# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2014

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_5
_database_code_depnum_ccdc_archive 'CCDC 1030570'
_audit_update_record             
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
_cell_length_a                   13.0584(3)
_cell_length_b                   17.2823(3)
_cell_length_c                   17.4795(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.228(2)
_cell_angle_gamma                90
_cell_volume                     3934.00(13)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  '-P 2ybc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4


_chemical_formula_sum            'C36.00 H36.00 N4 O12 S4'
_chemical_formula_moiety         'C36.00 H36.00 N4 O12 S4'
_chemical_compound_source        ?
_chemical_formula_weight         844.96


_cell_measurement_reflns_used    7099
_cell_measurement_theta_min      4
_cell_measurement_theta_max      73
_cell_measurement_temperature    190

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.240
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_max          0.350

_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    2.794

# Sheldrick geometric approximatio 0.48 0.51 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_T_max  0.51
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      190
_diffrn_ambient_pressure         101
_diffrn_reflns_number            17653
_reflns_number_total             7553
_diffrn_reflns_av_R_equivalents  0.035
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7553 
# Theoretical number of reflections is about 15641 


_diffrn_reflns_theta_min         4.821
_diffrn_reflns_theta_max         72.654
_diffrn_measured_fraction_theta_max 0.967

_diffrn_reflns_theta_full        67.68
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              21
_reflns_limit_l_min              0
_reflns_limit_l_max              21

_oxford_diffrn_Wilson_B_factor   3.72
_oxford_diffrn_Wilson_scale      0.14

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.33
_refine_diff_density_max         0.62


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     28
_refine_ls_number_parameters     533
_oxford_refine_ls_R_factor_ref   0.0619
_refine_ls_wR_factor_ref         0.1598
_refine_ls_goodness_of_fit_ref   0.9865
_refine_ls_shift/su_max          0.0005454
_refine_ls_shift/su_mean         0.0000288


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7553
_refine_ls_R_factor_all          0.0619
_refine_ls_wR_factor_all         0.1598

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5985
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_gt          0.1378

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.193E+04 0.323E+04 0.198E+04 814. 170. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.6183(2) 0.34056(14) 0.38613(13) 0.0421 1.0000 Uani . . . . . .
S2 S 0.59589(5) 0.25178(3) 0.33530(3) 0.0457 1.0000 Uani . . . . . .
C3 C 0.62253(19) 0.27901(13) 0.24029(13) 0.0405 1.0000 Uani . . . . . .
C4 C 0.5406(2) 0.28954(15) 0.18608(14) 0.0451 1.0000 Uani . . . . . .
C5 C 0.5612(2) 0.30509(14) 0.11097(14) 0.0455 1.0000 Uani . . . . . .
C6 C 0.6592(2) 0.31453(15) 0.08875(14) 0.0480 1.0000 Uani . . . . . .
C7 C 0.7407(2) 0.30745(14) 0.14344(15) 0.0446 1.0000 Uani . . . . . .
S8 S 0.86871(5) 0.32506(4) 0.11726(4) 0.0558 1.0000 Uani . . . . . .
C9 C 0.85223(18) 0.42279(15) 0.08503(15) 0.0443 1.0000 Uani . . . . . .
C10 C 0.87378(19) 0.44099(16) 0.01042(15) 0.0473 1.0000 Uani . . . . . .
C11 C 0.86485(18) 0.51658(16) -0.01378(14) 0.0457 1.0000 Uani . . . . . .
C12 C 0.83243(18) 0.57467(15) 0.03225(15) 0.0460 1.0000 Uani . . . . . .
C13 C 0.81140(18) 0.55681(15) 0.10715(15) 0.0443 1.0000 Uani . . . . . .
S14 S 0.77717(5) 0.63185(4) 0.16918(4) 0.0511 1.0000 Uani . . . . . .
C15 C 0.65434(18) 0.59945(13) 0.19314(14) 0.0415 1.0000 Uani . . . . . .
C16 C 0.5787(2) 0.58179(15) 0.13591(15) 0.0462 1.0000 Uani . . . . . .
C17 C 0.4826(2) 0.56180(15) 0.15711(16) 0.0481 1.0000 Uani . . . . . .
C18 C 0.45939(19) 0.55711(15) 0.23247(16) 0.0475 1.0000 Uani . . . . . .
C19 C 0.53503(19) 0.57256(14) 0.28979(14) 0.0432 1.0000 Uani . . . . . .
S20 S 0.50670(5) 0.56122(4) 0.38711(4) 0.0516 1.0000 Uani . . . . . .
C21 C 0.5772(2) 0.47460(14) 0.40974(14) 0.0452 1.0000 Uani . . . . . .
C22 C 0.6521(2) 0.47634(15) 0.46991(14) 0.0475 1.0000 Uani . . . . . .
C23 C 0.7069(2) 0.40998(16) 0.48891(14) 0.0475 1.0000 Uani . . . . . .
C24 C 0.6938(2) 0.34211(15) 0.44667(13) 0.0464 1.0000 Uani . . . . . .
C25 C 0.72390(19) 0.28656(13) 0.21915(13) 0.0410 1.0000 Uani . . . . . .
C26 C 0.82423(17) 0.48093(14) 0.13479(13) 0.0411 1.0000 Uani . . . . . .
C27 C 0.63320(18) 0.59539(13) 0.27080(14) 0.0398 1.0000 Uani . . . . . .
C28 C 0.55614(19) 0.40520(14) 0.36945(13) 0.0424 1.0000 Uani . . . . . .
O29 O 0.80397(14) 0.27664(10) 0.27242(10) 0.0485 1.0000 Uani . . . . . .
C30 C 0.8507(3) 0.20128(18) 0.2722(2) 0.0653 1.0000 Uani . . . . . .
C31 C 0.9579(3) 0.2066(3) 0.3091(3) 0.0849 1.0000 Uani . . . . . .
C32 C 0.9680(4) 0.2380(3) 0.3879(3) 0.0980 1.0000 Uani . . . . . .
O33 O 0.80634(13) 0.46414(11) 0.20845(9) 0.0449 1.0000 Uani . . . . . .
C34 C 0.8978(2) 0.47155(19) 0.26120(15) 0.0539 1.0000 Uani . . . . . .
C35 C 0.8673(2) 0.45560(16) 0.34075(14) 0.0476 1.0000 Uani . . . . . .
C36 C 0.9580(3) 0.4661(2) 0.39975(17) 0.0673 1.0000 Uani . . . . . .
O37 O 0.70967(13) 0.60846(10) 0.32713(10) 0.0453 1.0000 Uani D . . . . .
C38 C 0.7346(7) 0.6899(4) 0.3391(5) 0.0558 0.534(10) Uani D U P 1 1 .
C39 C 0.8346(9) 0.6958(4) 0.3846(5) 0.0805 0.534(10) Uani D U P 1 1 .
C40 C 0.8345(9) 0.6605(5) 0.4642(5) 0.1013 0.534(10) Uani D U P 1 1 .
O41 O 0.47840(13) 0.40220(11) 0.31366(10) 0.0469 1.0000 Uani . . . . . .
C42 C 0.3807(2) 0.3800(2) 0.34151(17) 0.0588 1.0000 Uani . . . . . .
C43 C 0.2979(3) 0.3814(2) 0.27866(19) 0.0723 1.0000 Uani . . . . . .
C44 C 0.1953(2) 0.3574(2) 0.3036(2) 0.0651 1.0000 Uani . . . . . .
N45 N 0.4750(2) 0.31145(14) 0.05255(13) 0.0552 1.0000 Uani . . . . . .
O46 O 0.4892(2) 0.29065(16) -0.01294(12) 0.0748 1.0000 Uani . . . . . .
O47 O 0.39293(18) 0.33550(17) 0.07228(14) 0.0753 1.0000 Uani . . . . . .
N48 N 0.88898(18) 0.53563(16) -0.09229(13) 0.0560 1.0000 Uani . . . . . .
O49 O 0.9153(2) 0.48304(16) -0.13344(12) 0.0728 1.0000 Uani . . . . . .
O50 O 0.8839(2) 0.60296(16) -0.11208(13) 0.0787 1.0000 Uani . . . . . .
N51 N 0.4009(2) 0.54415(16) 0.09713(16) 0.0631 1.0000 Uani . . . . . .
O52 O 0.4189(2) 0.54737(17) 0.03040(14) 0.0782 1.0000 Uani . . . . . .
O53 O 0.3161(2) 0.5295(3) 0.11919(19) 0.1163 1.0000 Uani . . . . . .
N54 N 0.7822(2) 0.41120(16) 0.55547(14) 0.0604 1.0000 Uani . . . . . .
O55 O 0.8377(3) 0.35465(16) 0.56653(16) 0.0905 1.0000 Uani . . . . . .
O56 O 0.7875(2) 0.46856(18) 0.59519(15) 0.0878 1.0000 Uani . . . . . .
C138 C 0.7056(7) 0.6814(5) 0.3686(6) 0.0551 0.466(10) Uani D U P 1 2 .
C139 C 0.7953(8) 0.6843(6) 0.4291(6) 0.0757 0.466(10) Uani D U P 1 2 .
C140 C 0.8982(10) 0.6886(7) 0.3967(7) 0.1007 0.466(10) Uani D U P 1 2 .
H422 H 0.3651 0.4134 0.3832 0.0695 1.0000 Uiso R . . . . .
H421 H 0.3868 0.3273 0.3604 0.0700 1.0000 Uiso R . . . . .
H431 H 0.2951 0.4350 0.2588 0.0861 1.0000 Uiso R . . . . .
H432 H 0.3153 0.3492 0.2371 0.0855 1.0000 Uiso R . . . . .
H443 H 0.1432 0.3647 0.2618 0.0953 1.0000 Uiso R . . . . .
H441 H 0.1815 0.3877 0.3490 0.0956 1.0000 Uiso R . . . . .
H442 H 0.2007 0.3032 0.3160 0.0955 1.0000 Uiso R . . . . .
H302 H 0.8522 0.1831 0.2190 0.0768 1.0000 Uiso R . . . . .
H301 H 0.8102 0.1657 0.3022 0.0777 1.0000 Uiso R . . . . .
H311 H 0.9951 0.2408 0.2764 0.1022 1.0000 Uiso R . . . . .
H312 H 0.9866 0.1541 0.3101 0.1018 1.0000 Uiso R . . . . .
H321 H 1.0367 0.2309 0.4102 0.1404 1.0000 Uiso R . . . . .
H323 H 0.9485 0.2928 0.3875 0.1402 1.0000 Uiso R . . . . .
H322 H 0.9203 0.2105 0.4174 0.1397 1.0000 Uiso R . . . . .
H121 H 0.8234 0.6266 0.0137 0.0535 1.0000 Uiso R . . . . .
H101 H 0.8945 0.4012 -0.0234 0.0538 1.0000 Uiso R . . . . .
H341 H 0.9236 0.5247 0.2588 0.0638 1.0000 Uiso R . . . . .
H342 H 0.9498 0.4334 0.2470 0.0637 1.0000 Uiso R . . . . .
H351 H 0.8125 0.4922 0.3522 0.0565 1.0000 Uiso R . . . . .
H352 H 0.8419 0.4017 0.3420 0.0560 1.0000 Uiso R . . . . .
H361 H 0.9382 0.4571 0.4506 0.0979 1.0000 Uiso R . . . . .
H362 H 0.9852 0.5181 0.3983 0.0981 1.0000 Uiso R . . . . .
H363 H 1.0117 0.4304 0.3895 0.0976 1.0000 Uiso R . . . . .
H61 H 0.6703 0.3256 0.0374 0.0556 1.0000 Uiso R . . . . .
H41 H 0.4718 0.2860 0.1985 0.0520 1.0000 Uiso R . . . . .
H241 H 0.7351 0.2980 0.4586 0.0544 1.0000 Uiso R . . . . .
H221 H 0.6654 0.5218 0.4976 0.0571 1.0000 Uiso R . . . . .
H181 H 0.3923 0.5435 0.2447 0.0566 1.0000 Uiso R . . . . .
H161 H 0.5924 0.5837 0.0844 0.0541 1.0000 Uiso R . . . . .
H381 H 0.7415 0.7140 0.2893 0.0661 0.534(10) Uiso R . P 1 1 .
H382 H 0.6823 0.7166 0.3651 0.0660 0.534(10) Uiso R . P 1 1 .
H391 H 0.8500 0.7506 0.3921 0.0891 0.534(10) Uiso R . P 1 1 .
H392 H 0.8882 0.6712 0.3569 0.0891 0.534(10) Uiso R . P 1 1 .
H403 H 0.9000 0.6705 0.4908 0.1379 0.534(10) Uiso R . P 1 1 .
H402 H 0.7810 0.6837 0.4921 0.1379 0.534(10) Uiso R . P 1 1 .
H401 H 0.8247 0.6056 0.4590 0.1380 0.534(10) Uiso R . P 1 1 .
H1381 H 0.7143 0.7233 0.3335 0.0682 0.466(10) Uiso R . P 1 2 .
H1382 H 0.6407 0.6881 0.3914 0.0681 0.466(10) Uiso R . P 1 2 .
H1391 H 0.7877 0.7298 0.4617 0.0941 0.466(10) Uiso R . P 1 2 .
H1392 H 0.7939 0.6379 0.4605 0.0942 0.466(10) Uiso R . P 1 2 .
H1401 H 0.9516 0.6798 0.4365 0.1428 0.466(10) Uiso R . P 1 2 .
H1402 H 0.9061 0.7390 0.3743 0.1430 0.466(10) Uiso R . P 1 2 .
H1403 H 0.9006 0.6491 0.3577 0.1429 0.466(10) Uiso R . P 1 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.65(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . S2 . 1.786(2) yes
C1 . C24 . 1.392(4) yes
C1 . C28 . 1.399(4) yes
S2 . C3 . 1.785(2) yes
C3 . C4 . 1.388(4) yes
C3 . C25 . 1.406(3) yes
C4 . C5 . 1.386(3) yes
C4 . H41 . 0.941 no
C5 . C6 . 1.374(4) yes
C5 . N45 . 1.467(3) yes
C6 . C7 . 1.382(4) yes
C6 . H61 . 0.939 no
C7 . S8 . 1.792(2) yes
C7 . C25 . 1.404(3) yes
S8 . C9 . 1.788(3) yes
C9 . C10 . 1.390(3) yes
C9 . C26 . 1.395(4) yes
C10 . C11 . 1.376(4) yes
C10 . H101 . 0.959 no
C11 . C12 . 1.373(4) yes
C11 . N48 . 1.468(3) yes
C12 . C13 . 1.392(3) yes
C12 . H121 . 0.959 no
C13 . S14 . 1.769(3) yes
C13 . C26 . 1.403(4) yes
S14 . C15 . 1.778(2) yes
C15 . C16 . 1.387(4) yes
C15 . C27 . 1.407(3) yes
C16 . C17 . 1.377(4) yes
C16 . H161 . 0.932 no
C17 . C18 . 1.376(4) yes
C17 . N51 . 1.472(3) yes
C18 . C19 . 1.380(4) yes
C18 . H181 . 0.947 no
C19 . S20 . 1.778(3) yes
C19 . C27 . 1.404(3) yes
S20 . C21 . 1.787(3) yes
C21 . C22 . 1.382(4) yes
C21 . C28 . 1.408(3) yes
C22 . C23 . 1.380(4) yes
C22 . H221 . 0.933 no
C23 . C24 . 1.390(4) yes
C23 . N54 . 1.467(3) yes
C24 . H241 . 0.948 no
C25 . O29 . 1.359(3) yes
C26 . O33 . 1.357(3) yes
C27 . O37 . 1.369(3) yes
C28 . O41 . 1.356(3) yes
O29 . C30 . 1.438(3) yes
C30 . C31 . 1.500(5) yes
C30 . H302 . 0.983 no
C30 . H301 . 0.987 no
C31 . C32 . 1.477(6) yes
C31 . H311 . 0.977 no
C31 . H312 . 0.981 no
C32 . H321 . 0.960 no
C32 . H323 . 0.979 no
C32 . H322 . 0.964 no
O33 . C34 . 1.460(3) yes
C34 . C35 . 1.500(3) yes
C34 . H341 . 0.980 no
C34 . H342 . 0.990 no
C35 . C36 . 1.523(4) yes
C35 . H351 . 0.986 no
C35 . H352 . 0.990 no
C36 . H361 . 0.956 no
C36 . H362 . 0.967 no
C36 . H363 . 0.961 no
O37 . C38 . 1.456(7) yes
O37 . C138 . 1.457(8) yes
C38 . C39 . 1.482(12) yes
C38 . H381 . 0.976 no
C38 . H382 . 0.966 no
C39 . C40 . 1.520(13) yes
C39 . H391 . 0.975 no
C39 . H392 . 0.977 no
C40 . H403 . 0.959 no
C40 . H402 . 0.968 no
C40 . H401 . 0.961 no
O41 . C42 . 1.450(3) yes
C42 . C43 . 1.484(4) yes
C42 . H422 . 0.962 no
C42 . H421 . 0.971 no
C43 . C44 . 1.498(4) yes
C43 . H431 . 0.989 no
C43 . H432 . 0.956 no
C44 . H443 . 0.970 no
C44 . H441 . 0.979 no
C44 . H442 . 0.962 no
N45 . O46 . 1.227(3) yes
N45 . O47 . 1.223(3) yes
N48 . O49 . 1.224(4) yes
N48 . O50 . 1.214(4) yes
N51 . O52 . 1.208(4) yes
N51 . O53 . 1.224(4) yes
N54 . O55 . 1.223(4) yes
N54 . O56 . 1.209(4) yes
C138 . C139 . 1.520(14) yes
C138 . H1381 . 0.962 no
C138 . H1382 . 0.970 no
C139 . C140 . 1.497(16) yes
C139 . H1391 . 0.980 no
C139 . H1392 . 0.973 no
C140 . H1401 . 0.960 no
C140 . H1402 . 0.964 no
C140 . H1403 . 0.966 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 . C1 . C24 . 118.38(19) yes
S2 . C1 . C28 . 120.74(19) yes
C24 . C1 . C28 . 120.7(2) yes
C1 . S2 . C3 . 101.56(10) yes
S2 . C3 . C4 . 118.47(18) yes
S2 . C3 . C25 . 121.38(19) yes
C4 . C3 . C25 . 120.1(2) yes
C3 . C4 . C5 . 118.6(2) yes
C3 . C4 . H41 . 122.3 no
C5 . C4 . H41 . 119.1 no
C4 . C5 . C6 . 122.7(2) yes
C4 . C5 . N45 . 118.8(2) yes
C6 . C5 . N45 . 118.5(2) yes
C5 . C6 . C7 . 118.6(2) yes
C5 . C6 . H61 . 120.4 no
C7 . C6 . H61 . 121.0 no
C6 . C7 . S8 . 119.54(19) yes
C6 . C7 . C25 . 120.6(2) yes
S8 . C7 . C25 . 119.8(2) yes
C7 . S8 . C9 . 98.52(11) yes
S8 . C9 . C10 . 118.8(2) yes
S8 . C9 . C26 . 120.98(18) yes
C10 . C9 . C26 . 120.2(2) yes
C9 . C10 . C11 . 119.0(2) yes
C9 . C10 . H101 . 120.2 no
C11 . C10 . H101 . 120.8 no
C10 . C11 . C12 . 122.5(2) yes
C10 . C11 . N48 . 118.8(2) yes
C12 . C11 . N48 . 118.7(2) yes
C11 . C12 . C13 . 118.7(2) yes
C11 . C12 . H121 . 121.5 no
C13 . C12 . H121 . 119.9 no
C12 . C13 . S14 . 119.4(2) yes
C12 . C13 . C26 . 120.3(2) yes
S14 . C13 . C26 . 120.21(19) yes
C13 . S14 . C15 . 100.76(11) yes
S14 . C15 . C16 . 120.43(19) yes
S14 . C15 . C27 . 119.18(18) yes
C16 . C15 . C27 . 120.3(2) yes
C15 . C16 . C17 . 118.4(2) yes
C15 . C16 . H161 . 120.8 no
C17 . C16 . H161 . 120.8 no
C16 . C17 . C18 . 122.8(2) yes
C16 . C17 . N51 . 119.2(2) yes
C18 . C17 . N51 . 118.0(2) yes
C17 . C18 . C19 . 119.1(2) yes
C17 . C18 . H181 . 120.3 no
C19 . C18 . H181 . 120.6 no
C18 . C19 . S20 . 119.01(19) yes
C18 . C19 . C27 . 120.0(2) yes
S20 . C19 . C27 . 121.00(19) yes
C19 . S20 . C21 . 99.44(11) yes
S20 . C21 . C22 . 118.31(19) yes
S20 . C21 . C28 . 121.6(2) yes
C22 . C21 . C28 . 120.0(2) yes
C21 . C22 . C23 . 119.4(2) yes
C21 . C22 . H221 . 120.5 no
C23 . C22 . H221 . 120.1 no
C22 . C23 . C24 . 122.2(2) yes
C22 . C23 . N54 . 119.0(2) yes
C24 . C23 . N54 . 118.9(2) yes
C1 . C24 . C23 . 118.2(2) yes
C1 . C24 . H241 . 120.7 no
C23 . C24 . H241 . 121.1 no
C3 . C25 . C7 . 119.1(2) yes
C3 . C25 . O29 . 120.0(2) yes
C7 . C25 . O29 . 120.8(2) yes
C13 . C26 . C9 . 119.2(2) yes
C13 . C26 . O33 . 120.1(2) yes
C9 . C26 . O33 . 120.6(2) yes
C15 . C27 . C19 . 119.3(2) yes
C15 . C27 . O37 . 120.1(2) yes
C19 . C27 . O37 . 120.4(2) yes
C21 . C28 . C1 . 119.2(2) yes
C21 . C28 . O41 . 120.1(2) yes
C1 . C28 . O41 . 120.8(2) yes
C25 . O29 . C30 . 114.7(2) yes
O29 . C30 . C31 . 109.0(3) yes
O29 . C30 . H302 . 109.2 no
C31 . C30 . H302 . 110.1 no
O29 . C30 . H301 . 108.6 no
C31 . C30 . H301 . 109.2 no
H302 . C30 . H301 . 110.6 no
C30 . C31 . C32 . 116.1(4) yes
C30 . C31 . H311 . 105.9 no
C32 . C31 . H311 . 108.0 no
C30 . C31 . H312 . 107.1 no
C32 . C31 . H312 . 108.4 no
H311 . C31 . H312 . 111.4 no
C31 . C32 . H321 . 110.3 no
C31 . C32 . H323 . 110.1 no
H321 . C32 . H323 . 111.2 no
C31 . C32 . H322 . 107.5 no
H321 . C32 . H322 . 110.0 no
H323 . C32 . H322 . 107.7 no
C26 . O33 . C34 . 112.98(17) yes
O33 . C34 . C35 . 107.9(2) yes
O33 . C34 . H341 . 108.8 no
C35 . C34 . H341 . 109.1 no
O33 . C34 . H342 . 109.1 no
C35 . C34 . H342 . 110.1 no
H341 . C34 . H342 . 111.7 no
C34 . C35 . C36 . 111.0(2) yes
C34 . C35 . H351 . 108.5 no
C36 . C35 . H351 . 109.0 no
C34 . C35 . H352 . 107.8 no
C36 . C35 . H352 . 110.0 no
H351 . C35 . H352 . 110.5 no
C35 . C36 . H361 . 111.1 no
C35 . C36 . H362 . 111.2 no
H361 . C36 . H362 . 107.5 no
C35 . C36 . H363 . 109.8 no
H361 . C36 . H363 . 108.6 no
H362 . C36 . H363 . 108.5 no
C27 . O37 . C38 . 114.0(3) yes
C27 . O37 . C138 . 116.7(4) yes
O37 . C38 . C39 . 108.8(6) yes
O37 . C38 . H381 . 108.6 no
C39 . C38 . H381 . 108.3 no
O37 . C38 . H382 . 111.8 no
C39 . C38 . H382 . 109.9 no
H381 . C38 . H382 . 109.4 no
C38 . C39 . C40 . 113.8(10) yes
C38 . C39 . H391 . 107.6 no
C40 . C39 . H391 . 106.3 no
C38 . C39 . H392 . 109.8 no
C40 . C39 . H392 . 109.2 no
H391 . C39 . H392 . 110.0 no
C39 . C40 . H403 . 108.1 no
C39 . C40 . H402 . 110.2 no
H403 . C40 . H402 . 109.4 no
C39 . C40 . H401 . 108.6 no
H403 . C40 . H401 . 109.4 no
H402 . C40 . H401 . 111.1 no
C28 . O41 . C42 . 113.53(19) yes
O41 . C42 . C43 . 111.0(2) yes
O41 . C42 . H422 . 109.6 no
C43 . C42 . H422 . 111.5 no
O41 . C42 . H421 . 108.1 no
C43 . C42 . H421 . 107.7 no
H422 . C42 . H421 . 108.8 no
C42 . C43 . C44 . 113.5(3) yes
C42 . C43 . H431 . 106.3 no
C44 . C43 . H431 . 110.6 no
C42 . C43 . H432 . 110.6 no
C44 . C43 . H432 . 109.1 no
H431 . C43 . H432 . 106.5 no
C43 . C44 . H443 . 109.7 no
C43 . C44 . H441 . 108.0 no
H443 . C44 . H441 . 112.4 no
C43 . C44 . H442 . 106.5 no
H443 . C44 . H442 . 109.4 no
H441 . C44 . H442 . 110.6 no
C5 . N45 . O46 . 117.8(2) yes
C5 . N45 . O47 . 118.2(2) yes
O46 . N45 . O47 . 124.0(3) yes
C11 . N48 . O49 . 118.2(2) yes
C11 . N48 . O50 . 118.0(3) yes
O49 . N48 . O50 . 123.8(2) yes
C17 . N51 . O52 . 119.7(3) yes
C17 . N51 . O53 . 116.3(3) yes
O52 . N51 . O53 . 123.9(3) yes
C23 . N54 . O55 . 117.9(2) yes
C23 . N54 . O56 . 118.2(3) yes
O55 . N54 . O56 . 123.8(3) yes
O37 . C138 . C139 . 108.7(6) yes
O37 . C138 . H1381 . 108.9 no
C139 . C138 . H1381 . 107.3 no
O37 . C138 . H1382 . 111.8 no
C139 . C138 . H1382 . 111.3 no
H1381 . C138 . H1382 . 108.7 no
C138 . C139 . C140 . 113.9(11) yes
C138 . C139 . H1391 . 109.0 no
C140 . C139 . H1391 . 108.2 no
C138 . C139 . H1392 . 108.6 no
C140 . C139 . H1392 . 108.0 no
H1391 . C139 . H1392 . 109.0 no
C139 . C140 . H1401 . 110.1 no
C139 . C140 . H1402 . 108.9 no
H1401 . C140 . H1402 . 110.0 no
C139 . C140 . H1403 . 108.0 no
H1401 . C140 . H1403 . 109.9 no
H1402 . C140 . H1403 . 109.9 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C35 . H351 . O37 . 153 0.986 2.438 3.346(5) yes
C35 . H352 . O29 . 147 0.990 2.511 3.396(5) yes
C38 . H382 . O47 3_655 153 0.966 2.558 3.448(5) yes
C39 . H391 . O50 4_565 171 0.975 2.571 3.537(5) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/10/14 at 13:03:13
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 323,X'S) H   ( 322,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 422,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 443,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) H   (1382,X'S) 
RIDE C   ( 139,X'S) H   (1391,X'S) H   (1392,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) H   (1402,X'S) H   (1403,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 17/10/14 at 13:03:13
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.441000 , 0.050000 = O(37) TO C(38) 
DISTANCE 1.525000 , 0.050000 = C(38) TO C(39) 
DISTANCE 1.539000 , 0.050000 = C(39) TO C(40) 
DISTANCE 2.372000 , 0.050000 = O(37) TO C(39) 
DISTANCE 2.531000 , 0.050000 = C(38) TO C(40) 
DISTANCE 1.441000 , 0.050000 = O(37) TO C(138) 
DISTANCE 1.525000 , 0.050000 = C(138) TO C(139) 
DISTANCE 1.539000 , 0.050000 = C(139) TO C(140) 
DISTANCE 2.372000 , 0.050000 = O(37) TO C(139) 
DISTANCE 2.531000 , 0.050000 = C(138) TO C(140) 
U(IJ)'S  0.0, 0.010000 = C(38) TO C(138) 
U(IJ)'S  0.0, 0.010000 = C(39) TO C(139) 
U(IJ)'S  0.0, 0.010000 = C(40) TO C(140) 
END                                                                             
;
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_4c
_database_code_depnum_ccdc_archive 'CCDC 1030571'
_audit_update_record             
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
_cell_length_a                   11.0672(8)
_cell_length_b                   12.3077(11)
_cell_length_c                   18.3099(11)
_cell_angle_alpha                101.125(7)
_cell_angle_beta                 95.076(6)
_cell_angle_gamma                102.421(7)
_cell_volume                     2367.8(3)

_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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2


_chemical_formula_sum            'C44 H52 N4 O12 S4'
_chemical_formula_moiety         'C44 H52 N4 O12 S4'
_chemical_compound_source        ?
_chemical_formula_weight         957.18


_cell_measurement_reflns_used    9783
_cell_measurement_theta_min      5
_cell_measurement_theta_max      76
_cell_measurement_temperature    170

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.230
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_max          0.460

_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    2.383

# Sheldrick geometric approximatio 0.50 0.58 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.58
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      170
_diffrn_ambient_pressure         101
_diffrn_reflns_number            25548
_reflns_number_total             9372
_diffrn_reflns_av_R_equivalents  0.039
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9372 
# Theoretical number of reflections is about 19833 


_diffrn_reflns_theta_min         4.521
_diffrn_reflns_theta_max         76.222
_diffrn_measured_fraction_theta_max 0.947

_diffrn_reflns_theta_full        67.68
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              -15
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   3.75
_oxford_diffrn_Wilson_scale      0.05

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.42
_refine_diff_density_max         0.56


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         8878
_refine_ls_number_restraints     219
_refine_ls_number_parameters     697
_oxford_refine_ls_R_factor_ref   0.0709
_refine_ls_wR_factor_ref         0.1960
_refine_ls_goodness_of_fit_ref   0.9210
_refine_ls_shift/su_max          0.0020363
_refine_ls_shift/su_mean         0.0000763


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9372
_refine_ls_R_factor_all          0.0745
_refine_ls_wR_factor_all         0.2130

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7463
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_gt          0.1779

