archive 'CCDC 1894189'
loop_
_audit_author_name
_audit_author_address
'Wanzhi Chen'
;Zhejiang University
China
;
_audit_update_record             
;
2019-01-28 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H25 N3 O7 S'
_chemical_formula_weight         607.62

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   16.5068(7)
_cell_length_b                   12.2903(6)
_cell_length_c                   29.5223(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5989.3(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    2018
_cell_measurement_theta_min      3.1265
_cell_measurement_theta_max      29.3608

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9652
_exptl_absorpt_correction_T_max  0.9745
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(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  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17515
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         22.21
_reflns_number_total             3762
_reflns_number_gt                2920
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0366P)²+2.4972P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3762
_refine_ls_number_parameters     398
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0973
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.72981(4) 1.02213(6) 0.54118(2) 0.0603(2) Uani 1 1 d . . .
O7 O 0.90240(10) 0.69594(15) 0.64236(7) 0.0649(5) Uani 1 1 d . . .
O1 O 0.93223(13) 1.13778(16) 0.62022(7) 0.0716(6) Uani 1 1 d . . .
C1 C 0.87720(13) 0.88052(19) 0.62902(8) 0.0428(6) Uani 1 1 d . . .
C2 C 0.92159(16) 0.8791(2) 0.73821(8) 0.0527(7) Uani 1 1 d . . .
C3 C 0.82522(14) 1.0503(2) 0.65920(8) 0.0461(6) Uani 1 1 d . . .
N1 N 0.77993(12) 0.99030(16) 0.58741(7) 0.0499(5) Uani 1 1 d . . .
C4 C 0.93167(15) 0.7816(2) 0.63007(8) 0.0493(6) Uani 1 1 d . . .
C5 C 0.94137(14) 0.9435(2) 0.69976(8) 0.0504(6) Uani 1 1 d . . .
O3 O 0.74254(15) 1.0468(2) 0.72223(7) 0.0926(7) Uani 1 1 d . . .
O5 O 0.71253(13) 1.13574(16) 0.54475(7) 0.0853(7) Uani 1 1 d . . .
N3 N 0.86689(15) 1.15097(19) 0.63822(7) 0.0579(6) Uani 1 1 d . . .
C6 C 0.63824(15) 0.9505(2) 0.54204(8) 0.0499(6) Uani 1 1 d . . .
C7 C 0.74964(14) 1.0279(2) 0.63103(8) 0.0523(6) Uani 1 1 d . . .
H7A H 0.7164 0.9725 0.6452 0.063 Uiso 1 1 calc R . .
H7B H 0.7176 1.0935 0.6275 0.063 Uiso 1 1 calc R . .
C8 C 0.88183(13) 0.9547(2) 0.66159(8) 0.0442(6) Uani 1 1 d . . .
C9 C 1.07842(15) 0.7182(2) 0.62270(8) 0.0505(6) Uani 1 1 d . . .
O4 O 0.84711(14) 1.1489(2) 0.72613(7) 0.0943(7) Uani 1 1 d . . .
C10 C 1.01596(14) 0.7957(2) 0.61397(8) 0.0489(6) Uani 1 1 d . . .
O2 O 0.82951(13) 1.23576(16) 0.63985(8) 0.0836(7) Uani 1 1 d . . .
C11 C 0.81909(15) 0.8837(2) 0.58978(8) 0.0513(7) Uani 1 1 d . . .
H11A H 0.8481 0.8697 0.5618 0.062 Uiso 1 1 calc R . .
H11B H 0.7783 0.8276 0.5935 0.062 Uiso 1 1 calc R . .
N2 N 0.80268(16) 1.0871(2) 0.70670(8) 0.0634(6) Uani 1 1 d . . .
C12 C 0.97977(19) 0.8683(2) 0.77331(9) 0.0657(8) Uani 1 1 d . . .
C13 C 1.03194(16) 0.8855(2) 0.58764(9) 0.0620(7) Uani 1 1 d . . .
H13 H 0.9915 0.9371 0.5832 0.074 Uiso 1 1 calc R . .
C14 C 1.01533(16) 0.9928(3) 0.69734(10) 0.0738(9) Uani 1 1 d . . .
H14 H 1.0277 1.0355 0.6723 0.089 Uiso 1 1 calc R . .
C15 C 1.07221(17) 0.6302(2) 0.65343(9) 0.0626(7) Uani 1 1 d . . .
H15 H 1.0242 0.6198 0.6694 0.075 Uiso 1 1 calc R . .
C16 C 0.49846(19) 0.9370(3) 0.56099(11) 0.0874(10) Uani 1 1 d . . .
H16 H 0.4521 0.9684 0.5732 0.105 Uiso 1 1 calc R . .
C17 C 1.15430(15) 0.7329(2) 0.60053(9) 0.0603(7) Uani 1 1 d . . .
C18 C 1.10753(19) 0.9008(3) 0.56741(10) 0.0775(9) Uani 1 1 d . . .
H18 H 1.1173 0.9626 0.5500 0.093 Uiso 1 1 calc R . .
C19 C 0.8291(2) 0.7694(2) 0.78191(10) 0.0803(9) Uani 1 1 d . . .
H19 H 0.7788 0.7364 0.7852 0.096 Uiso 1 1 calc R . .
