# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1553849'
_audit_update_record             
;
2018-07-05 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
?
;
#--------------------------------------------------------------- 
_cell_length_a                   11.5904(4)
_cell_length_b                   31.735(2)
_cell_length_c                   12.3284(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.601(3)
_cell_angle_gamma                90
_cell_volume                     4534.4(2)
_cell_measurement_reflns_used    5542
_cell_measurement_theta_min      1.9510
_cell_measurement_theta_max      26.2030
_cell_oxdiff_length_a            11.5859(5)
_cell_oxdiff_length_b            31.7590(13)
_cell_oxdiff_length_c            12.3239(5)
_cell_oxdiff_angle_alpha         90.008(3)
_cell_oxdiff_angle_beta          90.620(3)
_cell_oxdiff_angle_gamma         90.030(3)
_cell_oxdiff_volume              4534.4(3)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 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            'C70 H78 N10 O35 S8 [+ solvent]'
_chemical_formula_moiety         
'2(C28 H20 O16 S4), 2(C7 H19 N5 O), O [+ solvent]'
_chemical_compound_source        ?
_chemical_formula_weight         1875.98


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_max          0.400
_exptl_absorpt_correction_T_min  0.81457
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.872
_oxdiff_exptl_absorpt_empirical_full_max 1.114
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1946.850
_exptl_absorpt_coefficient_mu    0.284
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_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       0.81
_montpellier_reflns_completeness_maxres 99.17
_montpellier_reflns_redundancy_maxres 3.73

#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 1.69 6.3 39.27 0.035 99.8 99.80
1 1.69 1.34 5.1 15.32 0.059 100.0 99.90
2 1.34 1.17 4.5 11.32 0.081 100.0 99.93
3 1.17 1.06 3.6 8.03 0.094 100.0 99.95
4 1.06 0.99 3.3 5.55 0.126 99.9 99.94
5 0.99 0.93 3.1 4.01 0.181 100.0 99.95
6 0.93 0.88 2.9 3.14 0.225 99.9 99.94
7 0.88 0.84 2.6 2.77 0.245 100.0 99.95
8 0.84 0.81 2.1 2.32 0.312 93.3 99.17
9 0.81 0.75 1.3 1.70 0.569 43.6 87.90
#End reflection statistics
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_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      -0.0419827000
_diffrn_orient_matrix_UB_12      0.0161155000
_diffrn_orient_matrix_UB_13      0.0049169000
_diffrn_orient_matrix_UB_21      -0.0372335000
_diffrn_orient_matrix_UB_22      -0.0111343000
_diffrn_orient_matrix_UB_23      -0.0359514000
_diffrn_orient_matrix_UB_31      -0.0244865000
_diffrn_orient_matrix_UB_32      -0.0107292000
_diffrn_orient_matrix_UB_33      0.0446796000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  24.00   1.00  341.12    --  -14.51-100.00   0.00   40
  2  ω    -24.00  56.00   1.00  341.12    --   15.21-100.00-180.00   80
  3  ω    -42.00  31.00   1.00  341.12    --   15.21 -57.00-150.00   73
  4  ω    -53.00  40.00   1.00  341.12    --   15.21 -77.00  60.00   93
  5  ω     -7.00  86.00   1.00  341.12    --   15.21  38.00   0.00   93
;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            10022
_reflns_number_total             10022
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_unetI/netI     0.0960
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 10022 
# Theoretical number of reflections is about 22656 


_diffrn_reflns_theta_min         1.772
_diffrn_reflns_theta_max         28.406
_diffrn_measured_fraction_theta_max 0.879

_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              40
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.23
_oxford_diffrn_Wilson_scale      3.06

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

_refine_diff_density_min         -1.59
_refine_diff_density_max         0.94


# 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         6649
_refine_ls_number_restraints     47
_refine_ls_number_parameters     578
_oxford_refine_ls_R_factor_ref   0.0971
_refine_ls_wR_factor_ref         0.0876
_refine_ls_goodness_of_fit_ref   1.2558
_refine_ls_shift/su_max          0.0061118
_refine_ls_shift/su_mean         0.0003124


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10022
_refine_ls_R_factor_all          0.1394
_refine_ls_wR_factor_all         0.1072

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6649
_refine_ls_R_factor_gt           0.0971
_refine_ls_wR_factor_gt          0.0876

