# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2015

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

data_new
_database_code_depnum_ccdc_archive 'CCDC 921593'
_audit_update_record             
;
2014-11-12 deposited with the CCDC.
2015-07-21 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97

_chemical_name_systematic        1a

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C46 H49 N O6 S3'

_chemical_formula_sum            'C46 H49 N O6 S3'

_chemical_formula_weight         808.04



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           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                   5.3262(3)

_cell_length_b                   13.1770(9)

_cell_length_c                   34.470(2)

_cell_angle_alpha                100.032(3)

_cell_angle_beta                 92.318(2)

_cell_angle_gamma                95.724(3)

_cell_volume                     2366.2(3)

_cell_formula_units_Z            2

_cell_measurement_temperature    298(2)

_cell_measurement_reflns_used    4483

_cell_measurement_theta_min      0.00

_cell_measurement_theta_max      0.00



_exptl_crystal_description       Rectangular

_exptl_crystal_colour            Brown

_exptl_crystal_size_max          0.25

_exptl_crystal_size_mid          0.20

_exptl_crystal_size_min          0.15

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.134

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             856

_exptl_absorpt_coefficient_mu    0.200

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9516

_exptl_absorpt_correction_T_max  0.9706

_exptl_absorpt_process_details   'SADABS (Bruker,2004)'



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      298(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  'Bruker APEXII CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            21926

_diffrn_reflns_av_R_equivalents  0.0408

_diffrn_reflns_av_sigmaI/netI    0.0634

_diffrn_reflns_limit_h_min       -6

_diffrn_reflns_limit_h_max       5

_diffrn_reflns_limit_k_min       -15

_diffrn_reflns_limit_k_max       15

_diffrn_reflns_limit_l_min       -40

_diffrn_reflns_limit_l_max       40

_diffrn_reflns_theta_min         0.60

_diffrn_reflns_theta_max         25.00

_reflns_number_total             7690

_reflns_number_gt                4335

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997) '
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'




_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)+(0.1691P)²+0.6385P] 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         7690