C20 C 1.21643(18) 0.6558(3) 0.60695(12) 0.0824(10) Uani 1 1 d . . .
H20 H 1.2647 0.6630 0.5910 0.099 Uiso 1 1 calc R . .
C21 C 1.20689(19) 0.5716(3) 0.63588(12) 0.0851(10) Uani 1 1 d . . .
H21 H 1.2483 0.5210 0.6396 0.102 Uiso 1 1 calc R . .
C22 C 0.84567(17) 0.8268(2) 0.74376(9) 0.0603(7) Uani 1 1 d . . .
H22 H 0.8069 0.8318 0.7210 0.072 Uiso 1 1 calc R . .
C23 C 1.16622(18) 0.8260(3) 0.57311(10) 0.0768(9) Uani 1 1 d . . .
H23 H 1.2158 0.8357 0.5587 0.092 Uiso 1 1 calc R . .
C24 C 0.5633(2) 0.7901(3) 0.52637(11) 0.0809(9) Uani 1 1 d . . .
H24 H 0.5614 0.7198 0.5148 0.097 Uiso 1 1 calc R . .
C25 C 1.07284(19) 0.9806(3) 0.73167(12) 0.0966(12) Uani 1 1 d . . .
H25 H 1.1231 1.0143 0.7292 0.116 Uiso 1 1 calc R . .
C26 C 0.49472(18) 0.8342(3) 0.54424(10) 0.0729(9) Uani 1 1 d . . .
C27 C 0.56994(18) 0.9961(3) 0.56031(10) 0.0762(9) Uani 1 1 d . . .
H27 H 0.5715 1.0662 0.5721 0.091 Uiso 1 1 calc R . .
C28 C 1.13511(19) 0.5607(3) 0.66002(11) 0.0762(9) Uani 1 1 d . . .
H28 H 1.1300 0.5049 0.6811 0.091 Uiso 1 1 calc R . .
C33 C 0.4160(2) 0.7699(4) 0.54568(13) 0.1183(15) Uani 1 1 d . . .
H33A H 0.3988 0.7539 0.5153 0.177 Uiso 1 1 calc R . .
H33B H 0.3751 0.8121 0.5607 0.177 Uiso 1 1 calc R . .
H33C H 0.4245 0.7032 0.5619 0.177 Uiso 1 1 calc R . .
C29 C 0.63559(17) 0.8468(2) 0.52498(10) 0.0686(8) Uani 1 1 d . . .
H29 H 0.6817 0.8151 0.5127 0.082 Uiso 1 1 calc R . .
C30 C 0.9598(2) 0.8071(3) 0.81220(11) 0.0850(10) Uani 1 1 d . . .
H30 H 0.9978 0.7997 0.8353 0.102 Uiso 1 1 calc R . .
C31 C 0.8869(3) 0.7592(3) 0.81661(11) 0.0887(11) Uani 1 1 d . . .
H31 H 0.8747 0.7194 0.8425 0.106 Uiso 1 1 calc R . .
C32 C 1.0553(2) 0.9198(3) 0.76855(12) 0.0926(11) Uani 1 1 d . . .
H32 H 1.0940 0.9118 0.7912 0.111 Uiso 1 1 calc R . .
O8 O 0.77780(11) 0.98114(19) 0.50477(6) 0.0802(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O8 1.427(2) . ?
S1 O5 1.429(2) . ?
S1 N1 1.643(2) . ?
S1 C6 1.749(2) . ?
O7 C4 1.214(3) . ?
O1 N3 1.213(3) . ?
C1 C8 1.328(3) . ?
C1 C11 1.505(3) . ?
C1 C4 1.512(3) . ?
C2 C22 1.418(4) . ?
C2 C12 1.419(4) . ?
C2 C5 1.421(3) . ?
C3 C8 1.503(3) . ?
C3 N2 1.519(3) . ?
C3 C7 1.525(3) . ?
C3 N3 1.545(3) . ?
N1 C7 1.457(3) . ?
N1 C11 1.462(3) . ?
C4 C10 1.481(3) . ?
C5 C14 1.365(4) . ?
C5 C8 1.502(3) . ?
O3 N2 1.200(3) . ?
N3 O2 1.212(3) . ?
C6 C27 1.370(4) . ?
C6 C29 1.371(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C9 C15 1.416(4) . ?
C9 C17 1.425(3) . ?
C9 C10 1.427(3) . ?
O4 N2 1.202(3) . ?
C10 C13 1.376(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C32 1.405(4) . ?
C12 C30 1.412(4) . ?
C13 C18 1.396(4) . ?
C13 H13 0.9300 . ?
C14 C25 1.397(4) . ?
C14 H14 0.9300 . ?
C15 C28 1.358(4) . ?
C15 H15 0.9300 . ?
C16 C26 1.359(5) . ?
C16 C27 1.386(4) . ?
C16 H16 0.9300 . ?
C17 C20 1.409(4) . ?
C17 C23 1.415(4) . ?
C18 C23 1.346(4) . ?
C18 H18 0.9300 . ?
C19 C22 1.356(4) . ?
C19 C31 1.405(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.351(4) . ?
C20 H20 0.9300 . ?
C21 C28 1.389(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C26 1.361(4) . ?
C24 C29 1.383(4) . ?
C24 H24 0.9300 . ?
