# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1442458'
_audit_update_record             
;
2015-12-26 deposited with the CCDC.
2016-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H14 N O4 S6'
_chemical_formula_weight         476.64

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                   8.837(3)
_cell_length_b                   9.956(2)
_cell_length_c                   12.431(4)
_cell_angle_alpha                67.08(2)
_cell_angle_beta                 85.63(3)
_cell_angle_gamma                73.08(2)
_cell_volume                     962.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4744
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            dark-green
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             490
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7578
_exptl_absorpt_correction_T_max  0.8671
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9011
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4290
_reflns_number_gt                3032
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of 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)+(0.0633P)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     SHELXL
_refine_ls_extinction_coef       0.130(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4290
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.31115(10) 0.62869(9) 0.39455(7) 0.0290(2) Uani 1 1 d . . .
S2 S 0.37744(9) 0.30789(9) 0.42523(7) 0.0278(2) Uani 1 1 d . . .
S3 S 0.09194(9) 0.55346(9) 0.63124(6) 0.0254(2) Uani 1 1 d . . .
S4 S 0.15705(10) 0.24350(9) 0.64027(7) 0.0300(2) Uani 1 1 d . . .
S5 S 0.00049(10) 0.47300(10) 0.87947(7) 0.0302(2) Uani 1 1 d . . .
S6 S 0.07070(10) 0.11551(10) 0.89116(7) 0.0337(2) Uani 1 1 d . . .
O1 O 0.4567(3) 0.8160(3) 0.2185(2) 0.0523(7) Uani 1 1 d . . .
O2 O 0.5886(3) 0.6656(3) 0.1308(2) 0.0466(7) Uani 1 1 d . . .
O3 O 0.6595(3) 0.3967(3) 0.1684(2) 0.0463(7) Uani 1 1 d . . .
O4 O 0.5894(3) 0.1937(3) 0.2885(2) 0.0355(6) Uani 1 1 d . . .
N11 N 0.2126(3) 0.1037(3) 0.2434(2) 0.0292(6) Uani 1 1 d . . .
C1 C 0.4493(3) 0.5642(4) 0.3040(3) 0.0255(7) Uani 1 1 d . . .
C2 C 0.4794(3) 0.4180(4) 0.3176(3) 0.0244(7) Uani 1 1 d . . .
C3 C 0.2817(3) 0.4515(3) 0.4764(2) 0.0217(6) Uani 1 1 d . . .
C4 C 0.1921(3) 0.4212(3) 0.5699(3) 0.0230(6) Uani 1 1 d . . .
C5 C 0.0641(3) 0.4137(3) 0.7651(2) 0.0223(6) Uani 1 1 d . . .
C6 C 0.0975(4) 0.2701(4) 0.7708(3) 0.0257(7) Uani 1 1 d . . .
C7 C -0.1918(4) 0.4421(5) 0.9054(3) 0.0414(9) Uani 1 1 d . . .
H7A H -0.2658 0.5186 0.8427 0.062 Uiso 1 1 calc R . .
H7B H -0.2278 0.4491 0.9792 0.062 Uiso 1 1 calc R . .
H7C H -0.1855 0.3418 0.9083 0.062 Uiso 1 1 calc R . .
C8 C 0.2667(4) -0.0174(4) 0.9145(3) 0.0415(9) Uani 1 1 d . . .
H8A H 0.2829 -0.0634 0.8571 0.062 Uiso 1 1 calc R . .
H8B H 0.2769 -0.0961 0.9924 0.062 Uiso 1 1 calc R . .
H8C H 0.3454 0.0361 0.9065 0.062 Uiso 1 1 calc R . .
C9 C 0.5020(4) 0.6911(4) 0.2128(3) 0.0356(8) Uani 1 1 d . . .
C10 C 0.5843(4) 0.3298(4) 0.2521(3) 0.0299(8) Uani 1 1 d . . .
C11 C 0.0556(4) 0.1243(4) 0.2369(3) 0.0314(8) Uani 1 1 d . . .
H11 H 0.0028 0.1686 0.1631 0.038 Uiso 1 1 calc R . .
C12 C -0.0285(4) 0.0824(4) 0.3350(3) 0.0313(7) Uani 1 1 d . . .
H12 H -0.1375 0.0960 0.3277 0.038 Uiso 1 1 calc R . .
C13 C 0.0450(3) 0.0197(3) 0.4461(3) 0.0237(7) Uani 1 1 d . . .