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.394E+04 0.668E+04 0.417E+04 0.178E+04 409. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.5511(3) 0.5888(3) 0.19606(15) 0.0469 1.0000 Uani . . . . . .
S2 S 0.60256(7) 0.53707(8) 0.27395(4) 0.0570 1.0000 Uani . . . . . .
C3 C 0.4988(2) 0.5590(3) 0.34059(15) 0.0446 1.0000 Uani . . . . . .
C4 C 0.4472(3) 0.4652(2) 0.36985(15) 0.0447 1.0000 Uani . . . . . .
C5 C 0.3772(3) 0.4829(2) 0.42810(15) 0.0428 1.0000 Uani . . . . . .
C6 C 0.3517(3) 0.5874(2) 0.45617(15) 0.0449 1.0000 Uani . . . . . .
C7 C 0.4025(3) 0.6789(2) 0.42573(15) 0.0445 1.0000 Uani . . . . . .
S8 S 0.37691(8) 0.81353(6) 0.46787(4) 0.0540 1.0000 Uani . . . . . .
C9 C 0.3262(3) 0.8671(2) 0.39084(15) 0.0449 1.0000 Uani . . . . . .
C10 C 0.3931(3) 0.9740(2) 0.38332(15) 0.0460 1.0000 Uani . . . . . .
C11 C 0.3479(3) 1.0235(2) 0.32955(16) 0.0458 1.0000 Uani . . . . . .
C12 C 0.2383(3) 0.9712(2) 0.28089(15) 0.0479 1.0000 Uani . . . . . .
C13 C 0.1738(3) 0.8646(2) 0.28704(15) 0.0462 1.0000 Uani . . . . . .
S14 S 0.02893(7) 0.80516(6) 0.22832(5) 0.0556 1.0000 Uani . . . . . .
C15 C 0.0429(3) 0.6712(2) 0.17759(15) 0.0455 1.0000 Uani . . . . . .
C16 C -0.0575(3) 0.5793(3) 0.17302(16) 0.0475 1.0000 Uani . . . . . .
C17 C -0.0592(3) 0.4761(2) 0.12744(15) 0.0458 1.0000 Uani . . . . . .
C18 C 0.0373(3) 0.4585(2) 0.08762(14) 0.0438 1.0000 Uani . . . . . .
C19 C 0.1391(3) 0.5496(2) 0.09249(14) 0.0439 1.0000 Uani . . . . . .
S20 S 0.25230(7) 0.52650(7) 0.03287(4) 0.0499 1.0000 Uani . . . . . .
C21 C 0.3997(3) 0.5806(2) 0.09017(15) 0.0449 1.0000 Uani . . . . . .
C22 C 0.4913(3) 0.6447(2) 0.05849(15) 0.0472 1.0000 Uani . . . . . .
C23 C 0.6106(3) 0.6806(2) 0.09646(16) 0.0471 1.0000 Uani . . . . . .
C24 C 0.6418(3) 0.6553(3) 0.16547(16) 0.0489 1.0000 Uani . . . . . .
C25 C 0.4798(3) 0.6667(2) 0.36979(15) 0.0457 1.0000 Uani . . . . . .
C26 C 0.2155(3) 0.8110(2) 0.34188(15) 0.0437 1.0000 Uani . . . . . .
C27 C 0.1410(3) 0.6577(2) 0.13609(16) 0.0467 1.0000 Uani . . . . . .
C28 C 0.4281(3) 0.5504(2) 0.15836(15) 0.0435 1.0000 Uani . . . . . .
O29 O 0.5352(2) 0.75842(18) 0.34278(12) 0.0541 1.0000 Uani . . . . . .
C30 C 0.6557(3) 0.8181(3) 0.3872(2) 0.0726 1.0000 Uani . . . . . .
C31 C 0.7191(4) 0.9089(3) 0.3494(3) 0.0762 1.0000 Uani . . . . . .
C32 C 0.8458(4) 0.9768(4) 0.3956(3) 0.0824 1.0000 Uani . . . . . .
C33 C 0.9223(5) 1.0545(4) 0.3565(3) 0.0940 1.0000 Uani . . . . . .
C34 C 1.0448(5) 1.1208(5) 0.4044(3) 0.1054 1.0000 Uani . . . . . .
O35 O 0.15206(19) 0.70572(16) 0.34666(11) 0.0506 1.0000 Uani D U . . . .
C36 C 0.0731(7) 0.7009(6) 0.4055(4) 0.0707 0.610(5) Uani D U P 2 1 .
C37 C -0.0282(5) 0.5909(5) 0.3797(4) 0.0718 0.610(5) Uani D U P 2 1 .
C38 C 0.0251(5) 0.4849(4) 0.3646(4) 0.0764 0.610(5) Uani D U P 2 1 .
C39 C -0.0735(6) 0.3749(5) 0.3271(4) 0.0861 0.610(5) Uani D U P 2 1 .
C40 C -0.1823(7) 0.3466(6) 0.3716(4) 0.0792 0.610(5) Uani D U P 2 1 .
O41 O 0.2394(2) 0.74836(19) 0.13757(13) 0.0617 1.0000 Uani D U . . . .
C42 C 0.2113(4) 0.8208(4) 0.0876(3) 0.0732 0.811(5) Uani D U P 3 1 .
C43 C 0.3280(4) 0.8919(5) 0.0675(3) 0.0824 0.811(5) Uani D U P 3 1 .
C44 C 0.4276(5) 0.9559(5) 0.1327(3) 0.0892 0.811(5) Uani D U P 3 1 .
C45 C 0.5410(5) 1.0296(5) 0.1099(3) 0.0938 0.811(5) Uani D U P 3 1 .
C46 C 0.6346(7) 1.0965(6) 0.1779(4) 0.1127 0.811(5) Uani D U P 3 1 .
O47 O 0.33874(19) 0.48995(17) 0.19093(11) 0.0490 1.0000 Uani D U . . . .
C48 C 0.3079(3) 0.3677(2) 0.16141(19) 0.0584 1.0000 Uani D U . . . .
C49 C 0.1975(3) 0.3145(2) 0.19700(18) 0.0577 1.0000 Uani D U . . . .
C50 C 0.1326(4) 0.1990(3) 0.1459(3) 0.0601 0.727(5) Uani D U P 1 1 .
C51 C 0.0230(4) 0.1414(4) 0.1810(3) 0.0710 0.727(5) Uani D U P 1 1 .
C52 C -0.0539(7) 0.0337(5) 0.1253(5) 0.1007 0.727(5) Uani D U P 1 1 .
N53 N 0.3254(2) 0.3860(2) 0.46178(14) 0.0495 1.0000 Uani . . . . . .
O54 O 0.2631(3) 0.4018(2) 0.51232(17) 0.0736 1.0000 Uani . . . . . .
O55 O 0.3492(3) 0.2942(2) 0.43839(16) 0.0734 1.0000 Uani . . . . . .
N56 N 0.4204(3) 1.1353(2) 0.32188(15) 0.0530 1.0000 Uani . . . . . .
O57 O 0.3736(3) 1.18261(19) 0.27772(14) 0.0698 1.0000 Uani . . . . . .
O58 O 0.5229(2) 1.1739(2) 0.35888(15) 0.0662 1.0000 Uani . . . . . .
N59 N -0.1671(3) 0.3812(2) 0.12202(15) 0.0574 1.0000 Uani . . . . . .
O60 O -0.1609(3) 0.2860(2) 0.08981(17) 0.0784 1.0000 Uani . . . . . .
O61 O -0.2605(3) 0.4026(2) 0.14797(17) 0.0781 1.0000 Uani . . . . . .
N62 N 0.7086(3) 0.7478(2) 0.06347(14) 0.0528 1.0000 Uani . . . . . .
O63 O 0.8174(2) 0.7614(2) 0.09017(16) 0.0715 1.0000 Uani . . . . . .
O64 O 0.6765(3) 0.7856(2) 0.00941(14) 0.0695 1.0000 Uani . . . . . .
C136 C 0.0508(11) 0.7075(8) 0.3914(8) 0.0708 0.390(5) Uani D U P 2 2 .
C137 C 0.0205(10) 0.5947(8) 0.4166(5) 0.0717 0.390(5) Uani D U P 2 2 .
C138 C -0.0487(10) 0.5014(7) 0.3491(5) 0.0767 0.390(5) Uani D U P 2 2 .
C139 C -0.0929(14) 0.3909(8) 0.3764(6) 0.0973 0.390(5) Uani D U P 2 2 .
C140 C -0.1907(14) 0.3106(11) 0.3135(9) 0.1123 0.390(5) Uani D U P 2 2 .
C142 C 0.2683(16) 0.8217(17) 0.0867(10) 0.0737 0.189(5) Uani D U P 3 2 .
C143 C 0.3984(15) 0.8916(15) 0.1210(14) 0.0826 0.189(5) Uani D U P 3 2 .
C144 C 0.4174(17) 1.0045(14) 0.0951(13) 0.0895 0.189(5) Uani D U P 3 2 .
C145 C 0.5395(19) 1.0854(15) 0.1381(14) 0.0941 0.189(5) Uani D U P 3 2 .
C146 C 0.6510(19) 1.029(2) 0.1373(17) 0.1128 0.189(5) Uani D U P 3 2 .
C150 C 0.1468(13) 0.1848(5) 0.1673(7) 0.0600 0.273(5) Uani D U P 1 2 .
C151 C 0.0465(12) 0.1571(8) 0.0983(7) 0.0710 0.273(5) Uani D U P 1 2 .
C152 C -0.0079(18) 0.0273(9) 0.0706(12) 0.1008 0.273(5) Uani D U P 1 2 .
H121 H 0.2099 1.0089 0.2444 0.0581 1.0000 Uiso R . . . . .
H101 H 0.4660 1.0095 0.4149 0.0568 1.0000 Uiso R . . . . .
H241 H 0.7195 0.6820 0.1923 0.0573 1.0000 Uiso R . . . . .
H221 H 0.4698 0.6607 0.0138 0.0557 1.0000 Uiso R . . . . .
H41 H 0.4558 0.3912 0.3510 0.0532 1.0000 Uiso R . . . . .
H61 H 0.2975 0.5915 0.4942 0.0548 1.0000 Uiso R . . . . .
H161 H -0.1259 0.5852 0.2018 0.0549 1.0000 Uiso R . . . . .
H181 H 0.0313 0.3851 0.0588 0.0533 1.0000 Uiso R . . . . .
H482 H 0.3779 0.3374 0.1765 0.0708 1.0000 Uiso R . . . . .
H481 H 0.2928 0.3511 0.1071 0.0719 1.0000 Uiso R . . . . .
H501 H 0.1897 0.1479 0.1423 0.0718 0.727(5) Uiso R . P 1 1 .
H502 H 0.1035 0.2047 0.0956 0.0717 0.727(5) Uiso R . P 1 1 .
H511 H 0.0532 0.1215 0.2259 0.0805 0.727(5) Uiso R . P 1 1 .
H512 H -0.0305 0.1923 0.1936 0.0804 0.727(5) Uiso R . P 1 1 .
H521 H -0.1217 0.0005 0.1468 0.1371 0.727(5) Uiso R . P 1 1 .
H522 H -0.0010 -0.0184 0.1138 0.1368 0.727(5) Uiso R . P 1 1 .
H523 H -0.0825 0.0534 0.0794 0.1367 0.727(5) Uiso R . P 1 1 .
H1502 H 0.0990 0.1585 0.2060 0.0720 0.273(5) Uiso R . P 1 2 .
H1501 H 0.2104 0.1424 0.1588 0.0720 0.273(5) Uiso R . P 1 2 .
H1511 H -0.0202 0.1960 0.1063 0.0881 0.273(5) Uiso R . P 1 2 .
H1512 H 0.0904 0.1818 0.0591 0.0880 0.273(5) Uiso R . P 1 2 .
H1522 H -0.0737 0.0159 0.0300 0.1500 0.273(5) Uiso R . P 1 2 .
H1523 H -0.0396 -0.0023 0.1114 0.1500 0.273(5) Uiso R . P 1 2 .
H1521 H 0.0560 -0.0093 0.0532 0.1499 0.273(5) Uiso R . P 1 2 .
H362 H 0.0302 0.7624 0.4076 0.0855 0.610(5) Uiso R . P 2 1 .
H361 H 0.1152 0.7027 0.4551 0.0853 0.610(5) Uiso R . P 2 1 .
H372 H -0.0731 0.5863 0.4231 0.0958 0.610(5) Uiso R . P 2 1 .
H371 H -0.0866 0.5900 0.3358 0.0963 0.610(5) Uiso R . P 2 1 .
H381 H 0.0584 0.4738 0.4134 0.0961 0.610(5) Uiso R . P 2 1 .
H382 H 0.0873 0.4933 0.3306 0.0959 0.610(5) Uiso R . P 2 1 .
H391 H -0.1048 0.3814 0.2767 0.1112 0.610(5) Uiso R . P 2 1 .
H392 H -0.0316 0.3111 0.3233 0.1107 0.610(5) Uiso R . P 2 1 .
H403 H -0.2402 0.2816 0.3424 0.1290 0.610(5) Uiso R . P 2 1 .
H401 H -0.2140 0.4145 0.3785 0.1290 0.610(5) Uiso R . P 2 1 .
H402 H -0.1443 0.3350 0.4185 0.1291 0.610(5) Uiso R . P 2 1 .
H1361 H 0.0745 0.7711 0.4347 0.0851 0.390(5) Uiso R . P 2 2 .
H1362 H -0.0238 0.7127 0.3610 0.0850 0.390(5) Uiso R . P 2 2 .
H1372 H -0.0298 0.6021 0.4568 0.0947 0.390(5) Uiso R . P 2 2 .
H1371 H 0.0952 0.5752 0.4345 0.0948 0.390(5) Uiso R . P 2 2 .
H1382 H -0.1205 0.5258 0.3295 0.0949 0.390(5) Uiso R . P 2 2 .
H1381 H 0.0015 0.4877 0.3098 0.0947 0.390(5) Uiso R . P 2 2 .
H1392 H -0.1331 0.4063 0.4203 0.0991 0.390(5) Uiso R . P 2 2 .
H1391 H -0.0217 0.3600 0.3885 0.0988 0.390(5) Uiso R . P 2 2 .
H302 H 0.6409 0.8528 0.4370 0.0845 1.0000 Uiso R . . . . .
H301 H 0.7067 0.7622 0.3895 0.0844 1.0000 Uiso R . . . . .
H311 H 0.6641 0.9568 0.3422 0.0897 1.0000 Uiso R . . . . .
H312 H 0.7272 0.8652 0.3009 0.0903 1.0000 Uiso R . . . . .
H321 H 0.8330 1.0235 0.4424 0.0996 1.0000 Uiso R . . . . .
H322 H 0.8955 0.9220 0.4048 0.0995 1.0000 Uiso R . . . . .
H331 H 0.8757 1.1113 0.3467 0.1112 1.0000 Uiso R . . . . .
H332 H 0.9443 1.0147 0.3067 0.1102 1.0000 Uiso R . . . . .
H341 H 1.0979 1.1647 0.3729 0.1556 1.0000 Uiso R . . . . .
H343 H 1.0300 1.1727 0.4468 0.1563 1.0000 Uiso R . . . . .
H342 H 1.0853 1.0676 0.4220 0.1559 1.0000 Uiso R . . . . .
H421 H 0.1616 0.8714 0.1148 0.0835 0.811(5) Uiso R . P 3 1 .
H422 H 0.1620 0.7767 0.0409 0.0829 0.811(5) Uiso R . P 3 1 .
H431 H 0.3048 0.9499 0.0462 0.0940 0.811(5) Uiso R . P 3 1 .
H432 H 0.3616 0.8409 0.0320 0.0946 0.811(5) Uiso R . P 3 1 .
H442 H 0.3875 1.0011 0.1702 0.1124 0.811(5) Uiso R . P 3 1 .
H441 H 0.4501 0.8982 0.1556 0.1121 0.811(5) Uiso R . P 3 1 .
H452 H 0.5128 1.0668 0.0713 0.1176 0.811(5) Uiso R . P 3 1 .
H451 H 0.5939 0.9777 0.0925 0.1176 0.811(5) Uiso R . P 3 1 .
H1422 H 0.2161 0.8810 0.1008 0.0842 0.189(5) Uiso R . P 3 2 .
H1421 H 0.2479 0.7888 0.0350 0.0840 0.189(5) Uiso R . P 3 2 .
H1431 H 0.4199 0.8711 0.1687 0.0950 0.189(5) Uiso R . P 3 2 .
H1432 H 0.4467 0.8596 0.0833 0.0948 0.189(5) Uiso R . P 3 2 .
H1441 H 0.4173 1.0363 0.1514 0.1131 0.189(5) Uiso R . P 3 2 .
H1442 H 0.3554 1.0170 0.0666 0.1130 0.189(5) Uiso R . P 3 2 .
H1451 H 0.5462 1.1530 0.1255 0.1170 0.189(5) Uiso R . P 3 2 .
H1452 H 0.5536 1.0248 0.0936 0.1172 0.189(5) Uiso R . P 3 2 .
H1401 H -0.2204 0.2411 0.3287 0.1243 0.390(5) Uiso R . P 2 2 .
H1403 H -0.2591 0.3417 0.3008 0.1243 0.390(5) Uiso R . P 2 2 .
H1402 H -0.1483 0.2964 0.2710 0.1243 0.390(5) Uiso R . P 2 2 .
H1462 H 0.7291 1.0624 0.1237 0.1368 0.189(5) Uiso R . P 3 2 .
H1461 H 0.6457 1.0640 0.1875 0.1368 0.189(5) Uiso R . P 3 2 .
H1463 H 0.6438 0.9497 0.1334 0.1368 0.189(5) Uiso R . P 3 2 .
H461 H 0.7057 1.1369 0.1606 0.1367 0.811(5) Uiso R . P 3 1 .
H463 H 0.5932 1.1492 0.2037 0.1367 0.811(5) Uiso R . P 3 1 .
H462 H 0.6604 1.0526 0.2110 0.1367 0.811(5) Uiso R . P 3 1 .
H493 H 0.2240 0.3285 0.2494 0.0673 0.273(5) Uiso R . P 1 2 .
H492 H 0.1336 0.3529 0.1883 0.0673 0.273(5) Uiso R . P 1 2 .
H491 H 0.2256 0.3035 0.2450 0.0673 0.727(5) Uiso R . P 1 1 .
H494 H 0.1408 0.3627 0.2023 0.0673 0.727(5) Uiso R . P 1 1 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.81(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . S2 . 1.768(3) yes
C1 . C24 . 1.383(4) yes
C1 . C28 . 1.408(4) yes
S2 . C3 . 1.770(3) yes
C3 . C4 . 1.399(4) yes
C3 . C25 . 1.398(4) yes
C4 . C5 . 1.384(4) yes
C4 . H41 . 0.938 no
C5 . C6 . 1.386(4) yes
C5 . N53 . 1.478(3) yes
C6 . C7 . 1.386(4) yes
C6 . H61 . 0.959 no
C7 . S8 . 1.780(3) yes
C7 . C25 . 1.398(4) yes
S8 . C9 . 1.766(3) yes
C9 . C10 . 1.403(4) yes
C9 . C26 . 1.409(4) yes
C10 . C11 . 1.366(4) yes
C10 . H101 . 0.919 no
C11 . C12 . 1.390(4) yes
C11 . N56 . 1.475(4) yes
C12 . C13 . 1.383(4) yes
C12 . H121 . 0.952 no
C13 . S14 . 1.774(3) yes
C13 . C26 . 1.400(4) yes
S14 . C15 . 1.774(3) yes
C15 . C16 . 1.388(4) yes
C15 . C27 . 1.400(4) yes
C16 . C17 . 1.375(4) yes
C16 . H161 . 0.967 no
C17 . C18 . 1.377(4) yes
C17 . N59 . 1.460(4) yes
C18 . C19 . 1.392(4) yes
C18 . H181 . 0.940 no
C19 . S20 . 1.765(3) yes
C19 . C27 . 1.408(4) yes
S20 . C21 . 1.779(3) yes
C21 . C22 . 1.387(4) yes
C21 . C28 . 1.399(4) yes
C22 . C23 . 1.375(4) yes
C22 . H221 . 0.901 no
C23 . C24 . 1.391(4) yes
C23 . N62 . 1.465(4) yes
C24 . H241 . 0.911 no
C25 . O29 . 1.365(3) yes
C26 . O35 . 1.358(3) yes
C27 . O41 . 1.375(3) yes
C28 . O47 . 1.359(3) yes
O29 . C30 . 1.462(4) yes
C30 . C31 . 1.506(5) yes
C30 . H302 . 0.973 no
C30 . H301 . 0.984 no
C31 . C32 . 1.547(6) yes
C31 . H311 . 0.953 no
C31 . H312 . 0.969 no
C32 . C33 . 1.473(6) yes
C32 . H321 . 0.975 no
C32 . H322 . 0.987 no
C33 . C34 . 1.520(7) yes
C33 . H331 . 0.987 no
C33 . H332 . 1.023 no
C34 . H341 . 1.007 no
C34 . H343 . 0.956 no
C34 . H342 . 0.957 no
O35 . C36 . 1.449(4) yes
O35 . C136 . 1.447(5) yes
C36 . C37 . 1.524(5) yes
C36 . H362 . 0.974 no
C36 . H361 . 0.977 no
C37 . C38 . 1.532(5) yes
C37 . H372 . 0.978 no
C37 . H371 . 0.983 no
C38 . C39 . 1.538(4) yes
C38 . H381 . 0.981 no
C38 . H382 . 0.971 no
C39 . C40 . 1.528(5) yes
C39 . H391 . 0.981 no
C39 . H392 . 0.988 no
C40 . H403 . 0.944 no
C40 . H401 . 0.965 no
C40 . H402 . 0.971 no
O41 . C42 . 1.454(4) yes
O41 . C142 . 1.428(5) yes
C42 . C43 . 1.513(4) yes
C42 . H421 . 1.008 no
C42 . H422 . 0.966 no
C43 . C44 . 1.514(4) yes
C43 . H431 . 0.947 no
C43 . H432 . 0.970 no
C44 . C45 . 1.523(4) yes
C44 . H442 . 0.995 no
C44 . H441 . 0.957 no
C45 . C46 . 1.520(4) yes
C45 . H452 . 0.977 no
C45 . H451 . 0.984 no
C46 . H461 . 0.950 no
C46 . H463 . 0.950 no
C46 . H462 . 0.950 no
O47 . C48 . 1.451(3) yes
C48 . C49 . 1.519(3) yes
C48 . H482 . 0.970 no
C48 . H481 . 0.968 no
C49 . C50 . 1.530(4) yes
C49 . H491 . 0.950 no
C49 . H494 . 0.950 no
C49 . C150 . 1.544(5) yes
C49 . H493 . 0.950 no
C49 . H492 . 0.950 no
C50 . C51 . 1.527(4) yes
C50 . H501 . 0.981 no
C50 . H502 . 0.969 no
C51 . C52 . 1.536(4) yes
C51 . H511 . 0.955 no
C51 . H512 . 0.962 no
C52 . H521 . 0.932 no
C52 . H522 . 0.964 no
C52 . H523 . 0.965 no
N53 . O54 . 1.213(4) yes
N53 . O55 . 1.221(3) yes
N56 . O57 . 1.224(3) yes
N56 . O58 . 1.216(4) yes
N59 . O60 . 1.225(4) yes
N59 . O61 . 1.233(4) yes
N62 . O63 . 1.223(4) yes
N62 . O64 . 1.228(3) yes
C136 . C137 . 1.525(5) yes
C136 . H1361 . 0.972 no
C136 . H1362 . 0.976 no
C137 . C138 . 1.529(5) yes
C137 . H1372 . 0.964 no
C137 . H1371 . 0.957 no
C138 . C139 . 1.535(5) yes
C138 . H1382 . 0.972 no
C138 . H1381 . 0.959 no
C139 . C140 . 1.534(5) yes
C139 . H1392 . 0.961 no
C139 . H1391 . 0.972 no
C140 . H1401 . 0.950 no
C140 . H1403 . 0.950 no
C140 . H1402 . 0.950 no
C142 . C143 . 1.519(5) yes
C142 . H1422 . 1.033 no
C142 . H1421 . 0.941 no
C143 . C144 . 1.531(5) yes
C143 . H1431 . 0.979 no
C143 . H1432 . 0.984 no
C144 . C145 . 1.539(5) yes
C144 . H1441 . 1.030 no
C144 . H1442 . 0.884 no
C145 . C146 . 1.540(5) yes
C145 . H1451 . 0.896 no
C145 . H1452 . 1.040 no
C146 . H1452 . 1.269 no
C146 . H1462 . 0.950 no
C146 . H1461 . 0.950 no
C146 . H1463 . 0.950 no
C150 . C151 . 1.539(5) yes
C150 . H1502 . 0.983 no
C150 . H1501 . 0.968 no
C151 . C152 . 1.546(5) yes
C151 . H1511 . 0.970 no
C151 . H1512 . 0.963 no
C152 . H1522 . 0.961 no
C152 . H1523 . 0.954 no
C152 . H1521 . 0.963 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 . C1 . C24 . 116.8(2) yes
S2 . C1 . C28 . 122.4(2) yes
C24 . C1 . C28 . 120.0(2) yes
C1 . S2 . C3 . 106.39(13) yes
S2 . C3 . C4 . 116.5(2) yes
S2 . C3 . C25 . 122.5(2) yes
C4 . C3 . C25 . 120.6(3) yes
C3 . C4 . C5 . 117.8(3) yes
C3 . C4 . H41 . 123.2 no
C5 . C4 . H41 . 119.0 no
C4 . C5 . C6 . 123.2(2) yes
C4 . C5 . N53 . 118.8(2) yes
C6 . C5 . N53 . 118.0(2) yes
C5 . C6 . C7 . 118.1(3) yes
C5 . C6 . H61 . 118.2 no
C7 . C6 . H61 . 123.7 no
C6 . C7 . S8 . 116.6(2) yes
C6 . C7 . C25 . 120.8(3) yes
S8 . C7 . C25 . 122.3(2) yes
C7 . S8 . C9 . 103.99(12) yes
S8 . C9 . C10 . 118.0(2) yes
S8 . C9 . C26 . 121.9(2) yes
C10 . C9 . C26 . 119.8(2) yes
C9 . C10 . C11 . 119.2(3) yes
C9 . C10 . H101 . 119.4 no
C11 . C10 . H101 . 121.4 no
C10 . C11 . C12 . 122.5(3) yes
C10 . C11 . N56 . 118.4(3) yes
C12 . C11 . N56 . 119.1(2) yes
C11 . C12 . C13 . 118.4(2) yes
C11 . C12 . H121 . 119.7 no
C13 . C12 . H121 . 121.9 no
C12 . C13 . S14 . 116.9(2) yes
C12 . C13 . C26 . 121.3(2) yes
S14 . C13 . C26 . 121.6(2) yes
C13 . S14 . C15 . 105.13(12) yes
S14 . C15 . C16 . 116.4(2) yes
S14 . C15 . C27 . 123.4(2) yes
C16 . C15 . C27 . 119.8(3) yes
C15 . C16 . C17 . 119.3(3) yes
C15 . C16 . H161 . 121.9 no
C17 . C16 . H161 . 118.7 no
C16 . C17 . C18 . 122.5(3) yes
C16 . C17 . N59 . 118.5(3) yes
C18 . C17 . N59 . 119.0(3) yes
C17 . C18 . C19 . 118.6(2) yes
C17 . C18 . H181 . 118.2 no
C19 . C18 . H181 . 123.2 no
C18 . C19 . S20 . 116.7(2) yes
C18 . C19 . C27 . 120.1(3) yes
S20 . C19 . C27 . 122.7(2) yes
C19 . S20 . C21 . 106.04(12) yes
S20 . C21 . C22 . 115.3(2) yes
S20 . C21 . C28 . 123.3(2) yes
C22 . C21 . C28 . 121.0(3) yes
C21 . C22 . C23 . 118.6(3) yes
C21 . C22 . H221 . 118.4 no
C23 . C22 . H221 . 123.0 no
C22 . C23 . C24 . 122.1(3) yes
C22 . C23 . N62 . 119.2(3) yes
C24 . C23 . N62 . 118.7(3) yes
C23 . C24 . C1 . 119.2(3) yes
C23 . C24 . H241 . 122.8 no
C1 . C24 . H241 . 118.0 no
C7 . C25 . C3 . 119.4(2) yes
C7 . C25 . O29 . 120.7(3) yes
C3 . C25 . O29 . 119.9(3) yes
C9 . C26 . C13 . 118.8(2) yes
C9 . C26 . O35 . 120.5(2) yes
C13 . C26 . O35 . 120.6(2) yes
C19 . C27 . C15 . 119.5(3) yes
C19 . C27 . O41 . 119.6(3) yes
C15 . C27 . O41 . 120.9(2) yes
C1 . C28 . C21 . 119.1(3) yes
C1 . C28 . O47 . 119.3(2) yes
C21 . C28 . O47 . 121.6(2) yes
C25 . O29 . C30 . 111.5(2) yes
O29 . C30 . C31 . 109.0(3) yes
O29 . C30 . H302 . 108.4 no
C31 . C30 . H302 . 109.9 no
O29 . C30 . H301 . 108.1 no
C31 . C30 . H301 . 109.8 no
H302 . C30 . H301 . 111.6 no
C30 . C31 . C32 . 110.9(4) yes
C30 . C31 . H311 . 108.7 no
C32 . C31 . H311 . 112.1 no
C30 . C31 . H312 . 102.6 no
C32 . C31 . H312 . 113.4 no
H311 . C31 . H312 . 108.7 no
C31 . C32 . C33 . 113.9(4) yes
C31 . C32 . H321 . 110.6 no
C33 . C32 . H321 . 106.7 no
C31 . C32 . H322 . 108.1 no
C33 . C32 . H322 . 105.6 no
H321 . C32 . H322 . 111.8 no
C32 . C33 . C34 . 112.1(5) yes
C32 . C33 . H331 . 107.9 no
C34 . C33 . H331 . 106.6 no
C32 . C33 . H332 . 114.1 no
C34 . C33 . H332 . 106.9 no
H331 . C33 . H332 . 109.0 no
C33 . C34 . H341 . 108.7 no
C33 . C34 . H343 . 110.6 no
H341 . C34 . H343 . 109.4 no
C33 . C34 . H342 . 108.2 no
H341 . C34 . H342 . 111.1 no
H343 . C34 . H342 . 108.8 no
C26 . O35 . C36 . 116.5(3) yes
C26 . O35 . C136 . 113.6(4) yes
O35 . C36 . C37 . 106.5(4) yes
O35 . C36 . H362 . 108.1 no
C37 . C36 . H362 . 105.8 no
O35 . C36 . H361 . 115.7 no
C37 . C36 . H361 . 109.3 no
H362 . C36 . H361 . 110.9 no
C36 . C37 . C38 . 112.7(5) yes
C36 . C37 . H372 . 103.9 no
C38 . C37 . H372 . 106.6 no
C36 . C37 . H371 . 114.0 no
C38 . C37 . H371 . 109.5 no
H372 . C37 . H371 . 109.7 no
C37 . C38 . C39 . 113.6(5) yes
C37 . C38 . H381 . 107.4 no
C39 . C38 . H381 . 106.6 no
C37 . C38 . H382 . 110.5 no
C39 . C38 . H382 . 105.8 no
H381 . C38 . H382 . 113.1 no
C38 . C39 . C40 . 114.3(5) yes
C38 . C39 . H391 . 108.6 no
C40 . C39 . H391 . 110.1 no
C38 . C39 . H392 . 107.4 no
C40 . C39 . H392 . 106.6 no
H391 . C39 . H392 . 109.8 no
C39 . C40 . H403 . 107.7 no
C39 . C40 . H401 . 103.4 no
H403 . C40 . H401 . 113.2 no
C39 . C40 . H402 . 104.8 no
H403 . C40 . H402 . 114.2 no
H401 . C40 . H402 . 112.4 no
C27 . O41 . C42 . 113.0(3) yes
C27 . O41 . C142 . 132.5(6) yes
O41 . C42 . C43 . 112.4(4) yes
O41 . C42 . H421 . 106.3 no
C43 . C42 . H421 . 110.4 no
O41 . C42 . H422 . 111.7 no
C43 . C42 . H422 . 107.0 no
H421 . C42 . H422 . 109.1 no
C42 . C43 . C44 . 115.9(4) yes
C42 . C43 . H431 . 107.9 no
C44 . C43 . H431 . 104.2 no
C42 . C43 . H432 . 106.9 no
C44 . C43 . H432 . 110.2 no
H431 . C43 . H432 . 111.8 no
C43 . C44 . C45 . 113.9(4) yes
C43 . C44 . H442 . 107.7 no
C45 . C44 . H442 . 112.1 no
C43 . C44 . H441 . 105.0 no
C45 . C44 . H441 . 111.4 no
H442 . C44 . H441 . 106.2 no
C44 . C45 . C46 . 111.6(4) yes
C44 . C45 . H452 . 109.0 no
C46 . C45 . H452 . 121.3 no
C44 . C45 . H451 . 105.8 no
C46 . C45 . H451 . 94.2 no
H452 . C45 . H451 . 113.3 no
C45 . C46 . H461 . 108.3 no
C45 . C46 . H463 . 104.5 no
H461 . C46 . H463 . 109.5 no
C45 . C46 . H462 . 115.4 no
H461 . C46 . H462 . 109.5 no
H463 . C46 . H462 . 109.5 no
C28 . O47 . C48 . 114.8(2) yes
O47 . C48 . C49 . 108.2(2) yes
O47 . C48 . H482 . 109.0 no
C49 . C48 . H482 . 107.6 no
O47 . C48 . H481 . 110.1 no
C49 . C48 . H481 . 113.4 no
H482 . C48 . H481 . 108.4 no
C48 . C49 . C50 . 108.1(3) yes
C48 . C49 . H491 . 110.0 no
C50 . C49 . H491 . 109.3 no
C48 . C49 . H494 . 110.0 no
C50 . C49 . H494 . 109.9 no
H491 . C49 . H494 . 109.5 no
C48 . C49 . C150 . 114.8(7) yes
C48 . C49 . H493 . 107.3 no
C150 . C49 . H493 . 108.4 no
C48 . C49 . H492 . 107.0 no
C150 . C49 . H492 . 109.8 no
H493 . C49 . H492 . 109.5 no
C49 . C50 . C51 . 109.7(3) yes
C49 . C50 . H501 . 110.1 no
C51 . C50 . H501 . 105.7 no
C49 . C50 . H502 . 113.1 no
C51 . C50 . H502 . 109.6 no
H501 . C50 . H502 . 108.5 no
C50 . C51 . C52 . 110.1(4) yes
C50 . C51 . H511 . 109.9 no
C52 . C51 . H511 . 109.7 no
C50 . C51 . H512 . 110.3 no
C52 . C51 . H512 . 108.5 no
H511 . C51 . H512 . 108.3 no
C51 . C52 . H521 . 109.3 no
C51 . C52 . H522 . 108.6 no
H521 . C52 . H522 . 110.5 no
C51 . C52 . H523 . 109.7 no
H521 . C52 . H523 . 110.2 no
H522 . C52 . H523 . 108.4 no
C5 . N53 . O54 . 118.5(2) yes
C5 . N53 . O55 . 118.5(3) yes
O54 . N53 . O55 . 122.9(2) yes
C11 . N56 . O57 . 117.5(3) yes
C11 . N56 . O58 . 118.3(2) yes
O57 . N56 . O58 . 124.2(3) yes
C17 . N59 . O60 . 118.2(3) yes
C17 . N59 . O61 . 117.8(3) yes
O60 . N59 . O61 . 123.9(3) yes
C23 . N62 . O63 . 118.4(3) yes
C23 . N62 . O64 . 117.9(3) yes
O63 . N62 . O64 . 123.7(3) yes
O35 . C136 . C137 . 107.9(6) yes
O35 . C136 . H1361 . 110.5 no
C137 . C136 . H1361 . 110.5 no
O35 . C136 . H1362 . 110.2 no
C137 . C136 . H1362 . 107.6 no
H1361 . C136 . H1362 . 110.1 no
C136 . C137 . C138 . 108.4(7) yes
C136 . C137 . H1372 . 108.8 no
C138 . C137 . H1372 . 111.3 no
C136 . C137 . H1371 . 110.9 no
C138 . C137 . H1371 . 108.8 no
H1372 . C137 . H1371 . 108.6 no
C137 . C138 . C139 . 108.4(6) yes
C137 . C138 . H1382 . 107.3 no
C139 . C138 . H1382 . 109.8 no
C137 . C138 . H1381 . 113.2 no
C139 . C138 . H1381 . 109.3 no
H1382 . C138 . H1381 . 108.9 no
C138 . C139 . C140 . 106.5(7) yes
C138 . C139 . H1392 . 109.8 no
C140 . C139 . H1392 . 108.0 no
C138 . C139 . H1391 . 109.7 no
C140 . C139 . H1391 . 113.5 no
H1392 . C139 . H1391 . 109.3 no
C139 . C140 . H1401 . 108.8 no
C139 . C140 . H1403 . 113.4 no
H1401 . C140 . H1403 . 109.5 no
C139 . C140 . H1402 . 106.2 no
H1401 . C140 . H1402 . 109.5 no
H1403 . C140 . H1402 . 109.5 no
O41 . C142 . C143 . 102.2(8) yes
O41 . C142 . H1422 . 102.8 no
C143 . C142 . H1422 . 100.8 no
O41 . C142 . H1421 . 117.3 no
C143 . C142 . H1421 . 122.2 no
H1422 . C142 . H1421 . 108.9 no
C142 . C143 . C144 . 107.2(8) yes
C142 . C143 . H1431 . 108.4 no
C144 . C143 . H1431 . 133.9 no
C142 . C143 . H1432 . 99.3 no
C144 . C143 . H1432 . 92.5 no
H1431 . C143 . H1432 . 109.4 no
C143 . C144 . C145 . 109.0(9) yes
C143 . C144 . H1441 . 81.9 no
C145 . C144 . H1441 . 63.6 no
C143 . C144 . H1442 . 118.8 no
C145 . C144 . H1442 . 131.2 no
H1441 . C144 . H1442 . 112.5 no
C144 . C145 . C146 . 113.0(9) yes
C144 . C145 . H1451 . 108.2 no
C146 . C145 . H1451 . 120.2 no
C144 . C145 . H1452 . 66.7 no
C146 . C145 . H1452 . 54.9 no
H1451 . C145 . H1452 . 110.7 no
C145 . C146 . H1452 . 42.1 no
C145 . C146 . H1462 . 123.2 no
H1452 . C146 . H1462 . 117.2 no
C145 . C146 . H1461 . 70.6 no
H1452 . C146 . H1461 . 111.2 no
H1462 . C146 . H1461 . 109.5 no
C145 . C146 . H1463 . 124.2 no
H1452 . C146 . H1463 . 99.5 no
H1462 . C146 . H1463 . 109.5 no
H1461 . C146 . H1463 . 109.5 no
C49 . C150 . C151 . 112.0(6) yes
C49 . C150 . H1502 . 105.4 no
C151 . C150 . H1502 . 102.8 no
C49 . C150 . H1501 . 114.7 no
C151 . C150 . H1501 . 111.8 no
H1502 . C150 . H1501 . 109.2 no
C150 . C151 . C152 . 112.0(7) yes
C150 . C151 . H1511 . 113.3 no
C152 . C151 . H1511 . 110.2 no
C150 . C151 . H1512 . 105.1 no
C152 . C151 . H1512 . 106.2 no
H1511 . C151 . H1512 . 109.7 no
C151 . C152 . H1522 . 108.0 no
C151 . C152 . H1523 . 108.4 no
H1522 . C152 . H1523 . 110.6 no
C151 . C152 . H1521 . 110.1 no
H1522 . C152 . H1521 . 109.7 no
H1523 . C152 . H1521 . 110.0 no
C145 . H1452 . C146 . 83.0 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C4 . H41 . O57 1_545 153 0.938 2.582 3.447(3) yes
C48 . H481 . O64 2_665 142 0.968 2.547 3.366(10) yes
C151 . H1511 . O60 . 163 0.970 2.129 3.068(10) yes
C37 . H372 . O54 2_566 151 0.978 2.520 3.408(10) yes
C42 . H422 . O60 2_565 145 0.966 2.367 3.210(10) yes
C142 . H1421 . O60 2_565 169 0.941 2.327 3.256(10) yes
C49 . H491 . O57 1_545 129 0.950 2.544 3.224(10) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/10/14 at 13:49:41
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
EQUIVALENCE PART(2001, OCC) PART(2002, OCC) 
WEIGHT -1 PART(2002, OCC) 
EQUIVALENCE PART(3001, OCC) PART(3002, OCC) 
WEIGHT -1 PART(3002, OCC) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 343,X'S) H   ( 342,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 372,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 442,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 452,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 463,X'S) H   ( 462,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 493,X'S) H   ( 492,X'S) H   ( 491,X'S) H   ( 494,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) H   ( 523,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) H   (1362,X'S) 
RIDE C   ( 137,X'S) H   (1372,X'S) H   (1371,X'S) 
RIDE C   ( 138,X'S) H   (1382,X'S) H   (1381,X'S) 
RIDE C   ( 139,X'S) H   (1392,X'S) H   (1391,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) H   (1403,X'S) H   (1402,X'S) 
RIDE C   ( 142,X'S) H   (1422,X'S) H   (1421,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) H   (1432,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) H   (1442,X'S) 
RIDE C   ( 145,X'S) H   (1451,X'S) H   (1452,X'S) 
RIDE C   ( 146,X'S) H   (1462,X'S) H   (1461,X'S) H   (1463,X'S) 
RIDE C   ( 150,X'S) H   (1502,X'S) H   (1501,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) H   (1512,X'S) 
RIDE C   ( 152,X'S) H   (1522,X'S) H   (1523,X'S) H   (1521,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 17/10/14 at 13:49:41
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.441000 , 0.005000 = O(35) TO C(36) 
DISTANCE 1.525000 , 0.005000 = C(36) TO C(37) 
DISTANCE 1.539000 , 0.005000 = C(37) TO C(38) 
DISTANCE 1.539000 , 0.005000 = C(38) TO C(39) 
DISTANCE 1.539000 , 0.005000 = C(39) TO C(40) 
ANGLE 109.000000 , 1.000000 = O(35) TO C(36) TO C(37) 
ANGLE 109.000000 , 1.000000 = C(36) TO C(37) TO C(38) 
ANGLE 109.000000 , 1.000000 = C(37) TO C(38) TO C(39) 
ANGLE 109.000000 , 1.000000 = C(38) TO C(39) TO C(40) 
DISTANCE 1.441000 , 0.005000 = O(35) TO C(136) 
DISTANCE 1.525000 , 0.005000 = C(136) TO C(137) 
DISTANCE 1.539000 , 0.005000 = C(137) TO C(138) 
DISTANCE 1.539000 , 0.005000 = C(138) TO C(139) 
DISTANCE 1.539000 , 0.005000 = C(139) TO C(140) 
ANGLE 109.000000 , 1.000000 = O(35) TO C(136) TO C(137) 
ANGLE 109.000000 , 1.000000 = C(136) TO C(137) TO C(138) 
ANGLE 109.000000 , 1.000000 = C(137) TO C(138) TO C(139) 
ANGLE 109.000000 , 1.000000 = C(138) TO C(139) TO C(140) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(36) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(37) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(38) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(39) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(40) 
U(IJ)'S  0.0, 0.001000 = C(36) TO C(136) 
U(IJ)'S  0.0, 0.001000 = C(37) TO C(137) 
U(IJ)'S  0.0, 0.001000 = C(38) TO C(138) 
U(IJ)'S  0.0, 0.010000 = C(39) TO C(139) 
U(IJ)'S  0.0, 0.010000 = C(40) TO C(140) 
DISTANCE 1.441000 , 0.005000 = O(41) TO C(42) 
DISTANCE 1.525000 , 0.005000 = C(42) TO C(43) 
DISTANCE 1.539000 , 0.005000 = C(43) TO C(44) 
DISTANCE 1.539000 , 0.005000 = C(44) TO C(45) 
DISTANCE 1.539000 , 0.005000 = C(45) TO C(46) 
ANGLE 109.000000 , 1.000000 = O(41) TO C(42) TO C(43) 
ANGLE 109.000000 , 1.000000 = C(42) TO C(43) TO C(44) 
ANGLE 109.000000 , 1.000000 = C(43) TO C(44) TO C(45) 
ANGLE 109.000000 , 1.000000 = C(44) TO C(45) TO C(46) 
DISTANCE 1.441000 , 0.005000 = O(41) TO C(142) 
DISTANCE 1.525000 , 0.005000 = C(142) TO C(143) 
DISTANCE 1.539000 , 0.005000 = C(143) TO C(144) 
DISTANCE 1.539000 , 0.005000 = C(144) TO C(145) 
DISTANCE 1.539000 , 0.005000 = C(145) TO C(146) 
ANGLE 109.000000 , 1.000000 = O(41) TO C(142) TO C(143) 
ANGLE 109.000000 , 1.000000 = C(142) TO C(143) TO C(144) 
ANGLE 109.000000 , 1.000000 = C(143) TO C(144) TO C(145) 
ANGLE 109.000000 , 1.000000 = C(144) TO C(145) TO C(146) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(42) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(43) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(44) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(45) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(46) 
U(IJ)'S  0.0, 0.001000 = C(42) TO C(142) 
U(IJ)'S  0.0, 0.001000 = C(43) TO C(143) 
U(IJ)'S  0.0, 0.001000 = C(44) TO C(144) 
U(IJ)'S  0.0, 0.001000 = C(45) TO C(145) 
U(IJ)'S  0.0, 0.001000 = C(46) TO C(146) 
DISTANCE 1.441000 , 0.005000 = O(47) TO C(48) 
DISTANCE 1.525000 , 0.005000 = C(48) TO C(49) 
DISTANCE 1.539000 , 0.005000 = C(49) TO C(50) 
DISTANCE 1.539000 , 0.005000 = C(50) TO C(51) 
DISTANCE 1.539000 , 0.005000 = C(51) TO C(52) 
ANGLE 109.000000 , 1.000000 = O(47) TO C(48) TO C(49) 
ANGLE 109.000000 , 1.000000 = C(48) TO C(49) TO C(50) 
ANGLE 109.000000 , 1.000000 = C(49) TO C(50) TO C(51) 
ANGLE 109.000000 , 1.000000 = C(50) TO C(51) TO C(52) 
DISTANCE 1.539000 , 0.005000 = C(49) TO C(150) 
DISTANCE 1.539000 , 0.005000 = C(150) TO C(151) 
DISTANCE 1.539000 , 0.005000 = C(151) TO C(152) 
ANGLE 109.000000 , 1.000000 = C(48) TO C(49) TO C(150) 
ANGLE 109.000000 , 1.000000 = C(49) TO C(150) TO C(151) 
ANGLE 109.000000 , 1.000000 = C(150) TO C(151) TO C(152) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(48) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(49) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(50) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(51) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(52) 
U(IJ)'S  0.0, 0.001000 = C(50) TO C(150) 
U(IJ)'S  0.0, 0.001000 = C(51) TO C(151) 
U(IJ)'S  0.0, 0.001000 = C(52) TO C(152) 
END                                                                             
;
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_4c_solv
_database_code_depnum_ccdc_archive 'CCDC 1030572'
_audit_update_record             
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
_cell_length_a                   13.24520(12)
_cell_length_b                   13.24520(12)
_cell_length_c                   14.9787(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2627.79(5)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/n '
_symmetry_space_group_name_Hall  '-P 4bc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-y,x+1/2,z+1/2
y,-x+1/2,-z+1/2
-x+1/2,-y+1/2,z
x+1/2,y+1/2,-z
y+1/2,-x,z+1/2
-y+1/2,x,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C55 H50 N5 O10 S5 
# Dc =      1.39 Fooo =   1096.00 Mu =     25.67 M =    275.34
# Found Formula = C48 H58 N6 O12 S4 
# Dc =      1.31 FOOO =   1096.00 Mu =     22.01 M =    259.82