C25 C32 1.352(4) . ?
C25 H25 0.9300 . ?
C26 C33 1.520(4) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C29 H29 0.9300 . ?
C30 C31 1.346(5) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 H32 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
O8 S1 O5 120.75(14) . . ?
O8 S1 N1 105.19(11) . . ?
O5 S1 N1 105.77(12) . . ?
O8 S1 C6 108.23(12) . . ?
O5 S1 C6 108.56(13) . . ?
N1 S1 C6 107.65(11) . . ?
C8 C1 C11 125.2(2) . . ?
C8 C1 C4 120.2(2) . . ?
C11 C1 C4 114.6(2) . . ?
C22 C2 C12 118.1(3) . . ?
C22 C2 C5 123.2(2) . . ?
C12 C2 C5 118.7(3) . . ?
C8 C3 N2 109.96(19) . . ?
C8 C3 C7 113.1(2) . . ?
N2 C3 C7 110.9(2) . . ?
C8 C3 N3 111.58(19) . . ?
N2 C3 N3 103.9(2) . . ?
C7 C3 N3 106.90(19) . . ?
C7 N1 C11 113.16(19) . . ?
C7 N1 S1 119.08(16) . . ?
C11 N1 S1 118.40(16) . . ?
O7 C4 C10 124.9(2) . . ?
O7 C4 C1 117.8(2) . . ?
C10 C4 C1 117.3(2) . . ?
C14 C5 C2 119.6(2) . . ?
C14 C5 C8 120.3(2) . . ?
C2 C5 C8 120.0(2) . . ?
O2 N3 O1 125.8(2) . . ?
O2 N3 C3 116.5(2) . . ?
O1 N3 C3 117.7(2) . . ?
C27 C6 C29 119.9(3) . . ?
C27 C6 S1 120.7(2) . . ?
C29 C6 S1 119.3(2) . . ?
N1 C7 C3 105.00(19) . . ?
N1 C7 H7A 110.7 . . ?
C3 C7 H7A 110.7 . . ?
N1 C7 H7B 110.7 . . ?
C3 C7 H7B 110.7 . . ?
H7A C7 H7B 108.8 . . ?
C1 C8 C5 121.2(2) . . ?
C1 C8 C3 117.9(2) . . ?
C5 C8 C3 120.9(2) . . ?
C15 C9 C17 117.1(2) . . ?
C15 C9 C10 125.0(2) . . ?
C17 C9 C10 117.9(2) . . ?
C13 C10 C9 119.9(2) . . ?
C13 C10 C4 117.1(2) . . ?
C9 C10 C4 122.9(2) . . ?
N1 C11 C1 110.0(2) . . ?
N1 C11 H11A 109.7 . . ?
C1 C11 H11A 109.7 . . ?
N1 C11 H11B 109.7 . . ?
C1 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
O3 N2 O4 125.7(3) . . ?
O3 N2 C3 115.6(2) . . ?
O4 N2 C3 118.6(2) . . ?
C32 C12 C30 121.9(3) . . ?
C32 C12 C2 119.0(3) . . ?
C30 C12 C2 119.1(3) . . ?
C10 C13 C18 121.4(3) . . ?
C10 C13 H13 119.3 . . ?
C18 C13 H13 119.3 . . ?
C5 C14 C25 121.5(3) . . ?
C5 C14 H14 119.3 . . ?
C25 C14 H14 119.3 . . ?
C28 C15 C9 121.1(3) . . ?
C28 C15 H15 119.4 . . ?
C9 C15 H15 119.4 . . ?
C26 C16 C27 121.4(3) . . ?
C26 C16 H16 119.3 . . ?
C27 C16 H16 119.3 . . ?
C20 C17 C23 121.3(3) . . ?
C20 C17 C9 119.5(3) . . ?
C23 C17 C9 119.2(3) . . ?
C23 C18 C13 119.8(3) . . ?
C23 C18 H18 120.1 . . ?
C13 C18 H18 120.1 . . ?
C22 C19 C31 121.1(3) . . ?
C22 C19 H19 119.5 . . ?
C31 C19 H19 119.5 . . ?
C21 C20 C17 121.0(3) . . ?
C21 C20 H20 119.5 . . ?
C17 C20 H20 119.5 . . ?
C20 C21 C28 119.8(3) . . ?
C20 C21 H21 120.1 . . ?
C28 C21 H21 120.1 . . ?
C19 C22 C2 120.6(3) . . ?
C19 C22 H22 119.7 . . ?
C2 C22 H22 119.7 . . ?
C18 C23 C17 121.6(3) . . ?
C18 C23 H23 119.2 . . ?
C17 C23 H23 119.2 . . ?
C26 C24 C29 121.9(3) . . ?
C26 C24 H24 119.1 . . ?
C29 C24 H24 119.1 . . ?
C32 C25 C14 119.9(3) . . ?
C32 C25 H25 120.1 . . ?
C14 C25 H25 120.1 . . ?
C16 C26 C24 118.3(3) . . ?
C16 C26 C33 120.8(3) . . ?
C24 C26 C33 120.9(4) . . ?
C6 C27 C16 119.4(3) . . ?
C6 C27 H27 120.3 . . ?
C16 C27 H27 120.3 . . ?
C15 C28 C21 121.2(3) . . ?