C14 C 0.2086(4) -0.0034(4) 0.4500(3) 0.0337(8) Uani 1 1 d . . .
H14 H 0.2642 -0.0477 0.5227 0.040 Uiso 1 1 calc R . .
C15 C 0.2887(4) 0.0376(4) 0.3495(3) 0.0323(8) Uani 1 1 d . . .
H15 H 0.3990 0.0195 0.3542 0.039 Uiso 1 1 calc R . .
C16 C 0.2998(4) 0.1532(4) 0.1368(3) 0.0391(9) Uani 1 1 d . . .
H16A H 0.3522 0.0665 0.1166 0.059 Uiso 1 1 calc R . .
H16B H 0.3782 0.1966 0.1500 0.059 Uiso 1 1 calc R . .
H16C H 0.2266 0.2291 0.0733 0.059 Uiso 1 1 calc R . .
H1 H 0.631(5) 0.548(5) 0.151(4) 0.060(13) Uiso 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 C3 1.745(3) . ?
S1 C1 1.751(3) . ?
S2 C2 1.747(3) . ?
S2 C3 1.757(3) . ?
S3 C5 1.760(3) . ?
S3 C4 1.760(3) . ?
S4 C4 1.751(3) . ?
S4 C6 1.762(3) . ?
S5 C5 1.739(3) . ?
S5 C7 1.797(4) . ?
S6 C6 1.740(3) . ?
S6 C8 1.811(4) . ?
O1 C9 1.219(4) . ?
O2 C9 1.288(4) . ?
O2 H1 1.05(5) . ?
O3 C10 1.257(4) . ?
O3 H1 1.38(5) . ?
O4 C10 1.238(4) . ?
N11 C11 1.346(4) . ?
N11 C15 1.351(4) . ?
N11 C16 1.467(5) . ?
C1 C2 1.344(4) . ?
C1 C9 1.499(5) . ?
C2 C10 1.504(4) . ?
C3 C4 1.339(4) . ?
C5 C6 1.347(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C11 C12 1.364(5) . ?
C11 H11 0.9400 . ?
C12 C13 1.395(4) . ?
C12 H12 0.9400 . ?
C13 C14 1.398(4) . ?
C13 C13 1.481(6) 2_556 ?
C14 C15 1.366(5) . ?
C14 H14 0.9400 . ?
C15 H15 0.9400 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 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
C3 S1 C1 95.11(15) . . ?
C2 S2 C3 95.32(15) . . ?
C5 S3 C4 94.29(14) . . ?
C4 S4 C6 94.83(14) . . ?
C5 S5 C7 102.86(15) . . ?
C6 S6 C8 101.41(17) . . ?
C9 O2 H1 110(2) . . ?
C10 O3 H1 111.6(17) . . ?
C11 N11 C15 119.2(3) . . ?
C11 N11 C16 120.4(3) . . ?
C15 N11 C16 120.4(3) . . ?
C2 C1 C9 130.0(3) . . ?
C2 C1 S1 117.6(2) . . ?
C9 C1 S1 111.9(2) . . ?
C1 C2 C10 131.0(3) . . ?
C1 C2 S2 116.9(2) . . ?
C10 C2 S2 112.1(2) . . ?
C4 C3 S1 125.2(2) . . ?
C4 C3 S2 120.2(2) . . ?
S1 C3 S2 114.62(17) . . ?
C3 C4 S4 122.1(2) . . ?
C3 C4 S3 124.8(2) . . ?
S4 C4 S3 113.02(17) . . ?
C6 C5 S5 125.8(2) . . ?
C6 C5 S3 117.3(2) . . ?
S5 C5 S3 116.83(18) . . ?
C5 C6 S6 125.5(2) . . ?
C5 C6 S4 116.0(2) . . ?
S6 C6 S4 118.33(18) . . ?
S5 C7 H7A 109.5 . . ?
S5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
S5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
S6 C8 H8A 109.5 . . ?
S6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
S6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C9 O2 122.9(3) . . ?
O1 C9 C1 117.7(3) . . ?
O2 C9 C1 119.4(3) . . ?
O4 C10 O3 125.8(3) . . ?
O4 C10 C2 115.1(3) . . ?
O3 C10 C2 119.1(3) . . ?
N11 C11 C12 121.4(3) . . ?
N11 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 116.2(3) . . ?
C12 C13 C13 122.0(3) . 2_556 ?