_chemical_formula_sum            'C48 H58 N6 O12 S4'
_chemical_formula_moiety         'C44 H52 N4 O12 S4, 2(C2 H3 N)'
_chemical_compound_source        ?
_chemical_formula_weight         1039.29


_cell_measurement_reflns_used    6670
_cell_measurement_theta_min      4
_cell_measurement_theta_max      77
_cell_measurement_temperature    170

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_max          0.360

_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1096.000
_exptl_absorpt_coefficient_mu    2.201

# Sheldrick geometric approximatio 0.59 0.72 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_T_max  0.72
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      170
_diffrn_ambient_pressure         101
_diffrn_reflns_number            11942
_reflns_number_total             2754
_diffrn_reflns_av_R_equivalents  0.027
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 2754 
# Theoretical number of reflections is about 5558 


_diffrn_reflns_theta_min         4.456
_diffrn_reflns_theta_max         77.022
_diffrn_measured_fraction_theta_max 0.987

_diffrn_reflns_theta_full        73.941
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   4.70
_oxford_diffrn_Wilson_scale      0.06

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.54
_refine_diff_density_max         0.67


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         2754
_refine_ls_number_restraints     80
_refine_ls_number_parameters     208
_oxford_refine_ls_R_factor_ref   0.0851
_refine_ls_wR_factor_ref         0.2601
_refine_ls_goodness_of_fit_ref   1.0650
_refine_ls_shift/su_max          0.0180496
_refine_ls_shift/su_mean         0.0022868


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2754
_refine_ls_R_factor_all          0.0851
_refine_ls_wR_factor_all         0.2601

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2451
_refine_ls_R_factor_gt           0.0800
_refine_ls_wR_factor_gt          0.2505

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.435E+04 0.738E+04 0.448E+04 0.181E+04 381. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.03603(18) 0.3412(2) 0.69543(18) 0.0512 1.0000 Uani . . . . . .
S2 S 0.04044(6) 0.45958(6) 0.74981(6) 0.0653 1.0000 Uani . . . . . .
C3 C 0.1587(2) 0.46409(18) 0.80452(18) 0.0509 1.0000 Uani . . . . . .
C4 C 0.1587(3) 0.4974(2) 0.89261(19) 0.0604 1.0000 Uani . . . . . .
C5 C 0.2510(3) 0.5136(2) 0.93402(18) 0.0622 1.0000 Uani . . . . . .
C6 C 0.3412(3) 0.49730(19) 0.8926(2) 0.0600 1.0000 Uani . . . . . .
C7 C 0.2502(2) 0.4470(2) 0.76046(19) 0.0497 1.0000 Uani . . . . . .
O8 O 0.24997(15) 0.40848(17) 0.67667(14) 0.0661 1.0000 Uani D U . . . .
C9 C 0.2545(4) 0.4772(4) 0.6041(3) 0.0818 0.766(6) Uani D U P 1 1 .
C10 C 0.2502(3) 0.4080(3) 0.5231(2) 0.0625 0.766(6) Uani D U P 1 1 .
C11 C 0.2505(4) 0.4734(4) 0.4396(2) 0.0734 0.766(6) Uani D U P 1 1 .
C12 C 0.2461(6) 0.4066(5) 0.3563(3) 0.1100 0.766(6) Uani D U P 1 1 .
C13 C 0.2504(7) 0.4767(6) 0.2747(4) 0.0947 0.766(6) Uani D U P 1 1 .
N14 N 0.2506(4) 0.5494(2) 1.0266(2) 0.0891 1.0000 Uani . . . . . .
O15 O 0.3328(4) 0.5633(3) 1.06281(19) 0.1165 1.0000 Uani . . . . . .
O16 O 0.1677(4) 0.5628(3) 1.06256(19) 0.1188 1.0000 Uani . . . . . .
C109 C 0.2286(16) 0.4904(10) 0.6146(7) 0.0817 0.234(6) Uani D U P 1 2 .
C110 C 0.2730(13) 0.4866(9) 0.5199(6) 0.0816 0.234(6) Uani D U P 1 2 .
C111 C 0.2218(14) 0.4038(11) 0.4643(9) 0.0856 0.234(6) Uani D U P 1 2 .
C112 C 0.2777(17) 0.3875(18) 0.3755(11) 0.1102 0.234(6) Uani D U P 1 2 .
C113 C 0.244(3) 0.467(2) 0.3073(14) 0.0946 0.234(6) Uani D U P 1 2 .
N17 N 0.2500 0.7500 0.8966(3) 0.0793 1.0000 Uani S T . . . .
C18 C 0.2500 0.7500 0.8199(4) 0.0734 1.0000 Uani S T . . . .
C19 C 0.250000(11) 0.750000(11) 0.7256(6) 0.1412 1.0000 Uani S T . . . .
H61 H 0.4018 0.5106 0.9244 0.0752 1.0000 Uiso R . . . . .
H41 H 0.0987 0.5079 0.9221 0.0749 1.0000 Uiso R . . . . .
H91 H 0.3152 0.5156 0.6076 0.0959 0.766(6) Uiso R . P 1 1 .
H92 H 0.1964 0.5216 0.6032 0.0959 0.766(6) Uiso R . P 1 1 .
H101 H 0.3086 0.3616 0.5201 0.0783 0.766(6) Uiso R . P 1 1 .
H102 H 0.1886 0.3703 0.5268 0.0789 0.766(6) Uiso R . P 1 1 .
H111 H 0.3125 0.5142 0.4395 0.0894 0.766(6) Uiso R . P 1 1 .
H112 H 0.1894 0.5197 0.4416 0.0898 0.766(6) Uiso R . P 1 1 .
H121 H 0.3038 0.3622 0.3571 0.1296 0.766(6) Uiso R . P 1 1 .
H122 H 0.1849 0.3699 0.3563 0.1290 0.766(6) Uiso R . P 1 1 .
H132 H 0.2424 0.4378 0.2210 0.1462 0.766(6) Uiso R . P 1 1 .
H131 H 0.3122 0.5144 0.2734 0.1461 0.766(6) Uiso R . P 1 1 .
H133 H 0.1941 0.5249 0.2800 0.1462 0.766(6) Uiso R . P 1 1 .
H1092 H 0.2595 0.5519 0.6423 0.0960 0.234(6) Uiso R . P 1 2 .
H1091 H 0.1570 0.4988 0.6127 0.0959 0.234(6) Uiso R . P 1 2 .
H1102 H 0.3404 0.4671 0.5200 0.0930 0.234(6) Uiso R . P 1 2 .
H1101 H 0.2603 0.5500 0.4909 0.0930 0.234(6) Uiso R . P 1 2 .
H1111 H 0.2000 0.3465 0.5072 0.1012 0.234(6) Uiso R . P 1 2 .
H1112 H 0.1425 0.4329 0.4531 0.1011 0.234(6) Uiso R . P 1 2 .
H1121 H 0.3324 0.3628 0.3961 0.1280 0.234(6) Uiso R . P 1 2 .
H1122 H 0.2329 0.3089 0.3608 0.1280 0.234(6) Uiso R . P 1 2 .
H1131 H 0.2766 0.4330 0.2560 0.1460 0.234(6) Uiso R . P 1 2 .
H1133 H 0.2825 0.5155 0.3314 0.1460 0.234(6) Uiso R . P 1 2 .
H1132 H 0.1775 0.4690 0.3046 0.1460 0.234(6) Uiso R . P 1 2 .
H193 H 0.2497 0.8176 0.7044 0.1724 0.5000 Uiso R . . . . .
H191 H 0.3087 0.7164 0.7044 0.1724 0.5000 Uiso R . . . . .
H192 H 0.1916 0.7159 0.7044 0.1724 0.5000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.39(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C7 8_556 1.393(4) yes
C1 . C6 8_556 1.390(4) yes
C1 . S2 . 1.768(3) yes
S2 . C3 . 1.769(3) yes
C3 . C4 . 1.391(4) yes
C3 . C7 . 1.399(4) yes
C4 . C5 . 1.388(5) yes
C4 . H41 . 0.920 no
C5 . C6 . 1.363(5) yes
C5 . N14 . 1.466(4) yes
C6 . H61 . 0.950 no
C7 . O8 . 1.355(3) yes
O8 . C9 . 1.418(4) yes
O8 . C109 . 1.457(5) yes
C9 . C10 . 1.521(4) yes
C9 . H91 . 0.953 no
C9 . H92 . 0.969 no
C10 . C11 . 1.521(4) yes
C10 . H101 . 0.989 no
C10 . H102 . 0.958 no
C11 . C12 . 1.530(4) yes
C11 . H111 . 0.983 no
C11 . H112 . 1.017 no
C12 . C13 . 1.536(5) yes
C12 . H121 . 0.965 no
C12 . H122 . 0.945 no
C13 . H132 . 0.961 no
C13 . H131 . 0.959 no
C13 . H133 . 0.985 no
N14 . O15 . 1.230(6) yes
N14 . O16 . 1.235(6) yes
C109 . C110 . 1.537(5) yes
C109 . H1092 . 1.001 no
C109 . H1091 . 0.956 no
C110 . C111 . 1.534(5) yes
C110 . H1102 . 0.929 no
C110 . H1101 . 0.961 no
C111 . C112 . 1.538(5) yes
C111 . H1111 . 1.036 no
C111 . H1112 . 1.131 no
C112 . C113 . 1.537(5) yes
C112 . H1121 . 0.853 no
C112 . H1122 . 1.218 no
C113 . H1131 . 0.993 no
C113 . H1133 . 0.896 no
C113 . H1132 . 0.879 no
N17 . C18 . 1.149(8) yes
C18 . C19 . 1.414(10) yes
C19 . H192 5_565 0.950 no
C19 . H193 5_565 0.950 no
C19 . H191 5_565 0.950 no
C19 . H193 . 0.950 no
C19 . H191 . 0.950 no
C19 . H192 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C7 8_556 C1 . C6 8_556 120.0(3) yes
C7 8_556 C1 . S2 . 122.9(2) yes
C6 8_556 C1 . S2 . 116.6(2) yes
C1 . S2 . C3 . 105.82(11) yes
S2 . C3 . C4 . 116.8(2) yes
S2 . C3 . C7 . 122.9(2) yes
C4 . C3 . C7 . 119.9(3) yes
C3 . C4 . C5 . 118.2(3) yes
C3 . C4 . H41 . 120.2 no
C5 . C4 . H41 . 121.6 no
C4 . C5 . C6 . 123.0(3) yes
C4 . C5 . N14 . 118.0(3) yes
C6 . C5 . N14 . 119.1(3) yes
C1 4_556 C6 . C5 . 118.8(3) yes
C1 4_556 C6 . H61 . 122.3 no
C5 . C6 . H61 . 118.9 no
C3 . C7 . C1 4_556 120.0(3) yes
C3 . C7 . O8 . 119.7(2) yes
C1 4_556 C7 . O8 . 120.2(2) yes
C7 . O8 . C9 . 117.9(3) yes
C7 . O8 . C109 . 108.1(6) yes
O8 . C9 . C10 . 102.9(3) yes
O8 . C9 . H91 . 109.6 no
C10 . C9 . H91 . 113.4 no
O8 . C9 . H92 . 111.5 no
C10 . C9 . H92 . 109.0 no
H91 . C9 . H92 . 110.2 no
C9 . C10 . C11 . 108.3(3) yes
C9 . C10 . H101 . 112.4 no
C11 . C10 . H101 . 108.3 no
C9 . C10 . H102 . 107.4 no
C11 . C10 . H102 . 110.3 no
H101 . C10 . H102 . 110.1 no
C10 . C11 . C12 . 110.0(4) yes
C10 . C11 . H111 . 108.4 no
C12 . C11 . H111 . 110.4 no
C10 . C11 . H112 . 108.5 no
C12 . C11 . H112 . 110.0 no
H111 . C11 . H112 . 109.5 no
C11 . C12 . C13 . 107.4(5) yes
C11 . C12 . H121 . 108.2 no
C13 . C12 . H121 . 110.4 no
C11 . C12 . H122 . 109.3 no
C13 . C12 . H122 . 110.0 no
H121 . C12 . H122 . 111.4 no
C12 . C13 . H132 . 109.8 no
C12 . C13 . H131 . 111.3 no
H132 . C13 . H131 . 110.9 no
C12 . C13 . H133 . 107.5 no
H132 . C13 . H133 . 109.3 no
H131 . C13 . H133 . 108.0 no
C5 . N14 . O15 . 117.5(4) yes
C5 . N14 . O16 . 117.6(4) yes
O15 . N14 . O16 . 124.9(4) yes
O8 . C109 . C110 . 119.3(7) yes
O8 . C109 . H1092 . 105.1 no
C110 . C109 . H1092 . 104.7 no
O8 . C109 . H1091 . 107.3 no
C110 . C109 . H1091 . 110.9 no
H1092 . C109 . H1091 . 108.9 no
C109 . C110 . C111 . 110.8(9) yes
C109 . C110 . H1102 . 112.0 no
C111 . C110 . H1102 . 103.2 no
C109 . C110 . H1101 . 108.7 no
C111 . C110 . H1101 . 107.6 no
H1102 . C110 . H1101 . 114.4 no
C110 . C111 . C112 . 110.9(9) yes
C110 . C111 . H1111 . 108.1 no
C112 . C111 . H1111 . 124.6 no
C110 . C111 . H1112 . 104.3 no
C112 . C111 . H1112 . 111.5 no
H1111 . C111 . H1112 . 94.8 no
C111 . C112 . C113 . 109.7(9) yes
C111 . C112 . H1121 . 98.6 no
C113 . C112 . H1121 . 138.9 no
C111 . C112 . H1122 . 92.4 no
C113 . C112 . H1122 . 109.0 no
H1121 . C112 . H1122 . 98.7 no
C112 . C113 . H1131 . 94.1 no
C112 . C113 . H1133 . 93.1 no
H1131 . C113 . H1133 . 112.8 no
C112 . C113 . H1132 . 109.9 no
H1131 . C113 . H1132 . 114.4 no
H1133 . C113 . H1132 . 124.9 no
N17 . C18 . C19 . 179.992 yes
C18 . C19 . H192 5_565 109.5 no
C18 . C19 . H193 5_565 109.5 no
H192 5_565 C19 . H193 5_565 109.5 no
C18 . C19 . H191 5_565 109.5 no
H192 5_565 C19 . H191 5_565 109.5 no
H193 5_565 C19 . H191 5_565 109.5 no
C18 . C19 . H193 . 109.5 no
H192 5_565 C19 . H193 . 56.3 no
H193 5_565 C19 . H193 . 141.1 no
H191 5_565 C19 . H193 . 56.3 no
C18 . C19 . H191 . 109.5 no
H192 5_565 C19 . H191 . 56.3 no
H193 5_565 C19 . H191 . 56.3 no
H191 5_565 C19 . H191 . 141.1 no
H193 . C19 . H191 . 109.5 no
C18 . C19 . H192 . 109.5 no
H192 5_565 C19 . H192 . 141.1 no
H193 5_565 C19 . H192 . 56.3 no
H191 5_565 C19 . H192 . 56.3 no
H193 . C19 . H192 . 109.5 no
H191 . C19 . H192 . 109.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C111 . H102 . O8 . 123.6(8) 1.126 2.440 3.203(11) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/10/14 at 17:01:49
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   ( 109,X'S) H   (1092,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1102,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1112,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1122,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1133,X'S) H   (1132,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 17/10/14 at 17:01:49
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.441000 , 0.005000 = O(8) TO C(9) 
DISTANCE 1.525000 , 0.005000 = C(9) TO C(10) 
DISTANCE 1.539000 , 0.005000 = C(10) TO C(11) 
DISTANCE 1.539000 , 0.005000 = C(11) TO C(12) 
DISTANCE 1.539000 , 0.005000 = C(12) TO C(13) 
ANGLE 109.000000 , 1.000000 = O(8) TO C(9) TO C(10) 
ANGLE 109.000000 , 1.000000 = C(9) TO C(10) TO C(11) 
ANGLE 109.000000 , 1.000000 = C(10) TO C(11) TO C(12) 
ANGLE 109.000000 , 1.000000 = C(11) TO C(12) TO C(13) 
DISTANCE 1.441000 , 0.005000 = O(8) TO C(109) 
DISTANCE 1.525000 , 0.005000 = C(109) TO C(110) 
DISTANCE 1.539000 , 0.005000 = C(110) TO C(111) 
DISTANCE 1.539000 , 0.005000 = C(111) TO C(112) 
DISTANCE 1.539000 , 0.005000 = C(112) TO C(113) 
ANGLE 109.000000 , 1.000000 = O(8) TO C(109) TO C(110) 
ANGLE 109.000000 , 1.000000 = C(109) TO C(110) TO C(111) 
ANGLE 109.000000 , 1.000000 = C(110) TO C(111) TO C(112) 
ANGLE 109.000000 , 1.000000 = C(111) TO C(112) TO C(113) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(9) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(10) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(11) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(12) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(13) 
U(IJ)'S  0.0, 0.001000 = C(9) TO C(109) 
U(IJ)'S  0.0, 0.010000 = C(10) TO C(110) 
U(IJ)'S  0.0, 0.010000 = C(11) TO C(111) 
U(IJ)'S  0.0, 0.001000 = C(12) TO C(112) 
U(IJ)'S  0.0, 0.001000 = C(13) TO C(113) 
END                                                                             
;
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_4g
_database_code_depnum_ccdc_archive 'CCDC 1030573'
_audit_update_record             
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
_cell_length_a                   12.73537(12)
_cell_length_b                   12.73537(12)
_cell_length_c                   28.8831(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4684.54(8)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41 21 2 '
_symmetry_space_group_name_Hall  'P 4abw 2nw'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,-y+1/2,-z+3/4
y,x,-z
-y+1/2,x+1/2,z+1/4
-y,-x,-z+1/2
y+1/2,-x+1/2,z+3/4
-x,-y,z+1/2
-x+1/2,y+1/2,-z+1/4

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C60 H5 N1 O8 S4 
# Dc =      1.41 Fooo =   2144.00 Mu =     23.81 M =    497.98
# Found Formula = C52 H36 N4 O12 S4 
# Dc =      1.47 FOOO =   2144.00 Mu =     24.69 M =    518.57

_chemical_formula_sum            'C52 H36 N4 O12 S4'
_chemical_formula_moiety         'C52 H36 N4 O12 S4'
_chemical_compound_source        ?
_chemical_formula_weight         1037.14


_cell_measurement_reflns_used    11504
_cell_measurement_theta_min      5
_cell_measurement_theta_max      76
_cell_measurement_temperature    190

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.260
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_max          0.410

_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2144
_exptl_absorpt_coefficient_mu    2.469

# Sheldrick geometric approximatio 0.44 0.53 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_T_max  0.53
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      190
_diffrn_ambient_pressure         101
_diffrn_reflns_number            21324
_reflns_number_total             4801
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 4801 
# Number of reflections with Friedels Law is 2839 
# Theoretical number of reflections is about 2438 


_diffrn_reflns_theta_min         4.629
_diffrn_reflns_theta_max         75.778
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        74.263
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_reflns_limit_h_min              -10
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              35

_oxford_diffrn_Wilson_B_factor   2.83
_oxford_diffrn_Wilson_scale      0.38

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.33
_refine_diff_density_max         0.21


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         4801
_refine_ls_number_restraints     0
_refine_ls_number_parameters     327
_oxford_refine_ls_R_factor_ref   0.0464
_refine_ls_wR_factor_ref         0.1148
_refine_ls_goodness_of_fit_ref   1.0794
_refine_ls_shift/su_max          0.0017159
_refine_ls_shift/su_mean         0.0000570


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4801
_refine_ls_R_factor_all          0.0464
_refine_ls_wR_factor_all         0.1148

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4516
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_gt          0.1044