C15 C28 H28 119.4 . . ?
C21 C28 H28 119.4 . . ?
C26 C33 H33A 109.5 . . ?
C26 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C26 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C6 C29 C24 119.1(3) . . ?
C6 C29 H29 120.5 . . ?
C24 C29 H29 120.5 . . ?
C31 C30 C12 121.3(3) . . ?
C31 C30 H30 119.3 . . ?
C12 C30 H30 119.3 . . ?
C30 C31 C19 119.8(3) . . ?
C30 C31 H31 120.1 . . ?
C19 C31 H31 120.1 . . ?
C25 C32 C12 121.3(3) . . ?
C25 C32 H32 119.4 . . ?
C12 C32 H32 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 S1 N1 C7 175.67(18) . . . . ?
O5 S1 N1 C7 46.8(2) . . . . ?
C6 S1 N1 C7 -69.1(2) . . . . ?
O8 S1 N1 C11 -40.0(2) . . . . ?
O5 S1 N1 C11 -168.87(18) . . . . ?
C6 S1 N1 C11 75.2(2) . . . . ?
C8 C1 C4 O7 102.7(3) . . . . ?
C11 C1 C4 O7 -76.0(3) . . . . ?
C8 C1 C4 C10 -80.1(3) . . . . ?
C11 C1 C4 C10 101.3(2) . . . . ?
C22 C2 C5 C14 178.9(3) . . . . ?
C12 C2 C5 C14 0.2(4) . . . . ?
C22 C2 C5 C8 -2.6(4) . . . . ?
C12 C2 C5 C8 178.7(2) . . . . ?
C8 C3 N3 O2 -171.3(2) . . . . ?
N2 C3 N3 O2 -52.9(3) . . . . ?
C7 C3 N3 O2 64.5(3) . . . . ?
C8 C3 N3 O1 11.3(3) . . . . ?
N2 C3 N3 O1 129.8(2) . . . . ?
C7 C3 N3 O1 -112.9(2) . . . . ?
O8 S1 C6 C27 -154.7(2) . . . . ?
O5 S1 C6 C27 -22.0(3) . . . . ?
N1 S1 C6 C27 92.1(2) . . . . ?
O8 S1 C6 C29 26.6(2) . . . . ?
O5 S1 C6 C29 159.3(2) . . . . ?
N1 S1 C6 C29 -86.6(2) . . . . ?
C11 N1 C7 C3 68.4(2) . . . . ?
S1 N1 C7 C3 -145.56(17) . . . . ?
C8 C3 C7 N1 -54.1(3) . . . . ?
N2 C3 C7 N1 -178.15(19) . . . . ?
N3 C3 C7 N1 69.2(2) . . . . ?
C11 C1 C8 C5 179.2(2) . . . . ?
C4 C1 C8 C5 0.7(3) . . . . ?
C11 C1 C8 C3 -0.5(3) . . . . ?
C4 C1 C8 C3 -179.0(2) . . . . ?
C14 C5 C8 C1 94.4(3) . . . . ?
C2 C5 C8 C1 -84.1(3) . . . . ?
C14 C5 C8 C3 -85.9(3) . . . . ?
C2 C5 C8 C3 95.6(3) . . . . ?
N2 C3 C8 C1 147.3(2) . . . . ?
C7 C3 C8 C1 22.7(3) . . . . ?
N3 C3 C8 C1 -97.9(2) . . . . ?
N2 C3 C8 C5 -32.4(3) . . . . ?
C7 C3 C8 C5 -157.1(2) . . . . ?
N3 C3 C8 C5 82.4(3) . . . . ?
C15 C9 C10 C13 172.0(3) . . . . ?
C17 C9 C10 C13 -4.9(4) . . . . ?
C15 C9 C10 C4 -11.3(4) . . . . ?
C17 C9 C10 C4 171.8(2) . . . . ?
O7 C4 C10 C13 158.8(3) . . . . ?
C1 C4 C10 C13 -18.3(3) . . . . ?
O7 C4 C10 C9 -18.0(4) . . . . ?
C1 C4 C10 C9 165.0(2) . . . . ?
C7 N1 C11 C1 -47.1(3) . . . . ?
S1 N1 C11 C1 166.59(16) . . . . ?
C8 C1 C11 N1 11.5(3) . . . . ?
C4 C1 C11 N1 -169.98(19) . . . . ?
C8 C3 N2 O3 -91.8(3) . . . . ?
C7 C3 N2 O3 34.1(3) . . . . ?
N3 C3 N2 O3 148.7(2) . . . . ?
C8 C3 N2 O4 85.1(3) . . . . ?
C7 C3 N2 O4 -149.0(2) . . . . ?
N3 C3 N2 O4 -34.5(3) . . . . ?
C22 C2 C12 C32 -179.8(3) . . . . ?
C5 C2 C12 C32 -1.1(4) . . . . ?
C22 C2 C12 C30 -0.5(4) . . . . ?
C5 C2 C12 C30 178.2(3) . . . . ?
C9 C10 C13 C18 2.8(4) . . . . ?
C4 C10 C13 C18 -174.1(3) . . . . ?
C2 C5 C14 C25 0.7(5) . . . . ?
C8 C5 C14 C25 -177.8(3) . . . . ?
