# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_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                   7.8956(4)
_cell_length_b                   9.6557(3)
_cell_length_c                   14.9160(6)
_cell_angle_alpha                77.311(3)
_cell_angle_beta                 81.835(4)
_cell_angle_gamma                86.214(3)
_cell_volume                     1097.43(8)
_cell_measurement_reflns_used    6458
_cell_measurement_theta_min      2.3010
_cell_measurement_theta_max      29.0590
_cell_oxdiff_length_a            7.8956(4)
_cell_oxdiff_length_b            9.6557(3)
_cell_oxdiff_length_c            14.9160(6)
_cell_oxdiff_angle_alpha         77.311(3)
_cell_oxdiff_angle_beta          81.835(4)
_cell_oxdiff_angle_gamma         86.214(3)
_cell_oxdiff_volume              1097.43(8)

_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 0.0033 0.0016 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'
S 0.1246 0.1234 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'
O 0.0106 0.0060 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'
N 0.0061 0.0033 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'
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'


_cell_formula_units_Z            1

_chemical_formula_sum            'C36 H66 N4 O16 S4'
_chemical_formula_moiety         'C16 H6 O12 S4, 2(C10 H26 N2), 4(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         939.21


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.25
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_max          0.50
_exptl_absorpt_correction_T_min  0.97075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             502
_exptl_absorpt_coefficient_mu    0.290
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 16.0143

_diffrn_measurement_device       Area
_diffrn_radiation_wavelength     0.71073
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
#montpellier_reflns_maxres is minimum d (highest resolution)
#where <I/sigI> <= 2.0
#(Z. Dauter, Acta Cryst. D55, 1703-1717, 1999)
_montpellier_reflns_maxres       0.72
_montpellier_reflns_completeness_maxres 86.85
_montpellier_reflns_redundancy_maxres 2.94

#montpellier_diffrn_reflns_class_completeness_shell is completeness in shell
#montpellier_diffrn_class_reflns_cumul_completeness is cumulative
#completeness to resolution of shell
#Note: completeness percentage takes into account the fact whether
#group is centrosymmetric or not
loop_
_montpellier_diffrn_reflns_class_number
_montpellier_diffrn_reflns_class_d_res_high
_montpellier_diffrn_reflns_class_d_res_low
_montpellier_diffrn_reflns_class_redundancy
_montpellier_diffrn_reflns_class_av_I/uI
_diffrn_reflns_class_av_R_eq
_montpellier_diffrn_reflns_class_completeness_shell
_montpellier_diffrn_reflns_class_cumul_completeness
0 100.0 1.63 5.3 65.01 0.023 99.8 99.81
1 1.63 1.30 4.1 35.30 0.034 100.0 99.90
2 1.30 1.13 3.7 28.56 0.033 100.0 99.94
3 1.13 1.03 3.0 18.76 0.041 100.0 99.95
4 1.03 0.96 2.8 13.89 0.050 100.0 99.96
5 0.96 0.90 2.6 10.95 0.062 100.0 99.97
6 0.90 0.86 2.4 9.48 0.069 100.0 99.97
7 0.86 0.82 2.3 7.82 0.084 100.0 99.98
8 0.82 0.78 2.0 6.95 0.095 93.8 99.24
9 0.78 0.72 1.3 5.26 0.080 41.3 86.85
#End reflection statistics
_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_orient_matrix_UB_11      0.0824545000
_diffrn_orient_matrix_UB_12      0.0249365000
_diffrn_orient_matrix_UB_13      0.0001357000
_diffrn_orient_matrix_UB_21      0.0322593000
_diffrn_orient_matrix_UB_22      -0.0314879000
_diffrn_orient_matrix_UB_23      -0.0380024000
_diffrn_orient_matrix_UB_31      -0.0201907000
_diffrn_orient_matrix_UB_32      0.0637491000
_diffrn_orient_matrix_UB_33      -0.0311959000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -53.00   44.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -       15.4892  -19.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega   49.00   88.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -       15.4892  179.0000 -150.0000 39

#__ type_ start__ end____ width___ exp.time_
  3 omega  -52.00   15.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -       15.4892  -57.0000   30.0000 67

#__ type_ start__ end____ width___ exp.time_
  4 omega  -82.00   -5.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -57.0000 -120.0000 77

#__ type_ start__ end____ width___ exp.time_
  5 omega  -86.00  -51.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  151.0000  -49.2221 35

#__ type_ start__ end____ width___ exp.time_
  6 omega  -47.00    8.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -77.0000  150.0000 55

#__ type_ start__ end____ width___ exp.time_
  7 omega   34.00   88.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -       15.4892  179.0000  -60.0000 54

#__ type_ start__ end____ width___ exp.time_
  8 omega  -33.00   51.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704   57.0000  150.0000 84

#__ type_ start__ end____ width___ exp.time_
  9 omega  -85.00    3.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -38.0000   60.0000 88

#__ type_ start__ end____ width___ exp.time_
 10 omega  -84.00  -59.00   1.0000   46.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -57.0000    0.0000 25

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            15468
_reflns_number_total             5259
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_unetI/netI     0.0422
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 5259
# Theoretical number of reflections is about 12102


_diffrn_reflns_theta_min         2.163
_diffrn_reflns_theta_max         29.386
_diffrn_measured_fraction_theta_max 0.869

_diffrn_reflns_theta_full        26.370
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              -12
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              20

_oxford_diffrn_Wilson_B_factor   1.72
_oxford_diffrn_Wilson_scale      0.42

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

_refine_diff_density_min         -0.49
_refine_diff_density_max         0.50


# 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>2.0\s(I)
_refine_ls_number_reflns         4495
_refine_ls_number_restraints     106
_refine_ls_number_parameters     289
_oxford_refine_ls_R_factor_ref   0.0437
_refine_ls_wR_factor_ref         0.0483
_refine_ls_goodness_of_fit_ref   1.0944
_refine_ls_shift/su_max          0.0014653
_refine_ls_shift/su_mean         0.0000751


# The values computed with all filters except I/sigma
_oxford_reflns_number_all        5259
_refine_ls_R_factor_all          0.0529
_refine_ls_wR_factor_all         0.0532

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4495
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_gt          0.0483

# 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 F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #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: 
 9.17 2.69 7.17 1.57 
;

# 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
S1 S 0.61657(5) 0.65860(4) 0.82010(3) 0.0170 1.0000 Uani . . . . . .
O2 O 0.70559(19) 0.68183(13) 0.72515(9) 0.0294 1.0000 Uani . . . . . .
O3 O 0.71402(18) 0.56851(12) 0.88554(9) 0.0270 1.0000 Uani . . . . . .
O4 O 0.44326(17) 0.61495(15) 0.82546(11) 0.0355 1.0000 Uani . . . . . .
C5 C 0.59868(19) 0.83031(15) 0.84706(10) 0.0155 1.0000 Uani . . . . . .
C6 C 0.53428(19) 0.84914(15) 0.93648(10) 0.0146 1.0000 Uani . . . . . .
C7 C 0.53112(18) 0.98824(15) 0.95456(10) 0.0135 1.0000 Uani . . . . . .
C8 C 0.58954(19) 1.10548(15) 0.88256(10) 0.0146 1.0000 Uani . . . . . .
C9 C 0.6432(2) 1.08060(15) 0.79319(10) 0.0157 1.0000 Uani . . . . . .
C10 C 0.6490(2) 0.94477(16) 0.77668(10) 0.0170 1.0000 Uani . . . . . .
S11 S 0.70350(5) 1.22094(4) 0.69666(3) 0.0190 1.0000 Uani . . . . . .
O12 O 0.55669(18) 1.32014(14) 0.68737(9) 0.0298 1.0000 Uani . . . . . .
O13 O 0.74462(19) 1.15592(13) 0.61715(8) 0.0289 1.0000 Uani . . . . . .
O14 O 0.84941(18) 1.28476(15) 0.71869(9) 0.0322 1.0000 Uani . . . . . .
C15 C 0.5908(2) 1.24265(15) 0.90450(10) 0.0177 1.0000 Uani . . . . . .
C16 C 0.5314(2) 1.26417(15) 0.99010(11) 0.0168 1.0000 Uani . . . . . .
O17 O 1.00158(17) 0.53761(14) 0.67319(10) 0.0300 1.0000 Uani . . . . . .
O18 O 0.26496(19) 0.61281(16) 1.53130(9) 0.0355 1.0000 Uani . . . . . .
N19 N 0.2555(2) 0.41369(16) 0.78547(11) 0.0257 1.0000 Uani . . . . . .
C20 C 0.1703(2) 0.29025(18) 0.85046(12) 0.0242 1.0000 Uani . . . . . .
C21 C 0.0780(2) 0.33155(18) 0.93709(12) 0.0250 1.0000 Uani . . . . . .
C22 C 0.0103(2) 0.19935(19) 1.00535(13) 0.0268 1.0000 Uani . . . . . .
C23 C -0.0611(2) 0.2264(2) 1.10009(13) 0.0286 1.0000 Uani . . . . . .
C24 C -0.1162(2) 0.0903(2) 1.16821(14) 0.0298 1.0000 Uani . . . . . .
C25 C -0.1466(3) 0.1039(2) 1.26828(14) 0.0323 1.0000 Uani . U . . . .
C26 C -0.2098(3) -0.0319(2) 1.33370(14) 0.0370 1.0000 Uani . U . . . .
N30 N -0.3914(2) -0.38524(17) 1.56764(11) 0.0307 1.0000 Uani . U . . . .
C280 C -0.3371(5) -0.1355(4) 1.5005(2) 0.0286 0.5000 Uani . U . . 1 .
C281 C -0.1939(6) -0.1904(5) 1.4958(3) 0.0408 0.5000 Uani . U . . 2 .
C290 C -0.3727(6) -0.2335(5) 1.5067(3) 0.0400 0.5000 Uani . U . . 2 .
C291 C -0.2803(5) -0.2859(4) 1.4949(2) 0.0235 0.5000 Uani . U . . 1 .
C271 C -0.2019(4) -0.0316(3) 1.43422(16) 0.0550 1.0000 Uani . U . . . .
H1 H 0.6872 0.9311 0.7176 0.0204 1.0000 Uiso . . . . . .
H2 H 0.6343 1.3182 0.8587 0.0227 1.0000 Uiso . . . . . .
H3 H 0.0903 0.2533 0.8183 0.0295 1.0000 Uiso . . . . . .
H4 H 0.5323 1.3538 1.0019 0.0207 1.0000 Uiso . . . . . .
H5 H -0.0785 0.1605 0.9789 0.0333 1.0000 Uiso . . . . . .
H6 H 0.3366 0.3826 0.7448 0.0396 1.0000 Uiso . . . . . .
H7 H -0.2216 0.0584 1.1525 0.0365 1.0000 Uiso . . . . . .
H8 H -0.1604 0.2930 1.0946 0.0350 1.0000 Uiso . . . . . .
H9 H 0.0263 0.2691 1.1240 0.0349 1.0000 Uiso . . . . . .
H10 H -0.0146 0.3968 0.9212 0.0311 1.0000 Uiso . . . . . .
H11 H 0.1051 0.1280 1.0124 0.0324 1.0000 Uiso . . . . . .
H12 H 0.2584 0.2164 0.8681 0.0299 1.0000 Uiso . . . . . .
H13 H 0.1796 0.4691 0.7538 0.0400 1.0000 Uiso . . . . . .
H15 H 0.3059 0.4658 0.8161 0.0401 1.0000 Uiso . . . . . .
H16 H -0.0398 0.1284 1.2867 0.0398 1.0000 Uiso . . . . . .
H17 H 0.9282 0.5906 0.6936 0.0462 1.0000 Uiso . . . . . .
H18 H 0.9499 0.4636 0.6813 0.0461 1.0000 Uiso . . . . . .
H19 H 0.1577 0.3767 0.9652 0.0312 1.0000 Uiso . . . . . .
H20 H 0.2473 0.6870 1.4941 0.0543 1.0000 Uiso . . . . . .
H21 H -0.2270 0.1814 1.2763 0.0399 1.0000 Uiso . . . . . .
H23 H -0.0259 0.0162 1.1622 0.0370 1.0000 Uiso . . . . . .
H24 H -0.1387 -0.1118 1.3180 0.0452 1.0000 Uiso . . . . . .
H25 H 0.1811 0.6019 1.5700 0.0536 1.0000 Uiso . . . . . .
H26 H -0.3276 -0.0443 1.3240 0.0457 1.0000 Uiso . . . . . .
H2801 H -0.3453 -0.1236 1.5631 0.0288 0.5000 Uiso . . . . 1 .
H2802 H -0.4492 -0.1151 1.4811 0.0288 0.5000 Uiso . . . . 1 .
H2811 H -0.1578 -0.1940 1.5548 0.0662 0.5000 Uiso . . . . 2 .
H2812 H -0.1180 -0.2528 1.4649 0.0662 0.5000 Uiso . . . . 2 .
H2911 H -0.1605 -0.3030 1.5054 0.0253 0.5000 Uiso . . . . 1 .
H2912 H -0.2860 -0.3033 1.4343 0.0253 0.5000 Uiso . . . . 1 .
H2901 H -0.4416 -0.1666 1.5339 0.0675 0.5000 Uiso . . . . 2 .
H2902 H -0.4001 -0.2307 1.4462 0.0675 0.5000 Uiso . . . . 2 .
H2711 H -0.2268 0.0620 1.4440 0.0668 0.5000 Uiso . . . . 1 .
H2712 H -0.0904 -0.0618 1.4488 0.0668 0.5000 Uiso . . . . 1 .
H2713 H -0.3015 0.0171 1.4575 0.0668 0.5000 Uiso . . . . 2 .
H2714 H -0.1031 0.0159 1.4386 0.0668 0.5000 Uiso . . . . 2 .
H301 H -0.5068 -0.4119 1.5741 0.0369 0.5000 Uiso . . . . 2 .
H302 H -0.3600 -0.3866 1.6270 0.0369 0.5000 Uiso . . . . 2 .
H303 H -0.3187 -0.4499 1.5390 0.0369 0.5000 Uiso . . . . 2 .
H304 H -0.3571 -0.4805 1.5650 0.0369 0.5000 Uiso . . . . 1 .
H305 H -0.3799 -0.3693 1.6270 0.0369 0.5000 Uiso . . . . 1 .
H306 H -0.5074 -0.3685 1.5568 0.0369 0.5000 Uiso . . . . 1 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.558(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
S1 . O2 . 1.4658(13) yes
S1 . O3 . 1.4330(13) yes
S1 . O4 . 1.4446(14) yes
S1 . C5 . 1.7823(14) yes
C5 . C6 . 1.404(2) yes
C5 . C10 . 1.382(2) yes
C6 . C16 2_677 1.433(2) yes
C6 . C7 . 1.4247(19) yes
C7 . C7 2_677 1.436(3) yes
C7 . C8 . 1.429(2) yes
C8 . C9 . 1.407(2) yes
C8 . C15 . 1.4333(19) yes
C9 . C10 . 1.383(2) yes
C9 . S11 . 1.7804(15) yes
C10 . H1 . 0.926 no
S11 . O12 . 1.4564(14) yes
S11 . O13 . 1.4480(12) yes
S11 . O14 . 1.4509(13) yes
C15 . C16 . 1.352(2) yes
C15 . H2 . 0.930 no
C16 . H4 . 0.921 no
O17 . H17 . 0.819 no
O17 . H18 . 0.823 no
O18 . H20 . 0.822 no
O18 . H25 . 0.810 no
N19 . C20 . 1.492(2) yes
N19 . H6 . 0.901 no
N19 . H13 . 0.893 no
N19 . H15 . 0.893 no
C20 . C21 . 1.510(2) yes
C20 . H3 . 0.973 no
C20 . H12 . 0.982 no
C21 . C22 . 1.522(2) yes
C21 . H10 . 0.954 no
C21 . H19 . 0.976 no
C22 . C23 . 1.516(3) yes
C22 . H5 . 0.983 no
C22 . H11 . 0.985 no
C23 . C24 . 1.521(3) yes
C23 . H8 . 0.982 no
C23 . H9 . 0.973 no
C24 . C25 . 1.511(3) yes
C24 . H7 . 0.981 no
C24 . H23 . 0.986 no
C25 . C26 . 1.519(3) yes
C25 . H16 . 0.981 no
C25 . H21 . 0.966 no
C26 . C271 . 1.510(3) yes
C26 . H24 . 0.975 no
C26 . H26 . 0.980 no
N30 . C291 . 1.500(4) yes
N30 . H304 . 0.949 no
N30 . H305 . 0.950 no
N30 . H306 . 0.950 no
C280 . C291 . 1.507(5) yes
C280 . C271 . 1.591(5) yes
C280 . H2801 . 0.958 no
C280 . H2802 . 0.965 no
C281 . C290 . 1.475(6) yes
C281 . C271 . 1.608(5) yes
C281 . H2811 . 0.955 no
C281 . H2812 . 0.964 no
C290 . H2901 . 0.940 no
C290 . H2902 . 0.952 no
C291 . H2911 . 0.978 no
C291 . H2912 . 0.963 no
C271 . H2711 . 0.949 no
C271 . H2712 . 0.948 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
O2 . S1 . O3 . 112.51(8) yes
O2 . S1 . O4 . 111.94(9) yes
O3 . S1 . O4 . 113.87(9) yes
O2 . S1 . C5 . 104.40(7) yes
O3 . S1 . C5 . 107.38(7) yes
O4 . S1 . C5 . 105.94(7) yes
S1 . C5 . C6 . 121.25(11) yes
S1 . C5 . C10 . 117.73(11) yes
C6 . C5 . C10 . 121.02(13) yes
C16 2_677 C6 . C5 . 123.20(13) yes
C16 2_677 C6 . C7 . 118.41(13) yes
C5 . C6 . C7 . 118.38(13) yes
C7 2_677 C7 . C6 . 120.18(17) yes
C7 2_677 C7 . C8 . 119.42(16) yes
C6 . C7 . C8 . 120.40(13) yes
C7 . C8 . C9 . 118.27(13) yes
C7 . C8 . C15 . 118.67(13) yes
C9 . C8 . C15 . 123.07(14) yes
C8 . C9 . C10 . 120.87(14) yes
C8 . C9 . S11 . 122.01(11) yes
C10 . C9 . S11 . 117.11(11) yes
C9 . C10 . C5 . 120.89(14) yes
C9 . C10 . H1 . 119.1 no
C5 . C10 . H1 . 120.0 no
C9 . S11 . O12 . 106.93(7) yes
C9 . S11 . O13 . 106.21(7) yes
O12 . S11 . O13 . 111.90(8) yes
C9 . S11 . O14 . 106.25(8) yes
O12 . S11 . O14 . 111.99(9) yes
O13 . S11 . O14 . 113.02(9) yes
C8 . C15 . C16 . 121.56(14) yes
C8 . C15 . H2 . 119.0 no
C16 . C15 . H2 . 119.5 no
C6 2_677 C16 . C15 . 121.68(13) yes
C6 2_677 C16 . H4 . 118.7 no
C15 . C16 . H4 . 119.6 no
H17 . O17 . H18 . 102.0 no
H20 . O18 . H25 . 106.5 no
C20 . N19 . H6 . 109.9 no
C20 . N19 . H13 . 110.6 no
H6 . N19 . H13 . 108.5 no
C20 . N19 . H15 . 111.1 no
H6 . N19 . H15 . 108.0 no
H13 . N19 . H15 . 108.7 no
N19 . C20 . C21 . 111.62(14) yes
N19 . C20 . H3 . 108.4 no
C21 . C20 . H3 . 110.3 no
N19 . C20 . H12 . 108.4 no
C21 . C20 . H12 . 108.8 no
H3 . C20 . H12 . 109.2 no
C20 . C21 . C22 . 109.50(15) yes
C20 . C21 . H10 . 109.4 no
C22 . C21 . H10 . 110.0 no
C20 . C21 . H19 . 109.2 no
C22 . C21 . H19 . 109.4 no
H10 . C21 . H19 . 109.3 no
C21 . C22 . C23 . 113.45(15) yes
C21 . C22 . H5 . 108.7 no
C23 . C22 . H5 . 109.9 no
C21 . C22 . H11 . 108.0 no
C23 . C22 . H11 . 108.7 no
H5 . C22 . H11 . 107.9 no
C22 . C23 . C24 . 111.93(16) yes
C22 . C23 . H8 . 109.6 no
C24 . C23 . H8 . 108.7 no
C22 . C23 . H9 . 108.9 no
C24 . C23 . H9 . 109.2 no
H8 . C23 . H9 . 108.5 no
C23 . C24 . C25 . 114.08(16) yes
C23 . C24 . H7 . 109.7 no
C25 . C24 . H7 . 108.4 no
C23 . C24 . H23 . 108.4 no
C25 . C24 . H23 . 108.2 no
H7 . C24 . H23 . 107.9 no
C24 . C25 . C26 . 112.55(17) yes
C24 . C25 . H16 . 109.6 no
C26 . C25 . H16 . 108.6 no
C24 . C25 . H21 . 110.9 no
C26 . C25 . H21 . 109.4 no
H16 . C25 . H21 . 105.4 no
C25 . C26 . C271 . 112.93(17) yes
C25 . C26 . H24 . 108.7 no
C271 . C26 . H24 . 108.2 no
C25 . C26 . H26 . 108.1 no
C271 . C26 . H26 . 110.3 no
H24 . C26 . H26 . 108.5 no
C291 . N30 . H304 . 109.4 no
C291 . N30 . H305 . 109.4 no
H304 . N30 . H305 . 109.6 no
C291 . N30 . H306 . 109.4 no
H304 . N30 . H306 . 109.5 no
H305 . N30 . H306 . 109.5 no
C291 . C280 . C271 . 108.2(3) yes
C291 . C280 . H2801 . 110.5 no
C271 . C280 . H2801 . 110.8 no
C291 . C280 . H2802 . 109.6 no
C271 . C280 . H2802 . 110.2 no
H2801 . C280 . H2802 . 107.6 no
C290 . C281 . C271 . 102.6(3) yes
C290 . C281 . H2811 . 110.8 no
C271 . C281 . H2811 . 112.7 no
C290 . C281 . H2812 . 110.7 no
C271 . C281 . H2812 . 112.1 no
H2811 . C281 . H2812 . 107.9 no
N30 . C290 . C281 . 110.1(3) yes
N30 . C290 . H2901 . 111.5 no
C281 . C290 . H2901 . 107.3 no
N30 . C290 . H2902 . 110.6 no
C281 . C290 . H2902 . 107.0 no
H2901 . C290 . H2902 . 110.1 no
C280 . C291 . N30 . 108.4(3) yes
C280 . C291 . H2911 . 110.2 no
N30 . C291 . H2911 . 109.8 no
C280 . C291 . H2912 . 111.5 no
N30 . C291 . H2912 . 110.7 no
H2911 . C291 . H2912 . 106.1 no
C26 . C271 . C280 . 111.0(2) yes
C26 . C271 . H2711 . 109.1 no
C280 . C271 . H2711 . 108.9 no
C26 . C271 . H2712 . 109.2 no
C280 . C271 . H2712 . 109.0 no
H2711 . C271 . H2712 . 109.7 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
C15 . H2 . O14 . 122.96(10) 0.930 2.563 3.166(3) yes
C20 . H3 . O14 1_445 152.19(11) 0.973 2.539 3.430(3) yes
N19 . H6 . O12 1_545 161.56(11) 0.901 1.945 2.814(3) yes
C23 . H8 . O4 2_567 147.29(12) 0.982 2.578 3.445(3) yes
N19 . H13 . O17 1_455 162.79(10) 0.893 1.966 2.831(3) yes
N19 . H15 . O4 . 154.49(11) 0.893 1.900 2.733(3) yes
O17 . H17 . O2 . 161.27(10) 0.819 1.957 2.744(3) yes
O17 . H18 . O14 1_545 170.13(11) 0.823 1.886 2.700(3) yes
O18 . H20 . O13 2_677 164.41(10) 0.822 1.984 2.784(3) yes
O18 . H25 . O17 1_456 168.09(11) 0.810 1.960 2.758(3) yes
N30 . H301 . O18 1_445 150.45(11) 0.949 1.979 2.844(3) yes
N30 . H302 . O2 1_446 159.04(10) 0.950 1.880 2.788(3) yes
N30 . H303 . O18 2_558 154.98(11) 0.950 2.065 2.953(3) yes
N30 . H304 . O12 1_436 123.01(10) 0.949 2.404 3.027(3) yes
N30 . H304 . O18 2_558 141.90(10) 0.949 2.147 2.953(3) yes
N30 . H305 . O2 1_446 162.80(11) 0.950 1.866 2.788(3) yes
N30 . H306 . O18 1_445 164.41(11) 0.950 1.917 2.844(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 10/06/14 at 14:06:19
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 10/06/14 at 14:06:19
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(26) TO C(271) 
VIBR .0, 0.00500 = C(271) TO C(25) 
VIBR .0, 0.00200 = N(30) TO C(290) 
VIBR .0, 0.00200 = N(30) TO C(291) 
VIBR .0, 0.00500 = C(291) TO C(290) 
VIBR .0, 0.00200 = C(280) TO C(281) 
VIBR .0, 0.00200 = C(280) TO C(290) 
VIBR .0, 0.00200 = C(280) TO C(291) 
VIBR .0, 0.00200 = C(280) TO C(271) 
VIBR .0, 0.00500 = C(290) TO C(281) 
VIBR .0, 0.00500 = C(291) TO C(281)
VIBR .0, 0.00500 = C(291) TO C(290) 
VIBR .0, 0.00500 = C(271) TO C(281) 
VIBR .0, 0.00500 = C(271) TO C(290) 
VIBR .0, 0.00500 = C(271) TO C(291) 
VIBR .0, 0.00200 = C(281) TO C(290) 
VIBR .0, 0.00200 = C(281) TO C(291) 
VIBR .0, 0.00200 = C(281) TO C(271) 
VIBR .0, 0.00500 = C(290) TO C(280) 
VIBR .0, 0.00500 = C(291) TO C(280) 
VIBR .0, 0.00500 = C(291) TO C(290) 
VIBR .0, 0.00500 = C(271) TO C(280) 
VIBR .0, 0.00500 = C(271) TO C(290) 
VIBR .0, 0.00500 = C(271) TO C(291) 
VIBR .0, 0.00200 = C(290) TO C(291) 
VIBR .0, 0.00500 = C(281) TO N(30)
VIBR .0, 0.00500 = C(280) TO N(30) 
VIBR .0, 0.00500 = C(280) TO C(281) 
VIBR .0, 0.00500 = C(291) TO N(30) 
VIBR .0, 0.00500 = C(291) TO C(281) 
VIBR .0, 0.00500 = C(291) TO C(280) 
VIBR .0, 0.00500 = C(280) TO N(30) 
VIBR .0, 0.00500 = C(281) TO N(30) 
VIBR .0, 0.00500 = C(281) TO C(280) 
VIBR .0, 0.00500 = C(290) TO N(30) 
VIBR .0, 0.00500 = C(290) TO C(280) 
VIBR .0, 0.00500 = C(290) TO C(281) 
VIBR .0, 0.00500 = C(280) TO C(26) 
VIBR .0, 0.00500 = C(281) TO C(26) 
VIBR .0, 0.00500 = C(281) TO C(280) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(26) TO C(271) 
U(IJ) .0, 0.04000 = N(30) TO C(290) 
U(IJ) .0, 0.04000 = N(30) TO C(291) 
U(IJ) .0, 0.04000 = C(280) TO C(281) 
U(IJ) .0, 0.04000 = C(280) TO C(290) 
U(IJ) .0, 0.04000 = C(280) TO C(291) 
U(IJ) .0, 0.04000 = C(280) TO C(271) 
U(IJ) .0, 0.04000 = C(281) TO C(290) 
U(IJ) .0, 0.04000 = C(281) TO C(291) 
U(IJ) .0, 0.04000 = C(281) TO C(271) 
U(IJ) .0, 0.04000 = C(290) TO C(291) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_database_code_depnum_ccdc_archive 'CCDC 986088'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_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                   9.7336(8)
_cell_length_b                   9.7556(8)
_cell_length_c                   10.1940(7)
_cell_angle_alpha                95.207(6)
_cell_angle_beta                 95.926(6)
_cell_angle_gamma                95.224(7)
_cell_volume                     953.91(13)
_cell_measurement_reflns_used    6774
_cell_measurement_theta_min      2.1090
_cell_measurement_theta_max      32.3830
_cell_oxdiff_length_a            9.7662(4)
_cell_oxdiff_length_b            9.7818(5)
_cell_oxdiff_length_c            10.2045(5)
_cell_oxdiff_angle_alpha         95.342(4)
_cell_oxdiff_angle_beta          95.497(4)
_cell_oxdiff_angle_gamma         95.663(4)
_cell_oxdiff_volume              960.43(8)