_refine_ls_number_parameters     506

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.1416

_refine_ls_R_factor_gt           0.0793

_refine_ls_wR_factor_ref         0.2921

_refine_ls_wR_factor_gt          0.2482

_refine_ls_goodness_of_fit_ref   1.062

_refine_ls_restrained_S_all      1.062

_refine_ls_shift/su_max          0.009

_refine_ls_shift/su_mean         0.001



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









































































































C1 C 0.0573(8) 0.4771(3) 0.26894(13) 0.0406(11) Uani 1 1 d . . .
C2 C 0.2262(9) 0.4798(4) 0.30076(14) 0.0508(12) Uani 1 1 d . . .
H2 H 0.2362 0.5361 0.3214 0.061 Uiso 1 1 calc R . .
C3 C 0.3804(9) 0.4029(4) 0.30318(16) 0.0563(13) Uani 1 1 d . . .
H3 H 0.4958 0.4099 0.3247 0.068 Uiso 1 1 calc R . .
C4 C 0.3659(8) 0.3161(4) 0.27433(15) 0.0495(12) Uani 1 1 d . . .
C5 C 0.1878(9) 0.3093(3) 0.24316(15) 0.0501(12) Uani 1 1 d . . .
H5 H 0.1706 0.2502 0.2237 0.060 Uiso 1 1 calc R . .
C6 C 0.0353(8) 0.3864(3) 0.23980(13) 0.0419(11) Uani 1 1 d . . .
C7 C -0.3370(8) 0.4756(4) 0.20579(13) 0.0458(12) Uani 1 1 d . . .
C8 C -0.5331(9) 0.4775(4) 0.17886(14) 0.0544(13) Uani 1 1 d . . .
H8 H -0.5770 0.4198 0.1592 0.065 Uiso 1 1 calc R . .
C9 C -0.6671(9) 0.5625(5) 0.18020(14) 0.0569(14) Uani 1 1 d . . .
C10 C -0.6081(9) 0.6454(4) 0.21076(14) 0.0588(14) Uani 1 1 d . . .
H10 H -0.6978 0.7029 0.2126 0.071 Uiso 1 1 calc R . .
C11 C -0.4180(9) 0.6431(4) 0.23841(14) 0.0518(13) Uani 1 1 d . . .
H11 H -0.3831 0.6992 0.2590 0.062 Uiso 1 1 calc R . .
C12 C -0.2740(8) 0.5592(4) 0.23680(13) 0.0439(11) Uani 1 1 d . . .
C13 C 0.5313(9) 0.2378(4) 0.27536(16) 0.0554(13) Uani 1 1 d . . .
C14 C 0.6705(9) 0.1711(4) 0.27554(16) 0.0555(13) Uani 1 1 d . . .
C15 C 0.8350(9) 0.0943(4) 0.27420(15) 0.0504(12) Uani 1 1 d . . .
C16 C 1.1599(9) -0.0204(3) 0.28806(16) 0.0508(12) Uani 1 1 d . . .
C17 C 1.0430(10) -0.0482(4) 0.25163(16) 0.0579(14) Uani 1 1 d . . .
C18 C 0.9624(18) -0.1410(7) 0.1870(2) 0.131(3) Uani 1 1 d . . .
H18A H 0.9472 -0.2126 0.1736 0.157 Uiso 1 1 calc R . .
H18B H 1.0650 -0.1000 0.1715 0.157 Uiso 1 1 calc R . .
C19 C 0.7087(19) -0.1053(8) 0.1888(3) 0.162(5) Uani 1 1 d . . .
H19A H 0.6360 -0.1105 0.1622 0.194 Uiso 1 1 calc R . .
H19B H 0.6008 -0.1503 0.2022 0.194 Uiso 1 1 calc R . .
