# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_pcm15s_0t
_database_code_depnum_ccdc_archive 'CCDC 1499264'
_audit_update_record             
;
2016-08-16 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_absolute_configuration ad
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H26 Br N O6 S, 2.5(C H Cl3)'
_chemical_formula_sum            'C30.50 H28.50 Br Cl7.50 N O6 S'
_chemical_formula_weight         882.89

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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)

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

_cell_length_a                   9.6708(8)
_cell_length_b                   24.094(2)
_cell_length_c                   15.4897(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.783(4)
_cell_angle_gamma                90.00
_cell_volume                     3605.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    6307
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      24.11

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1780
_exptl_absorpt_coefficient_mu    1.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5333
_exptl_absorpt_correction_T_max  0.5333
_exptl_absorpt_process_details   twinabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      103(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18305
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         27.90
_reflns_number_total             18305
_reflns_number_gt                15829
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0334P)²+10.1732P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.097(9)
_refine_ls_number_reflns         18305
_refine_ls_number_parameters     871
_refine_ls_number_restraints     131
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1217
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.067
_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
Br1 Br 0.19077(8) 0.74368(3) 0.62942(4) 0.02399(16) Uani 1 1 d . . .
Br2 Br 0.10970(8) 0.41293(3) 0.87647(4) 0.02312(15) Uani 1 1 d . . .
C1 C 0.2026(6) 0.7690(3) 0.9972(4) 0.0101(12) Uani 1 1 d . . .
C2 C 0.1242(7) 0.7932(2) 1.0605(4) 0.0146(13) Uani 1 1 d . . .
H2 H 0.0571 0.8208 1.0451 0.017 Uiso 1 1 calc R . .
C3 C 0.1449(7) 0.7768(3) 1.1459(4) 0.0134(13) Uani 1 1 d . . .
H3 H 0.0935 0.7938 1.1895 0.016 Uiso 1 1 calc R . .
C4 C 0.2407(7) 0.7355(3) 1.1682(4) 0.0192(14) Uani 1 1 d . . .
H4 H 0.2530 0.7237 1.2266 0.023 Uiso 1 1 calc R . .
C5 C 0.3183(7) 0.7116(3) 1.1049(4) 0.0154(14) Uani 1 1 d . . .
H5 H 0.3849 0.6840 1.1207 0.019 Uiso 1 1 calc R . .
C6 C 0.3001(6) 0.7274(2) 1.0190(4) 0.0104(12) Uani 1 1 d . . .
C7 C 0.3682(7) 0.7008(2) 0.9453(4) 0.0118(13) Uani 1 1 d . . .
H7 H 0.4311 0.7287 0.9199 0.014 Uiso 1 1 calc R . .
C8 C 0.4504(6) 0.6501(3) 0.9668(4) 0.0127(13) Uani 1 1 d . . .
H8 H 0.5177 0.6512 1.0135 0.015 Uiso 1 1 calc R . .
C9 C 0.4322(6) 0.6034(3) 0.9226(4) 0.0127(13) Uani 1 1 d . . .
C10 C 0.5049(7) 0.5497(3) 0.9449(4) 0.0178(14) Uani 1 1 d . . .
C11 C 0.6708(8) 0.5058(3) 1.0401(5) 0.0244(17) Uani 1 1 d . . .
H11A H 0.7089 0.4858 0.9908 0.029 Uiso 1 1 calc R . .
H11B H 0.6054 0.4810 1.0685 0.029 Uiso 1 1 calc R . .
C12 C 0.7851(8) 0.5226(3) 1.1029(5) 0.0237(16) Uani 1 1 d . . .
H12A H 0.8470 0.5485 1.0750 0.036 Uiso 1 1 calc R . .
H12B H 0.8374 0.4896 1.1221 0.036 Uiso 1 1 calc R . .
H12C H 0.7460 0.5407 1.1529 0.036 Uiso 1 1 calc R . .
C13 C 0.3059(7) 0.6486(3) 0.8096(4) 0.0137(13) Uani 1 1 d . . .
H13 H 0.2320 0.6415 0.7635 0.016 Uiso 1 1 calc R . .
C14 C 0.2501(6) 0.6882(2) 0.8780(4) 0.0095(12) Uani 1 1 d . . .
H14 H 0.1742 0.6689 0.9077 0.011 Uiso 1 1 calc R . .
C15 C 0.1925(6) 0.7419(3) 0.8381(4) 0.0114(12) Uani 1 1 d . . .
H15 H 0.2598 0.7559 0.7962 0.014 Uiso 1 1 calc R . .
C16 C 0.0527(6) 0.7345(2) 0.7901(4) 0.0101(12) Uani 1 1 d U . .
C17 C 0.0359(7) 0.7364(3) 0.6996(4) 0.0170(14) Uani 1 1 d . . .
C18 C -0.0934(8) 0.7318(3) 0.6584(5) 0.0219(16) Uani 1 1 d . . .
H18 H -0.1028 0.7327 0.5971 0.026 Uiso 1 1 calc R . .
C19 C -0.2081(7) 0.7261(3) 0.7060(5) 0.0215(16) Uani 1 1 d . . .
H19 H -0.2971 0.7238 0.6774 0.026 Uiso 1 1 calc R . .
C20 C -0.1962(7) 0.7236(3) 0.7953(5) 0.0207(15) Uani 1 1 d . . .
H20 H -0.2758 0.7188 0.8282 0.025 Uiso 1 1 calc R . .
C21 C -0.0654(7) 0.7283(3) 0.8360(4) 0.0145(14) Uani 1 1 d . . .
H21 H -0.0569 0.7273 0.8974 0.017 Uiso 1 1 calc R . .
C22 C 0.4021(6) 0.8536(2) 0.8831(4) 0.0104(12) Uani 1 1 d . . .
C23 C 0.4727(7) 0.8403(3) 0.8083(4) 0.0174(14) Uani 1 1 d . . .
H23 H 0.4235 0.8286 0.7570 0.021 Uiso 1 1 calc R . .
C24 C 0.6158(7) 0.8448(3) 0.8114(4) 0.0173(14) Uani 1 1 d . . .
H24 H 0.6647 0.8350 0.7619 0.021 Uiso 1 1 calc R . .
C25 C 0.6888(7) 0.8630(3) 0.8847(5) 0.0170(15) Uani 1 1 d U . .
C26 C 0.8433(7) 0.8701(3) 0.8870(5) 0.0248(16) Uani 1 1 d . . .
H26A H 0.8797 0.8544 0.8343 0.037 Uiso 1 1 calc R . .
H26B H 0.8849 0.8509 0.9376 0.037 Uiso 1 1 calc R . .
H26C H 0.8662 0.9097 0.8905 0.037 Uiso 1 1 calc R . .