_refine_ls_abs_structure_Flack   0.65(2)
_refine_ls_abs_structure_details 'Flack (1983), 1962 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 648. 0.102E+04 517. 128. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.10067(17) 0.78574(15) 0.52612(7) 0.0334 1.0000 Uani . . . . . .
S2 S 0.22131(4) 0.78424(4) 0.495665(19) 0.0377 1.0000 Uani . . . . . .
C3 C 0.22052(15) 0.90763(17) 0.46739(7) 0.0326 1.0000 Uani . . . . . .
C4 C 0.23083(16) 0.91050(18) 0.41959(7) 0.0376 1.0000 Uani . . . . . .
C5 C 0.23334(15) 1.00680(19) 0.39800(7) 0.0373 1.0000 Uani . . . . . .
C6 C 0.22340(16) 1.10119(18) 0.42136(7) 0.0360 1.0000 Uani . . . . . .
C7 C 0.21562(15) 1.09851(16) 0.46947(7) 0.0309 1.0000 Uani . . . . . .
S8 S 0.21896(3) 1.21896(3) 0.5000 0.0347 1.0000 Uani S T . . . .
S9 S -0.21477(4) 0.78523(4) 0.5000 0.0376 1.0000 Uani S T . . . .
C10 C -0.09078(16) 0.78334(15) 0.52781(7) 0.0326 1.0000 Uani . . . . . .
C11 C -0.0871(2) 0.75958(17) 0.57483(7) 0.0402 1.0000 Uani . . . . . .
C12 C 0.0090(2) 0.75211(16) 0.59637(7) 0.0403 1.0000 Uani . . . . . .
C13 C 0.1029(2) 0.76527(17) 0.57351(7) 0.0395 1.0000 Uani . . . . . .
C14 C 0.21671(13) 1.00148(16) 0.49274(6) 0.0293 1.0000 Uani . . . . . .
C15 C 0.00412(15) 0.79588(15) 0.50310(6) 0.0311 1.0000 Uani . . . . . .
O16 O 0.21347(10) 0.99993(11) 0.54021(5) 0.0332 1.0000 Uani . . . . . .
C17 C 0.31793(16) 0.99478(18) 0.55945(7) 0.0385 1.0000 Uani . . . . . .
C18 C 0.31338(16) 0.99405(16) 0.61160(7) 0.0353 1.0000 Uani . . . . . .
C19 C 0.40802(19) 0.99120(18) 0.63506(7) 0.0428 1.0000 Uani . . . . . .
C20 C 0.4104(2) 0.9916(2) 0.68344(8) 0.0474 1.0000 Uani . . . . . .
C21 C 0.3193(2) 0.99550(19) 0.70838(8) 0.0489 1.0000 Uani . . . . . .
C22 C 0.2255(2) 0.9996(3) 0.68476(9) 0.0685 1.0000 Uani . . . . . .
C23 C 0.2217(2) 0.9968(3) 0.63652(8) 0.0592 1.0000 Uani . . . . . .
O24 O 0.00152(11) 0.82318(10) 0.45758(5) 0.0339 1.0000 Uani . . . . . .
C25 C -0.0029(2) 0.73618(15) 0.42601(7) 0.0412 1.0000 Uani . . . . . .
C26 C -0.00453(16) 0.77591(17) 0.37692(7) 0.0360 1.0000 Uani . . . . . .
C27 C 0.0021(2) 0.7055(2) 0.34093(8) 0.0510 1.0000 Uani . . . . . .
C28 C -0.0020(2) 0.7373(2) 0.29512(8) 0.0571 1.0000 Uani . . . . . .
C29 C -0.0135(2) 0.8417(2) 0.28510(9) 0.0597 1.0000 Uani . . . . . .
C30 C -0.0187(3) 0.9140(2) 0.32041(9) 0.0630 1.0000 Uani . . . . . .
C31 C -0.0142(2) 0.88276(19) 0.36677(8) 0.0460 1.0000 Uani . . . . . .
N32 N 0.24691(16) 1.01032(18) 0.34740(6) 0.0479 1.0000 Uani . . . . . .
O33 O 0.2744(2) 0.9296(2) 0.32786(6) 0.0795 1.0000 Uani . . . . . .
O34 O 0.2308(2) 1.09294(18) 0.32719(6) 0.0662 1.0000 Uani . . . . . .
N35 N 0.0123(2) 0.73092(16) 0.64624(7) 0.0530 1.0000 Uani . . . . . .
O36 O -0.0673(2) 0.6982(2) 0.66452(6) 0.0774 1.0000 Uani . . . . . .
O37 O 0.0940(2) 0.7461(2) 0.66679(7) 0.0690 1.0000 Uani . . . . . .
H41 H 0.2358 0.8465 0.4028 0.0446 1.0000 Uiso R . . . . .
H61 H 0.2207 1.1652 0.4062 0.0433 1.0000 Uiso R . . . . .
H171 H 0.3588 1.0579 0.5501 0.0481 1.0000 Uiso R . . . . .
H172 H 0.3537 0.9309 0.5489 0.0479 1.0000 Uiso R . . . . .
H191 H 0.4717 0.9886 0.6181 0.0506 1.0000 Uiso R . . . . .
H201 H 0.4761 0.9909 0.6987 0.0561 1.0000 Uiso R . . . . .
H211 H 0.3191 0.9961 0.7411 0.0588 1.0000 Uiso R . . . . .
H221 H 0.1614 1.0028 0.7018 0.0822 1.0000 Uiso R . . . . .
H231 H 0.1563 0.9992 0.6209 0.0725 1.0000 Uiso R . . . . .
H251 H -0.0677 0.6980 0.4319 0.0499 1.0000 Uiso R . . . . .
H252 H 0.0577 0.6906 0.4318 0.0494 1.0000 Uiso R . . . . .
H311 H -0.0181 0.9329 0.3906 0.0542 1.0000 Uiso R . . . . .
H301 H -0.0253 0.9856 0.3135 0.0744 1.0000 Uiso R . . . . .
H291 H -0.0179 0.8638 0.2541 0.0713 1.0000 Uiso R . . . . .
H281 H 0.0031 0.6878 0.2711 0.0701 1.0000 Uiso R . . . . .
H271 H 0.0101 0.6343 0.3473 0.0595 1.0000 Uiso R . . . . .
H111 H -0.1495 0.7496 0.5915 0.0490 1.0000 Uiso R . . . . .
H131 H 0.1668 0.7611 0.5887 0.0478 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.742(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . S2 . 1.770(2) yes
C1 . C13 . 1.394(3) yes
C1 . C15 . 1.404(3) yes
S2 . C3 . 1.771(2) yes
C3 . C4 . 1.387(3) yes
C3 . C14 . 1.403(3) yes
C4 . C5 . 1.376(3) yes
C4 . H41 . 0.952 no
C5 . C6 . 1.384(3) yes
C5 . N32 . 1.473(2) yes
C6 . C7 . 1.394(3) yes
C6 . H61 . 0.927 no
C7 . S8 . 1.770(2) yes
C7 . C14 . 1.407(3) yes
S9 . C10 3_466 1.772(2) yes
S9 . C10 . 1.772(2) yes
C10 . C11 . 1.392(3) yes
C10 . C15 . 1.413(3) yes
C11 . C12 . 1.376(3) yes
C11 . H111 . 0.938 no
C12 . C13 . 1.377(3) yes
C12 . N35 . 1.466(3) yes
C13 . H131 . 0.926 no
C14 . O16 . 1.372(2) yes
C15 . O24 . 1.361(2) yes
O16 . C17 . 1.443(2) yes
C17 . C18 . 1.507(3) yes
C17 . H171 . 0.995 no
C17 . H172 . 0.981 no
C18 . C19 . 1.383(3) yes
C18 . C23 . 1.372(3) yes
C19 . C20 . 1.397(3) yes
C19 . H191 . 0.949 no
C20 . C21 . 1.367(4) yes
C20 . H201 . 0.945 no
C21 . C22 . 1.376(4) yes
C21 . H211 . 0.946 no
C22 . C23 . 1.395(3) yes
C22 . H221 . 0.954 no
C23 . H231 . 0.948 no
O24 . C25 . 1.436(2) yes
C25 . C26 . 1.506(3) yes
C25 . H251 . 0.973 no
C25 . H252 . 0.980 no
C26 . C27 . 1.375(3) yes
C26 . C31 . 1.397(3) yes
C27 . C28 . 1.385(3) yes
C27 . H271 . 0.931 no
C28 . C29 . 1.370(4) yes
C28 . H281 . 0.939 no
C29 . C30 . 1.376(4) yes
C29 . H291 . 0.940 no
C30 . C31 . 1.398(3) yes
C30 . H301 . 0.937 no
C31 . H311 . 0.940 no
N32 . O33 . 1.224(3) yes
N32 . O34 . 1.221(3) yes
N35 . O36 . 1.217(3) yes
N35 . O37 . 1.213(3) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 . C1 . C13 . 117.92(17) yes
S2 . C1 . C15 . 121.73(14) yes
C13 . C1 . C15 . 120.0(2) yes
C1 . S2 . C3 . 102.39(9) yes
S2 . C3 . C4 . 118.80(17) yes
S2 . C3 . C14 . 121.04(15) yes
C4 . C3 . C14 . 120.02(19) yes
C3 . C4 . C5 . 118.5(2) yes
C3 . C4 . H41 . 119.5 no
C5 . C4 . H41 . 122.1 no
C4 . C5 . C6 . 123.44(18) yes
C4 . C5 . N32 . 118.7(2) yes
C6 . C5 . N32 . 117.9(2) yes
C5 . C6 . C7 . 118.11(19) yes
C5 . C6 . H61 . 122.5 no
C7 . C6 . H61 . 119.4 no
C6 . C7 . S8 . 118.28(16) yes
C6 . C7 . C14 . 119.83(19) yes
S8 . C7 . C14 . 121.53(14) yes
C7 . S8 . C7 3_466 101.92(12) yes
C10 3_466 S9 . C10 . 103.28(13) yes
S9 . C10 . C11 . 118.38(17) yes
S9 . C10 . C15 . 122.14(14) yes
C11 . C10 . C15 . 119.2(2) yes
C10 . C11 . C12 . 119.1(2) yes
C10 . C11 . H111 . 120.1 no
C12 . C11 . H111 . 120.8 no
C11 . C12 . C13 . 123.18(18) yes
C11 . C12 . N35 . 118.9(2) yes
C13 . C12 . N35 . 117.9(2) yes
C1 . C13 . C12 . 118.4(2) yes
C1 . C13 . H131 . 119.7 no
C12 . C13 . H131 . 121.9 no
C7 . C14 . C3 . 119.96(17) yes
C7 . C14 . O16 . 119.34(18) yes
C3 . C14 . O16 . 120.70(18) yes
C10 . C15 . C1 . 119.99(17) yes
C10 . C15 . O24 . 119.76(18) yes
C1 . C15 . O24 . 120.16(17) yes
C14 . O16 . C17 . 110.97(14) yes
O16 . C17 . C18 . 110.47(16) yes
O16 . C17 . H171 . 109.9 no
C18 . C17 . H171 . 107.2 no
O16 . C17 . H172 . 110.2 no
C18 . C17 . H172 . 108.9 no
H171 . C17 . H172 . 110.1 no
C17 . C18 . C19 . 117.14(19) yes
C17 . C18 . C23 . 123.83(19) yes
C19 . C18 . C23 . 119.03(19) yes
C18 . C19 . C20 . 120.6(2) yes
C18 . C19 . H191 . 119.5 no
C20 . C19 . H191 . 119.9 no
C19 . C20 . C21 . 120.6(2) yes
C19 . C20 . H201 . 119.1 no
C21 . C20 . H201 . 120.3 no
C20 . C21 . C22 . 118.5(2) yes
C20 . C21 . H211 . 122.0 no
C22 . C21 . H211 . 119.6 no
C21 . C22 . C23 . 121.6(2) yes
C21 . C22 . H221 . 119.2 no
C23 . C22 . H221 . 119.1 no
C22 . C23 . C18 . 119.7(2) yes
C22 . C23 . H231 . 120.4 no
C18 . C23 . H231 . 119.9 no
C15 . O24 . C25 . 114.67(14) yes
O24 . C25 . C26 . 109.83(16) yes
O24 . C25 . H251 . 107.9 no
C26 . C25 . H251 . 108.8 no
O24 . C25 . H252 . 108.5 no
C26 . C25 . H252 . 111.8 no
H251 . C25 . H252 . 109.9 no
C25 . C26 . C27 . 119.5(2) yes
C25 . C26 . C31 . 121.73(19) yes
C27 . C26 . C31 . 118.8(2) yes
C26 . C27 . C28 . 122.0(2) yes
C26 . C27 . H271 . 119.5 no
C28 . C27 . H271 . 118.6 no
C27 . C28 . C29 . 119.3(3) yes
C27 . C28 . H281 . 120.5 no
C29 . C28 . H281 . 120.2 no
C28 . C29 . C30 . 119.9(2) yes
C28 . C29 . H291 . 119.8 no
C30 . C29 . H291 . 120.3 no
C29 . C30 . C31 . 121.2(3) yes
C29 . C30 . H301 . 119.9 no
C31 . C30 . H301 . 119.0 no
C30 . C31 . C26 . 118.8(2) yes
C30 . C31 . H311 . 120.4 no
C26 . C31 . H311 . 120.8 no
C5 . N32 . O33 . 117.7(2) yes
C5 . N32 . O34 . 118.7(2) yes
O33 . N32 . O34 . 123.5(2) yes
C12 . N35 . O36 . 117.7(2) yes
C12 . N35 . O37 . 118.5(2) yes
O36 . N35 . O37 . 123.8(2) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C25 . H252 . O36 6_454 157.86(7) 0.980 2.433 3.361(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/10/14 at 14:13:17
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 17/10/14 at 14:13:17
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_4d
_database_code_depnum_ccdc_archive 'CCDC 1030574'
_audit_update_record             
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
_cell_length_a                   27.2610(14)
_cell_length_b                   16.3468(3)
_cell_length_c                   17.9466(9)
_cell_angle_alpha                90
_cell_angle_beta                 139.366(10)
_cell_angle_gamma                90
_cell_volume                     5208.2(11)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C48 H60 N4 O12 S4 
# Dc =      1.29 Fooo =   2144.00 Mu =     21.95 M =   1013.29
# Found Formula = C48 H60 N4 O12 S4 
# Dc =      1.29 FOOO =   2144.00 Mu =     21.95 M =   1013.29

_chemical_formula_sum            'C48 H60 N4 O12 S4'
_chemical_formula_moiety         'C48 H60 N4 O12 S4'
_chemical_compound_source        ?
_chemical_formula_weight         1013.29


_cell_measurement_reflns_used    9774
_cell_measurement_theta_min      5
_cell_measurement_theta_max      76
_cell_measurement_temperature    180

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.093
_exptl_crystal_size_mid          0.362
_exptl_crystal_size_max          0.544

_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2143.999
_exptl_absorpt_coefficient_mu    2.195

# Sheldrick geometric approximatio 0.45 0.82 
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_T_max  0.82
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      180
_diffrn_ambient_pressure         101
_diffrn_reflns_number            26066
_reflns_number_total             10476
_diffrn_reflns_av_R_equivalents  0.026
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 10476 
# Theoretical number of reflections is about 21744 


_diffrn_reflns_theta_min         4.651
_diffrn_reflns_theta_max         75.985
_diffrn_measured_fraction_theta_max 0.962

_diffrn_reflns_theta_full        69.147
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              -34
_reflns_limit_h_max              22
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   4.25
_oxford_diffrn_Wilson_scale      0.30

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.51
_refine_diff_density_max         0.57


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         10434
_refine_ls_number_restraints     262
_refine_ls_number_parameters     791
_oxford_refine_ls_R_factor_ref   0.0765
_refine_ls_wR_factor_ref         0.1309
_refine_ls_goodness_of_fit_ref   1.0005
_refine_ls_shift/su_max          0.0030609
_refine_ls_shift/su_mean         0.0000634


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10436
_refine_ls_R_factor_all          0.0766
_refine_ls_wR_factor_all         0.1310

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7831
_refine_ls_R_factor_gt           0.0588
_refine_ls_wR_factor_gt          0.1079