C14 C13 C13 121.8(3) . 2_556 ?
C15 C14 C13 120.8(3) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
N11 C15 C14 121.3(3) . . ?
N11 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
N11 C16 H16A 109.5 . . ?
N11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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
C3 S1 C1 C2 4.1(3) . . . . ?
C3 S1 C1 C9 177.6(2) . . . . ?
C9 C1 C2 C10 5.0(5) . . . . ?
S1 C1 C2 C10 177.2(2) . . . . ?
C9 C1 C2 S2 -172.5(2) . . . . ?
S1 C1 C2 S2 -0.4(3) . . . . ?
C3 S2 C2 C1 -3.5(3) . . . . ?
C3 S2 C2 C10 178.5(2) . . . . ?
C1 S1 C3 C4 175.1(3) . . . . ?
C1 S1 C3 S2 -6.29(19) . . . . ?
C2 S2 C3 C4 -175.2(2) . . . . ?
C2 S2 C3 S1 6.17(18) . . . . ?
S1 C3 C4 S4 175.01(16) . . . . ?
S2 C3 C4 S4 -3.5(4) . . . . ?
S1 C3 C4 S3 -2.3(4) . . . . ?
S2 C3 C4 S3 179.21(16) . . . . ?
C6 S4 C4 C3 161.4(3) . . . . ?
C6 S4 C4 S3 -21.05(19) . . . . ?
C5 S3 C4 C3 -162.6(3) . . . . ?
C5 S3 C4 S4 19.88(18) . . . . ?
C7 S5 C5 C6 -66.3(3) . . . . ?
C7 S5 C5 S3 115.4(2) . . . . ?
C4 S3 C5 C6 -10.6(3) . . . . ?
C4 S3 C5 S5 167.88(18) . . . . ?
S5 C5 C6 S6 4.8(4) . . . . ?
S3 C5 C6 S6 -176.94(17) . . . . ?
S5 C5 C6 S4 179.15(16) . . . . ?
S3 C5 C6 S4 -2.6(4) . . . . ?
C8 S6 C6 C5 -125.3(3) . . . . ?
C8 S6 C6 S4 60.4(2) . . . . ?
C4 S4 C6 C5 14.3(3) . . . . ?
C4 S4 C6 S6 -170.86(19) . . . . ?
C2 C1 C9 O1 179.1(3) . . . . ?
S1 C1 C9 O1 6.5(4) . . . . ?
C2 C1 C9 O2 0.9(5) . . . . ?
S1 C1 C9 O2 -171.7(3) . . . . ?
C1 C2 C10 O4 178.2(3) . . . . ?
S2 C2 C10 O4 -4.2(3) . . . . ?
C1 C2 C10 O3 -0.8(5) . . . . ?
S2 C2 C10 O3 176.8(2) . . . . ?
C15 N11 C11 C12 1.2(5) . . . . ?
C16 N11 C11 C12 -178.5(3) . . . . ?
N11 C11 C12 C13 1.5(5) . . . . ?
C11 C12 C13 C14 -2.8(4) . . . . ?
C11 C12 C13 C13 177.0(3) . . . 2_556 ?
C12 C13 C14 C15 1.6(5) . . . . ?
C13 C13 C14 C15 -178.2(3) 2_556 . . . ?
C11 N11 C15 C14 -2.4(5) . . . . ?
C16 N11 C15 C14 177.2(3) . . . . ?
C13 C14 C15 N11 1.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.210
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1442459'
_audit_update_record             
;
2016-02-05 deposited with the CCDC.
2016-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H40 N2 O11 S12'
_chemical_formula_weight         1061.49
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5145(19)
_cell_length_b                   9.960(2)
_cell_length_c                   13.139(3)
_cell_angle_alpha                107.14(3)
_cell_angle_beta                 106.56(3)
_cell_angle_gamma                94.37(3)
_cell_volume                     1122.8(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5630
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chip
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_F_000             560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.646
_shelx_estimated_absorpt_T_min   0.626
_shelx_estimated_absorpt_T_max   0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7022
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            10281
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.092
_diffrn_reflns_theta_max         27.439
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4971
_reflns_number_gt                3637
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
'One restraint dfix is used to fix the hydrogen atom of the carboxylate group'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0430P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.155(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4971
_refine_ls_number_parameters     290
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.1109
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.072
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.15529(7) 0.72847(6) 0.29815(5) 0.02543(18) Uani 1 1 d . . . . .