C27 C 0.6130(7) 0.8755(3) 0.9582(4) 0.0166(14) Uani 1 1 d . . .
H27 H 0.6619 0.8879 1.0093 0.020 Uiso 1 1 calc R . .
C28 C 0.4740(7) 0.8705(3) 0.9587(4) 0.0160(14) Uani 1 1 d . . .
H28 H 0.4262 0.8784 1.0094 0.019 Uiso 1 1 calc R . .
C29 C 0.1312(6) 0.3880(3) 0.5118(4) 0.0141(10) Uani 1 1 d . . .
C30 C 0.0484(6) 0.3637(3) 0.4450(4) 0.0141(10) Uani 1 1 d . . .
H30 H -0.0243 0.3389 0.4574 0.017 Uiso 1 1 calc R . .
C31 C 0.0756(7) 0.3769(3) 0.3611(4) 0.0170(14) Uani 1 1 d U . .
H31 H 0.0224 0.3600 0.3151 0.020 Uiso 1 1 calc R . .
C32 C 0.1770(7) 0.4137(3) 0.3424(4) 0.0204(14) Uani 1 1 d . . .
H32 H 0.1950 0.4218 0.2840 0.024 Uiso 1 1 calc R . .
C33 C 0.2529(7) 0.4388(3) 0.4085(4) 0.0183(14) Uani 1 1 d . . .
H33 H 0.3204 0.4658 0.3955 0.022 Uiso 1 1 calc R . .
C34 C 0.2325(7) 0.4255(2) 0.4939(4) 0.0132(13) Uani 1 1 d . . .
C35 C 0.3116(6) 0.4516(2) 0.5719(4) 0.0106(12) Uani 1 1 d . . .
H35 H 0.3713 0.4227 0.6013 0.013 Uiso 1 1 calc R . .
C36 C 0.3990(7) 0.5005(3) 0.5504(4) 0.0146(14) Uani 1 1 d . . .
H36 H 0.4580 0.4982 0.5032 0.018 Uiso 1 1 calc R . .
C37 C 0.3955(7) 0.5470(3) 0.5959(4) 0.0168(14) Uani 1 1 d . A .
C38 C 0.4820(7) 0.5966(3) 0.5761(4) 0.0168(14) Uani 1 1 d D . .
O8 O 0.4753(5) 0.63993(19) 0.6132(3) 0.0217(11) Uani 1 1 d . A .
C39 C 0.6295(15) 0.6399(5) 0.4791(8) 0.022(3) Uani 0.68(2) 1 d PDU A 1
H39A H 0.5788 0.6745 0.4909 0.027 Uiso 0.68(2) 1 calc PR A 1
H39B H 0.7190 0.6406 0.5129 0.027 Uiso 0.68(2) 1 calc PR A 1
C40 C 0.6529(16) 0.6357(6) 0.3879(8) 0.036(4) Uani 0.68(2) 1 d PDU A 1
H40A H 0.7031 0.6012 0.3768 0.053 Uiso 0.68(2) 1 calc PR A 1
H40B H 0.7078 0.6675 0.3700 0.053 Uiso 0.68(2) 1 calc PR A 1
H40C H 0.5638 0.6354 0.3550 0.053 Uiso 0.68(2) 1 calc PR A 1
O7 O 0.5465(11) 0.5907(4) 0.5039(6) 0.018(2) Uani 0.68(2) 1 d PDU A 1
C39A C 0.688(3) 0.6234(12) 0.4920(16) 0.034(5) Uani 0.32(2) 1 d PDU A 2
H39C H 0.7112 0.6520 0.5364 0.041 Uiso 0.32(2) 1 calc PR A 2
H39D H 0.7751 0.6048 0.4769 0.041 Uiso 0.32(2) 1 calc PR A 2
C40A C 0.622(4) 0.6485(14) 0.417(2) 0.053(9) Uani 0.32(2) 1 d PDU A 2
H40D H 0.5906 0.6194 0.3762 0.080 Uiso 0.32(2) 1 calc PR A 2
H40E H 0.6886 0.6726 0.3889 0.080 Uiso 0.32(2) 1 calc PR A 2
H40F H 0.5430 0.6705 0.4337 0.080 Uiso 0.32(2) 1 calc PR A 2
O7A O 0.588(2) 0.5816(8) 0.5260(14) 0.019(4) Uani 0.32(2) 1 d PDU A 2
C41 C 0.2638(6) 0.5062(2) 0.7044(4) 0.0099(8) Uani 1 1 d . A .
H41 H 0.1922 0.5164 0.7460 0.012 Uiso 1 1 calc R . .
C42 C 0.1989(6) 0.4694(2) 0.6323(4) 0.0099(8) Uani 1 1 d . . .
H42 H 0.1281 0.4917 0.5983 0.012 Uiso 1 1 calc R . .
C43 C 0.1278(6) 0.4183(3) 0.6688(4) 0.0100(12) Uani 1 1 d . . .
H43 H 0.1903 0.4028 0.7162 0.012 Uiso 1 1 calc R . .
C44 C -0.0116(6) 0.4286(2) 0.7054(4) 0.0112(13) Uani 1 1 d . . .
C45 C -0.0360(7) 0.4236(3) 0.7934(4) 0.0167(14) Uani 1 1 d . . .
C46 C -0.1706(7) 0.4269(3) 0.8238(5) 0.0204(16) Uani 1 1 d . . .
H46 H -0.1851 0.4221 0.8835 0.025 Uiso 1 1 calc R . .
C47 C -0.2815(8) 0.4373(3) 0.7665(6) 0.0297(18) Uani 1 1 d . . .
H47 H -0.3729 0.4386 0.7864 0.036 Uiso 1 1 calc R . .
C48 C -0.2584(7) 0.4458(3) 0.6788(5) 0.0224(16) Uani 1 1 d . . .
H48 H -0.3336 0.4552 0.6398 0.027 Uiso 1 1 calc R . .
C49 C -0.1271(7) 0.4408(3) 0.6492(5) 0.0186(14) Uani 1 1 d . . .
H49 H -0.1138 0.4455 0.5893 0.022 Uiso 1 1 calc R . .
C50 C 0.3321(6) 0.3044(2) 0.6281(4) 0.0139(13) Uani 1 1 d . . .
C51 C 0.4134(6) 0.3154(3) 0.7008(4) 0.0143(14) Uani 1 1 d . . .
H51 H 0.3736 0.3233 0.7544 0.017 Uiso 1 1 calc R . .
C52 C 0.5545(7) 0.3146(3) 0.6938(4) 0.0181(15) Uani 1 1 d . . .
H52 H 0.6136 0.3225 0.7431 0.022 Uiso 1 1 calc R . .
C53 C 0.6120(7) 0.3023(3) 0.6147(5) 0.0188(15) Uani 1 1 d . . .
C54 C 0.7680(7) 0.3013(3) 0.6123(5) 0.0290(18) Uani 1 1 d . . .
H54A H 0.8030 0.2655 0.6342 0.044 Uiso 1 1 calc R . .
H54B H 0.8073 0.3313 0.6485 0.044 Uiso 1 1 calc R . .
H54C H 0.7950 0.3064 0.5527 0.044 Uiso 1 1 calc R . .
C55 C 0.5285(7) 0.2922(3) 0.5446(4) 0.0154(14) Uani 1 1 d . . .
H55 H 0.5682 0.2845 0.4910 0.018 Uiso 1 1 calc R . .
C56 C 0.3876(7) 0.2929(3) 0.5488(4) 0.0168(14) Uani 1 1 d . . .
H56 H 0.3292 0.2856 0.4990 0.020 Uiso 1 1 calc R . .
C57 C 0.1357(8) 0.0645(3) 0.2243(5) 0.0322(18) Uani 1 1 d . . .
H57 H 0.1385 0.0236 0.2347 0.039 Uiso 1 1 calc R . .
C58 C 0.9055(8) 0.1584(4) 0.5842(6) 0.039(2) Uani 1 1 d . . .
H58 H 0.9212 0.1953 0.5567 0.047 Uiso 1 1 calc R . .
C59 C 0.7856(9) 0.0691(4) 0.8454(6) 0.042(2) Uani 1 1 d . . .
H59 H 0.8162 0.1086 0.8424 0.050 Uiso 1 1 calc R . .
C60 C 0.1883(8) 0.2151(3) 0.8767(5) 0.0270(17) Uani 1 1 d . . .
H60 H 0.1266 0.2374 0.8364 0.032 Uiso 1 1 calc R . .
C61 C 0.2674(8) 0.9443(3) 0.6486(5) 0.0287(18) Uani 1 1 d . . .
H61 H 0.2172 0.9198 0.6888 0.034 Uiso 1 1 calc R . .
Cl1 Cl 0.0457(2) 0.09448(8) 0.30784(14) 0.0344(5) Uani 1 1 d . . .
Cl2 Cl 0.0486(3) 0.07531(9) 0.12410(15) 0.0466(6) Uani 1 1 d . . .
Cl3 Cl 0.3068(2) 0.08784(8) 0.22527(15) 0.0391(5) Uani 1 1 d . . .
Cl4 Cl 0.7280(3) 0.15193(12) 0.6003(2) 0.0638(8) Uani 1 1 d . . .