C20 C 0.8575(10) 0.0166(4) 0.24405(16) 0.0588(14) Uani 1 1 d . . .
C21 C 1.3637(9) -0.0629(4) 0.30640(19) 0.0622(15) Uani 1 1 d . . .
H21 H 1.4249 -0.0300 0.3316 0.075 Uiso 1 1 calc R . .
C22 C -0.8701(10) 0.5615(5) 0.15107(15) 0.0701(17) Uani 1 1 d . . .
C23 C -1.0340(11) 0.5599(6) 0.12681(16) 0.083(2) Uani 1 1 d . . .
C24 C -1.2432(10) 0.5429(6) 0.09803(15) 0.085(2) Uani 1 1 d . . .
C25 C -1.5836(12) 0.4669(8) 0.04808(18) 0.098(3) Uani 1 1 d . . .
C26 C -1.5840(11) 0.5682(8) 0.05865(16) 0.092(2) Uani 1 1 d . . .
C27 C -1.7274(17) 0.7254(9) 0.0603(3) 0.141(4) Uani 1 1 d . . .
H27A H -1.8593 0.7339 0.0788 0.170 Uiso 1 1 calc R . .
H27B H -1.7661 0.7640 0.0396 0.170 Uiso 1 1 calc R . .
C28 C -1.499(3) 0.7750(9) 0.0805(3) 0.203(6) Uani 1 1 d . . .
H28A H -1.3942 0.8008 0.0612 0.244 Uiso 1 1 calc R . .
H28B H -1.5407 0.8350 0.0987 0.244 Uiso 1 1 calc R . .
C29 C -1.3839(11) 0.6186(8) 0.08723(16) 0.085(2) Uani 1 1 d . . .
C30 C -1.7565(16) 0.3949(11) 0.0205(2) 0.130(4) Uani 1 1 d . . .
H30 H -1.8818 0.4224 0.0073 0.156 Uiso 1 1 calc R . .
C31 C -0.0003(9) 0.6597(3) 0.29212(13) 0.0452(11) Uani 1 1 d . . .
H31A H -0.0243 0.7163 0.2782 0.054 Uiso 1 1 calc R . .
H31B H 0.1783 0.6639 0.2997 0.054 Uiso 1 1 calc R . .
C32 C -0.1477(9) 0.6738(3) 0.32941(13) 0.0497(12) Uani 1 1 d . . .
H32A H -0.3273 0.6610 0.3221 0.060 Uiso 1 1 calc R . .
H32B H -0.1060 0.6231 0.3453 0.060 Uiso 1 1 calc R . .
C33 C -0.0897(9) 0.7823(4) 0.35400(14) 0.0535(13) Uani 1 1 d . . .
H33A H 0.0877 0.7926 0.3629 0.064 Uiso 1 1 calc R . .
H33B H -0.1178 0.8327 0.3373 0.064 Uiso 1 1 calc R . .
C34 C -0.2444(10) 0.8024(4) 0.38921(15) 0.0586(14) Uani 1 1 d . . .
H34A H -0.1982 0.7585 0.4076 0.070 Uiso 1 1 calc R . .
H34B H -0.4211 0.7823 0.3808 0.070 Uiso 1 1 calc R . .
C35 C -0.2156(10) 0.9137(4) 0.41065(16) 0.0614(14) Uani 1 1 d . . .
H35A H -0.2651 0.9570 0.3923 0.074 Uiso 1 1 calc R . .
H35B H -0.3331 0.9195 0.4315 0.074 Uiso 1 1 calc R . .
C36 C 0.0421(9) 0.9561(4) 0.42848(16) 0.0590(14) Uani 1 1 d . . .
H36A H 0.1587 0.9546 0.4075 0.071 Uiso 1 1 calc R . .
H36B H 0.0963 0.9110 0.4459 0.071 Uiso 1 1 calc R . .
C37 C 0.0595(10) 1.0650(4) 0.45144(16) 0.0620(14) Uani 1 1 d . . .
H37A H 0.0085 1.1100 0.4338 0.074 Uiso 1 1 calc R . .
H37B H -0.0608 1.0666 0.4719 0.074 Uiso 1 1 calc R . .
C38 C 0.3143(10) 1.1087(4) 0.47048(16) 0.0601(14) Uani 1 1 d . . .