S2 S -0.15447(7) 0.57963(6) 0.23302(5) 0.02648(19) Uani 1 1 d . . . . .
S3 S 0.26722(8) 0.49010(7) 0.42741(6) 0.02820(19) Uani 1 1 d . . . . .
S4 S -0.04978(8) 0.35199(7) 0.34447(6) 0.0304(2) Uani 1 1 d . . . . .
S5 S 0.35933(8) 0.30698(7) 0.57608(5) 0.0311(2) Uani 1 1 d . . . . .
S6 S 0.01451(8) 0.14197(7) 0.47035(6) 0.0309(2) Uani 1 1 d . . . . .
O1 O 0.2052(2) 0.9724(2) 0.24315(17) 0.0400(5) Uani 1 1 d . . . . .
O2 O -0.0232(2) 0.9987(2) 0.15815(17) 0.0406(5) Uani 1 1 d D . . . .
O3 O -0.2762(2) 0.8789(2) 0.11017(17) 0.0397(5) Uani 1 1 d . . . . .
O4 O -0.3917(2) 0.6944(2) 0.13339(16) 0.0363(5) Uani 1 1 d . . . . .
O5 O -0.6508(3) 0.7320(2) -0.01268(19) 0.0544(7) Uani 1 1 d . . . . .
H5 H -0.5755 0.7321 0.0370 0.082 Uiso 1 1 calc R U . . .
O6 O 0.4946(5) -0.0724(5) 0.2853(4) 0.0611(13) Uani 0.5 1 d . . P . .
N1 N -1.3959(2) 0.6861(2) -0.17831(16) 0.0261(5) Uani 1 1 d . . . . .
C1 C 0.0112(3) 0.8045(2) 0.23163(19) 0.0229(6) Uani 1 1 d . . . . .
C2 C -0.1307(3) 0.7371(2) 0.20354(19) 0.0233(6) Uani 1 1 d . . . . .
C3 C 0.0355(3) 0.5887(2) 0.3025(2) 0.0225(5) Uani 1 1 d . . . . .
C4 C 0.0817(3) 0.4925(2) 0.3530(2) 0.0236(6) Uani 1 1 d . . . . .
C5 C 0.2206(3) 0.3517(2) 0.4778(2) 0.0249(6) Uani 1 1 d . . . . .
C6 C 0.0764(3) 0.2873(2) 0.4370(2) 0.0229(6) Uani 1 1 d . . . . .
C7 C 0.4397(3) 0.1854(3) 0.4884(3) 0.0448(8) Uani 1 1 d . . . . .
H7A H 0.3633 0.1087 0.4340 0.067 Uiso 1 1 calc R U . . .
H7B H 0.5133 0.1477 0.5339 0.067 Uiso 1 1 calc R U . . .
H7C H 0.4858 0.2347 0.4502 0.067 Uiso 1 1 calc R U . . .
C8 C -0.1842(3) 0.1093(3) 0.4016(2) 0.0339(7) Uani 1 1 d . . . . .
H8A H -0.2242 0.1924 0.4311 0.051 Uiso 1 1 calc R U . . .
H8B H -0.2295 0.0295 0.4151 0.051 Uiso 1 1 calc R U . . .
H8C H -0.2048 0.0886 0.3221 0.051 Uiso 1 1 calc R U . . .
C9 C 0.0697(3) 0.9345(3) 0.2102(2) 0.0288(6) Uani 1 1 d . . . . .
C10 C -0.2771(3) 0.7731(3) 0.1449(2) 0.0269(6) Uani 1 1 d . . . . .
C11 C -1.2609(3) 0.7561(3) -0.1634(2) 0.0298(6) Uani 1 1 d . . . . .
H11 H -1.2544 0.8336 -0.1887 0.036 Uiso 1 1 calc R U . . .
C12 C -1.1334(3) 0.7151(3) -0.1119(2) 0.0283(6) Uani 1 1 d . . . . .
H12 H -1.0413 0.7655 -0.1019 0.034 Uiso 1 1 calc R U . . .
C13 C -1.1401(3) 0.5984(2) -0.07419(19) 0.0236(6) Uani 1 1 d . . . . .
C14 C -1.2818(3) 0.5270(3) -0.0920(2) 0.0275(6) Uani 1 1 d . . . . .
H14 H -1.2914 0.4479 -0.0691 0.033 Uiso 1 1 calc R U . . .