# 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: 
 11.9 9.51 10.7 4.31 0.135 
;

# 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 0.31097(9) 0.38824(4) 1.10910(8) 0.0287 1.0000 Uani . . . . . .
O2 O 0.2389(3) 0.41526(13) 1.1734(3) 0.0556 1.0000 Uani . . . . . .
O3 O 0.3504(4) 0.40742(13) 1.0108(3) 0.0613 1.0000 Uani . . . . . .
O4 O 0.4046(3) 0.37195(14) 1.1749(4) 0.0587 1.0000 Uani . . . . . .
C5 C 0.2260(3) 0.34406(13) 1.0694(3) 0.0220 1.0000 Uani . . . . . .
C6 C 0.1513(3) 0.32594(13) 1.1422(3) 0.0217 1.0000 Uani . . . . . .
C7 C 0.0883(3) 0.29031(12) 1.1129(3) 0.0212 1.0000 Uani . . . . . .
C8 C 0.1055(3) 0.27298(13) 1.0093(3) 0.0239 1.0000 Uani . . . . . .
O9 O 0.0528(3) 0.23632(10) 0.9814(3) 0.0373 1.0000 Uani . . . . . .
C10 C 0.1792(3) 0.29204(13) 0.9349(3) 0.0233 1.0000 Uani . . . . . .
C11 C 0.2395(3) 0.32800(14) 0.9660(3) 0.0228 1.0000 Uani . . . . . .
C12 C 0.1965(3) 0.27396(15) 0.8220(3) 0.0281 1.0000 Uani . . . . . .
C13 C 0.1190(3) 0.29270(14) 0.7350(3) 0.0265 1.0000 Uani . . . . . .
C14 C 0.0028(3) 0.28016(14) 0.7236(3) 0.0258 1.0000 Uani . . . . . .
O15 O -0.0385(3) 0.24812(10) 0.7861(3) 0.0363 1.0000 Uani . . . . . .
C16 C -0.0715(3) 0.29866(14) 0.6471(3) 0.0260 1.0000 Uani . . . . . .
C17 C -0.0279(3) 0.32846(15) 0.5782(3) 0.0303 1.0000 Uani . . . . . .
C18 C 0.0886(4) 0.33945(16) 0.5833(4) 0.0344 1.0000 Uani . . . . . .
C19 C 0.1600(3) 0.32259(16) 0.6630(3) 0.0313 1.0000 Uani . . . . . .
S20 S 0.14586(12) 0.37312(7) 0.48500(11) 0.0658 1.0000 Uani D . . . . .
O21 O 0.2283(5) 0.39884(18) 0.5336(4) 0.0890 1.0000 Uani D U . . . .
C24 C -0.1984(3) 0.28630(14) 0.6421(3) 0.0276 1.0000 Uani . . . . . .
C25 C -0.2704(3) 0.30719(14) 0.7293(3) 0.0253 1.0000 Uani . . . . . .
C26 C -0.2975(3) 0.28741(13) 0.8267(3) 0.0248 1.0000 Uani . . . . . .
O27 O -0.2600(3) 0.24652(9) 0.8447(2) 0.0294 1.0000 Uani . . . . . .
C28 C -0.3650(3) 0.30638(15) 0.9053(3) 0.0276 1.0000 Uani . . . . . .
C29 C -0.4089(3) 0.34649(14) 0.8833(4) 0.0285 1.0000 Uani . . . . . .
C30 C -0.3833(4) 0.36636(15) 0.7877(4) 0.0326 1.0000 Uani . . . . . .
C31 C -0.3135(4) 0.34739(15) 0.7119(4) 0.0304 1.0000 Uani . . . . . .
S32 S -0.44679(13) 0.41593(4) 0.75688(12) 0.0463 1.0000 Uani . . . . . .
O33 O -0.4504(4) 0.43997(12) 0.8541(3) 0.0528 1.0000 Uani . . . . . .
O34 O -0.5629(4) 0.40654(16) 0.7163(5) 0.0809 1.0000 Uani . . . . . .
O35 O -0.3802(6) 0.43427(15) 0.6717(5) 0.0985 1.0000 Uani . . . . . .
C36 C -0.3902(3) 0.28544(14) 1.0145(3) 0.0266 1.0000 Uani . . . . . .
C37 C -0.3033(3) 0.29819(14) 1.1020(3) 0.0248 1.0000 Uani . . . . . .
C38 C -0.1943(3) 0.27851(13) 1.1110(3) 0.0237 1.0000 Uani . . . . . .
O39 O -0.1672(2) 0.24557(10) 1.0441(2) 0.0300 1.0000 Uani . . . . . .
C40 C -0.1139(3) 0.29108(14) 1.1889(3) 0.0241 1.0000 Uani . . . . . .
C41 C 0.0051(3) 0.27080(14) 1.1944(3) 0.0245 1.0000 Uani . . . . . .
C42 C -0.1429(3) 0.32285(14) 1.2605(3) 0.0267 1.0000 Uani . . . . . .
C43 C -0.2505(3) 0.34229(14) 1.2541(3) 0.0257 1.0000 Uani . . . . . .
C44 C -0.3302(3) 0.32970(14) 1.1747(3) 0.0263 1.0000 Uani . . . . . .
S45 S -0.28492(9) 0.38199(4) 1.34804(9) 0.0314 1.0000 Uani . . . . . .
O46 O -0.3795(6) 0.4044(2) 1.3049(4) 0.1138 1.0000 Uani . . . . . .
O47 O -0.3086(6) 0.36325(15) 1.4478(4) 0.0937 1.0000 Uani . . . . . .
O48 O -0.1866(5) 0.4078(2) 1.3564(6) 0.1333 1.0000 Uani . . . . . .
O49 O 0.0934(4) 0.49493(13) 0.8254(4) 0.0602 1.0000 Uani . . . . . .
C50 C 0.1525(4) 0.46422(16) 0.8063(4) 0.0413 1.0000 Uani . . . . . .
N51 N 0.2693(4) 0.46719(16) 0.8040(5) 0.0613 1.0000 Uani . . . . . .
N52 N 0.3226(4) 0.50583(15) 0.8090(5) 0.0553 1.0000 Uani . . . . . .
C53 C 0.3583(4) 0.52113(17) 0.9055(5) 0.0466 1.0000 Uani . . . . . .
N54 N 0.3996(4) 0.55970(15) 0.9087(5) 0.0553 1.0000 Uani . . . . . .
N55 N 0.3523(4) 0.49837(15) 0.9926(4) 0.0527 1.0000 Uani . . . . . .
C56 C 0.1054(6) 0.42121(19) 0.7814(5) 0.0552 1.0000 Uani . . . . . .
C57 C -0.0236(5) 0.4158(2) 0.7972(6) 0.0620 1.0000 Uani . . . . . .
C58 C -0.0550(5) 0.3987(2) 0.9062(6) 0.0659 1.0000 Uani . . . . . .
C59 C -0.0175(5) 0.42495(18) 1.0037(5) 0.0506 1.0000 Uani . . . . . .
C60 C -0.0593(5) 0.40637(19) 1.1064(5) 0.0545 1.0000 Uani . . . . . .
N61 N -0.0054(4) 0.42602(16) 1.2017(4) 0.0569 1.0000 Uani . . . . . .
H61 H 0.1425 0.3376 1.2111 0.0256 1.0000 Uiso R . . . . .
H111 H 0.2895 0.3413 0.9171 0.0262 1.0000 Uiso R . . . . .
H122 H 0.2767 0.2792 0.8024 0.0336 1.0000 Uiso R . . . . .
H121 H 0.1811 0.2441 0.8239 0.0335 1.0000 Uiso R . . . . .
H171 H -0.0743 0.3410 0.5280 0.0357 1.0000 Uiso R . . . . .
H191 H 0.2368 0.3314 0.6682 0.0383 1.0000 Uiso R . . . . .
H241 H -0.2314 0.2944 0.5721 0.0329 1.0000 Uiso R . . . . .
H242 H -0.2043 0.2561 0.6500 0.0326 1.0000 Uiso R . . . . .
H291 H -0.4549 0.3595 0.9349 0.0338 1.0000 Uiso R . . . . .
H311 H -0.2952 0.3620 0.6488 0.0363 1.0000 Uiso R . . . . .
H361 H -0.4666 0.2938 1.0372 0.0318 1.0000 Uiso R . . . . .
H362 H -0.3866 0.2555 1.0049 0.0321 1.0000 Uiso R . . . . .
H412 H 0.0373 0.2750 1.2669 0.0298 1.0000 Uiso R . . . . .
H411 H -0.0028 0.2409 1.1795 0.0294 1.0000 Uiso R . . . . .
H421 H -0.0896 0.3318 1.3129 0.0319 1.0000 Uiso R . . . . .
H441 H -0.4032 0.3427 1.1709 0.0318 1.0000 Uiso R . . . . .
H562 H 0.1228 0.4155 0.7055 0.0662 1.0000 Uiso R . . . . .
H561 H 0.1453 0.4008 0.8272 0.0660 1.0000 Uiso R . . . . .
H571 H -0.0516 0.3960 0.7428 0.0748 1.0000 Uiso R . . . . .
H572 H -0.0627 0.4428 0.7864 0.0748 1.0000 Uiso R . . . . .
H581 H -0.1379 0.3973 0.9090 0.0789 1.0000 Uiso R . . . . .
H582 H -0.0229 0.3707 0.9139 0.0791 1.0000 Uiso R . . . . .
H591 H -0.0479 0.4537 0.9955 0.0610 1.0000 Uiso R . . . . .
H592 H 0.0673 0.4262 1.0073 0.0610 1.0000 Uiso R . . . . .
H601 H -0.0430 0.3762 1.1098 0.0659 1.0000 Uiso R . . . . .
H602 H -0.1431 0.4111 1.1097 0.0658 1.0000 Uiso R . . . . .
H541 H 0.4300 0.5692 0.9677 0.0669 1.0000 Uiso R . . . . .
H611 H -0.0301 0.4136 1.2617 0.0849 1.0000 Uiso R . . . . .
H511 H 0.3099 0.4451 0.7891 0.0738 1.0000 Uiso R . . . . .
H521 H 0.3267 0.5214 0.7516 0.0674 1.0000 Uiso R . . . . .
H15 H 0.3380 0.4717 0.9899 0.0627 1.0000 Uiso R . . . . .
H47 H 0.0714 0.4239 1.2000 0.0848 1.0000 Uiso R . . . . .
H52 H -0.0237 0.4533 1.2050 0.0846 1.0000 Uiso R . . . . .
H56 H 0.3597 0.5096 1.0552 0.0632 1.0000 Uiso R . . . . .
H542 H 0.4200 0.5717 0.8500 0.0673 1.0000 Uiso R . . . . .
O220 O 0.0648(8) 0.4081(3) 0.4786(10) 0.0904 0.459(9) Uani D U P 1 1 .
O221 O 0.0717(7) 0.3723(3) 0.3930(5) 0.0737 0.541(9) Uani D U P 1 2 .
O230 O 0.1633(10) 0.3501(3) 0.3898(6) 0.0743 0.459(9) Uani D U P 1 1 .
O231 O 0.2344(8) 0.3448(3) 0.4415(8) 0.0964 0.541(9) Uani D U P 1 2 .
O100 O 0.3608(5) 0.3368(3) 0.3589(7) 0.0601 0.5000 Uani . . . . . .
H391 H -0.2102 0.2487 0.9917 0.0457 1.0000 Uiso R . . . . .
H91 H -0.0090 0.2298 1.0054 0.0563 1.0000 Uiso R . . . . .
H271 H -0.2008 0.2445 0.8091 0.0448 1.0000 Uiso R . . . . .
H151 H -0.0001 0.2442 0.8429 0.0555 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.954(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 . O2 . 1.441(4) yes
S1 . O3 . 1.436(4) yes
S1 . O4 . 1.444(4) yes
S1 . C5 . 1.779(4) yes
C5 . C6 . 1.378(5) yes
C5 . C11 . 1.384(6) yes
C6 . C7 . 1.391(6) yes
C6 . H61 . 0.934 no
C7 . C8 . 1.408(6) yes
C7 . C41 . 1.531(5) yes
C8 . O9 . 1.357(5) yes
C8 . C10 . 1.397(6) yes
O9 . H91 . 0.805 no
C10 . C11 . 1.390(6) yes
C10 . C12 . 1.521(6) yes
C11 . H111 . 0.941 no
C12 . C13 . 1.513(6) yes
C12 . H122 . 0.976 no
C12 . H121 . 0.964 no
C13 . C14 . 1.410(6) yes
C13 . C19 . 1.387(7) yes
C14 . O15 . 1.366(6) yes
C14 . C16 . 1.400(6) yes
O15 . H151 . 0.836 no
C16 . C17 . 1.371(6) yes
C16 . C24 . 1.522(6) yes
C17 . C18 . 1.395(6) yes
C17 . H171 . 0.908 no
C18 . C19 . 1.385(7) yes
C18 . S20 . 1.752(5) yes
C19 . H191 . 0.935 no
S20 . O21 . 1.388(4) yes
S20 . O220 . 1.455(5) yes
S20 . O230 . 1.400(5) yes
S20 . O21 . 1.388(4) yes
S20 . O221 . 1.416(4) yes
S20 . O231 . 1.470(5) yes
C24 . C25 . 1.521(6) yes
C24 . H241 . 0.974 no
C24 . H242 . 0.965 no
C25 . C26 . 1.394(6) yes
C25 . C31 . 1.386(6) yes
C26 . O27 . 1.385(5) yes
C26 . C28 . 1.389(6) yes
O27 . H271 . 0.821 no
C28 . C29 . 1.396(7) yes
C28 . C36 . 1.532(6) yes
C29 . C30 . 1.372(6) yes
C29 . H291 . 0.931 no
C30 . C31 . 1.380(6) yes
C30 . S32 . 1.776(5) yes
C31 . H311 . 0.933 no
S32 . O33 . 1.421(4) yes
S32 . O34 . 1.461(5) yes
S32 . O35 . 1.433(5) yes
C36 . C37 . 1.523(6) yes
C36 . H361 . 0.969 no
C36 . H362 . 0.960 no
C37 . C38 . 1.413(6) yes
C37 . C44 . 1.381(6) yes
C38 . O39 . 1.370(5) yes
C38 . C40 . 1.389(6) yes
O39 . H391 . 0.818 no
C40 . C41 . 1.523(5) yes
C40 . C42 . 1.384(6) yes
C41 . H412 . 0.974 no
C41 . H411 . 0.972 no
C42 . C43 . 1.393(6) yes
C42 . H421 . 0.934 no
C43 . C44 . 1.397(6) yes
C43 . S45 . 1.760(4) yes
C44 . H441 . 0.943 no
S45 . O46 . 1.406(4) yes
S45 . O47 . 1.396(4) yes
S45 . O48 . 1.407(5) yes
O49 . C50 . 1.216(6) yes
C50 . N51 . 1.357(7) yes
C50 . C56 . 1.501(8) yes
N51 . N52 . 1.374(7) yes
N51 . H511 . 0.864 no
N52 . C53 . 1.347(8) yes
N52 . H521 . 0.863 no
C53 . N54 . 1.315(7) yes
C53 . N55 . 1.296(8) yes
N54 . H541 . 0.860 no
N54 . H542 . 0.854 no
N55 . H15 . 0.863 no
N55 . H56 . 0.853 no
C56 . C57 . 1.520(9) yes
C56 . H562 . 0.976 no
C56 . H561 . 0.974 no
C57 . C58 . 1.498(10) yes
C57 . H571 . 0.970 no
C57 . H572 . 0.978 no
C58 . C59 . 1.521(9) yes
C58 . H581 . 0.962 no
C58 . H582 . 0.969 no
C59 . C60 . 1.483(8) yes
C59 . H591 . 0.982 no
C59 . H592 . 0.985 no
C60 . N61 . 1.465(9) yes
C60 . H601 . 0.977 no
C60 . H602 . 0.984 no
N61 . H611 . 0.889 no
N61 . H47 . 0.892 no
N61 . H52 . 0.894 no
O231 . O100 . 1.811(10) 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
O2 . S1 . O3 . 113.8(3) yes
O2 . S1 . O4 . 109.9(3) yes
O3 . S1 . O4 . 112.4(3) yes
O2 . S1 . C5 . 107.3(2) yes
O3 . S1 . C5 . 106.4(2) yes
O4 . S1 . C5 . 106.4(2) yes
S1 . C5 . C6 . 120.0(3) yes
S1 . C5 . C11 . 118.4(3) yes
C6 . C5 . C11 . 121.6(4) yes
C5 . C6 . C7 . 120.1(4) yes
C5 . C6 . H61 . 120.2 no
C7 . C6 . H61 . 119.7 no
C6 . C7 . C8 . 118.3(4) yes
C6 . C7 . C41 . 119.4(4) yes
C8 . C7 . C41 . 122.3(4) yes
C7 . C8 . O9 . 119.8(4) yes
C7 . C8 . C10 . 121.4(4) yes
O9 . C8 . C10 . 118.8(4) yes
C8 . O9 . H91 . 121.8 no
C8 . C10 . C11 . 118.9(4) yes
C8 . C10 . C12 . 121.7(4) yes
C11 . C10 . C12 . 119.4(4) yes
C10 . C11 . C5 . 119.7(4) yes
C10 . C11 . H111 . 120.2 no
C5 . C11 . H111 . 120.1 no
C10 . C12 . C13 . 114.6(3) yes
C10 . C12 . H122 . 107.4 no
C13 . C12 . H122 . 108.5 no
C10 . C12 . H121 . 108.8 no
C13 . C12 . H121 . 107.1 no
H122 . C12 . H121 . 110.4 no
C12 . C13 . C14 . 121.3(4) yes
C12 . C13 . C19 . 121.2(4) yes
C14 . C13 . C19 . 117.5(4) yes
C13 . C14 . O15 . 119.6(4) yes
C13 . C14 . C16 . 122.0(4) yes
O15 . C14 . C16 . 118.4(4) yes
C14 . O15 . H151 . 113.4 no
C14 . C16 . C17 . 118.6(4) yes
C14 . C16 . C24 . 120.5(4) yes
C17 . C16 . C24 . 121.0(4) yes
C16 . C17 . C18 . 120.5(4) yes
C16 . C17 . H171 . 120.4 no
C18 . C17 . H171 . 119.2 no
C17 . C18 . C19 . 120.4(4) yes
C17 . C18 . S20 . 119.7(4) yes
C19 . C18 . S20 . 119.9(3) yes
C13 . C19 . C18 . 120.8(4) yes
C13 . C19 . H191 . 119.5 no
C18 . C19 . H191 . 119.7 no
C18 . S20 . O21 . 108.9(2) yes
C18 . S20 . O220 . 104.7(4) yes
O21 . S20 . O220 . 90.9(6) yes
C18 . S20 . O230 . 108.7(5) yes
O21 . S20 . O230 . 124.4(5) yes
O220 . S20 . O230 . 116.8(7) yes
C18 . S20 . O21 . 108.9(2) yes
C18 . S20 . O221 . 108.1(4) yes
O21 . S20 . O221 . 140.0(4) yes
C18 . S20 . O231 . 98.6(4) yes
O21 . S20 . O231 . 92.1(6) yes
O221 . S20 . O231 . 96.7(7) yes
C16 . C24 . C25 . 113.3(3) yes
C16 . C24 . H241 . 109.8 no
C25 . C24 . H241 . 107.3 no
C16 . C24 . H242 . 108.7 no
C25 . C24 . H242 . 108.7 no
H241 . C24 . H242 . 108.9 no
C24 . C25 . C26 . 122.9(4) yes
C24 . C25 . C31 . 119.4(4) yes
C26 . C25 . C31 . 117.6(4) yes
C25 . C26 . O27 . 119.1(4) yes
C25 . C26 . C28 . 122.6(4) yes
O27 . C26 . C28 . 118.2(4) yes
C26 . O27 . H271 . 104.6 no
C26 . C28 . C29 . 117.8(4) yes
C26 . C28 . C36 . 122.6(4) yes
C29 . C28 . C36 . 119.6(4) yes
C28 . C29 . C30 . 120.3(4) yes
C28 . C29 . H291 . 118.8 no
C30 . C29 . H291 . 120.9 no
C29 . C30 . C31 . 121.0(4) yes
C29 . C30 . S32 . 119.9(3) yes
C31 . C30 . S32 . 119.1(3) yes
C25 . C31 . C30 . 120.6(4) yes
C25 . C31 . H311 . 120.2 no
C30 . C31 . H311 . 119.2 no
C30 . S32 . O33 . 108.1(2) yes
C30 . S32 . O34 . 105.7(3) yes
O33 . S32 . O34 . 111.3(3) yes
C30 . S32 . O35 . 106.9(2) yes
O33 . S32 . O35 . 114.9(3) yes
O34 . S32 . O35 . 109.5(4) yes
C28 . C36 . C37 . 112.1(3) yes
C28 . C36 . H361 . 108.5 no
C37 . C36 . H361 . 108.8 no
C28 . C36 . H362 . 108.2 no
C37 . C36 . H362 . 108.8 no
H361 . C36 . H362 . 110.3 no
C36 . C37 . C38 . 121.5(4) yes
C36 . C37 . C44 . 120.0(4) yes
C38 . C37 . C44 . 118.5(4) yes
C37 . C38 . O39 . 120.0(4) yes
C37 . C38 . C40 . 121.3(4) yes
O39 . C38 . C40 . 118.7(4) yes
C38 . O39 . H391 . 104.0 no
C38 . C40 . C41 . 120.6(4) yes
C38 . C40 . C42 . 119.0(4) yes
C41 . C40 . C42 . 120.3(4) yes
C7 . C41 . C40 . 112.1(3) yes
C7 . C41 . H412 . 108.0 no
C40 . C41 . H412 . 108.7 no
C7 . C41 . H411 . 109.3 no
C40 . C41 . H411 . 108.7 no
H412 . C41 . H411 . 110.1 no
C40 . C42 . C43 . 120.6(4) yes
C40 . C42 . H421 . 120.0 no
C43 . C42 . H421 . 119.3 no
C42 . C43 . C44 . 119.9(4) yes
C42 . C43 . S45 . 119.3(3) yes
C44 . C43 . S45 . 120.9(3) yes
C43 . C44 . C37 . 120.7(4) yes
C43 . C44 . H441 . 119.8 no
C37 . C44 . H441 . 119.6 no
C43 . S45 . O46 . 107.1(2) yes
C43 . S45 . O47 . 108.8(2) yes
O46 . S45 . O47 . 112.9(4) yes
C43 . S45 . O48 . 106.1(2) yes
O46 . S45 . O48 . 111.2(5) yes
O47 . S45 . O48 . 110.5(5) yes
O49 . C50 . N51 . 120.9(5) yes
O49 . C50 . C56 . 124.3(5) yes
N51 . C50 . C56 . 114.8(4) yes
C50 . N51 . N52 . 120.6(4) yes
C50 . N51 . H511 . 119.6 no
N52 . N51 . H511 . 119.1 no
N51 . N52 . C53 . 119.6(5) yes
N51 . N52 . H521 . 120.1 no
C53 . N52 . H521 . 119.9 no
N52 . C53 . N54 . 118.0(6) yes
N52 . C53 . N55 . 120.8(5) yes
N54 . C53 . N55 . 121.1(6) yes
C53 . N54 . H541 . 119.8 no
C53 . N54 . H542 . 119.7 no
H541 . N54 . H542 . 116.5 no
C53 . N55 . H15 . 121.8 no
C53 . N55 . H56 . 120.7 no
H15 . N55 . H56 . 117.4 no
C50 . C56 . C57 . 115.7(5) yes
C50 . C56 . H562 . 106.7 no
C57 . C56 . H562 . 108.3 no
C50 . C56 . H561 . 108.5 no
C57 . C56 . H561 . 108.2 no
H562 . C56 . H561 . 109.2 no
C56 . C57 . C58 . 113.9(5) yes
C56 . C57 . H571 . 107.9 no
C58 . C57 . H571 . 107.7 no
C56 . C57 . H572 . 109.7 no
C58 . C57 . H572 . 108.8 no
H571 . C57 . H572 . 108.7 no
C57 . C58 . C59 . 116.2(5) yes
C57 . C58 . H581 . 107.5 no
C59 . C58 . H581 . 105.9 no
C57 . C58 . H582 . 108.8 no
C59 . C58 . H582 . 108.6 no
H581 . C58 . H582 . 109.7 no
C58 . C59 . C60 . 111.3(5) yes
C58 . C59 . H591 . 109.1 no
C60 . C59 . H591 . 109.7 no
C58 . C59 . H592 . 109.5 no
C60 . C59 . H592 . 108.2 no
H591 . C59 . H592 . 108.9 no
C59 . C60 . N61 . 112.0(5) yes
C59 . C60 . H601 . 111.2 no
N61 . C60 . H601 . 107.6 no
C59 . C60 . H602 . 107.8 no
N61 . C60 . H602 . 108.4 no
H601 . C60 . H602 . 109.7 no
C60 . N61 . H611 . 109.9 no
C60 . N61 . H47 . 111.4 no
H611 . N61 . H47 . 108.4 no
C60 . N61 . H52 . 110.5 no
H611 . N61 . H52 . 108.3 no
H47 . N61 . H52 . 108.2 no
S20 . O231 . O100 . 149.6(8) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H61 . O230 1_556 161.8(3) 0.934 2.248 3.149(6) yes
C31 . H311 . O47 1_554 145.96(17) 0.933 2.481 3.296(6) yes
C42 . H421 . O221 1_556 158.36(18) 0.934 2.465 3.350(6) yes
C44 . H441 . O4 1_455 174.64(14) 0.943 2.414 3.354(6) yes
C56 . H562 . O21 . 162.63(19) 0.976 2.514 3.458(6) yes
N54 . H541 . O33 2_567 145.91(16) 0.860 2.226 2.978(6) yes
N61 . H611 . O48 . 139.7(3) 0.889 2.175 2.910(6) yes
N61 . H611 . O221 1_556 130.4(2) 0.889 2.385 3.037(6) yes
N51 . H511 . O34 1_655 159.9(2) 0.864 2.123 2.950(6) yes
N52 . H521 . O46 2_567 140.48(15) 0.863 2.535 3.248(6) yes
N55 . H15 . O3 . 162.31(19) 0.863 2.061 2.895(6) yes
N61 . H47 . O2 . 171.2(2) 0.892 1.991 2.876(6) yes
N61 . H52 . O49 2_567 161.2(2) 0.894 1.866 2.727(6) yes
N55 . H56 . O33 2_567 143.27(17) 0.853 2.213 2.941(6) yes
N54 . H542 . O46 2_567 150.4(2) 0.854 2.104 2.877(6) yes
O39 . H391 . C26 . 155.99(11) 0.818 2.574 3.338(6) yes
O39 . H391 . O27 . 158.05(13) 0.818 1.897 2.673(6) yes
O9 . H91 . O39 . 149.40(13) 0.805 1.964 2.689(6) yes
O27 . H271 . O15 . 154.86(14) 0.821 1.909 2.675(6) yes
O15 . H151 . C8 . 150.4(2) 0.836 2.546 3.299(6) yes
O15 . H151 . O9 . 167.3(2) 0.836 1.825 2.646(6) yes


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.008 0.000 0.000 343 107 ' '
2 -0.016 0.500 0.500 343 107 ' '
3 0.015 0.832 0.138 6 1 ' '
4 0.484 0.332 0.362 6 1 ' '
5 0.515 0.668 0.638 7 2 ' '
6 0.984 0.168 0.862 6 2 ' '
# start Validation Reply Form
_vrf_PLAT601_1                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        314 Ang3
RESPONSE: The Squeeze procedure was used in order to treat a disordered region
of aminoguanadine counter cations.
;
# start Validation Reply Form
_vrf_PLAT430_1                   
;
PROBLEM: Short Inter D...A Contact  O100   ..  O231    ..       1.81 Ang.
RESPONSE: Both the water molecule and the disordered sulfonate 
moeity are at 50% occupation probablity.
;
# end Validation Reply Form
# end Validation Reply Form
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1553851'
_audit_update_record             
;
2018-07-05 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
;
? 
;
#--------------------------------------------------------------- 
_cell_length_a                   11.9051(3)
_cell_length_b                   29.1899(7)
_cell_length_c                   12.3382(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.712(2)
_cell_angle_gamma                90
_cell_volume                     4287.28(9)
_cell_measurement_reflns_used    10475
_cell_measurement_theta_min      1.8220
_cell_measurement_theta_max      28.5050
_cell_oxdiff_length_a            11.9054(4)
_cell_oxdiff_length_b            29.1876(9)
_cell_oxdiff_length_c            12.3389(3)
_cell_oxdiff_angle_alpha         89.996(2)
_cell_oxdiff_angle_beta          90.743(2)
_cell_oxdiff_angle_gamma         90.004(2)
_cell_oxdiff_volume              4287.3(2)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 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'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

_chemical_formula_sum            'C68 H92 N2 Na O48 S8 '
_chemical_formula_moiety         'C62 H58 N Na O36 S8, C6 H14 N O2, 10(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         1984.91


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.210
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_max          0.450
_exptl_absorpt_correction_T_min  0.86785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.912
_oxdiff_exptl_absorpt_empirical_full_max 1.092
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2074
_exptl_absorpt_coefficient_mu    0.318
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_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 88.20
_montpellier_reflns_redundancy_maxres 3.60

#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 1.65 6.3 71.18 0.027 99.8 99.81
1 1.65 1.31 5.0 36.68 0.042 100.0 99.90
2 1.30 1.14 4.4 29.00 0.047 100.0 99.94
3 1.14 1.03 3.8 20.38 0.053 100.0 99.95
4 1.03 0.96 3.5 13.15 0.082 100.0 99.96
5 0.96 0.90 3.2 9.77 0.099 100.0 99.97
6 0.90 0.86 3.0 8.09 0.116 100.0 99.97
7 0.86 0.82 2.8 7.20 0.129 100.0 99.98
8 0.82 0.79 2.4 6.02 0.151 95.5 99.46
9 0.79 0.73 1.5 3.65 0.181 43.8 88.20
#End reflection statistics
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_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      -0.0280232000
_diffrn_orient_matrix_UB_12      -0.0174454000
_diffrn_orient_matrix_UB_13      0.0291600000
_diffrn_orient_matrix_UB_21      0.0497688000
_diffrn_orient_matrix_UB_22      -0.0133595000
_diffrn_orient_matrix_UB_23      0.0004204000
_diffrn_orient_matrix_UB_31      0.0169672000
_diffrn_orient_matrix_UB_32      0.0103802000
_diffrn_orient_matrix_UB_33      0.0495440000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  24.00   1.00   76.84    --  -16.62-100.00   0.00   34
  2  ω    -23.00   5.00   1.00   76.84    --  -16.62-100.00 -60.00   28
  3  ω    -50.00  36.00   1.00   76.84    --   17.25 -57.00 -30.00   86
  4  ω    -23.00  58.00   1.00   76.84    --   17.25-100.00-150.00   81
  5  ω     51.00  87.00   1.00   76.84    --   17.25 179.00   0.00   36
  6  ω    -51.00  51.00   1.00   76.84    --   17.25 -19.00  30.00  102
  7  ω     11.00  46.00   1.00   76.84    --   17.25 -77.00  90.00   35
;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            37233
_reflns_number_total             16839
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_unetI/netI     0.0506
# Number of reflections without Friedels Law is 16839 
# Number of reflections with Friedels Law is 10280 
# Theoretical number of reflections is about 11623 