H38A H 0.4352 1.1073 0.4501 0.072 Uiso 1 1 calc R . .
H38B H 0.3655 1.0642 0.4883 0.072 Uiso 1 1 calc R . .
C39 C 0.3269(10) 1.2199(4) 0.49359(16) 0.0613(14) Uani 1 1 d . . .
H39A H 0.2716 1.2640 0.4759 0.074 Uiso 1 1 calc R . .
H39B H 0.2085 1.2209 0.5143 0.074 Uiso 1 1 calc R . .
C40 C 0.5834(10) 1.2655(4) 0.51208(17) 0.0655(15) Uani 1 1 d . . .
H40A H 0.6401 1.2208 0.5295 0.079 Uiso 1 1 calc R . .
H40B H 0.7013 1.2657 0.4914 0.079 Uiso 1 1 calc R . .
C41 C 0.5930(10) 1.3725(4) 0.53500(17) 0.0649(15) Uani 1 1 d . . .
H41A H 0.4839 1.3710 0.5568 0.078 Uiso 1 1 calc R . .
H41B H 0.5235 1.4158 0.5181 0.078 Uiso 1 1 calc R . .
C42 C 0.8495(11) 1.4230(4) 0.55135(19) 0.0799(18) Uani 1 1 d . . .
H42A H 0.9204 1.3787 0.5677 0.096 Uiso 1 1 calc R . .
H42B H 0.9573 1.4257 0.5295 0.096 Uiso 1 1 calc R . .
C43 C 0.8615(10) 1.5284(4) 0.57491(18) 0.0736(17) Uani 1 1 d . . .
H43A H 0.7754 1.5237 0.5989 0.088 Uiso 1 1 calc R . .
H43B H 0.7669 1.5698 0.5601 0.088 Uiso 1 1 calc R . .
C44 C 1.1171(11) 1.5854(4) 0.5863(2) 0.0804(18) Uani 1 1 d . . .
H44A H 1.2116 1.5441 0.6011 0.096 Uiso 1 1 calc R . .
H44B H 1.2034 1.5900 0.5623 0.096 Uiso 1 1 calc R . .
C45 C 1.1282(11) 1.6907(5) 0.6097(2) 0.092(2) Uani 1 1 d . . .
H45A H 1.0669 1.6852 0.6355 0.110 Uiso 1 1 calc R . .
H45B H 1.0126 1.7289 0.5970 0.110 Uiso 1 1 calc R . .
C46 C 1.3804(11) 1.7526(5) 0.61559(19) 0.0811(18) Uani 1 1 d . . .
H46A H 1.4907 1.7215 0.6317 0.122 Uiso 1 1 calc R . .
H46B H 1.3627 1.8221 0.6284 0.122 Uiso 1 1 calc R . .
H46C H 1.4506 1.7541 0.5905 0.122 Uiso 1 1 calc R . .
N1 N -0.0743(7) 0.5617(3) 0.26525(10) 0.0423(9) Uani 1 1 d . . .
O7 O 1.0883(8) -0.1335(3) 0.22496(12) 0.0869(13) Uani 1 1 d . . .
O8 O 0.7141(8) 0.0017(3) 0.20958(12) 0.0900(14) Uani 1 1 d . . .
O9 O 1.4597(8) -0.1371(3) 0.29169(14) 0.0888(13) Uani 1 1 d . . .
O10 O -1.7499(9) 0.6235(6) 0.04325(14) 0.119(2) Uani 1 1 d . . .
O11 O -1.3500(9) 0.7191(5) 0.10196(13) 0.1013(16) Uani 1 1 d . . .
O12 O -1.7518(14) 0.3000(7) 0.0130(2) 0.154(3) Uani 1 1 d . . .
S1 S -0.1719(3) 0.36580(11) 0.19802(4) 0.0636(5) Uani 1 1 d . . .
S2 S 1.0420(2) 0.08824(10) 0.31324(4) 0.0609(5) Uani 1 1 d . . .
S3 S -1.3417(3) 0.42092(19) 0.07324(5) 0.1017(7) 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















































































