_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 0.0033 0.0016 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 0.0106 0.0060 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'
N 0.0061 0.0033 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'
S 0.1246 0.1234 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            1

_chemical_formula_sum            'C28 H48 N8 O14 S4'
_chemical_formula_moiety         
'C16 H6 O12 S4, C10 H26 N2, 2(C H6 N3), 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         849.02


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.300
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_max          0.600
_exptl_absorpt_correction_T_min  0.98990
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             448
_exptl_absorpt_coefficient_mu    0.324
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 16.0143

_diffrn_measurement_device       Area
_diffrn_radiation_wavelength     0.71073
#montpellier_reflns_maxres is minimum d (highest resolution)
#where <I/sigI> <= 2.0
#(Z. Dauter, Acta Cryst. D55, 1703-1717, 1999)
_montpellier_reflns_maxres       0.66
_montpellier_reflns_completeness_maxres 93.05
_montpellier_reflns_redundancy_maxres 3.50

#montpellier_diffrn_reflns_class_completeness_shell is completeness in shell
#montpellier_diffrn_class_reflns_cumul_completeness is cumulative
#completeness to resolution of shell
#Note: completeness percentage takes into account the fact whether
#group is centrosymmetric or not
loop_
_montpellier_diffrn_reflns_class_number
_montpellier_diffrn_reflns_class_d_res_high
_montpellier_diffrn_reflns_class_d_res_low
_montpellier_diffrn_reflns_class_redundancy
_montpellier_diffrn_reflns_class_av_I/uI
_diffrn_reflns_class_av_R_eq
_montpellier_diffrn_reflns_class_completeness_shell
_montpellier_diffrn_reflns_class_cumul_completeness
0 100.0 1.46 5.2 73.81 0.022 100.0 100.00
1 1.46 1.16 4.8 42.60 0.025 100.0 100.00
2 1.16 1.01 4.3 28.07 0.033 100.0 100.00
3 1.01 0.92 3.9 19.32 0.048 100.0 100.00
4 0.92 0.85 3.5 13.81 0.064 100.0 100.00
5 0.85 0.80 3.2 10.91 0.073 100.0 100.00
6 0.80 0.76 3.0 8.77 0.092 100.0 100.00
7 0.76 0.73 2.8 8.20 0.096 99.7 99.96
8 0.73 0.70 2.6 6.11 0.130 99.7 99.93
9 0.70 0.66 1.6 4.55 0.138 57.6 93.05
#End reflection statistics
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_orient_matrix_UB_11      -0.0164071000
_diffrn_orient_matrix_UB_12      0.0404693000
_diffrn_orient_matrix_UB_13      0.0565565000
_diffrn_orient_matrix_UB_21      0.0073328000
_diffrn_orient_matrix_UB_22      0.0600098000
_diffrn_orient_matrix_UB_23      -0.0338628000
_diffrn_orient_matrix_UB_31      -0.0711515000
_diffrn_orient_matrix_UB_32      -0.0113477000
_diffrn_orient_matrix_UB_33      -0.0241764000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -24.00   67.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732 -100.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
  2 omega   35.00   92.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732  179.0000  150.0000 57

#__ type_ start__ end____ width___ exp.time_
  3 omega    4.00   99.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   38.0000  -60.0000 95

#__ type_ start__ end____ width___ exp.time_
  4 omega   -4.00   96.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   77.0000   90.0000 100

#__ type_ start__ end____ width___ exp.time_
  5 omega    5.00   95.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   57.0000 -150.0000 90

#__ type_ start__ end____ width___ exp.time_
  6 omega    5.00   95.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   57.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
  7 omega   34.00  102.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732  179.0000   90.0000 68

#__ type_ start__ end____ width___ exp.time_
  8 omega   34.00  102.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732  179.0000  -30.0000 68

#__ type_ start__ end____ width___ exp.time_
  9 omega -103.00  -56.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -      -26.9544 -179.0000 -180.0000 47

#__ type_ start__ end____ width___ exp.time_
 10 omega  -24.00   69.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732 -100.0000  -30.0000 93

#__ type_ start__ end____ width___ exp.time_
 11 omega    0.00   95.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -       26.1732   71.0000  -72.0000 95

#__ type_ start__ end____ width___ exp.time_
 12 omega  -52.00  -27.00   1.0000   26.0500
omega____ theta____ kappa____ phi______ frames
    -      -26.9544   38.0000 -120.0000 25

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            36619
_reflns_number_total             6564
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0408
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6564
# Theoretical number of reflections is about 13798


_diffrn_reflns_theta_min         2.019
_diffrn_reflns_theta_max         32.489
_diffrn_measured_fraction_theta_max 0.951

_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              -14
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              15

_oxford_diffrn_Wilson_B_factor   1.57
_oxford_diffrn_Wilson_scale      0.32

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

_refine_diff_density_min         -0.48
_refine_diff_density_max         0.52


# 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>2.0\s(I)
_refine_ls_number_reflns         5743
_refine_ls_number_restraints     0
_refine_ls_number_parameters     244
_oxford_refine_ls_R_factor_ref   0.0353
_refine_ls_wR_factor_ref         0.0299
_refine_ls_goodness_of_fit_ref   0.9998
_refine_ls_shift/su_max          0.0008218
_refine_ls_shift/su_mean         0.0000709


# The values computed with all filters except I/sigma
_oxford_reflns_number_all        6564
_refine_ls_R_factor_all          0.0426
_refine_ls_wR_factor_all         0.0343

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5743
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_gt          0.0299

# 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 F
_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: 
 0.584 -10.0 -3.38 -3.86 -2.49 
;