Cl5 Cl 1.0002(3) 0.15638(11) 0.68042(17) 0.0590(7) Uani 1 1 d . . .
Cl6 Cl 0.9567(4) 0.10669(12) 0.5126(2) 0.0804(10) Uani 1 1 d . . .
Cl7 Cl 0.8824(3) 0.03198(10) 0.77445(16) 0.0571(7) Uani 1 1 d . . .
Cl8 Cl 0.6104(3) 0.06785(11) 0.81709(19) 0.0597(7) Uani 1 1 d . . .
Cl9 Cl 0.8206(3) 0.04675(15) 0.95232(18) 0.0746(9) Uani 1 1 d . . .
Cl10 Cl 0.3063(2) 0.17868(9) 0.81533(13) 0.0344(5) Uani 1 1 d . . .
Cl11 Cl 0.0844(2) 0.16776(8) 0.93212(14) 0.0382(5) Uani 1 1 d . . .
Cl12 Cl 0.2741(2) 0.26043(8) 0.94935(15) 0.0420(5) Uani 1 1 d . . .
Cl13 Cl 0.3334(2) 0.90309(8) 0.56455(12) 0.0357(5) Uani 1 1 d . . .
Cl14 Cl 0.1506(2) 0.99384(8) 0.60273(16) 0.0427(5) Uani 1 1 d . . .
Cl15 Cl 0.4043(2) 0.97708(9) 0.70617(14) 0.0386(5) Uani 1 1 d . . .
N1 N 0.1812(5) 0.7844(2) 0.9084(3) 0.0073(10) Uani 1 1 d . . .
N2 N 0.1092(5) 0.3748(2) 0.6002(3) 0.0135(11) Uani 1 1 d . . .
O1 O 0.5991(5) 0.55643(18) 1.0095(3) 0.0180(10) Uani 1 1 d . . .
O2 O 0.4799(5) 0.50620(17) 0.9084(3) 0.0187(10) Uani 1 1 d . . .
O3 O 0.3473(5) 0.59673(17) 0.8503(3) 0.0144(10) Uani 1 1 d . . .
O4 O 0.4184(5) 0.67433(18) 0.7736(3) 0.0174(10) Uani 1 1 d . . .
H4A H 0.4245 0.6636 0.7223 0.026 Uiso 1 1 calc R . .
O5 O 0.1691(4) 0.85466(18) 0.7919(3) 0.0149(10) Uani 1 1 d . . .
O6 O 0.1750(5) 0.88506(17) 0.9454(3) 0.0148(10) Uani 1 1 d . . .
O9 O 0.3173(4) 0.55594(16) 0.6648(3) 0.0122(9) Uani 1 1 d U . .
O10 O 0.3704(5) 0.47706(17) 0.7469(3) 0.0141(9) Uani 1 1 d . . .
H10 H 0.3940 0.4934 0.7932 0.021 Uiso 1 1 calc R A .
O11 O 0.1116(4) 0.30536(18) 0.7192(3) 0.0150(10) Uani 1 1 d . . .
O12 O 0.0882(5) 0.27277(17) 0.5679(3) 0.0144(9) Uani 1 1 d . . .
S1 S 0.22037(16) 0.84862(6) 0.88018(10) 0.0108(3) Uani 1 1 d . . .
S2 S 0.14881(16) 0.30976(6) 0.63141(11) 0.0117(3) 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
Br1 C17 1.901(7) . ?
Br2 C45 1.879(7) . ?
C1 C2 1.396(8) . ?
C1 C6 1.406(8) . ?
C1 N1 1.431(7) . ?
C2 C3 1.386(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.490(8) . ?
C7 C8 1.486(8) . ?
C7 C14 1.538(8) . ?
C7 H7 1.0000 . ?
C8 C9 1.324(9) . ?
C8 H8 0.9500 . ?
C9 O3 1.366(7) . ?
C9 C10 1.505(9) . ?
C10 O2 1.210(8) . ?
C10 O1 1.330(8) . ?
C11 O1 1.469(7) . ?
C11 C12 1.493(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O4 1.392(8) . ?
C13 O3 1.447(7) . ?
C13 C14 1.543(8) . ?
C13 H13 1.0000 . ?
C14 C15 1.528(8) . ?
C14 H14 1.0000 . ?
C15 N1 1.503(8) . ?
C15 C16 1.521(8) . ?
C15 H15 1.0000 . ?
C16 C21 1.383(9) . ?
C16 C17 1.405(9) . ?
C17 C18 1.380(9) . ?
C18 C19 1.369(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.384(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.390(9) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C28 1.395(9) . ?
C22 C23 1.410(9) . ?
C22 S1 1.760(6) . ?
C23 C24 1.386(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(10) . ?
C24 H24 0.9500 . ?
C25 C27 1.416(10) . ?
C25 C26 1.502(8) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.350(9) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.371(9) . ?
C29 C30 1.404(9) . ?
C29 N2 1.432(8) . ?
C30 C31 1.376(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.363(9) . ?
C31 H31 0.9500 . ?
C32 C33 1.372(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.385(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.532(8) . ?
C35 C36 1.498(8) . ?
C35 C42 1.532(8) . ?
C35 H35 1.0000 . ?
C36 C37 1.325(9) . ?
C36 H36 0.9500 . ?
C37 O9 1.355(8) . ?
C37 C38 1.498(9) . ?
C38 O8 1.195(8) . ?
C38 O7 1.315(9) . ?
C38 O7A 1.362(14) . ?
C39 C40 1.444(14) . ?
C39 O7 1.492(11) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C39A C40A 1.43(2) . ?
C39A O7A 1.514(17) . ?
C39A H39C 0.9900 . ?
C39A H39D 0.9900 . ?
C40A H40D 0.9800 . ?
C40A H40E 0.9800 . ?
C40A H40F 0.9800 . ?
C41 O10 1.387(7) . ?
C41 O9 1.453(7) . ?
C41 C42 1.535(8) . ?
C41 H41 1.0000 . ?
C42 C43 1.531(8) . ?
C42 H42 1.0000 . ?
C43 N2 1.499(8) . ?
C43 C44 1.508(8) . ?
C43 H43 1.0000 . ?
C44 C45 1.400(9) . ?
C44 C49 1.413(9) . ?
C45 C46 1.407(9) . ?
C46 C47 1.381(10) . ?
C46 H46 0.9500 . ?
C47 C48 1.402(11) . ?
C47 H47 0.9500 . ?
C48 C49 1.377(9) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.367(9) . ?
C50 C56 1.393(9) . ?
C50 S2 1.780(6) . ?
C51 C52 1.374(8) . ?
C51 H51 0.9500 . ?
C52 C53 1.402(10) . ?
C52 H52 0.9500 . ?
C53 C55 1.343(9) . ?
C53 C54 1.512(9) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.368(9) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 Cl3 1.747(8) . ?
C57 Cl2 1.749(8) . ?
C57 Cl1 1.750(8) . ?
C57 H57 1.0000 . ?
C58 Cl5 1.712(9) . ?
C58 Cl4 1.753(8) . ?
C58 Cl6 1.755(9) . ?
C58 H58 1.0000 . ?
C59 Cl7 1.728(9) . ?
C59 Cl8 1.729(9) . ?
C59 Cl9 1.758(9) . ?
C59 H59 1.0000 . ?
C60 Cl12 1.748(8) . ?
C60 Cl10 1.755(8) . ?
C60 Cl11 1.769(8) . ?
C60 H60 1.0000 . ?
C61 Cl15 1.748(8) . ?
C61 Cl14 1.768(8) . ?
C61 Cl13 1.781(8) . ?
C61 H61 1.0000 . ?
N1 S1 1.656(5) . ?
N2 S2 1.678(5) . ?
O4 H4A 0.8400 . ?
O5 S1 1.439(5) . ?
O6 S1 1.423(5) . ?
O10 H10 0.8400 . ?
O11 S2 1.428(5) . ?
O12 S2 1.432(5) . ?