C1 C2 1.383(6) . ?
C1 N1 1.396(5) . ?
C1 C6 1.412(6) . ?
C2 C3 1.378(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(6) . ?
C4 C13 1.425(6) . ?
C5 C6 1.379(6) . ?
C5 H5 0.9300 . ?
C6 S1 1.744(4) . ?
C7 C8 1.374(6) . ?
C7 C12 1.398(6) . ?
C7 S1 1.754(5) . ?
C8 C9 1.383(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(7) . ?
C9 C22 1.443(7) . ?
C10 C11 1.368(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.402(6) . ?
C11 H11 0.9300 . ?
C12 N1 1.411(5) . ?
C13 C14 1.206(6) . ?
C14 C15 1.399(6) . ?
C15 C20 1.344(7) . ?
C15 S2 1.723(5) . ?
C16 C17 1.353(7) . ?
C16 C21 1.442(7) . ?
C16 S2 1.729(5) . ?
C17 O7 1.371(6) . ?
C17 C20 1.414(6) . ?
C18 O7 1.429(8) . ?
C18 C19 1.475(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 O8 1.462(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 O8 1.360(6) . ?
C21 O9 1.193(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.180(7) . ?
C23 C24 1.435(7) . ?
C24 C29 1.397(9) . ?
C24 S3 1.704(8) . ?
C25 C26 1.322(11) . ?
C25 C30 1.446(12) . ?
C25 S3 1.740(7) . ?
C26 O10 1.348(8) . ?
C26 C29 1.447(9) . ?
C27 O10 1.360(10) . ?
C27 C28 1.416(13) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 O11 1.407(9) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 O11 1.325(9) . ?
C30 O12 1.235(12) . ?
C30 H30 0.9300 . ?
C31 N1 1.460(5) . ?
C31 C32 1.526(6) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.525(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.495(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.512(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.495(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.505(7) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.498(7) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.534(7) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.505(7) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.487(7) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.501(7) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.476(7) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.490(7) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.474(8) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C46 1.487(8) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 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








































































































































































