# 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
S1 S 0.79397(2) 0.90507(2) 0.87820(2) 0.0148 1.0000 Uani . . . . . .
O2 O 0.91031(8) 0.83841(8) 0.93641(8) 0.0225 1.0000 Uani . . . . . .
O3 O 0.73968(9) 1.00104(8) 0.97245(8) 0.0245 1.0000 Uani . . . . . .
O4 O 0.68497(8) 0.80420(8) 0.80787(8) 0.0222 1.0000 Uani . . . . . .
C5 C 0.85951(9) 1.00512(9) 0.75711(9) 0.0139 1.0000 Uani . . . . . .
C6 C 0.91634(9) 0.94308(9) 0.64760(9) 0.0135 1.0000 Uani . . . . . .
C7 C 0.96949(9) 1.03002(9) 0.55543(8) 0.0127 1.0000 Uani . . . . . .
C8 C 0.96153(9) 1.17580(9) 0.57295(9) 0.0135 1.0000 Uani . . . . . .
C9 C 0.89711(10) 1.23062(9) 0.68077(9) 0.0141 1.0000 Uani . . . . . .
C10 C 0.84840(10) 1.14639(9) 0.77198(9) 0.0153 1.0000 Uani . . . . . .
S11 S 0.87213(3) 1.40951(2) 0.70495(2) 0.0157 1.0000 Uani . . . . . .
O12 O 1.01142(9) 1.48341(8) 0.73821(9) 0.0247 1.0000 Uani . . . . . .
O13 O 0.80357(9) 1.44644(8) 0.58217(8) 0.0225 1.0000 Uani . . . . . .
O14 O 0.78832(10) 1.42143(8) 0.81460(9) 0.0287 1.0000 Uani . . . . . .
C15 C 1.02137(10) 1.26015(9) 0.48141(9) 0.0156 1.0000 Uani . . . . . .
C16 C 1.07956(10) 1.20359(9) 0.37672(9) 0.0155 1.0000 Uani . . . . . .
O17 O 0.56147(12) 0.61119(14) 0.60030(14) 0.0566 1.0000 Uani . . . . . .
N18 N 0.40217(10) 0.82072(12) 0.85804(11) 0.0308 1.0000 Uani . . . . . .
C19 C 0.29177(11) 0.73939(11) 0.80072(10) 0.0210 1.0000 Uani . . . . . .
N20 N 0.16971(10) 0.75142(11) 0.84542(11) 0.0282 1.0000 Uani . . . . . .
N21 N 0.30330(12) 0.64260(12) 0.70288(11) 0.0319 1.0000 Uani . . . . . .
N22 N 0.81083(10) 0.59877(10) 1.04586(9) 0.0230 1.0000 Uani . . . . . .
C23 C 0.67686(12) 0.63473(12) 1.09315(11) 0.0240 1.0000 Uani . . . . . .
C24 C 0.70634(12) 0.74103(13) 1.21349(11) 0.0262 1.0000 Uani . . . . . .
C25 C 0.57525(13) 0.79231(15) 1.26142(13) 0.0312 1.0000 Uani . . . . . .
C26 C 0.60936(13) 0.89535(15) 1.38490(12) 0.0309 1.0000 Uani . . . . . .
C27 C 0.48202(13) 0.94936(15) 1.43773(13) 0.0326 1.0000 Uani . . . . . .
H1 H 0.8566 0.6747 1.0201 0.0350 1.0000 Uiso R . . . . .
H2 H 1.1186 1.2614 0.3190 0.0189 1.0000 Uiso R . . . . .
H3 H 0.8071 1.1857 0.8422 0.0192 1.0000 Uiso R . . . . .
H4 H 0.4298 0.9958 1.3689 0.0389 1.0000 Uiso R . . . . .
H5 H 0.8669 0.5689 1.1126 0.0346 1.0000 Uiso R . . . . .
H6 H 0.4848 0.8168 0.8323 0.0374 1.0000 Uiso R . . . . .
H7 H 0.3939 0.8828 0.9209 0.0371 1.0000 Uiso R . . . . .
H8 H 0.0986 0.6994 0.8085 0.0339 1.0000 Uiso R . . . . .
H9 H 0.6596 0.8504 1.4546 0.0370 1.0000 Uiso R . . . . .
H11 H 0.7658 0.8200 1.1913 0.0322 1.0000 Uiso R . . . . .
H12 H 0.7582 0.6995 1.2843 0.0321 1.0000 Uiso R . . . . .
H13 H 0.1575 0.8229 0.8944 0.0340 1.0000 Uiso R . . . . .
H14 H 1.0208 1.3563 0.4939 0.0187 1.0000 Uiso R . . . . .
H15 H 0.2283 0.6042 0.6554 0.0387 1.0000 Uiso R . . . . .
H17 H 0.6726 0.9732 1.3653 0.0378 1.0000 Uiso R . . . . .
H19 H 0.4192 0.8722 1.4572 0.0392 1.0000 Uiso R . . . . .
H20 H 0.5137 0.7146 1.2808 0.0380 1.0000 Uiso R . . . . .
H21 H 0.5810 0.5318 0.6206 0.0901 1.0000 Uiso R . . . . .
H22 H 0.5242 0.8368 1.1909 0.0380 1.0000 Uiso R . . . . .
H26 H 0.3805 0.6364 0.6729 0.0385 1.0000 Uiso R . . . . .
H10 H 0.7996 0.5341 0.9790 0.0358 1.0000 Uiso R . . . . .
H16 H 0.6217 0.6705 1.0202 0.0285 1.0000 Uiso R . . . . .
H18 H 0.6251 0.5510 1.1143 0.0297 1.0000 Uiso R . . . . .
H24 H 0.6213 0.6635 0.6553 0.0897 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          5.076(4)
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
S1 . O2 . 1.4570(8) yes
S1 . O3 . 1.4528(8) yes
S1 . O4 . 1.4604(8) yes
S1 . C5 . 1.7752(9) yes
C5 . C6 . 1.4086(12) yes
C5 . C10 . 1.3880(12) yes
C6 . C16 2_776 1.4348(12) yes
C6 . C7 . 1.4266(12) yes
C7 . C7 2_776 1.4334(16) yes
C7 . C8 . 1.4273(12) yes
C8 . C9 . 1.4085(12) yes
C8 . C15 . 1.4324(12) yes
C9 . C10 . 1.3869(12) yes
C9 . S11 . 1.7825(9) yes
C10 . H3 . 0.927 no
S11 . O12 . 1.4682(8) yes
S11 . O13 . 1.4473(8) yes
S11 . O14 . 1.4527(8) yes
C15 . C16 . 1.3561(12) yes
C15 . H14 . 0.936 no
C16 . H2 . 0.936 no
O17 . H21 . 0.852 no
O17 . H24 . 0.860 no
N18 . C19 . 1.3254(14) yes
N18 . H6 . 0.874 no
N18 . H7 . 0.856 no
C19 . N20 . 1.3268(14) yes
C19 . N21 . 1.3306(14) yes
N20 . H8 . 0.853 no
N20 . H13 . 0.845 no
N21 . H15 . 0.867 no
N21 . H26 . 0.845 no
N22 . C23 . 1.4961(14) yes
N22 . H1 . 0.903 no
N22 . H5 . 0.913 no
N22 . H10 . 0.877 no
C23 . C24 . 1.5181(16) yes
C23 . H16 . 0.981 no
C23 . H18 . 0.973 no
C24 . C25 . 1.5224(16) yes
C24 . H11 . 0.979 no
C24 . H12 . 0.978 no
C25 . C26 . 1.5260(17) yes
C25 . H20 . 0.970 no
C25 . H22 . 0.987 no
C26 . C27 . 1.5196(17) yes
C26 . H9 . 0.980 no
C26 . H17 . 0.982 no
C27 . C27 2_678 1.526(2) yes
C27 . H4 . 0.991 no
C27 . H19 . 0.974 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
O2 . S1 . O3 . 113.34(5) yes
O2 . S1 . O4 . 111.76(5) yes
O3 . S1 . O4 . 111.96(5) yes
O2 . S1 . C5 . 106.34(4) yes
O3 . S1 . C5 . 106.39(4) yes
O4 . S1 . C5 . 106.48(5) yes
S1 . C5 . C6 . 121.36(7) yes
S1 . C5 . C10 . 117.45(7) yes
C6 . C5 . C10 . 121.16(8) yes
C16 2_776 C6 . C5 . 122.95(8) yes
C16 2_776 C6 . C7 . 118.65(8) yes
C5 . C6 . C7 . 118.38(8) yes
C7 2_776 C7 . C6 . 119.57(10) yes
C7 2_776 C7 . C8 . 120.12(10) yes
C6 . C7 . C8 . 120.31(8) yes
C7 . C8 . C9 . 118.53(8) yes
C7 . C8 . C15 . 118.57(8) yes
C9 . C8 . C15 . 122.89(8) yes
C8 . C9 . C10 . 121.03(8) yes
C8 . C9 . S11 . 121.87(7) yes
C10 . C9 . S11 . 117.10(7) yes
C5 . C10 . C9 . 120.47(8) yes
C5 . C10 . H3 . 120.5 no
C9 . C10 . H3 . 119.0 no
C9 . S11 . O12 . 105.90(5) yes
C9 . S11 . O13 . 107.42(4) yes
O12 . S11 . O13 . 112.14(5) yes
C9 . S11 . O14 . 105.18(5) yes
O12 . S11 . O14 . 112.28(5) yes
O13 . S11 . O14 . 113.27(5) yes
C8 . C15 . C16 . 121.34(8) yes
C8 . C15 . H14 . 119.6 no
C16 . C15 . H14 . 119.0 no
C6 2_776 C16 . C15 . 121.63(8) yes
C6 2_776 C16 . H2 . 119.0 no
C15 . C16 . H2 . 119.4 no
H21 . O17 . H24 . 100.1 no
C19 . N18 . H6 . 122.8 no
C19 . N18 . H7 . 120.2 no
H6 . N18 . H7 . 117.0 no
N18 . C19 . N20 . 119.31(10) yes
N18 . C19 . N21 . 120.73(10) yes
N20 . C19 . N21 . 119.90(10) yes
C19 . N20 . H8 . 119.4 no
C19 . N20 . H13 . 120.0 no
H8 . N20 . H13 . 118.5 no
C19 . N21 . H15 . 118.5 no
C19 . N21 . H26 . 119.9 no
H15 . N21 . H26 . 119.0 no
C23 . N22 . H1 . 109.7 no
C23 . N22 . H5 . 110.7 no
H1 . N22 . H5 . 107.3 no
C23 . N22 . H10 . 113.2 no
H1 . N22 . H10 . 108.0 no
H5 . N22 . H10 . 107.7 no
N22 . C23 . C24 . 109.59(9) yes
N22 . C23 . H16 . 108.2 no
C24 . C23 . H16 . 111.3 no
N22 . C23 . H18 . 109.1 no
C24 . C23 . H18 . 111.0 no
H16 . C23 . H18 . 107.5 no
C23 . C24 . C25 . 113.05(10) yes
C23 . C24 . H11 . 108.9 no
C25 . C24 . H11 . 109.0 no
C23 . C24 . H12 . 108.3 no
C25 . C24 . H12 . 110.0 no
H11 . C24 . H12 . 107.5 no
C24 . C25 . C26 . 111.29(10) yes
C24 . C25 . H20 . 109.8 no
C26 . C25 . H20 . 109.5 no
C24 . C25 . H22 . 110.1 no
C26 . C25 . H22 . 109.2 no
H20 . C25 . H22 . 106.7 no
C25 . C26 . C27 . 113.56(10) yes
C25 . C26 . H9 . 108.8 no
C27 . C26 . H9 . 108.7 no
C25 . C26 . H17 . 109.3 no
C27 . C26 . H17 . 109.7 no
H9 . C26 . H17 . 106.6 no
C27 2_678 C27 . C26 . 112.82(13) yes
C27 2_678 C27 . H4 . 108.8 no
C26 . C27 . H4 . 110.0 no
C27 2_678 C27 . H19 . 109.1 no
C26 . C27 . H19 . 109.7 no
H4 . C27 . H19 . 106.2 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
N22 . H1 . O2 . 165.26(4) 0.903 1.934 2.8165(15) yes
C16 . H2 . O4 2_776 122.09(3) 0.936 2.514 3.1138(15) yes
N22 . H5 . O12 2_777 176.33(3) 0.913 1.964 2.8754(15) yes
N18 . H6 . O4 . 169.58(4) 0.874 2.003 2.8672(15) yes
N18 . H7 . O3 2_677 147.87(4) 0.856 2.120 2.8811(15) yes
N20 . H8 . O12 1_445 145.67(3) 0.853 2.224 2.9672(15) yes
N20 . H13 . O3 2_677 144.98(3) 0.845 2.186 2.9184(15) yes
N21 . H15 . O12 1_445 127.40(3) 0.867 2.579 3.1816(15) yes
N21 . H15 . O13 2_676 126.35(4) 0.867 2.409 3.0055(15) yes
O17 . H21 . O13 1_545 121.61(4) 0.852 2.446 2.9827(15) yes
N21 . H26 . O17 . 177.05(5) 0.845 2.006 2.8508(15) yes
N22 . H10 . O14 1_545 168.87(4) 0.877 1.906 2.7717(15) yes
O17 . H24 . O4 . 155.95(4) 0.860 1.986 2.7941(15) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 18/12/13 at 11:37:47
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  10,X'S) H   (   3,X'S) 
RIDE C   (  15,X'S) H   (  14,X'S) 
RIDE C   (  16,X'S) H   (   2,X'S) 
RIDE O   (  17,X'S) H   (  21,X'S) H   (  24,X'S) 
RIDE N   (  18,X'S) H   (   6,X'S) H   (   7,X'S) 
RIDE N   (  20,X'S) H   (   8,X'S) H   (  13,X'S) 
RIDE N   (  21,X'S) H   (  15,X'S) H   (  26,X'S) 
RIDE N   (  22,X'S) H   (   1,X'S) H   (   5,X'S) H   (  10,X'S) 
RIDE C   (  23,X'S) H   (  16,X'S) H   (  18,X'S)
RIDE C   (  24,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (  25,X'S) H   (  20,X'S) H   (  22,X'S) 
RIDE C   (  26,X'S) H   (   9,X'S) H   (  17,X'S) 
RIDE C   (  27,X'S) H   (   4,X'S) H   (  19,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 18/12/13 at 11:37:47
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_database_code_depnum_ccdc_archive 'CCDC 986089'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_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                   9.8126(4)
_cell_length_b                   10.2605(4)
_cell_length_c                   19.4731(7)
_cell_angle_alpha                96.737(3)
_cell_angle_beta                 95.763(3)
_cell_angle_gamma                94.085(3)
_cell_volume                     1930.36(13)
_cell_measurement_reflns_used    5085
_cell_measurement_theta_min      2.0090
_cell_measurement_theta_max      28.6500
_cell_oxdiff_length_a            9.8099(4)
_cell_oxdiff_length_b            10.2612(4)
_cell_oxdiff_length_c            19.4704(7)
_cell_oxdiff_angle_alpha         96.760(3)
_cell_oxdiff_angle_beta          95.758(3)
_cell_oxdiff_angle_gamma         94.072(3)
_cell_oxdiff_volume              1929.65(13)

_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 0.0033 0.0016 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 0.0061 0.0033 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 0.0106 0.0060 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 0.1246 0.1234 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            2

_chemical_formula_sum            'C29 H50 N8 O14 S4'
_chemical_formula_moiety         
'C11 H28 N2, C16 H6 O12 S4, 2(C H6 N3), 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         863.05


_cell_measurement_temperature    125

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.300
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_max          0.700
_exptl_absorpt_correction_T_min  0.97948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    0.322
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 16.0143

_diffrn_measurement_device       Area
_diffrn_radiation_wavelength     0.71073
#montpellier_reflns_maxres is minimum d (highest resolution)
#where <I/sigI> <= 2.0
#(Z. Dauter, Acta Cryst. D55, 1703-1717, 1999)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 84.91
_montpellier_reflns_redundancy_maxres 1.74

#montpellier_diffrn_reflns_class_completeness_shell is completeness in shell
#montpellier_diffrn_class_reflns_cumul_completeness is cumulative
#completeness to resolution of shell
#Note: completeness percentage takes into account the fact whether
#group is centrosymmetric or not
loop_
_montpellier_diffrn_reflns_class_number
_montpellier_diffrn_reflns_class_d_res_high
_montpellier_diffrn_reflns_class_d_res_low
_montpellier_diffrn_reflns_class_redundancy
_montpellier_diffrn_reflns_class_av_I/uI
_diffrn_reflns_class_av_R_eq
_montpellier_diffrn_reflns_class_completeness_shell
_montpellier_diffrn_reflns_class_cumul_completeness
0 100.0 1.66 2.9 42.14 0.016 99.9 99.89
1 1.66 1.33 2.3 25.06 0.020 100.0 99.94
2 1.33 1.16 2.0 21.37 0.023 100.0 99.96
3 1.16 1.05 1.8 15.49 0.028 100.0 99.97
4 1.05 0.98 1.7 12.06 0.033 100.0 99.98
5 0.98 0.92 1.5 9.91 0.040 100.0 99.98
6 0.92 0.87 1.4 8.28 0.046 99.9 99.97
7 0.87 0.84 1.3 7.46 0.048 100.0 99.97
8 0.83 0.80 1.3 6.61 0.052 99.9 99.96
9 0.80 0.73 1.2 5.40 0.072 36.2 84.91
#End reflection statistics
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_orient_matrix_UB_11      -0.0349949000
_diffrn_orient_matrix_UB_12      -0.0449600000
_diffrn_orient_matrix_UB_13      -0.0276864000
_diffrn_orient_matrix_UB_21      0.0589793000
_diffrn_orient_matrix_UB_22      -0.0360427000
_diffrn_orient_matrix_UB_23      -0.0011680000
_diffrn_orient_matrix_UB_31      -0.0248044000
_diffrn_orient_matrix_UB_32      -0.0394863000
_diffrn_orient_matrix_UB_33      0.0243776000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -24.00   58.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668 -100.0000 -180.0000 82

#__ type_ start__ end____ width___ exp.time_
  2 omega  -51.00  -19.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668  -57.0000   30.0000 32

#__ type_ start__ end____ width___ exp.time_
  3 omega  -54.00   43.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668  -38.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
  4 omega   32.00   58.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668 -179.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega   -8.00   86.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668   77.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega  -12.00   34.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       17.7668   77.0000  -60.0000 46

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      125
_diffrn_reflns_number            15112
_reflns_number_total             8700
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_unetI/netI     0.0368
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 8700
# Theoretical number of reflections is about 20470


_diffrn_reflns_theta_min         2.006
_diffrn_reflns_theta_max         28.969
_diffrn_measured_fraction_theta_max 0.850

_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -12
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   1.06
_oxford_diffrn_Wilson_scale      0.07

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

_refine_diff_density_min         -0.38
_refine_diff_density_max         0.50


# 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>2.0\s(I)
_refine_ls_number_reflns         6676
_refine_ls_number_restraints     0
_refine_ls_number_parameters     496
_oxford_refine_ls_R_factor_ref   0.0418
_refine_ls_wR_factor_ref         0.0489
_refine_ls_goodness_of_fit_ref   0.9891
_refine_ls_shift/su_max          0.0006551
_refine_ls_shift/su_mean         0.0000345