C17 C9 C15 C28 -2.4(4) . . . . ?
C10 C9 C15 C28 -179.3(3) . . . . ?
C15 C9 C17 C20 5.3(4) . . . . ?
C10 C9 C17 C20 -177.6(3) . . . . ?
C15 C9 C17 C23 -173.6(3) . . . . ?
C10 C9 C17 C23 3.6(4) . . . . ?
C10 C13 C18 C23 0.8(5) . . . . ?
C23 C17 C20 C21 174.9(3) . . . . ?
C9 C17 C20 C21 -4.0(5) . . . . ?
C17 C20 C21 C28 -0.4(5) . . . . ?
C31 C19 C22 C2 -0.8(5) . . . . ?
C12 C2 C22 C19 1.0(4) . . . . ?
C5 C2 C22 C19 -177.7(3) . . . . ?
C13 C18 C23 C17 -2.1(5) . . . . ?
C20 C17 C23 C18 -179.0(3) . . . . ?
C9 C17 C23 C18 -0.1(5) . . . . ?
C5 C14 C25 C32 -0.7(6) . . . . ?
C27 C16 C26 C24 -0.3(5) . . . . ?
C27 C16 C26 C33 179.4(3) . . . . ?
C29 C24 C26 C16 0.1(5) . . . . ?
C29 C24 C26 C33 -179.6(3) . . . . ?
C29 C6 C27 C16 -0.5(4) . . . . ?
S1 C6 C27 C16 -179.3(2) . . . . ?
C26 C16 C27 C6 0.5(5) . . . . ?
C9 C15 C28 C21 -1.9(5) . . . . ?
C20 C21 C28 C15 3.4(5) . . . . ?
C27 C6 C29 C24 0.3(4) . . . . ?
S1 C6 C29 C24 179.1(2) . . . . ?
C26 C24 C29 C6 -0.1(5) . . . . ?
C32 C12 C30 C31 179.2(3) . . . . ?
C2 C12 C30 C31 -0.1(5) . . . . ?
C12 C30 C31 C19 0.3(5) . . . . ?
C22 C19 C31 C30 0.2(5) . . . . ?
C14 C25 C32 C12 -0.2(6) . . . . ?
C30 C12 C32 C25 -178.2(3) . . . . ?
C2 C12 C32 C25 1.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        22.21
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.032
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_190117_yxf181225_1_0m
_database_code_depnum_ccdc_archive 'CCDC 1894190'
loop_
_audit_author_name
_audit_author_address
'Wanzhi Chen'
;Zhejiang University
China
;
_audit_update_record             
;
2019-01-28 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H20 N4 O9 S'
_chemical_formula_weight         504.47

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   16.1433(7)
_cell_length_b                   9.7950(4)
_cell_length_c                   16.3549(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.957(2)
_cell_angle_gamma                90.00
_cell_volume                     2344.62(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2674
_cell_measurement_theta_min      3.6275
_cell_measurement_theta_max      29.2265

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9505
_exptl_absorpt_correction_T_max  0.9691
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14081
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4094
_reflns_number_gt                2634
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1360P)²+1.8498P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4094
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0805
_refine_ls_wR_factor_ref         0.2554
_refine_ls_wR_factor_gt          0.2259
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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 0.51672(7) 0.89518(12) 0.81654(7) 0.0473(4) Uani 1 1 d . . .
N3 N 0.6230(2) 0.8473(4) 0.8448(2) 0.0452(9) Uani 1 1 d . . .
C18 C 0.7720(3) 0.5884(5) 0.7893(3) 0.0460(10) Uani 1 1 d . . .
C20 C 0.6345(3) 0.7158(5) 0.8055(3) 0.0470(10) Uani 1 1 d . . .
H20A H 0.5991 0.7167 0.7406 0.056 Uiso 1 1 calc R . .
H20B H 0.6130 0.6409 0.8303 0.056 Uiso 1 1 calc R . .
C22 C 0.8013(3) 0.7746(5) 0.8859(3) 0.0482(11) Uani 1 1 d . . .
O1 O 0.4713(2) 0.8811(3) 0.72109(19) 0.0565(9) Uani 1 1 d . . .
N5 N 0.7324(3) 0.6003(5) 0.6870(3) 0.0599(11) Uani 1 1 d . . .
C2 C 0.7820(3) 0.8815(5) 0.9404(3) 0.0505(11) Uani 1 1 d . . .
O2 O 0.5225(2) 1.0271(3) 0.8566(2) 0.0593(9) Uani 1 1 d . . .
C1 C 0.6874(3) 0.8646(5) 0.9387(3) 0.0487(11) Uani 1 1 d . . .
H1A H 0.6861 0.7854 0.9737 0.058 Uiso 1 1 calc R . .
H1B H 0.6717 0.9446 0.9641 0.058 Uiso 1 1 calc R . .
N1 N 0.8520(3) 0.8752(5) 1.0383(3) 0.0642(12) Uani 1 1 d . . .
C3 C 0.7335(3) 0.6972(5) 0.8276(3) 0.0460(10) Uani 1 1 d . . .
C21 C 1.0295(3) 0.6019(6) 0.8616(4) 0.0683(14) Uani 1 1 d . . .
C17 C 0.8898(3) 0.7300(5) 0.8891(3) 0.0537(12) Uani 1 1 d . . .