_diffrn_reflns_theta_min         1.792
_diffrn_reflns_theta_max         29.206
_diffrn_measured_fraction_theta_max 0.882

_diffrn_reflns_theta_full        26.330
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -14
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              39
_reflns_limit_l_min              -16
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.37
_oxford_diffrn_Wilson_scale      0.47

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

_refine_diff_density_min         -1.15
_refine_diff_density_max         2.10


# 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         15162
_refine_ls_number_restraints     120
_refine_ls_number_parameters     1190
_oxford_refine_ls_R_factor_ref   0.0888
_refine_ls_wR_factor_ref         0.0969
_refine_ls_goodness_of_fit_ref   1.1067
_refine_ls_shift/su_max          0.0006734
_refine_ls_shift/su_mean         0.0000327


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        16839
_refine_ls_R_factor_all          0.0957
_refine_ls_wR_factor_all         0.1024

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                15162
_refine_ls_R_factor_gt           0.0888
_refine_ls_wR_factor_gt          0.0969

# 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 unk


_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: 
 17.0 6.29 13.5 4.85 
;

# 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 0.33354(13) 0.13753(4) 0.58521(12) 0.0274 1.0000 Uani . . . . . .
O2 O 0.3795(4) 0.15976(16) 0.4899(3) 0.0436 1.0000 Uani . . . . . .
O3 O 0.4204(4) 0.11358(18) 0.6490(3) 0.0420 1.0000 Uani . . . . . .
O4 O 0.2688(5) 0.16705(15) 0.6555(4) 0.0476 1.0000 Uani . . . . . .
C5 C 0.2410(4) 0.09437(14) 0.5386(4) 0.0192 1.0000 Uani . . . . . .
C6 C 0.2532(4) 0.07648(16) 0.4357(4) 0.0207 1.0000 Uani . . . . . .
C7 C 0.1865(4) 0.04012(15) 0.4006(4) 0.0179 1.0000 Uani . . . . . .
C8 C 0.1093(4) 0.02120(15) 0.4748(4) 0.0173 1.0000 Uani . . . . . .
O9 O 0.0499(3) -0.01640(11) 0.4418(3) 0.0257 1.0000 Uani . . . . . .
C10 C 0.0966(4) 0.03984(15) 0.5780(4) 0.0182 1.0000 Uani . . . . . .
C11 C 0.1622(4) 0.07663(16) 0.6086(4) 0.0198 1.0000 Uani . . . . . .
H111 H 0.1538 0.0897 0.6785 0.0221 1.0000 Uiso R . . . . .
C12 C 0.0113(4) 0.01997(15) 0.6574(4) 0.0192 1.0000 Uani . . . . . .
C13 C -0.1009(4) 0.04383(15) 0.6503(3) 0.0167 1.0000 Uani . . . . . .
C14 C -0.1836(4) 0.03110(15) 0.5731(3) 0.0173 1.0000 Uani . . . . . .
O15 O -0.1609(3) -0.00666(11) 0.5108(3) 0.0239 1.0000 Uani . . . . . .
C16 C -0.2871(4) 0.05379(15) 0.5635(4) 0.0196 1.0000 Uani . . . . . .
C17 C -0.3730(4) 0.04088(16) 0.4771(4) 0.0208 1.0000 Uani . . . . . .
C18 C -0.3490(4) 0.06288(16) 0.3676(3) 0.0197 1.0000 Uani . . . . . .
C19 C -0.2836(4) 0.04164(15) 0.2904(4) 0.0196 1.0000 Uani . . . . . .
O20 O -0.2474(3) -0.00197(11) 0.3105(3) 0.0240 1.0000 Uani . . . . . .
C21 C -0.2579(4) 0.06255(15) 0.1910(3) 0.0172 1.0000 Uani . . . . . .
C22 C -0.2993(4) 0.10667(16) 0.1724(4) 0.0206 1.0000 Uani . . . . . .
C23 C -0.3670(4) 0.12773(16) 0.2481(4) 0.0226 1.0000 Uani . . . . . .
C24 C -0.3920(4) 0.10647(16) 0.3445(4) 0.0209 1.0000 Uani . . . . . .
H241 H -0.4384 0.1216 0.3954 0.0254 1.0000 Uiso R . . . . .
S25 S -0.42730(13) 0.18120(4) 0.21311(11) 0.0281 1.0000 Uani . . . . . .
O26 O -0.4544(4) 0.20485(12) 0.3123(3) 0.0321 1.0000 Uani . . . . . .
Na27 Na -0.3652(2) 0.25880(7) 0.4251(2) 0.0358 1.0000 Uani . . . . . .
O28 O -0.5141(4) 0.31737(16) 0.3917(4) 0.0459 1.0000 Uani . . . . . .
S29 S -0.53516(13) 0.34296(5) 0.29371(12) 0.0298 1.0000 Uani . . . . . .
O30 O -0.4345(4) 0.36090(19) 0.2441(5) 0.0549 1.0000 Uani . . . . . .
O31 O -0.6012(5) 0.3186(2) 0.2149(4) 0.0570 1.0000 Uani . . . . . .
C32 C -0.6151(4) 0.39179(17) 0.3291(4) 0.0223 1.0000 Uani . . . . . .
C33 C -0.5956(4) 0.41300(17) 0.4272(4) 0.0216 1.0000 Uani . . . . . .
C34 C -0.6529(4) 0.45248(16) 0.4535(3) 0.0183 1.0000 Uani . . . . . .
C35 C -0.6369(4) 0.47482(16) 0.5643(4) 0.0212 1.0000 Uani . . . . . .
C36 C -0.7154(4) 0.45624(16) 0.6479(3) 0.0197 1.0000 Uani . . . . . .
C37 C -0.8259(4) 0.47279(16) 0.6590(4) 0.0220 1.0000 Uani . . . . . .
O38 O -0.8629(3) 0.50924(12) 0.5996(3) 0.0256 1.0000 Uani . . . . . .
C39 C -0.9003(4) 0.45404(17) 0.7337(4) 0.0222 1.0000 Uani . . . . . .
C40 C -0.8625(4) 0.41816(18) 0.7994(4) 0.0262 1.0000 Uani . . . . . .
C41 C -0.7537(5) 0.40216(17) 0.7910(4) 0.0249 1.0000 Uani . . . . . .
C42 C -0.6812(4) 0.42079(17) 0.7161(4) 0.0225 1.0000 Uani . . . . . .
H421 H -0.6073 0.4088 0.7113 0.0267 1.0000 Uiso R . . . . .
S43 S -0.70818(15) 0.35709(6) 0.87633(15) 0.0451 1.0000 Uani . . . . . .
O44 O -0.5987(5) 0.34359(17) 0.8384(4) 0.0492 1.0000 Uani . . . . . .
O45 O -0.7033(5) 0.3752(3) 0.9859(4) 0.0766 1.0000 Uani . . . . . .
O46 O -0.7891(6) 0.3204(2) 0.8627(7) 0.0829 1.0000 Uani . . . . . .
H401 H -0.9121 0.4045 0.8497 0.0309 1.0000 Uiso R . . . . .
C47 C -1.0198(4) 0.47173(17) 0.7417(4) 0.0232 1.0000 Uani . . . . . .
C48 C -1.0978(4) 0.44902(16) 0.6604(4) 0.0197 1.0000 Uani . . . . . .
C49 C -1.1231(4) 0.46753(15) 0.5590(4) 0.0192 1.0000 Uani . . . . . .
O50 O -1.0815(3) 0.51033(11) 0.5299(3) 0.0264 1.0000 Uani . . . . . .
C51 C -1.1921(4) 0.44574(17) 0.4816(4) 0.0207 1.0000 Uani . . . . . .
C52 C -1.2145(4) 0.46605(16) 0.3702(4) 0.0205 1.0000 Uani . . . . . .
C53 C -1.1323(4) 0.44906(15) 0.2849(3) 0.0179 1.0000 Uani . . . . . .
C54 C -1.1650(4) 0.41480(16) 0.2109(4) 0.0200 1.0000 Uani . . . . . .
C55 C -1.0915(4) 0.39894(16) 0.1337(3) 0.0214 1.0000 Uani . . . . . .
S56 S -1.13844(14) 0.36122(5) 0.03123(12) 0.0321 1.0000 Uani . . . . . .
O57 O -1.1606(7) 0.3919(3) -0.0594(4) 0.0779 1.0000 Uani . . . . . .
O58 O -1.2424(5) 0.3419(2) 0.0656(5) 0.0597 1.0000 Uani . . . . . .
O59 O -1.0510(6) 0.3300(3) 0.0107(7) 0.0954 1.0000 Uani . . . . . .
C60 C -0.9832(4) 0.41657(17) 0.1279(4) 0.0232 1.0000 Uani . . . . . .
C61 C -0.9475(4) 0.45072(16) 0.1988(4) 0.0207 1.0000 Uani . . . . . .
C62 C -1.0239(4) 0.46751(16) 0.2742(4) 0.0204 1.0000 Uani . . . . . .
O63 O -0.9915(3) 0.50376(13) 0.3357(3) 0.0293 1.0000 Uani . . . . . .
H631 H -1.0450 0.5053 0.3780 0.0500 1.0000 Uiso R . . . . .
C64 C -0.8293(4) 0.46990(19) 0.1917(4) 0.0268 1.0000 Uani . . . . . .
C65 C -0.7477(4) 0.45007(16) 0.2766(4) 0.0222 1.0000 Uani . . . . . .
C66 C -0.7268(4) 0.47129(14) 0.3764(4) 0.0182 1.0000 Uani . . . . . .
O67 O -0.7781(3) 0.51190(12) 0.4009(3) 0.0286 1.0000 Uani . . . . . .
H671 H -0.8073 0.5168 0.3603 0.0500 1.0000 Uiso R . . . . .
C68 C -0.6896(4) 0.40916(17) 0.2529(3) 0.0215 1.0000 Uani . . . . . .
H681 H -0.7017 0.3938 0.1859 0.0255 1.0000 Uiso R . . . . .
H642 H -0.8326 0.5022 0.2016 0.0337 1.0000 Uiso R . . . . .
H641 H -0.8016 0.4633 0.1216 0.0337 1.0000 Uiso R . . . . .
H601 H -0.9330 0.4052 0.0750 0.0296 1.0000 Uiso R . . . . .
H541 H -1.2389 0.4026 0.2142 0.0262 1.0000 Uiso R . . . . .
H521 H -1.2085 0.4984 0.3752 0.0248 1.0000 Uiso R . . . . .
H522 H -1.2885 0.4580 0.3477 0.0248 1.0000 Uiso R . . . . .
C69 C -1.2402(4) 0.40413(18) 0.5093(4) 0.0261 1.0000 Uani . . . . . .
C70 C -1.2180(5) 0.38513(17) 0.6109(4) 0.0264 1.0000 Uani . . . . . .
C71 C -1.1478(5) 0.40667(19) 0.6852(4) 0.0290 1.0000 Uani . . . . . .
H711 H -1.1325 0.3927 0.7533 0.0382 1.0000 Uiso R . . . . .
S72 S -1.2815(2) 0.33298(7) 0.64956(13) 0.0623 1.0000 Uani . . . . . .
O73 O -1.3078(8) 0.3082(2) 0.5567(5) 0.1014 1.0000 Uani . . . . . .
O74 O -1.2173(12) 0.3143(3) 0.7338(8) 0.1443 1.0000 Uani . . . . . .
O75 O -1.3909(10) 0.3483(4) 0.6951(8) 0.1371 1.0000 Uani . . . . . .
H691 H -1.2886 0.3888 0.4595 0.0334 1.0000 Uiso R . . . . .
H472 H -1.0197 0.5038 0.7291 0.0295 1.0000 Uiso R . . . . .
H471 H -1.0462 0.4657 0.8127 0.0295 1.0000 Uiso R . . . . .
H351 H -0.6503 0.5068 0.5568 0.0257 1.0000 Uiso R . . . . .
H352 H -0.5618 0.4699 0.5883 0.0257 1.0000 Uiso R . . . . .
H331 H -0.5435 0.4001 0.4777 0.0274 1.0000 Uiso R . . . . .
O76 O -0.4371(4) 0.21378(15) 0.5671(4) 0.0414 1.0000 Uani . . . . . .
O77 O -0.2671(4) 0.2936(2) 0.2835(5) 0.0616 1.0000 Uani . . . . . .
O78 O -0.2032(8) 0.2110(4) 0.4153(12) 0.1250 1.0000 Uani . . . . . .
C79 C -0.1392(11) 0.1934(3) 0.4804(12) 0.0801 1.0000 Uani . . . . . .
O80 O -0.1211(16) 0.2106(5) 0.5741(12) 0.1739 1.0000 Uani . . . . . .
C81 C -0.0825(9) 0.1481(4) 0.4588(15) 0.1066 1.0000 Uani . . . . . .
C82 C -0.0099(11) 0.1503(3) 0.3616(15) 0.1059 1.0000 Uani . . . . . .
C83 C 0.0888(9) 0.1845(3) 0.3696(7) 0.0659 1.0000 Uani . . . . . .
C84 C 0.1581(11) 0.1886(3) 0.2797(8) 0.0759 1.0000 Uani . . . . . .
C85 C 0.2572(12) 0.2236(3) 0.2978(8) 0.0809 1.0000 Uani . . . . . .
N86 N 0.3015(8) 0.2312(4) 0.1830(13) 0.1295 1.0000 Uani . . . . . .
H822 H -0.0566 0.1622 0.3053 0.1456 1.0000 Uiso R . . . . .
H821 H 0.0169 0.1209 0.3414 0.1456 1.0000 Uiso R . . . . .
H812 H -0.0331 0.1383 0.5152 0.1613 1.0000 Uiso R . . . . .
H811 H -0.1415 0.1265 0.4499 0.1613 1.0000 Uiso R . . . . .
O87 O -0.5280(5) 0.17003(18) 0.1496(4) 0.0562 1.0000 Uani . . . . . .
O88 O -0.3441(5) 0.20520(17) 0.1486(4) 0.0565 1.0000 Uani . . . . . .
H221 H -0.2821 0.1222 0.1070 0.0253 1.0000 Uiso R . . . . .
C89 C -0.1846(4) 0.03992(15) 0.1060(3) 0.0190 1.0000 Uani . . . . . .
C90 C -0.0617(4) 0.05332(16) 0.1164(3) 0.0202 1.0000 Uani . . . . . .
C91 C 0.0098(4) 0.03094(15) 0.1883(3) 0.0183 1.0000 Uani . . . . . .
O92 O -0.0325(3) -0.00526(11) 0.2453(3) 0.0264 1.0000 Uani . . . . . .
C93 C 0.1216(4) 0.04382(16) 0.2031(3) 0.0190 1.0000 Uani . . . . . .
C94 C 0.1988(4) 0.02073(16) 0.2865(4) 0.0223 1.0000 Uani . . . . . .
H941 H 0.2743 0.0253 0.2651 0.0273 1.0000 Uiso R . . . . .
H942 H 0.1829 -0.0112 0.2882 0.0273 1.0000 Uiso R . . . . .
C95 C 0.1636(4) 0.07968(18) 0.1386(4) 0.0244 1.0000 Uani . . . . . .
C96 C 0.0926(4) 0.10076(18) 0.0640(4) 0.0246 1.0000 Uani . . . . . .
C97 C -0.0196(4) 0.08879(16) 0.0525(4) 0.0214 1.0000 Uani . . . . . .
H971 H -0.0665 0.1048 0.0025 0.0284 1.0000 Uiso R . . . . .
S98 S 0.14745(14) 0.14375(6) -0.02322(14) 0.0383 1.0000 Uani . . . . . .
O99 O 0.2574(4) 0.15633(15) 0.0186(4) 0.0378 1.0000 Uani . . . . . .
O100 O 0.1540(5) 0.1219(2) -0.1290(4) 0.0625 1.0000 Uani . . . . . .
O101 O 0.0694(5) 0.1821(2) -0.0234(6) 0.0723 1.0000 Uani . . . . . .
H951 H 0.2395 0.0892 0.1461 0.0303 1.0000 Uiso R . . . . .
H892 H -0.2113 0.0490 0.0363 0.0257 1.0000 Uiso R . . . . .
H891 H -0.1911 0.0076 0.1131 0.0257 1.0000 Uiso R . . . . .
H172 H -0.4452 0.0504 0.5003 0.0271 1.0000 Uiso R . . . . .
H171 H -0.3723 0.0085 0.4684 0.0271 1.0000 Uiso R . . . . .
C102 C -0.3084(4) 0.08927(17) 0.6340(4) 0.0232 1.0000 Uani . . . . . .
C103 C -0.2290(4) 0.10223(16) 0.7121(3) 0.0225 1.0000 Uani . . . . . .
C104 C -0.1258(4) 0.08003(17) 0.7200(4) 0.0240 1.0000 Uani . . . . . .
H1041 H -0.0718 0.0898 0.7724 0.0318 1.0000 Uiso R . . . . .
S105 S -0.26044(15) 0.14440(6) 0.80988(13) 0.0396 1.0000 Uani . . . . . .
O106 O -0.3028(5) 0.1199(2) 0.9034(4) 0.0642 1.0000 Uani . . . . . .
O107 O -0.1553(6) 0.1668(3) 0.8392(6) 0.0792 1.0000 Uani . . . . . .
O108 O -0.3428(5) 0.17477(18) 0.7621(4) 0.0549 1.0000 Uani . . . . . .
H1021 H -0.3777 0.1053 0.6290 0.0290 1.0000 Uiso R . . . . .
H122 H 0.0408 0.0234 0.7288 0.0260 1.0000 Uiso R . . . . .
H121 H 0.0014 -0.0117 0.6419 0.0260 1.0000 Uiso R . . . . .
H61 H 0.3073 0.0894 0.3886 0.0239 1.0000 Uiso R . . . . .
O109 O 0.3651(4) 0.09068(14) 0.8450(3) 0.0389 1.0000 Uani . . . . . .
O110 O 0.6295(5) 0.39709(18) 0.8777(4) 0.0548 1.0000 Uani . . . . . .
O111 O 0.5150(5) 0.3974(2) 0.0398(4) 0.0621 1.0000 Uani . . . . . .
O112 O 0.4923(6) 0.1116(3) 0.9869(5) 0.0735 1.0000 Uani . . . . . .
O113 O 0.6912(7) 0.27310(17) 0.0836(6) 0.0749 1.0000 Uani . . . . . .
O114 O 0.0520(6) 0.1860(2) 0.7268(7) 0.0821 1.0000 Uani . . . . . .
O115 O 0.1343(12) 0.3380(5) 0.2839(15) 0.0882 0.512(16) Uani D U P 1 1 .
O116 O 0.1265(11) 0.3190(9) 0.2845(14) 0.1028 0.488(16) Uani D U P 1 2 .
C117 C 0.0207(10) 0.3139(7) 0.3054(12) 0.0713 0.488(16) Uani D U P 1 2 .
C118 C 0.0464(10) 0.3317(5) 0.3428(10) 0.0654 0.512(16) Uani D U P 1 1 .
O119 O -0.0334(9) 0.3067(5) 0.3047(10) 0.0587 0.512(16) Uani D U P 1 1 .
C120 C -0.0260(10) 0.3325(6) 0.4084(11) 0.0730 0.488(16) Uani D U P 1 2 .
C121 C 0.0301(16) 0.3614(4) 0.4416(11) 0.0746 0.512(16) Uani D U P 1 1 .
C122 C 0.0654(13) 0.3436(4) 0.4905(13) 0.0814 0.488(16) Uani D U P 1 2 .
C123 C 0.0305(13) 0.3351(6) 0.5449(11) 0.0825 0.512(16) Uani D U P 1 1 .
C124 C 0.1207(9) 0.3004(3) 0.5410(9) 0.0829 1.0000 Uani D U . . . .
C125 C 0.2366(9) 0.3158(3) 0.5664(8) 0.0659 1.0000 Uani D U . . . .
C126 C 0.3139(8) 0.2782(3) 0.5995(7) 0.0615 1.0000 Uani . U . . . .
N127 N 0.4260(6) 0.2941(3) 0.6212(8) 0.0693 1.0000 Uani . U . . . .
H1261 H 0.2842 0.2657 0.6642 0.0802 1.0000 Uiso R . . . . .
H1262 H 0.3148 0.2553 0.5448 0.0802 1.0000 Uiso R . . . . .
H1252 H 0.2374 0.3397 0.6189 0.0847 1.0000 Uiso R . . . . .