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 C6 120.8(5) . . ?
C2 C1 N1 120.5(5) . . ?
C6 C1 N1 118.7(5) . . ?
C3 C2 C1 119.5(6) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.3(6) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.9(6) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C6 C5 C4 121.1(6) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C1 118.5(5) . . ?
C5 C6 C7 125.2(5) . . ?
C1 C6 C7 116.1(5) . . ?
C8 C7 C6 115.7(5) . . ?
C8 C7 C14 111.2(5) . . ?
C6 C7 C14 105.2(5) . . ?
C8 C7 H7 108.2 . . ?
C6 C7 H7 108.2 . . ?
C14 C7 H7 108.2 . . ?
C9 C8 C7 121.7(6) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 O3 125.7(6) . . ?
C8 C9 C10 124.3(6) . . ?
O3 C9 C10 110.0(5) . . ?
O2 C10 O1 124.9(6) . . ?
O2 C10 C9 123.9(6) . . ?
O1 C10 C9 111.3(6) . . ?
O1 C11 C12 108.0(5) . . ?
O1 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
O1 C11 H11B 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O4 C13 O3 110.7(5) . . ?
O4 C13 C14 107.8(5) . . ?
O3 C13 C14 109.4(5) . . ?
O4 C13 H13 109.6 . . ?
O3 C13 H13 109.6 . . ?
C14 C13 H13 109.6 . . ?
C15 C14 C7 110.6(5) . . ?
C15 C14 C13 112.2(5) . . ?
C7 C14 C13 108.3(5) . . ?
C15 C14 H14 108.5 . . ?
C7 C14 H14 108.5 . . ?
C13 C14 H14 108.5 . . ?
N1 C15 C16 109.8(5) . . ?
N1 C15 C14 108.8(4) . . ?
C16 C15 C14 113.4(5) . . ?
N1 C15 H15 108.2 . . ?
C16 C15 H15 108.2 . . ?
C14 C15 H15 108.2 . . ?
C21 C16 C17 117.3(6) . . ?
C21 C16 C15 119.9(6) . . ?
C17 C16 C15 122.8(6) . . ?
C18 C17 C16 121.1(6) . . ?
C18 C17 Br1 117.7(5) . . ?
C16 C17 Br1 121.2(5) . . ?
C19 C18 C17 120.0(6) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.8(7) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C21 118.7(7) . . ?
C19 C20 H20 120.7 . . ?
C21 C20 H20 120.7 . . ?
C16 C21 C20 122.1(6) . . ?
C16 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
C28 C22 C23 121.0(6) . . ?
C28 C22 S1 119.8(5) . . ?
C23 C22 S1 119.2(5) . . ?
C24 C23 C22 118.5(6) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C25 C24 C23 121.6(6) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C27 117.7(6) . . ?
C24 C25 C26 121.6(7) . . ?
C27 C25 C26 120.7(6) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C25 122.7(6) . . ?
C28 C27 H27 118.7 . . ?
C25 C27 H27 118.7 . . ?
C27 C28 C22 118.5(6) . . ?
C27 C28 H28 120.7 . . ?
C22 C28 H28 120.7 . . ?
C34 C29 C30 120.9(6) . . ?
C34 C29 N2 118.7(5) . . ?
C30 C29 N2 120.4(6) . . ?
C31 C30 C29 118.1(6) . . ?
C31 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
C32 C31 C30 121.5(6) . . ?
C32 C31 H31 119.2 . . ?
C30 C31 H31 119.2 . . ?
C31 C32 C33 119.5(6) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C32 C33 C34 121.0(6) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C29 C34 C33 118.8(6) . . ?
C29 C34 C35 116.5(5) . . ?
C33 C34 C35 124.7(6) . . ?
C36 C35 C34 114.4(5) . . ?
C36 C35 C42 109.9(5) . . ?
C34 C35 C42 104.7(5) . . ?
C36 C35 H35 109.2 . . ?
C34 C35 H35 109.2 . . ?
C42 C35 H35 109.2 . . ?
C37 C36 C35 121.2(6) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 O9 125.6(6) . . ?
C36 C37 C38 122.5(6) . . ?
O9 C37 C38 111.9(5) . . ?
O8 C38 O7 122.8(7) . . ?
O8 C38 O7A 124.4(10) . . ?
O7 C38 O7A 23.9(9) . . ?
O8 C38 C37 123.7(6) . . ?
O7 C38 C37 112.3(6) . . ?
O7A C38 C37 110.3(9) . . ?
C40 C39 O7 107.9(9) . . ?
C40 C39 H39A 110.1 . . ?
O7 C39 H39A 110.1 . . ?
C40 C39 H39B 110.1 . . ?
O7 C39 H39B 110.1 . . ?
H39A C39 H39B 108.4 . . ?
C38 O7 C39 114.7(8) . . ?
C40A C39A O7A 107.1(19) . . ?
C40A C39A H39C 110.3 . . ?
O7A C39A H39C 110.3 . . ?
C40A C39A H39D 110.3 . . ?
O7A C39A H39D 110.3 . . ?
H39C C39A H39D 108.6 . . ?
C39A C40A H40D 109.5 . . ?
C39A C40A H40E 109.5 . . ?
H40D C40A H40E 109.5 . . ?
C39A C40A H40F 109.5 . . ?
H40D C40A H40F 109.5 . . ?
H40E C40A H40F 109.5 . . ?
C38 O7A C39A 122.4(18) . . ?
O10 C41 O9 110.3(5) . . ?
O10 C41 C42 108.8(5) . . ?
O9 C41 C42 108.1(5) . . ?
O10 C41 H41 109.9 . . ?
O9 C41 H41 109.9 . . ?
C42 C41 H41 109.9 . . ?
C43 C42 C35 110.2(5) . . ?
C43 C42 C41 111.8(5) . . ?
C35 C42 C41 109.2(5) . . ?
C43 C42 H42 108.5 . . ?
C35 C42 H42 108.5 . . ?
C41 C42 H42 108.5 . . ?
N2 C43 C44 107.6(5) . . ?
N2 C43 C42 110.0(5) . . ?
C44 C43 C42 115.6(5) . . ?
N2 C43 H43 107.8 . . ?
C44 C43 H43 107.8 . . ?
C42 C43 H43 107.8 . . ?
C45 C44 C49 116.9(6) . . ?
C45 C44 C43 123.2(6) . . ?
C49 C44 C43 119.8(5) . . ?
C44 C45 C46 121.5(6) . . ?
C44 C45 Br2 121.5(5) . . ?
C46 C45 Br2 117.0(5) . . ?
C47 C46 C45 119.9(7) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C46 C47 C48 119.5(7) . . ?
C46 C47 H47 120.2 . . ?
C48 C47 H47 120.2 . . ?
C49 C48 C47 120.2(6) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C48 C49 C44 121.8(6) . . ?
C48 C49 H49 119.1 . . ?
C44 C49 H49 119.1 . . ?
C51 C50 C56 122.3(6) . . ?
C51 C50 S2 119.7(5) . . ?
C56 C50 S2 117.8(5) . . ?
C50 C51 C52 117.8(6) . . ?
C50 C51 H51 121.1 . . ?
C52 C51 H51 121.1 . . ?
C51 C52 C53 120.6(6) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 H52 119.7 . . ?
C55 C53 C52 119.8(6) . . ?
C55 C53 C54 122.6(7) . . ?
C52 C53 C54 117.7(6) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 C56 121.4(6) . . ?
C53 C55 H55 119.3 . . ?
C56 C55 H55 119.3 . . ?
C55 C56 C50 118.2(6) . . ?
C55 C56 H56 120.9 . . ?
C50 C56 H56 120.9 . . ?
Cl3 C57 Cl2 112.0(4) . . ?
Cl3 C57 Cl1 111.5(4) . . ?
Cl2 C57 Cl1 111.1(5) . . ?
Cl3 C57 H57 107.3 . . ?
Cl2 C57 H57 107.3 . . ?
Cl1 C57 H57 107.3 . . ?
Cl5 C58 Cl4 111.1(5) . . ?
Cl5 C58 Cl6 112.0(5) . . ?
Cl4 C58 Cl6 109.5(5) . . ?
Cl5 C58 H58 108.0 . . ?
Cl4 C58 H58 108.0 . . ?
Cl6 C58 H58 108.0 . . ?
Cl7 C59 Cl8 112.6(5) . . ?
Cl7 C59 Cl9 110.8(5) . . ?
Cl8 C59 Cl9 112.0(5) . . ?
Cl7 C59 H59 107.0 . . ?
Cl8 C59 H59 107.0 . . ?
Cl9 C59 H59 107.0 . . ?
Cl12 C60 Cl10 111.1(4) . . ?
Cl12 C60 Cl11 110.7(4) . . ?
Cl10 C60 Cl11 109.9(4) . . ?
Cl12 C60 H60 108.4 . . ?
Cl10 C60 H60 108.4 . . ?
Cl11 C60 H60 108.4 . . ?
Cl15 C61 Cl14 110.7(4) . . ?
Cl15 C61 Cl13 109.6(4) . . ?
Cl14 C61 Cl13 109.1(4) . . ?
Cl15 C61 H61 109.2 . . ?
Cl14 C61 H61 109.2 . . ?
Cl13 C61 H61 109.2 . . ?
C1 N1 C15 120.5(5) . . ?
C1 N1 S1 118.2(4) . . ?
C15 N1 S1 114.8(4) . . ?
C29 N2 C43 120.2(5) . . ?
C29 N2 S2 116.2(4) . . ?
C43 N2 S2 115.6(4) . . ?
C10 O1 C11 115.9(5) . . ?
C9 O3 C13 113.4(5) . . ?
C13 O4 H4A 109.5 . . ?
C37 O9 C41 115.2(4) . . ?
C41 O10 H10 109.5 . . ?
O6 S1 O5 120.5(3) . . ?
O6 S1 N1 107.9(3) . . ?
O5 S1 N1 105.8(3) . . ?
O6 S1 C22 106.4(3) . . ?
O5 S1 C22 108.4(3) . . ?
N1 S1 C22 107.3(3) . . ?
O11 S2 O12 119.7(3) . . ?
O11 S2 N2 106.2(3) . . ?
O12 S2 N2 107.6(3) . . ?
O11 S2 C50 108.6(3) . . ?
O12 S2 C50 108.1(3) . . ?
N2 S2 C50 105.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.90
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.123
####################################################################### 
# 
# 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_zgf61
_database_code_depnum_ccdc_archive 'CCDC 1499265'
_audit_update_record             
;
2016-08-16 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;
_chemical_absolute_configuration ad