C15 C -1.4069(3) 0.5726(3) -0.1432(2) 0.0275(6) Uani 1 1 d . . . . .
H15 H -1.5004 0.5247 -0.1537 0.033 Uiso 1 1 calc R U . . .
C16 C -1.5333(3) 0.7296(3) -0.2349(3) 0.0406(7) Uani 1 1 d . . . . .
H16A H -1.5092 0.8212 -0.2418 0.061 Uiso 1 1 calc R U . . .
H16B H -1.5997 0.7354 -0.1913 0.061 Uiso 1 1 calc R U . . .
H16C H -1.5806 0.6605 -0.3083 0.061 Uiso 1 1 calc R U . . .
C17 C -1.0033(3) 0.5550(2) -0.0191(2) 0.0248(6) Uani 1 1 d . . . . .
H17 H -0.9134 0.6087 -0.0099 0.030 Uiso 1 1 calc R U . . .
C18 C -0.6782(5) 0.8693(4) 0.0041(4) 0.0751(13) Uani 1 1 d . . . . .
H18A H -0.6960 0.9049 0.0748 0.113 Uiso 1 1 calc R U . . .
H18B H -0.7642 0.8698 -0.0556 0.113 Uiso 1 1 calc R U . . .
H18C H -0.5935 0.9290 0.0049 0.113 Uiso 1 1 calc R U . . .
H1 H -0.132(4) 0.951(4) 0.141(3) 0.080(13) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.755(3) . ?
S1 C3 1.756(3) . ?
S2 C2 1.736(2) . ?
S2 C3 1.759(3) . ?
S3 C4 1.763(3) . ?
S3 C5 1.774(2) . ?
S4 C6 1.755(2) . ?
S4 C4 1.759(3) . ?
S5 C5 1.751(3) . ?
S5 C7 1.789(3) . ?
S6 C6 1.739(2) . ?
S6 C8 1.805(3) . ?
O1 C9 1.225(3) . ?
O2 C9 1.288(3) . ?
O3 C10 1.266(3) . ?
O4 C10 1.238(3) . ?
O5 C18 1.377(4) . ?
N1 C11 1.346(3) . ?
N1 C15 1.349(3) . ?
N1 C16 1.474(3) . ?
C1 C2 1.357(4) . ?
C1 C9 1.503(3) . ?
C2 C10 1.513(4) . ?
C3 C4 1.351(3) . ?
C5 C6 1.351(4) . ?
C11 C12 1.366(4) . ?
C12 C13 1.396(3) . ?
C13 C14 1.398(4) . ?
C13 C17 1.463(3) . ?
C14 C15 1.371(4) . ?
C17 C17 1.331(5) 2_365 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C3 94.72(12) . . ?
C2 S2 C3 95.48(12) . . ?
C4 S3 C5 95.02(12) . . ?
C6 S4 C4 95.25(12) . . ?
C5 S5 C7 102.34(13) . . ?
C6 S6 C8 103.01(12) . . ?
C11 N1 C15 120.0(2) . . ?
C11 N1 C16 121.1(2) . . ?
C15 N1 C16 118.9(2) . . ?
C2 C1 C9 130.3(2) . . ?
C2 C1 S1 117.56(18) . . ?
C9 C1 S1 112.05(19) . . ?
C1 C2 C10 130.5(2) . . ?
C1 C2 S2 117.1(2) . . ?
C10 C2 S2 112.37(19) . . ?
C4 C3 S1 124.1(2) . . ?
C4 C3 S2 121.1(2) . . ?
S1 C3 S2 114.78(13) . . ?
C3 C4 S4 119.4(2) . . ?
C3 C4 S3 126.0(2) . . ?
S4 C4 S3 114.59(13) . . ?
C6 C5 S5 123.93(19) . . ?
C6 C5 S3 116.51(19) . . ?
S5 C5 S3 119.55(15) . . ?
C5 C6 S6 122.30(19) . . ?
C5 C6 S4 117.86(19) . . ?
S6 C6 S4 119.83(15) . . ?
O1 C9 O2 123.7(2) . . ?
O1 C9 C1 117.2(2) . . ?
O2 C9 C1 119.1(2) . . ?
O4 C10 O3 124.1(2) . . ?
O4 C10 C2 116.6(2) . . ?
O3 C10 C2 119.3(2) . . ?
N1 C11 C12 121.1(2) . . ?
C11 C12 C13 120.6(3) . . ?