H1251 H 0.2623 0.3275 0.4992 0.0847 1.0000 Uiso R . . . . .
O128 O -0.0418(11) 0.2881(5) 0.2439(14) 0.0821 0.488(16) Uani D U P 1 2 .
O129 O 0.1589(9) 0.2950(5) 0.0921(9) 0.1568 1.0000 Uani . . . . . .
O130 O 0.7244(12) 0.2584(3) 0.9074(10) 0.1413 1.0000 Uani . . . . . .
O131 O -0.0004(10) 0.2714(4) 0.8199(8) 0.1142 1.0000 Uani . . . . . .
O132 O -0.0593(18) 0.2370(5) 0.9798(15) 0.3408 1.0000 Uani . . . . . .
H1221 H 0.0347 0.3619 0.5465 0.1062 0.488(16) Uiso R . P 1 2 .
H1222 H 0.1226 0.3603 0.4547 0.1062 0.488(16) Uiso R . P 1 2 .
H1201 H -0.0663 0.3599 0.3925 0.0998 0.488(16) Uiso R . P 1 2 .
H1202 H -0.0754 0.3107 0.4391 0.0998 0.488(16) Uiso R . P 1 2 .
H1211 H 0.0912 0.3823 0.4439 0.1035 0.512(16) Uiso R . P 1 1 .
H1212 H -0.0384 0.3779 0.4343 0.1035 0.512(16) Uiso R . P 1 1 .
H1231 H 0.0458 0.3555 0.6032 0.1127 0.512(16) Uiso R . P 1 1 .
H1232 H -0.0412 0.3215 0.5542 0.1127 0.512(16) Uiso R . P 1 1 .
H1241 H 0.1019 0.2779 0.5934 0.1060 0.5028 Uiso R . . . . .
H1242 H 0.1188 0.2870 0.4708 0.1060 0.5028 Uiso R . . . . .
H1243 H 0.0836 0.2923 0.6059 0.1060 0.4972 Uiso R . . . . .
H1244 H 0.1190 0.2752 0.4923 0.1060 0.4972 Uiso R . . . . .
H1271 H 0.4719 0.2690 0.6427 0.0842 1.0000 Uiso R . . . . .
H1272 H 0.4257 0.3164 0.6775 0.0842 1.0000 Uiso R . . . . .
H1273 H 0.4549 0.3074 0.5572 0.0842 1.0000 Uiso R . . . . .
H841 H 0.1130 0.1995 0.2211 0.0990 1.0000 Uiso R . . . . .
H842 H 0.1873 0.1593 0.2622 0.0990 1.0000 Uiso R . . . . .
H831 H 0.0589 0.2139 0.3852 0.0856 1.0000 Uiso R . . . . .
H832 H 0.1355 0.1748 0.4282 0.0856 1.0000 Uiso R . . . . .
H851 H 0.2322 0.2510 0.3312 0.0970 1.0000 Uiso R . . . . .
H852 H 0.3143 0.2099 0.3415 0.0970 1.0000 Uiso R . . . . .
H861 H 0.3630 0.2517 0.1862 0.1253 1.0000 Uiso R . . . . .
H862 H 0.2427 0.2443 0.1396 0.1253 1.0000 Uiso R . . . . .
H863 H 0.3248 0.2032 0.1499 0.1253 1.0000 Uiso R . . . . .
H751 H 0.6973 0.3952 0.8970 0.0675 1.0000 Uiso R . . . . .
H752 H 0.6226 0.3813 0.8183 0.0675 1.0000 Uiso R . . . . .
H771 H -0.1967 0.2976 0.2903 0.0728 1.0000 Uiso R . . . . .
H772 H -0.3174 0.3137 0.2718 0.0728 1.0000 Uiso R . . . . .
H761 H -0.4091 0.2023 0.6247 0.0497 1.0000 Uiso R . . . . .
H762 H -0.4918 0.1977 0.5440 0.0497 1.0000 Uiso R . . . . .
H1111 H 0.5308 0.3864 0.1019 0.0733 1.0000 Uiso R . . . . .
H1112 H 0.4477 0.3907 0.0230 0.0733 1.0000 Uiso R . . . . .
H1091 H 0.3831 0.0981 0.7810 0.0478 1.0000 Uiso R . . . . .
H1092 H 0.2984 0.1005 0.8533 0.0478 1.0000 Uiso R . . . . .
H1151 H 0.1428 0.3229 0.2222 0.1157 0.512(16) Uiso R . P 1 1 .
H1161 H 0.1369 0.3115 0.2213 0.1296 0.488(16) Uiso R . P 1 2 .
H801 H -0.0699 0.2034 0.6199 0.2559 1.0000 Uiso R . . . . .
H501 H -1.0054 0.5100 0.5541 0.0326 1.0000 Uiso R . . . . .
H381 H -0.8327 0.5101 0.5288 0.0308 1.0000 Uiso R . . . . .
H91 H -0.0056 -0.0249 0.4939 0.0500 1.0000 Uiso R . . . . .
H921 H -0.0026 -0.0093 0.3165 0.0324 1.0000 Uiso R . . . . .
H151 H -0.1916 -0.0050 0.4396 0.0290 1.0000 Uiso R . . . . .
H201 H -0.1717 -0.0032 0.2876 0.0295 1.0000 Uiso R . . . . .
H1291 H 0.0923 0.3020 0.0673 0.1856 1.0000 Uiso R . . . . .
H1292 H 0.1997 0.2886 0.0382 0.1856 1.0000 Uiso R . . . . .
H1121 H 0.4854 0.1301 1.0397 0.0932 1.0000 Uiso R . . . . .
H1122 H 0.5576 0.1139 0.9603 0.0932 1.0000 Uiso R . . . . .
H1141 H 0.0860 0.1646 0.7751 0.1005 1.0000 Uiso R . . . . .
H1142 H 0.1257 0.1797 0.7020 0.1005 1.0000 Uiso R . . . . .
H1132 H 0.7063 0.2927 0.1318 0.0932 1.0000 Uiso R . . . . .
H1131 H 0.6720 0.2490 0.1138 0.0932 1.0000 Uiso R . . . . .
H1301 H 0.7115 0.2639 0.9741 0.1857 1.0000 Uiso R . . . . .
H1302 H 0.7423 0.2751 0.8541 0.1857 1.0000 Uiso R . . . . .
H1311 H 0.0610 0.2855 0.8324 0.1406 1.0000 Uiso R . . . . .
H1312 H 0.0153 0.2455 0.7919 0.1406 1.0000 Uiso R . . . . .
H1321 H -0.0098 0.2160 0.9787 0.3695 1.0000 Uiso R . . . . .
H1322 H -0.0567 0.2657 0.9894 0.3695 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.094(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 . 1.456(4) yes
S1 . O3 . 1.468(5) yes
S1 . O4 . 1.451(5) yes
S1 . C5 . 1.765(5) yes
C5 . C6 . 1.382(6) yes
C5 . C11 . 1.384(7) yes
C6 . C7 . 1.392(7) yes
C6 . H61 . 0.950 no
C7 . C8 . 1.417(6) yes
C7 . C94 . 1.525(6) yes
C8 . O9 . 1.365(6) yes
C8 . C10 . 1.395(6) yes
O9 . H91 . 0.960 no
C10 . C11 . 1.378(7) yes
C10 . C12 . 1.534(6) yes
C11 . H111 . 0.950 no
C12 . C13 . 1.507(6) yes
C12 . H122 . 0.950 no
C12 . H121 . 0.950 no
C13 . C14 . 1.411(6) yes
C13 . C104 . 1.397(7) yes
C14 . O15 . 1.372(6) yes
C14 . C16 . 1.403(6) yes
O15 . H151 . 0.949 no
C16 . C17 . 1.516(6) yes
C16 . C102 . 1.378(7) yes
C17 . C18 . 1.526(6) yes
C17 . H172 . 0.950 no
C17 . H171 . 0.950 no
C18 . C19 . 1.384(7) yes
C18 . C24 . 1.399(7) yes
C19 . O20 . 1.366(6) yes
C19 . C21 . 1.406(6) yes
O20 . H201 . 0.949 no
C21 . C22 . 1.397(7) yes
C21 . C89 . 1.524(6) yes
C22 . C23 . 1.385(7) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.378(7) yes
C23 . S25 . 1.769(5) yes
C24 . H241 . 0.950 no
S25 . O26 . 1.445(4) yes
S25 . O87 . 1.461(5) yes
S25 . O88 . 1.458(5) yes
O26 . Na27 . 2.347(4) yes
Na27 . O73 1_655 2.271(6) yes
Na27 . O28 . 2.493(5) yes
Na27 . O76 . 2.359(5) yes
Na27 . O77 . 2.346(6) yes
Na27 . O78 . 2.384(10) yes
O28 . S29 . 1.441(5) yes
S29 . O30 . 1.451(5) yes
S29 . O31 . 1.432(6) yes
S29 . C32 . 1.771(5) yes
C32 . C33 . 1.377(6) yes
C32 . C68 . 1.381(7) yes
C33 . C34 . 1.380(7) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.524(6) yes
C34 . C66 . 1.400(6) yes
C35 . C36 . 1.502(7) yes
C35 . H351 . 0.950 no
C35 . H352 . 0.950 no
C36 . C37 . 1.409(7) yes
C36 . C42 . 1.392(7) yes
C37 . O38 . 1.362(6) yes
C37 . C39 . 1.398(7) yes
O38 . H381 . 0.949 no
C39 . C40 . 1.395(7) yes
C39 . C47 . 1.517(7) yes
C40 . C41 . 1.382(7) yes
C40 . H401 . 0.950 no
C41 . C42 . 1.383(7) yes
C41 . S43 . 1.766(5) yes
C42 . H421 . 0.950 no
S43 . O44 . 1.445(5) yes
S43 . O45 . 1.451(6) yes
S43 . O46 . 1.449(7) yes
C47 . C48 . 1.512(6) yes
C47 . H472 . 0.950 no
C47 . H471 . 0.950 no
C48 . C49 . 1.393(6) yes
C48 . C71 . 1.407(7) yes
C49 . O50 . 1.393(6) yes
C49 . C51 . 1.404(6) yes
O50 . H501 . 0.950 no
C51 . C52 . 1.517(6) yes
C51 . C69 . 1.388(7) yes
C52 . C53 . 1.529(6) yes
C52 . H521 . 0.950 no
C52 . H522 . 0.950 no
C53 . C54 . 1.406(7) yes
C53 . C62 . 1.407(6) yes
C54 . C55 . 1.381(7) yes
C54 . H541 . 0.950 no
C55 . S56 . 1.763(5) yes
C55 . C60 . 1.390(7) yes
S56 . O57 . 1.454(6) yes
S56 . O58 . 1.429(5) yes
S56 . O59 . 1.409(6) yes
C60 . C61 . 1.389(7) yes
C60 . H601 . 0.950 no
C61 . C62 . 1.397(6) yes
C61 . C64 . 1.518(7) yes
C62 . O63 . 1.355(6) yes
O63 . H631 . 0.830 no
C64 . C65 . 1.534(7) yes
C64 . H642 . 0.950 no
C64 . H641 . 0.950 no
C65 . C66 . 1.397(7) yes
C65 . C68 . 1.412(7) yes
C66 . O67 . 1.369(6) yes
O67 . H671 . 0.624 no
C68 . H681 . 0.950 no
C69 . C70 . 1.393(7) yes
C69 . H691 . 0.950 no
C70 . C71 . 1.384(7) yes
C70 . S72 . 1.768(5) yes
C71 . H711 . 0.950 no
S72 . O73 . 1.387(6) yes
S72 . O74 . 1.394(9) yes
S72 . O75 . 1.495(12) yes
O76 . H761 . 0.851 no
O76 . H762 . 0.849 no
O77 . H771 . 0.850 no
O77 . H772 . 0.849 no
O78 . C79 . 1.214(16) yes
C79 . O80 . 1.277(18) yes
C79 . C81 . 1.511(16) yes
O80 . H801 . 0.853 no
C81 . C82 . 1.49(2) yes
C81 . H812 . 0.950 no
C81 . H811 . 0.950 no
C82 . C83 . 1.546(15) yes
C82 . H822 . 0.950 no
C82 . H821 . 0.950 no
C83 . C84 . 1.395(15) yes
C83 . H831 . 0.950 no
C83 . H832 . 0.950 no
C84 . C85 . 1.575(17) yes
C84 . H841 . 0.950 no
C84 . H842 . 0.950 no
C85 . N86 . 1.534(16) yes
C85 . H851 . 0.950 no
C85 . H852 . 0.950 no
N86 . H861 . 0.945 no
N86 . H862 . 0.955 no
N86 . H863 . 0.957 no
C89 . C90 . 1.518(6) yes
C89 . H892 . 0.950 no
C89 . H891 . 0.950 no
C90 . C91 . 1.386(7) yes
C90 . C97 . 1.398(6) yes
C91 . O92 . 1.368(6) yes
C91 . C93 . 1.394(6) yes
O92 . H921 . 0.950 no
C93 . C94 . 1.528(6) yes
C93 . C95 . 1.410(7) yes
C94 . H941 . 0.950 no
C94 . H942 . 0.950 no
C95 . C96 . 1.385(7) yes
C95 . H951 . 0.950 no
C96 . C97 . 1.386(7) yes
C96 . S98 . 1.783(5) yes
C97 . H971 . 0.950 no
S98 . O99 . 1.448(5) yes
S98 . O100 . 1.454(6) yes
S98 . O101 . 1.455(6) yes
C102 . C103 . 1.393(7) yes
C102 . H1021 . 0.950 no
C103 . C104 . 1.391(7) yes
C103 . S105 . 1.767(5) yes
C104 . H1041 . 0.950 no
S105 . O106 . 1.454(6) yes
S105 . O107 . 1.453(7) yes
S105 . O108 . 1.442(5) yes
O109 . H1091 . 0.849 no
O109 . H1092 . 0.851 no
O110 . H751 . 0.840 no
O110 . H752 . 0.869 no
O111 . H1111 . 0.850 no
O111 . H1112 . 0.848 no
O112 . H1121 . 0.850 no
O112 . H1122 . 0.850 no
O113 . H1132 . 0.843 no
O113 . H1131 . 0.828 no
O114 . H1141 . 0.950 no
O114 . H1142 . 0.950 no
O115 . C118 . 1.295(9) yes
O115 . H1151 . 0.887 no
O116 . C117 . 1.297(9) yes
O116 . H1161 . 0.820 no
C117 . C120 . 1.496(9) yes
C117 . O128 . 1.298(9) yes
C118 . O119 . 1.284(9) yes
C118 . C121 . 1.509(9) yes
C120 . C122 . 1.512(9) yes
C120 . H1201 . 0.950 no
C120 . H1202 . 0.950 no
C121 . C123 . 1.487(9) yes
C121 . H1211 . 0.950 no
C121 . H1212 . 0.950 no
C122 . C124 . 1.549(9) yes
C122 . H1221 . 0.950 no
C122 . H1222 . 0.950 no
C123 . C124 . 1.477(9) yes
C123 . H1231 . 0.950 no
C123 . H1232 . 0.950 no
C124 . C125 . 1.481(15) yes
C124 . H1241 . 0.950 no
C124 . H1242 . 0.950 no
C124 . H1243 . 0.950 no
C124 . H1244 . 0.950 no
C124 . C125 . 1.481(15) yes
C124 . H1241 . 0.950 no
C124 . H1242 . 0.950 no
C124 . H1243 . 0.950 no
C124 . H1244 . 0.950 no
C125 . C126 . 1.488(13) yes
C125 . H1252 . 0.950 no
C125 . H1251 . 0.950 no
C126 . N127 . 1.435(12) yes
C126 . H1261 . 0.950 no
C126 . H1262 . 0.950 no
N127 . H1271 . 0.952 no
N127 . H1272 . 0.951 no
N127 . H1273 . 0.948 no
O129 . H1291 . 0.870 no
O129 . H1292 . 0.849 no
O130 . H1301 . 0.853 no
O130 . H1302 . 0.848 no
O131 . H1311 . 0.851 no
O131 . H1312 . 0.852 no
O132 . H1321 . 0.850 no
O132 . H1322 . 0.848 no
H1241 . H1243 . 0.497 no
H1242 . H1244 . 0.435 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 . 112.1(3) yes
O2 . S1 . O4 . 115.2(3) yes
O3 . S1 . O4 . 109.8(3) yes
O2 . S1 . C5 . 107.1(2) yes
O3 . S1 . C5 . 105.5(2) yes
O4 . S1 . C5 . 106.5(3) yes
S1 . C5 . C6 . 119.8(4) yes
S1 . C5 . C11 . 119.3(3) yes
C6 . C5 . C11 . 120.8(4) yes
C5 . C6 . C7 . 120.5(4) yes
C5 . C6 . H61 . 119.4 no
C7 . C6 . H61 . 120.1 no
C6 . C7 . C8 . 117.9(4) yes
C6 . C7 . C94 . 120.6(4) yes
C8 . C7 . C94 . 121.4(4) yes
C7 . C8 . O9 . 117.3(4) yes
C7 . C8 . C10 . 121.1(4) yes
O9 . C8 . C10 . 121.6(4) yes
C8 . O9 . H91 . 111.4 no
C8 . C10 . C11 . 119.1(4) yes
C8 . C10 . C12 . 121.0(4) yes
C11 . C10 . C12 . 119.9(4) yes
C5 . C11 . C10 . 120.5(4) yes
C5 . C11 . H111 . 119.8 no
C10 . C11 . H111 . 119.7 no
C10 . C12 . C13 . 112.4(3) yes
C10 . C12 . H122 . 108.2 no
C13 . C12 . H122 . 108.8 no
C10 . C12 . H121 . 108.7 no
C13 . C12 . H121 . 109.3 no
H122 . C12 . H121 . 109.5 no
C12 . C13 . C14 . 121.9(4) yes
C12 . C13 . C104 . 120.6(4) yes
C14 . C13 . C104 . 117.5(4) yes
C13 . C14 . O15 . 116.7(4) yes
C13 . C14 . C16 . 122.5(4) yes
O15 . C14 . C16 . 120.7(4) yes
C14 . O15 . H151 . 113.7 no
C14 . C16 . C17 . 121.8(4) yes
C14 . C16 . C102 . 118.0(4) yes
C17 . C16 . C102 . 120.2(4) yes
C16 . C17 . C18 . 112.7(4) yes
C16 . C17 . H172 . 108.7 no
C18 . C17 . H172 . 108.9 no
C16 . C17 . H171 . 108.6 no
C18 . C17 . H171 . 108.4 no
H172 . C17 . H171 . 109.5 no
C17 . C18 . C19 . 122.3(4) yes
C17 . C18 . C24 . 119.4(4) yes
C19 . C18 . C24 . 118.4(4) yes
C18 . C19 . O20 . 118.1(4) yes
C18 . C19 . C21 . 122.4(4) yes
O20 . C19 . C21 . 119.4(4) yes
C19 . O20 . H201 . 106.2 no
C19 . C21 . C22 . 117.6(4) yes
C19 . C21 . C89 . 123.0(4) yes
C22 . C21 . C89 . 119.4(4) yes
C21 . C22 . C23 . 120.4(4) yes
C21 . C22 . H221 . 120.0 no
C23 . C22 . H221 . 119.6 no
C22 . C23 . C24 . 121.1(4) yes
C22 . C23 . S25 . 117.7(4) yes
C24 . C23 . S25 . 121.1(4) yes
C18 . C24 . C23 . 120.1(4) yes
C18 . C24 . H241 . 120.2 no
C23 . C24 . H241 . 119.7 no
C23 . S25 . O26 . 108.0(2) yes
C23 . S25 . O87 . 105.2(3) yes
O26 . S25 . O87 . 111.7(3) yes
C23 . S25 . O88 . 106.3(3) yes
O26 . S25 . O88 . 113.1(3) yes
O87 . S25 . O88 . 111.9(4) yes
S25 . O26 . Na27 . 135.9(3) yes
O26 . Na27 . O73 1_655 168.6(3) yes
O26 . Na27 . O28 . 92.68(19) yes
O73 1_655 Na27 . O28 . 83.7(3) yes
O26 . Na27 . O76 . 84.31(16) yes
O73 1_655 Na27 . O76 . 86.06(19) yes
O28 . Na27 . O76 . 103.95(19) yes
O26 . Na27 . O77 . 94.3(2) yes
O73 1_655 Na27 . O77 . 96.3(2) yes
O28 . Na27 . O77 . 86.51(19) yes
O76 . Na27 . O77 . 169.5(2) yes
O26 . Na27 . O78 . 86.4(3) yes
O73 1_655 Na27 . O78 . 99.9(5) yes
O28 . Na27 . O78 . 165.1(3) yes
O76 . Na27 . O78 . 90.7(3) yes
O77 . Na27 . O78 . 78.8(3) yes
Na27 . O28 . S29 . 127.6(2) yes
O28 . S29 . O30 . 113.9(3) yes
O28 . S29 . O31 . 113.6(3) yes
O30 . S29 . O31 . 110.0(4) yes
O28 . S29 . C32 . 107.4(2) yes
O30 . S29 . C32 . 105.2(3) yes
O31 . S29 . C32 . 106.0(3) yes
S29 . C32 . C33 . 119.6(4) yes
S29 . C32 . C68 . 118.0(4) yes
C33 . C32 . C68 . 122.2(4) yes
C32 . C33 . C34 . 120.2(4) yes
C32 . C33 . H331 . 120.0 no