C2 C1 N1 121.3(4) . . ?
C2 C1 C6 116.3(4) . . ?
N1 C1 C6 122.3(4) . . ?
C3 C2 C1 122.9(4) . . ?
C3 C2 H2 118.6 . . ?
C1 C2 H2 118.6 . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 116.9(4) . . ?
C3 C4 C13 121.9(4) . . ?
C5 C4 C13 121.2(4) . . ?
C6 C5 C4 123.0(4) . . ?
C6 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C5 C6 C1 119.8(4) . . ?
C5 C6 S1 116.5(3) . . ?
C1 C6 S1 123.7(3) . . ?
C8 C7 C12 120.4(4) . . ?
C8 C7 S1 116.3(4) . . ?
C12 C7 S1 123.3(3) . . ?
C7 C8 C9 121.9(5) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C10 C9 C8 118.3(4) . . ?
C10 C9 C22 121.6(5) . . ?
C8 C9 C22 120.0(5) . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 122.4(5) . . ?
C10 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C7 C12 C11 116.7(4) . . ?
C7 C12 N1 122.9(4) . . ?
C11 C12 N1 120.4(4) . . ?
C14 C13 C4 178.9(6) . . ?
C13 C14 C15 177.6(6) . . ?
C20 C15 C14 127.2(5) . . ?
C20 C15 S2 110.3(3) . . ?
C14 C15 S2 122.5(4) . . ?
C17 C16 C21 130.7(5) . . ?
C17 C16 S2 110.0(3) . . ?
C21 C16 S2 119.3(4) . . ?
C16 C17 O7 124.1(4) . . ?
C16 C17 C20 113.4(5) . . ?
O7 C17 C20 122.4(5) . . ?
O7 C18 C19 113.3(6) . . ?
O7 C18 H18A 108.9 . . ?
C19 C18 H18A 108.9 . . ?
O7 C18 H18B 108.9 . . ?
C19 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
O8 C19 C18 112.4(8) . . ?
O8 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
O8 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C15 C20 O8 123.0(4) . . ?
C15 C20 C17 113.7(5) . . ?
O8 C20 C17 123.3(5) . . ?
O9 C21 C16 124.9(6) . . ?
O9 C21 H21 117.6 . . ?
C16 C21 H21 117.6 . . ?
C23 C22 C9 179.0(6) . . ?
C22 C23 C24 171.7(8) . . ?
C29 C24 C23 126.3(7) . . ?
C29 C24 S3 113.5(5) . . ?
C23 C24 S3 120.2(5) . . ?
C26 C25 C30 128.6(8) . . ?
C26 C25 S3 111.7(5) . . ?
C30 C25 S3 119.6(8) . . ?
C25 C26 O10 123.7(7) . . ?
C25 C26 C29 115.2(6) . . ?
O10 C26 C29 121.1(8) . . ?
O10 C27 C28 121.3(8) . . ?
O10 C27 H27A 107.0 . . ?
C28 C27 H27A 107.0 . . ?
O10 C27 H27B 107.0 . . ?
C28 C27 H27B 107.0 . . ?
H27A C27 H27B 106.8 . . ?
O11 C28 C27 119.6(11) . . ?
O11 C28 H28A 107.4 . . ?
C27 C28 H28A 107.4 . . ?
O11 C28 H28B 107.4 . . ?
C27 C28 H28B 107.4 . . ?
H28A C28 H28B 107.0 . . ?
O11 C29 C24 126.2(6) . . ?
O11 C29 C26 125.1(7) . . ?
C24 C29 C26 108.6(8) . . ?
O12 C30 C25 125.5(10) . . ?
O12 C30 H30 117.2 . . ?
C25 C30 H30 117.2 . . ?
N1 C31 C32 114.0(4) . . ?
N1 C31 H31A 108.8 . . ?
C32 C31 H31A 108.8 . . ?
N1 C31 H31B 108.8 . . ?
C32 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C33 C32 C31 112.3(4) . . ?
C33 C32 H32A 109.1 . . ?
C31 C32 H32A 109.1 . . ?