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C48 H51 N3 O8 S2'

_chemical_formula_sum            'C48 H51 N3 O8 S2'

_chemical_formula_weight         862.04



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source










C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Monoclinic

_symmetry_space_group_name_H-M   P2(1)



loop_

_symmetry_equiv_pos_as_xyz


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



_cell_length_a                   11.2130(4)

_cell_length_b                   13.1574(5)

_cell_length_c                   14.6972(4)

_cell_angle_alpha                90.00

_cell_angle_beta                 95.529(2)

_cell_angle_gamma                90.00

_cell_volume                     2158.25(13)

_cell_formula_units_Z            2

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    5100

_cell_measurement_theta_min      2.68

_cell_measurement_theta_max      22.76



_exptl_crystal_description       plate

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.15

_exptl_crystal_size_mid          0.14

_exptl_crystal_size_min          0.05

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.326

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             912

_exptl_absorpt_coefficient_mu    0.182

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9732

_exptl_absorpt_correction_T_max  0.9909

_exptl_absorpt_process_details   sadabs



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      173(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  '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            23247

_diffrn_reflns_av_R_equivalents  0.0471

_diffrn_reflns_av_sigmaI/netI    0.0636

_diffrn_reflns_limit_h_min       -14

_diffrn_reflns_limit_h_max       14

_diffrn_reflns_limit_k_min       -16

_diffrn_reflns_limit_k_max       16

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       18

_diffrn_reflns_theta_min         1.82

_diffrn_reflns_theta_max         26.43

_reflns_number_total             7860

_reflns_number_gt                6327

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_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)+(0.0903P)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    constr

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   0.06(8)