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 737. 0.115E+04 560. 132. 0.00 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.10600(15) 0.55465(17) 0.2674(2) 0.0448 1.0000 Uani . . . . . .
S2 S 0.05099(4) 0.50350(5) 0.13626(6) 0.0480 1.0000 Uani . . . . . .
C3 C 0.11720(14) 0.45793(16) 0.1515(2) 0.0409 1.0000 Uani . . . . . .
C4 C 0.10340(15) 0.37694(17) 0.1154(2) 0.0441 1.0000 Uani . . . . . .
C5 C 0.14778(16) 0.34147(16) 0.1130(2) 0.0454 1.0000 Uani . . . . . .
C6 C 0.20650(17) 0.38173(17) 0.1468(2) 0.0479 1.0000 Uani . . . . . .
C7 C 0.22038(16) 0.46263(17) 0.1825(2) 0.0441 1.0000 Uani . . . . . .
S8 S 0.28876(5) 0.51687(5) 0.20979(8) 0.0601 1.0000 Uani . . . . . .
C9 C 0.34698(17) 0.56012(18) 0.3467(3) 0.0490 1.0000 Uani . . . . . .
C10 C 0.35864(18) 0.64438(19) 0.3580(3) 0.0529 1.0000 Uani . . . . . .
C11 C 0.40708(19) 0.67890(19) 0.4645(3) 0.0542 1.0000 Uani . . . . . .
C12 C 0.44444(18) 0.6337(2) 0.5611(3) 0.0554 1.0000 Uani . . . . . .
C13 C 0.43252(16) 0.54975(19) 0.5497(3) 0.0520 1.0000 Uani . . . . . .
S14 S 0.48686(4) 0.49211(6) 0.67642(8) 0.0667 1.0000 Uani . . . . . .
C15 C 0.41730(16) 0.4436(2) 0.6519(2) 0.0517 1.0000 Uani . . . . . .
C16 C 0.41899(16) 0.3600(2) 0.6606(3) 0.0537 1.0000 Uani . . . . . .
C17 C 0.36945(16) 0.32101(19) 0.6509(2) 0.0509 1.0000 Uani . . . . . .
C18 C 0.31627(16) 0.36368(19) 0.6304(2) 0.0498 1.0000 Uani . . . . . .
C19 C 0.31384(16) 0.44791(19) 0.6211(2) 0.0469 1.0000 Uani . . . . . .
S20 S 0.24945(5) 0.50224(6) 0.60331(7) 0.0591 1.0000 Uani . . . . . .
C21 C 0.19224(16) 0.55331(19) 0.4714(2) 0.0474 1.0000 Uani . . . . . .
C22 C 0.17918(18) 0.63630(19) 0.4667(3) 0.0536 1.0000 Uani . . . . . .
C23 C 0.12996(19) 0.67668(19) 0.3628(3) 0.0536 1.0000 Uani . . . . . .
C24 C 0.09403(17) 0.63729(18) 0.2638(3) 0.0492 1.0000 Uani . . . . . .
C25 C 0.17478(16) 0.50126(16) 0.1835(2) 0.0418 1.0000 Uani . . . . . .
C26 C 0.38447(16) 0.51243(18) 0.4427(3) 0.0486 1.0000 Uani . . . . . .
C27 C 0.36505(16) 0.48923(19) 0.6339(2) 0.0474 1.0000 Uani . . . . . .
C28 C 0.15452(15) 0.51140(17) 0.3709(2) 0.0438 1.0000 Uani . . . . . .
O29 O 0.18895(12) 0.58055(11) 0.21827(16) 0.0506 1.0000 Uani D U . . . .
C30 C 0.14303(19) 0.64015(16) 0.1268(3) 0.0599 1.0000 Uani D . . . . .
C31 C 0.1694(2) 0.72421(17) 0.1823(3) 0.0700 1.0000 Uani D . . . . .
C32 C 0.1158(2) 0.7940(2) 0.1012(4) 0.0673 0.681(15) Uani D U P 4 1 .
C33 C 0.1528(5) 0.8768(2) 0.1631(7) 0.0722 0.681(15) Uani D U P 4 1 .
C34 C 0.1002(6) 0.9475(3) 0.0824(9) 0.0969 0.681(15) Uani D U P 4 1 .
C35 C 0.1331(7) 1.0293(4) 0.1472(11) 0.0971 0.681(15) Uani D U P 4 1 .
O36 O 0.37345(13) 0.43002(13) 0.4336(2) 0.0586 1.0000 Uani D U . . . .
C37 C 0.4229(5) 0.3864(3) 0.4396(9) 0.0789 0.786(5) Uani D U P 2 1 .
C38 C 0.4280(3) 0.2967(3) 0.4683(5) 0.0820 0.786(5) Uani D U P 2 1 .
C39 C 0.3533(3) 0.2520(3) 0.3848(5) 0.0896 0.786(5) Uani D U P 2 1 .
C40 C 0.3575(4) 0.1624(3) 0.4149(6) 0.0947 0.786(5) Uani D U P 2 1 .
C41 C 0.4090(4) 0.1082(3) 0.4269(5) 0.1078 0.786(5) Uani D U P 2 1 .
C42 C 0.4050(5) 0.0175(3) 0.4448(7) 0.1130 0.786(5) Uani D U P 2 1 .
O43 O 0.36233(12) 0.57220(13) 0.62532(16) 0.0536 1.0000 Uani D U . . . .
C44 C 0.4171(3) 0.6145(3) 0.7355(3) 0.0610 0.719(8) Uani D U P 3 1 .
C45 C 0.3837(4) 0.6986(3) 0.7128(5) 0.0574 0.719(8) Uani D U P 3 1 .
C46 C 0.3726(3) 0.7498(3) 0.6289(5) 0.0590 0.719(8) Uani D U P 3 1 .
C47 C 0.3392(5) 0.8347(4) 0.6092(7) 0.0630 0.719(8) Uani D U P 3 1 .
C48 C 0.3277(5) 0.8850(4) 0.5244(7) 0.0839 0.719(8) Uani D U P 3 1 .
C49 C 0.2866(6) 0.9665(5) 0.4918(9) 0.1110 0.719(8) Uani D U P 3 1 .
O50 O 0.16728(11) 0.43015(12) 0.37374(17) 0.0507 1.0000 Uani D U . . . .
C51 C 0.11541(19) 0.37430(19) 0.3494(3) 0.0669 1.0000 Uani D . . . . .
C52 C 0.1368(2) 0.2888(2) 0.3459(4) 0.0743 1.0000 Uani D . . . . .
C53 C 0.0800(8) 0.2266(4) 0.309(2) 0.0988 0.586(6) Uani D U P 1 1 .
C54 C 0.1138(5) 0.1401(4) 0.3428(8) 0.0974 0.586(6) Uani D U P 1 1 .
C55 C 0.0619(5) 0.0790(5) 0.3214(10) 0.1021 0.586(6) Uani D U P 1 1 .
C56 C 0.0862(7) -0.0082(5) 0.3296(12) 0.1254 0.586(6) Uani D U P 1 1 .
N57 N 0.13176(16) 0.25701(16) 0.0726(3) 0.0611 1.0000 Uani . . . . . .
O58 O 0.17770(15) 0.22090(15) 0.0870(2) 0.0764 1.0000 Uani . . . . . .
O59 O 0.07180(17) 0.22731(17) 0.0227(3) 0.1002 1.0000 Uani . . . . . .
N60 N 0.4185(2) 0.76829(18) 0.4763(3) 0.0683 1.0000 Uani . . . . . .
O61 O 0.46884(18) 0.79667(17) 0.5735(3) 0.0854 1.0000 Uani . . . . . .
O62 O 0.3778(2) 0.80838(16) 0.3887(3) 0.0923 1.0000 Uani . . . . . .
N63 N 0.37109(16) 0.23189(18) 0.6581(2) 0.0622 1.0000 Uani . . . . . .
O64 O 0.3289(2) 0.19835(18) 0.6531(3) 0.0984 1.0000 Uani . . . . . .
O65 O 0.41523(15) 0.19444(16) 0.6693(2) 0.0756 1.0000 Uani . . . . . .
N66 N 0.1169(2) 0.76452(18) 0.3584(3) 0.0702 1.0000 Uani . . . . . .
O67 O 0.0797(2) 0.80060(17) 0.2688(3) 0.1040 1.0000 Uani . . . . . .
O68 O 0.1444(2) 0.79680(16) 0.4454(3) 0.0919 1.0000 Uani . . . . . .
C132 C 0.1160(2) 0.7864(2) 0.0840(4) 0.0656 0.319(15) Uani D U P 4 2 .
C133 C 0.1277(5) 0.8739(2) 0.1276(7) 0.0794 0.319(15) Uani D U P 4 2 .
C134 C 0.0779(11) 0.9341(7) 0.0266(12) 0.0931 0.319(15) Uani D U P 4 2 .
C135 C 0.0979(12) 1.0224(7) 0.072(2) 0.0943 0.319(15) Uani D U P 4 2 .
C137 C 0.409(2) 0.3731(8) 0.425(4) 0.0808 0.214(5) Uani D U P 2 2 .
C138 C 0.3753(12) 0.2913(8) 0.408(2) 0.1403 0.214(5) Uani D U P 2 2 .
C139 C 0.4193(12) 0.2229(8) 0.420(2) 0.1439 0.214(5) Uani D U P 2 2 .
C140 C 0.4105(10) 0.1492(9) 0.4622(14) 0.0956 0.214(5) Uani D U P 2 2 .
C141 C 0.3323(10) 0.1097(11) 0.3649(17) 0.1239 0.214(5) Uani D U P 2 2 .
C142 C 0.3444(17) 0.0166(10) 0.383(3) 0.1362 0.214(5) Uani D U P 2 2 .
C144 C 0.3893(10) 0.6132(7) 0.7229(10) 0.0807 0.281(8) Uani D U P 3 2 .
C145 C 0.4060(6) 0.7025(7) 0.7241(12) 0.0557 0.281(8) Uani D U P 3 2 .
C146 C 0.3362(8) 0.7470(7) 0.6128(12) 0.0844 0.281(8) Uani D U P 3 2 .
C147 C 0.3563(8) 0.8360(9) 0.6160(16) 0.0646 0.281(8) Uani D U P 3 2 .
C148 C 0.2893(10) 0.8804(9) 0.5021(14) 0.1052 0.281(8) Uani D U P 3 2 .
C149 C 0.3112(12) 0.9717(9) 0.5240(18) 0.0800 0.281(8) Uani D U P 3 2 .
C153 C 0.0852(14) 0.2187(7) 0.312(3) 0.0982 0.414(6) Uani D U P 1 2 .
C154 C 0.1033(8) 0.1387(6) 0.2902(12) 0.0986 0.414(6) Uani D U P 1 2 .
C155 C 0.0566(7) 0.0640(6) 0.2621(10) 0.1017 0.414(6) Uani D U P 1 2 .
C156 C 0.0911(10) 0.0275(10) 0.3729(12) 0.1255 0.414(6) Uani D U P 1 2 .
H41 H 0.0646 0.3482 0.0935 0.0532 1.0000 Uiso R . . . . .
H61 H 0.2372 0.3557 0.1478 0.0572 1.0000 Uiso R . . . . .
H101 H 0.3333 0.6758 0.2936 0.0634 1.0000 Uiso R . . . . .
H121 H 0.4750 0.6602 0.6316 0.0657 1.0000 Uiso R . . . . .
H161 H 0.4538 0.3287 0.6738 0.0631 1.0000 Uiso R . . . . .
H181 H 0.2829 0.3358 0.6231 0.0601 1.0000 Uiso R . . . . .
H221 H 0.2032 0.6648 0.5312 0.0628 1.0000 Uiso R . . . . .
H241 H 0.0610 0.6662 0.1942 0.0583 1.0000 Uiso R . . . . .
H512 H 0.1191 0.3787 0.4076 0.0793 1.0000 Uiso R . . . . .
H511 H 0.0619 0.3870 0.2735 0.0801 1.0000 Uiso R . . . . .
H532 H 0.0706 0.2385 0.3534 0.1202 0.586(6) Uiso R . P 1 1 .
H531 H 0.0308 0.2311 0.2252 0.1202 0.586(6) Uiso R . P 1 1 .
H542 H 0.1640 0.1357 0.4234 0.1241 0.586(6) Uiso R . P 1 1 .
H541 H 0.1176 0.1263 0.2941 0.1239 0.586(6) Uiso R . P 1 1 .
H551 H 0.0629 0.0898 0.3772 0.1350 0.586(6) Uiso R . P 1 1 .
H552 H 0.0102 0.0873 0.2419 0.1352 0.586(6) Uiso R . P 1 1 .
H562 H 0.0575 -0.0455 0.3277 0.1991 0.586(6) Uiso R . P 1 1 .
H561 H 0.1398 -0.0119 0.4029 0.1989 0.586(6) Uiso R . P 1 1 .
H563 H 0.0772 -0.0189 0.2669 0.1992 0.586(6) Uiso R . P 1 1 .
H1531 H 0.0903 0.2089 0.3723 0.1193 0.414(6) Uiso R . P 1 2 .
H1532 H 0.0328 0.2356 0.2400 0.1191 0.414(6) Uiso R . P 1 2 .
H1542 H 0.1570 0.1270 0.3565 0.1208 0.414(6) Uiso R . P 1 2 .
H1541 H 0.0903 0.1471 0.2234 0.1210 0.414(6) Uiso R . P 1 2 .
H1551 H 0.0039 0.0795 0.2092 0.1170 0.414(6) Uiso R . P 1 2 .
H1552 H 0.0586 0.0214 0.2268 0.1171 0.414(6) Uiso R . P 1 2 .
H1561 H 0.0628 -0.0210 0.3575 0.1760 0.414(6) Uiso R . P 1 2 .
H1563 H 0.0882 0.0712 0.4077 0.1760 0.414(6) Uiso R . P 1 2 .
H1562 H 0.1444 0.0131 0.4258 0.1759 0.414(6) Uiso R . P 1 2 .
H371 H 0.4739 0.4108 0.4984 0.0982 0.786(5) Uiso R . P 2 1 .
H372 H 0.4017 0.3897 0.3636 0.0979 0.786(5) Uiso R . P 2 1 .
H381 H 0.4515 0.2933 0.5457 0.1062 0.786(5) Uiso R . P 2 1 .
H382 H 0.4590 0.2686 0.4664 0.1055 0.786(5) Uiso R . P 2 1 .
H392 H 0.3262 0.2815 0.3921 0.1154 0.786(5) Uiso R . P 2 1 .
H391 H 0.3284 0.2564 0.3069 0.1158 0.786(5) Uiso R . P 2 1 .
H402 H 0.3741 0.1586 0.4869 0.1198 0.786(5) Uiso R . P 2 1 .
H401 H 0.3069 0.1372 0.3514 0.1188 0.786(5) Uiso R . P 2 1 .
H411 H 0.4628 0.1276 0.4912 0.1396 0.786(5) Uiso R . P 2 1 .
H412 H 0.3913 0.1132 0.3541 0.1394 0.786(5) Uiso R . P 2 1 .
H422 H 0.4461 -0.0121 0.4660 0.1787 0.786(5) Uiso R . P 2 1 .
H421 H 0.4135 0.0120 0.5088 0.1790 0.786(5) Uiso R . P 2 1 .
H423 H 0.3559 -0.0037 0.3739 0.1791 0.786(5) Uiso R . P 2 1 .
H1371 H 0.4600 0.3685 0.5032 0.0989 0.214(5) Uiso R . P 2 2 .
H1372 H 0.4113 0.3896 0.3753 0.0990 0.214(5) Uiso R . P 2 2 .
H1381 H 0.3628 0.2828 0.4458 0.1609 0.214(5) Uiso R . P 2 2 .
H1382 H 0.3297 0.2936 0.3257 0.1611 0.214(5) Uiso R . P 2 2 .
H1391 H 0.4722 0.2386 0.4821 0.1470 0.214(5) Uiso R . P 2 2 .
H1392 H 0.4048 0.2073 0.3533 0.1471 0.214(5) Uiso R . P 2 2 .
H1402 H 0.4495 0.1082 0.5006 0.1201 0.214(5) Uiso R . P 2 2 .
H1401 H 0.4126 0.1700 0.5155 0.1200 0.214(5) Uiso R . P 2 2 .
H1412 H 0.3158 0.1205 0.2954 0.1320 0.214(5) Uiso R . P 2 2 .
H1411 H 0.2955 0.1316 0.3571 0.1319 0.214(5) Uiso R . P 2 2 .
H1421 H 0.2882 -0.0123 0.2904 0.2120 0.214(5) Uiso R . P 2 2 .
H1422 H 0.4013 -0.0017 0.4157 0.2120 0.214(5) Uiso R . P 2 2 .
H1423 H 0.3478 0.0087 0.4535 0.2120 0.214(5) Uiso R . P 2 2 .
H441 H 0.4661 0.6184 0.7676 0.0740 0.719(8) Uiso R . P 3 1 .
H442 H 0.4218 0.5851 0.7885 0.0742 0.719(8) Uiso R . P 3 1 .
H451 H 0.4200 0.7279 0.7864 0.0704 0.719(8) Uiso R . P 3 1 .
H452 H 0.3373 0.6926 0.6874 0.0693 0.719(8) Uiso R . P 3 1 .
H462 H 0.4207 0.7558 0.6568 0.0730 0.719(8) Uiso R . P 3 1 .
H461 H 0.3379 0.7213 0.5564 0.0729 0.719(8) Uiso R . P 3 1 .
H472 H 0.3735 0.8646 0.6812 0.0748 0.719(8) Uiso R . P 3 1 .
H471 H 0.2917 0.8287 0.5803 0.0746 0.719(8) Uiso R . P 3 1 .
H481 H 0.3772 0.8935 0.5579 0.1040 0.719(8) Uiso R . P 3 1 .
H482 H 0.2934 0.8537 0.4529 0.1036 0.719(8) Uiso R . P 3 1 .
H492 H 0.2751 0.9916 0.4308 0.1701 0.719(8) Uiso R . P 3 1 .
H491 H 0.3198 1.0013 0.5596 0.1699 0.719(8) Uiso R . P 3 1 .
H493 H 0.2393 0.9556 0.4641 0.1700 0.719(8) Uiso R . P 3 1 .
H1441 H 0.4341 0.5864 0.7935 0.0970 0.281(8) Uiso R . P 3 2 .
H1442 H 0.3504 0.6115 0.7160 0.0970 0.281(8) Uiso R . P 3 2 .
H1451 H 0.4240 0.7299 0.7897 0.0641 0.281(8) Uiso R . P 3 2 .
H1452 H 0.4453 0.7042 0.7315 0.0641 0.281(8) Uiso R . P 3 2 .
H1461 H 0.2975 0.7480 0.6069 0.1030 0.281(8) Uiso R . P 3 2 .
H1462 H 0.3171 0.7184 0.5473 0.1030 0.281(8) Uiso R . P 3 2 .
H1472 H 0.3723 0.8657 0.6787 0.0749 0.281(8) Uiso R . P 3 2 .
H1471 H 0.3970 0.8355 0.6264 0.0750 0.281(8) Uiso R . P 3 2 .
H1482 H 0.2453 0.8748 0.4833 0.1269 0.281(8) Uiso R . P 3 2 .
H1481 H 0.2775 0.8589 0.4396 0.1267 0.281(8) Uiso R . P 3 2 .
H1491 H 0.2695 1.0028 0.4565 0.1152 0.281(8) Uiso R . P 3 2 .
H1492 H 0.3247 0.9921 0.5880 0.1149 0.281(8) Uiso R . P 3 2 .
H1493 H 0.3537 0.9772 0.5400 0.1150 0.281(8) Uiso R . P 3 2 .
H302 H 0.1486 0.6339 0.0786 0.0732 1.0000 Uiso R . . . . .
H301 H 0.0900 0.6324 0.0800 0.0742 1.0000 Uiso R . . . . .
H321 H 0.1096 0.7965 0.0395 0.0856 0.681(15) Uiso R . P 4 1 .
H322 H 0.0669 0.7836 0.0690 0.0852 0.681(15) Uiso R . P 4 1 .
H331 H 0.2047 0.8830 0.2057 0.0933 0.681(15) Uiso R . P 4 1 .
H332 H 0.1510 0.8776 0.2156 0.0928 0.681(15) Uiso R . P 4 1 .
H341 H 0.1011 0.9472 0.0285 0.1131 0.681(15) Uiso R . P 4 1 .
H342 H 0.0486 0.9419 0.0413 0.1123 0.681(15) Uiso R . P 4 1 .
H351 H 0.0977 1.0735 0.1005 0.1411 0.681(15) Uiso R . P 4 1 .
H353 H 0.1802 1.0415 0.1753 0.1409 0.681(15) Uiso R . P 4 1 .
H352 H 0.1443 1.0231 0.2128 0.1411 0.681(15) Uiso R . P 4 1 .
H1322 H 0.1108 0.7767 0.0243 0.0872 0.319(15) Uiso R . P 4 2 .
H1321 H 0.0670 0.7792 0.0519 0.0871 0.319(15) Uiso R . P 4 2 .
H1332 H 0.1747 0.8846 0.1544 0.0903 0.319(15) Uiso R . P 4 2 .
H1331 H 0.1370 0.8827 0.1905 0.0905 0.319(15) Uiso R . P 4 2 .
H1341 H 0.0716 0.9318 -0.0353 0.1130 0.319(15) Uiso R . P 4 2 .
H1342 H 0.0299 0.9189 -0.0060 0.1131 0.319(15) Uiso R . P 4 2 .
H1352 H 0.0664 1.0610 0.0097 0.1410 0.319(15) Uiso R . P 4 2 .
H1353 H 0.1503 1.0312 0.1198 0.1412 0.319(15) Uiso R . P 4 2 .
H1351 H 0.0908 1.0280 0.1176 0.1409 0.319(15) Uiso R . P 4 2 .
H522 H 0.1871 0.2753 0.4197 0.0905 1.0000 Uiso R . . . . .
H521 H 0.1360 0.2874 0.2915 0.0905 1.0000 Uiso R . . . . .
H312 H 0.2176 0.7354 0.2152 0.0846 1.0000 Uiso R . . . . .
H311 H 0.1768 0.7231 0.2439 0.0846 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.931(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . S2 . 1.769(3) yes
C1 . C24 . 1.380(4) yes
C1 . C28 . 1.404(4) yes
S2 . C3 . 1.772(3) yes
C3 . C4 . 1.394(4) yes
C3 . C25 . 1.388(4) yes
C4 . C5 . 1.372(4) yes
C4 . H41 . 0.929 no
C5 . C6 . 1.374(4) yes
C5 . N57 . 1.463(4) yes
C6 . C7 . 1.391(4) yes
C6 . H61 . 0.928 no
C7 . S8 . 1.765(3) yes
C7 . C25 . 1.406(4) yes
S8 . C9 . 1.771(3) yes
C9 . C10 . 1.393(4) yes
C9 . C26 . 1.396(4) yes
C10 . C11 . 1.373(4) yes
C10 . H101 . 0.930 no
C11 . C12 . 1.381(5) yes
C11 . N60 . 1.476(4) yes
C12 . C13 . 1.389(4) yes
C12 . H121 . 0.939 no
C13 . S14 . 1.772(3) yes
C13 . C26 . 1.399(4) yes
S14 . C15 . 1.776(3) yes
C15 . C16 . 1.371(4) yes
C15 . C27 . 1.411(4) yes
C16 . C17 . 1.380(4) yes
C16 . H161 . 0.936 no
C17 . C18 . 1.384(4) yes
C17 . N63 . 1.460(4) yes
C18 . C19 . 1.383(4) yes
C18 . H181 . 0.933 no
C19 . S20 . 1.766(3) yes
C19 . C27 . 1.405(4) yes
S20 . C21 . 1.769(3) yes
C21 . C22 . 1.389(4) yes
C21 . C28 . 1.402(4) yes
C22 . C23 . 1.384(4) yes
C22 . H221 . 0.914 no
C23 . C24 . 1.374(4) yes
C23 . N66 . 1.467(4) yes
C24 . H241 . 0.942 no
C25 . O29 . 1.361(3) yes
C26 . O36 . 1.363(3) yes
C27 . O43 . 1.361(4) yes
C28 . O50 . 1.364(3) yes
O29 . C30 . 1.446(3) yes
C30 . C31 . 1.520(3) yes
C30 . H302 . 0.989 no
C30 . H301 . 0.983 no
C31 . C32 . 1.526(3) yes
C31 . H312 . 0.965 no
C31 . H311 . 0.960 no
C31 . C132 . 1.538(3) yes
C31 . H312 . 0.965 no
C31 . H311 . 0.960 no
C32 . C33 . 1.544(3) yes
C32 . H321 . 0.988 no
C32 . H322 . 0.985 no
C33 . C34 . 1.530(4) yes
C33 . H331 . 0.977 no
C33 . H332 . 0.980 no
C34 . C35 . 1.536(5) yes
C34 . H341 . 0.986 no
C34 . H342 . 0.978 no
C35 . H351 . 0.965 no
C35 . H353 . 0.979 no
C35 . H352 . 0.973 no
O36 . C37 . 1.454(4) yes
O36 . C137 . 1.436(5) yes
C37 . C38 . 1.525(4) yes
C37 . H371 . 0.990 no
C37 . H372 . 1.000 no
C38 . C39 . 1.515(4) yes
C38 . H381 . 0.997 no
C38 . H382 . 0.985 no
C39 . C40 . 1.536(4) yes
C39 . H392 . 0.971 no
C39 . H391 . 0.990 no
C40 . C41 . 1.531(5) yes
C40 . H402 . 0.995 no
C40 . H401 . 0.993 no
C41 . C42 . 1.538(4) yes
C41 . H411 . 1.006 no
C41 . H412 . 0.994 no
C42 . H422 . 0.994 no
C42 . H421 . 0.989 no
C42 . H423 . 0.973 no
O43 . C44 . 1.462(4) yes
O43 . C144 . 1.449(5) yes
C44 . C45 . 1.524(4) yes
C44 . H441 . 0.974 no
C44 . H442 . 0.984 no
C45 . C46 . 1.540(4) yes
C45 . H451 . 0.984 no
C45 . H452 . 0.970 no
C46 . C47 . 1.546(4) yes
C46 . H462 . 0.989 no
C46 . H461 . 0.967 no
C47 . C48 . 1.539(5) yes
C47 . H472 . 0.974 no
C47 . H471 . 0.968 no
C48 . C49 . 1.541(5) yes
C48 . H481 . 0.985 no
C48 . H482 . 0.980 no
C49 . H492 . 0.973 no
C49 . H491 . 0.976 no
C49 . H493 . 0.984 no
O50 . C51 . 1.444(3) yes
C51 . C52 . 1.533(4) yes
C51 . H512 . 0.974 no
C51 . H511 . 1.005 no
C52 . C53 . 1.523(5) yes
C52 . H522 . 0.963 no
C52 . H521 . 0.959 no
C52 . C153 . 1.537(5) yes
C52 . H522 . 0.963 no
C52 . H521 . 0.959 no
C53 . C54 . 1.540(5) yes
C53 . H532 . 1.016 no
C53 . H531 . 1.007 no
C54 . C55 . 1.525(5) yes
C54 . H542 . 0.982 no
C54 . H541 . 0.979 no
C55 . C56 . 1.532(5) yes
C55 . H551 . 0.995 no
C55 . H552 . 0.994 no
C56 . H562 . 0.974 no
C56 . H561 . 0.975 no
C56 . H563 . 0.969 no
N57 . O58 . 1.222(3) yes
N57 . O59 . 1.220(4) yes
N60 . O61 . 1.227(4) yes
N60 . O62 . 1.219(4) yes
N63 . O64 . 1.215(4) yes
N63 . O65 . 1.223(4) yes
N66 . O67 . 1.221(4) yes
N66 . O68 . 1.223(4) yes
C132 . C133 . 1.543(3) yes
C132 . H1322 . 0.983 no
C132 . H1321 . 0.980 no
C133 . C134 . 1.538(5) yes
C133 . H1332 . 0.983 no
C133 . H1331 . 0.962 no
C134 . C135 . 1.540(5) yes
C134 . H1341 . 0.988 no
C134 . H1342 . 0.976 no
C135 . H1352 . 0.966 no
C135 . H1353 . 0.971 no
C135 . H1351 . 0.972 no
C137 . C138 . 1.517(5) yes
C137 . H1371 . 0.971 no
C137 . H1372 . 0.978 no
C138 . C139 . 1.528(5) yes
C138 . H1381 . 0.972 no
C138 . H1382 . 0.970 no
C139 . C140 . 1.533(5) yes
C139 . H1391 . 0.974 no
C139 . H1392 . 0.974 no
C140 . C141 . 1.536(5) yes
C140 . H1402 . 0.972 no
C140 . H1401 . 0.976 no
C141 . C142 . 1.540(5) yes
C141 . H1412 . 0.967 no
C141 . H1411 . 0.970 no
C142 . H1421 . 1.209 no
C142 . H1422 . 1.203 no
C142 . H1423 . 1.211 no
C144 . C145 . 1.525(5) yes
C144 . H1441 . 0.970 no
C144 . H1442 . 0.972 no
C145 . C146 . 1.540(5) yes
C145 . H1451 . 0.975 no
C145 . H1452 . 0.974 no
C146 . C147 . 1.540(5) yes
C146 . H1461 . 0.976 no
C146 . H1462 . 0.972 no
C147 . C148 . 1.541(5) yes
C147 . H1472 . 0.973 no
C147 . H1471 . 0.974 no
C148 . C149 . 1.542(5) yes
C148 . H1482 . 0.974 no
C148 . H1481 . 0.968 no
C149 . H1491 . 0.964 no
C149 . H1492 . 0.962 no
C149 . H1493 . 0.963 no
C153 . C154 . 1.548(5) yes
C153 . H1531 . 0.994 no
C153 . H1532 . 0.992 no
C154 . C155 . 1.547(5) yes
C154 . H1542 . 0.977 no
C154 . H1541 . 0.968 no
C155 . C156 . 1.535(5) yes
C155 . H1551 . 0.979 no
C155 . H1552 . 0.970 no
C156 . H1561 . 0.988 no
C156 . H1563 . 0.990 no
C156 . H1562 . 0.988 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 . C1 . C24 . 118.0(2) yes
S2 . C1 . C28 . 121.2(2) yes
C24 . C1 . C28 . 120.4(3) yes
C1 . S2 . C3 . 104.92(12) yes
S2 . C3 . C4 . 116.3(2) yes
S2 . C3 . C25 . 123.3(2) yes
C4 . C3 . C25 . 119.9(2) yes
C3 . C4 . C5 . 118.9(3) yes
C3 . C4 . H41 . 119.7 no
C5 . C4 . H41 . 121.5 no
C4 . C5 . C6 . 122.9(3) yes
C4 . C5 . N57 . 118.4(3) yes
C6 . C5 . N57 . 118.7(3) yes
C5 . C6 . C7 . 118.5(3) yes
C5 . C6 . H61 . 121.4 no
C7 . C6 . H61 . 120.1 no
C6 . C7 . S8 . 117.8(2) yes
C6 . C7 . C25 . 119.9(3) yes
S8 . C7 . C25 . 121.9(2) yes
C7 . S8 . C9 . 103.38(13) yes
S8 . C9 . C10 . 117.5(2) yes
S8 . C9 . C26 . 122.4(2) yes
C10 . C9 . C26 . 120.0(3) yes
C9 . C10 . C11 . 118.8(3) yes
C9 . C10 . H101 . 119.5 no
C11 . C10 . H101 . 121.8 no
C10 . C11 . C12 . 122.8(3) yes
C10 . C11 . N60 . 118.8(3) yes
C12 . C11 . N60 . 118.4(3) yes
C11 . C12 . C13 . 118.4(3) yes
C11 . C12 . H121 . 119.9 no
C13 . C12 . H121 . 121.6 no
C12 . C13 . S14 . 117.5(2) yes
C12 . C13 . C26 . 120.2(3) yes
S14 . C13 . C26 . 122.0(2) yes
C13 . S14 . C15 . 102.96(13) yes
S14 . C15 . C16 . 118.7(2) yes
S14 . C15 . C27 . 121.5(2) yes
C16 . C15 . C27 . 119.6(3) yes
C15 . C16 . C17 . 120.1(3) yes
C15 . C16 . H161 . 120.9 no
C17 . C16 . H161 . 119.0 no
C16 . C17 . C18 . 121.9(3) yes
C16 . C17 . N63 . 119.3(3) yes
C18 . C17 . N63 . 118.8(3) yes
C17 . C18 . C19 . 118.6(3) yes
C17 . C18 . H181 . 120.2 no
C19 . C18 . H181 . 121.2 no
C18 . C19 . S20 . 118.2(2) yes
C18 . C19 . C27 . 120.6(3) yes
S20 . C19 . C27 . 121.1(2) yes
C19 . S20 . C21 . 103.01(13) yes
S20 . C21 . C22 . 117.9(2) yes
S20 . C21 . C28 . 122.2(2) yes
C22 . C21 . C28 . 119.7(3) yes
C21 . C22 . C23 . 119.3(3) yes
C21 . C22 . H221 . 121.2 no
C23 . C22 . H221 . 119.5 no
C22 . C23 . C24 . 121.9(3) yes
C22 . C23 . N66 . 119.1(3) yes
C24 . C23 . N66 . 118.9(3) yes
C1 . C24 . C23 . 119.2(3) yes
C1 . C24 . H241 . 120.4 no
C23 . C24 . H241 . 120.4 no
C7 . C25 . C3 . 119.9(2) yes
C7 . C25 . O29 . 119.2(3) yes
C3 . C25 . O29 . 120.9(2) yes
C13 . C26 . C9 . 119.8(3) yes
C13 . C26 . O36 . 119.2(3) yes
C9 . C26 . O36 . 121.0(3) yes
C15 . C27 . C19 . 119.2(3) yes
C15 . C27 . O43 . 120.8(3) yes
C19 . C27 . O43 . 119.9(3) yes
C1 . C28 . C21 . 119.4(3) yes
C1 . C28 . O50 . 119.8(2) yes
C21 . C28 . O50 . 120.7(3) yes
C25 . O29 . C30 . 114.9(2) yes
O29 . C30 . C31 . 107.1(2) yes
O29 . C30 . H302 . 110.3 no
C31 . C30 . H302 . 110.9 no
O29 . C30 . H301 . 109.2 no
C31 . C30 . H301 . 109.5 no
H302 . C30 . H301 . 109.8 no
C30 . C31 . C32 . 114.6(3) yes
C30 . C31 . H312 . 108.6 no
C32 . C31 . H312 . 108.5 no
C30 . C31 . H311 . 108.6 no
C32 . C31 . H311 . 108.9 no
H312 . C31 . H311 . 107.4 no
C30 . C31 . C132 . 106.3(3) yes
C30 . C31 . H312 . 108.6 no
C132 . C31 . H312 . 104.0 no
C30 . C31 . H311 . 108.6 no
C132 . C31 . H311 . 121.4 no
H312 . C31 . H311 . 107.4 no
C31 . C32 . C33 . 109.8(3) yes
C31 . C32 . H321 . 109.0 no
C33 . C32 . H321 . 103.4 no
C31 . C32 . H322 . 108.8 no
C33 . C32 . H322 . 115.3 no
H321 . C32 . H322 . 110.3 no
C32 . C33 . C34 . 110.5(4) yes
C32 . C33 . H331 . 115.0 no
C34 . C33 . H331 . 115.0 no
C32 . C33 . H332 . 102.8 no
C34 . C33 . H332 . 101.8 no
H331 . C33 . H332 . 110.3 no
C33 . C34 . C35 . 110.6(5) yes
C33 . C34 . H341 . 102.7 no
C35 . C34 . H341 . 108.2 no
C33 . C34 . H342 . 114.9 no
C35 . C34 . H342 . 109.5 no
H341 . C34 . H342 . 110.6 no
C34 . C35 . H351 . 111.7 no
C34 . C35 . H353 . 110.6 no
H351 . C35 . H353 . 110.6 no
C34 . C35 . H352 . 107.0 no
H351 . C35 . H352 . 108.4 no
H353 . C35 . H352 . 108.3 no
C26 . O36 . C37 . 111.6(3) yes
C26 . O36 . C137 . 123.3(7) yes
O36 . C37 . C38 . 109.8(4) yes
O36 . C37 . H371 . 110.8 no
C38 . C37 . H371 . 109.4 no
O36 . C37 . H372 . 109.2 no
C38 . C37 . H372 . 108.8 no
H371 . C37 . H372 . 108.8 no
C37 . C38 . C39 . 114.8(4) yes
C37 . C38 . H381 . 108.8 no
C39 . C38 . H381 . 108.1 no
C37 . C38 . H382 . 107.3 no
C39 . C38 . H382 . 106.6 no
H381 . C38 . H382 . 111.2 no
C38 . C39 . C40 . 115.2(4) yes
C38 . C39 . H392 . 102.5 no
C40 . C39 . H392 . 106.7 no
C38 . C39 . H391 . 109.1 no
C40 . C39 . H391 . 110.7 no
H392 . C39 . H391 . 112.3 no
C39 . C40 . C41 . 114.6(5) yes
C39 . C40 . H402 . 110.8 no
C41 . C40 . H402 . 108.5 no
C39 . C40 . H401 . 108.9 no
C41 . C40 . H401 . 104.4 no
H402 . C40 . H401 . 109.4 no
C40 . C41 . C42 . 112.5(5) yes
C40 . C41 . H411 . 111.1 no
C42 . C41 . H411 . 109.7 no
C40 . C41 . H412 . 106.8 no
C42 . C41 . H412 . 108.2 no
H411 . C41 . H412 . 108.3 no
C41 . C42 . H422 . 108.1 no
C41 . C42 . H421 . 110.0 no
H422 . C42 . H421 . 108.0 no
C41 . C42 . H423 . 108.4 no
H422 . C42 . H423 . 111.0 no
H421 . C42 . H423 . 111.3 no
C27 . O43 . C44 . 114.0(3) yes
C27 . O43 . C144 . 113.0(5) yes
O43 . C44 . C45 . 106.0(4) yes
O43 . C44 . H441 . 111.5 no
C45 . C44 . H441 . 111.8 no
O43 . C44 . H442 . 109.0 no
C45 . C44 . H442 . 108.2 no
H441 . C44 . H442 . 110.2 no
C44 . C45 . C46 . 112.7(4) yes
C44 . C45 . H451 . 107.0 no
C46 . C45 . H451 . 107.4 no
C44 . C45 . H452 . 109.7 no
C46 . C45 . H452 . 112.1 no
H451 . C45 . H452 . 107.7 no
C45 . C46 . C47 . 110.8(4) yes
C45 . C46 . H462 . 110.9 no
C47 . C46 . H462 . 110.6 no
C45 . C46 . H461 . 108.5 no
C47 . C46 . H461 . 108.6 no
H462 . C46 . H461 . 107.3 no
C46 . C47 . C48 . 110.3(5) yes
C46 . C47 . H472 . 110.0 no
C48 . C47 . H472 . 108.3 no
C46 . C47 . H471 . 110.4 no
C48 . C47 . H471 . 109.8 no
H472 . C47 . H471 . 107.9 no
C47 . C48 . C49 . 112.4(6) yes
C47 . C48 . H481 . 108.3 no
C49 . C48 . H481 . 112.0 no
C47 . C48 . H482 . 107.0 no
C49 . C48 . H482 . 104.9 no
H481 . C48 . H482 . 112.1 no
C48 . C49 . H492 . 108.2 no
C48 . C49 . H491 . 108.1 no
H492 . C49 . H491 . 110.9 no
C48 . C49 . H493 . 109.5 no
H492 . C49 . H493 . 109.2 no
H491 . C49 . H493 . 110.9 no
C28 . O50 . C51 . 116.2(2) yes
O50 . C51 . C52 . 105.8(2) yes
O50 . C51 . H512 . 110.4 no
C52 . C51 . H512 . 112.3 no
O50 . C51 . H511 . 111.1 no
C52 . C51 . H511 . 109.8 no
H512 . C51 . H511 . 107.5 no
C51 . C52 . C53 . 109.4(4) yes
C51 . C52 . H522 . 110.1 no
C53 . C52 . H522 . 111.1 no
C51 . C52 . H521 . 110.4 no
C53 . C52 . H521 . 108.3 no
H522 . C52 . H521 . 107.6 no
C51 . C52 . C153 . 115.7(5) yes
C51 . C52 . H522 . 110.1 no
C153 . C52 . H522 . 107.1 no
C51 . C52 . H521 . 110.4 no
C153 . C52 . H521 . 105.6 no
H522 . C52 . H521 . 107.6 no
C52 . C53 . C54 . 109.4(5) yes
C52 . C53 . H532 . 108.1 no
C54 . C53 . H532 . 107.7 no
C52 . C53 . H531 . 111.1 no
C54 . C53 . H531 . 111.9 no
H532 . C53 . H531 . 108.5 no
C53 . C54 . C55 . 109.6(5) yes
C53 . C54 . H542 . 113.2 no
C55 . C54 . H542 . 108.1 no
C53 . C54 . H541 . 107.5 no
C55 . C54 . H541 . 109.3 no
H542 . C54 . H541 . 109.1 no
C54 . C55 . C56 . 109.4(6) yes
C54 . C55 . H551 . 108.6 no
C56 . C55 . H551 . 112.9 no
C54 . C55 . H552 . 107.9 no
C56 . C55 . H552 . 107.6 no
H551 . C55 . H552 . 110.4 no
C55 . C56 . H562 . 107.5 no
C55 . C56 . H561 . 106.5 no
H562 . C56 . H561 . 110.5 no
C55 . C56 . H563 . 110.4 no
H562 . C56 . H563 . 111.0 no
H561 . C56 . H563 . 110.8 no
C5 . N57 . O58 . 118.6(3) yes
C5 . N57 . O59 . 118.0(3) yes
O58 . N57 . O59 . 123.4(3) yes
C11 . N60 . O61 . 117.7(3) yes
C11 . N60 . O62 . 117.4(3) yes
O61 . N60 . O62 . 124.9(3) yes
C17 . N63 . O64 . 118.7(3) yes
C17 . N63 . O65 . 118.3(3) yes
O64 . N63 . O65 . 123.0(3) yes
C23 . N66 . O67 . 117.9(3) yes
C23 . N66 . O68 . 117.7(3) yes
O67 . N66 . O68 . 124.4(3) yes
C31 . C132 . C133 . 112.3(3) yes
C31 . C132 . H1322 . 111.8 no
C133 . C132 . H1322 . 120.3 no
C31 . C132 . H1321 . 106.1 no
C133 . C132 . H1321 . 94.3 no
H1322 . C132 . H1321 . 109.6 no
C132 . C133 . C134 . 109.8(5) yes
C132 . C133 . H1332 . 96.0 no
C134 . C133 . H1332 . 96.8 no
C132 . C133 . H1331 . 120.1 no
C134 . C133 . H1331 . 119.9 no
H1332 . C133 . H1331 . 108.4 no
C133 . C134 . C135 . 109.5(8) yes
C133 . C134 . H1341 . 123.1 no
C135 . C134 . H1341 . 108.8 no
C133 . C134 . H1342 . 97.2 no
C135 . C134 . H1342 . 109.2 no
H1341 . C134 . H1342 . 107.9 no
C134 . C135 . H1352 . 110.5 no
C134 . C135 . H1353 . 107.3 no
H1352 . C135 . H1353 . 110.0 no
C134 . C135 . H1351 . 108.6 no
H1352 . C135 . H1351 . 110.2 no
H1353 . C135 . H1351 . 110.2 no
O36 . C137 . C138 . 103.6(8) yes
O36 . C137 . H1371 . 103.7 no
C138 . C137 . H1371 . 102.0 no
O36 . C137 . H1372 . 115.7 no
C138 . C137 . H1372 . 120.6 no
H1371 . C137 . H1372 . 109.4 no
C137 . C138 . C139 . 108.9(9) yes
C137 . C138 . H1381 . 117.8 no
C139 . C138 . H1381 . 116.5 no
C137 . C138 . H1382 . 98.9 no
C139 . C138 . H1382 . 101.9 no
H1381 . C138 . H1382 . 110.1 no
C138 . C139 . C140 . 104.4(9) yes
C138 . C139 . H1391 . 107.1 no
C140 . C139 . H1391 . 107.3 no
C138 . C139 . H1392 . 118.4 no
C140 . C139 . H1392 . 109.4 no
H1391 . C139 . H1392 . 109.7 no
C139 . C140 . C141 . 111.8(9) yes
C139 . C140 . H1402 . 113.3 no
C141 . C140 . H1402 . 110.2 no
C139 . C140 . H1401 . 107.0 no
C141 . C140 . H1401 . 105.0 no
H1402 . C140 . H1401 . 109.1 no
C140 . C141 . C142 . 106.6(9) yes
C140 . C141 . H1412 . 106.1 no
C142 . C141 . H1412 . 105.2 no
C140 . C141 . H1411 . 113.6 no
C142 . C141 . H1411 . 115.5 no
H1412 . C141 . H1411 . 109.2 no
C141 . C142 . H1421 . 104.6 no
C141 . C142 . H1422 . 110.0 no
H1421 . C142 . H1422 . 113.5 no
C141 . C142 . H1423 . 98.9 no
H1421 . C142 . H1423 . 113.8 no
H1422 . C142 . H1423 . 114.4 no
O43 . C144 . C145 . 109.4(8) yes
O43 . C144 . H1441 . 110.5 no
C145 . C144 . H1441 . 110.3 no
O43 . C144 . H1442 . 109.2 no
C145 . C144 . H1442 . 108.3 no
H1441 . C144 . H1442 . 108.9 no
C144 . C145 . C146 . 111.9(8) yes
C144 . C145 . H1451 . 109.1 no
C146 . C145 . H1451 . 110.0 no
C144 . C145 . H1452 . 108.4 no
C146 . C145 . H1452 . 108.2 no
H1451 . C145 . H1452 . 109.2 no
C145 . C146 . C147 . 110.1(7) yes
C145 . C146 . H1461 . 108.6 no
C147 . C146 . H1461 . 108.3 no
C145 . C146 . H1462 . 110.0 no
C147 . C146 . H1462 . 110.3 no
H1461 . C146 . H1462 . 109.5 no
C146 . C147 . C148 . 111.5(8) yes
C146 . C147 . H1472 . 110.4 no
C148 . C147 . H1472 . 109.8 no
C146 . C147 . H1471 . 108.7 no
C148 . C147 . H1471 . 106.7 no
H1472 . C147 . H1471 . 109.7 no
C147 . C148 . C149 . 106.1(8) yes
C147 . C148 . H1482 . 108.8 no
C149 . C148 . H1482 . 108.4 no
C147 . C148 . H1481 . 112.5 no
C149 . C148 . H1481 . 111.9 no
H1482 . C148 . H1481 . 109.0 no
C148 . C149 . H1491 . 109.3 no
C148 . C149 . H1492 . 111.4 no
H1491 . C149 . H1492 . 109.5 no
C148 . C149 . H1493 . 108.1 no
H1491 . C149 . H1493 . 109.3 no
H1492 . C149 . H1493 . 109.2 no
C52 . C153 . C154 . 111.1(6) yes
C52 . C153 . H1531 . 111.0 no
C154 . C153 . H1531 . 109.2 no
C52 . C153 . H1532 . 106.8 no
C154 . C153 . H1532 . 109.0 no
H1531 . C153 . H1532 . 109.7 no
C153 . C154 . C155 . 114.2(7) yes
C153 . C154 . H1542 . 109.2 no
C155 . C154 . H1542 . 110.2 no
C153 . C154 . H1541 . 107.7 no
C155 . C154 . H1541 . 105.7 no
H1542 . C154 . H1541 . 109.7 no
C154 . C155 . C156 . 109.9(8) yes
C154 . C155 . H1551 . 110.5 no
C156 . C155 . H1551 . 111.2 no
C154 . C155 . H1552 . 109.9 no
C156 . C155 . H1552 . 106.6 no
H1551 . C155 . H1552 . 108.7 no
C155 . C156 . H1561 . 111.6 no
C155 . C156 . H1563 . 106.0 no
H1561 . C156 . H1563 . 109.7 no
C155 . C156 . H1562 . 110.2 no
H1561 . C156 . H1562 . 110.0 no
H1563 . C156 . H1562 . 109.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H61 . O64 3_554 173 0.928 2.582 3.505(8) yes
C12 . H121 . O65 4_656 160 0.939 2.410 3.307(4) yes
C18 . H181 . O58 3_555 171 0.933 2.586 3.511(7) yes
C40 . H402 . O65 . 163 0.995 2.598 3.563(17) yes
C139 . H1391 . N60 2_666 138 0.974 2.463 3.249(17) yes
C30 . H302 . O68 3_564 147 0.989 2.571 3.443(17) yes
C132 . H1322 . O68 3_564 152 0.983 2.503 3.403(17) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/10/14 at 15:19:40
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
EQUIVALENCE PART(2001, OCC) PART(2002, OCC) 
WEIGHT -1 PART(2002, OCC) 
EQUIVALENCE PART(3001, OCC) PART(3002, OCC) 
WEIGHT -1 PART(3002, OCC) 
EQUIVALENCE PART(4001, OCC) PART(4002, OCC) 
WEIGHT -1 PART(4002, OCC) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 312,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
CONTINUE C   ( 132,X'S) H   (1322,X'S) H   (1321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
CONTINUE C   ( 133,X'S) H   (1332,X'S) H   (1331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 353,X'S) H   ( 352,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 392,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 422,X'S) H   ( 421,X'S) H   ( 423,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 462,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 472,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 492,X'S) H   ( 491,X'S) H   ( 493,X'S) 
RIDE C   (  51,X'S) H   ( 512,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 522,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 562,X'S) H   ( 561,X'S) H   ( 563,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) H   (1342,X'S) 
RIDE C   ( 135,X'S) H   (1352,X'S) H   (1353,X'S) H   (1351,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) H   (1372,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) H   (1382,X'S) 
RIDE C   ( 139,X'S) H   (1391,X'S) H   (1392,X'S) 
RIDE C   ( 140,X'S) H   (1402,X'S) H   (1401,X'S) 
RIDE C   ( 141,X'S) H   (1412,X'S) H   (1411,X'S) 
RIDE C   ( 142,X'S) H   (1421,X'S) H   (1422,X'S) H   (1423,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) H   (1442,X'S) 
RIDE C   ( 145,X'S) H   (1451,X'S) H   (1452,X'S) 
RIDE C   ( 146,X'S) H   (1461,X'S) H   (1462,X'S) 
RIDE C   ( 147,X'S) H   (1472,X'S) H   (1471,X'S) 
RIDE C   ( 148,X'S) H   (1482,X'S) H   (1481,X'S) 
RIDE C   ( 149,X'S) H   (1491,X'S) H   (1492,X'S) H   (1493,X'S) 
RIDE C   ( 153,X'S) H   (1531,X'S) H   (1532,X'S) 
RIDE C   ( 154,X'S) H   (1542,X'S) H   (1541,X'S) 
RIDE C   ( 155,X'S) H   (1551,X'S) H   (1552,X'S) 
RIDE C   ( 156,X'S) H   (1561,X'S) H   (1563,X'S) H   (1562,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 17/10/14 at 15:19:40
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.441000 , 0.005000 = O(29) TO C(30) 
DISTANCE 1.525000 , 0.005000 = C(30) TO C(31) 
DISTANCE 1.539000 , 0.005000 = C(31) TO C(32) 
DISTANCE 1.539000 , 0.005000 = C(32) TO C(33) 
DISTANCE 1.539000 , 0.005000 = C(33) TO C(34) 
DISTANCE 1.539000 , 0.005000 = C(34) TO C(35) 
ANGLE 109.000000 , 1.000000 = O(29) TO C(30) TO C(31) 
ANGLE 109.000000 , 1.000000 = C(30) TO C(31) TO C(32) 
ANGLE 109.000000 , 1.000000 = C(31) TO C(32) TO C(33) 
ANGLE 109.000000 , 1.000000 = C(32) TO C(33) TO C(34) 
ANGLE 109.000000 , 1.000000 = C(33) TO C(34) TO C(35) 
DISTANCE 1.539000 , 0.005000 = C(31) TO C(132) 
DISTANCE 1.539000 , 0.005000 = C(132) TO C(133) 
DISTANCE 1.539000 , 0.005000 = C(133) TO C(134) 
DISTANCE 1.539000 , 0.005000 = C(134) TO C(135) 
ANGLE 109.000000 , 1.000000 = C(30) TO C(31) TO C(132) 
ANGLE 109.000000 , 1.000000 = C(31) TO C(132) TO C(133) 
ANGLE 109.000000 , 1.000000 = C(132) TO C(133) TO C(134) 
ANGLE 109.000000 , 1.000000 = C(133) TO C(134) TO C(135) 
U(IJ)'S  0.0, 0.001000 = C(32) TO C(132) 
U(IJ)'S  0.0, 0.010000 = C(33) TO C(133) 
U(IJ)'S  0.0, 0.010000 = C(34) TO C(134) 
U(IJ)'S  0.0, 0.010000 = C(35) TO C(135) 
U(IJ)'S  0.0, 0.020000 = O(29) TO C(35) 
DISTANCE 1.441000 , 0.005000 = O(36) TO C(37) 
DISTANCE 1.525000 , 0.005000 = C(37) TO C(38) 
DISTANCE 1.539000 , 0.005000 = C(38) TO C(39) 
DISTANCE 1.539000 , 0.005000 = C(39) TO C(40) 
DISTANCE 1.539000 , 0.005000 = C(40) TO C(41) 
DISTANCE 1.539000 , 0.005000 = C(41) TO C(42) 
ANGLE 109.000000 , 1.000000 = O(36) TO C(37) TO C(38) 
ANGLE 109.000000 , 1.000000 = C(37) TO C(38) TO C(39) 
ANGLE 109.000000 , 1.000000 = C(38) TO C(39) TO C(40) 
ANGLE 109.000000 , 1.000000 = C(39) TO C(40) TO C(41) 
ANGLE 109.000000 , 1.000000 = C(40) TO C(41) TO C(42) 
DISTANCE 1.441000 , 0.005000 = O(36) TO C(137) 
DISTANCE 1.525000 , 0.005000 = C(137) TO C(138) 
DISTANCE 1.539000 , 0.005000 = C(138) TO C(139) 
DISTANCE 1.539000 , 0.005000 = C(139) TO C(140) 
DISTANCE 1.539000 , 0.005000 = C(140) TO C(141) 
DISTANCE 1.539000 , 0.005000 = C(141) TO C(142) 
ANGLE 109.000000 , 1.000000 = O(36) TO C(137) TO C(138) 
ANGLE 109.000000 , 1.000000 = C(137) TO C(138) TO C(139) 
ANGLE 109.000000 , 1.000000 = C(138) TO C(139) TO C(140) 
ANGLE 109.000000 , 1.000000 = C(139) TO C(140) TO C(141) 
ANGLE 109.000000 , 1.000000 = C(140) TO C(141) TO C(142) 
U(IJ)'S  0.0, 0.010000 = O(36) TO C(37) 
U(IJ)'S  0.0, 0.010000 = O(36) TO C(40) 
U(IJ)'S  0.0, 0.010000 = O(36) TO C(41) 
U(IJ)'S  0.0, 0.010000 = O(36) TO C(42) 
U(IJ)'S  0.0, 0.001000 = C(37) TO C(137) 
U(IJ)'S  0.0, 0.010000 = C(38) TO C(138) 
U(IJ)'S  0.0, 0.010000 = C(39) TO C(139) 
U(IJ)'S  0.0, 0.001000 = C(40) TO C(140) 
U(IJ)'S  0.0, 0.010000 = C(41) TO C(141) 
U(IJ)'S  0.0, 0.010000 = C(42) TO C(142) 
DISTANCE 1.441000 , 0.005000 = O(43) TO C(44) 
DISTANCE 1.525000 , 0.005000 = C(44) TO C(45) 
DISTANCE 1.539000 , 0.005000 = C(45) TO C(46) 
DISTANCE 1.539000 , 0.005000 = C(46) TO C(47) 
DISTANCE 1.539000 , 0.005000 = C(47) TO C(48) 
DISTANCE 1.539000 , 0.005000 = C(48) TO C(49) 
ANGLE 109.000000 , 1.000000 = O(43) TO C(44) TO C(45) 
ANGLE 109.000000 , 1.000000 = C(44) TO C(45) TO C(46) 
ANGLE 109.000000 , 1.000000 = C(45) TO C(46) TO C(47) 
ANGLE 109.000000 , 1.000000 = C(46) TO C(47) TO C(48) 
ANGLE 109.000000 , 1.000000 = C(47) TO C(48) TO C(49) 
DISTANCE 1.441000 , 0.005000 = O(43) TO C(144) 
DISTANCE 1.525000 , 0.005000 = C(144) TO C(145) 
DISTANCE 1.539000 , 0.005000 = C(145) TO C(146) 
DISTANCE 1.539000 , 0.005000 = C(146) TO C(147) 
DISTANCE 1.539000 , 0.005000 = C(147) TO C(148) 
DISTANCE 1.539000 , 0.005000 = C(148) TO C(149) 
ANGLE 109.000000 , 1.000000 = O(43) TO C(144) TO C(145) 
ANGLE 109.000000 , 1.000000 = C(144) TO C(145) TO C(146) 
ANGLE 109.000000 , 1.000000 = C(145) TO C(146) TO C(147) 
ANGLE 109.000000 , 1.000000 = C(146) TO C(147) TO C(148) 
ANGLE 109.000000 , 1.000000 = C(147) TO C(148) TO C(149) 
U(IJ)'S  0.0, 0.010000 = O(43) TO C(44) 
U(IJ)'S  0.0, 0.010000 = O(43) TO C(47) 
U(IJ)'S  0.0, 0.010000 = O(43) TO C(48) 
U(IJ)'S  0.0, 0.010000 = O(43) TO C(49) 
U(IJ)'S  0.0, 0.010000 = C(44) TO C(144) 
U(IJ)'S  0.0, 0.010000 = C(45) TO C(145) 
U(IJ)'S  0.0, 0.010000 = C(46) TO C(146) 
U(IJ)'S  0.0, 0.010000 = C(47) TO C(147) 
U(IJ)'S  0.0, 0.010000 = C(48) TO C(148) 
U(IJ)'S  0.0, 0.010000 = C(49) TO C(149) 
DISTANCE 1.441000 , 0.005000 = O(50) TO C(51) 
DISTANCE 1.525000 , 0.005000 = C(51) TO C(52) 
DISTANCE 1.539000 , 0.005000 = C(52) TO C(53) 
DISTANCE 1.539000 , 0.005000 = C(53) TO C(54) 
DISTANCE 1.539000 , 0.005000 = C(54) TO C(55) 
DISTANCE 1.539000 , 0.005000 = C(55) TO C(56) 
ANGLE 109.000000 , 1.000000 = O(50) TO C(51) TO C(52) 
ANGLE 109.000000 , 1.000000 = C(51) TO C(52) TO C(53) 
ANGLE 109.000000 , 1.000000 = C(52) TO C(53) TO C(54) 
ANGLE 109.000000 , 1.000000 = C(53) TO C(54) TO C(55) 
ANGLE 109.000000 , 1.000000 = C(54) TO C(55) TO C(56) 
DISTANCE 1.539000 , 0.005000 = C(52) TO C(153) 
DISTANCE 1.539000 , 0.005000 = C(153) TO C(154) 
DISTANCE 1.539000 , 0.005000 = C(154) TO C(155) 
DISTANCE 1.539000 , 0.005000 = C(155) TO C(156) 
ANGLE 109.000000 , 1.000000 = C(51) TO C(52) TO C(153) 
ANGLE 109.000000 , 1.000000 = C(52) TO C(153) TO C(154) 
ANGLE 109.000000 , 1.000000 = C(153) TO C(154) TO C(155) 
ANGLE 109.000000 , 1.000000 = C(154) TO C(155) TO C(156) 
U(IJ)'S  0.0, 0.001000 = C(53) TO C(153) 
U(IJ)'S  0.0, 0.001000 = C(54) TO C(154) 
U(IJ)'S  0.0, 0.001000 = C(55) TO C(155) 
U(IJ)'S  0.0, 0.001000 = C(56) TO C(156) 
U(IJ)'S  0.0, 0.020000 = O(50) TO C(56) 
END                                                                             
;
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_4f
_database_code_depnum_ccdc_archive 'CCDC 1030575'
_audit_update_record             
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;