C34 . C33 . H331 . 119.8 no
C33 . C34 . C35 . 120.7(4) yes
C33 . C34 . C66 . 118.4(4) yes
C35 . C34 . C66 . 120.8(4) yes
C34 . C35 . C36 . 112.9(4) yes
C34 . C35 . H351 . 108.3 no
C36 . C35 . H351 . 108.4 no
C34 . C35 . H352 . 108.8 no
C36 . C35 . H352 . 108.9 no
H351 . C35 . H352 . 109.5 no
C35 . C36 . C37 . 122.2(4) yes
C35 . C36 . C42 . 120.3(4) yes
C37 . C36 . C42 . 117.6(4) yes
C36 . C37 . O38 . 120.8(4) yes
C36 . C37 . C39 . 122.0(4) yes
O38 . C37 . C39 . 117.2(4) yes
C37 . O38 . H381 . 113.1 no
C37 . C39 . C40 . 118.3(4) yes
C37 . C39 . C47 . 120.8(4) yes
C40 . C39 . C47 . 120.9(4) yes
C39 . C40 . C41 . 120.4(5) yes
C39 . C40 . H401 . 119.7 no
C41 . C40 . H401 . 119.8 no
C40 . C41 . C42 . 120.7(5) yes
C40 . C41 . S43 . 119.2(4) yes
C42 . C41 . S43 . 120.1(4) yes
C36 . C42 . C41 . 121.1(5) yes
C36 . C42 . H421 . 120.1 no
C41 . C42 . H421 . 118.8 no
C41 . S43 . O44 . 106.3(3) yes
C41 . S43 . O45 . 107.0(3) yes
O44 . S43 . O45 . 112.0(3) yes
C41 . S43 . O46 . 106.4(3) yes
O44 . S43 . O46 . 111.2(4) yes
O45 . S43 . O46 . 113.3(5) yes
C39 . C47 . C48 . 112.1(4) yes
C39 . C47 . H472 . 108.8 no
C48 . C47 . H472 . 109.0 no
C39 . C47 . H471 . 108.6 no
C48 . C47 . H471 . 108.8 no
H472 . C47 . H471 . 109.5 no
C47 . C48 . C49 . 123.4(4) yes
C47 . C48 . C71 . 119.9(4) yes
C49 . C48 . C71 . 116.7(4) yes
C48 . C49 . O50 . 120.4(4) yes
C48 . C49 . C51 . 123.6(4) yes
O50 . C49 . C51 . 116.0(4) yes
C49 . O50 . H501 . 104.5 no
C49 . C51 . C52 . 122.3(4) yes
C49 . C51 . C69 . 117.9(4) yes
C52 . C51 . C69 . 119.8(4) yes
C51 . C52 . C53 . 113.0(4) yes
C51 . C52 . H521 . 108.6 no
C53 . C52 . H521 . 108.6 no
C51 . C52 . H522 . 108.7 no
C53 . C52 . H522 . 108.5 no
H521 . C52 . H522 . 109.5 no
C52 . C53 . C54 . 120.2(4) yes
C52 . C53 . C62 . 122.5(4) yes
C54 . C53 . C62 . 117.3(4) yes
C53 . C54 . C55 . 120.9(4) yes
C53 . C54 . H541 . 119.2 no
C55 . C54 . H541 . 119.9 no
C54 . C55 . S56 . 120.4(4) yes
C54 . C55 . C60 . 120.5(4) yes
S56 . C55 . C60 . 118.7(4) yes
C55 . S56 . O57 . 102.8(3) yes
C55 . S56 . O58 . 107.5(3) yes
O57 . S56 . O58 . 108.7(4) yes
C55 . S56 . O59 . 107.7(3) yes
O57 . S56 . O59 . 112.8(5) yes
O58 . S56 . O59 . 116.3(5) yes
C55 . C60 . C61 . 120.6(4) yes
C55 . C60 . H601 . 119.9 no
C61 . C60 . H601 . 119.5 no
C60 . C61 . C62 . 118.3(4) yes
C60 . C61 . C64 . 120.4(4) yes
C62 . C61 . C64 . 121.3(5) yes
C53 . C62 . C61 . 122.3(4) yes
C53 . C62 . O63 . 120.0(4) yes
C61 . C62 . O63 . 117.7(4) yes
C62 . O63 . H631 . 100.3 no
C61 . C64 . C65 . 113.7(4) yes
C61 . C64 . H642 . 108.6 no
C65 . C64 . H642 . 108.3 no
C61 . C64 . H641 . 108.0 no
C65 . C64 . H641 . 108.8 no
H642 . C64 . H641 . 109.5 no
C64 . C65 . C66 . 122.6(4) yes
C64 . C65 . C68 . 119.0(4) yes
C66 . C65 . C68 . 118.4(4) yes
C34 . C66 . C65 . 121.9(4) yes
C34 . C66 . O67 . 117.9(4) yes
C65 . C66 . O67 . 120.3(4) yes
C66 . O67 . H671 . 105.4 no
C65 . C68 . C32 . 118.7(4) yes
C65 . C68 . H681 . 120.7 no
C32 . C68 . H681 . 120.5 no
C51 . C69 . C70 . 119.8(4) yes
C51 . C69 . H691 . 120.2 no
C70 . C69 . H691 . 120.1 no
C69 . C70 . C71 . 121.4(4) yes
C69 . C70 . S72 . 120.6(4) yes
C71 . C70 . S72 . 118.0(4) yes
C48 . C71 . C70 . 120.6(5) yes
C48 . C71 . H711 . 119.6 no
C70 . C71 . H711 . 119.8 no
C70 . S72 . O73 . 108.6(3) yes
C70 . S72 . O74 . 107.8(4) yes
O73 . S72 . O74 . 121.8(7) yes
C70 . S72 . O75 . 102.8(4) yes
O73 . S72 . O75 . 106.1(6) yes
O74 . S72 . O75 . 108.0(8) yes
Na27 1_455 O73 . S72 . 169.9(4) yes
Na27 . O76 . H761 . 134.3 no
Na27 . O76 . H762 . 110.1 no
H761 . O76 . H762 . 110.7 no
Na27 . O77 . H771 . 119.0 no
Na27 . O77 . H772 . 94.0 no
H771 . O77 . H772 . 127.9 no
Na27 . O78 . C79 . 135.6(11) yes
O78 . C79 . O80 . 122.1(14) yes
O78 . C79 . C81 . 122.1(14) yes
O80 . C79 . C81 . 115.7(15) yes
C79 . O80 . H801 . 127.8 no
C79 . C81 . C82 . 111.8(10) yes
C79 . C81 . H812 . 114.1 no
C82 . C81 . H812 . 104.1 no
C79 . C81 . H811 . 105.8 no
C82 . C81 . H811 . 111.8 no
H812 . C81 . H811 . 109.5 no
C81 . C82 . C83 . 115.2(12) yes
C81 . C82 . H822 . 105.4 no
C83 . C82 . H822 . 104.3 no
C81 . C82 . H821 . 111.9 no
C83 . C82 . H821 . 110.1 no
H822 . C82 . H821 . 109.5 no
C82 . C83 . C84 . 117.5(10) yes
C82 . C83 . H831 . 108.0 no
C84 . C83 . H831 . 108.1 no
C82 . C83 . H832 . 107.0 no
C84 . C83 . H832 . 106.5 no
H831 . C83 . H832 . 109.5 no
C83 . C84 . C85 . 113.1(8) yes
C83 . C84 . H841 . 107.4 no
C85 . C84 . H841 . 107.9 no
C83 . C84 . H842 . 109.0 no
C85 . C84 . H842 . 109.9 no
H841 . C84 . H842 . 109.5 no
C84 . C85 . N86 . 103.2(9) yes
C84 . C85 . H851 . 111.7 no
N86 . C85 . H851 . 113.1 no
C84 . C85 . H852 . 109.7 no
N86 . C85 . H852 . 109.5 no
H851 . C85 . H852 . 109.5 no
C85 . N86 . H861 . 109.1 no
C85 . N86 . H862 . 108.5 no
H861 . N86 . H862 . 109.5 no
C85 . N86 . H863 . 112.0 no
H861 . N86 . H863 . 109.3 no
H862 . N86 . H863 . 108.5 no
C21 . C89 . C90 . 112.9(3) yes
C21 . C89 . H892 . 108.3 no
C90 . C89 . H892 . 108.4 no
C21 . C89 . H891 . 108.6 no
C90 . C89 . H891 . 109.1 no
H892 . C89 . H891 . 109.5 no
C89 . C90 . C91 . 121.1(4) yes
C89 . C90 . C97 . 119.7(4) yes
C91 . C90 . C97 . 119.2(4) yes
C90 . C91 . O92 . 117.8(4) yes
C90 . C91 . C93 . 122.4(4) yes
O92 . C91 . C93 . 119.9(4) yes
C91 . O92 . H921 . 115.7 no
C91 . C93 . C94 . 122.3(4) yes
C91 . C93 . C95 . 118.1(4) yes
C94 . C93 . C95 . 119.6(4) yes
C93 . C94 . C7 . 113.2(3) yes
C93 . C94 . H941 . 108.3 no
C7 . C94 . H941 . 107.9 no
C93 . C94 . H942 . 109.1 no
C7 . C94 . H942 . 108.8 no
H941 . C94 . H942 . 109.5 no
C93 . C95 . C96 . 119.2(5) yes
C93 . C95 . H951 . 120.4 no
C96 . C95 . H951 . 120.4 no
C95 . C96 . C97 . 122.3(5) yes
C95 . C96 . S98 . 119.3(4) yes
C97 . C96 . S98 . 118.4(4) yes
C90 . C97 . C96 . 118.7(4) yes
C90 . C97 . H971 . 121.2 no
C96 . C97 . H971 . 120.1 no
C96 . S98 . O99 . 107.4(2) yes
C96 . S98 . O100 . 104.9(3) yes
O99 . S98 . O100 . 111.8(3) yes
C96 . S98 . O101 . 107.7(3) yes
O99 . S98 . O101 . 112.3(4) yes
O100 . S98 . O101 . 112.1(4) yes
C16 . C102 . C103 . 120.8(4) yes
C16 . C102 . H1021 . 119.7 no
C103 . C102 . H1021 . 119.5 no
C102 . C103 . C104 . 120.8(4) yes
C102 . C103 . S105 . 120.9(4) yes
C104 . C103 . S105 . 118.1(4) yes
C13 . C104 . C103 . 120.3(5) yes
C13 . C104 . H1041 . 119.9 no
C103 . C104 . H1041 . 119.8 no
C103 . S105 . O106 . 106.1(3) yes
C103 . S105 . O107 . 107.1(3) yes
O106 . S105 . O107 . 109.2(4) yes
C103 . S105 . O108 . 107.3(3) yes
O106 . S105 . O108 . 112.7(3) yes
O107 . S105 . O108 . 113.9(4) yes
H1091 . O109 . H1092 . 105.8 no
H751 . O110 . H752 . 106.6 no
H1111 . O111 . H1112 . 109.3 no
H1121 . O112 . H1122 . 110.1 no
H1132 . O113 . H1131 . 108.5 no
H1141 . O114 . H1142 . 71.8 no
C118 . O115 . H1151 . 120.9 no
C117 . O116 . H1161 . 108.6 no
O116 . C117 . C120 . 120.0(7) yes
O116 . C117 . O128 . 120.0(8) yes
C120 . C117 . O128 . 119.4(7) yes
O115 . C118 . O119 . 118.3(7) yes
O115 . C118 . C121 . 119.0(7) yes
O119 . C118 . C121 . 121.4(7) yes
C117 . C120 . C122 . 112.0(8) yes
C117 . C120 . H1201 . 108.7 no
C122 . C120 . H1201 . 108.5 no
C117 . C120 . H1202 . 109.4 no
C122 . C120 . H1202 . 108.7 no
H1201 . C120 . H1202 . 109.5 no
C118 . C121 . C123 . 113.4(8) yes
C118 . C121 . H1211 . 106.7 no
C123 . C121 . H1211 . 108.1 no
C118 . C121 . H1212 . 109.5 no
C123 . C121 . H1212 . 109.7 no
H1211 . C121 . H1212 . 109.5 no
C120 . C122 . C124 . 113.2(8) yes
C120 . C122 . H1221 . 109.1 no
C124 . C122 . H1221 . 109.4 no
C120 . C122 . H1222 . 108.2 no
C124 . C122 . H1222 . 107.5 no
H1221 . C122 . H1222 . 109.5 no
C121 . C123 . C124 . 108.7(7) yes
C121 . C123 . H1231 . 108.9 no
C124 . C123 . H1231 . 108.8 no
C121 . C123 . H1232 . 109.0 no
C124 . C123 . H1232 . 111.8 no
H1231 . C123 . H1232 . 109.5 no
C123 . C124 . C125 . 117.4(8) yes
C123 . C124 . H1241 . 105.9 no
C125 . C124 . H1241 . 107.0 no
C123 . C124 . H1242 . 107.6 no
C125 . C124 . H1242 . 109.2 no
H1241 . C124 . H1242 . 109.5 no
C123 . C124 . H1243 . 78.4 no
C125 . C124 . H1243 . 109.9 no
H1241 . C124 . H1243 . 30.3 no
H1242 . C124 . H1243 . 131.3 no
C123 . C124 . H1244 . 122.8 no
C125 . C124 . H1244 . 112.4 no
H1241 . C124 . H1244 . 83.8 no
H1242 . C124 . H1244 . 26.5 no
H1243 . C124 . H1244 . 109.5 no
C122 . C124 . C125 . 103.1(7) yes
C122 . C124 . H1241 . 137.2 no
C125 . C124 . H1241 . 107.0 no
C122 . C124 . H1242 . 87.9 no
C125 . C124 . H1242 . 109.2 no
H1241 . C124 . H1242 . 109.5 no
C122 . C124 . H1243 . 110.1 no
C125 . C124 . H1243 . 109.9 no
H1241 . C124 . H1243 . 30.3 no
H1242 . C124 . H1243 . 131.3 no
C122 . C124 . H1244 . 111.7 no
C125 . C124 . H1244 . 112.4 no
H1241 . C124 . H1244 . 83.8 no
H1242 . C124 . H1244 . 26.5 no
H1243 . C124 . H1244 . 109.5 no
C124 . C125 . C126 . 113.9(7) yes
C124 . C125 . H1252 . 111.6 no
C126 . C125 . H1252 . 110.6 no
C124 . C125 . H1251 . 103.5 no
C126 . C125 . H1251 . 107.4 no
H1252 . C125 . H1251 . 109.5 no
C125 . C126 . N127 . 112.5(8) yes
C125 . C126 . H1261 . 106.2 no
N127 . C126 . H1261 . 108.9 no
C125 . C126 . H1262 . 109.7 no
N127 . C126 . H1262 . 110.1 no
H1261 . C126 . H1262 . 109.5 no
C126 . N127 . H1271 . 109.4 no
C126 . N127 . H1272 . 110.3 no
H1271 . N127 . H1272 . 109.2 no
C126 . N127 . H1273 . 108.9 no
H1271 . N127 . H1273 . 109.5 no
H1272 . N127 . H1273 . 109.6 no
H1291 . O129 . H1292 . 107.7 no
H1301 . O130 . H1302 . 133.6 no
H1311 . O131 . H1312 . 108.0 no
H1321 . O132 . H1322 . 133.6 no
C124 . H1241 . H1243 . 74.8 no
C124 . H1242 . H1244 . 76.8 no
C124 . H1243 . H1241 . 74.8 no
C124 . H1244 . H1242 . 76.8 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
C11 . H111 . O100 1_556 173.48(18) 0.950 2.555 3.500(9) yes
O63 . H631 . O50 . 142.83(16) 0.830 1.934 2.643(9) yes
O63 . H631 . C52 . 128.41(15) 0.830 2.321 2.910(9) yes
C68 . H681 . O45 1_554 161.9(2) 0.950 2.527 3.443(9) yes
C71 . H711 . O57 1_556 148.2(3) 0.950 2.339 3.186(9) yes
C22 . H221 . O106 1_554 144.5(2) 0.950 2.522 3.341(9) yes
C102 . H1021 . O3 1_455 154.30(16) 0.950 2.432 3.314(9) yes
C121 . H1222 . C125 . 132.4(13) 1.111 2.319 3.176(9) yes
C124 . H1242 . O116 . 133.5(6) 0.950 2.484 3.213(9) yes
C124 . H1242 . C117 . 129.0(4) 0.950 2.467 3.152(9) yes
N127 . H1271 . O76 1_655 138.1(3) 0.952 2.160 2.938(9) yes
N127 . H1272 . O44 1_655 157.5(3) 0.951 2.161 3.061(9) yes
N127 . H1273 . O28 1_655 159.6(3) 0.948 2.099 3.006(9) yes
C85 . H851 . O116 . 138.9(5) 0.950 2.415 3.192(9) yes
C85 . H852 . O2 . 152.7(3) 0.950 2.463 3.336(9) yes
N86 . H861 . O31 1_655 140.9(3) 0.945 2.029 2.826(9) yes
N86 . H862 . O129 . 150.9(6) 0.955 1.877 2.750(9) yes
N86 . H863 . O87 1_655 132.3(5) 0.957 2.002 2.739(9) yes
N86 . H863 . O99 . 136.1(3) 0.957 2.260 3.024(9) yes
O110 . H751 . O57 1_756 178.6(3) 0.840 1.772 2.611(9) yes
O110 . H752 . O75 1_755 179.6(5) 0.869 1.804 2.673(9) yes
O77 . H771 . O119 . 179.5(4) 0.850 1.967 2.817(9) yes
O77 . H771 . O128 . 152.1(5) 0.850 1.957 2.737(9) yes
O77 . H772 . O30 . 179.8(2) 0.849 1.986 2.835(9) yes
O76 . H761 . O108 . 179.8(2) 0.851 2.027 2.878(9) yes
O76 . H762 . O2 1_455 179.9(2) 0.849 1.998 2.847(9) yes
O111 . H1111 . O30 1_655 179.4(2) 0.850 1.945 2.795(9) yes
O111 . H1112 . O45 1_654 179.6(3) 0.848 1.904 2.752(9) yes
O109 . H1091 . O3 . 179.9(2) 0.849 1.753 2.602(9) yes
O109 . H1092 . O100 1_556 179.7(2) 0.851 1.845 2.696(9) yes
O115 . H1151 . O129 . 176.9(6) 0.887 1.812 2.698(9) yes
O116 . H1151 . O129 . 144.3(20) 0.803 1.812 2.509(9) yes
O115 . H1161 . O129 . 151.0(19) 1.093 1.689 2.698(9) yes
O116 . H1161 . O129 . 178.7(9) 0.820 1.689 2.509(9) yes
O80 . H801 . O114 . 179.5(5) 0.853 2.014 2.867(9) yes
O50 . H501 . O38 . 179.83(15) 0.950 1.781 2.731(9) yes
O38 . H381 . C66 . 149.89(12) 0.949 2.544 3.399(9) yes
O38 . H381 . O67 . 179.86(16) 0.949 1.715 2.664(9) yes
O9 . H91 . O15 . 131.83(14) 0.960 1.937 2.675(9) yes
O92 . H921 . C8 . 149.66(13) 0.950 2.514 3.368(9) yes
O92 . H921 . O9 . 179.92(16) 0.950 1.674 2.624(9) yes
O15 . H151 . C19 . 149.31(12) 0.949 2.529 3.380(9) yes
O15 . H151 . O20 . 179.89(17) 0.949 1.721 2.670(9) yes
O20 . H201 . O92 . 179.87(16) 0.949 1.744 2.694(9) yes
O129 . H1291 . O59 1_655 169.4(5) 0.870 2.010 2.869(9) yes
O129 . H1292 . O46 1_654 132.2(4) 0.849 2.361 2.998(9) yes
O112 . H1121 . O87 1_656 178.8(3) 0.850 1.797 2.647(9) yes
O112 . H1122 . O106 1_655 179.1(3) 0.850 1.821 2.671(9) yes
O114 . H1141 . O100 1_556 179.8(3) 0.950 1.894 2.844(9) yes
O114 . H1142 . O4 . 179.3(3) 0.950 1.843 2.793(9) yes
O113 . H1132 . O77 1_655 137.6(2) 0.843 1.894 2.580(9) yes
O113 . H1131 . O88 1_655 167.9(3) 0.828 1.364 2.181(9) yes
O130 . H1301 . O58 1_756 123.0(3) 0.853 2.599 3.146(9) yes
O130 . H1301 . O113 1_556 179.6(5) 0.853 1.402 2.256(9) yes
O130 . H1302 . O74 1_755 178.9(5) 0.848 1.941 2.788(9) yes
O131 . H1311 . O46 1_655 179.6(3) 0.851 2.085 2.936(9) yes
O131 . H1312 . O114 . 179.7(4) 0.852 1.964 2.816(9) yes
O132 . H1321 . O101 1_556 179.6(13) 0.850 1.367 2.217(9) yes
O132 . H1322 . O59 1_656 179.9(8) 0.848 1.895 2.744(9) yes