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8700
_refine_ls_R_factor_all          0.0587
_refine_ls_wR_factor_all         0.0591

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6676
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_gt          0.0489

# 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 F
_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: 
 15.5 16.3 14.6 5.06 
;

# 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
S1 S 0.59554(3) 0.62386(3) 0.102466(16) 0.0108 1.0000 Uani . . . . . .
O2 O 0.66249(11) 0.56636(10) 0.04376(5) 0.0166 1.0000 Uani . . . . . .
O3 O 0.50033(11) 0.53080(10) 0.12783(5) 0.0173 1.0000 Uani . . . . . .
O4 O 0.69574(11) 0.69167(10) 0.15817(5) 0.0166 1.0000 Uani . . . . . .
C5 C 0.49616(14) 0.74649(13) 0.07048(7) 0.0107 1.0000 Uani . . . . . .
C6 C 0.35604(14) 0.73284(14) 0.07479(7) 0.0120 1.0000 Uani . . . . . .
C7 C 0.27132(13) 0.82348(13) 0.04988(7) 0.0104 1.0000 Uani . . . . . .
S8 S 0.09357(3) 0.80154(3) 0.061711(17) 0.0113 1.0000 Uani . . . . . .
O9 O 0.01909(10) 0.76803(10) -0.00812(5) 0.0171 1.0000 Uani . . . . . .
O10 O 0.08328(11) 0.69209(11) 0.10256(6) 0.0201 1.0000 Uani . . . . . .
O11 O 0.05644(10) 0.92390(10) 0.09690(5) 0.0170 1.0000 Uani . . . . . .
C12 C 0.32546(14) 0.92962(13) 0.01819(7) 0.0106 1.0000 Uani . . . . . .
C13 C 0.47084(13) 0.94555(13) 0.01526(6) 0.0098 1.0000 Uani . . . . . .
C14 C 0.55776(13) 0.85421(13) 0.04286(7) 0.0097 1.0000 Uani . . . . . .
C15 C 0.70398(14) 0.87777(14) 0.04192(7) 0.0128 1.0000 Uani . . . . . .
C16 C 0.75884(14) 0.97956(13) 0.01304(7) 0.0111 1.0000 Uani . . . . . .
S17 S 0.40787(3) 0.37385(3) 0.394511(16) 0.0115 1.0000 Uani . . . . . .
O18 O 0.31319(11) 0.30135(11) 0.33781(5) 0.0177 1.0000 Uani . . . . . .
O19 O 0.33510(11) 0.43421(11) 0.44986(5) 0.0186 1.0000 Uani . . . . . .
O20 O 0.50457(11) 0.46541(11) 0.36908(6) 0.0190 1.0000 Uani . . . . . .
C21 C 0.50669(14) 0.25531(13) 0.43099(7) 0.0110 1.0000 Uani . . . . . .
C22 C 0.44385(14) 0.14630(13) 0.45718(7) 0.0110 1.0000 Uani . . . . . .
C23 C 0.29768(14) 0.12165(14) 0.45567(7) 0.0124 1.0000 Uani . . . . . .
C24 C 0.24114(14) 0.01776(14) 0.48255(7) 0.0121 1.0000 Uani . . . . . .
C25 C 0.67540(14) 0.07362(13) 0.48630(6) 0.0104 1.0000 Uani . . . . . .
C26 C 0.53009(14) 0.05548(13) 0.48601(6) 0.0100 1.0000 Uani . . . . . .
C27 C 0.73100(13) 0.18126(13) 0.45642(7) 0.0109 1.0000 Uani . . . . . .
C28 C 0.64742(14) 0.27107(14) 0.42977(7) 0.0123 1.0000 Uani . . . . . .
S29 S 0.90994(3) 0.20355(3) 0.448158(17) 0.0123 1.0000 Uani . . . . . .
O30 O 0.94545(11) 0.08774(11) 0.40617(5) 0.0180 1.0000 Uani . . . . . .
O31 O 0.92628(12) 0.32365(12) 0.41600(7) 0.0251 1.0000 Uani . . . . . .
O32 O 0.98040(10) 0.21954(11) 0.51922(5) 0.0176 1.0000 Uani . . . . . .
O33 O 0.8955(2) 0.89339(18) 0.22213(8) 0.0580 1.0000 Uani . . . . . .
O34 O 0.08962(18) 0.12692(19) 0.28163(8) 0.0559 1.0000 Uani . . . . . .
N35 N 0.90855(13) 0.46397(12) 0.08800(6) 0.0160 1.0000 Uani . . . . . .
C36 C 0.88087(16) 0.42101(15) 0.15648(7) 0.0177 1.0000 Uani . . . . . .
C37 C 0.77599(16) 0.30229(16) 0.14457(8) 0.0199 1.0000 Uani . . . . . .
C38 C 0.73108(17) 0.25925(16) 0.21167(8) 0.0222 1.0000 Uani . . . . . .
C39 C 0.63319(19) 0.13535(16) 0.19548(8) 0.0244 1.0000 Uani . . . . . .
C40 C 0.57410(18) 0.08786(16) 0.25885(8) 0.0227 1.0000 Uani . . . . . .
C41 C 0.47676(19) -0.03568(17) 0.23781(8) 0.0267 1.0000 Uani . . . . . .
C42 C 0.40378(19) -0.08533(17) 0.29639(8) 0.0264 1.0000 Uani . . . . . .
C43 C 0.31521(18) -0.21217(17) 0.26975(8) 0.0245 1.0000 Uani . . . . . .
C44 C 0.22617(18) -0.26702(16) 0.32127(8) 0.0243 1.0000 Uani . . . . . .
N45 N 0.33879(14) 0.34883(14) 0.19696(7) 0.0218 1.0000 Uani . . . . . .
C46 C 0.24811(15) 0.29854(14) 0.14365(7) 0.0152 1.0000 Uani . . . . . .
N47 N 0.25407(14) 0.34463(14) 0.08296(6) 0.0206 1.0000 Uani . . . . . .
N48 N 0.15176(15) 0.20518(14) 0.15039(7) 0.0232 1.0000 Uani . . . . . .
N49 N 0.73703(15) 0.66103(14) 0.41551(6) 0.0224 1.0000 Uani . . . . . .
C50 C 0.74421(16) 0.70668(15) 0.35478(8) 0.0168 1.0000 Uani . . . . . .
N51 N 0.83189(15) 0.80780(14) 0.34958(7) 0.0249 1.0000 Uani . . . . . .
N52 N 0.66561(15) 0.64602(14) 0.29934(7) 0.0228 1.0000 Uani . . . . . .
N53 N 0.08960(13) -0.45706(12) 0.40563(6) 0.0156 1.0000 Uani . . . . . .
C54 C 0.05335(17) -0.46538(16) 0.32880(8) 0.0208 1.0000 Uani . . . . . .
C1 C 0.16667(18) -0.40514(16) 0.29242(8) 0.0240 1.0000 Uani . . . . . .
H25 H 0.1468 0.0051 0.4812 0.0152 1.0000 Uiso R . . . . .
H33 H 0.7615 0.8207 0.0624 0.0151 1.0000 Uiso R . . . . .
H36 H 0.3200 0.6632 0.0948 0.0163 1.0000 Uiso R . . . . .
H1 H 0.2407 0.1787 0.4342 0.0149 1.0000 Uiso R . . . . .
H2 H 0.3339 0.3250 0.2382 0.0255 1.0000 Uiso R . . . . .
H11 H 0.8533 0.9914 0.0126 0.0150 1.0000 Uiso R . . . . .
H4 H 0.6702 0.6068 0.4201 0.0268 1.0000 Uiso R . . . . .
H5 H 0.8123 0.2395 0.2410 0.0261 1.0000 Uiso R . . . . .
H6 H 0.9695 0.4010 0.1800 0.0214 1.0000 Uiso R . . . . .
H7 H 0.3245 0.3932 0.0761 0.0262 1.0000 Uiso R . . . . .
H8 H 0.6692 0.6701 0.2580 0.0272 1.0000 Uiso R . . . . .
H9 H 0.2027 0.3046 0.0476 0.0266 1.0000 Uiso R . . . . .
H10 H 0.8458 0.4925 0.1838 0.0219 1.0000 Uiso R . . . . .
H12 H 0.1775 -0.4753 0.4168 0.0242 1.0000 Uiso R . . . . .
H14 H 0.2571 -0.1981 0.2284 0.0299 1.0000 Uiso R . . . . .
H15 H 0.6874 0.3303 0.2359 0.0276 1.0000 Uiso R . . . . .
H16 H 0.1474 0.1769 0.1902 0.0289 1.0000 Uiso R . . . . .
H17 H -0.0295 -0.4183 0.3222 0.0257 1.0000 Uiso R . . . . .
H18 H 0.5222 0.1562 0.2804 0.0270 1.0000 Uiso R . . . . .
H19 H 0.3975 0.4115 0.1912 0.0269 1.0000 Uiso R . . . . .
H20 H 0.9393 0.3968 0.0611 0.0245 1.0000 Uiso R . . . . .
H21 H 0.1062 0.1651 0.1137 0.0287 1.0000 Uiso R . . . . .
H22 H 0.0782 -0.3760 0.4259 0.0234 1.0000 Uiso R . . . . .
H23 H 0.3470 -0.0169 0.3135 0.0314 1.0000 Uiso R . . . . .
H24 H 0.9705 0.5334 0.0936 0.0242 1.0000 Uiso R . . . . .
H26 H 0.5566 0.1506 0.1623 0.0277 1.0000 Uiso R . . . . .
H27 H 0.6473 0.0702 0.2919 0.0266 1.0000 Uiso R . . . . .
H28 H 0.5291 -0.1073 0.2182 0.0310 1.0000 Uiso R . . . . .
H29 H 0.8474 0.8306 0.3098 0.0285 1.0000 Uiso R . . . . .
H30 H 0.4720 -0.1017 0.3338 0.0307 1.0000 Uiso R . . . . .
H31 H 0.7870 0.6998 0.4509 0.0276 1.0000 Uiso R . . . . .
H32 H 0.0326 -0.5567 0.3115 0.0252 1.0000 Uiso R . . . . .
H34 H 0.3772 -0.2795 0.2558 0.0293 1.0000 Uiso R . . . . .
H35 H 0.6070 0.5800 0.3037 0.0268 1.0000 Uiso R . . . . .
H37 H 0.8152 0.2290 0.1193 0.0227 1.0000 Uiso R . . . . .
H38 H 0.6960 0.3233 0.1155 0.0245 1.0000 Uiso R . . . . .
H39 H 0.6806 0.0655 0.1731 0.0290 1.0000 Uiso R . . . . .
H40 H 0.1266 -0.4034 0.2436 0.0292 1.0000 Uiso R . . . . .
H41 H 0.2814 -0.2686 0.3655 0.0289 1.0000 Uiso R . . . . .
H43 H 0.8299 0.4868 0.0667 0.0246 1.0000 Uiso R . . . . .
H44 H 0.4063 -0.0178 0.2023 0.0328 1.0000 Uiso R . . . . .
H45 H 0.8787 0.8472 0.3866 0.0303 1.0000 Uiso R . . . . .
H46 H 0.2437 -0.4639 0.2943 0.0293 1.0000 Uiso R . . . . .
H47 H 0.0343 -0.5152 0.4227 0.0233 1.0000 Uiso R . . . . .
H48 H 0.0243 0.1048 0.3017 0.0838 1.0000 Uiso R . . . . .
H49 H 0.1535 -0.2098 0.3306 0.0301 1.0000 Uiso R . . . . .
H13 H 0.6871 0.3418 0.4118 0.0171 1.0000 Uiso R . . . . .
H50 H 0.1503 0.1728 0.3088 0.0837 1.0000 Uiso R . . . . .
H3 H 0.8528 0.8382 0.1912 0.0871 1.0000 Uiso R . . . . .
H55 H 0.9739 0.9039 0.2139 0.0879 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.549(4)
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
S1 . O2 . 1.4610(10) yes
S1 . O3 . 1.4508(11) yes
S1 . O4 . 1.4624(10) yes
S1 . C5 . 1.7773(14) yes
C5 . C6 . 1.3840(19) yes
C5 . C14 . 1.4093(19) yes
C6 . C7 . 1.3879(19) yes
C6 . H36 . 0.919 no
C7 . S8 . 1.7840(13) yes
C7 . C12 . 1.4108(19) yes
S8 . O9 . 1.4685(10) yes
S8 . O10 . 1.4539(11) yes
S8 . O11 . 1.4464(10) yes
C12 . C16 2_675 1.4367(19) yes
C12 . C13 . 1.4319(18) yes
C13 . C13 2_675 1.436(3) yes
C13 . C14 . 1.4264(18) yes
C14 . C15 . 1.4402(18) yes
C15 . C16 . 1.3474(19) yes
C15 . H33 . 0.937 no
C16 . H11 . 0.928 no
S17 . O18 . 1.4623(10) yes
S17 . O19 . 1.4546(11) yes
S17 . O20 . 1.4507(11) yes
S17 . C21 . 1.7767(14) yes
C21 . C22 . 1.4108(19) yes
C21 . C28 . 1.3817(19) yes
C22 . C23 . 1.4354(19) yes
C22 . C26 . 1.4280(19) yes
C23 . C24 . 1.350(2) yes
C23 . H1 . 0.942 no
C24 . C25 2_656 1.4355(19) yes
C24 . H25 . 0.923 no
C25 . C26 . 1.4241(19) yes
C25 . C27 . 1.4089(19) yes
C26 . C26 2_656 1.434(3) yes
C27 . C28 . 1.3876(19) yes
C27 . S29 . 1.7802(14) yes
C28 . H13 . 0.921 no
S29 . O30 . 1.4457(11) yes
S29 . O31 . 1.4525(11) yes
S29 . O32 . 1.4692(10) yes
O33 . H3 . 0.834 no
O33 . H55 . 0.805 no
O34 . H48 . 0.816 no
O34 . H50 . 0.833 no
N35 . C36 . 1.4967(18) yes
N35 . H20 . 0.903 no
N35 . H24 . 0.893 no
N35 . H43 . 0.898 no
C36 . C37 . 1.518(2) yes
C36 . H6 . 0.988 no
C36 . H10 . 0.960 no
C37 . C38 . 1.523(2) yes
C37 . H37 . 0.974 no
C37 . H38 . 0.973 no
C38 . C39 . 1.520(2) yes
C38 . H5 . 0.981 no
C38 . H15 . 0.971 no
C39 . C40 . 1.530(2) yes
C39 . H26 . 0.975 no
C39 . H39 . 0.967 no
C40 . C41 . 1.521(2) yes
C40 . H18 . 0.975 no
C40 . H27 . 0.957 no
C41 . C42 . 1.524(2) yes
C41 . H28 . 0.989 no
C41 . H44 . 0.971 no
C42 . C43 . 1.519(2) yes
C42 . H23 . 0.976 no
C42 . H30 . 0.977 no
C43 . C44 . 1.525(2) yes
C43 . H14 . 0.971 no
C43 . H34 . 0.985 no
C44 . C1 . 1.515(2) yes
C44 . H41 . 0.974 no
C44 . H49 . 0.973 no
N45 . C46 . 1.3262(19) yes
N45 . H2 . 0.870 no
N45 . H19 . 0.857 no
C46 . N47 . 1.3286(19) yes
C46 . N48 . 1.324(2) yes
N47 . H7 . 0.854 no
N47 . H9 . 0.855 no
N48 . H16 . 0.863 no
N48 . H21 . 0.848 no
N49 . C50 . 1.329(2) yes
N49 . H4 . 0.848 no
N49 . H31 . 0.844 no
C50 . N51 . 1.320(2) yes
C50 . N52 . 1.3246(19) yes
N51 . H29 . 0.859 no
N51 . H45 . 0.856 no
N52 . H8 . 0.872 no
N52 . H35 . 0.875 no
N53 . C54 . 1.4937(19) yes
N53 . H12 . 0.906 no
N53 . H22 . 0.897 no
N53 . H47 . 0.893 no
C54 . C1 . 1.511(2) yes
C54 . H17 . 0.980 no
C54 . H32 . 0.958 no
C1 . H40 . 0.995 no
C1 . H46 . 1.000 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
O2 . S1 . O3 . 113.45(6) yes
O2 . S1 . O4 . 111.59(6) yes
O3 . S1 . O4 . 112.14(6) yes
O2 . S1 . C5 . 106.01(6) yes
O3 . S1 . C5 . 106.52(6) yes
O4 . S1 . C5 . 106.55(6) yes
S1 . C5 . C6 . 117.23(11) yes
S1 . C5 . C14 . 121.38(10) yes
C6 . C5 . C14 . 121.39(13) yes
C5 . C6 . C7 . 120.60(13) yes
C5 . C6 . H36 . 119.0 no
C7 . C6 . H36 . 120.4 no
C6 . C7 . S8 . 117.09(10) yes
C6 . C7 . C12 . 120.83(12) yes
S8 . C7 . C12 . 122.07(10) yes
C7 . S8 . O9 . 106.33(6) yes
C7 . S8 . O10 . 104.84(6) yes
O9 . S8 . O10 . 111.58(7) yes
C7 . S8 . O11 . 107.44(6) yes
O9 . S8 . O11 . 112.48(6) yes
O10 . S8 . O11 . 113.51(7) yes
C16 2_675 C12 . C7 . 123.07(12) yes
C16 2_675 C12 . C13 . 118.38(12) yes
C7 . C12 . C13 . 118.53(12) yes
C13 2_675 C13 . C12 . 119.74(15) yes
C13 2_675 C13 . C14 . 119.99(15) yes
C12 . C13 . C14 . 120.27(12) yes
C13 . C14 . C5 . 118.25(12) yes
C13 . C14 . C15 . 118.35(12) yes
C5 . C14 . C15 . 123.40(12) yes
C14 . C15 . C16 . 121.69(12) yes
C14 . C15 . H33 . 118.5 no
C16 . C15 . H33 . 119.9 no
C12 2_675 C16 . C15 . 121.72(12) yes
C12 2_675 C16 . H11 . 118.6 no
C15 . C16 . H11 . 119.7 no
O18 . S17 . O19 . 111.76(7) yes
O18 . S17 . O20 . 111.68(6) yes
O19 . S17 . O20 . 113.59(7) yes
O18 . S17 . C21 . 106.34(6) yes
O19 . S17 . C21 . 106.56(6) yes
O20 . S17 . C21 . 106.34(6) yes
S17 . C21 . C22 . 121.48(10) yes
S17 . C21 . C28 . 117.17(11) yes
C22 . C21 . C28 . 121.28(13) yes
C21 . C22 . C23 . 123.24(12) yes
C21 . C22 . C26 . 118.27(12) yes
C23 . C22 . C26 . 118.49(12) yes
C22 . C23 . C24 . 121.64(13) yes
C22 . C23 . H1 . 118.4 no
C24 . C23 . H1 . 119.9 no
C25 2_656 C24 . C23 . 121.47(13) yes
C25 2_656 C24 . H25 . 119.0 no
C23 . C24 . H25 . 119.6 no
C24 2_656 C25 . C26 . 118.68(12) yes
C24 2_656 C25 . C27 . 122.87(12) yes
C26 . C25 . C27 . 118.45(12) yes
C26 2_656 C26 . C22 . 119.81(15) yes
C26 2_656 C26 . C25 . 119.84(15) yes
C22 . C26 . C25 . 120.34(12) yes
C25 . C27 . C28 . 121.16(13) yes
C25 . C27 . S29 . 121.35(10) yes
C28 . C27 . S29 . 117.44(11) yes
C27 . C28 . C21 . 120.40(13) yes
C27 . C28 . H13 . 119.1 no
C21 . C28 . H13 . 120.5 no
C27 . S29 . O30 . 107.26(6) yes
C27 . S29 . O31 . 104.80(7) yes
O30 . S29 . O31 . 113.80(7) yes
C27 . S29 . O32 . 106.21(6) yes
O30 . S29 . O32 . 112.54(6) yes
O31 . S29 . O32 . 111.53(7) yes
H3 . O33 . H55 . 108.8 no
H48 . O34 . H50 . 111.3 no
C36 . N35 . H20 . 109.6 no
C36 . N35 . H24 . 111.3 no
H20 . N35 . H24 . 109.5 no
C36 . N35 . H43 . 108.7 no
H20 . N35 . H43 . 109.2 no
H24 . N35 . H43 . 108.5 no
N35 . C36 . C37 . 109.58(12) yes
N35 . C36 . H6 . 107.3 no
C37 . C36 . H6 . 112.1 no
N35 . C36 . H10 . 108.6 no
C37 . C36 . H10 . 109.9 no
H6 . C36 . H10 . 109.4 no
C36 . C37 . C38 . 113.37(13) yes
C36 . C37 . H37 . 108.9 no
C38 . C37 . H37 . 108.7 no
C36 . C37 . H38 . 108.7 no
C38 . C37 . H38 . 109.4 no
H37 . C37 . H38 . 107.7 no
C37 . C38 . C39 . 110.04(13) yes
C37 . C38 . H5 . 109.0 no
C39 . C38 . H5 . 108.4 no
C37 . C38 . H15 . 109.1 no
C39 . C38 . H15 . 110.8 no
H5 . C38 . H15 . 109.5 no
C38 . C39 . C40 . 114.61(13) yes
C38 . C39 . H26 . 109.4 no
C40 . C39 . H26 . 108.0 no
C38 . C39 . H39 . 108.9 no
C40 . C39 . H39 . 108.7 no
H26 . C39 . H39 . 106.9 no
C39 . C40 . C41 . 111.02(13) yes
C39 . C40 . H18 . 109.3 no
C41 . C40 . H18 . 107.9 no
C39 . C40 . H27 . 109.7 no
C41 . C40 . H27 . 109.6 no
H18 . C40 . H27 . 109.2 no
C40 . C41 . C42 . 115.23(14) yes
C40 . C41 . H28 . 108.8 no
C42 . C41 . H28 . 107.8 no
C40 . C41 . H44 . 108.6 no
C42 . C41 . H44 . 107.3 no
H28 . C41 . H44 . 108.9 no
C41 . C42 . C43 . 110.24(13) yes
C41 . C42 . H23 . 107.6 no
C43 . C42 . H23 . 110.4 no
C41 . C42 . H30 . 109.4 no
C43 . C42 . H30 . 109.3 no
H23 . C42 . H30 . 109.8 no
C42 . C43 . C44 . 116.02(13) yes
C42 . C43 . H14 . 108.5 no
C44 . C43 . H14 . 109.3 no
C42 . C43 . H34 . 107.5 no
C44 . C43 . H34 . 107.7 no
H14 . C43 . H34 . 107.5 no
C43 . C44 . C1 . 109.51(13) yes
C43 . C44 . H41 . 109.7 no
C1 . C44 . H41 . 109.8 no
C43 . C44 . H49 . 110.3 no
C1 . C44 . H49 . 110.9 no
H41 . C44 . H49 . 106.6 no
C46 . N45 . H2 . 121.1 no
C46 . N45 . H19 . 118.6 no
H2 . N45 . H19 . 120.0 no
N45 . C46 . N47 . 118.82(14) yes
N45 . C46 . N48 . 121.15(14) yes
N47 . C46 . N48 . 120.03(14) yes
C46 . N47 . H7 . 120.0 no
C46 . N47 . H9 . 118.1 no
H7 . N47 . H9 . 118.5 no
C46 . N48 . H16 . 119.6 no
C46 . N48 . H21 . 118.1 no
H16 . N48 . H21 . 121.3 no
C50 . N49 . H4 . 119.1 no
C50 . N49 . H31 . 118.8 no
H4 . N49 . H31 . 120.4 no
N49 . C50 . N51 . 120.31(14) yes
N49 . C50 . N52 . 118.83(14) yes
N51 . C50 . N52 . 120.81(14) yes
C50 . N51 . H29 . 121.5 no
C50 . N51 . H45 . 118.7 no
H29 . N51 . H45 . 119.7 no
C50 . N52 . H8 . 122.3 no
C50 . N52 . H35 . 119.7 no
H8 . N52 . H35 . 118.0 no
C54 . N53 . H12 . 112.1 no
C54 . N53 . H22 . 109.8 no
H12 . N53 . H22 . 108.9 no
C54 . N53 . H47 . 109.4 no
H12 . N53 . H47 . 108.0 no
H22 . N53 . H47 . 108.7 no
N53 . C54 . C1 . 112.87(13) yes
N53 . C54 . H17 . 106.1 no
C1 . C54 . H17 . 110.2 no
N53 . C54 . H32 . 107.2 no
C1 . C54 . H32 . 110.7 no
H17 . C54 . H32 . 109.7 no
C44 . C1 . C54 . 117.17(13) yes
C44 . C1 . H40 . 108.0 no
C54 . C1 . H40 . 105.9 no
C44 . C1 . H46 . 107.5 no
C54 . C1 . H46 . 107.4 no
H40 . C1 . H46 . 110.8 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
C24 . H25 . O30 1_455 133.16(4) 0.923 2.590 3.290(2) yes
C24 . H25 . O32 2_656 123.13(4) 0.923 2.540 3.141(2) yes
C15 . H33 . O4 . 123.15(4) 0.937 2.520 3.132(2) yes
C23 . H1 . O18 . 122.15(4) 0.942 2.512 3.117(2) yes
N45 . H2 . O18 . 170.18(5) 0.870 2.012 2.874(2) yes
N49 . H4 . O20 . 147.27(4) 0.848 2.175 2.925(2) yes
N47 . H7 . O3 . 144.52(4) 0.854 2.225 2.963(2) yes
N52 . H8 . O4 . 168.40(5) 0.872 2.023 2.883(2) yes
N47 . H9 . O9 2_565 143.05(4) 0.855 2.276 3.004(2) yes
N53 . H12 . O19 1_545 161.05(5) 0.906 1.953 2.825(2) yes
N48 . H16 . O34 . 165.68(7) 0.863 2.032 2.876(2) yes
N45 . H19 . O3 . 152.19(5) 0.857 2.113 2.899(2) yes
N35 . H20 . O9 2_665 170.17(5) 0.903 1.966 2.861(2) yes
N48 . H21 . O9 2_565 135.41(4) 0.848 2.481 3.142(2) yes
N48 . H21 . O11 1_545 121.90(4) 0.848 2.465 3.001(2) yes
N53 . H22 . O32 2_656 166.59(5) 0.897 1.975 2.856(2) yes
N35 . H24 . O10 1_655 173.02(5) 0.893 1.882 2.770(2) yes
N51 . H29 . O33 . 175.36(6) 0.859 1.982 2.840(2) yes
N49 . H31 . O32 2_766 137.72(4) 0.844 2.363 3.041(2) yes
N52 . H35 . O20 . 149.01(5) 0.875 2.110 2.895(2) yes
N35 . H43 . O2 . 164.77(5) 0.898 1.922 2.798(2) yes
N51 . H45 . O30 1_565 123.80(4) 0.856 2.483 3.043(2) yes
N51 . H45 . O32 2_766 135.31(4) 0.856 2.380 3.049(2) yes
N53 . H47 . O31 1_445 152.60(5) 0.893 1.883 2.707(2) yes
O34 . H48 . O30 1_455 146.01(5) 0.816 2.268 2.980(2) yes
O34 . H50 . O18 . 157.43(5) 0.833 1.989 2.777(2) yes
O33 . H3 . O4 . 150.82(5) 0.834 2.072 2.829(2) yes
O33 . H55 . O11 1_655 126.85(5) 0.805 2.519 3.070(2) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 11/12/13 at 18:20:17
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   6,X'S) H   (  36,X'S) 
RIDE C   (  15,X'S) H   (  33,X'S) 
RIDE C   (  16,X'S) H   (  11,X'S) 
RIDE C   (  23,X'S) H   (   1,X'S) 
RIDE C   (  24,X'S) H   (  25,X'S) 
RIDE C   (  28,X'S) H   (  13,X'S) 
RIDE O   (  33,X'S) H   (   3,X'S) H   (  55,X'S) 
RIDE O   (  34,X'S) H   (  48,X'S) H   (  50,X'S) 
RIDE N   (  35,X'S) H   (  20,X'S) H   (  24,X'S) H   (  43,X'S) 
RIDE C   (  36,X'S) H   (   6,X'S) H   (  10,X'S) 
RIDE C   (  37,X'S) H   (  37,X'S) H   (  38,X'S) 
RIDE C   (  38,X'S) H   (   5,X'S) H   (  15,X'S) 
RIDE C   (  39,X'S) H   (  26,X'S) H   (  39,X'S) 
RIDE C   (  40,X'S) H   (  18,X'S) H   (  27,X'S) 
RIDE C   (  41,X'S) H   (  28,X'S) H   (  44,X'S) 
RIDE C   (  42,X'S) H   (  23,X'S) H   (  30,X'S) 
RIDE C   (  43,X'S) H   (  14,X'S) H   (  34,X'S) 
RIDE C   (  44,X'S) H   (  41,X'S) H   (  49,X'S) 
RIDE N   (  45,X'S) H   (   2,X'S) H   (  19,X'S) 
RIDE N   (  47,X'S) H   (   7,X'S) H   (   9,X'S) 
RIDE N   (  48,X'S) H   (  16,X'S) H   (  21,X'S) 
RIDE N   (  49,X'S) H   (   4,X'S) H   (  31,X'S)
RIDE N   (  51,X'S) H   (  29,X'S) H   (  45,X'S) 
RIDE N   (  52,X'S) H   (   8,X'S) H   (  35,X'S) 
RIDE N   (  53,X'S) H   (  12,X'S) H   (  22,X'S) H   (  47,X'S) 
RIDE C   (  54,X'S) H   (  17,X'S) H   (  32,X'S) 
RIDE C   (   1,X'S) H   (  40,X'S) H   (  46,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 11/12/13 at 18:20:17
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
# start Validation Reply Form
_vrf_PLAT112_1                   
;
PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem...          Z
RESPONSE: True, this is described in the text, it is really pseudo
;
# end Validation Reply For
_database_code_depnum_ccdc_archive 'CCDC 986090'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_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                   9.8826(4)
_cell_length_b                   10.2939(4)
_cell_length_c                   9.8156(4)
_cell_angle_alpha                96.289(3)
_cell_angle_beta                 95.622(3)
_cell_angle_gamma                94.839(3)
_cell_volume                     983.19(7)
_cell_measurement_reflns_used    8267
_cell_measurement_theta_min      2.0830
_cell_measurement_theta_max      32.0910
_cell_oxdiff_length_a            9.8156(4)
_cell_oxdiff_length_b            9.8831(4)
_cell_oxdiff_length_c            10.2952(4)
_cell_oxdiff_angle_alpha         94.845(3)
_cell_oxdiff_angle_beta          96.293(3)
_cell_oxdiff_angle_gamma         95.622(3)
_cell_oxdiff_volume              983.34(7)