O8 O 0.7335(4) 0.5026(6) 0.6434(3) 0.1135(17) Uani 1 1 d . . .
C19 C 0.8725(3) 0.6217(5) 0.8284(3) 0.0504(11) Uani 1 1 d . . .
C6 C 0.9408(3) 0.5588(6) 0.8124(3) 0.0621(13) Uani 1 1 d . . .
H6 H 0.9274 0.4896 0.7699 0.074 Uiso 1 1 calc R . .
C23 C 0.9794(3) 0.7703(6) 0.9394(4) 0.0698(15) Uani 1 1 d . . .
H23 H 0.9932 0.8389 0.9824 0.084 Uiso 1 1 calc R . .
O11 O 1.1037(2) 0.5510(5) 0.8524(3) 0.0890(13) Uani 1 1 d . . .
C24 C 0.4683(3) 0.7825(5) 0.8660(3) 0.0449(10) Uani 1 1 d . . .
N4 N 0.7922(3) 1.0258(5) 0.9084(3) 0.0632(11) Uani 1 1 d . . .
O3 O 0.8496(4) 1.0405(5) 0.8811(4) 0.1076(17) Uani 1 1 d . . .
O4 O 0.7453(3) 1.1160(4) 0.9162(4) 0.0957(14) Uani 1 1 d . . .
O5 O 0.8606(3) 0.7658(5) 1.0740(3) 0.1059(16) Uani 1 1 d . . .
O7 O 0.7050(3) 0.7113(6) 0.6543(3) 0.1015(15) Uani 1 1 d . . .
C29 C 0.3897(3) 0.6033(5) 0.9453(3) 0.0545(12) Uani 1 1 d . . .
C30 C 0.3809(3) 0.5824(5) 0.8587(3) 0.0578(12) Uani 1 1 d . . .
H30 H 0.3482 0.5071 0.8266 0.069 Uiso 1 1 calc R . .
C28 C 0.4398(3) 0.7161(5) 0.9929(3) 0.0591(13) Uani 1 1 d . . .
H28 H 0.4468 0.7316 1.0515 0.071 Uiso 1 1 calc R . .
C31 C 0.4191(3) 0.6696(5) 0.8185(3) 0.0538(12) Uani 1 1 d . . .
H31 H 0.4122 0.6534 0.7599 0.065 Uiso 1 1 calc R . .
O6 O 0.8919(3) 0.9748(5) 1.0737(3) 0.1075(17) Uani 1 1 d . . .
C27 C 0.4788(3) 0.8039(5) 0.9545(3) 0.0539(12) Uani 1 1 d . . .
H27 H 0.5125 0.8781 0.9872 0.065 Uiso 1 1 calc R . .
C33 C 0.3471(4) 0.5071(7) 0.9883(4) 0.0799(17) Uani 1 1 d . . .
H33A H 0.2993 0.5534 0.9975 0.120 Uiso 1 1 calc R . .
H33B H 0.3927 0.4766 1.0453 0.120 Uiso 1 1 calc R . .
H33C H 0.3220 0.4298 0.9496 0.120 Uiso 1 1 calc R . .
C34 C 1.0479(3) 0.7060(7) 0.9240(4) 0.0755(16) Uani 1 1 d . . .
H34 H 1.1081 0.7336 0.9566 0.091 Uiso 1 1 calc R . .
C35 C 1.0875(4) 0.4615(8) 0.7784(4) 0.089(2) Uani 1 1 d . . .
H35A H 1.0565 0.3812 0.7844 0.134 Uiso 1 1 calc R . .
H35B H 1.1448 0.4361 0.7780 0.134 Uiso 1 1 calc R . .
H35C H 1.0505 0.5071 0.7230 0.134 Uiso 1 1 calc R . .
C36 C 0.7548(3) 0.4439(5) 0.8146(4) 0.0645(13) Uani 1 1 d . . .
H36A H 0.7804 0.3784 0.7881 0.097 Uiso 1 1 calc R . .
H36B H 0.6903 0.4288 0.7926 0.097 Uiso 1 1 calc R . .
H36C H 0.7831 0.4341 0.8790 0.097 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 1.424(3) . ?
S1 O2 1.435(3) . ?
S1 N3 1.645(4) . ?
S1 C24 1.737(4) . ?
N3 C1 1.456(5) . ?
N3 C20 1.486(6) . ?
C18 C3 1.498(6) . ?
C18 C19 1.506(6) . ?
C18 N5 1.522(6) . ?
C18 C36 1.533(6) . ?
C20 C3 1.493(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C22 C3 1.342(6) . ?
C22 C17 1.474(6) . ?
C22 C2 1.491(6) . ?
N5 O8 1.198(6) . ?
N5 O7 1.210(6) . ?
C2 N1 1.523(6) . ?
C2 C1 1.524(6) . ?
C2 N4 1.541(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 O6 1.178(6) . ?
N1 O5 1.199(6) . ?
C21 O11 1.362(6) . ?
C21 C6 1.380(7) . ?
C21 C34 1.384(8) . ?
C17 C23 1.386(6) . ?
C17 C19 1.398(6) . ?
C19 C6 1.381(6) . ?
C6 H6 0.9300 . ?
C23 C34 1.385(7) . ?
C23 H23 0.9300 . ?