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

data_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1553852'
_audit_update_record             
;
2018-07-05 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
_cell_length_a                   11.7762(2)
_cell_length_b                   31.6823(5)
_cell_length_c                   12.3285(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.9994(16)
_cell_angle_gamma                90
_cell_volume                     4593.43(9)
_cell_measurement_reflns_used    11021
_cell_measurement_theta_min      1.8580
_cell_measurement_theta_max      29.0070
_cell_oxdiff_length_a            11.77818(17)
_cell_oxdiff_length_b            31.6894(4)
_cell_oxdiff_length_c            12.33011(19)
_cell_oxdiff_angle_alpha         89.9990(12)
_cell_oxdiff_angle_beta          92.9966(12)
_cell_oxdiff_angle_gamma         90.0132(11)
_cell_oxdiff_volume              4595.83(12)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 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'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

_chemical_formula_sum            'C35 H49 N6 Na O21 S4'
_chemical_formula_moiety         'C28 H20 O16 S4, C7 H21 N6 O, 4(H2 O), Na'
_chemical_compound_source        ?
_chemical_formula_weight         1041.07


_cell_measurement_temperature    175

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_max          0.600
_exptl_absorpt_correction_T_min  0.89803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.9e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.926
_oxdiff_exptl_absorpt_empirical_full_max 1.078
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2176
_exptl_absorpt_coefficient_mu    0.303
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_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 88.44
_montpellier_reflns_redundancy_maxres 3.61

#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 1.65 6.3 68.24 0.026 99.8 99.82
1 1.65 1.31 5.0 36.39 0.034 100.0 99.91
2 1.31 1.14 4.5 28.95 0.039 100.0 99.94
3 1.14 1.03 3.9 21.26 0.044 100.0 99.96
4 1.03 0.96 3.5 13.87 0.057 100.0 99.96
5 0.96 0.90 3.3 10.70 0.071 100.0 99.97
6 0.90 0.86 3.0 8.59 0.088 100.0 99.97
7 0.86 0.82 2.8 7.67 0.096 100.0 99.98
8 0.82 0.79 2.4 6.28 0.114 96.2 99.54
9 0.79 0.73 1.4 4.01 0.132 44.2 88.44
#End reflection statistics
_computing_data_collection       'CrysAlisPro 1.171.39.9e (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.9e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9e (Rigaku OD, 2015)'
_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      -0.0387826000
_diffrn_orient_matrix_UB_12      0.0161027000
_diffrn_orient_matrix_UB_13      -0.0170066000
_diffrn_orient_matrix_UB_21      -0.0406392000
_diffrn_orient_matrix_UB_22      -0.0155435000
_diffrn_orient_matrix_UB_23      -0.0165622000
_diffrn_orient_matrix_UB_31      -0.0219305000
_diffrn_orient_matrix_UB_32      0.0003127000
_diffrn_orient_matrix_UB_33      0.0524858000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  46.00   0.50   24.47    --  -16.62  77.00-150.00  110
  2  ω    -44.00  46.00   0.50   24.47    --  -16.62  77.00  90.00  180
  3  ω      8.00  62.00   0.50   24.47    --   17.25  77.00  30.00  108
  4  ω     54.00  80.00   0.50   24.47    --   17.25  77.00 -30.00   52
  5  ω    -11.00  75.00   0.50   24.47    --   17.25  77.00 -60.00  172
  6  ω     -9.00  85.00   0.50   24.47    --   17.25  77.00-180.00  188
;
_diffrn_measurement_method       'ω scans'

_diffrn_ambient_temperature      175
_diffrn_reflns_number            39835
_reflns_number_total             10955
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_unetI/netI     0.0418
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 10955 
# Theoretical number of reflections is about 24812 


_diffrn_reflns_theta_min         1.775
_diffrn_reflns_theta_max         29.166
_diffrn_measured_fraction_theta_max 0.884

_diffrn_reflns_theta_full        26.420
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              43
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.50
_oxford_diffrn_Wilson_scale      0.39

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

_refine_diff_density_min         -1.20
_refine_diff_density_max         3.36


# 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         9026
_refine_ls_number_restraints     47
_refine_ls_number_parameters     673
_oxford_refine_ls_R_factor_ref   0.1003
_refine_ls_wR_factor_ref         0.1081
_refine_ls_goodness_of_fit_ref   1.0333
_refine_ls_shift/su_max          0.0024420
_refine_ls_shift/su_mean         0.0000489


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10951
_refine_ls_R_factor_all          0.1142
_refine_ls_wR_factor_all         0.1136

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9026
_refine_ls_R_factor_gt           0.1003
_refine_ls_wR_factor_gt          0.1081

# 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    mixed #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: 
 16.6 11.7 12.2 4.19 
;