C12 C13 C14 116.9(2) . . ?
C12 C13 C17 120.4(2) . . ?
C14 C13 C17 122.7(2) . . ?
C15 C14 C13 120.6(2) . . ?
N1 C15 C14 120.8(2) . . ?
C17 C17 C13 125.4(3) 2_365 . ?

_refine_diff_density_max         0.435
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.118

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1442460'
_audit_update_record             
;
2016-02-05 deposited with the CCDC.
2016-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H16 N O4 S6'
_chemical_formula_weight         490.67

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5801(15)
_cell_length_b                   11.601(2)
_cell_length_c                   12.317(3)
_cell_angle_alpha                89.25(3)
_cell_angle_beta                 74.54(3)
_cell_angle_gamma                88.44(3)
_cell_volume                     1043.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3688
_cell_measurement_theta_min      3.3143
_cell_measurement_theta_max      27.4932

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_F_000             506
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.680
_shelx_estimated_absorpt_T_min   0.686
_shelx_estimated_absorpt_T_max   0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8336
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9979
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.314
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4685
_reflns_number_gt                3461
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
'one restraint dfix is used to fix the hydrogen atom of the carboxylate group'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0508P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4685
_refine_ls_number_parameters     260
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1025
_refine_ls_wR_factor_gt          0.0926
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.19301(7) 0.56117(5) 0.74375(5) 0.04345(17) Uani 1 1 d . . . . .
S2 S 0.53142(8) 0.69490(5) 0.69203(5) 0.04426(17) Uani 1 1 d . . . . .
S3 S 0.41466(7) 0.34039(5) 0.62124(5) 0.03915(16) Uani 1 1 d . . . . .
S4 S 0.76243(7) 0.46359(5) 0.57121(5) 0.04044(16) Uani 1 1 d . . . . .
S5 S 0.60629(9) 0.10565(5) 0.59216(6) 0.05479(19) Uani 1 1 d . . . . .
S6 S 0.99332(8) 0.24553(6) 0.53614(6) 0.05114(18) Uani 1 1 d . . . . .
O1 O -0.1116(2) 0.63802(17) 0.90862(18) 0.0766(7) Uani 1 1 d . . . . .
O2 O -0.0244(3) 0.80515(16) 0.95677(15) 0.0607(5) Uani 1 1 d D . . . .
O3 O 0.2500(3) 0.91769(14) 0.90999(15) 0.0608(5) Uani 1 1 d . . . . .
O4 O 0.5390(3) 0.89825(15) 0.80675(18) 0.0674(6) Uani 1 1 d . . . . .
N1 N 0.7814(2) 0.16497(15) 0.84611(15) 0.0375(4) Uani 1 1 d . . . . .
C1 C 0.1890(3) 0.68779(18) 0.82076(18) 0.0368(5) Uani 1 1 d . . . . .
C2 C 0.3432(3) 0.74878(18) 0.79648(18) 0.0363(5) Uani 1 1 d . . . . .
C3 C 0.4297(3) 0.56314(18) 0.68109(17) 0.0345(5) Uani 1 1 d . . . . .
C4 C 0.5249(3) 0.46916(18) 0.63190(17) 0.0344(5) Uani 1 1 d . . . . .
C5 C 0.6165(3) 0.25519(19) 0.59480(18) 0.0363(5) Uani 1 1 d . . . . .
C6 C 0.7755(3) 0.31165(19) 0.57072(18) 0.0381(5) Uani 1 1 d . . . . .
C7 C 0.3696(3) 0.0792(2) 0.6539(2) 0.0578(7) Uani 1 1 d . . . . .
H7A H 0.3361 0.1040 0.7309 0.087 Uiso 1 1 calc R U . . .
H7B H 0.3485 -0.0018 0.6510 0.087 Uiso 1 1 calc R U . . .
H7C H 0.2971 0.1212 0.6129 0.087 Uiso 1 1 calc R U . . .
C8 C 1.0146(4) 0.1863(3) 0.3993(2) 0.0721(9) Uani 1 1 d . . . . .
H8A H 0.9137 0.1369 0.4025 0.108 Uiso 1 1 calc R U . . .
H8B H 1.1274 0.1425 0.3758 0.108 Uiso 1 1 calc R U . . .
H8C H 1.0140 0.2477 0.3464 0.108 Uiso 1 1 calc R U . . .