_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 0.0033 0.0016 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 0.0061 0.0033 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 0.0106 0.0060 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 0.1246 0.1234 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            1

_chemical_formula_sum            'C29 H50 N8 O14 S4'
_chemical_formula_moiety         
'C16 H6 O12 S4, C11 H28 N2, 2(C H6 N3), 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         863.05


_cell_measurement_temperature    293

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.400
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_max          0.500
_exptl_absorpt_correction_T_min  0.98185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             456
_exptl_absorpt_coefficient_mu    0.316
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 16.0143

_diffrn_measurement_device       Area
_diffrn_radiation_wavelength     0.71073
#montpellier_reflns_maxres is minimum d (highest resolution)
#where <I/sigI> <= 2.0
#(Z. Dauter, Acta Cryst. D55, 1703-1717, 1999)
_montpellier_reflns_maxres       0.66
_montpellier_reflns_completeness_maxres 94.29
_montpellier_reflns_redundancy_maxres 4.71

#montpellier_diffrn_reflns_class_completeness_shell is completeness in shell
#montpellier_diffrn_class_reflns_cumul_completeness is cumulative
#completeness to resolution of shell
#Note: completeness percentage takes into account the fact whether
#group is centrosymmetric or not
loop_
_montpellier_diffrn_reflns_class_number
_montpellier_diffrn_reflns_class_d_res_high
_montpellier_diffrn_reflns_class_d_res_low
_montpellier_diffrn_reflns_class_redundancy
_montpellier_diffrn_reflns_class_av_I/uI
_diffrn_reflns_class_av_R_eq
_montpellier_diffrn_reflns_class_completeness_shell
_montpellier_diffrn_reflns_class_cumul_completeness
0 100.0 1.45 7.0 75.87 0.026 100.0 100.00
1 1.45 1.16 6.5 43.85 0.027 100.0 100.00
2 1.16 1.01 5.8 28.15 0.040 100.0 100.00
3 1.01 0.92 5.2 19.11 0.060 100.0 100.00
4 0.92 0.85 4.8 13.87 0.082 100.0 100.00
5 0.85 0.80 4.4 10.55 0.101 100.0 100.00
6 0.80 0.76 4.1 7.96 0.137 100.0 100.00
7 0.76 0.73 3.8 7.49 0.141 100.0 100.00
8 0.73 0.70 3.6 5.66 0.191 99.7 99.97
9 0.70 0.66 1.8 3.62 0.217 62.7 94.29
#End reflection statistics
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_orient_matrix_UB_11      -0.0581866000
_diffrn_orient_matrix_UB_12      0.0257566000
_diffrn_orient_matrix_UB_13      0.0243784000
_diffrn_orient_matrix_UB_21      0.0219316000
_diffrn_orient_matrix_UB_22      0.0657031000
_diffrn_orient_matrix_UB_23      -0.0178313000
_diffrn_orient_matrix_UB_31      -0.0384888000
_diffrn_orient_matrix_UB_32      -0.0164025000
_diffrn_orient_matrix_UB_33      -0.0627459000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   12.00   72.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   19.0000  150.0000 60

#__ type_ start__ end____ width___ exp.time_
  2 omega   68.00   95.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   57.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  -23.00   68.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169 -100.0000   60.0000 91

#__ type_ start__ end____ width___ exp.time_
  4 omega   28.00   96.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   77.0000  -60.0000 68

#__ type_ start__ end____ width___ exp.time_
  5 omega   43.00   68.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169 -100.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
  6 omega   10.00   93.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   57.0000 -180.0000 83

#__ type_ start__ end____ width___ exp.time_
  7 omega   -1.00   68.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169 -100.0000  -90.0000 69

#__ type_ start__ end____ width___ exp.time_
  8 omega -103.00  -78.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9544  179.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
  9 omega   -4.00   96.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   77.0000  150.0000 100

#__ type_ start__ end____ width___ exp.time_
 10 omega    5.00   95.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   57.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
 11 omega  -43.00   46.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  -57.0000 -180.0000 89

#__ type_ start__ end____ width___ exp.time_
 12 omega   34.00  102.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  179.0000   60.0000 68

#__ type_ start__ end____ width___ exp.time_
 13 omega -103.00  -56.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9544 -179.0000    0.0000 47

#__ type_ start__ end____ width___ exp.time_
 14 omega  -97.00    3.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9544  -77.0000   30.0000 100

#__ type_ start__ end____ width___ exp.time_
 15 omega   -4.00   96.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169   77.0000  -30.0000 100

#__ type_ start__ end____ width___ exp.time_
 16 omega   34.00  102.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  179.0000  150.0000 68

#__ type_ start__ end____ width___ exp.time_
 17 omega   34.00   84.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  179.0000    0.0000 50

#__ type_ start__ end____ width___ exp.time_
 18 omega  -43.00   46.00   1.0000  147.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0169  -57.0000  120.0000 89