# 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 0.62570(8) 0.38579(3) 0.70596(7) 0.0306 1.0000 Uani . . . . . .
O2 O 0.7327(3) 0.40227(17) 0.7514(4) 0.0796 1.0000 Uani . . . . . .
O3 O 0.5669(3) 0.36280(13) 0.7884(3) 0.0540 1.0000 Uani . . . . . .
O4 O 0.5540(3) 0.41709(10) 0.6519(3) 0.0433 1.0000 Uani . . . . . .
C5 C 0.6605(3) 0.34792(11) 0.6085(3) 0.0203 1.0000 Uani . . . . . .
C6 C 0.5807(3) 0.33584(11) 0.5274(3) 0.0209 1.0000 Uani . . . . . .
C7 C 0.6055(3) 0.30400(10) 0.4555(2) 0.0188 1.0000 Uani . . . . . .
C8 C 0.7117(3) 0.28387(10) 0.4687(2) 0.0181 1.0000 Uani . . . . . .
O9 O 0.7331(2) 0.25070(8) 0.4025(2) 0.0264 1.0000 Uani D . . . . .
H91 H 0.796(3) 0.2456(19) 0.383(5) 0.0500 1.0000 Uiso D . . . . .
C10 C 0.7933(2) 0.29618(10) 0.5492(2) 0.0181 1.0000 Uani . . . . . .
C11 C 0.7664(3) 0.32845(10) 0.6191(2) 0.0196 1.0000 Uani . . . . . .
H111 H 0.8203 0.3374 0.6743 0.0231 1.0000 Uiso R . . . . .
C12 C 0.9084(3) 0.27466(11) 0.5615(3) 0.0203 1.0000 Uani . . . . . .
C13 C 0.9927(3) 0.29015(10) 0.4813(2) 0.0186 1.0000 Uani . . . . . .
C14 C 1.0066(3) 0.26989(10) 0.3822(3) 0.0187 1.0000 Uani . . . . . .
O15 O 0.9454(2) 0.23337(8) 0.3614(2) 0.0276 1.0000 Uani D . . . . .
H151 H 0.936(5) 0.2345(19) 0.2961(16) 0.0500 1.0000 Uiso D . . . . .
C16 C 1.0835(3) 0.28425(10) 0.3077(2) 0.0195 1.0000 Uani . . . . . .
C17 C 1.0971(3) 0.26226(11) 0.1991(3) 0.0226 1.0000 Uani . . . . . .
C18 C 1.0252(3) 0.28181(11) 0.1074(3) 0.0206 1.0000 Uani . . . . . .
C19 C 0.9085(3) 0.27255(11) 0.0919(3) 0.0207 1.0000 Uani . . . . . .
O20 O 0.8645(2) 0.24234(8) 0.1565(2) 0.0308 1.0000 Uani D . . . . .
H201 H 0.7968(18) 0.2385(19) 0.151(5) 0.0500 1.0000 Uiso D . . . . .
C21 C 0.8390(3) 0.29228(11) 0.0120(3) 0.0210 1.0000 Uani . . . . . .
C22 C 0.8895(3) 0.31985(12) -0.0587(3) 0.0254 1.0000 Uani . . . . . .
C23 C 1.0056(3) 0.32745(13) -0.0484(3) 0.0284 1.0000 Uani . . . . . .
C24 C 1.0726(3) 0.30941(12) 0.0364(3) 0.0254 1.0000 Uani . . . . . .
H241 H 1.1511 0.3162 0.0448 0.0299 1.0000 Uiso R . . . . .
S25 S 1.07384(8) 0.35865(3) -0.14335(8) 0.0327 1.0000 Uani . . . . . .
O26 O 0.9975(3) 0.36358(13) -0.2350(3) 0.0539 1.0000 Uani . . . . . .
O27 O 1.1068(4) 0.39621(11) -0.0888(3) 0.0548 1.0000 Uani . . . . . .
O28 O 1.1753(3) 0.33450(10) -0.1728(3) 0.0429 1.0000 Uani . . . . . .
H221 H 0.8445 0.3336 -0.1143 0.0308 1.0000 Uiso R . . . . .
C29 C 0.7127(3) 0.28305(11) -0.0002(3) 0.0218 1.0000 Uani . . . . . .
C30 C 0.6416(3) 0.30627(11) 0.0807(2) 0.0199 1.0000 Uani . . . . . .
C31 C 0.6123(3) 0.28816(10) 0.1791(3) 0.0188 1.0000 Uani . . . . . .
O32 O 0.6451(2) 0.24691(8) 0.1994(2) 0.0256 1.0000 Uani D . . . . .
H321 H 0.645(5) 0.2432(19) 0.2646(17) 0.0500 1.0000 Uiso D . . . . .
C33 C 0.5484(3) 0.30984(11) 0.2542(2) 0.0204 1.0000 Uani . . . . . .
C34 C 0.5205(3) 0.29110(11) 0.3640(3) 0.0212 1.0000 Uani . . . . . .
H342 H 0.4470 0.3004 0.3815 0.0252 1.0000 Uiso R . . . . .
H341 H 0.5207 0.2612 0.3581 0.0252 1.0000 Uiso R . . . . .
C35 C 0.5107(3) 0.35020(12) 0.2277(3) 0.0242 1.0000 Uani . . . . . .
C36 C 0.5374(3) 0.36855(11) 0.1291(3) 0.0247 1.0000 Uani . . . . . .
C37 C 0.6025(3) 0.34690(11) 0.0569(3) 0.0225 1.0000 Uani . . . . . .
H371 H 0.6203 0.3599 -0.0096 0.0266 1.0000 Uiso R . . . . .
S38 S 0.48231(9) 0.41910(3) 0.09567(7) 0.0314 1.0000 Uani . . . . . .
O39 O 0.4865(3) 0.44406(10) 0.1935(3) 0.0452 1.0000 Uani . . . . . .
O40 O 0.3639(3) 0.41202(11) 0.0541(3) 0.0467 1.0000 Uani . . . . . .
O41 O 0.5467(3) 0.43518(11) 0.0076(3) 0.0512 1.0000 Uani . . . . . .
H351 H 0.4665 0.3655 0.2767 0.0286 1.0000 Uiso R . . . . .
H291 H 0.6864 0.2911 -0.0714 0.0262 1.0000 Uiso R . . . . .
H292 H 0.7016 0.2536 0.0089 0.0262 1.0000 Uiso R . . . . .
C42 C 1.1495(3) 0.31957(11) 0.3349(3) 0.0211 1.0000 Uani . . . . . .
C43 C 1.1387(3) 0.33946(11) 0.4338(3) 0.0217 1.0000 Uani . . . . . .
C44 C 1.0607(3) 0.32519(11) 0.5068(3) 0.0203 1.0000 Uani . . . . . .
H441 H 1.0539 0.3395 0.5738 0.0239 1.0000 Uiso R . . . . .
S45 S 1.23098(8) 0.38158(3) 0.47210(8) 0.0337 1.0000 Uani . . . . . .
O46 O 1.2975(4) 0.39032(14) 0.3804(3) 0.0647 1.0000 Uani . . . . . .
O47 O 1.3027(3) 0.36591(13) 0.5650(3) 0.0555 1.0000 Uani . . . . . .
O48 O 1.1625(3) 0.41680(10) 0.5068(3) 0.0484 1.0000 Uani . . . . . .
H421 H 1.2018 0.3301 0.2853 0.0249 1.0000 Uiso R . . . . .
H122 H 0.9395 0.2795 0.6331 0.0246 1.0000 Uiso R . . . . .
H121 H 0.8978 0.2452 0.5506 0.0246 1.0000 Uiso R . . . . .
H61 H 0.5140 0.3482 0.5220 0.0500 1.0000 Uiso R . . . . .
Na49 Na 0.4604(7) 0.0651(3) 0.1310(6) 0.1888 1.0000 Uani . . . . . .
O50 O 0.4766(4) 0.44962(15) 0.4462(3) 0.0591 1.0000 Uani D . . . . .
H502 H 0.500(6) 0.441(2) 0.507(3) 0.0700 1.0000 Uiso D . . . . .
H501 H 0.439(5) 0.4704(15) 0.425(6) 0.0700 1.0000 Uiso D . . . . .
O51 O 0.7726(5) 0.44583(19) 0.9389(5) 0.0803 1.0000 Uani D . . . . .
H511 H 0.779(8) 0.4711(11) 0.922(8) 0.1050 1.0000 Uiso D . . . . .
H512 H 0.727(7) 0.446(3) 0.987(6) 0.1050 1.0000 Uiso D . . . . .
O52 O 0.1022(7) 0.48029(17) 0.8471(6) 0.1133 1.0000 Uani D . . . . .
O53 O 0.7958(6) 0.5282(2) 0.8743(8) 0.1248 1.0000 Uani D . . . . .
H531 H 0.792(4) 0.541(3) 0.814(4) 0.1510 1.0000 Uiso D . . . . .
H532 H 0.758(10) 0.542(3) 0.918(7) 0.1510 1.0000 Uiso D . . . . .
O54 O 0.1411(4) 0.52079(13) 0.6440(6) 0.0923 1.0000 Uani . . . . . .
C55 C 0.2334(5) 0.53686(14) 0.6330(4) 0.0462 1.0000 Uani D . . . . .
N56 N 0.3297(4) 0.51416(12) 0.6435(3) 0.0410 1.0000 Uani D . . . . .
N57 N 0.3204(3) 0.47079(11) 0.6525(3) 0.0386 1.0000 Uani D . . . . .
C58 C 0.3508(3) 0.45201(12) 0.7468(3) 0.0297 1.0000 Uani D . . . . .
N59 N 0.3162(3) 0.41187(10) 0.7533(3) 0.0299 1.0000 Uani D . . . . .
N60 N 0.3567(3) 0.38587(10) 0.8409(3) 0.0288 1.0000 Uani D . . . . .
H601 H 0.314(3) 0.3625(8) 0.842(3) 0.0500 1.0000 Uiso D . . . . .
H603 H 0.351(3) 0.3998(8) 0.9020(17) 0.0500 1.0000 Uiso D . . . . .
H602 H 0.4282(19) 0.3787(11) 0.834(2) 0.0500 1.0000 Uiso D . . . . .
H591 H 0.308(4) 0.3990(7) 0.6921(16) 0.0500 1.0000 Uiso D . . . . .
N61 N 0.4073(3) 0.47249(11) 0.8254(3) 0.0359 1.0000 Uani D . . . . .
H612 H 0.428(4) 0.4983(8) 0.818(3) 0.0500 1.0000 Uiso D . . . . .
H611 H 0.433(4) 0.4590(9) 0.882(3) 0.0500 1.0000 Uiso D . . . . .
H571 H 0.266(3) 0.4587(8) 0.612(3) 0.0500 1.0000 Uiso D . . . . .
H561 H 0.392(2) 0.5244(7) 0.621(4) 0.0500 1.0000 Uiso D . . . . .
C62 C 0.2520(5) 0.58221(15) 0.6018(5) 0.0557 1.0000 Uani . . . . . .
C63 C 0.1547(5) 0.61118(16) 0.6216(5) 0.0506 1.0000 Uani . . . . . .
C64 C 0.1585(5) 0.63150(18) 0.7314(5) 0.0574 1.0000 Uani . . . . . .
C65 C 0.1431(6) 0.6021(2) 0.8240(5) 0.0628 1.0000 Uani . . . . . .
C66 C 0.0239(6) 0.58565(19) 0.8273(6) 0.0673 1.0000 Uani D . . . . .
N67 N 0.0139(7) 0.5547(2) 0.9183(6) 0.0874 1.0000 Uani D . . . . .
H673 H -0.059(2) 0.5466(13) 0.922(3) 0.0842 1.0000 Uiso D . . . . .
H672 H 0.038(4) 0.5663(10) 0.9823(19) 0.0842 1.0000 Uiso D . . . . .
H671 H 0.057(4) 0.5314(9) 0.905(3) 0.0842 1.0000 Uiso D . . . . .
H662 H -0.0252 0.6089 0.8375 0.0883 1.0000 Uiso R . . . . .
H661 H 0.0030 0.5721 0.7604 0.0883 1.0000 Uiso R . . . . .
H652 H 0.1632 0.6161 0.8904 0.0812 1.0000 Uiso R . . . . .
H651 H 0.1922 0.5787 0.8157 0.0812 1.0000 Uiso R . . . . .
H642 H 0.0989 0.6517 0.7326 0.0706 1.0000 Uiso R . . . . .
H641 H 0.2297 0.6454 0.7418 0.0706 1.0000 Uiso R . . . . .
H632 H 0.1528 0.6328 0.5682 0.0661 1.0000 Uiso R . . . . .
H631 H 0.0868 0.5950 0.6141 0.0661 1.0000 Uiso R . . . . .
H621 H 0.3168 0.5925 0.6428 0.0714 1.0000 Uiso R . . . . .
H622 H 0.2660 0.5831 0.5267 0.0714 1.0000 Uiso R . . . . .
H521 H 0.117(8) 0.4549(11) 0.856(7) 0.1301 1.0000 Uiso D . . . . .
H522 H 0.140(8) 0.4894(10) 0.798(6) 0.1301 1.0000 Uiso D . . . . .
H171 H 1.1747 0.2638 0.1819 0.0274 1.0000 Uiso R . . . . .
H172 H 1.0755 0.2335 0.2061 0.0274 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.368(6)
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 . 1.449(4) yes
S1 . O3 . 1.455(4) yes
S1 . O4 . 1.443(3) yes
S1 . C5 . 1.762(3) yes
C5 . C6 . 1.388(5) yes
C5 . C11 . 1.392(4) yes
C6 . C7 . 1.385(5) yes
C6 . H61 . 0.878 no
C7 . C8 . 1.405(4) yes
C7 . C34 . 1.524(4) yes
C8 . O9 . 1.362(4) yes
C8 . C10 . 1.400(4) yes
O9 . H91 . 0.806(19) no
C10 . C11 . 1.385(5) yes
C10 . C12 . 1.518(4) yes
C11 . H111 . 0.950 no
C12 . C13 . 1.519(4) yes
C12 . H122 . 0.950 no
C12 . H121 . 0.950 no
C13 . C14 . 1.397(4) yes
C13 . C44 . 1.395(5) yes
C14 . O15 . 1.380(4) yes
C14 . C16 . 1.399(5) yes
O15 . H151 . 0.807(19) no
C16 . C17 . 1.524(4) yes
C16 . C42 . 1.393(5) yes
C17 . C18 . 1.509(5) yes
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C18 . C19 . 1.408(4) yes
C18 . C24 . 1.377(5) yes
C19 . O20 . 1.365(4) yes
C19 . C21 . 1.395(5) yes
O20 . H201 . 0.806(19) no
C21 . C22 . 1.389(5) yes
C21 . C29 . 1.516(4) yes
C22 . C23 . 1.388(5) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.398(5) yes
C23 . S25 . 1.758(4) yes
C24 . H241 . 0.950 no
S25 . O26 . 1.415(4) yes
S25 . O27 . 1.412(4) yes
S25 . O28 . 1.480(3) yes
C29 . C30 . 1.524(5) yes
C29 . H291 . 0.950 no
C29 . H292 . 0.950 no
C30 . C31 . 1.402(4) yes
C30 . C37 . 1.393(5) yes
C31 . O32 . 1.382(4) yes
C31 . C33 . 1.403(5) yes
O32 . H321 . 0.813(19) no
C33 . C34 . 1.529(4) yes
C33 . C35 . 1.387(5) yes
C34 . H342 . 0.950 no
C34 . H341 . 0.950 no
C35 . C36 . 1.398(5) yes
C35 . H351 . 0.950 no
C36 . C37 . 1.386(5) yes
C36 . S38 . 1.769(4) yes
C37 . H371 . 0.950 no
S38 . O39 . 1.441(3) yes
S38 . O40 . 1.477(4) yes
S38 . O41 . 1.448(3) yes
C42 . C43 . 1.385(4) yes
C42 . H421 . 0.950 no
C43 . C44 . 1.394(5) yes
C43 . S45 . 1.769(3) yes
C44 . H441 . 0.950 no
S45 . O46 . 1.436(3) yes
S45 . O47 . 1.474(4) yes
S45 . O48 . 1.454(3) yes
O50 . H502 . 0.828(19) no
O50 . H501 . 0.827(19) no
O51 . H511 . 0.83(2) no
O51 . H512 . 0.82(2) no
O52 . H521 . 0.83(2) no
O52 . H522 . 0.83(2) no
O53 . H531 . 0.84(2) no
O53 . H532 . 0.83(2) no
O54 . C55 . 1.214(7) yes
C55 . N56 . 1.344(7) yes
C55 . C62 . 1.507(6) yes
N56 . N57 . 1.383(5) yes
N56 . H561 . 0.861(19) no
N57 . C58 . 1.337(5) yes
N57 . H571 . 0.873(19) no
C58 . N59 . 1.339(5) yes
C58 . N61 . 1.317(5) yes
N59 . N60 . 1.421(4) yes
N59 . H591 . 0.858(19) no
N60 . H601 . 0.897(19) no
N60 . H603 . 0.878(19) no
N60 . H602 . 0.880(19) no
N61 . H612 . 0.860(19) no
N61 . H611 . 0.864(19) no
C62 . C63 . 1.499(8) yes
C62 . H621 . 0.950 no
C62 . H622 . 0.950 no
C63 . C64 . 1.497(8) yes
C63 . H632 . 0.950 no
C63 . H631 . 0.950 no
C64 . C65 . 1.492(9) yes
C64 . H642 . 0.950 no
C64 . H641 . 0.950 no
C65 . C66 . 1.500(9) yes
C65 . H652 . 0.950 no
C65 . H651 . 0.950 no
C66 . N67 . 1.499(9) yes
C66 . H662 . 0.950 no
C66 . H661 . 0.950 no
N67 . H673 . 0.903(19) no
N67 . H672 . 0.904(19) no
N67 . H671 . 0.914(19) 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 . 110.3(3) yes
O2 . S1 . O4 . 114.0(3) yes
O3 . S1 . O4 . 112.2(2) yes
O2 . S1 . C5 . 106.29(18) yes
O3 . S1 . C5 . 105.76(19) yes
O4 . S1 . C5 . 107.70(17) yes
S1 . C5 . C6 . 120.4(2) yes
S1 . C5 . C11 . 118.5(2) yes
C6 . C5 . C11 . 121.0(3) yes
C5 . C6 . C7 . 120.3(3) yes
C5 . C6 . H61 . 120.1 no
C7 . C6 . H61 . 119.6 no
C6 . C7 . C8 . 118.2(3) yes
C6 . C7 . C34 . 121.1(3) yes
C8 . C7 . C34 . 120.7(3) yes
C7 . C8 . O9 . 118.2(3) yes
C7 . C8 . C10 . 122.0(3) yes
O9 . C8 . C10 . 119.8(3) yes
C8 . O9 . H91 . 122(4) no
C8 . C10 . C11 . 118.4(3) yes
C8 . C10 . C12 . 121.5(3) yes
C11 . C10 . C12 . 120.1(3) yes
C5 . C11 . C10 . 120.1(3) yes
C5 . C11 . H111 . 119.8 no
C10 . C11 . H111 . 120.1 no
C10 . C12 . C13 . 113.6(3) yes
C10 . C12 . H122 . 108.6 no
C13 . C12 . H122 . 108.6 no
C10 . C12 . H121 . 108.4 no
C13 . C12 . H121 . 108.1 no
H122 . C12 . H121 . 109.5 no
C12 . C13 . C14 . 122.1(3) yes
C12 . C13 . C44 . 119.8(3) yes
C14 . C13 . C44 . 118.1(3) yes
C13 . C14 . O15 . 117.6(3) yes
C13 . C14 . C16 . 122.3(3) yes
O15 . C14 . C16 . 120.0(3) yes
C14 . O15 . H151 . 101(4) no
C14 . C16 . C17 . 121.9(3) yes
C14 . C16 . C42 . 118.4(3) yes
C17 . C16 . C42 . 119.7(3) yes
C16 . C17 . C18 . 112.9(3) yes
C16 . C17 . H171 . 108.6 no
C18 . C17 . H171 . 108.7 no
C16 . C17 . H172 . 108.6 no
C18 . C17 . H172 . 108.6 no
H171 . C17 . H172 . 109.5 no
C17 . C18 . C19 . 121.4(3) yes
C17 . C18 . C24 . 120.5(3) yes
C19 . C18 . C24 . 118.1(3) yes
C18 . C19 . O20 . 117.7(3) yes
C18 . C19 . C21 . 122.4(3) yes
O20 . C19 . C21 . 119.9(3) yes
C19 . O20 . H201 . 118(4) no
C19 . C21 . C22 . 118.0(3) yes
C19 . C21 . C29 . 121.3(3) yes
C22 . C21 . C29 . 120.6(3) yes
C21 . C22 . C23 . 120.3(3) yes
C21 . C22 . H221 . 120.0 no
C23 . C22 . H221 . 119.8 no
C22 . C23 . C24 . 120.8(3) yes
C22 . C23 . S25 . 121.3(3) yes
C24 . C23 . S25 . 117.9(3) yes
C23 . C24 . C18 . 120.3(3) yes
C23 . C24 . H241 . 119.8 no
C18 . C24 . H241 . 120.0 no
C23 . S25 . O26 . 107.44(19) yes
C23 . S25 . O27 . 106.29(18) yes
O26 . S25 . O27 . 115.8(2) yes
C23 . S25 . O28 . 105.99(19) yes
O26 . S25 . O28 . 110.4(2) yes
O27 . S25 . O28 . 110.3(2) yes
C21 . C29 . C30 . 114.3(3) yes
C21 . C29 . H291 . 108.1 no
C30 . C29 . H291 . 108.1 no
C21 . C29 . H292 . 108.6 no
C30 . C29 . H292 . 108.2 no
H291 . C29 . H292 . 109.5 no
C29 . C30 . C31 . 122.5(3) yes
C29 . C30 . C37 . 119.7(3) yes
C31 . C30 . C37 . 117.8(3) yes
C30 . C31 . O32 . 117.7(3) yes
C30 . C31 . C33 . 122.4(3) yes
O32 . C31 . C33 . 119.9(3) yes
C31 . O32 . H321 . 107(4) no
C31 . C33 . C34 . 122.8(3) yes
C31 . C33 . C35 . 118.2(3) yes
C34 . C33 . C35 . 119.0(3) yes
C33 . C34 . C7 . 112.8(3) yes
C33 . C34 . H342 . 108.7 no
C7 . C34 . H342 . 108.7 no
C33 . C34 . H341 . 108.6 no
C7 . C34 . H341 . 108.6 no
H342 . C34 . H341 . 109.5 no
C33 . C35 . C36 . 120.3(3) yes
C33 . C35 . H351 . 119.9 no
C36 . C35 . H351 . 119.8 no
C35 . C36 . C37 . 120.6(3) yes
C35 . C36 . S38 . 118.9(3) yes
C37 . C36 . S38 . 120.4(3) yes
C30 . C37 . C36 . 120.7(3) yes
C30 . C37 . H371 . 119.7 no
C36 . C37 . H371 . 119.6 no
C36 . S38 . O39 . 107.80(17) yes
C36 . S38 . O40 . 105.76(18) yes
O39 . S38 . O40 . 111.3(2) yes
C36 . S38 . O41 . 107.05(19) yes
O39 . S38 . O41 . 116.0(2) yes
O40 . S38 . O41 . 108.4(2) yes
C16 . C42 . C43 . 120.1(3) yes
C16 . C42 . H421 . 119.9 no
C43 . C42 . H421 . 119.9 no
C42 . C43 . C44 . 121.0(3) yes
C42 . C43 . S45 . 119.7(3) yes
C44 . C43 . S45 . 119.3(2) yes
C13 . C44 . C43 . 120.2(3) yes
C13 . C44 . H441 . 120.1 no
C43 . C44 . H441 . 119.7 no
C43 . S45 . O46 . 106.75(18) yes
C43 . S45 . O47 . 105.8(2) yes
O46 . S45 . O47 . 111.3(3) yes
C43 . S45 . O48 . 108.36(18) yes
O46 . S45 . O48 . 114.7(3) yes
O47 . S45 . O48 . 109.5(2) yes
H502 . O50 . H501 . 133(8) no
H511 . O51 . H512 . 100(10) no
H521 . O52 . H522 . 108.50(3) no
H531 . O53 . H532 . 108.50(5) no
O54 . C55 . N56 . 121.4(4) yes
O54 . C55 . C62 . 124.9(5) yes
N56 . C55 . C62 . 113.6(4) yes
C55 . N56 . N57 . 118.0(4) yes
C55 . N56 . H561 . 119.6(15) no
N57 . N56 . H561 . 118.3(15) no
N56 . N57 . C58 . 119.6(4) yes
N56 . N57 . H571 . 116.6(16) no
C58 . N57 . H571 . 116.8(16) no
N57 . C58 . N59 . 114.0(4) yes
N57 . C58 . N61 . 121.5(4) yes
N59 . C58 . N61 . 124.5(4) yes
C58 . N59 . N60 . 120.4(3) yes
C58 . N59 . H591 . 114.7(16) no
N60 . N59 . H591 . 114.3(16) no
N59 . N60 . H601 . 108.8(16) no
N59 . N60 . H603 . 108.8(16) no
H601 . N60 . H603 . 109.4(17) no
N59 . N60 . H602 . 110.9(16) no
H601 . N60 . H602 . 109.3(17) no
H603 . N60 . H602 . 109.6(17) no
C58 . N61 . H612 . 121.5(18) no
C58 . N61 . H611 . 119.9(18) no
H612 . N61 . H611 . 118(3) no
C55 . C62 . C63 . 114.8(5) yes
C55 . C62 . H621 . 108.4 no
C63 . C62 . H621 . 107.6 no
C55 . C62 . H622 . 108.2 no
C63 . C62 . H622 . 108.3 no
H621 . C62 . H622 . 109.5 no
C62 . C63 . C64 . 115.0(5) yes
C62 . C63 . H632 . 108.6 no
C64 . C63 . H632 . 108.4 no
C62 . C63 . H631 . 107.5 no
C64 . C63 . H631 . 107.8 no
H632 . C63 . H631 . 109.5 no
C63 . C64 . C65 . 115.1(5) yes
C63 . C64 . H642 . 108.4 no
C65 . C64 . H642 . 106.7 no
C63 . C64 . H641 . 107.8 no
C65 . C64 . H641 . 109.2 no
H642 . C64 . H641 . 109.5 no
C64 . C65 . C66 . 112.9(6) yes
C64 . C65 . H652 . 109.4 no
C66 . C65 . H652 . 109.3 no
C64 . C65 . H651 . 107.8 no
C66 . C65 . H651 . 107.9 no
H652 . C65 . H651 . 109.5 no
C65 . C66 . N67 . 110.9(7) yes
C65 . C66 . H662 . 108.1 no
N67 . C66 . H662 . 109.7 no
C65 . C66 . H661 . 109.5 no
N67 . C66 . H661 . 109.1 no
H662 . C66 . H661 . 109.5 no
C66 . N67 . H673 . 109.5(17) no
C66 . N67 . H672 . 110.7(17) no
H673 . N67 . H672 . 109.3(18) no
C66 . N67 . H671 . 109.3(17) no
H673 . N67 . H671 . 108.5(18) no
H672 . N67 . H671 . 109.4(18) 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
O9 . H91 . C14 . 146(5) 0.806 2.598 3.300(5) yes
O9 . H91 . O15 . 171(6) 0.806 1.835 2.634(5) yes
C11 . H111 . O26 1_556 161.15(10) 0.950 2.459 3.372(5) yes
O15 . H151 . O20 . 160(6) 0.807 1.893 2.668(5) yes
O20 . H201 . O32 . 152(6) 0.806 1.930 2.668(5) yes
O32 . H321 . O9 . 144(6) 0.813 1.960 2.663(5) yes
C37 . H371 . O3 1_554 143.90(13) 0.950 2.538 3.353(5) yes
C35 . H351 . O46 1_455 160.93(11) 0.950 2.545 3.457(5) yes
C44 . H441 . O26 1_556 165.37(11) 0.950 2.597 3.524(5) yes
O50 . H502 . O4 . 176(7) 0.828 2.016 2.843(5) yes
O51 . H511 . O53 . 180(10) 0.829 1.919 2.746(5) yes
O51 . H512 . O41 1_556 139(9) 0.822 2.183 2.854(5) yes
O53 . H532 . O40 2_666 150(10) 0.833 2.093 2.842(5) yes
N60 . H601 . O28 1_456 152(3) 0.897 1.858 2.684(5) yes
N60 . H603 . O40 1_556 159(2) 0.878 1.914 2.754(5) yes
N60 . H602 . O3 . 168(3) 0.880 1.825 2.692(5) yes
N59 . H591 . O47 1_455 173(3) 0.858 1.884 2.737(5) yes
N61 . H612 . O39 2_666 167(5) 0.860 2.094 2.939(5) yes
N61 . H611 . O41 1_556 161(5) 0.864 2.127 2.959(5) yes
N57 . H571 . O48 1_455 166(4) 0.873 2.189 3.044(5) yes
N56 . H561 . O50 2_666 173(4) 0.861 1.973 2.829(5) yes
N67 . H673 . O53 1_455 159(4) 0.903 1.869 2.730(5) yes
N67 . H672 . O51 2_667 122(4) 0.904 2.416 2.993(5) yes
N67 . H671 . O52 . 161(5) 0.914 1.860 2.739(5) yes
O52 . H521 . O27 1_456 160(4) 0.826 1.988 2.778(5) yes
O52 . H522 . O54 . 150(10) 0.829 2.138 2.871(5) yes