C33 C32 H32B 109.1 . . ?
C31 C32 H32B 109.1 . . ?
H32A C32 H32B 107.9 . . ?
C34 C33 C32 114.2(4) . . ?
C34 C33 H33A 108.7 . . ?
C32 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
C32 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C33 C34 C35 114.8(4) . . ?
C33 C34 H34A 108.6 . . ?
C35 C34 H34A 108.6 . . ?
C33 C34 H34B 108.6 . . ?
C35 C34 H34B 108.6 . . ?
H34A C34 H34B 107.5 . . ?
C36 C35 C34 116.3(4) . . ?
C36 C35 H35A 108.2 . . ?
C34 C35 H35A 108.2 . . ?
C36 C35 H35B 108.2 . . ?
C34 C35 H35B 108.2 . . ?
H35A C35 H35B 107.4 . . ?
C35 C36 C37 114.6(4) . . ?
C35 C36 H36A 108.6 . . ?
C37 C36 H36A 108.6 . . ?
C35 C36 H36B 108.6 . . ?
C37 C36 H36B 108.6 . . ?
H36A C36 H36B 107.6 . . ?
C38 C37 C36 115.9(4) . . ?
C38 C37 H37A 108.3 . . ?
C36 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
C36 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C37 C38 C39 114.8(4) . . ?
C37 C38 H38A 108.6 . . ?
C39 C38 H38A 108.6 . . ?
C37 C38 H38B 108.6 . . ?
C39 C38 H38B 108.6 . . ?
H38A C38 H38B 107.5 . . ?
C40 C39 C38 115.2(4) . . ?
C40 C39 H39A 108.5 . . ?
C38 C39 H39A 108.5 . . ?
C40 C39 H39B 108.5 . . ?
C38 C39 H39B 108.5 . . ?
H39A C39 H39B 107.5 . . ?
C41 C40 C39 114.9(5) . . ?
C41 C40 H40A 108.6 . . ?
C39 C40 H40A 108.6 . . ?
C41 C40 H40B 108.6 . . ?
C39 C40 H40B 108.6 . . ?
H40A C40 H40B 107.5 . . ?
C40 C41 C42 116.1(5) . . ?
C40 C41 H41A 108.3 . . ?
C42 C41 H41A 108.3 . . ?
C40 C41 H41B 108.3 . . ?
C42 C41 H41B 108.3 . . ?
H41A C41 H41B 107.4 . . ?
C43 C42 C41 116.8(5) . . ?
C43 C42 H42A 108.1 . . ?
C41 C42 H42A 108.1 . . ?
C43 C42 H42B 108.1 . . ?
C41 C42 H42B 108.1 . . ?
H42A C42 H42B 107.3 . . ?
C42 C43 C44 117.2(5) . . ?
C42 C43 H43A 108.0 . . ?
C44 C43 H43A 108.0 . . ?
C42 C43 H43B 108.0 . . ?
C44 C43 H43B 108.0 . . ?
H43A C43 H43B 107.2 . . ?
C45 C44 C43 117.1(5) . . ?
C45 C44 H44A 108.0 . . ?
C43 C44 H44A 108.0 . . ?
C45 C44 H44B 108.0 . . ?
C43 C44 H44B 108.0 . . ?
H44A C44 H44B 107.3 . . ?
C44 C45 C46 116.4(5) . . ?
C44 C45 H45A 108.2 . . ?
C46 C45 H45A 108.2 . . ?
C44 C45 H45B 108.2 . . ?
C46 C45 H45B 108.2 . . ?
H45A C45 H45B 107.3 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C1 N1 C12 124.1(4) . . ?
C1 N1 C31 118.4(3) . . ?
C12 N1 C31 117.5(3) . . ?
C17 O7 C18 113.9(4) . . ?
C20 O8 C19 110.7(4) . . ?
C26 O10 C27 113.9(6) . . ?
C29 O11 C28 111.3(6) . . ?
C6 S1 C7 102.5(2) . . ?
C15 S2 C16 92.5(2) . . ?
C24 S3 C25 91.0(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


















































































