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      293
_diffrn_reflns_number            31497
_reflns_number_total             6688
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0473
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6688 
# Theoretical number of reflections is about 14171


_diffrn_reflns_theta_min         2.000
_diffrn_reflns_theta_max         32.446
_diffrn_measured_fraction_theta_max 0.943

_diffrn_reflns_theta_full        28.552
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              -15
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              14

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -0.38
_refine_diff_density_max         0.50


# 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>2.0\s(I)
_refine_ls_number_reflns         5199
_refine_ls_number_restraints     42
_refine_ls_number_parameters     298
_oxford_refine_ls_R_factor_ref   0.0479
_refine_ls_wR_factor_ref         0.0539
_refine_ls_goodness_of_fit_ref   1.0233
_refine_ls_shift/su_max          0.0004576
_refine_ls_shift/su_mean         0.0000217


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6688
_refine_ls_R_factor_all          0.0670
_refine_ls_wR_factor_all         0.0632

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5199
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_gt          0.0539

# 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 F
_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:
 14.7 14.1 13.5 4.57 
;

# 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
S1 S 0.40880(3) 0.37230(3) 0.79005(4) 0.0263 1.0000 Uani . . . . . .
O2 O 0.50523(13) 0.46560(13) 0.74148(16) 0.0441 1.0000 Uani . . . . . .
O3 O 0.33827(14) 0.42963(12) 0.90236(13) 0.0400 1.0000 Uani . . . . . .
O4 O 0.31298(13) 0.30284(13) 0.67854(13) 0.0400 1.0000 Uani . . . . . .
C5 C 0.50651(12) 0.25261(12) 0.85900(13) 0.0229 1.0000 Uani . . . . . .
C6 C 0.44440(11) 0.14461(12) 0.91345(13) 0.0212 1.0000 Uani . . . . . .
C7 C 0.29924(12) 0.11936(13) 0.91245(15) 0.0256 1.0000 Uani . . . . . .
H71 H 0.2376 0.1763 0.8721 0.0500 1.0000 Uiso R . . . . .
C8 C 0.24273(12) 0.01613(13) 0.96825(15) 0.0257 1.0000 Uani . . . . . .
C9 C 0.67426(11) 0.07323(11) 0.96882(13) 0.0215 1.0000 Uani . . . . . .
C10 C 0.52974(11) 0.05499(11) 0.97062(12) 0.0197 1.0000 Uani . . . . . .
C11 C 0.72955(12) 0.17967(12) 0.90646(14) 0.0233 1.0000 Uani . . . . . .
C12 C 0.64669(12) 0.26834(12) 0.85425(14) 0.0258 1.0000 Uani . . . . . .
H121 H 0.6948 0.3396 0.8116 0.0500 1.0000 Uiso R . . . . .
S13 S 0.90714(3) 0.20368(3) 0.88755(4) 0.0282 1.0000 Uani . . . . . .
O14 O 0.94462(12) 0.08444(13) 0.81508(14) 0.0407 1.0000 Uani . . . . . .
O15 O 0.92066(13) 0.31537(16) 0.8101(2) 0.0615 1.0000 Uani . . . . . .
O16 O 0.97781(12) 0.23083(14) 1.02687(15) 0.0442 1.0000 Uani . . . . . .
O17 O 0.0865(4) 0.1247(5) 0.5605(3) 0.1337 1.0000 Uani . . . . . .
N18 N 0.09668(15) 0.53743(14) 0.81667(17) 0.0383 1.0000 Uani . . . . . .
H183 H 0.1695 0.5138 0.8553 0.0500 1.0000 Uiso R . . . . .
H302 H 0.3895 0.4305 0.3893 0.0500 1.0000 Uiso R . . . . .
H321 H 0.3221 0.3786 0.1610 0.0500 1.0000 Uiso R . . . . .
H301 H 0.3282 0.3361 0.4862 0.0500 1.0000 Uiso R . . . . .
H81 H 0.1535 0.0011 0.9693 0.0500 1.0000 Uiso R . . . . .
H331 H 0.1217 0.1474 0.2305 0.0500 1.0000 Uiso R . . . . .
H322 H 0.2096 0.2902 0.0966 0.0500 1.0000 Uiso R . . . . .
H332 H 0.1486 0.1821 0.3986 0.0500 1.0000 Uiso R . . . . .
H171 H 0.1551 0.1789 0.5960 0.1580 1.0000 Uiso R . . . . .
H182 H 0.0417 0.4741 0.8225 0.0500 1.0000 Uiso R . . . . .
H181 H 0.0732 0.6057 0.8644 0.0500 1.0000 Uiso R . . . . .
C31 C 0.24946(18) 0.29699(16) 0.28980(17) 0.0367 1.0000 Uani . . . . . .
N32 N 0.2579(2) 0.3380(2) 0.16771(17) 0.0513 1.0000 Uani . . . . . .
N33 N 0.1592(2) 0.1983(2) 0.3029(2) 0.0594 1.0000 Uani . . . . . .
H172 H 0.0456 0.1130 0.6322 0.1580 1.0000 Uiso R . . . . .
C191 C 0.1231(4) 0.5797(4) 0.6841(4) 0.0379 0.5000 Uani . U . . 1 .
N30 N 0.3272(2) 0.35907(19) 0.39842(17) 0.0519 1.0000 Uani . . . . 1 .
H1911 H 0.0416 0.6053 0.6393 0.0463 0.5000 Uiso R . . . 1 .
H2011 H 0.1941 0.7638 0.7615 0.0603 0.5000 Uiso R . . . 1 .
H2012 H 0.3071 0.6680 0.7587 0.0603 0.5000 Uiso R . . . 1 .
C211 C 0.2689(7) 0.7414(5) 0.5771(7) 0.0604 0.5000 Uani . U . . 1 .
H2111 H 0.1911 0.7641 0.5233 0.0788 0.5000 Uiso R . . . 1 .
H2112 H 0.3097 0.6746 0.5255 0.0788 0.5000 Uiso R . . . 1 .
C221 C 0.3727(7) 0.8597(5) 0.6110(6) 0.0595 0.5000 Uani . U . . 1 .
H1912 H 0.1545 0.5099 0.6278 0.0463 0.5000 Uiso R . . . 1 .
C201 C 0.2290(4) 0.6940(4) 0.7082(5) 0.0438 0.5000 Uani . U . . 1 .
C241 C 0.4260(7) 0.9158(6) 0.4833(6) 0.0660 0.5000 Uani . U . . 1 .
H2412 H 0.4695 0.8507 0.4322 0.0875 0.5000 Uiso R . . . 1 .
H2411 H 0.3519 0.9414 0.4263 0.0875 0.5000 Uiso R . . . 1 .
H2211 H 0.3294 0.9259 0.6608 0.0740 0.5000 Uiso R . . . 1 .
H2212 H 0.4476 0.8360 0.6682 0.0740 0.5000 Uiso R . . . 1 .
H1921 H -0.0131 0.5828 0.6487 0.0711 0.5000 Uiso R . . . 2 .
C212 C 0.2371(7) 0.7263(7) 0.6491(9) 0.0741 0.5000 Uani . U . . 2 .
H2022 H 0.1266 0.6088 0.5019 0.0974 0.5000 Uiso R . . . 2 .
H2021 H 0.2373 0.5400 0.5823 0.0974 0.5000 Uiso R . . . 2 .
C222 C 0.3160(9) 0.7882(8) 0.5469(8) 0.0769 0.5000 Uani . U . . 2 .
H2221 H 0.2519 0.8084 0.4755 0.0920 0.5000 Uiso R . . . 2 .
H2222 H 0.3706 0.7240 0.5104 0.0920 0.5000 Uiso R . . . 2 .
C232 C 0.4093(8) 0.9078(9) 0.5929(7) 0.0760 0.5000 Uani . U . . 2 .
H2321 H 0.3575 0.9708 0.6365 0.0905 0.5000 Uiso R . . . 2 .
H2322 H 0.4794 0.8870 0.6579 0.0905 0.5000 Uiso R . . . 2 .
H2121 H 0.1707 0.7827 0.6762 0.1585 0.5000 Uiso R . . . 2 .
H2122 H 0.2977 0.7154 0.7275 0.1585 0.5000 Uiso R . . . 2 .
C192 C 0.0665(7) 0.5382(6) 0.6629(6) 0.0602 0.5000 Uani . U . . 2 .
C242 C 0.4742(8) 0.9681(7) 0.4769(7) 0.0773 0.5000 Uani . U . . 2 .
H1922 H 0.0478 0.4494 0.6228 0.0711 0.5000 Uiso R . . . 2 .
C202 C 0.1688(9) 0.5989(7) 0.5909(8) 0.0828 0.5000 Uani . U . . 2 .
H2421 H 0.4026 0.9926 0.4159 0.1462 0.5000 Uiso R . . . 2 .
H2422 H 0.5190 0.9012 0.4301 0.1462 0.5000 Uiso R . . . 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.238(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
S1 . O2 . 1.4466(12) yes
S1 . O3 . 1.4583(13) yes
S1 . O4 . 1.4551(13) yes
S1 . C5 . 1.7787(12) yes
C5 . C6 . 1.4063(16) yes
C5 . C12 . 1.3872(16) yes
C6 . C7 . 1.4351(16) yes
C6 . C10 . 1.4245(15) yes
C7 . H71 . 0.967 no
C7 . C8 . 1.3522(17) yes
C8 . C9 2_657 1.4328(16) yes
C8 . H81 . 0.883 no
C9 . C10 . 1.4268(15) yes
C9 . C11 . 1.4090(16) yes
C10 . C10 2_657 1.434(2) yes
C11 . C12 . 1.3830(17) yes
C11 . S13 . 1.7823(12) yes
C12 . H121 . 0.994 no
S13 . O14 . 1.4446(13) yes
S13 . O15 . 1.4502(14) yes
S13 . O16 . 1.4601(14) yes
O17 . H171 . 0.860 no
O17 . H172 . 0.860 no
N18 . H183 . 0.847 no
N18 . H182 . 0.824 no
N18 . H181 . 0.862 no
N18 . C191 . 1.457(4) yes
H302 . N30 . 0.936 no
H321 . N32 . 0.743 no
H301 . N30 . 0.917 no
H331 . N33 . 0.867 no
H322 . N32 . 0.881 no
H332 . N33 . 0.986 no
C31 . N32 . 1.321(2) yes
C31 . N33 . 1.319(2) yes
C31 . N30 . 1.320(2) yes
C191 . H1911 . 0.950 no
C191 . H1912 . 0.950 no
C191 . C201 . 1.489(6) yes
H2011 . C201 . 0.950 no
H2012 . C201 . 0.950 no
C211 . H2111 . 0.950 no
C211 . H2112 . 0.950 no
C211 . C221 . 1.509(7) yes
C211 . C201 . 1.502(8) yes
C221 . C241 . 1.556(8) yes
C221 . H2211 . 0.950 no
C221 . H2212 . 0.950 no
C241 . H2412 . 0.950 no
C241 . H2411 . 0.950 no
H1921 . C192 . 0.950 no
C212 . C222 . 1.493(11) yes
C212 . H2121 . 0.950 no
C212 . H2122 . 0.950 no
C212 . C202 . 1.453(9) yes
H2022 . C202 . 0.950 no
H2021 . C202 . 0.950 no
C222 . H2221 . 0.950 no
C222 . H2222 . 0.950 no
C222 . C232 . 1.475(10) yes
C232 . H2321 . 0.950 no
C232 . H2322 . 0.950 no
C232 . C242 . 1.525(9) yes
C192 . H1922 . 0.950 no
C192 . C202 . 1.429(9) yes
C242 . C242 2_676 0.855(12) yes
C242 . H2421 . 0.950 no
C242 . H2422 . 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
O2 . S1 . O3 . 113.30(9) yes
O2 . S1 . O4 . 112.26(8) yes
O3 . S1 . O4 . 111.53(8) yes
O2 . S1 . C5 . 106.22(6) yes
O3 . S1 . C5 . 106.29(7) yes
O4 . S1 . C5 . 106.68(7) yes
S1 . C5 . C6 . 121.59(9) yes
S1 . C5 . C12 . 117.30(9) yes
C6 . C5 . C12 . 121.09(11) yes
C5 . C6 . C7 . 123.19(10) yes
C5 . C6 . C10 . 118.35(10) yes
C7 . C6 . C10 . 118.46(10) yes
C6 . C7 . H71 . 121.1 no
C6 . C7 . C8 . 121.78(11) yes
H71 . C7 . C8 . 117.1 no
C9 2_657 C8 . C7 . 121.23(11) yes
C9 2_657 C8 . H81 . 116.7 no
C7 . C8 . H81 . 122.1 no
C8 2_657 C9 . C10 . 118.85(10) yes
C8 2_657 C9 . C11 . 122.71(10) yes
C10 . C9 . C11 . 118.44(10) yes
C10 2_657 C10 . C9 . 119.65(12) yes
C10 2_657 C10 . C6 . 119.94(12) yes
C9 . C10 . C6 . 120.41(10) yes
C9 . C11 . C12 . 120.92(11) yes
C9 . C11 . S13 . 121.81(9) yes
C12 . C11 . S13 . 117.25(9) yes
C5 . C12 . C11 . 120.67(11) yes
C5 . C12 . H121 . 124.2 no
C11 . C12 . H121 . 115.1 no
C11 . S13 . O14 . 107.54(6) yes
C11 . S13 . O15 . 104.88(7) yes
O14 . S13 . O15 . 113.01(11) yes
C11 . S13 . O16 . 106.32(7) yes
O14 . S13 . O16 . 111.96(8) yes
O15 . S13 . O16 . 112.51(11) yes
H171 . O17 . H172 . 101.0 no
H183 . N18 . H182 . 101.4 no
H183 . N18 . H181 . 109.9 no
H182 . N18 . H181 . 109.0 no
H183 . N18 . C191 . 109.1 no
H182 . N18 . C191 . 121.8 no
H181 . N18 . C191 . 105.5 no
N32 . C31 . N33 . 119.65(18) yes
N32 . C31 . N30 . 119.54(16) yes
N33 . C31 . N30 . 120.74(17) yes
H322 . N32 . C31 . 116.9 no
H322 . N32 . H321 . 122.4 no
C31 . N32 . H321 . 115.1 no
H332 . N33 . C31 . 115.1 no
H332 . N33 . H331 . 124.4 no
C31 . N33 . H331 . 120.0 no
N18 . C191 . H1911 . 109.8 no
N18 . C191 . H1912 . 109.8 no
H1911 . C191 . H1912 . 109.5 no
N18 . C191 . C201 . 108.7(3) yes
H1911 . C191 . C201 . 109.2 no
H1912 . C191 . C201 . 109.8 no
H302 . N30 . H301 . 114.5 no
H302 . N30 . C31 . 120.6 no
H301 . N30 . C31 . 124.8 no
H2111 . C211 . H2112 . 109.5 no
H2111 . C211 . C221 . 109.6 no
H2112 . C211 . C221 . 108.1 no
H2111 . C211 . C201 . 110.4 no
H2112 . C211 . C201 . 109.8 no
C221 . C211 . C201 . 109.5(5) yes
C211 . C221 . C241 . 114.6(5) yes
C211 . C221 . H2211 . 106.8 no
C241 . C221 . H2211 . 108.5 no
C211 . C221 . H2212 . 108.2 no
C241 . C221 . H2212 . 109.2 no
H2211 . C221 . H2212 . 109.5 no
C211 . C201 . C191 . 113.0(4) yes
C211 . C201 . H2012 . 109.3 no
C191 . C201 . H2012 . 107.8 no
C211 . C201 . H2011 . 108.8 no
C191 . C201 . H2011 . 108.4 no
H2012 . C201 . H2011 . 109.5 no
C221 . C241 . H2412 . 109.6 no
C221 . C241 . H2411 . 109.8 no
H2412 . C241 . H2411 . 109.5 no
C222 . C212 . H2121 . 108.5 no
C222 . C212 . H2122 . 109.2 no
H2121 . C212 . H2122 . 109.5 no
C222 . C212 . C202 . 111.4(7) yes
H2121 . C212 . C202 . 109.2 no
H2122 . C212 . C202 . 109.0 no
C212 . C222 . H2221 . 107.4 no
C212 . C222 . H2222 . 106.7 no
H2221 . C222 . H2222 . 109.5 no
C212 . C222 . C232 . 119.4(6) yes
H2221 . C222 . C232 . 107.4 no
H2222 . C222 . C232 . 106.3 no
C222 . C232 . H2321 . 107.3 no
C222 . C232 . H2322 . 108.4 no
H2321 . C232 . H2322 . 109.5 no
C222 . C232 . C242 . 114.2(6) yes
H2321 . C232 . C242 . 108.3 no
H2322 . C232 . C242 . 109.0 no
N18 . C192 . H1921 . 106.8 no
N18 . C192 . H1922 . 107.4 no
H1921 . C192 . H1922 . 109.5 no
N18 . C192 . C202 . 118.1(6) yes
H1921 . C192 . C202 . 107.3 no
H1922 . C192 . C202 . 107.6 no
C232 . C242 . C242 2_676 100.4(10) yes
C232 . C242 . H2421 . 107.6 no
C242 2_676 C242 . H2421 . 115.3 no
C232 . C242 . H2422 . 106.7 no
C242 2_676 C242 . H2422 . 116.3 no
H2421 . C242 . H2422 . 109.5 no
C212 . C202 . C192 . 118.9(7) yes
C212 . C202 . H2022 . 107.1 no
C192 . C202 . H2022 . 107.0 no
C212 . C202 . H2021 . 107.3 no
C192 . C202 . H2021 . 106.9 no
H2022 . C202 . H2021 . 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
N18 . H183 . O3 . 165.82(6) 0.847 1.981 2.810(6) yes
N30 . H302 . O2 2_666 147.18(6) 0.936 2.062 2.893(6) yes
N32 . H321 . O2 2_666 149.05(6) 0.743 2.298 2.960(6) yes
N30 . H301 . O4 . 172.71(8) 0.917 1.973 2.885(6) yes
N33 . H331 . O14 2_656 133.58(7) 0.867 2.402 3.065(6) yes
N32 . H322 . O16 1_454 135.94(6) 0.881 2.336 3.031(6) yes
N33 . H332 . O17 . 165.14(11) 0.986 1.894 2.858(6) yes
O17 . H171 . O4 . 179.66(11) 0.860 1.977 2.837(6) yes
N18 . H182 . O15 1_455 171.49(8) 0.824 1.927 2.744(6) yes
N18 . H181 . O16 2_667 178.22(6) 0.862 2.021 2.882(6) yes
O17 . H172 . O14 1_455 179.32(9) 0.860 2.173 3.033(6) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 10/06/14 at 14:40:03
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE N   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE N   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE N   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE N   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S)  H   ( 183,X'S) 
RIDE C   (  191,X'S) H   ( 1911,X'S) H   ( 1912,X'S) 
RIDE C   (  201,X'S) H   ( 2011,X'S) H   ( 2012,X'S) 
RIDE C   (  211,X'S) H   ( 2111,X'S) H   ( 2112,X'S) 
RIDE C   (  221,X'S) H   ( 2211,X'S) H   ( 2212,X'S) 
RIDE C   (  192,X'S) H   ( 1921,X'S) H   ( 1922,X'S)
RIDE C   (  202,X'S) H   ( 2021,X'S) H   ( 2022,X'S) 
RIDE C   (  212,X'S) H   ( 2121,X'S) H   ( 2122,X'S)
RIDE C   (  222,X'S) H   ( 2221,X'S) H   ( 2222,X'S) 
RIDE C   (  232,X'S) H   ( 2321,X'S) H   ( 2322,X'S) 
RIDE C   (  241,X'S) H   ( 2411,X'S) H   ( 2412,X'S) 
RIDE C   (  242,X'S) H   ( 2421,X'S) H   ( 2422,X'S) 
RIDE O(17,X'S) H(171,X'S) H(172,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 10/06/14 at 14:40:03
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.02 = C(191) TO C(192), C(201) TO C(202), C(211) TO C(212), 
CONT C(221) TO C(222), C(241) TO C(242), C(232) TO C(241), C(232) TO C(222) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# start Validation Reply Form
_vrf_PLAT417_1                   
;
PROBLEM: Short Inter D-H..H-D       H171   ..  H332    ..       1.94 Ang.
RESPONSE: This is caused by the disorder in the chains; it explains also
other C-alerts
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 986091'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_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                   9.7985(3)
_cell_length_b                   9.8928(3)
_cell_length_c                   10.2589(4)
_cell_angle_alpha                94.489(3)
_cell_angle_beta                 97.927(3)
_cell_angle_gamma                95.090(3)
_cell_volume                     976.92(6)
_cell_measurement_reflns_used    11991
_cell_measurement_theta_min      2.0400
_cell_measurement_theta_max      32.7610
_cell_oxdiff_length_a            9.7985(3)
_cell_oxdiff_length_b            9.8928(3)
_cell_oxdiff_length_c            10.2589(4)
_cell_oxdiff_angle_alpha         94.490(3)
_cell_oxdiff_angle_beta          97.927(3)
_cell_oxdiff_angle_gamma         95.090(3)
_cell_oxdiff_volume              976.93(6)