_refine_ls_number_reflns         7860

_refine_ls_number_parameters     555

_refine_ls_number_restraints     1

_refine_ls_R_factor_all          0.0711

_refine_ls_R_factor_gt           0.0483

_refine_ls_wR_factor_ref         0.1578

_refine_ls_wR_factor_gt          0.1202

_refine_ls_goodness_of_fit_ref   1.110

_refine_ls_restrained_S_all      1.110

_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
















































































































C1 C -0.0643(3) 0.5436(3) 0.5540(2) 0.0242(8) Uani 1 1 d . . .
C2 C -0.1371(3) 0.5801(4) 0.4789(3) 0.0296(9) Uani 1 1 d . . .
H2 H -0.1205 0.6433 0.4517 0.036 Uiso 1 1 calc R . .
C3 C -0.2336(3) 0.5222(4) 0.4452(3) 0.0360(11) Uani 1 1 d . . .
H3 H -0.2854 0.5467 0.3950 0.043 Uiso 1 1 calc R . .
C4 C -0.2562(3) 0.4296(4) 0.4829(3) 0.0371(11) Uani 1 1 d . . .
H4 H -0.3220 0.3899 0.4577 0.044 Uiso 1 1 calc R . .
C5 C -0.1837(3) 0.3938(4) 0.5574(3) 0.0312(10) Uani 1 1 d . . .
H5 H -0.1995 0.3294 0.5829 0.037 Uiso 1 1 calc R . .
C6 C -0.0879(3) 0.4516(3) 0.5951(2) 0.0241(8) Uani 1 1 d . . .
C7 C 0.0064(3) 0.4179(3) 0.6705(2) 0.0226(8) Uani 1 1 d . . .
H7 H 0.0112 0.4703 0.7201 0.027 Uiso 1 1 calc R . .
C8 C 0.1266(3) 0.4184(3) 0.6262(2) 0.0198(8) Uani 1 1 d . . .
H8 H 0.1162 0.3759 0.5696 0.024 Uiso 1 1 calc R . .
C9 C -0.0123(3) 0.3167(3) 0.7122(2) 0.0280(9) Uani 1 1 d . . .
H9 H -0.0898 0.2996 0.7284 0.034 Uiso 1 1 calc R . .
C10 C 0.0751(4) 0.2501(3) 0.7275(3) 0.0274(9) Uani 1 1 d . . .
C11 C 0.0513(4) 0.1469(3) 0.7652(3) 0.0301(10) Uani 1 1 d . . .
C12 C 0.1265(5) -0.0189(4) 0.7970(4) 0.0544(14) Uani 1 1 d . . .
H12A H 0.0830 -0.0181 0.8525 0.065 Uiso 1 1 calc R . .
H12B H 0.0776 -0.0569 0.7487 0.065 Uiso 1 1 calc R . .
C13 C 0.2410(5) -0.0678(4) 0.8167(4) 0.0590(15) Uani 1 1 d . . .
H13A H 0.2755 -0.0825 0.7594 0.089 Uiso 1 1 calc R . .
H13B H 0.2304 -0.1315 0.8496 0.089 Uiso 1 1 calc R . .
H13C H 0.2949 -0.0229 0.8546 0.089 Uiso 1 1 calc R . .
C14 C 0.2250(3) 0.3703(3) 0.6918(2) 0.0204(8) Uani 1 1 d . . .
H14 H 0.2307 0.4084 0.7510 0.025 Uiso 1 1 calc R . .
C15 C 0.3485(3) 0.3126(3) 0.5718(2) 0.0265(9) Uani 1 1 d . . .
H15A H 0.3014 0.3452 0.5193 0.032 Uiso 1 1 calc R . .
H15B H 0.3205 0.2418 0.5780 0.032 Uiso 1 1 calc R . .
C16 C 0.4804(3) 0.3162(3) 0.5614(2) 0.0286(9) Uani 1 1 d . . .
H16A H 0.5046 0.3837 0.5398 0.034 Uiso 1 1 calc R . .
H16B H 0.5037 0.2633 0.5187 0.034 Uiso 1 1 calc R . .
C17 C 0.5348(3) 0.2954(3) 0.6596(3) 0.0283(9) Uani 1 1 d . . .
H17A H 0.6126 0.3308 0.6720 0.034 Uiso 1 1 calc R . .
H17B H 0.5476 0.2216 0.6695 0.034 Uiso 1 1 calc R . .
C18 C 0.4423(3) 0.3369(3) 0.7221(2) 0.0208(8) Uani 1 1 d . . .
H18 H 0.4140 0.2786 0.7580 0.025 Uiso 1 1 calc R . .
C19 C 0.4922(3) 0.4200(3) 0.7913(2) 0.0201(8) Uani 1 1 d . . .
C20 C 0.6129(3) 0.3836(3) 0.8401(2) 0.0246(9) Uani 1 1 d . . .
C21 C 0.6304(4) 0.2827(4) 0.8625(3) 0.0309(9) Uani 1 1 d . . .
H21 H 0.5670 0.2355 0.8489 0.037 Uiso 1 1 calc R . .
C22 C 0.7396(4) 0.2487(4) 0.9047(3) 0.0409(11) Uani 1 1 d . . .
H22 H 0.7507 0.1787 0.9186 0.049 Uiso 1 1 calc R . .
C23 C 0.8316(4) 0.3162(4) 0.9262(3) 0.0426(12) Uani 1 1 d . . .
H23 H 0.9065 0.2931 0.9544 0.051 Uiso 1 1 calc R . .
C24 C 0.8141(4) 0.4167(4) 0.9067(3) 0.0417(11) Uani 1 1 d . . .
H24 H 0.8768 0.4638 0.9230 0.050 Uiso 1 1 calc R . .
C25 C 0.7058(3) 0.4514(4) 0.8633(3) 0.0307(9) Uani 1 1 d . . .
H25 H 0.6956 0.5216 0.8495 0.037 Uiso 1 1 calc R . .
C26 C 0.5040(3) 0.5243(3) 0.7470(2) 0.0237(8) Uani 1 1 d . . .
C27 C 0.5896(3) 0.5410(3) 0.6846(3) 0.0283(9) Uani 1 1 d . . .
H27 H 0.6384 0.4863 0.6681 0.034 Uiso 1 1 calc R . .
C28 C 0.6038(4) 0.6368(4) 0.6468(3) 0.0344(11) Uani 1 1 d . . .
H28 H 0.6606 0.6467 0.6036 0.041 Uiso 1 1 calc R . .
C29 C 0.5350(4) 0.7176(4) 0.6722(3) 0.0363(10) Uani 1 1 d . . .
H29 H 0.5468 0.7835 0.6482 0.044 Uiso 1 1 calc R . .
C30 C 0.4505(4) 0.7025(4) 0.7314(3) 0.0357(10) Uani 1 1 d . . .
H30 H 0.4026 0.7578 0.7480 0.043 Uiso 1 1 calc R . .
C31 C 0.4337(4) 0.6059(3) 0.7679(2) 0.0266(9) Uani 1 1 d . . .
H31 H 0.3729 0.5961 0.8079 0.032 Uiso 1 1 calc R . .
C32 C 0.4631(4) 0.3338(4) 1.0347(3) 0.0348(10) Uani 1 1 d . . .
H32A H 0.4296 0.2714 1.0062 0.052 Uiso 1 1 calc R . .
H32B H 0.4397 0.3391 1.0970 0.052 Uiso 1 1 calc R . .
H32C H 0.5507 0.3319 1.0366 0.052 Uiso 1 1 calc R . .
C33 C 0.4928(4) 0.5578(4) 1.0074(3) 0.0396(11) Uani 1 1 d . . .
H33A H 0.5752 0.5511 0.9914 0.059 Uiso 1 1 calc R . .
H33B H 0.4932 0.5637 1.0739 0.059 Uiso 1 1 calc R . .
H33C H 0.4561 0.6186 0.9782 0.059 Uiso 1 1 calc R . .
C34 C 0.2443(4) 0.4652(4) 0.9793(3) 0.0405(12) Uani 1 1 d . . .
H34A H 0.2194 0.5307 0.9520 0.061 Uiso 1 1 calc R . .
H34B H 0.2310 0.4653 1.0442 0.061 Uiso 1 1 calc R . .