N1 C1 C2 C3 -172.4(4) . . . . ?
C6 C1 C2 C3 4.7(7) . . . . ?
C1 C2 C3 C4 -2.8(8) . . . . ?
C2 C3 C4 C5 -0.8(8) . . . . ?
C2 C3 C4 C13 177.1(5) . . . . ?
C3 C4 C5 C6 2.1(8) . . . . ?
C13 C4 C5 C6 -175.8(5) . . . . ?
C4 C5 C6 C1 0.0(7) . . . . ?
C4 C5 C6 S1 178.5(4) . . . . ?
C2 C1 C6 C5 -3.3(7) . . . . ?
N1 C1 C6 C5 173.8(4) . . . . ?
C2 C1 C6 S1 178.3(4) . . . . ?
N1 C1 C6 S1 -4.6(7) . . . . ?
C12 C7 C8 C9 2.9(8) . . . . ?
S1 C7 C8 C9 -175.7(4) . . . . ?
C7 C8 C9 C10 -3.2(8) . . . . ?
C7 C8 C9 C22 179.4(5) . . . . ?
C8 C9 C10 C11 1.2(8) . . . . ?
C22 C9 C10 C11 178.6(5) . . . . ?
C9 C10 C11 C12 1.1(8) . . . . ?
C8 C7 C12 C11 -0.6(7) . . . . ?
S1 C7 C12 C11 177.9(4) . . . . ?
C8 C7 C12 N1 -179.8(4) . . . . ?
S1 C7 C12 N1 -1.4(7) . . . . ?
C10 C11 C12 C7 -1.4(7) . . . . ?
C10 C11 C12 N1 177.9(5) . . . . ?
C3 C4 C13 C14 -156(100) . . . . ?
C5 C4 C13 C14 22(31) . . . . ?
C4 C13 C14 C15 34(38) . . . . ?
C13 C14 C15 C20 -48(14) . . . . ?
C13 C14 C15 S2 132(14) . . . . ?
C21 C16 C17 O7 6.0(9) . . . . ?
S2 C16 C17 O7 -177.6(4) . . . . ?
C21 C16 C17 C20 -177.1(5) . . . . ?
S2 C16 C17 C20 -0.7(6) . . . . ?
O7 C18 C19 O8 57.2(12) . . . . ?
C14 C15 C20 O8 -0.7(9) . . . . ?
S2 C15 C20 O8 179.0(4) . . . . ?
C14 C15 C20 C17 179.6(5) . . . . ?
S2 C15 C20 C17 -0.7(6) . . . . ?
C16 C17 C20 C15 0.9(7) . . . . ?
O7 C17 C20 C15 177.9(5) . . . . ?
C16 C17 C20 O8 -178.8(5) . . . . ?
O7 C17 C20 O8 -1.8(9) . . . . ?
C17 C16 C21 O9 -3.6(10) . . . . ?
S2 C16 C21 O9 -179.7(5) . . . . ?
C10 C9 C22 C23 143(45) . . . . ?
C8 C9 C22 C23 -40(46) . . . . ?
C9 C22 C23 C24 81(46) . . . . ?
C22 C23 C24 C29 153(4) . . . . ?
C22 C23 C24 S3 -27(4) . . . . ?
C30 C25 C26 O10 -2.8(13) . . . . ?
S3 C25 C26 O10 179.1(5) . . . . ?
C30 C25 C26 C29 179.8(7) . . . . ?
S3 C25 C26 C29 1.8(8) . . . . ?
O10 C27 C28 O11 -34.8(18) . . . . ?
C23 C24 C29 O11 -0.7(10) . . . . ?
S3 C24 C29 O11 179.4(5) . . . . ?
C23 C24 C29 C26 -177.5(6) . . . . ?
S3 C24 C29 C26 2.6(7) . . . . ?
C25 C26 C29 O11 -179.6(6) . . . . ?
O10 C26 C29 O11 2.9(10) . . . . ?
C25 C26 C29 C24 -2.8(8) . . . . ?
O10 C26 C29 C24 179.8(5) . . . . ?
C26 C25 C30 O12 -177.0(10) . . . . ?
S3 C25 C30 O12 0.9(14) . . . . ?
N1 C31 C32 C33 -172.5(4) . . . . ?
C31 C32 C33 C34 175.5(4) . . . . ?
C32 C33 C34 C35 -171.9(4) . . . . ?
C33 C34 C35 C36 -62.6(6) . . . . ?
C34 C35 C36 C37 -176.8(5) . . . . ?
C35 C36 C37 C38 178.6(5) . . . . ?
C36 C37 C38 C39 179.8(5) . . . . ?
C37 C38 C39 C40 -178.7(5) . . . . ?
C38 C39 C40 C41 -179.0(5) . . . . ?
C39 C40 C41 C42 -175.8(5) . . . . ?
C40 C41 C42 C43 -178.7(6) . . . . ?
C41 C42 C43 C44 -171.2(6) . . . . ?
C42 C43 C44 C45 179.9(6) . . . . ?
C43 C44 C45 C46 -171.0(6) . . . . ?
C2 C1 N1 C12 -170.7(4) . . . . ?
C6 C1 N1 C12 12.4(7) . . . . ?
C2 C1 N1 C31 10.0(7) . . . . ?
C6 C1 N1 C31 -167.0(4) . . . . ?
C7 C12 N1 C1 -9.3(7) . . . . ?
C11 C12 N1 C1 171.5(4) . . . . ?
C7 C12 N1 C31 170.0(4) . . . . ?
C11 C12 N1 C31 -9.2(6) . . . . ?
C32 C31 N1 C1 -92.3(5) . . . . ?
C32 C31 N1 C12 88.3(5) . . . . ?
C16 C17 O7 C18 -173.7(7) . . . . ?
C20 C17 O7 C18 9.6(9) . . . . ?
C19 C18 O7 C17 -36.5(11) . . . . ?
C15 C20 O8 C19 -158.9(7) . . . . ?
C17 C20 O8 C19 20.8(9) . . . . ?
C18 C19 O8 C20 -47.1(10) . . . . ?
C25 C26 O10 C27 175.7(9) . . . . ?
C29 C26 O10 C27 -7.1(10) . . . . ?
C28 C27 O10 C26 22.5(15) . . . . ?
C24 C29 O11 C28 171.2(9) . . . . ?
C26 C29 O11 C28 -12.5(11) . . . . ?
C27 C28 O11 C29 27.1(15) . . . . ?
C5 C6 S1 C7 177.5(4) . . . . ?
C1 C6 S1 C7 -4.1(5) . . . . ?
C8 C7 S1 C6 -174.5(4) . . . . ?
C12 C7 S1 C6 7.0(5) . . . . ?
C20 C15 S2 C16 0.3(4) . . . . ?
C14 C15 S2 C16 180.0(4) . . . . ?
C17 C16 S2 C15 0.2(4) . . . . ?
C21 C16 S2 C15 177.1(4) . . . . ?
C29 C24 S3 C25 -1.5(5) . . . . ?
C23 C24 S3 C25 178.6(5) . . . . ?
C26 C25 S3 C24 -0.2(6) . . . . ?
C30 C25 S3 C24 -178.4(6) . . . . ?



_diffrn_measured_fraction_theta_max 0.920

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.920

_refine_diff_density_max         0.743

_refine_diff_density_min         -0.322

_refine_diff_density_rms         0.112



_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.920 Note  
RESPONSE: Even though crystal data was collected up to 0.73 \%A 
resolution, the crystal (the largest available) still 
diffracted quite weakly at high angle. On repeated recrystallisation
we could get only small sized crystals.
 
;
_vrf_PLAT601_I                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        384 Ang3  
RESPONSE: The highest peak in the final difference map is just 0.74e/A3 and no 
model for any solvent could be found.The resulting crystal structure is unusual 
in that it contains large voids (384 \%A3) within which there is no evidence of
included solvent.
 
;
# end Validation Reply Form