C9 C 0.0037(3) 0.7105(2) 0.9007(2) 0.0480(6) Uani 1 1 d . . . . .
C10 C 0.3820(4) 0.8631(2) 0.8413(2) 0.0472(6) Uani 1 1 d . . . . .
C11 C 0.5985(3) 0.16648(19) 0.88495(19) 0.0399(5) Uani 1 1 d . . . . .
H11 H 0.5356 0.0979 0.8917 0.048 Uiso 1 1 calc R U . . .
C12 C 0.5035(3) 0.26883(19) 0.91483(19) 0.0426(6) Uani 1 1 d . . . . .
H12 H 0.3766 0.2691 0.9422 0.051 Uiso 1 1 calc R U . . .
C13 C 0.5958(3) 0.37195(18) 0.90438(17) 0.0369(5) Uani 1 1 d . . . . .
C14 C 0.7850(3) 0.3670(2) 0.86287(19) 0.0449(6) Uani 1 1 d . . . . .
H14 H 0.8511 0.4345 0.8541 0.054 Uiso 1 1 calc R U . . .
C15 C 0.8742(3) 0.2636(2) 0.8350(2) 0.0448(6) Uani 1 1 d . . . . .
H15 H 1.0011 0.2611 0.8079 0.054 Uiso 1 1 calc R U . . .
C16 C 0.4985(3) 0.4851(2) 0.93946(19) 0.0432(5) Uani 1 1 d . . . . .
H16A H 0.3727 0.4810 0.9355 0.052 Uiso 1 1 calc R U . . .
H16B H 0.5574 0.5453 0.8882 0.052 Uiso 1 1 calc R U . . .
C17 C 0.8821(3) 0.0538(2) 0.8183(2) 0.0540(7) Uani 1 1 d . . . . .
H17A H 0.8033 -0.0082 0.8507 0.081 Uiso 1 1 calc R U . . .
H17B H 0.9870 0.0521 0.8481 0.081 Uiso 1 1 calc R U . . .
H17C H 0.9215 0.0451 0.7379 0.081 Uiso 1 1 calc R U . . .
H2 H 0.072(3) 0.848(3) 0.942(3) 0.093(12) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.754(2) . ?
S1 C3 1.754(2) . ?
S2 C3 1.753(2) . ?
S2 C2 1.753(2) . ?
S3 C4 1.755(2) . ?
S3 C5 1.756(2) . ?
S4 C4 1.756(2) . ?
S4 C6 1.763(2) . ?
S5 C5 1.740(2) . ?
S5 C7 1.785(3) . ?
S6 C6 1.749(2) . ?
S6 C8 1.794(3) . ?
O1 C9 1.213(3) . ?
O2 C9 1.288(3) . ?
O3 C10 1.283(3) . ?
O4 C10 1.231(3) . ?
N1 C11 1.340(3) . ?
N1 C15 1.345(3) . ?
N1 C17 1.478(3) . ?
C1 C2 1.345(3) . ?
C1 C9 1.504(3) . ?
C2 C10 1.509(3) . ?
C3 C4 1.348(3) . ?
C5 C6 1.348(3) . ?
C11 C12 1.374(3) . ?
C12 C13 1.390(3) . ?
C13 C14 1.389(3) . ?
C13 C16 1.498(3) . ?
C14 C15 1.363(3) . ?
C16 C16 1.541(4) 2_667 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C3 94.39(10) . . ?
C3 S2 C2 94.15(10) . . ?
C4 S3 C5 94.25(10) . . ?
C4 S4 C6 93.81(10) . . ?
C5 S5 C7 103.31(11) . . ?
C6 S6 C8 103.60(12) . . ?
C11 N1 C15 120.5(2) . . ?
C11 N1 C17 119.66(19) . . ?
C15 N1 C17 119.81(19) . . ?
C2 C1 C9 131.6(2) . . ?
C2 C1 S1 116.90(16) . . ?
C9 C1 S1 111.45(16) . . ?
C1 C2 C10 130.3(2) . . ?
C1 C2 S2 117.61(15) . . ?
C10 C2 S2 112.00(17) . . ?
C4 C3 S2 123.28(16) . . ?
C4 C3 S1 122.10(16) . . ?
S2 C3 S1 114.59(12) . . ?
C3 C4 S3 121.16(16) . . ?
C3 C4 S4 124.61(16) . . ?
S3 C4 S4 114.21(12) . . ?
C6 C5 S5 122.97(18) . . ?