H34C H 0.1973 0.4105 0.9479 0.061 Uiso 1 1 calc R . .
C35 C 0.1575(3) 0.5281(3) 0.5982(2) 0.0225(8) Uani 1 1 d . . .
H35 H 0.2133 0.5579 0.6483 0.027 Uiso 1 1 calc R . .
C36 C 0.2191(3) 0.5307(3) 0.5109(2) 0.0216(8) Uani 1 1 d . . .
C37 C 0.3383(3) 0.5603(3) 0.5129(2) 0.0249(8) Uani 1 1 d . . .
H37 H 0.3786 0.5850 0.5683 0.030 Uiso 1 1 calc R . .
C38 C 0.3989(3) 0.5545(3) 0.4359(3) 0.0275(9) Uani 1 1 d . . .
H38 H 0.4809 0.5734 0.4380 0.033 Uiso 1 1 calc R . .
C39 C 0.3379(3) 0.5207(3) 0.3562(2) 0.0266(9) Uani 1 1 d . . .
C40 C 0.2192(3) 0.4935(3) 0.3502(3) 0.0281(9) Uani 1 1 d . . .
H40 H 0.1791 0.4716 0.2937 0.034 Uiso 1 1 calc R . .
C41 C 0.1593(3) 0.4985(4) 0.4278(2) 0.0284(9) Uani 1 1 d . . .
H41 H 0.0771 0.4800 0.4249 0.034 Uiso 1 1 calc R . .
C42 C -0.0113(3) 0.7020(3) 0.7342(3) 0.0287(9) Uani 1 1 d . . .
C43 C 0.0595(4) 0.6656(4) 0.8100(3) 0.0350(10) Uani 1 1 d . . .
H43 H 0.1399 0.6451 0.8050 0.042 Uiso 1 1 calc R . .
C44 C 0.0107(4) 0.6597(4) 0.8934(3) 0.0358(10) Uani 1 1 d . . .
H44 H 0.0585 0.6341 0.9452 0.043 Uiso 1 1 calc R . .
C45 C -0.1044(4) 0.6897(4) 0.9029(3) 0.0366(11) Uani 1 1 d . . .
C46 C -0.1554(4) 0.6809(4) 0.9941(3) 0.0469(13) Uani 1 1 d . . .
H46A H -0.1875 0.6124 1.0008 0.070 Uiso 1 1 calc R . .
H46B H -0.2198 0.7308 0.9971 0.070 Uiso 1 1 calc R . .
H46C H -0.0921 0.6940 1.0434 0.070 Uiso 1 1 calc R . .
C47 C -0.1733(4) 0.7277(4) 0.8257(3) 0.0409(11) Uani 1 1 d . . .
H47 H -0.2529 0.7502 0.8308 0.049 Uiso 1 1 calc R . .
C48 C -0.1267(4) 0.7327(4) 0.7426(3) 0.0360(11) Uani 1 1 d . . .
H48 H -0.1748 0.7576 0.6906 0.043 Uiso 1 1 calc R . .
N1 N 0.0470(3) 0.5926(3) 0.5869(2) 0.0254(7) Uani 1 1 d . . .
N2 N 0.3404(3) 0.3710(3) 0.65721(19) 0.0207(7) Uani 1 1 d . . .
N3 N 0.4022(3) 0.5115(3) 0.2737(2) 0.0375(9) Uani 1 1 d . . .
O1 O 0.1914(2) 0.2647(2) 0.70890(18) 0.0275(6) Uani 1 1 d . . .
O2 O -0.0438(3) 0.1230(3) 0.7898(2) 0.0444(8) Uani 1 1 d . . .
O3 O 0.1449(3) 0.0855(2) 0.7664(2) 0.0389(7) Uani 1 1 d . . .
O4 O 0.4040(2) 0.4267(2) 0.85599(15) 0.0232(6) Uani 1 1 d . . .
O5 O 0.5070(3) 0.5361(4) 0.2781(2) 0.0617(12) Uani 1 1 d . . .
O6 O 0.3480(3) 0.4794(4) 0.2042(2) 0.0682(13) Uani 1 1 d . . .
O7 O 0.1733(3) 0.7355(2) 0.6435(2) 0.0388(7) Uani 1 1 d . . .
O8 O -0.0317(3) 0.7683(2) 0.5691(2) 0.0403(8) Uani 1 1 d . . .
S1 S 0.40569(9) 0.44443(9) 0.96746(6) 0.0311(2) Uani 1 1 d . . .
S2 S 0.04930(9) 0.70812(8) 0.62753(7) 0.0297(2) 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 C6 1.389(6) . ?
C1 C2 1.393(5) . ?
C1 N1 1.445(5) . ?
C2 C3 1.377(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.372(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.522(5) . ?
C7 C9 1.489(6) . ?
C7 C8 1.552(5) . ?
C7 H7 1.0000 . ?
C8 C14 1.532(5) . ?
C8 C35 1.549(5) . ?
C8 H8 1.0000 . ?
C9 C10 1.318(6) . ?
C9 H9 0.9500 . ?
C10 O1 1.372(5) . ?
C10 C11 1.501(6) . ?
C11 O2 1.200(5) . ?
C11 O3 1.323(5) . ?
C12 C13 1.441(7) . ?
C12 O3 1.465(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 N2 1.435(4) . ?
C14 O1 1.467(5) . ?
C14 H14 1.0000 . ?
C15 N2 1.482(4) . ?
C15 C16 1.502(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.536(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.551(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 N2 1.486(4) . ?
C18 C19 1.560(5) . ?
C18 H18 1.0000 . ?
C19 O4 1.439(4) . ?
C19 C26 1.530(5) . ?
C19 C20 1.546(5) . ?
C20 C21 1.378(6) . ?
C20 C25 1.388(6) . ?
C21 C22 1.392(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.374(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.363(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.383(6) . ?
C26 C27 1.408(5) . ?
C27 C28 1.392(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.362(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.400(6) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 S1 1.840(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 S1 1.847(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 S1 1.854(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N1 1.498(5) . ?
C35 C36 1.516(5) . ?
C35 H35 1.0000 . ?
C36 C37 1.389(5) . ?
C36 C41 1.401(5) . ?
C37 C38 1.377(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.372(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.373(5) . ?
C39 N3 1.475(5) . ?
C40 C41 1.380(5) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C48 1.372(5) . ?
C42 C43 1.389(6) . ?
C42 S2 1.770(4) . ?
C43 C44 1.393(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.369(6) . ?
C44 H44 0.9500 . ?
C45 C47 1.403(6) . ?
C45 C46 1.511(6) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.375(6) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
N1 S2 1.632(4) . ?
N3 O6 1.212(5) . ?
N3 O5 1.215(5) . ?
O4 S1 1.653(2) . ?
O7 S2 1.434(3) . ?
O8 S2 1.428(3) . ?