O11 C35 1.426(7) . ?
C24 C31 1.392(6) . ?
C24 C27 1.399(6) . ?
N4 O3 1.194(6) . ?
N4 O4 1.204(6) . ?
C29 C30 1.378(6) . ?
C29 C28 1.396(7) . ?
C29 C33 1.505(7) . ?
C30 C31 1.373(6) . ?
C30 H30 0.9300 . ?
C28 C27 1.366(6) . ?
C28 H28 0.9300 . ?
C31 H31 0.9300 . ?
C27 H27 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 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 O2 119.5(2) . . ?
O1 S1 N3 105.89(17) . . ?
O2 S1 N3 105.6(2) . . ?
O1 S1 C24 109.0(2) . . ?
O2 S1 C24 108.3(2) . . ?
N3 S1 C24 107.97(19) . . ?
C1 N3 C20 113.2(3) . . ?
C1 N3 S1 117.3(3) . . ?
C20 N3 S1 115.6(3) . . ?
C3 C18 C19 103.4(3) . . ?
C3 C18 N5 110.4(4) . . ?
C19 C18 N5 109.2(3) . . ?
C3 C18 C36 112.9(4) . . ?
C19 C18 C36 111.7(4) . . ?
N5 C18 C36 109.1(4) . . ?
N3 C20 C3 108.5(3) . . ?
N3 C20 H20A 110.0 . . ?
C3 C20 H20A 110.0 . . ?
N3 C20 H20B 110.0 . . ?
C3 C20 H20B 110.0 . . ?
H20A C20 H20B 108.4 . . ?
C3 C22 C17 110.2(4) . . ?
C3 C22 C2 120.5(4) . . ?
C17 C22 C2 129.1(4) . . ?
O8 N5 O7 123.4(5) . . ?
O8 N5 C18 119.2(5) . . ?
O7 N5 C18 117.4(4) . . ?
C22 C2 N1 110.5(4) . . ?
C22 C2 C1 111.9(4) . . ?
N1 C2 C1 108.0(3) . . ?
C22 C2 N4 111.2(4) . . ?
N1 C2 N4 104.8(4) . . ?
C1 C2 N4 110.1(4) . . ?
N3 C1 C2 107.3(3) . . ?
N3 C1 H1A 110.3 . . ?
C2 C1 H1A 110.3 . . ?
N3 C1 H1B 110.3 . . ?
C2 C1 H1B 110.3 . . ?
H1A C1 H1B 108.5 . . ?
O6 N1 O5 125.0(5) . . ?
O6 N1 C2 119.5(5) . . ?
O5 N1 C2 115.5(4) . . ?
C22 C3 C20 124.9(4) . . ?
C22 C3 C18 109.9(4) . . ?
C20 C3 C18 125.2(4) . . ?
O11 C21 C6 124.7(5) . . ?
O11 C21 C34 115.3(5) . . ?
C6 C21 C34 120.0(5) . . ?
C23 C17 C19 118.9(4) . . ?
C23 C17 C22 133.7(5) . . ?
C19 C17 C22 107.4(4) . . ?
C6 C19 C17 122.4(4) . . ?
C6 C19 C18 128.7(4) . . ?
C17 C19 C18 108.8(4) . . ?
C21 C6 C19 118.0(5) . . ?
C21 C6 H6 121.0 . . ?
C19 C6 H6 121.0 . . ?
C34 C23 C17 118.4(5) . . ?
C34 C23 H23 120.8 . . ?
C17 C23 H23 120.8 . . ?
C21 O11 C35 117.6(4) . . ?
C31 C24 C27 119.2(4) . . ?
C31 C24 S1 120.5(3) . . ?
C27 C24 S1 120.3(3) . . ?
O3 N4 O4 124.9(5) . . ?
O3 N4 C2 116.7(5) . . ?
O4 N4 C2 118.3(4) . . ?
C30 C29 C28 118.3(4) . . ?
C30 C29 C33 121.2(5) . . ?
C28 C29 C33 120.4(4) . . ?
C31 C30 C29 121.9(5) . . ?
C31 C30 H30 119.1 . . ?
C29 C30 H30 119.1 . . ?
C27 C28 C29 120.9(4) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
C30 C31 C24 119.5(4) . . ?
C30 C31 H31 120.2 . . ?
C24 C31 H31 120.2 . . ?
C28 C27 C24 120.2(4) . . ?
C28 C27 H27 119.9 . . ?
C24 C27 H27 119.9 . . ?
C29 C33 H33A 109.5 . . ?
C29 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C29 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C21 C34 C23 122.1(5) . . ?
C21 C34 H34 119.0 . . ?
C23 C34 H34 119.0 . . ?
O11 C35 H35A 109.5 . . ?
O11 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O11 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C18 C36 H36A 109.5 . . ?
C18 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C18 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 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
O1 S1 N3 C1 174.0(3) . . . . ?
O2 S1 N3 C1 46.3(4) . . . . ?
C24 S1 N3 C1 -69.4(4) . . . . ?
O1 S1 N3 C20 -48.4(3) . . . . ?
O2 S1 N3 C20 -176.1(3) . . . . ?
C24 S1 N3 C20 68.2(3) . . . . ?
C1 N3 C20 C3 -48.2(4) . . . . ?