_cell_length_a                   11.2845(12)
_cell_length_b                   18.1827(17)
_cell_length_c                   18.8706(19)
_cell_angle_alpha                90
_cell_angle_beta                 105.953(10)
_cell_angle_gamma                90
_cell_volume                     3722.8(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  '-C 2yc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C36 H20 N4 O8 S4 
# Dc =      1.36 Fooo =   1696.00 Mu =     28.21 M =    382.42
# Found Formula = C36 H20.00 N4 O12 S4 
# Dc =      1.48 FOOO =   1696.00 Mu =     29.51 M =    414.42

_chemical_formula_sum            'C36 H20.00 N4 O12 S4'
_chemical_formula_moiety         'C36 H20.00 N4 O12 S4'
_chemical_compound_source        ?
_chemical_formula_weight         828.84


_cell_measurement_reflns_used    15913
_cell_measurement_theta_min      5
_cell_measurement_theta_max      77
_cell_measurement_temperature    180

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.145
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_max          0.448

_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    2.951

# Sheldrick geometric approximatio 0.46 0.65 
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_T_max  0.65
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      180
_diffrn_ambient_pressure         101
_diffrn_reflns_number            41863
_reflns_number_total             3857
_diffrn_reflns_av_R_equivalents  0.111
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3857 
# Theoretical number of reflections is about 7871 


_diffrn_reflns_theta_min         4.746
_diffrn_reflns_theta_max         76.994
_diffrn_measured_fraction_theta_max 0.979

_diffrn_reflns_theta_full        73.144
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -14
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   4.55
_oxford_diffrn_Wilson_scale      0.15

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.75
_refine_diff_density_max         0.56


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3857
_refine_ls_number_restraints     16
_refine_ls_number_parameters     283
_oxford_refine_ls_R_factor_ref   0.1203
_refine_ls_wR_factor_ref         0.2180
_refine_ls_goodness_of_fit_ref   0.9798
_refine_ls_shift/su_max          0.0035863
_refine_ls_shift/su_mean         0.0005259


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3857
_refine_ls_R_factor_all          0.1203
_refine_ls_wR_factor_all         0.2180

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3203
_refine_ls_R_factor_gt           0.1094
_refine_ls_wR_factor_gt          0.2151

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.247E+04 0.388E+04 0.223E+04 843. 160. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.7013(5) 0.2869(4) 0.6840(3) 0.0503 1.0000 Uani . . . . . .
S2 S 0.69073(16) 0.34722(12) 0.60818(9) 0.0648 1.0000 Uani . . . . . .
C3 C 0.5693(5) 0.4071(4) 0.6125(3) 0.0453 1.0000 Uani . . . . . .
C4 C 0.4696(6) 0.4156(4) 0.5506(3) 0.0484 1.0000 Uani . . . . . .
C5 C 0.3827(6) 0.4679(4) 0.5525(3) 0.0516 1.0000 Uani . . . . . .
C6 C 0.3882(6) 0.5120(4) 0.6125(3) 0.0581 1.0000 Uani . . . . . .
C7 C 0.4879(6) 0.5037(4) 0.6756(3) 0.0516 1.0000 Uani . . . . . .
S8 S 0.5000 0.56435(14) 0.7500 0.0744 1.0000 Uani S T . . . .
S9 S 0.5000 0.12914(12) 0.7500 0.0579 1.0000 Uani S T . . . .
C10 C 0.6193(5) 0.1909(3) 0.7456(3) 0.0436 1.0000 Uani . . . . . .
C11 C 0.7284(5) 0.1900(3) 0.8012(3) 0.0464 1.0000 Uani . . . . . .
C12 C 0.8230(5) 0.2372(4) 0.7970(3) 0.0477 1.0000 Uani . . . . . .
C13 C 0.8108(5) 0.2859(4) 0.7413(3) 0.0505 1.0000 Uani . . . . . .
C14 C 0.5777(5) 0.4515(3) 0.6749(3) 0.0469 1.0000 Uani . . . . . .
C15 C 0.6069(5) 0.2387(3) 0.6856(3) 0.0453 1.0000 Uani . . . . . .
O16 O 0.6736(4) 0.4416(2) 0.7367(2) 0.0540 1.0000 Uani . . . . . .
C17 C 0.7788(7) 0.4869(5) 0.7398(4) 0.0874 1.0000 Uani . . . . . .
C18 C 0.8721(7) 0.4734(5) 0.8085(4) 0.0774 1.0000 Uani . . . . . .
C19 C 0.9484(8) 0.4589(6) 0.8621(5) 0.1110 1.0000 Uani . . . . . .
O20 O 0.5021(4) 0.2380(3) 0.6283(2) 0.0548 1.0000 Uani D . . . . .
C21 C 0.5069(11) 0.1833(12) 0.5713(15) 0.0805 0.794(10) Uani D U P 1 1 .
C22 C 0.3929(10) 0.1867(6) 0.5121(5) 0.0762 0.794(10) Uani D . P 1 1 .
C23 C 0.2972(11) 0.1889(8) 0.4626(6) 0.1048 0.794(10) Uani D . P 1 1 .
N24 N 0.2767(6) 0.4785(4) 0.4869(3) 0.0715 1.0000 Uani . . . . . .
O25 O 0.2750(5) 0.4454(3) 0.4310(2) 0.0800 1.0000 Uani . . . . . .
O26 O 0.1951(6) 0.5205(5) 0.4930(3) 0.1202 1.0000 Uani . . . . . .
N27 N 0.9409(5) 0.2318(4) 0.8544(3) 0.0620 1.0000 Uani . . . . . .
O28 O 0.9596(6) 0.1778(4) 0.8947(3) 0.1011 1.0000 Uani . . . . . .
O29 O 1.0163(5) 0.2814(4) 0.8585(3) 0.0894 1.0000 Uani . . . . . .
C121 C 0.498(4) 0.180(5) 0.578(6) 0.0805 0.206(10) Uani D U P 1 2 .
C122 C 0.617(3) 0.1754(15) 0.5624(15) 0.0443 0.206(10) Uani D . P 1 2 .
C123 C 0.710(3) 0.171(2) 0.5481(18) 0.0692 0.206(10) Uani D . P 1 2 .
H111 H 0.7379 0.1585 0.8416 0.0536 1.0000 Uiso R . . . . .
H131 H 0.8743 0.3188 0.7416 0.0594 1.0000 Uiso R . . . . .
H171 H 0.7539 0.5382 0.7368 0.1022 1.0000 Uiso R . . . . .
H172 H 0.8119 0.4744 0.6981 0.1021 1.0000 Uiso R . . . . .
H191 H 1.0073 0.4508 0.9076 0.1293 1.0000 Uiso R . . . . .
H61 H 0.3253 0.5463 0.6110 0.0691 1.0000 Uiso R . . . . .
H41 H 0.4611 0.3867 0.5078 0.0559 1.0000 Uiso R . . . . .
H212 H 0.5185 0.1353 0.5920 0.0877 0.794(10) Uiso R . P 1 1 .
H211 H 0.5734 0.1950 0.5516 0.0877 0.794(10) Uiso R . P 1 1 .
H231 H 0.2227 0.1906 0.4240 0.1176 0.794(10) Uiso R . P 1 1 .
H1212 H 0.5006 0.1372 0.6073 0.0876 0.206(10) Uiso R . P 1 2 .
H1211 H 0.4262 0.1791 0.5376 0.0876 0.206(10) Uiso R . P 1 2 .
H1231 H 0.7881 0.1675 0.5384 0.0980 0.206(10) Uiso R . P 1 2 .

_refine_ls_extinction_coef       42(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          2.47(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . S2 . 1.782(6) yes
C1 . C13 . 1.400(8) yes
C1 . C15 . 1.386(9) yes
S2 . C3 . 1.770(7) yes
C3 . C4 . 1.390(7) yes
C3 . C14 . 1.409(9) yes
C4 . C5 . 1.374(9) yes
C4 . H41 . 0.946 no
C5 . C6 . 1.374(9) yes
C5 . N24 . 1.479(7) yes
C6 . C7 . 1.404(8) yes
C6 . H61 . 0.939 no
C7 . S8 . 1.761(6) yes
C7 . C14 . 1.391(9) yes
S9 . C10 5_656 1.772(6) yes
S9 . C10 . 1.772(6) yes
C10 . C11 . 1.381(8) yes
C10 . C15 . 1.404(8) yes
C11 . C12 . 1.388(9) yes
C11 . H111 . 0.937 no
C12 . C13 . 1.352(8) yes
C12 . N27 . 1.470(8) yes
C13 . H131 . 0.932 no
C14 . O16 . 1.368(6) yes
C15 . O20 . 1.365(7) yes
O16 . C17 . 1.433(8) yes
C17 . C18 . 1.449(9) yes
C17 . H171 . 0.972 no
C17 . H172 . 0.986 no
C18 . C19 . 1.164(10) yes
C19 . H191 . 0.943 no
O20 . C21 . 1.477(13) yes
O20 . C121 . 1.41(3) yes
C21 . C22 . 1.46(2) yes
C21 . H212 . 0.950 no
C21 . H211 . 0.950 no
C22 . C23 . 1.219(13) yes
C23 . H231 . 0.950 no
N24 . O25 . 1.210(8) yes
N24 . O26 . 1.225(9) yes
N27 . O28 . 1.224(8) yes
N27 . O29 . 1.228(8) yes
C121 . C122 . 1.45(3) yes
C121 . H1212 . 0.950 no
C121 . H1211 . 0.950 no
C122 . C123 . 1.16(3) yes
C123 . H1231 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 . C1 . C13 . 118.5(5) yes
S2 . C1 . C15 . 121.6(5) yes
C13 . C1 . C15 . 119.8(6) yes
C1 . S2 . C3 . 102.9(3) yes
S2 . C3 . C4 . 119.2(5) yes
S2 . C3 . C14 . 121.1(4) yes
C4 . C3 . C14 . 119.4(6) yes
C3 . C4 . C5 . 118.3(6) yes
C3 . C4 . H41 . 121.6 no
C5 . C4 . H41 . 120.1 no
C4 . C5 . C6 . 123.7(5) yes
C4 . C5 . N24 . 119.2(6) yes
C6 . C5 . N24 . 117.1(6) yes
C5 . C6 . C7 . 118.6(7) yes
C5 . C6 . H61 . 120.0 no
C7 . C6 . H61 . 121.4 no
C6 . C7 . S8 . 118.5(5) yes
C6 . C7 . C14 . 118.8(6) yes
S8 . C7 . C14 . 122.6(4) yes
C7 5_656 S8 . C7 . 102.4(4) yes
C10 5_656 S9 . C10 . 101.4(4) yes
S9 . C10 . C11 . 119.2(5) yes
S9 . C10 . C15 . 121.4(5) yes
C11 . C10 . C15 . 119.3(6) yes
C10 . C11 . C12 . 119.3(6) yes
C10 . C11 . H111 . 120.2 no
C12 . C11 . H111 . 120.5 no
C11 . C12 . C13 . 122.3(6) yes
C11 . C12 . N27 . 118.1(6) yes
C13 . C12 . N27 . 119.6(6) yes
C1 . C13 . C12 . 119.2(6) yes
C1 . C13 . H131 . 120.7 no
C12 . C13 . H131 . 120.1 no
C3 . C14 . C7 . 121.1(5) yes
C3 . C14 . O16 . 119.5(6) yes
C7 . C14 . O16 . 119.3(6) yes
C10 . C15 . C1 . 120.1(5) yes
C10 . C15 . O20 . 120.3(6) yes
C1 . C15 . O20 . 119.5(5) yes
C14 . O16 . C17 . 114.2(5) yes
O16 . C17 . C18 . 109.2(6) yes
O16 . C17 . H171 . 109.1 no
C18 . C17 . H171 . 110.0 no
O16 . C17 . H172 . 109.1 no
C18 . C17 . H172 . 109.4 no
H171 . C17 . H172 . 109.9 no
C17 . C18 . C19 . 176.3(12) yes
C18 . C19 . H191 . 174.7 no
C15 . O20 . C21 . 112.7(8) yes
C15 . O20 . C121 . 114(4) yes
O20 . C21 . C22 . 109.2(9) yes
O20 . C21 . H212 . 110.4 no
C22 . C21 . H212 . 110.3 no
O20 . C21 . H211 . 109.0 no
C22 . C21 . H211 . 108.4 no
H212 . C21 . H211 . 109.5 no
C21 . C22 . C23 . 179.4(13) yes
C22 . C23 . H231 . 179.9 no
C5 . N24 . O25 . 118.7(7) yes
C5 . N24 . O26 . 117.3(6) yes
O25 . N24 . O26 . 124.0(6) yes
C12 . N27 . O28 . 118.5(7) yes
C12 . N27 . O29 . 118.0(6) yes
O28 . N27 . O29 . 123.5(6) yes
O20 . C121 . C122 . 108.7(10) yes
O20 . C121 . H1212 . 103.5 no
C122 . C121 . H1212 . 100.8 no
O20 . C121 . H1211 . 114.7 no
C122 . C121 . H1211 . 117.8 no
H1212 . C121 . H1211 . 109.5 no
C121 . C122 . C123 . 178(4) yes
C122 . C123 . H1231 . 177.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C11 . H111 . O25 8_555 167 0.937 2.490 3.410(7) yes
C19 . H191 . O26 6_665 151 0.943 2.342 3.20(2) yes
C4 . H41 . O28 8_454 173 0.946 2.433 3.372(9) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/10/14 at 15:40:05
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
CONT EXTPARAM 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   ( 121,X'S) H   (1212,X'S) H   (1211,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 17/10/14 at 15:40:05
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.440000 , 0.050000 = O(20) TO C(21) 
DISTANCE 1.460000 , 0.050000 = C(21) TO C(22) 
DISTANCE 1.160000 , 0.050000 = C(22) TO C(23) 
ANGLE 109.000000 , 1.000000 = O(20) TO C(21) TO C(22) 
DISTANCE 2.620000 , 0.050000 = C(21) TO C(23) 
DISTANCE 1.440000 , 0.050000 = O(20) TO C(121) 
DISTANCE 1.460000 , 0.050000 = C(121) TO C(122) 
DISTANCE 1.160000 , 0.050000 = C(122) TO C(123) 
ANGLE 109.000000 , 1.000000 = O(20) TO C(121) TO C(122) 
DISTANCE 2.620000 , 0.050000 = C(121) TO C(123) 
U(IJ)'S  0.0, 0.001000 = C(21) TO C(121) 
END                                                                             
;
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_4e
_database_code_depnum_ccdc_archive 'CCDC 1030576'
_audit_update_record             
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
_cell_length_a                   12.64786(19)
_cell_length_b                   14.04823(19)
_cell_length_c                   13.3958(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.2335(15)
_cell_angle_gamma                90
_cell_volume                     2334.57(6)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1 '
_symmetry_space_group_name_Hall  'P 2yb '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C49.50 H45 N5 O9 S4.50 
# Dc =      1.42 Fooo =   1008.00 Mu =     26.08 M =    998.23
# Found Formula = C44 H52 N4 O12 S4 
# Dc =      1.36 FOOO =   1008.00 Mu =     24.17 M =    957.18

_chemical_formula_sum            'C44 H52 N4 O12 S4'
_chemical_formula_moiety         'C44 H52 N4 O12 S4'
_chemical_compound_source        ?
_chemical_formula_weight         957.18


_cell_measurement_reflns_used    12738
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    190

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.120
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_max          0.430

_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1008.000
_exptl_absorpt_coefficient_mu    2.417

# Sheldrick geometric approximatio 0.68 0.75 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_T_max  0.75
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      190
_diffrn_ambient_pressure         101
_diffrn_reflns_number            20129
_reflns_number_total             9361
_diffrn_reflns_av_R_equivalents  0.039
# Number of reflections without Friedels Law is 9361 
# Number of reflections with Friedels Law is 4976 
# Theoretical number of reflections is about 4864 


_diffrn_reflns_theta_min         4.399
_diffrn_reflns_theta_max         75.832
_diffrn_measured_fraction_theta_max 0.981

_diffrn_reflns_theta_full        71.282
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              -17
_reflns_limit_k_max              17
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.70
_oxford_diffrn_Wilson_scale      0.08

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.40
_refine_diff_density_max         0.44


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         9361
_refine_ls_number_restraints     259
_refine_ls_number_parameters     716
_oxford_refine_ls_R_factor_ref   0.0547
_refine_ls_wR_factor_ref         0.1274
_refine_ls_goodness_of_fit_ref   0.9794
_refine_ls_shift/su_max          0.0005035
_refine_ls_shift/su_mean         0.0000544


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9361
_refine_ls_R_factor_all          0.0547
_refine_ls_wR_factor_all         0.1274

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9039
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_gt          0.1223