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





















































































































































































































C6 C1 C2 121.4(4) . . ?
C6 C1 N1 116.0(3) . . ?
C2 C1 N1 122.2(4) . . ?
C3 C2 C1 118.4(4) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 118.5(3) . . ?
C5 C6 C7 126.0(4) . . ?
C1 C6 C7 114.9(3) . . ?
C9 C7 C6 116.4(3) . . ?
C9 C7 C8 109.8(3) . . ?
C6 C7 C8 105.3(3) . . ?
C9 C7 H7 108.4 . . ?
C6 C7 H7 108.4 . . ?
C8 C7 H7 108.4 . . ?
C14 C8 C35 112.7(3) . . ?
C14 C8 C7 109.7(3) . . ?
C35 C8 C7 109.9(3) . . ?
C14 C8 H8 108.1 . . ?
C35 C8 H8 108.1 . . ?
C7 C8 H8 108.1 . . ?
C10 C9 C7 122.2(4) . . ?
C10 C9 H9 118.9 . . ?
C7 C9 H9 118.9 . . ?
C9 C10 O1 125.3(4) . . ?
C9 C10 C11 120.6(4) . . ?
O1 C10 C11 114.0(3) . . ?
O2 C11 O3 124.3(4) . . ?
O2 C11 C10 122.9(4) . . ?
O3 C11 C10 112.9(3) . . ?
C13 C12 O3 109.4(4) . . ?
C13 C12 H12A 109.8 . . ?
O3 C12 H12A 109.8 . . ?
C13 C12 H12B 109.8 . . ?
O3 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 O1 108.8(3) . . ?
N2 C14 C8 113.2(3) . . ?
O1 C14 C8 108.5(3) . . ?
N2 C14 H14 108.8 . . ?
O1 C14 H14 108.8 . . ?
C8 C14 H14 108.8 . . ?
N2 C15 C16 102.2(3) . . ?
N2 C15 H15A 111.3 . . ?
C16 C15 H15A 111.3 . . ?
N2 C15 H15B 111.3 . . ?
C16 C15 H15B 111.3 . . ?
H15A C15 H15B 109.2 . . ?
C15 C16 C17 101.8(3) . . ?
C15 C16 H16A 111.4 . . ?
C17 C16 H16A 111.4 . . ?
C15 C16 H16B 111.4 . . ?
C17 C16 H16B 111.4 . . ?
H16A C16 H16B 109.3 . . ?
C16 C17 C18 105.4(3) . . ?
C16 C17 H17A 110.7 . . ?
C18 C17 H17A 110.7 . . ?
C16 C17 H17B 110.7 . . ?
C18 C17 H17B 110.7 . . ?
H17A C17 H17B 108.8 . . ?
N2 C18 C17 104.1(3) . . ?
N2 C18 C19 114.4(3) . . ?
C17 C18 C19 114.5(3) . . ?
N2 C18 H18 107.8 . . ?
C17 C18 H18 107.8 . . ?
C19 C18 H18 107.8 . . ?
O4 C19 C26 108.6(3) . . ?
O4 C19 C20 109.8(3) . . ?
C26 C19 C20 111.6(3) . . ?
O4 C19 C18 104.3(3) . . ?
C26 C19 C18 113.0(3) . . ?
C20 C19 C18 109.2(3) . . ?
C21 C20 C25 118.3(4) . . ?
C21 C20 C19 120.5(4) . . ?
C25 C20 C19 121.2(4) . . ?
C20 C21 C22 121.0(4) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C23 C22 C21 120.3(5) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 119.3(4) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 121.0(5) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C20 C25 C24 120.2(4) . . ?
C20 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C31 C26 C27 117.6(4) . . ?
C31 C26 C19 121.8(3) . . ?
C27 C26 C19 120.6(3) . . ?
C28 C27 C26 120.8(4) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C29 C28 C27 119.9(4) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 120.0(4) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C31 120.4(4) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C26 C31 C30 121.2(4) . . ?
C26 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
S1 C32 H32A 109.5 . . ?
S1 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
S1 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
S1 C33 H33A 109.5 . . ?
S1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
S1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
S1 C34 H34A 109.5 . . ?
S1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
S1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C35 C36 109.5(3) . . ?
N1 C35 C8 110.7(3) . . ?
C36 C35 C8 112.2(3) . . ?
N1 C35 H35 108.1 . . ?
C36 C35 H35 108.1 . . ?
C8 C35 H35 108.1 . . ?
C37 C36 C41 118.8(3) . . ?
C37 C36 C35 120.3(3) . . ?
C41 C36 C35 120.8(3) . . ?
C38 C37 C36 121.1(3) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C39 C38 C37 118.4(3) . . ?
C39 C38 H38 120.8 . . ?
C37 C38 H38 120.8 . . ?
C38 C39 C40 122.6(3) . . ?
C38 C39 N3 119.1(3) . . ?
C40 C39 N3 118.3(3) . . ?
C39 C40 C41 118.7(3) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?
C40 C41 C36 120.3(4) . . ?
C40 C41 H41 119.8 . . ?
C36 C41 H41 119.8 . . ?
C48 C42 C43 120.1(4) . . ?
C48 C42 S2 120.8(3) . . ?
C43 C42 S2 119.1(3) . . ?
C42 C43 C44 118.8(4) . . ?
C42 C43 H43 120.6 . . ?
C44 C43 H43 120.6 . . ?
C45 C44 C43 121.9(4) . . ?
C45 C44 H44 119.1 . . ?
C43 C44 H44 119.1 . . ?
C44 C45 C47 118.1(4) . . ?
C44 C45 C46 120.6(4) . . ?
C47 C45 C46 121.2(4) . . ?
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 . . ?
C48 C47 C45 120.6(4) . . ?
C48 C47 H47 119.7 . . ?
C45 C47 H47 119.7 . . ?
C42 C48 C47 120.5(4) . . ?
C42 C48 H48 119.7 . . ?
C47 C48 H48 119.7 . . ?
C1 N1 C35 117.5(3) . . ?
C1 N1 S2 121.3(3) . . ?
C35 N1 S2 120.3(3) . . ?
C14 N2 C15 115.4(3) . . ?
C14 N2 C18 115.7(3) . . ?
C15 N2 C18 106.3(3) . . ?
O6 N3 O5 122.8(3) . . ?
O6 N3 C39 118.4(4) . . ?
O5 N3 C39 118.8(3) . . ?
C10 O1 C14 115.6(3) . . ?
C11 O3 C12 116.2(4) . . ?
C19 O4 S1 136.1(2) . . ?
O4 S1 C32 112.98(17) . . ?
O4 S1 C33 112.60(18) . . ?
C32 S1 C33 108.7(2) . . ?
O4 S1 C34 101.27(16) . . ?
C32 S1 C34 111.1(2) . . ?
C33 S1 C34 110.0(2) . . ?
O8 S2 O7 120.6(2) . . ?
O8 S2 N1 108.06(18) . . ?
O7 S2 N1 105.95(17) . . ?
O8 S2 C42 106.36(19) . . ?
O7 S2 C42 108.41(18) . . ?
N1 S2 C42 106.73(18) . . ?



_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        26.43

_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         0.418

_refine_diff_density_min         -0.529

_refine_diff_density_rms         0.128