_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 0.0033 0.0016 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 0.0061 0.0033 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 0.0106 0.0060 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 0.1246 0.1234 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'
Nap1 0.0300 0.0250 3.2565 2.6671 3.9362 6.1153 1.3998 0.2001 1.0032 14.0390
0.4040 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            1

_chemical_formula_sum            'C30 H52 N8 O14 S4'
_chemical_formula_moiety         
'C12 H30 N2, C16 H6 O12 S4, 2(C H6 N3), 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         877.08


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.300
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_max          0.700
_exptl_absorpt_correction_T_min  0.95880
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             463.805
_exptl_absorpt_coefficient_mu    0.319
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 16.0143

_diffrn_measurement_device       Area
_diffrn_radiation_wavelength     0.71073
#montpellier_reflns_maxres is minimum d (highest resolution)
#where <I/sigI> <= 2.0
#(Z. Dauter, Acta Cryst. D55, 1703-1717, 1999)
_montpellier_reflns_maxres       0.66
_montpellier_reflns_completeness_maxres 93.94
_montpellier_reflns_redundancy_maxres 5.20

#montpellier_diffrn_reflns_class_completeness_shell is completeness in shell
#montpellier_diffrn_class_reflns_cumul_completeness is cumulative
#completeness to resolution of shell
#Note: completeness percentage takes into account the fact whether
#group is centrosymmetric or not
loop_
_montpellier_diffrn_reflns_class_number
_montpellier_diffrn_reflns_class_d_res_high
_montpellier_diffrn_reflns_class_d_res_low
_montpellier_diffrn_reflns_class_redundancy
_montpellier_diffrn_reflns_class_av_I/uI
_diffrn_reflns_class_av_R_eq
_montpellier_diffrn_reflns_class_completeness_shell
_montpellier_diffrn_reflns_class_cumul_completeness
0 100.0 1.45 8.0 79.14 0.034 100.0 100.00
1 1.45 1.15 7.2 47.88 0.028 100.0 100.00
2 1.15 1.00 6.5 35.29 0.034 100.0 100.00
3 1.00 0.91 5.8 25.13 0.045 100.0 100.00
4 0.91 0.85 5.3 20.23 0.054 100.0 100.00
5 0.85 0.80 4.9 16.94 0.060 100.0 100.00
6 0.80 0.75 4.5 13.44 0.072 100.0 100.00
7 0.75 0.72 4.2 13.20 0.070 100.0 100.00
8 0.72 0.69 3.8 10.40 0.086 99.7 99.97
9 0.69 0.66 1.7 7.07 0.085 61.2 93.94
#End reflection statistics
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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_orient_matrix_UB_11      0.0185242000
_diffrn_orient_matrix_UB_12      -0.0073150000
_diffrn_orient_matrix_UB_13      -0.0644365000
_diffrn_orient_matrix_UB_21      -0.0099762000
_diffrn_orient_matrix_UB_22      -0.0719131000
_diffrn_orient_matrix_UB_23      -0.0001654000
_diffrn_orient_matrix_UB_31      -0.0703835000
_diffrn_orient_matrix_UB_32      0.0006634000
_diffrn_orient_matrix_UB_33      -0.0276089000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -42.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955    0.0000  -60.0000 134

#__ type_ start__ end____ width___ exp.time_
  2 omega  -60.00  -11.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330   92.0000 -124.0000 49

#__ type_ start__ end____ width___ exp.time_
  3 omega  -92.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -77.0000  -60.0000 93

#__ type_ start__ end____ width___ exp.time_
  4 omega  -31.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -77.0000  120.0000 33

#__ type_ start__ end____ width___ exp.time_
  5 omega  -60.00   -3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330   92.0000   55.0000 57

#__ type_ start__ end____ width___ exp.time_
  6 omega  -91.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -38.0000   90.0000 70

#__ type_ start__ end____ width___ exp.time_
  7 omega   34.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  179.0000 -120.0000 62

#__ type_ start__ end____ width___ exp.time_
  8 omega   34.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  179.0000   30.0000 62

#__ type_ start__ end____ width___ exp.time_
  9 omega  -92.00   -8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -57.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 10 omega  -92.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -77.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
 11 omega  -94.00   -6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.8330  -38.0000    0.0000 88

#__ type_ start__ end____ width___ exp.time_
 12 omega    7.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955   57.0000  150.0000 84

#__ type_ start__ end____ width___ exp.time_
 13 omega  -25.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  -99.0000 -120.0000 88

#__ type_ start__ end____ width___ exp.time_
 14 omega  -43.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  -57.0000   90.0000 84

#__ type_ start__ end____ width___ exp.time_
 15 omega    7.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955   57.0000  -60.0000 84

#__ type_ start__ end____ width___ exp.time_
 16 omega  -25.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  -99.0000   30.0000 88

#__ type_ start__ end____ width___ exp.time_
 17 omega  -25.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       23.8955  -99.0000  150.0000 75

;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            35243
_reflns_number_total             6778
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0433
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 6778
# Theoretical number of reflections is about 14439 


_diffrn_reflns_theta_min         2.013
_diffrn_reflns_theta_max         32.752
_diffrn_measured_fraction_theta_max 0.939

_diffrn_reflns_theta_full        28.822
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              -15
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              15

_oxford_diffrn_Wilson_B_factor   1.22
_oxford_diffrn_Wilson_scale      0.01

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

_refine_diff_density_min         -0.61
_refine_diff_density_max         1.01


# 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>2.0\s(I)
_refine_ls_number_reflns         5973
_refine_ls_number_restraints     199
_refine_ls_number_parameters     299
_oxford_refine_ls_R_factor_ref   0.0404
_refine_ls_wR_factor_ref         0.0494
_refine_ls_goodness_of_fit_ref   1.0533
_refine_ls_shift/su_max          0.0007422
_refine_ls_shift/su_mean         0.0000395


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6778
_refine_ls_R_factor_all          0.0470
_refine_ls_wR_factor_all         0.0562

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5973
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_gt          0.0494

# 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 F
_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: 
 14.7 13.7 13.3 4.41 
;