_refine_ls_abs_structure_Flack   0.082(17)
_refine_ls_abs_structure_details 'Flack (1983), 4385 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.137E+04 0.219E+04 0.116E+04 329. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.7479(3) 0.3860(3) 0.9628(2) 0.0357 1.0000 Uani . . . . . .
S2 S 0.80485(7) 0.50071(11) 0.95546(6) 0.0388 1.0000 Uani . . . . . .
C3 C 0.8324(2) 0.5049(2) 0.8308(2) 0.0293 1.0000 Uani . . . . . .
C4 C 0.9361(3) 0.5334(3) 0.8214(3) 0.0368 1.0000 Uani . . . . . .
C5 C 0.9571(2) 0.5468(3) 0.7264(3) 0.0344 1.0000 Uani . . . . . .
C6 C 0.8824(2) 0.5314(2) 0.6372(2) 0.0316 1.0000 Uani . . . . . .
C7 C 0.7798(2) 0.5025(2) 0.6467(2) 0.0279 1.0000 Uani . . . . . .
S8 S 0.68320(5) 0.49473(10) 0.53174(5) 0.0289 1.0000 Uani . . . . . .
C9 C 0.6209(2) 0.3822(2) 0.5327(2) 0.0256 1.0000 Uani . . . . . .
C10 C 0.5090(2) 0.3817(2) 0.5055(2) 0.0274 1.0000 Uani . . . . . .
C11 C 0.45664(19) 0.2949(3) 0.49243(19) 0.0280 1.0000 Uani . . . . . .
C12 C 0.5104(2) 0.2086(2) 0.5091(2) 0.0292 1.0000 Uani . . . . . .
C13 C 0.6225(2) 0.2099(2) 0.5370(2) 0.0256 1.0000 Uani . . . . . .
S14 S 0.68561(6) 0.09687(10) 0.53665(5) 0.0293 1.0000 Uani . . . . . .
C15 C 0.7860(2) 0.0933(2) 0.6482(2) 0.0273 1.0000 Uani . . . . . .
C16 C 0.8895(2) 0.0671(2) 0.6372(2) 0.0309 1.0000 Uani . . . . . .
C17 C 0.9682(3) 0.0543(2) 0.7241(3) 0.0347 1.0000 Uani . . . . . .
C18 C 0.9481(3) 0.0713(2) 0.8214(3) 0.0356 1.0000 Uani . . . . . .
C19 C 0.8454(2) 0.0974(2) 0.8313(2) 0.0323 1.0000 Uani . . . . . .
S20 S 0.82150(7) 0.10321(12) 0.95772(6) 0.0398 1.0000 Uani . . . . . .
C21 C 0.7534(3) 0.2132(3) 0.9624(2) 0.0351 1.0000 Uani . . . . . .
C22 C 0.6507(3) 0.2093(3) 0.9837(2) 0.0406 1.0000 Uani . . . . . .
C23 C 0.5993(2) 0.2951(3) 0.9967(2) 0.0398 1.0000 Uani . . . . . .
C24 C 0.6460(3) 0.3819(3) 0.9863(2) 0.0385 1.0000 Uani . . . . . .
C25 C 0.7530(2) 0.4916(3) 0.7433(2) 0.0295 1.0000 Uani . . . . . .
C26 C 0.6794(2) 0.2959(3) 0.54548(17) 0.0261 1.0000 Uani . . . . . .
C27 C 0.7620(2) 0.1038(3) 0.7451(2) 0.0282 1.0000 Uani . . . . . .
C28 C 0.8050(2) 0.3012(4) 0.95461(18) 0.0360 1.0000 Uani . . . . . .
O29 O 0.65025(16) 0.46673(19) 0.74930(18) 0.0393 1.0000 Uani D U . . . .
C30 C 0.5826(3) 0.5400(4) 0.7732(5) 0.0412 0.688(7) Uani D U P 1 1 .
C31 C 0.4645(3) 0.5173(3) 0.7249(4) 0.0455 0.688(7) Uani D U P 1 1 .
C32 C 0.3869(4) 0.5841(4) 0.7653(5) 0.0680 0.688(7) Uani D U P 1 1 .
C33 C 0.4057(6) 0.6868(4) 0.7456(5) 0.0713 0.688(7) Uani D U P 1 1 .
C34 C 0.4445(5) 0.4158(4) 0.7483(7) 0.0684 0.688(7) Uani D U P 1 1 .
O35 O 0.78895(14) 0.29540(19) 0.56677(14) 0.0348 1.0000 Uani D U . . . .
C36 C 0.8320(3) 0.3033(4) 0.4733(3) 0.0414 0.775(6) Uani D U P 2 1 .
C37 C 0.9530(2) 0.2788(4) 0.4991(3) 0.0454 0.775(6) Uani D U P 2 1 .
C38 C 1.0143(3) 0.3317(5) 0.5903(4) 0.0681 0.775(6) Uani D U P 2 1 .
C39 C 1.1275(4) 0.3010(8) 0.6271(6) 0.0945 0.775(6) Uani D U P 2 1 .
C40 C 0.9981(4) 0.2942(6) 0.4054(3) 0.0554 0.775(6) Uani D U P 2 1 .
O41 O 0.65870(17) 0.12093(18) 0.75528(17) 0.0343 1.0000 Uani . . . . . .
C42 C 0.5991(3) 0.0330(3) 0.7649(3) 0.0449 1.0000 Uani . . . . . .
C43 C 0.4817(3) 0.0513(3) 0.7303(3) 0.0450 1.0000 Uani . . . . . .
C44 C 0.4410(4) 0.1317(4) 0.7888(4) 0.0736 1.0000 Uani . . . . . .
C45 C 0.3277(4) 0.1646(5) 0.7382(7) 0.1057 1.0000 Uani . . . . . .
C46 C 0.4191(4) -0.0430(4) 0.7401(3) 0.0578 1.0000 Uani . . . . . .
O47 O 0.90655(15) 0.3003(2) 0.93573(15) 0.0439 1.0000 Uani D U . . . .
C48 C 0.9872(4) 0.3494(6) 1.0091(7) 0.0599 0.524(8) Uani D U P 3 1 .
C49 C 1.0861(4) 0.2847(6) 1.0425(5) 0.0493 0.524(8) Uani D U P 3 1 .
C50 C 1.1700(5) 0.3298(5) 1.1272(5) 0.0563 0.524(8) Uani D U P 3 1 .
C51 C 1.2545(6) 0.2621(6) 1.1780(6) 0.0671 0.524(8) Uani D U P 3 1 .
C52 C 1.1328(6) 0.2664(7) 0.9500(6) 0.0657 0.524(8) Uani D U P 3 1 .
N53 N 1.0660(2) 0.5789(3) 0.7169(3) 0.0480 1.0000 Uani . . . . . .
O54 O 1.0926(2) 0.5723(3) 0.6344(2) 0.0557 1.0000 Uani . . . . . .
O55 O 1.1241(2) 0.6110(4) 0.7933(3) 0.0815 1.0000 Uani . . . . . .
N56 N 0.33890(19) 0.2947(3) 0.4596(2) 0.0395 1.0000 Uani . . . . . .
O57 O 0.2935(2) 0.2172(2) 0.4469(3) 0.0637 1.0000 Uani . . . . . .
O58 O 0.2930(2) 0.3704(2) 0.4454(3) 0.0603 1.0000 Uani . . . . . .
N59 N 1.0753(2) 0.0242(2) 0.7124(3) 0.0439 1.0000 Uani . . . . . .
O60 O 1.1368(2) -0.0070(3) 0.7894(3) 0.0736 1.0000 Uani . . . . . .
O61 O 1.0989(2) 0.0279(2) 0.6291(2) 0.0492 1.0000 Uani . . . . . .
N62 N 0.4896(2) 0.2918(4) 1.0170(2) 0.0509 1.0000 Uani . . . . . .
O63 O 0.4449(2) 0.3664(3) 1.0262(3) 0.0704 1.0000 Uani . . . . . .
O64 O 0.4477(3) 0.2117(3) 1.0237(3) 0.0641 1.0000 Uani . . . . . .
C130 C 0.5821(7) 0.5510(6) 0.7285(11) 0.0538 0.312(7) Uani D U P 1 2 .
C131 C 0.4837(5) 0.5401(5) 0.7797(7) 0.0422 0.312(7) Uani D U P 1 2 .
C132 C 0.4182(9) 0.4505(7) 0.7473(14) 0.0643 0.312(7) Uani D U P 1 2 .
C133 C 0.3212(10) 0.4413(12) 0.7960(15) 0.0843 0.312(7) Uani D U P 1 2 .
C134 C 0.4158(7) 0.6273(6) 0.7526(11) 0.0475 0.312(7) Uani D U P 1 2 .
C136 C 0.8640(6) 0.3096(12) 0.5001(7) 0.0417 0.225(6) Uani D U P 2 2 .
C137 C 0.9710(5) 0.2584(9) 0.5474(8) 0.0746 0.225(6) Uani D U P 2 2 .
C138 C 1.0561(7) 0.2667(13) 0.4825(10) 0.0640 0.225(6) Uani D U P 2 2 .
C139 C 1.0136(14) 0.295(2) 0.3744(11) 0.0551 0.225(6) Uani D U P 2 2 .
C140 C 1.0076(9) 0.3031(12) 0.6498(8) 0.0511 0.225(6) Uani D U P 2 2 .
C148 C 0.9909(4) 0.3214(9) 1.0222(6) 0.0601 0.476(8) Uani D U P 3 2 .
C149 C 1.0956(4) 0.2717(7) 1.0068(5) 0.0483 0.476(8) Uani D U P 3 2 .
C150 C 1.1914(4) 0.2948(13) 1.0907(5) 0.0827 0.476(8) Uani D U P 3 2 .
C151 C 1.1669(8) 0.3010(11) 1.1949(5) 0.0760 0.476(8) Uani D U P 3 2 .
C152 C 1.1155(7) 0.3032(12) 0.9052(5) 0.0817 0.476(8) Uani D U P 3 2 .
H421 H 0.6245 -0.0186 0.7247 0.0517 1.0000 Uiso R . . . . .
H422 H 0.6109 0.0122 0.8351 0.0519 1.0000 Uiso R . . . . .
H431 H 0.4717 0.0712 0.6563 0.0521 1.0000 Uiso R . . . . .
H101 H 0.4690 0.4373 0.4938 0.0318 1.0000 Uiso R . . . . .
H121 H 0.4710 0.1499 0.5005 0.0345 1.0000 Uiso R . . . . .
H161 H 0.9059 0.0589 0.5737 0.0348 1.0000 Uiso R . . . . .
H181 H 1.0052 0.0658 0.8780 0.0411 1.0000 Uiso R . . . . .
H221 H 0.6187 0.1513 0.9885 0.0446 1.0000 Uiso R . . . . .
H241 H 0.6100 0.4386 0.9920 0.0467 1.0000 Uiso R . . . . .
H41 H 0.9917 0.5428 0.8786 0.0435 1.0000 Uiso R . . . . .
H61 H 0.8997 0.5416 0.5734 0.0360 1.0000 Uiso R . . . . .
H463 H 0.3415 -0.0363 0.7217 0.0821 1.0000 Uiso R . . . . .
H462 H 0.4393 -0.0928 0.6965 0.0819 1.0000 Uiso R . . . . .
H461 H 0.4344 -0.0650 0.8082 0.0818 1.0000 Uiso R . . . . .
H442 H 0.4403 0.1093 0.8587 0.0855 1.0000 Uiso R . . . . .
H441 H 0.4915 0.1851 0.7952 0.0853 1.0000 Uiso R . . . . .
H452 H 0.3175 0.2265 0.7691 0.1389 1.0000 Uiso R . . . . .
H451 H 0.2754 0.1205 0.7543 0.1379 1.0000 Uiso R . . . . .
H453 H 0.3211 0.1702 0.6658 0.1379 1.0000 Uiso R . . . . .
H302 H 0.5902 0.5426 0.8474 0.0519 0.688(7) Uiso R . P 1 1 .
H301 H 0.6006 0.6010 0.7467 0.0520 0.688(7) Uiso R . P 1 1 .
H311 H 0.4565 0.5253 0.6512 0.0561 0.688(7) Uiso R . P 1 1 .
H322 H 0.3128 0.5712 0.7327 0.0744 0.688(7) Uiso R . P 1 1 .
H321 H 0.3976 0.5735 0.8393 0.0744 0.688(7) Uiso R . P 1 1 .
H332 H 0.3618 0.7264 0.7777 0.1022 0.688(7) Uiso R . P 1 1 .
H331 H 0.3883 0.6991 0.6729 0.1019 0.688(7) Uiso R . P 1 1 .
H333 H 0.4797 0.7029 0.7685 0.1021 0.688(7) Uiso R . P 1 1 .
H341 H 0.3827 0.3886 0.7055 0.1069 0.688(7) Uiso R . P 1 1 .
H342 H 0.5075 0.3777 0.7472 0.1067 0.688(7) Uiso R . P 1 1 .
H343 H 0.4317 0.4180 0.8179 0.1070 0.688(7) Uiso R . P 1 1 .
H1302 H 0.5629 0.5700 0.6573 0.0522 0.312(7) Uiso R . P 1 2 .
H1301 H 0.6233 0.6015 0.7662 0.0523 0.312(7) Uiso R . P 1 2 .
H1311 H 0.5037 0.5357 0.8542 0.0548 0.312(7) Uiso R . P 1 2 .
H1321 H 0.4218 0.4074 0.8047 0.0692 0.312(7) Uiso R . P 1 2 .
H1322 H 0.4530 0.4211 0.6970 0.0691 0.312(7) Uiso R . P 1 2 .
H1342 H 0.3428 0.6166 0.7822 0.0641 0.312(7) Uiso R . P 1 2 .
H1341 H 0.3990 0.6349 0.6691 0.0637 0.312(7) Uiso R . P 1 2 .
H1343 H 0.4624 0.6882 0.7883 0.0641 0.312(7) Uiso R . P 1 2 .
H362 H 0.7931 0.2616 0.4198 0.0518 0.775(6) Uiso R . P 2 1 .
H361 H 0.8252 0.3707 0.4474 0.0510 0.775(6) Uiso R . P 2 1 .
H371 H 0.9570 0.2100 0.5152 0.0565 0.775(6) Uiso R . P 2 1 .
H381 H 0.9769 0.3254 0.6471 0.0805 0.775(6) Uiso R . P 2 1 .
H382 H 1.0160 0.3992 0.5688 0.0803 0.775(6) Uiso R . P 2 1 .
H393 H 1.1555 0.3292 0.6941 0.1344 0.775(6) Uiso R . P 2 1 .
H391 H 1.1235 0.2304 0.6347 0.1341 0.775(6) Uiso R . P 2 1 .
H392 H 1.1746 0.3175 0.5797 0.1342 0.775(6) Uiso R . P 2 1 .
H403 H 1.0603 0.2566 0.4034 0.0798 0.775(6) Uiso R . P 2 1 .
H402 H 0.9476 0.2825 0.3441 0.0781 0.775(6) Uiso R . P 2 1 .
H401 H 1.0207 0.3594 0.4051 0.0788 0.775(6) Uiso R . P 2 1 .
H1362 H 0.8360 0.2803 0.4349 0.0512 0.225(6) Uiso R . P 2 2 .
H1361 H 0.8756 0.3772 0.4898 0.0511 0.225(6) Uiso R . P 2 2 .
H1371 H 0.9578 0.1903 0.5577 0.0760 0.225(6) Uiso R . P 2 2 .
H1381 H 1.0945 0.2066 0.4836 0.0581 0.225(6) Uiso R . P 2 2 .
H1382 H 1.1056 0.3162 0.5128 0.0580 0.225(6) Uiso R . P 2 2 .
H1392 H 1.0504 0.2588 0.3308 0.0779 0.225(6) Uiso R . P 2 2 .
H1391 H 0.9381 0.2818 0.3570 0.0779 0.225(6) Uiso R . P 2 2 .
H1393 H 1.0261 0.3613 0.3664 0.0781 0.225(6) Uiso R . P 2 2 .
H1401 H 1.0716 0.2745 0.6869 0.0749 0.225(6) Uiso R . P 2 2 .
H1403 H 0.9517 0.2951 0.6882 0.0750 0.225(6) Uiso R . P 2 2 .
H1402 H 1.0198 0.3696 0.6417 0.0751 0.225(6) Uiso R . P 2 2 .
H481 H 0.9556 0.3680 1.0660 0.0661 0.524(8) Uiso R . P 3 1 .
H482 H 1.0108 0.4055 0.9748 0.0662 0.524(8) Uiso R . P 3 1 .
H491 H 1.0594 0.2227 1.0637 0.0646 0.524(8) Uiso R . P 3 1 .
H501 H 1.1338 0.3545 1.1802 0.0775 0.524(8) Uiso R . P 3 1 .
H502 H 1.2050 0.3823 1.0997 0.0773 0.524(8) Uiso R . P 3 1 .
H512 H 1.2931 0.2896 1.2423 0.1070 0.524(8) Uiso R . P 3 1 .
H511 H 1.2207 0.2029 1.1931 0.1074 0.524(8) Uiso R . P 3 1 .
H513 H 1.3046 0.2494 1.1335 0.1075 0.524(8) Uiso R . P 3 1 .
H521 H 1.1965 0.2282 0.9684 0.1079 0.524(8) Uiso R . P 3 1 .
H523 H 1.0839 0.2338 0.8977 0.1077 0.524(8) Uiso R . P 3 1 .
H522 H 1.1533 0.3258 0.9215 0.1080 0.524(8) Uiso R . P 3 1 .
H1481 H 0.9690 0.2942 1.0805 0.0658 0.476(8) Uiso R . P 3 2 .
H1482 H 1.0016 0.3894 1.0297 0.0665 0.476(8) Uiso R . P 3 2 .
H1491 H 1.0860 0.2016 1.0074 0.0501 0.476(8) Uiso R . P 3 2 .
H1501 H 1.2479 0.2488 1.0903 0.0790 0.476(8) Uiso R . P 3 2 .
H1502 H 1.2156 0.3570 1.0734 0.0793 0.476(8) Uiso R . P 3 2 .
H1511 H 1.2225 0.2713 1.2448 0.0940 0.476(8) Uiso R . P 3 2 .
H1512 H 1.0997 0.2702 1.1975 0.0940 0.476(8) Uiso R . P 3 2 .
H1513 H 1.1627 0.3662 1.2163 0.0940 0.476(8) Uiso R . P 3 2 .
H1522 H 1.1430 0.2502 0.8737 0.1058 0.476(8) Uiso R . P 3 2 .
H1523 H 1.0482 0.3229 0.8629 0.1062 0.476(8) Uiso R . P 3 2 .
H1521 H 1.1669 0.3549 0.9109 0.1058 0.476(8) Uiso R . P 3 2 .
H1332 H 0.2875 0.3832 0.7712 0.1229 0.312(7) Uiso R . P 1 2 .
H1331 H 0.2891 0.4924 0.7544 0.1229 0.312(7) Uiso R . P 1 2 .
H1333 H 0.3123 0.4514 0.8640 0.1229 0.312(7) Uiso R . P 1 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.84(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . S2 . 1.776(4) yes
C1 . C24 . 1.386(4) yes
C1 . C28 . 1.409(6) yes
S2 . C3 . 1.772(3) yes
C3 . C4 . 1.401(4) yes
C3 . C25 . 1.399(4) yes
C4 . C5 . 1.363(5) yes
C4 . H41 . 0.943 no
C5 . C6 . 1.388(5) yes
C5 . N53 . 1.479(4) yes
C6 . C7 . 1.389(4) yes
C6 . H61 . 0.933 no
C7 . S8 . 1.772(3) yes
C7 . C25 . 1.408(4) yes
S8 . C9 . 1.768(3) yes
C9 . C10 . 1.391(4) yes
C9 . C26 . 1.413(5) yes
C10 . C11 . 1.383(4) yes
C10 . H101 . 0.927 no
C11 . C12 . 1.386(4) yes
C11 . N56 . 1.468(3) yes
C12 . C13 . 1.395(4) yes
C12 . H121 . 0.958 no
C13 . S14 . 1.777(3) yes
C13 . C26 . 1.399(5) yes
S14 . C15 . 1.763(3) yes
C15 . C16 . 1.395(4) yes
C15 . C27 . 1.397(4) yes
C16 . C17 . 1.388(5) yes
C16 . H161 . 0.921 no
C17 . C18 . 1.397(5) yes
C17 . N59 . 1.455(4) yes
C18 . C19 . 1.380(5) yes
C18 . H181 . 0.943 no
C19 . S20 . 1.780(3) yes
C19 . C27 . 1.407(4) yes
S20 . C21 . 1.777(4) yes
C21 . C22 . 1.384(5) yes
C21 . C28 . 1.411(6) yes
C22 . C23 . 1.396(6) yes
C22 . H221 . 0.918 no
C23 . C24 . 1.374(6) yes
C23 . N62 . 1.467(4) yes
C24 . H241 . 0.927 no
C25 . O29 . 1.363(3) yes
C26 . O35 . 1.359(3) yes
C27 . O41 . 1.362(4) yes
C28 . O47 . 1.357(3) yes
O29 . C30 . 1.415(4) yes
O29 . C130 . 1.459(5) yes
C30 . C31 . 1.542(4) yes
C30 . H302 . 0.980 no
C30 . H301 . 0.972 no
C31 . C32 . 1.530(4) yes
C31 . C34 . 1.492(4) yes
C31 . H311 . 0.978 no
C32 . C33 . 1.495(5) yes
C32 . H322 . 0.971 no
C32 . H321 . 0.985 no
C33 . H332 . 0.947 no
C33 . H331 . 0.971 no
C33 . H333 . 0.953 no
C34 . H341 . 0.954 no
C34 . H342 . 0.963 no
C34 . H343 . 0.976 no
O35 . C36 . 1.463(3) yes
O35 . C136 . 1.438(5) yes
C36 . C37 . 1.541(4) yes
C36 . H362 . 0.981 no
C36 . H361 . 1.007 no
C37 . C38 . 1.509(4) yes
C37 . C40 . 1.492(4) yes
C37 . H371 . 0.990 no
C38 . C39 . 1.485(4) yes
C38 . H381 . 0.974 no
C38 . H382 . 0.993 no
C39 . H393 . 0.982 no
C39 . H391 . 1.000 no
C39 . H392 . 0.979 no
C40 . H403 . 0.953 no
C40 . H402 . 0.952 no
C40 . H401 . 0.959 no
O41 . C42 . 1.466(4) yes
C42 . C43 . 1.490(5) yes
C42 . H421 . 0.993 no
C42 . H422 . 0.968 no
C43 . C44 . 1.521(6) yes
C43 . C46 . 1.562(6) yes
C43 . H431 . 1.014 no
C44 . C45 . 1.533(7) yes
C44 . H442 . 0.989 no
C44 . H441 . 0.978 no
C45 . H452 . 0.982 no
C45 . H451 . 0.961 no
C45 . H453 . 0.959 no
C46 . H463 . 0.969 no
C46 . H462 . 0.977 no
C46 . H461 . 0.947 no
O47 . C48 . 1.447(4) yes
O47 . C148 . 1.445(5) yes
C48 . C49 . 1.540(5) yes
C48 . H481 . 0.963 no
C48 . H482 . 0.987 no
C49 . C50 . 1.532(4) yes
C49 . C52 . 1.496(5) yes
C49 . H491 . 0.994 no
C50 . C51 . 1.492(5) yes
C50 . H501 . 0.981 no
C50 . H502 . 0.969 no
C51 . H512 . 0.983 no
C51 . H511 . 0.975 no
C51 . H513 . 0.967 no
C52 . H521 . 0.959 no
C52 . H523 . 0.956 no
C52 . H522 . 0.974 no
N53 . O54 . 1.218(4) yes
N53 . O55 . 1.224(5) yes
N56 . O57 . 1.227(4) yes
N56 . O58 . 1.209(4) yes
N59 . O60 . 1.244(4) yes
N59 . O61 . 1.213(4) yes
N62 . O63 . 1.208(6) yes
N62 . O64 . 1.254(6) yes
C130 . C131 . 1.541(5) yes
C130 . H1302 . 0.974 no
C130 . H1301 . 0.963 no
C131 . C132 . 1.524(5) yes
C131 . C134 . 1.500(5) yes
C131 . H1311 . 0.982 no
C132 . C133 . 1.503(5) yes
C132 . H1321 . 0.973 no
C132 . H1322 . 0.966 no
C133 . H1332 . 0.950 no
C133 . H1331 . 0.950 no
C133 . H1333 . 0.950 no
C134 . H1342 . 1.084 no
C134 . H1341 . 1.102 no
C134 . H1343 . 1.095 no
C136 . C137 . 1.556(5) yes
C136 . H1362 . 0.968 no
C136 . H1361 . 0.975 no
C137 . C138 . 1.515(5) yes
C137 . C140 . 1.498(5) yes
C137 . H1371 . 0.985 no
C138 . C139 . 1.497(5) yes
C138 . H1381 . 0.971 no
C138 . H1382 . 0.970 no
C139 . H1392 . 0.960 no
C139 . H1391 . 0.955 no
C139 . H1393 . 0.956 no
C140 . H1401 . 0.953 no
C140 . H1403 . 0.959 no
C140 . H1402 . 0.955 no
C148 . C149 . 1.546(5) yes
C148 . H1481 . 0.957 no
C148 . H1482 . 0.967 no
C149 . C150 . 1.519(5) yes
C149 . C152 . 1.498(5) yes
C149 . H1491 . 0.993 no
C150 . C151 . 1.490(5) yes
C150 . H1501 . 0.965 no
C150 . H1502 . 0.968 no
C151 . H1511 . 0.965 no
C151 . H1512 . 0.960 no
C151 . H1513 . 0.965 no
C152 . H1522 . 0.954 no
C152 . H1523 . 0.967 no
C152 . H1521 . 0.968 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 . C1 . C24 . 117.1(3) yes
S2 . C1 . C28 . 122.9(3) yes
C24 . C1 . C28 . 119.8(4) yes
C1 . S2 . C3 . 103.80(15) yes
S2 . C3 . C4 . 117.0(2) yes
S2 . C3 . C25 . 123.0(2) yes
C4 . C3 . C25 . 119.6(3) yes
C3 . C4 . C5 . 118.7(3) yes
C3 . C4 . H41 . 122.0 no
C5 . C4 . H41 . 119.3 no
C4 . C5 . C6 . 124.0(3) yes
C4 . C5 . N53 . 118.5(3) yes
C6 . C5 . N53 . 117.5(3) yes
C5 . C6 . C7 . 117.2(3) yes
C5 . C6 . H61 . 121.5 no
C7 . C6 . H61 . 121.2 no
C6 . C7 . S8 . 115.9(2) yes
C6 . C7 . C25 . 120.8(3) yes
S8 . C7 . C25 . 122.9(2) yes
C7 . S8 . C9 . 106.35(13) yes
S8 . C9 . C10 . 115.8(2) yes
S8 . C9 . C26 . 123.0(2) yes
C10 . C9 . C26 . 120.6(2) yes
C9 . C10 . C11 . 118.4(3) yes
C9 . C10 . H101 . 122.3 no
C11 . C10 . H101 . 119.3 no
C10 . C11 . C12 . 122.9(2) yes
C10 . C11 . N56 . 118.2(3) yes
C12 . C11 . N56 . 118.9(3) yes
C11 . C12 . C13 . 118.3(3) yes
C11 . C12 . H121 . 120.4 no
C13 . C12 . H121 . 121.4 no
C12 . C13 . S14 . 114.9(2) yes
C12 . C13 . C26 . 120.8(3) yes
S14 . C13 . C26 . 123.2(2) yes
C13 . S14 . C15 . 105.83(13) yes
S14 . C15 . C16 . 117.0(2) yes
S14 . C15 . C27 . 122.2(2) yes
C16 . C15 . C27 . 120.2(3) yes
C15 . C16 . C17 . 118.7(3) yes
C15 . C16 . H161 . 121.0 no
C17 . C16 . H161 . 120.3 no
C16 . C17 . C18 . 121.9(3) yes
C16 . C17 . N59 . 118.6(3) yes
C18 . C17 . N59 . 119.5(3) yes
C17 . C18 . C19 . 118.7(3) yes
C17 . C18 . H181 . 119.1 no
C19 . C18 . H181 . 122.2 no
C18 . C19 . S20 . 116.1(2) yes
C18 . C19 . C27 . 120.5(3) yes
S20 . C19 . C27 . 122.6(2) yes
C19 . S20 . C21 . 104.29(15) yes
S20 . C21 . C22 . 117.0(3) yes
S20 . C21 . C28 . 121.7(3) yes
C22 . C21 . C28 . 121.1(3) yes
C21 . C22 . C23 . 118.0(3) yes
C21 . C22 . H221 . 119.6 no
C23 . C22 . H221 . 122.4 no
C22 . C23 . C24 . 122.3(3) yes
C22 . C23 . N62 . 118.4(4) yes
C24 . C23 . N62 . 119.2(4) yes
C1 . C24 . C23 . 119.7(3) yes
C1 . C24 . H241 . 118.4 no
C23 . C24 . H241 . 121.8 no
C7 . C25 . C3 . 119.6(3) yes
C7 . C25 . O29 . 119.0(2) yes
C3 . C25 . O29 . 121.4(3) yes
C9 . C26 . C13 . 118.9(2) yes
C9 . C26 . O35 . 121.2(3) yes
C13 . C26 . O35 . 120.0(3) yes
C19 . C27 . C15 . 119.5(3) yes
C19 . C27 . O41 . 120.6(3) yes
C15 . C27 . O41 . 119.9(2) yes
C21 . C28 . C1 . 118.9(3) yes
C21 . C28 . O47 . 118.3(4) yes
C1 . C28 . O47 . 122.7(4) yes
C25 . O29 . C30 . 116.9(3) yes
C25 . O29 . C130 . 108.4(4) yes
O29 . C30 . C31 . 109.5(3) yes
O29 . C30 . H302 . 108.2 no
C31 . C30 . H302 . 109.2 no
O29 . C30 . H301 . 111.3 no
C31 . C30 . H301 . 107.8 no
H302 . C30 . H301 . 110.7 no
C30 . C31 . C32 . 111.1(3) yes
C30 . C31 . C34 . 107.4(3) yes
C32 . C31 . C34 . 111.4(4) yes
C30 . C31 . H311 . 107.5 no
C32 . C31 . H311 . 109.8 no
C34 . C31 . H311 . 109.5 no
C31 . C32 . C33 . 113.2(4) yes
C31 . C32 . H322 . 110.9 no
C33 . C32 . H322 . 105.9 no
C31 . C32 . H321 . 107.0 no
C33 . C32 . H321 . 109.1 no
H322 . C32 . H321 . 110.8 no
C32 . C33 . H332 . 111.0 no
C32 . C33 . H331 . 109.6 no
H332 . C33 . H331 . 108.2 no
C32 . C33 . H333 . 110.6 no
H332 . C33 . H333 . 109.9 no
H331 . C33 . H333 . 107.4 no
C31 . C34 . H341 . 114.1 no
C31 . C34 . H342 . 110.6 no
H341 . C34 . H342 . 110.6 no
C31 . C34 . H343 . 103.7 no
H341 . C34 . H343 . 108.6 no
H342 . C34 . H343 . 108.9 no
C26 . O35 . C36 . 110.7(2) yes
C26 . O35 . C136 . 129.6(4) yes
O35 . C36 . C37 . 108.1(3) yes
O35 . C36 . H362 . 111.3 no
C37 . C36 . H362 . 111.4 no
O35 . C36 . H361 . 110.2 no
C37 . C36 . H361 . 107.6 no
H362 . C36 . H361 . 108.3 no
C36 . C37 . C38 . 113.7(3) yes
C36 . C37 . C40 . 107.7(3) yes
C38 . C37 . C40 . 112.9(3) yes
C36 . C37 . H371 . 105.8 no
C38 . C37 . H371 . 108.0 no
C40 . C37 . H371 . 108.3 no
C37 . C38 . C39 . 115.8(4) yes
C37 . C38 . H381 . 109.7 no
C39 . C38 . H381 . 107.3 no
C37 . C38 . H382 . 105.8 no
C39 . C38 . H382 . 107.5 no
H381 . C38 . H382 . 110.8 no
C38 . C39 . H393 . 109.8 no
C38 . C39 . H391 . 104.9 no
H393 . C39 . H391 . 108.9 no
C38 . C39 . H392 . 112.7 no
H393 . C39 . H392 . 109.9 no
H391 . C39 . H392 . 110.5 no
C37 . C40 . H403 . 113.4 no
C37 . C40 . H402 . 113.5 no
H403 . C40 . H402 . 107.3 no
C37 . C40 . H401 . 107.8 no
H403 . C40 . H401 . 106.4 no
H402 . C40 . H401 . 108.2 no
C27 . O41 . C42 . 112.3(3) yes
O41 . C42 . C43 . 109.0(3) yes
O41 . C42 . H421 . 109.9 no
C43 . C42 . H421 . 111.4 no
O41 . C42 . H422 . 110.8 no
C43 . C42 . H422 . 108.1 no
H421 . C42 . H422 . 107.6 no
C42 . C43 . C44 . 112.6(3) yes
C42 . C43 . C46 . 108.6(4) yes
C44 . C43 . C46 . 111.0(4) yes
C42 . C43 . H431 . 106.2 no
C44 . C43 . H431 . 108.0 no
C46 . C43 . H431 . 110.4 no
C43 . C44 . C45 . 112.1(4) yes
C43 . C44 . H442 . 108.5 no
C45 . C44 . H442 . 109.6 no
C43 . C44 . H441 . 109.5 no
C45 . C44 . H441 . 110.2 no
H442 . C44 . H441 . 106.7 no
C44 . C45 . H452 . 105.5 no
C44 . C45 . H451 . 109.3 no
H452 . C45 . H451 . 109.0 no
C44 . C45 . H453 . 111.2 no
H452 . C45 . H453 . 111.2 no
H451 . C45 . H453 . 110.6 no
C43 . C46 . H463 . 113.7 no
C43 . C46 . H462 . 111.1 no
H463 . C46 . H462 . 106.7 no
C43 . C46 . H461 . 110.3 no
H463 . C46 . H461 . 106.5 no
H462 . C46 . H461 . 108.3 no
C28 . O47 . C48 . 115.9(4) yes
C28 . O47 . C148 . 115.3(3) yes
O47 . C48 . C49 . 109.9(4) yes
O47 . C48 . H481 . 108.7 no
C49 . C48 . H481 . 111.6 no
O47 . C48 . H482 . 107.5 no
C49 . C48 . H482 . 107.8 no
H481 . C48 . H482 . 111.2 no
C48 . C49 . C50 . 112.2(4) yes
C48 . C49 . C52 . 106.9(4) yes
C50 . C49 . C52 . 110.8(4) yes
C48 . C49 . H491 . 107.4 no
C50 . C49 . H491 . 112.0 no
C52 . C49 . H491 . 107.3 no
C49 . C50 . C51 . 114.0(4) yes
C49 . C50 . H501 . 109.2 no
C51 . C50 . H501 . 106.8 no
C49 . C50 . H502 . 109.6 no
C51 . C50 . H502 . 108.6 no
H501 . C50 . H502 . 108.5 no
C50 . C51 . H512 . 109.8 no
C50 . C51 . H511 . 109.5 no
H512 . C51 . H511 . 108.4 no
C50 . C51 . H513 . 109.5 no
H512 . C51 . H513 . 109.9 no
H511 . C51 . H513 . 109.7 no
C49 . C52 . H521 . 109.3 no
C49 . C52 . H523 . 112.6 no
H521 . C52 . H523 . 108.2 no
C49 . C52 . H522 . 110.9 no
H521 . C52 . H522 . 107.8 no
H523 . C52 . H522 . 107.9 no
C5 . N53 . O54 . 118.7(3) yes
C5 . N53 . O55 . 117.3(3) yes
O54 . N53 . O55 . 124.0(3) yes
C11 . N56 . O57 . 117.6(3) yes
C11 . N56 . O58 . 118.3(3) yes
O57 . N56 . O58 . 124.1(2) yes
C17 . N59 . O60 . 117.3(3) yes
C17 . N59 . O61 . 119.2(3) yes
O60 . N59 . O61 . 123.5(3) yes
C23 . N62 . O63 . 118.0(4) yes
C23 . N62 . O64 . 118.0(4) yes
O63 . N62 . O64 . 124.0(3) yes
O29 . C130 . C131 . 109.4(4) yes
O29 . C130 . H1302 . 115.8 no
C131 . C130 . H1302 . 113.2 no
O29 . C130 . H1301 . 105.0 no
C131 . C130 . H1301 . 103.9 no
H1302 . C130 . H1301 . 108.5 no
C130 . C131 . C132 . 113.4(5) yes
C130 . C131 . C134 . 106.6(4) yes
C132 . C131 . C134 . 110.6(5) yes
C130 . C131 . H1311 . 112.8 no
C132 . C131 . H1311 . 104.8 no
C134 . C131 . H1311 . 108.7 no
C131 . C132 . C133 . 113.1(5) yes
C131 . C132 . H1321 . 110.5 no
C133 . C132 . H1321 . 61.4 no
C131 . C132 . H1322 . 104.8 no
C133 . C132 . H1322 . 141.9 no
H1321 . C132 . H1322 . 109.1 no
C132 . C133 . H1332 . 105.7 no
C132 . C133 . H1331 . 88.4 no
H1332 . C133 . H1331 . 109.5 no
C132 . C133 . H1333 . 131.5 no
H1332 . C133 . H1333 . 109.5 no
H1331 . C133 . H1333 . 109.5 no
C131 . C134 . H1342 . 106.6 no
C131 . C134 . H1341 . 108.3 no
H1342 . C134 . H1341 . 112.0 no
C131 . C134 . H1343 . 107.3 no
H1342 . C134 . H1343 . 111.8 no
H1341 . C134 . H1343 . 110.4 no
O35 . C136 . C137 . 108.0(5) yes
O35 . C136 . H1362 . 109.4 no
C137 . C136 . H1362 . 107.9 no
O35 . C136 . H1361 . 111.0 no
C137 . C136 . H1361 . 111.4 no
H1362 . C136 . H1361 . 109.1 no
C136 . C137 . C138 . 112.9(5) yes
C136 . C137 . C140 . 105.5(5) yes
C138 . C137 . C140 . 111.5(5) yes
C136 . C137 . H1371 . 110.4 no
C138 . C137 . H1371 . 108.3 no
C140 . C137 . H1371 . 108.1 no
C137 . C138 . C139 . 114.5(5) yes
C137 . C138 . H1381 . 109.4 no
C139 . C138 . H1381 . 109.2 no
C137 . C138 . H1382 . 106.7 no
C139 . C138 . H1382 . 107.2 no
H1381 . C138 . H1382 . 109.7 no
C138 . C139 . H1392 . 108.9 no
C138 . C139 . H1391 . 109.8 no
H1392 . C139 . H1391 . 109.3 no
C138 . C139 . H1393 . 109.3 no
H1392 . C139 . H1393 . 109.7 no
H1391 . C139 . H1393 . 109.8 no
C137 . C140 . H1401 . 112.3 no
C137 . C140 . H1403 . 108.2 no
H1401 . C140 . H1403 . 108.1 no
C137 . C140 . H1402 . 109.5 no
H1401 . C140 . H1402 . 109.4 no
H1403 . C140 . H1402 . 109.2 no
O47 . C148 . C149 . 108.5(4) yes
O47 . C148 . H1481 . 106.6 no
C149 . C148 . H1481 . 108.7 no
O47 . C148 . H1482 . 110.7 no
C149 . C148 . H1482 . 110.7 no
H1481 . C148 . H1482 . 111.5 no
C148 . C149 . C150 . 112.6(4) yes
C148 . C149 . C152 . 106.8(4) yes
C150 . C149 . C152 . 111.0(5) yes
C148 . C149 . H1491 . 109.8 no
C150 . C149 . H1491 . 106.7 no
C152 . C149 . H1491 . 110.1 no
C149 . C150 . C151 . 115.1(4) yes
C149 . C150 . H1501 . 109.7 no
C151 . C150 . H1501 . 109.5 no
C149 . C150 . H1502 . 105.0 no
C151 . C150 . H1502 . 107.8 no
H1501 . C150 . H1502 . 109.5 no
C150 . C151 . H1511 . 111.5 no
C150 . C151 . H1512 . 110.7 no
H1511 . C151 . H1512 . 108.2 no
C150 . C151 . H1513 . 111.5 no
H1511 . C151 . H1513 . 106.2 no
H1512 . C151 . H1513 . 108.5 no
C149 . C152 . H1522 . 108.1 no
C149 . C152 . H1523 . 109.3 no
H1522 . C152 . H1523 . 108.6 no
C149 . C152 . H1521 . 112.3 no
H1522 . C152 . H1521 . 108.9 no
H1523 . C152 . H1521 . 109.4 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C33 . H1343 . O64 2_657 147.1(10) 0.825 2.574 3.298(9) yes
C134 . H1343 . O64 2_657 128.7(3) 1.095 2.574 3.369(9) yes
C137 . H1371 . C16 . 152.8(2) 0.985 2.287 3.195(9) yes
C139 . H1391 . C36 . 120.3(6) 0.955 2.267 2.870(9) yes
C51 . H513 . O64 1_655 176.48(14) 0.967 2.600 3.565(9) yes
C51 . H1501 . C52 . 139.2(7) 1.176 2.155 3.141(9) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 17/10/14 at 16:27:18
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
EQUIVALENCE PART(2001, OCC) PART(2002, OCC) 
WEIGHT -1 PART(2002, OCC) 
EQUIVALENCE PART(3001, OCC) PART(3002, OCC) 
WEIGHT -1 PART(3002, OCC) 
CONT ENANTIO 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 393,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 442,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 452,X'S) H   ( 451,X'S) H   ( 453,X'S) 
RIDE C   (  46,X'S) H   ( 463,X'S) H   ( 462,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 512,X'S) H   ( 511,X'S) H   ( 513,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 523,X'S) H   ( 522,X'S) 
RIDE C   ( 130,X'S) H   (1302,X'S) H   (1301,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) H   (1322,X'S) 
RIDE C   ( 133,X'S) H   (1332,X'S) H   (1331,X'S) H   (1333,X'S) 
RIDE C   ( 134,X'S) H   (1342,X'S) H   (1341,X'S) H   (1343,X'S) 
RIDE C   ( 136,X'S) H   (1362,X'S) H   (1361,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) H   (1382,X'S) 
RIDE C   ( 139,X'S) H   (1392,X'S) H   (1391,X'S) H   (1393,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) H   (1403,X'S) H   (1402,X'S) 
RIDE C   ( 148,X'S) H   (1481,X'S) H   (1482,X'S) 
RIDE C   ( 149,X'S) H   (1491,X'S) 
RIDE C   ( 150,X'S) H   (1501,X'S) H   (1502,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) H   (1512,X'S) H   (1513,X'S) 
RIDE C   ( 152,X'S) H   (1522,X'S) H   (1523,X'S) H   (1521,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 17/10/14 at 16:27:18
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.440000 , 0.005000 = O(29) TO C(30) 
DISTANCE 1.560000 , 0.005000 = C(30) TO C(31) 
DISTANCE 1.520000 , 0.005000 = C(31) TO C(32) 
DISTANCE 1.500000 , 0.005000 = C(32) TO C(33) 
DISTANCE 1.500000 , 0.005000 = C(31) TO C(34) 
DISTANCE 2.420000 , 0.005000 = O(29) TO C(31) 
DISTANCE 2.560000 , 0.005000 = C(30) TO C(32) 
DISTANCE 2.530000 , 0.005000 = C(31) TO C(33) 
DISTANCE 2.420000 , 0.005000 = C(30) TO C(34) 
DISTANCE 2.490000 , 0.005000 = C(32) TO C(34) 
DISTANCE 1.440000 , 0.005000 = O(29) TO C(130) 
DISTANCE 1.560000 , 0.005000 = C(130) TO C(131) 
DISTANCE 1.520000 , 0.005000 = C(131) TO C(132) 
DISTANCE 1.500000 , 0.005000 = C(132) TO C(133) 
DISTANCE 1.500000 , 0.005000 = C(131) TO C(134) 
DISTANCE 2.420000 , 0.005000 = O(29) TO C(131) 
DISTANCE 2.560000 , 0.005000 = C(130) TO C(132) 
DISTANCE 2.530000 , 0.005000 = C(131) TO C(133) 
DISTANCE 2.420000 , 0.005000 = C(130) TO C(134) 
DISTANCE 2.490000 , 0.005000 = C(132) TO C(134) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(30) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(31) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(32) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(33) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(34) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(130) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(131) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(132) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(133) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(134) 
DISTANCE 1.440000 , 0.005000 = O(35) TO C(36) 
DISTANCE 1.560000 , 0.005000 = C(36) TO C(37) 
DISTANCE 1.520000 , 0.005000 = C(37) TO C(38) 
DISTANCE 1.500000 , 0.005000 = C(38) TO C(39) 
DISTANCE 1.500000 , 0.005000 = C(37) TO C(40) 
DISTANCE 2.420000 , 0.005000 = O(35) TO C(37) 
DISTANCE 2.560000 , 0.005000 = C(36) TO C(38) 
DISTANCE 2.530000 , 0.005000 = C(37) TO C(39) 
DISTANCE 2.420000 , 0.005000 = C(36) TO C(40) 
DISTANCE 2.490000 , 0.005000 = C(38) TO C(40) 
DISTANCE 1.440000 , 0.005000 = O(35) TO C(136) 
DISTANCE 1.560000 , 0.005000 = C(136) TO C(137) 
DISTANCE 1.520000 , 0.005000 = C(137) TO C(138) 
DISTANCE 1.500000 , 0.005000 = C(138) TO C(139) 
DISTANCE 1.500000 , 0.005000 = C(137) TO C(140) 
DISTANCE 2.420000 , 0.005000 = O(35) TO C(137) 
DISTANCE 2.560000 , 0.005000 = C(136) TO C(138) 
DISTANCE 2.530000 , 0.005000 = C(137) TO C(139) 
DISTANCE 2.420000 , 0.005000 = C(136) TO C(140) 
DISTANCE 2.490000 , 0.005000 = C(138) TO C(140) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(36) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(37) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(38) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(39) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(40) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(136) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(137) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(138) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(139) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(140) 
U(IJ)'S  0.0, 0.001000 = C(40) TO C(139) 
U(IJ)'S  0.0, 0.001000 = C(36) TO C(136) 
DISTANCE 1.440000 , 0.005000 = O(47) TO C(48) 
DISTANCE 1.560000 , 0.005000 = C(48) TO C(49) 
DISTANCE 1.520000 , 0.005000 = C(49) TO C(50) 
DISTANCE 1.500000 , 0.005000 = C(50) TO C(51) 
DISTANCE 1.500000 , 0.005000 = C(49) TO C(52) 
DISTANCE 2.420000 , 0.005000 = O(47) TO C(49) 
DISTANCE 2.560000 , 0.005000 = C(48) TO C(50) 
DISTANCE 2.530000 , 0.005000 = C(49) TO C(51) 
DISTANCE 2.420000 , 0.005000 = C(48) TO C(52) 
DISTANCE 2.490000 , 0.005000 = C(50) TO C(52) 
DISTANCE 1.440000 , 0.005000 = O(47) TO C(148) 
DISTANCE 1.560000 , 0.005000 = C(148) TO C(149) 
DISTANCE 1.520000 , 0.005000 = C(149) TO C(150) 
DISTANCE 1.500000 , 0.005000 = C(150) TO C(151) 
DISTANCE 1.500000 , 0.005000 = C(149) TO C(152) 
DISTANCE 2.420000 , 0.005000 = O(47) TO C(149) 
DISTANCE 2.560000 , 0.005000 = C(148) TO C(150) 
DISTANCE 2.530000 , 0.005000 = C(149) TO C(151) 
DISTANCE 2.420000 , 0.005000 = C(148) TO C(152) 
DISTANCE 2.490000 , 0.005000 = C(150) TO C(152) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(48) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(49) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(50) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(51) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(52) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(148) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(149) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(150) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(151) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(152) 
U(IJ)'S  0.0, 0.001000 = C(48) TO C(148) 
END                                                                             
;
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_4b
_database_code_depnum_ccdc_archive 'CCDC 1030577'
_audit_update_record             
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C40 H44 N4 O12 S4, 4(C2 H3 N)'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C48 H56 N8 O12 S4'
_chemical_formula_weight         1065.3
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_Int_Tables_number      12

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z

_cell_length_a                   28.7209(4)
_cell_length_b                   19.3593(4)
_cell_length_c                   13.9154(4)
_cell_angle_alpha                90
_cell_angle_beta                 136.110(3)
_cell_angle_gamma                90
_cell_volume                     5364.0(4)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
? ? ? ? ? ? ? ? ? ? ?