S1 N3 C20 C3 172.5(3) . . . . ?
C3 C18 N5 O8 -158.3(5) . . . . ?
C19 C18 N5 O8 88.7(6) . . . . ?
C36 C18 N5 O8 -33.7(6) . . . . ?
C3 C18 N5 O7 25.1(6) . . . . ?
C19 C18 N5 O7 -87.9(5) . . . . ?
C36 C18 N5 O7 149.7(5) . . . . ?
C3 C22 C2 N1 134.7(4) . . . . ?
C17 C22 C2 N1 -41.0(6) . . . . ?
C3 C22 C2 C1 14.3(6) . . . . ?
C17 C22 C2 C1 -161.3(4) . . . . ?
C3 C22 C2 N4 -109.3(5) . . . . ?
C17 C22 C2 N4 75.1(6) . . . . ?
C20 N3 C1 C2 68.5(4) . . . . ?
S1 N3 C1 C2 -153.0(3) . . . . ?
C22 C2 C1 N3 -48.6(5) . . . . ?
N1 C2 C1 N3 -170.4(4) . . . . ?
N4 C2 C1 N3 75.7(4) . . . . ?
C22 C2 N1 O6 127.3(5) . . . . ?
C1 C2 N1 O6 -109.9(5) . . . . ?
N4 C2 N1 O6 7.4(6) . . . . ?
C22 C2 N1 O5 -53.9(6) . . . . ?
C1 C2 N1 O5 68.8(6) . . . . ?
N4 C2 N1 O5 -173.9(5) . . . . ?
C17 C22 C3 C20 -178.3(4) . . . . ?
C2 C22 C3 C20 5.3(7) . . . . ?
C17 C22 C3 C18 2.6(5) . . . . ?
C2 C22 C3 C18 -173.8(4) . . . . ?
N3 C20 C3 C22 10.5(6) . . . . ?
N3 C20 C3 C18 -170.6(4) . . . . ?
C19 C18 C3 C22 -4.6(5) . . . . ?
N5 C18 C3 C22 -121.3(4) . . . . ?
C36 C18 C3 C22 116.3(4) . . . . ?
C19 C18 C3 C20 176.3(4) . . . . ?
N5 C18 C3 C20 59.6(5) . . . . ?
C36 C18 C3 C20 -62.9(5) . . . . ?
C3 C22 C17 C23 -177.0(6) . . . . ?
C2 C22 C17 C23 -0.9(9) . . . . ?
C3 C22 C17 C19 0.7(5) . . . . ?
C2 C22 C17 C19 176.8(4) . . . . ?
C23 C17 C19 C6 -4.2(7) . . . . ?
C22 C17 C19 C6 177.7(4) . . . . ?
C23 C17 C19 C18 174.4(5) . . . . ?
C22 C17 C19 C18 -3.7(5) . . . . ?
C3 C18 C19 C6 -176.5(5) . . . . ?
N5 C18 C19 C6 -58.9(6) . . . . ?
C36 C18 C19 C6 61.9(6) . . . . ?
C3 C18 C19 C17 5.0(5) . . . . ?
N5 C18 C19 C17 122.5(4) . . . . ?
C36 C18 C19 C17 -116.6(4) . . . . ?
O11 C21 C6 C19 -179.1(5) . . . . ?
C34 C21 C6 C19 -0.6(8) . . . . ?
C17 C19 C6 C21 2.8(7) . . . . ?
C18 C19 C6 C21 -175.5(5) . . . . ?
C19 C17 C23 C34 3.3(8) . . . . ?
C22 C17 C23 C34 -179.2(5) . . . . ?
C6 C21 O11 C35 9.5(9) . . . . ?
C34 C21 O11 C35 -169.0(6) . . . . ?
O1 S1 C24 C31 20.7(4) . . . . ?
O2 S1 C24 C31 152.2(4) . . . . ?
N3 S1 C24 C31 -93.9(4) . . . . ?
O1 S1 C24 C27 -159.7(4) . . . . ?
O2 S1 C24 C27 -28.2(4) . . . . ?
N3 S1 C24 C27 85.7(4) . . . . ?
C22 C2 N4 O3 -33.9(6) . . . . ?
N1 C2 N4 O3 85.6(5) . . . . ?
C1 C2 N4 O3 -158.5(4) . . . . ?
C22 C2 N4 O4 149.4(4) . . . . ?
N1 C2 N4 O4 -91.2(5) . . . . ?
C1 C2 N4 O4 24.7(6) . . . . ?
C28 C29 C30 C31 -0.6(8) . . . . ?
C33 C29 C30 C31 179.7(5) . . . . ?
C30 C29 C28 C27 0.3(8) . . . . ?
C33 C29 C28 C27 179.9(5) . . . . ?
C29 C30 C31 C24 0.1(8) . . . . ?
C27 C24 C31 C30 0.8(7) . . . . ?
S1 C24 C31 C30 -179.6(4) . . . . ?
C29 C28 C27 C24 0.6(7) . . . . ?
C31 C24 C27 C28 -1.1(7) . . . . ?
S1 C24 C27 C28 179.2(4) . . . . ?
O11 C21 C34 C23 178.5(5) . . . . ?
C6 C21 C34 C23 -0.1(9) . . . . ?
C17 C23 C34 C21 -1.2(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.083