# 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
H211 H 0.3717 0.8414 0.8136 0.0500 1.0000 Uiso R . . . . .
H212 H 0.3765 0.9727 0.8822 0.0500 1.0000 Uiso R . . . . .
H261 H 0.3083 0.5365 0.1605 0.0434 0.687(3) Uiso R . P . 2 .
H262 H 0.3007 0.6762 0.1023 0.0434 0.687(3) Uiso R . P . 2 .
H281 H 0.6221 0.5903 0.0137 0.0452 0.687(3) Uiso R . P . 2 .
H282 H 0.4780 0.6269 -0.0481 0.0452 0.687(3) Uiso R . P . 2 .
H271 H 0.5364 0.7298 0.1655 0.0482 0.687(3) Uiso R . P . 2 .
H272 H 0.5465 0.5878 0.2183 0.0482 0.687(3) Uiso R . P . 2 .
H321 H 0.4997 0.5605 0.2098 0.0611 0.313(3) Uiso R . P . 1 .
H322 H 0.3472 0.5881 0.1679 0.0611 0.313(3) Uiso R . P . 1 .
H331 H 0.3789 0.5441 -0.0527 0.0625 0.313(3) Uiso R . P . 1 .
H332 H 0.3921 0.4182 0.0275 0.0625 0.313(3) Uiso R . P . 1 .
H241 H 0.4482 0.8661 0.3125 0.0431 0.687(3) Uiso R . P . 2 .
H242 H 0.2981 0.8834 0.2499 0.0431 0.687(3) Uiso R . P . 2 .
H301 H 0.5174 0.7704 0.3602 0.0311 0.313(3) Uiso R . P . 1 .
H302 H 0.5208 0.9104 0.3016 0.0311 0.313(3) Uiso R . P . 1 .
H291 H 0.2989 0.7143 0.3514 0.0352 0.313(3) Uiso R . P . 1 .
H292 H 0.2561 0.8223 0.2560 0.0352 0.313(3) Uiso R . P . 1 .
C1 C 0.03100(10) 0.75623(9) 0.98044(9) 0.0155 1.0000 Uani . . . . . .
C2 C 0.08625(10) 0.69816(9) 0.87833(9) 0.0158 1.0000 Uani . . . . . .
C3 C 0.08513(9) 0.55339(8) 0.85535(8) 0.0124 1.0000 Uani . . . . . .
C4 C 0.13920(9) 0.49001(9) 0.74860(8) 0.0131 1.0000 Uani . . . . . .
C5 C 0.14353(9) 0.34970(9) 0.73427(9) 0.0141 1.0000 Uani . . . . . .
C6 C 0.09222(9) 0.26851(8) 0.82423(8) 0.0128 1.0000 Uani . . . . . .
C7 C 0.03091(9) 0.32515(8) 0.92964(8) 0.0121 1.0000 Uani . . . . . .
C8 C 0.02919(8) 0.46926(8) 0.94576(8) 0.0115 1.0000 Uani . . . . . .
S9 S 0.20630(2) 0.58522(2) 0.62753(2) 0.0145 1.0000 Uani . . . . . .
O10 O 0.09236(8) 0.65510(8) 0.56637(8) 0.0227 1.0000 Uani . . . . . .
O11 O 0.31949(8) 0.68101(8) 0.69775(8) 0.0226 1.0000 Uani . . . . . .
O12 O 0.25499(9) 0.48650(8) 0.53687(8) 0.0239 1.0000 Uani . . . . . .
S13 S 0.11085(2) 0.09101(2) 0.80291(2) 0.0143 1.0000 Uani . . . . . .
O14 O 0.18679(11) 0.07564(8) 0.69110(9) 0.0308 1.0000 Uani . . . . . .
O15 O 0.18493(9) 0.05409(8) 0.92463(8) 0.0227 1.0000 Uani . . . . . .
O16 O -0.02982(8) 0.02109(8) 0.77243(8) 0.0230 1.0000 Uani . . . . . .
N17 N -0.17195(10) 0.74628(12) 0.65748(11) 0.0296 1.0000 Uani . . . . . .
N18 N -0.40403(10) 0.67630(12) 0.63177(11) 0.0290 1.0000 Uani . . . . . .
N19 N -0.30751(12) 0.84053(12) 0.79893(11) 0.0317 1.0000 Uani . . . . . .
C20 C -0.29453(11) 0.75351(11) 0.69756(10) 0.0204 1.0000 Uani . . . . . .
O21 O 0.43529(17) 0.9072(2) 0.8752(2) 0.0834 1.0000 Uani . . . . . .
N22 N 0.17690(10) 0.90212(9) 0.46786(9) 0.0226 1.0000 Uani . U . . . .
C23 C 0.32446(13) 0.91039(12) 0.44965(12) 0.0266 1.0000 Uani . U . . . .
C24 C 0.3525(3) 0.8445(3) 0.3189(3) 0.0323 0.687(3) Uani . U P . 2 .
C25 C 0.3197(2) 0.6943(2) 0.3028(2) 0.0321 0.687(3) Uani . U P . 2 .
C26 C 0.3479(2) 0.6296(2) 0.1696(2) 0.0358 0.687(3) Uani . U P . 2 .
C27 C 0.4982(3) 0.6361(3) 0.1522(2) 0.0376 0.687(3) Uani . U P . 2 .
C28 C 0.5214(3) 0.5760(2) 0.0153(2) 0.0393 0.687(3) Uani . U P . 2 .
C29 C 0.3216(6) 0.8046(6) 0.3282(6) 0.0278 0.313(3) Uani . U P . 1 .
C30 C 0.4731(4) 0.8198(4) 0.2947(4) 0.0270 0.313(3) Uani . U P . 1 .
C31 C 0.4833(5) 0.7510(5) 0.1585(4) 0.0357 0.313(3) Uani . U P . 1 .
C32 C 0.4344(8) 0.5948(7) 0.1438(6) 0.0482 0.313(3) Uani . U P . 1 .
C33 C 0.4330(7) 0.5066(8) 0.0170(7) 0.0582 0.313(3) Uani . U P . 1 .
H51 H 0.1784 0.3073 0.6633 0.0500 1.0000 Uiso R . . . . .
H21 H 0.1293 0.7597 0.8184 0.0500 1.0000 Uiso R . . . . .
H11 H 0.0350 0.8554 0.9953 0.0500 1.0000 Uiso R . . . . .
H181 H -0.4830 0.6750 0.6542 0.0500 1.0000 Uiso R . . . . .
H182 H -0.3942 0.6222 0.5655 0.0500 1.0000 Uiso R . . . . .
H191 H -0.2360 0.8922 0.8468 0.0500 1.0000 Uiso R . . . . .
H192 H -0.3782 0.8466 0.8199 0.0500 1.0000 Uiso R . . . . .
H172 H -0.1574 0.6819 0.5974 0.0500 1.0000 Uiso R . . . . .
H171 H -0.0996 0.7966 0.6974 0.0500 1.0000 Uiso R . . . . .
H311 H 0.5673 0.7925 0.1310 0.0444 0.313(3) Uiso R . P . 1 .
H312 H 0.4071 0.7692 0.0993 0.0444 0.313(3) Uiso R . P . 1 .
H252 H 0.2251 0.6702 0.3113 0.0386 0.687(3) Uiso R . P . 2 .
H251 H 0.3771 0.6571 0.3712 0.0386 0.687(3) Uiso R . P . 2 .
H222 H 0.1230 0.9271 0.3958 0.0500 1.0000 Uiso R . . . . .
H221 H 0.1439 0.8209 0.4821 0.0500 1.0000 Uiso R . . . . .
H223 H 0.1589 0.9528 0.5293 0.0500 1.0000 Uiso R . . . . .
H231 H 0.3568 0.9993 0.4312 0.0319 0.313(3) Uiso R . P . 1 .
H232 H 0.3807 0.8856 0.5253 0.0319 0.313(3) Uiso R . P . 1 .
H233 H 0.3587 1.0039 0.4563 0.0319 0.687(3) Uiso R . P . 2 .
H234 H 0.3732 0.8670 0.5186 0.0319 0.687(3) Uiso R . P . 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          5.974(10)
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
H211 . O21 . 0.983 no
H212 . O21 . 0.910 no
H261 . C26 . 0.959 no
H262 . C26 . 0.950 no
H281 . C28 . 0.986 no
H282 . C28 . 0.933 no
H271 . C27 . 0.960 no
H272 . C27 . 0.957 no
H321 . C32 . 0.968 no
H322 . C32 . 0.920 no
H331 . C33 . 0.950 no
H332 . C33 . 0.950 no
H241 . C24 . 0.955 no
H242 . C24 . 0.953 no
H301 . C30 . 0.941 no
H302 . C30 . 0.966 no
H291 . C29 . 0.958 no
H292 . C29 . 0.949 no
C1 . C7 2_567 1.4322(12) yes
C1 . C2 . 1.3556(12) yes
C1 . H11 . 0.977 no
C2 . C3 . 1.4319(12) yes
C2 . H21 . 1.006 no
C3 . C4 . 1.4087(11) yes
C3 . C8 . 1.4261(12) yes
C4 . C5 . 1.3894(12) yes
C4 . S9 . 1.7778(9) yes
C5 . C6 . 1.3864(12) yes
C5 . H51 . 0.932 no
C6 . C7 . 1.4101(11) yes
C6 . S13 . 1.7811(9) yes
C7 . C8 . 1.4242(11) yes
C8 . C8 2_567 1.4377(16) yes
S9 . O10 . 1.4594(8) yes
S9 . O11 . 1.4607(8) yes
S9 . O12 . 1.4523(8) yes
S13 . O14 . 1.4563(8) yes
S13 . O15 . 1.4450(8) yes
S13 . O16 . 1.4677(8) yes
N17 . C20 . 1.3281(14) yes
N17 . H172 . 0.886 no
N17 . H171 . 0.862 no
N18 . C20 . 1.3282(13) yes
N18 . H181 . 0.836 no
N18 . H182 . 0.854 no
N19 . C20 . 1.3246(14) yes
N19 . H191 . 0.892 no
N19 . H192 . 0.759 no
N22 . C23 . 1.4792(16) yes
N22 . H222 . 0.911 no
N22 . H221 . 0.870 no
N22 . H223 . 0.822 no
C23 . C29 . 1.559(5) yes
C23 . H231 . 0.950 no
C23 . H232 . 0.950 no
C24 . C25 . 1.483(4) yes
C25 . C26 . 1.534(3) yes
C25 . H252 . 0.954 no
C25 . H251 . 0.955 no
C26 . C27 . 1.504(3) yes
C27 . C28 . 1.536(3) yes
C28 . C28 2_665 1.522(5) yes
C29 . C30 . 1.567(7) yes
C30 . C31 . 1.525(5) yes
C31 . C32 . 1.567(9) yes
C31 . H311 . 0.973 no
C31 . H312 . 0.936 no
C32 . C33 . 1.506(8) yes
C33 . C33 2_665 1.418(12) 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
C7 2_567 C1 . C2 . 121.19(8) yes
C7 2_567 C1 . H11 . 118.6 no
C2 . C1 . H11 . 120.2 no
C1 . C2 . C3 . 121.70(8) yes
C1 . C2 . H21 . 118.2 no
C3 . C2 . H21 . 120.1 no
C2 . C3 . C4 . 122.99(8) yes
C2 . C3 . C8 . 118.71(8) yes
C4 . C3 . C8 . 118.29(8) yes
C3 . C4 . C5 . 121.15(8) yes
C3 . C4 . S9 . 121.81(6) yes
C5 . C4 . S9 . 117.04(6) yes
C4 . C5 . C6 . 120.39(8) yes
C4 . C5 . H51 . 121.4 no
C6 . C5 . H51 . 118.2 no
C5 . C6 . C7 . 121.14(8) yes
C5 . C6 . S13 . 117.14(6) yes
C7 . C6 . S13 . 121.70(7) yes
C1 2_567 C7 . C6 . 122.76(8) yes
C1 2_567 C7 . C8 . 118.91(7) yes
C6 . C7 . C8 . 118.33(8) yes
C8 2_567 C8 . C3 . 119.60(9) yes
C8 2_567 C8 . C7 . 119.80(9) yes
C3 . C8 . C7 . 120.60(7) yes
C4 . S9 . O10 . 106.31(4) yes
C4 . S9 . O11 . 106.62(4) yes
O10 . S9 . O11 . 111.89(5) yes
C4 . S9 . O12 . 105.87(4) yes
O10 . S9 . O12 . 113.64(5) yes
O11 . S9 . O12 . 111.90(5) yes
C6 . S13 . O14 . 104.81(4) yes
C6 . S13 . O15 . 107.54(4) yes
O14 . S13 . O15 . 113.35(6) yes
C6 . S13 . O16 . 106.43(4) yes
O14 . S13 . O16 . 111.59(6) yes
O15 . S13 . O16 . 112.49(5) yes
C20 . N17 . H172 . 122.1 no
C20 . N17 . H171 . 121.0 no
H172 . N17 . H171 . 116.3 no
C20 . N18 . H181 . 123.1 no
C20 . N18 . H182 . 119.6 no
H181 . N18 . H182 . 117.3 no
C20 . N19 . H191 . 123.2 no
C20 . N19 . H192 . 119.9 no
H191 . N19 . H192 . 116.9 no
N18 . C20 . N17 . 119.16(10) yes
N18 . C20 . N19 . 120.77(10) yes
N17 . C20 . N19 . 120.03(10) yes
H211 . O21 . H212 . 97.3 no
C23 . N22 . H222 . 111.4 no
C23 . N22 . H221 . 113.1 no
H222 . N22 . H221 . 107.5 no
C23 . N22 . H223 . 115.4 no
H222 . N22 . H223 . 103.6 no
H221 . N22 . H223 . 105.1 no
N22 . C23 . C29 . 102.0(2) yes
N22 . C23 . H231 . 111.3 no
C29 . C23 . H231 . 111.3 no
N22 . C23 . H232 . 111.3 no
C29 . C23 . H232 . 111.3 no
H231 . C23 . H232 . 109.5 no
C23 . C24 . H241 . 108.1 no
C23 . C24 . H242 . 107.9 no
H241 . C24 . H242 . 108.7 no
C23 . C24 . C25 . 113.6(2) yes
H241 . C24 . C25 . 109.2 no
H242 . C24 . C25 . 109.1 no
C24 . C25 . C26 . 112.86(19) yes
C24 . C25 . H252 . 110.6 no
C26 . C25 . H252 . 108.7 no
C24 . C25 . H251 . 107.9 no
C26 . C25 . H251 . 108.0 no
H252 . C25 . H251 . 108.7 no
C25 . C26 . H261 . 107.3 no
C25 . C26 . H262 . 107.5 no
H261 . C26 . H262 . 108.7 no
C25 . C26 . C27 . 114.96(18) yes
H261 . C26 . C27 . 110.1 no
H262 . C26 . C27 . 108.2 no
C26 . C27 . H271 . 108.4 no
C26 . C27 . H272 . 109.0 no
H271 . C27 . H272 . 108.1 no
C26 . C27 . C28 . 113.3(2) yes
H271 . C27 . C28 . 109.0 no
H272 . C27 . C28 . 108.9 no
C27 . C28 . C28 2_665 115.2(2) yes
C27 . C28 . H281 . 106.0 no
C28 2_665 C28 . H281 . 107.1 no
C27 . C28 . H282 . 108.2 no
C28 2_665 C28 . H282 . 112.1 no
H281 . C28 . H282 . 107.8 no
C23 . C29 . H291 . 110.3 no
C23 . C29 . H292 . 111.5 no
H291 . C29 . H292 . 108.9 no
C23 . C29 . C30 . 104.4(4) yes
H291 . C29 . C30 . 109.9 no
H292 . C29 . C30 . 111.8 no
C29 . C30 . H302 . 118.0 no
C29 . C30 . H301 . 100.2 no
H302 . C30 . H301 . 108.9 no
C29 . C30 . C31 . 112.2(4) yes
H302 . C30 . C31 . 107.8 no
H301 . C30 . C31 . 109.4 no
C30 . C31 . C32 . 113.0(4) yes
C30 . C31 . H311 . 107.1 no
C32 . C31 . H311 . 125.6 no
C30 . C31 . H312 . 108.7 no
C32 . C31 . H312 . 91.9 no
H311 . C31 . H312 . 108.7 no
C31 . C32 . H321 . 102.4 no
C31 . C32 . H322 . 105.4 no
H321 . C32 . H322 . 110.4 no
C31 . C32 . C33 . 122.2(6) yes
H321 . C32 . C33 . 106.6 no
H322 . C32 . C33 . 109.4 no
C32 . C33 . C33 2_665 113.4(7) yes
C32 . C33 . H331 . 109.0 no
C33 2_665 C33 . H331 . 109.0 no
C32 . C33 . H332 . 108.0 no
C33 2_665 C33 . H332 . 107.9 no
H331 . C33 . H332 . 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
O21 . H211 . O11 . 155.92(5) 0.983 1.893 2.820(4) yes
O21 . H212 . O15 1_565 155.24(7) 0.910 2.191 3.041(4) yes
C1 . H11 . O15 1_565 134.23(3) 0.977 2.560 3.316(4) yes
N18 . H181 . O11 1_455 175.61(4) 0.836 2.050 2.885(4) yes
N18 . H182 . O12 2_566 147.00(4) 0.854 2.144 2.898(4) yes
N19 . H191 . O15 2_567 130.09(4) 0.892 2.338 2.991(4) yes
N19 . H191 . O16 1_565 129.65(3) 0.892 2.532 3.176(4) yes
N19 . H192 . O21 1_455 168.04(7) 0.759 2.109 2.856(4) yes
N17 . H172 . O12 2_566 144.22(3) 0.886 2.140 2.906(4) yes
N17 . H171 . O16 1_565 139.93(3) 0.862 2.305 3.016(4) yes
N22 . H222 . O16 2_566 171.83(4) 0.911 1.965 2.870(4) yes
N22 . H221 . O10 . 163.67(4) 0.870 1.972 2.817(4) yes
N22 . H223 . O14 1_565 159.74(4) 0.822 1.952 2.738(4) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 10/06/14 at 14:58:43
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV C(24,OCC) C(25,OCC) C(26,OCC)  C(27,OCC) C(28,OCC) 
CONT  H(241,OCC) H(242,OCC)  H(251,OCC) H(252,OCC) 
CONT  H(261,OCC) H(262,OCC)   H(271,OCC) H(272,OCC) 
CONT  H(281, OCC) H(282, OCC) 
CONT  C(29,OCC) C(30,OCC) C(31,OCC) C(32,OCC) C(33, OCC) 
CONT  H(291,OCC) H(292,OCC)  H(301,OCC) H(302,OCC)
CONT  H(311,OCC) H(312,OCC)   H(321,OCC) H(322,OCC) 
CONT  H(331, OCC) H(332, OCC) H(231,OCC) H(232,OCC) 
CONT H(233,OCC) H(234,OCC) 
WEIGHT -1  C(29,OCC) C(30,OCC) C(31,OCC) C(32,OCC) C(33, OCC) 
CONT  H(291,OCC) H(292,OCC)  H(301,OCC) H(302,OCC) 
CONT  H(311,OCC) H(312,OCC)   H(321,OCC) H(322,OCC) 
CONT  H(331, OCC) H(332, OCC) H(231,OCC) H(232,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE N   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE N   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE N   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S)
RIDE N   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S)  H   ( 223,X'S) 
RIDE C(  23,X'S) H( 231,X'S) H( 232,X'S) H( 233,X'S) H( 234,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S)
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,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 O(21,X'S) H(211,X'S) H(212,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 10/06/14 at 14:58:43
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = N(22) TO C(23) 
VIBR .0, 0.00200 = C(23) TO C(24) 
VIBR .0, 0.00200 = C(23) TO C(29) 
VIBR .0, 0.00500 = C(24) TO N(22)
VIBR .0, 0.00500 = C(29) TO N(22) 
VIBR .0, 0.00500 = C(29) TO C(24) 
VIBR .0, 0.00200 = C(24) TO C(25) 
VIBR .0, 0.00200 = C(24) TO C(30) 
VIBR .0, 0.00500 = C(25) TO C(23) 
VIBR .0, 0.00500 = C(30) TO C(23) 
VIBR .0, 0.00500 = C(30) TO C(25) 
VIBR .0, 0.00200 = C(25) TO C(26) 
VIBR .0, 0.00200 = C(25) TO C(29) 
VIBR .0, 0.00500 = C(26) TO C(24) 
VIBR .0, 0.00500 = C(29) TO C(24) 
VIBR .0, 0.00500 = C(29) TO C(26) 
VIBR .0, 0.00200 = C(26) TO C(27)
VIBR .0, 0.00200 = C(26) TO C(31) 
VIBR .0, 0.00200 = C(26) TO C(32) 
VIBR .0, 0.00500 = C(27) TO C(25) 
VIBR .0, 0.00500 = C(31) TO C(25) 
VIBR .0, 0.00500 = C(31) TO C(27)
VIBR .0, 0.00500 = C(32) TO C(25) 
VIBR .0, 0.00500 = C(32) TO C(27) 
VIBR .0, 0.00500 = C(32) TO C(31) 
VIBR .0, 0.00200 = C(27) TO C(28) 
VIBR .0, 0.00200 = C(27) TO C(31) 
VIBR .0, 0.00200 = C(27) TO C(33) 
VIBR .0, 0.00500 = C(28) TO C(26) 
VIBR .0, 0.00500 = C(31) TO C(26) 
VIBR .0, 0.00500 = C(31) TO C(28) 
VIBR .0, 0.00500 = C(33) TO C(26) 
VIBR .0, 0.00500 = C(33) TO C(28) 
VIBR .0, 0.00500 = C(33) TO C(31) 
VIBR .0, 0.00200 = C(28) TO C(28,-1,1,1,1) 
VIBR .0, 0.00200 = C(28) TO C(33,-1,1,1,1) 
VIBR .0, 0.00200 = C(28) TO C(32) 
VIBR .0, 0.00200 = C(28) TO C(33) 
VIBR .0, 0.00500 = C(28,-1,1,1,1) TO C(27) 
VIBR .0, 0.00500 = C(33,-1,1,1,1) TO C(27) 
VIBR .0, 0.00500 = C(33,-1,1,1,1) TO C(28,-1,1,1,1) 
VIBR .0, 0.00500 = C(32) TO C(27) 
VIBR .0, 0.00500 = C(32) TO C(28,-1,1,1,1) 
VIBR .0, 0.00500 = C(32) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(33) TO C(27) 
VIBR .0, 0.00500 = C(33) TO C(28,-1,1,1,1) 
VIBR .0, 0.00500 = C(33) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(33) TO C(32) 
VIBR .0, 0.00200 = C(29) TO C(30)
VIBR .0, 0.00500 = C(25) TO C(23)
VIBR .0, 0.00500 = C(30) TO C(23) 
VIBR .0, 0.00500 = C(30) TO C(25) 
VIBR .0, 0.00200 = C(30) TO C(31) 
VIBR .0, 0.00500 = C(24) TO C(29) 
VIBR .0, 0.00500 = C(31) TO C(29) 
VIBR .0, 0.00500 = C(31) TO C(24) 
VIBR .0, 0.00200 = C(31) TO C(32) 
VIBR .0, 0.00500 = C(26) TO C(30) 
VIBR .0, 0.00500 = C(27) TO C(30) 
VIBR .0, 0.00500 = C(27) TO C(26) 
VIBR .0, 0.00500 = C(32) TO C(30) 
VIBR .0, 0.00500 = C(32) TO C(26)
VIBR .0, 0.00500 = C(32) TO C(27)
VIBR .0, 0.00200 = C(32) TO C(33) 
VIBR .0, 0.00500 = C(28) TO C(31) 
VIBR .0, 0.00500 = C(26) TO C(31) 
VIBR .0, 0.00500 = C(26) TO C(28) 
VIBR .0, 0.00500 = C(33) TO C(31)
VIBR .0, 0.00500 = C(33) TO C(28) 
VIBR .0, 0.00500 = C(33) TO C(26) 
VIBR .0, 0.00200 = C(33) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(27) TO C(32) 
VIBR .0, 0.00500 = C(33,-1,1,1,1) TO C(32) 
VIBR .0, 0.00500 = C(33,-1,1,1,1) TO C(27) 
VIBR .0, 0.00500 = C(28,-1,1,1,1) TO C(32) 
VIBR .0, 0.00500 = C(28,-1,1,1,1) TO C(27) 
VIBR .0, 0.00500 = C(28,-1,1,1,1) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(28) TO C(32) 
VIBR .0, 0.00500 = C(28) TO C(27) 
VIBR .0, 0.00500 = C(28) TO C(33,-1,1,1,1) 
VIBR .0, 0.00500 = C(28) TO C(28,-1,1,1,1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = N(22) TO C(23) 
U(IJ) .0, 0.04000 = C(23) TO C(24) 
U(IJ) .0, 0.04000 = C(23) TO C(29) 
U(IJ) .0, 0.04000 = C(24) TO C(25) 
U(IJ) .0, 0.04000 = C(24) TO C(30) 
U(IJ) .0, 0.04000 = C(25) TO C(26) 
U(IJ) .0, 0.04000 = C(25) TO C(29) 
U(IJ) .0, 0.04000 = C(26) TO C(27) 
U(IJ) .0, 0.04000 = C(26) TO C(31) 
U(IJ) .0, 0.04000 = C(26) TO C(32) 
U(IJ) .0, 0.04000 = C(27) TO C(28) 
U(IJ) .0, 0.04000 = C(27) TO C(31) 
U(IJ) .0, 0.04000 = C(27) TO C(33) 
U(IJ) .0, 0.04000 = C(28) TO C(28,-1,1,1,1) 
U(IJ) .0, 0.04000 = C(28) TO C(33,-1,1,1,1) 
U(IJ) .0, 0.04000 = C(28) TO C(32) 
U(IJ) .0, 0.04000 = C(28) TO C(33) 
U(IJ) .0, 0.04000 = C(29) TO C(30) 
U(IJ) .0, 0.04000 = C(30) TO C(31) 
U(IJ) .0, 0.04000 = C(31) TO C(32) 
U(IJ) .0, 0.04000 = C(32) TO C(33) 
U(IJ) .0, 0.04000 = C(33) TO C(33,-1,1,1,1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_database_code_depnum_ccdc_archive 'CCDC 986092'