_cell_formula_units_Z            4

_cell_measurement_reflns_used    9027
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      67.01
_cell_measurement_temperature    120.00(14)
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.3191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2240

_exptl_absorpt_coefficient_mu    2.176
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.086
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_T_max  0.856
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      120
_diffrn_source                   ?
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            19122
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         67.05
_diffrn_reflns_theta_full        67.05
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measured_fraction_theta_full 0.99
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             4856
_reflns_number_gt                4198
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_gt          0.1383
_refine_ls_R_factor_all          0.0580
_refine_ls_wR_factor_ref         0.1425
_refine_ls_goodness_of_fit_ref   2.26
_refine_ls_goodness_of_fit_gt    2.37
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         4856
_refine_ls_number_parameters     373
_refine_ls_number_restraints     19
_refine_ls_number_constraints    328
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0016I²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0268
_refine_ls_shift/su_mean         0.0011
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0492 0.0322 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
S 0.3331 0.5567 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'Jana2006 (Petricek, Dusek & Palatinus, 2014)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'Jana2006 (Petricek, Dusek & Palatinus, 2014)'

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
C17 . C18 . 1.52 0.01
C21 . C22 . 1.52 0.01
C21a . C22a . 1.52 0.01
C25 . C26 . 1.52 0.01
C25a . C26a . 1.52 0.01
C18 . C19 . 1.54 0.01
C22 . C23 . 1.54 0.01
C22a . C23a . 1.54 0.01
C26 . C27 . 1.54 0.01
C26a . C27a . 1.54 0.01
C19 . C20 . 1.54 0.01
C23 . C24 . 1.54 0.01
C23a . C24a . 1.54 0.01
C27 . C28 . 1.54 0.01
C27a . C28a . 1.54 0.01

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
O1 . C17 . 1 0.01
O2 . C21 . 1 0.01
O2 . C21a . 1 0.01
O3 . C25 . 1 0.01
O3a . C25a . 1 0.01

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S4 S 0.38611(3) 0.14415(3) -0.00974(7) Uani 0.0346(5) 8 1 d . . .
S10 S 0.10831(3) 0.14338(3) -0.38415(6) Uani 0.0395(4) 8 1 d . . .
O1 O 0.35106(11) 0 0.0190(2) Uani 0.0326(17) 4 1 d . . .
O2 O 0.24174(9) 0.12326(8) -0.29078(16) Uani 0.0332(12) 8 1 d . . .
O3 O 0.1445(3) 0 -0.2558(7) Uani 0.0319(18) 4 0.458(6) d . 2 1
O3a O 0.1287(3) 0 -0.2674(6) Uani 0.0319 4 0.542(6) d . 2 2
O4 O 0.45343(11) 0.05557(10) -0.2466(2) Uani 0.0446(16) 8 1 d . . .
O5 O 0.32581(9) 0.18439(11) 0.25881(17) Uani 0.0448(13) 8 1 d . . .
O6 O 0.21807(10) 0.18819(11) 0.11387(19) Uani 0.0434(14) 8 1 d . . .
O7 O 0.05168(12) 0.05563(11) -0.8127(2) Uani 0.0517(17) 8 1 d . . .
N1 N 0.44414(14) 0 -0.2211(3) Uani 0.0323(19) 4 1 d . . .
N2 N 0.26893(11) 0.18074(10) 0.1412(2) Uani 0.0318(15) 8 1 d . . .
N3 N 0.05799(15) 0 -0.7633(3) Uani 0.036(2) 4 1 d . . .
C1 C 0.42064(15) 0 -0.1556(3) Uani 0.028(2) 4 1 d . . .
C2 C 0.41049(11) 0.06294(12) -0.1259(2) Uani 0.0289(15) 8 1 d . . .
C3 C 0.38770(11) 0.06271(12) -0.0652(2) Uani 0.0292(15) 8 1 d . . .
C5 C 0.31183(12) 0.14482(11) -0.0501(2) Uani 0.0288(16) 8 1 d . . .
C6 C 0.31858(12) 0.16018(12) 0.0569(2) Uani 0.0295(15) 8 1 d . . .
C7 C 0.26123(12) 0.16704(11) 0.0265(2) Uani 0.0276(15) 8 1 d . . .
C8 C 0.19715(12) 0.15984(12) -0.1063(2) Uani 0.0303(16) 8 1 d . . .
C9 C 0.19068(12) 0.14484(12) -0.2131(2) Uani 0.0305(15) 8 1 d . . .
C11 C 0.10449(11) 0.06263(13) -0.4499(2) Uani 0.0307(14) 8 1 d . . .
C12 C 0.08450(11) 0.06280(12) -0.5755(2) Uani 0.0299(14) 8 1 d . . .
C13 C 0.07544(15) 0 -0.6342(3) Uani 0.028(2) 4 1 d . . .
C14 C 0.37612(16) 0 -0.0349(3) Uani 0.029(2) 4 1 d . . .
C15 C 0.24794(12) 0.13786(11) -0.1860(2) Uani 0.0295(16) 8 1 d . . .
C16 C 0.11438(16) 0 -0.3868(3) Uani 0.0319(18) 4 1 d . . .
C17 C 0.40039(18) 0 0.1686(3) Uani 0.039(3) 4 1 d . . .
C18 C 0.36198(19) 0 0.2053(4) Uani 0.037(3) 4 1 d . . .
C19 C 0.4084(3) 0 0.3603(5) Uani 0.076(4) 4 1 d . . .
C20 C 0.3698(3) 0 0.3975(5) Uani 0.079(5) 4 1 d . . .
C21 C 0.2363(3) 0.1857(3) -0.3584(6) Uani 0.048(4) 8 0.759(5) d . 1 1
C22 C 0.2172(2) 0.1638(2) -0.4870(4) Uani 0.041(3) 8 0.759(5) d . 1 1
C23 C 0.2742(2) 0.1239(2) -0.4502(4) Uani 0.049(3) 8 0.759(5) d . 1 1
C24 C 0.2586(5) 0.1017(7) -0.5767(10) Uani 0.078(6) 8 0.759(5) d . 1 1
C21a C 0.2216(12) 0.1802(9) -0.382(2) Uani 0.048(4) 8 0.241(5) d . 1 2
C22a C 0.2507(7) 0.1654(6) -0.4373(13) Uani 0.041(3) 8 0.241(5) d . 1 2
C23a C 0.2361(7) 0.0961(6) -0.5078(13) Uani 0.049(3) 8 0.241(5) d . 1 2
C24a C 0.2699(18) 0.108(2) -0.555(4) Uani 0.078(6) 8 0.241(5) d . 1 2
C25 C 0.0980(5) 0 -0.2460(9) Uani 0.042(8) 4 0.458(6) d . 2 1
C26 C 0.1425(4) 0 -0.0905(8) Uani 0.046(5) 4 0.458(6) d . 2 1
C27 C 0.1001(5) 0 -0.0629(8) Uani 0.055(6) 4 0.458(6) d . 2 1
C28 C 0.1456(6) 0 0.0929(9) Uani 0.052(7) 4 0.458(6) d . 2 1
C25a C 0.0732(4) -0.0151(7) -0.2831(9) Uani 0.042(8) 8 0.271(3) d . 2 2
C26a C 0.0948(4) 0.0209(5) -0.1576(8) Uani 0.046(5) 8 0.271(3) d . 2 2
C27a C 0.1582(5) 0.0249(6) -0.0142(8) Uani 0.055(6) 8 0.271(3) d . 2 2
C28a C 0.1739(6) -0.0102(8) 0.1044(10) Uani 0.052(7) 8 0.271(3) d . 2 2
N1s N 0.95890(15) 0.20580(19) 0.2453(3) Uani 0.069(2) 8 1 d . . .
C2s C 0.99812(15) 0.25027(18) 0.3086(3) Uani 0.050(2) 8 1 d . . .
C3s C 1.04803(19) 0.30527(18) 0.3850(3) Uani 0.060(2) 8 1 d . . .
N4s N 0.5771(2) 0.2435(2) 0.1991(4) Uani 0.095(4) 8 1 d . . .
C5s C 0.58119(18) 0.2816(2) 0.1395(4) Uani 0.064(3) 8 1 d . . .
C6s C 0.58448(17) 0.32702(17) 0.0619(4) Uani 0.056(3) 8 1 d . . .
H1c2 H 0.418909 0.105546 -0.14659 Uiso 0.0347 8 1 d . . .
H1c6 H 0.362204 0.165905 0.150067 Uiso 0.0353 8 1 d . . .
H1c8 H 0.158267 0.165083 -0.12399 Uiso 0.0363 8 1 d . . .
H1c12 H 0.077214 0.105402 -0.620035 Uiso 0.0358 8 1 d . . .
H1c17 H 0.427198 0.041104 0.204257 Uiso 0.0471 8 1 d . . .
H1c18 H 0.333339 -0.039841 0.165348 Uiso 0.0439 8 1 d . . .
H1c19 H 0.437122 0.03982 0.400278 Uiso 0.0909 8 1 d . . .
H1c20 H 0.398946 -0.01493 0.49174 Uiso 0.0945 8 0.5 d . . .
H2c20 H 0.354 0.045834 0.387348 Uiso 0.0945 8 0.5 d . . .
H3c20 H 0.332286 -0.030904 0.336913 Uiso 0.0945 8 0.5 d . . .
H1c25 H 0.071794 -0.041631 -0.286378 Uiso 0.05 8 0.458(6) d . 2 1
H1c26 H 0.170786 0.040191 -0.049184 Uiso 0.0553 8 0.458(6) d . 2 1
H1c27 H 0.072193 -0.040418 -0.103474 Uiso 0.0663 8 0.458(6) d . 2 1
H1c28 H 0.121356 0.017764 0.111038 Uiso 0.0625 8 0.229(3) d . 2 1
H2c28 H 0.160046 -0.046334 0.127663 Uiso 0.0625 8 0.229(3) d . 2 1
H3c28 H 0.184102 0.02857 0.138 Uiso 0.0625 8 0.229(3) d . 2 1
H1c25a H 0.070598 -0.064059 -0.276486 Uiso 0.05 8 0.271(3) d . 2 2
H2c25a H 0.032636 0.005669 -0.366971 Uiso 0.05 8 0.271(3) d . 2 2
H1c26a H 0.059182 0.017876 -0.164368 Uiso 0.0553 8 0.271(3) d . 2 2
H2c26a H 0.071739 0.064189 -0.186179 Uiso 0.0553 8 0.271(3) d . 2 2
H1c27a H 0.172839 0.072088 0.009911 Uiso 0.0663 8 0.271(3) d . 2 2
H2c27a H 0.193983 0.01612 -0.005692 Uiso 0.0663 8 0.271(3) d . 2 2
H1c28a H 0.133025 -0.01738 0.078666 Uiso 0.0625 8 0.271(3) d . 2 2
H2c28a H 0.195099 -0.053962 0.123961 Uiso 0.0625 8 0.271(3) d . 2 2
H3c28a H 0.203598 0.018494 0.185414 Uiso 0.0625 8 0.271(3) d . 2 2
H1c3s H 1.071589 0.306492 0.359914 Uiso 0.0718 8 1 d . . .
H2c3s H 1.026058 0.348762 0.362822 Uiso 0.0718 8 1 d . . .
H3c3s H 1.079332 0.296794 0.482727 Uiso 0.0718 8 1 d . . .
H1c6s H 0.566747 0.371502 0.052402 Uiso 0.0672 8 1 d . . .
H2c6s H 0.63037 0.331886 0.110073 Uiso 0.0672 8 1 d . . .
H3c6s H 0.558514 0.307769 -0.028338 Uiso 0.0672 8 1 d . . .
H1c21 H 0.278953 0.208845 -0.296679 Uiso 0.0581 8 0.759(5) d . 1 1
H2c21 H 0.202147 0.215338 -0.383507 Uiso 0.0581 8 0.759(5) d . 1 1
H1c22 H 0.206584 0.203921 -0.540372 Uiso 0.0491 8 0.759(5) d . 1 1
H2c22 H 0.177767 0.135277 -0.542899 Uiso 0.0491 8 0.759(5) d . 1 1
H1c23 H 0.284894 0.08398 -0.396349 Uiso 0.0584 8 0.759(5) d . 1 1
H2c23 H 0.314243 0.151481 -0.389902 Uiso 0.0584 8 0.759(5) d . 1 1
H1c24 H 0.259485 0.141373 -0.616665 Uiso 0.0934 8 0.759(5) d . 1 1
H2c24 H 0.291586 0.068885 -0.548623 Uiso 0.0934 8 0.759(5) d . 1 1
H3c24 H 0.214829 0.080866 -0.644066 Uiso 0.0934 8 0.759(5) d . 1 1
H1c21a H 0.240182 0.22245 -0.330217 Uiso 0.0581 8 0.241(5) d . 1 2
H2c21a H 0.173541 0.181674 -0.45778 Uiso 0.0581 8 0.241(5) d . 1 2
H1c22a H 0.298235 0.173388 -0.365519 Uiso 0.0491 8 0.241(5) d . 1 2
H2c22a H 0.239386 0.20247 -0.497025 Uiso 0.0491 8 0.241(5) d . 1 2
H1c23a H 0.188582 0.091085 -0.587532 Uiso 0.0584 8 0.241(5) d . 1 2
H2c23a H 0.259153 0.059898 -0.439941 Uiso 0.0584 8 0.241(5) d . 1 2
H1c24a H 0.238563 0.129575 -0.644868 Uiso 0.0934 8 0.241(5) d . 1 2
H2c24a H 0.308172 0.137823 -0.489957 Uiso 0.0934 8 0.241(5) d . 1 2
H3c24a H 0.284252 0.064757 -0.559995 Uiso 0.0934 8 0.241(5) d . 1 2


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S4 C3 . . 1.770(3) ?
S4 C5 . . 1.772(4) ?
S10 C9 . . 1.7737(18) ?
S10 C11 . . 1.774(3) ?
O1 C14 . . 1.363(7) ?
O1 C17 . . 1.445(4) ?
O2 C15 . . 1.364(5) ?
O2 C21 . . 1.469(7) ?
O2 C21a . . 1.45(2) ?
O3 C16 . . 1.341(10) ?
O3 C25 . . 1.44(2) ?
O3a C16 . . 1.395(10) ?
O3a C25a . . 1.473(17) ?
O3a C25a . 4_555 1.473(17) ?
O4 N1 . . 1.222(3) ?
O5 N2 . . 1.224(2) ?
O6 N2 . . 1.224(4) ?
O7 N3 . . 1.219(3) ?
N1 C1 . . 1.473(8) ?
N2 C7 . . 1.469(5) ?
N3 C13 . . 1.477(6) ?
C1 C2 . . 1.384(4) ?
C1 C2 . 4_555 1.384(4) ?
C2 C3 . . 1.393(6) ?
C2 H1c2 . . 0.96 ?
C3 C14 . . 1.401(4) ?
C5 C6 . . 1.389(6) ?
C5 C15 . . 1.400(3) ?
C6 C7 . . 1.380(5) ?
C6 H1c6 . . 0.96 ?
C7 C8 . . 1.385(2) ?
C8 C9 . . 1.390(5) ?
C8 H1c8 . . 0.96 ?
C9 C15 . . 1.404(5) ?
C11 C12 . . 1.392(5) ?
C11 C16 . . 1.401(4) ?
C12 C13 . . 1.381(3) ?
C12 H1c12 . . 0.96 ?
C17 C18 . . 1.514(9) ?
C17 H1c17 . . 0.96 ?
C17 H1c17 . 4_555 0.96 ?
C18 C19 . . 1.511(7) ?
C18 H1c18 . . 0.96 ?
C18 H1c18 . 4_555 0.96 ?
C19 C20 . . 1.525(14) ?
C19 H1c19 . . 0.96 ?
C19 H1c19 . 4_555 0.96 ?
C20 H1c20 . . 0.96 ?
C20 H1c20 . 4_555 0.96 ?
C20 H2c20 . . 0.96 ?
C20 H2c20 . 4_555 0.96 ?
C20 H3c20 . . 0.96 ?
C20 H3c20 . 4_555 0.96 ?
C21 C22 . . 1.505(11) ?
C21 H1c21 . . 0.96 ?
C21 H2c21 . . 0.96 ?
C22 C23 . . 1.526(8) ?
C22 H1c22 . . 0.96 ?
C22 H2c22 . . 0.96 ?
C23 C24 . . 1.533(17) ?
C23 H1c23 . . 0.96 ?
C23 H2c23 . . 0.96 ?
C24 C23a . . 1.49(3) ?
C24 H1c24 . . 0.96 ?
C24 H2c24 . . 0.96 ?
C24 H3c24 . . 0.96 ?
C21a C22a . . 1.51(5) ?
C21a H1c21a . . 0.96 ?
C21a H2c21a . . 0.96 ?
C22a C23a . . 1.532(19) ?
C22a H1c22a . . 0.96 ?
C22a H2c22a . . 0.96 ?
C23a C24a . . 1.53(7) ?
C23a H1c23a . . 0.96 ?
C23a H2c23a . . 0.96 ?
C24a H1c24a . . 0.96 ?
C24a H2c24a . . 0.96 ?
C24a H3c24a . . 0.96 ?
C25 C26 . . 1.525(15) ?
C25 C25a . . 0.573(13) ?
C25 C25a . 4_555 0.573(13) ?
C25 C26a . . 1.36(2) ?
C25 C26a . 4_555 1.36(2) ?
C25 H1c25 . . 0.96 ?
C25 H1c25 . 4_555 0.96 ?
C26 C27 . . 1.52(2) ?
C26 C26a . . 1.034(12) ?
C26 C26a . 4_555 1.034(12) ?
C26 C27a . . 0.935(15) ?
C26 C27a . 4_555 0.935(15) ?
C26 H1c26 . . 0.96 ?
C26 H1c26 . 4_555 0.96 ?
C27 C28 . . 1.524(15) ?
C27 H1c27 . . 0.96 ?
C27 H1c27 . 4_555 0.96 ?
C28 H1c28 . . 0.96 ?
C28 H1c28 . 4_555 0.96 ?
C28 H2c28 . . 0.96 ?
C28 H2c28 . 4_555 0.96 ?
C28 H3c28 . . 0.96 ?
C28 H3c28 . 4_555 0.96 ?
C25a C26a . . 1.536(18) ?
C25a H1c25a . . 0.96 ?
C25a H2c25a . . 0.96 ?
C26a C27a . . 1.438(9) ?
C26a H1c26a . . 0.96 ?
C26a H2c26a . . 0.96 ?
C27a C28a . . 1.52(2) ?
C27a H1c27a . . 0.96 ?
C27a H2c27a . . 0.96 ?
C28a H1c28a . . 0.96 ?
C28a H2c28a . . 0.96 ?
C28a H3c28a . . 0.96 ?
N1s C2s . . 1.164(5) ?
C2s C3s . . 1.457(5) ?
C3s H1c3s . . 0.96 ?
C3s H2c3s . . 0.96 ?
C3s H3c3s . . 0.96 ?
N4s C5s . . 1.177(9) ?
C5s C6s . . 1.448(8) ?
C6s H1c6s . . 0.96 ?
C6s H2c6s . . 0.96 ?
C6s H3c6s . . 0.96 ?


loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 S4 C5 . . . 105.75(13) ?
C9 S10 C11 . . . 103.47(11) ?
C14 O1 C17 . . . 115.7(3) ?
C15 O2 C21 . . . 112.7(4) ?
C15 O2 C21a . . . 116.2(13) ?
C16 O3 C25 . . . 113.4(5) ?
C16 O3a C25a . . . 117.6(5) ?
C16 O3a C25a . . 4_555 117.6(5) ?
O4 N1 O4 . . 4_555 123.4(5) ?
O4 N1 C1 . . . 118.3(3) ?
O4 N1 C1 4_555 . . 118.3(3) ?
O5 N2 O6 . . . 123.5(3) ?
O5 N2 C7 . . . 118.3(3) ?
O6 N2 C7 . . . 118.19(18) ?
O7 N3 O7 . . 4_555 124.2(4) ?
O7 N3 C13 . . . 117.9(2) ?
O7 N3 C13 4_555 . . 117.9(2) ?
N1 C1 C2 . . . 118.3(3) ?
N1 C1 C2 . . 4_555 118.3(3) ?
C2 C1 C2 . . 4_555 123.5(5) ?
C1 C2 C3 . . . 118.1(3) ?
C1 C2 H1c2 . . . 120.96 ?
C3 C2 H1c2 . . . 120.96 ?
S4 C3 C2 . . . 115.6(2) ?
S4 C3 C14 . . . 123.7(3) ?
C2 C3 C14 . . . 120.1(3) ?
S4 C5 C6 . . . 117.11(16) ?
S4 C5 C15 . . . 122.3(3) ?
C6 C5 C15 . . . 120.2(3) ?
C5 C6 C7 . . . 118.6(2) ?
C5 C6 H1c6 . . . 120.72 ?
C7 C6 H1c6 . . . 120.72 ?
N2 C7 C6 . . . 118.17(19) ?
N2 C7 C8 . . . 118.8(3) ?
C6 C7 C8 . . . 123.0(3) ?
C7 C8 C9 . . . 118.2(3) ?
C7 C8 H1c8 . . . 120.9 ?
C9 C8 H1c8 . . . 120.9 ?
S10 C9 C8 . . . 117.4(3) ?
S10 C9 C15 . . . 122.0(3) ?
C8 C9 C15 . . . 120.3(2) ?
S10 C11 C12 . . . 117.50(19) ?
S10 C11 C16 . . . 122.0(3) ?
C12 C11 C16 . . . 120.2(3) ?
C11 C12 C13 . . . 118.2(3) ?
C11 C12 H1c12 . . . 120.91 ?
C13 C12 H1c12 . . . 120.91 ?
N3 C13 C12 . . . 118.3(2) ?
N3 C13 C12 . . 4_555 118.3(2) ?
C12 C13 C12 . . 4_555 123.4(4) ?
O1 C14 C3 . . . 119.9(3) ?
O1 C14 C3 . . 4_555 119.9(3) ?
C3 C14 C3 . . 4_555 120.1(5) ?
O2 C15 C5 . . . 119.9(3) ?
O2 C15 C9 . . . 120.48(18) ?
C5 C15 C9 . . . 119.7(3) ?
O3 C16 C11 . . . 119.51(17) ?
O3 C16 C11 . . 4_555 119.51(17) ?
O3a C16 C11 . . . 119.9(2) ?
O3a C16 C11 . . 4_555 119.9(2) ?
C11 C16 C11 . . 4_555 119.9(4) ?
O1 C17 C18 . . . 106.8(3) ?
O1 C17 H1c17 . . . 109.47 ?
O1 C17 H1c17 . . 4_555 109.47 ?
C18 C17 H1c17 . . . 109.47 ?
C18 C17 H1c17 . . 4_555 109.47 ?
H1c17 C17 H1c17 . . 4_555 111.97 ?
C17 C18 C19 . . . 111.9(4) ?
C17 C18 H1c18 . . . 109.47 ?
C17 C18 H1c18 . . 4_555 109.47 ?
C19 C18 H1c18 . . . 109.47 ?
C19 C18 H1c18 . . 4_555 109.47 ?
H1c18 C18 H1c18 . . 4_555 106.92 ?
C18 C19 C20 . . . 112.0(5) ?
C18 C19 H1c19 . . . 109.47 ?
C18 C19 H1c19 . . 4_555 109.47 ?
C20 C19 H1c19 . . . 109.47 ?
C20 C19 H1c19 . . 4_555 109.47 ?
H1c19 C19 H1c19 . . 4_555 106.84 ?
C19 C20 H1c20 . . . 109.47 ?
C19 C20 H1c20 . . 4_555 109.47 ?
C19 C20 H2c20 . . . 109.47 ?
C19 C20 H2c20 . . 4_555 109.47 ?
C19 C20 H3c20 . . . 109.47 ?
C19 C20 H3c20 . . 4_555 109.47 ?
H1c20 C20 H2c20 . . . 109.47 ?
H1c20 C20 H3c20 . . . 109.47 ?
H1c20 C20 H2c20 4_555 . 4_555 109.47 ?
H1c20 C20 H3c20 4_555 . 4_555 109.47 ?
H2c20 C20 H3c20 . . . 109.47 ?
H2c20 C20 H3c20 4_555 . 4_555 109.47 ?
O2 C21 C22 . . . 108.0(4) ?
O2 C21 H1c21 . . . 109.47 ?
O2 C21 H2c21 . . . 109.47 ?
C22 C21 H1c21 . . . 109.47 ?
C22 C21 H2c21 . . . 109.47 ?
H1c21 C21 H2c21 . . . 110.88 ?
C21 C22 C23 . . . 111.0(4) ?
C21 C22 H1c22 . . . 109.47 ?
C21 C22 H2c22 . . . 109.47 ?
C23 C22 H1c22 . . . 109.47 ?
C23 C22 H2c22 . . . 109.47 ?
H1c22 C22 H2c22 . . . 107.92 ?
C22 C23 C24 . . . 113.7(5) ?
C22 C23 H1c23 . . . 109.47 ?
C22 C23 H2c23 . . . 109.47 ?
C24 C23 H1c23 . . . 109.47 ?
C24 C23 H2c23 . . . 109.47 ?
H1c23 C23 H2c23 . . . 104.9 ?
C23 C24 H1c24 . . . 109.47 ?
C23 C24 H2c24 . . . 109.47 ?
C23 C24 H3c24 . . . 109.47 ?
H1c24 C24 H2c24 . . . 109.47 ?
H1c24 C24 H3c24 . . . 109.47 ?
H2c24 C24 H3c24 . . . 109.47 ?
O2 C21a C22a . . . 106.6(17) ?
O2 C21a H1c21a . . . 109.47 ?
O2 C21a H2c21a . . . 109.47 ?
C22a C21a H1c21a . . . 109.47 ?
C22a C21a H2c21a . . . 109.47 ?
H1c21a C21a H2c21a . . . 112.23 ?
C21a C22a C23a . . . 119.7(17) ?
C21a C22a H1c22a . . . 109.47 ?
C21a C22a H2c22a . . . 109.47 ?
C23a C22a H1c22a . . . 109.47 ?
C23a C22a H2c22a . . . 109.47 ?
H1c22a C22a H2c22a . . . 96.89 ?
C22a C23a C24a . . . 100(2) ?
C22a C23a H1c23a . . . 109.47 ?
C22a C23a H2c23a . . . 109.47 ?
C24a C23a H1c23a . . . 109.47 ?
C24a C23a H2c23a . . . 109.47 ?
H1c23a C23a H2c23a . . . 117.38 ?
C23a C24a H1c24a . . . 109.47 ?
C23a C24a H2c24a . . . 109.47 ?
C23a C24a H3c24a . . . 109.47 ?
H1c24a C24a H2c24a . . . 109.47 ?
H1c24a C24a H3c24a . . . 109.47 ?
H2c24a C24a H3c24a . . . 109.47 ?
O3 C25 C26 . . . 104.3(8) ?
O3 C25 H1c25 . . . 109.47 ?
O3 C25 H1c25 . . 4_555 109.47 ?
C26 C25 H1c25 . . . 109.47 ?
C26 C25 H1c25 . . 4_555 109.47 ?
H1c25 C25 H1c25 . . 4_555 114.18 ?
C25 C26 C27 . . . 110.6(8) ?
C25 C26 H1c26 . . . 109.47 ?
C25 C26 H1c26 . . 4_555 109.47 ?
C27 C26 H1c26 . . . 109.47 ?
C27 C26 H1c26 . . 4_555 109.47 ?
H1c26 C26 H1c26 . . 4_555 108.29 ?
C26 C27 C28 . . . 109.8(10) ?
C26 C27 H1c27 . . . 109.47 ?
C26 C27 H1c27 . . 4_555 109.47 ?
C28 C27 H1c27 . . . 109.47 ?
C28 C27 H1c27 . . 4_555 109.47 ?
H1c27 C27 H1c27 . . 4_555 109.19 ?
C27 C28 H1c28 . . . 109.47 ?
C27 C28 H1c28 . . 4_555 109.47 ?
C27 C28 H2c28 . . . 109.47 ?
C27 C28 H2c28 . . 4_555 109.47 ?
C27 C28 H3c28 . . . 109.47 ?
C27 C28 H3c28 . . 4_555 109.47 ?
H1c28 C28 H2c28 . . . 109.47 ?
H1c28 C28 H3c28 . . . 109.47 ?
H2c28 C28 H3c28 . . . 109.47 ?
H1c28 C28 H2c28 4_555 . 4_555 109.47 ?
H1c28 C28 H3c28 4_555 . 4_555 109.47 ?
H2c28 C28 H3c28 4_555 . 4_555 109.47 ?
O3a C25a C26a . . . 103.5(8) ?
O3a C25a H1c25 . . . 102.74 ?
O3a C25a H1c25a . . . 109.47 ?
O3a C25a H2c25a . . . 109.47 ?
C26a C25a H1c25 . . . 119.58 ?
C26a C25a H1c25a . . . 109.47 ?
C26a C25a H2c25a . . . 109.47 ?
H1c25a C25a H2c25a . . . 114.85 ?
C25a C26a C27a . . . 132.3(11) ?
C25a C26a H1c26a . . . 109.47 ?
C25a C26a H2c26a . . . 109.47 ?
C27a C26a H1c26a . . . 109.47 ?
C27a C26a H2c26a . . . 109.47 ?
H1c26a C26a H2c26a . . . 69.04 ?
C26a C27a C28a . . . 124.8(12) ?
C26a C27a H1c26 . . . 81.81 ?
C26a C27a H1c27a . . . 109.47 ?
C26a C27a H2c27a . . . 109.47 ?
C28a C27a H1c27a . . . 109.47 ?
C28a C27a H2c27a . . . 109.47 ?
H1c27a C27a H2c27a . . . 88.03 ?
C27a C28a H1c28a . . . 109.47 ?
C27a C28a H2c28a . . . 109.47 ?
C27a C28a H3c28a . . . 109.47 ?
H1c28a C28a H2c28a . . . 109.47 ?
H1c28a C28a H3c28a . . . 109.47 ?
H2c28a C28a H3c28a . . . 109.47 ?
N1s C2s C3s . . . 177.6(6) ?
C2s C3s H1c3s . . . 109.47 ?
C2s C3s H2c3s . . . 109.47 ?
C2s C3s H3c3s . . . 109.47 ?
H1c3s C3s H2c3s . . . 109.47 ?
H1c3s C3s H3c3s . . . 109.47 ?
H2c3s C3s H3c3s . . . 109.47 ?
N4s C5s C6s . . . 177.9(4) ?
C5s C6s H1c6s . . . 109.47 ?
C5s C6s H2c6s . . . 109.47 ?
C5s C6s H3c6s . . . 109.47 ?
H1c6s C6s H2c6s . . . 109.47 ?
H1c6s C6s H3c6s . . . 109.47 ?
H2c6s C6s H3c6s . . . 109.47 ?


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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C27a H1c27a O6 . . . 0.96 2.47 3.422(11) 169.22 ?