C6 C5 S3 116.70(17) . . ?
S5 C5 S3 120.22(12) . . ?
C5 C6 S6 124.92(18) . . ?
C5 C6 S4 117.35(17) . . ?
S6 C6 S4 117.71(12) . . ?
O1 C9 O2 123.5(2) . . ?
O1 C9 C1 117.9(2) . . ?
O2 C9 C1 118.6(2) . . ?
O4 C10 O3 124.8(2) . . ?
O4 C10 C2 116.9(2) . . ?
O3 C10 C2 118.4(2) . . ?
N1 C11 C12 120.3(2) . . ?
C11 C12 C13 120.4(2) . . ?
C14 C13 C12 117.6(2) . . ?
C14 C13 C16 120.1(2) . . ?
C12 C13 C16 122.2(2) . . ?
C15 C14 C13 120.2(2) . . ?
N1 C15 C14 121.0(2) . . ?
C13 C16 C16 110.6(2) . 2_667 ?

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
C3 S1 C1 C2 9.4(2) . . . . ?
C3 S1 C1 C9 -173.18(18) . . . . ?
C9 C1 C2 C10 -0.7(4) . . . . ?
S1 C1 C2 C10 176.1(2) . . . . ?
C9 C1 C2 S2 -177.4(2) . . . . ?
S1 C1 C2 S2 -0.6(3) . . . . ?
C3 S2 C2 C1 -8.6(2) . . . . ?
C3 S2 C2 C10 174.17(17) . . . . ?
C2 S2 C3 C4 -163.2(2) . . . . ?
C2 S2 C3 S1 14.78(14) . . . . ?
C1 S1 C3 C4 163.0(2) . . . . ?
C1 S1 C3 S2 -15.06(14) . . . . ?
S2 C3 C4 S3 -178.83(12) . . . . ?
S1 C3 C4 S3 3.3(3) . . . . ?
S2 C3 C4 S4 -0.3(3) . . . . ?
S1 C3 C4 S4 -178.10(12) . . . . ?
C5 S3 C4 C3 -162.41(19) . . . . ?
C5 S3 C4 S4 18.88(14) . . . . ?
C6 S4 C4 C3 163.0(2) . . . . ?
C6 S4 C4 S3 -18.31(14) . . . . ?
C7 S5 C5 C6 170.1(2) . . . . ?
C7 S5 C5 S3 -13.89(18) . . . . ?
C4 S3 C5 C6 -12.06(19) . . . . ?
C4 S3 C5 S5 171.71(14) . . . . ?
S5 C5 C6 S6 -1.2(3) . . . . ?
S3 C5 C6 S6 -177.35(13) . . . . ?
S5 C5 C6 S4 177.30(12) . . . . ?
S3 C5 C6 S4 1.2(2) . . . . ?
C8 S6 C6 C5 69.7(2) . . . . ?
C8 S6 C6 S4 -108.79(16) . . . . ?
C4 S4 C6 C5 10.4(2) . . . . ?
C4 S4 C6 S6 -171.00(13) . . . . ?
C2 C1 C9 O1 -177.8(3) . . . . ?
S1 C1 C9 O1 5.3(3) . . . . ?
C2 C1 C9 O2 2.2(4) . . . . ?
S1 C1 C9 O2 -174.70(19) . . . . ?
C1 C2 C10 O4 177.8(2) . . . . ?
S2 C2 C10 O4 -5.4(3) . . . . ?
C1 C2 C10 O3 -3.7(4) . . . . ?
S2 C2 C10 O3 173.11(19) . . . . ?
C15 N1 C11 C12 -0.5(3) . . . . ?
C17 N1 C11 C12 177.8(2) . . . . ?
N1 C11 C12 C13 0.4(4) . . . . ?
C11 C12 C13 C14 0.2(3) . . . . ?
C11 C12 C13 C16 -177.9(2) . . . . ?
C12 C13 C14 C15 -0.6(3) . . . . ?
C16 C13 C14 C15 177.5(2) . . . . ?
C11 N1 C15 C14 0.1(4) . . . . ?
C17 N1 C15 C14 -178.3(2) . . . . ?
C13 C14 C15 N1 0.5(4) . . . . ?
C14 C13 C16 C16 -83.2(3) . . . 2_667 ?
C12 C13 C16 C16 94.9(3) . . . 2_667 ?

_refine_diff_density_max         0.251
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.055