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 0 1 x .
0 3 1 x .
0 4 0 x .
1 1 0 x .
# start Validation Reply Form
_vrf_PLAT067_1                   
;
PROBLEM: Maximum Dimension Less Min. Xtal Dimension .....     Please Check
RESPONSE: ...
;
_vrf_PLAT097_1                   
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.36 eA-3
RESPONSE: This maximum density is found in the middle of a sulfonate group at 
0.8 angstrom from the sulfur atom. The oxygen atoms do not appear to be 
(strongly) disordered. This positive maximum can thus only be attributed to 
some kind of systematic measurement error. It does not affect the plausibility 
of the structural model.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1553850'
_audit_update_record             
;
2018-07-05 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   12.2682(7)
_cell_length_b                   13.7258(9)
_cell_length_c                   14.1574(8)
_cell_angle_alpha                70.256(5)
_cell_angle_beta                 83.703(4)
_cell_angle_gamma                84.488(5)
_cell_volume                     2225.85(12)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?
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'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            31

# Given Formula = C1 H1 N1 Na0.06 O1 S1 
# Dc =      1.77 Fooo =    994.00 Mu =      8.41 M =   1186.90
# Found Formula = C2.26 H2.58 N0.26 Na0.06 O1.16 S0.26 
# Dc =      1.43 FOOO =    994.00 Mu =      3.00 M =    955.97

_chemical_formula_sum            'C2.26 H2.58 N0.26 Na0.06 O1.16 S0.26'
_chemical_formula_moiety         'C2.26 H2.58 N0.26 Na0.06 O1.16 S0.26'
_chemical_compound_source        ?
_chemical_formula_weight         61.68


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    175

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_max          0.350

_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             994
_exptl_absorpt_coefficient_mu    0.300

# Sheldrick geometric approximatio 0.90 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.99
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      175
_diffrn_reflns_number            8669
_reflns_number_total             8669
_diffrn_reflns_av_R_equivalents  0.035
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8669 
# Theoretical number of reflections is about 21182 


_diffrn_reflns_theta_min         1.533
_diffrn_reflns_theta_max         27.850
_diffrn_measured_fraction_theta_max 0.819

_diffrn_reflns_theta_full        25.010
_diffrn_measured_fraction_theta_full 0.994


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

_oxford_diffrn_Wilson_B_factor   1.75
_oxford_diffrn_Wilson_scale      0.78

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

_refine_diff_density_min         -0.44
_refine_diff_density_max         0.40


# 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         6957
_refine_ls_number_restraints     0
_refine_ls_number_parameters     559
_oxford_refine_ls_R_factor_ref   0.0443
_refine_ls_wR_factor_ref         0.0435
_refine_ls_goodness_of_fit_ref   1.1060
_refine_ls_shift/su_max          0.0006592
_refine_ls_shift/su_mean         0.0000340


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8669
_refine_ls_R_factor_all          0.0603
_refine_ls_wR_factor_all         0.0484

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6957
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_gt          0.0435

# 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: 
 5.14 -2.65 3.58 
;

# 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 0.09834(4) 0.62954(4) 0.14946(4) 0.0155 1.0000 Uani . . . . . .
O2 O 0.19230(15) 0.56849(13) 0.12287(15) 0.0301 1.0000 Uani . . . . . .
O3 O -0.00420(14) 0.60175(13) 0.12677(13) 0.0249 1.0000 Uani . . . . . .
O4 O 0.09538(16) 0.62796(14) 0.25313(13) 0.0307 1.0000 Uani . . . . . .
C5 C 0.11549(17) 0.75898(17) 0.07259(16) 0.0141 1.0000 Uani . . . . . .
C6 C 0.03851(17) 0.81197(17) 0.00567(16) 0.0137 1.0000 Uani . . . . . .
C7 C 0.05562(17) 0.91250(17) -0.05804(16) 0.0138 1.0000 Uani . . . . . .
C8 C 0.15081(17) 0.95777(17) -0.05207(16) 0.0142 1.0000 Uani . . . . . .
O9 O 0.16112(13) 1.05866(12) -0.11399(12) 0.0201 1.0000 Uani . . . . . .
C10 C 0.22958(17) 0.90464(16) 0.01563(16) 0.0128 1.0000 Uani . . . . . .
C11 C 0.20996(17) 0.80507(17) 0.07679(16) 0.0145 1.0000 Uani . . . . . .
C12 C 0.33448(17) 0.95159(17) 0.02296(16) 0.0137 1.0000 Uani . . . . . .
C13 C 0.43341(17) 0.91765(16) -0.03557(16) 0.0130 1.0000 Uani . . . . . .
C14 C 0.50785(17) 0.83771(16) 0.01234(16) 0.0129 1.0000 Uani . . . . . .
C15 C 0.59704(18) 0.80695(17) -0.04270(17) 0.0149 1.0000 Uani . . . . . .
S16 S 0.69513(5) 0.71230(4) 0.02428(4) 0.0169 1.0000 Uani . . . . . .
O17 O 0.63386(18) 0.62590(18) 0.08798(18) 0.0527 1.0000 Uani . . . . . .
O18 O 0.74709(17) 0.76070(17) 0.08177(17) 0.0426 1.0000 Uani . . . . . .
O19 O 0.76919(18) 0.68441(17) -0.04998(14) 0.0397 1.0000 Uani . . . . . .
Na20 Na 0.90044(7) 0.56050(7) -0.07158(7) 0.0206 1.0000 Uani . . . . . .
O21 O -0.08819(15) 0.63954(13) -0.24539(12) 0.0233 1.0000 Uani . . . . . .
S22 S -0.11250(4) 0.72908(4) -0.33230(4) 0.0162 1.0000 Uani . . . . . .
O23 O -0.22800(14) 0.76399(14) -0.32934(15) 0.0309 1.0000 Uani . . . . . .
O24 O -0.07153(16) 0.71357(15) -0.42685(13) 0.0302 1.0000 Uani . . . . . .
C25 C -0.03913(17) 0.83093(17) -0.32520(17) 0.0160 1.0000 Uani . . . . . .
C26 C 0.04005(18) 0.87802(17) -0.40056(16) 0.0164 1.0000 Uani . . . . . .
C27 C 0.09940(17) 0.95538(18) -0.39110(16) 0.0166 1.0000 Uani . . . . . .
C28 C 0.07507(18) 0.98615(17) -0.30698(17) 0.0160 1.0000 Uani . . . . . .
O29 O 0.13214(14) 1.06571(13) -0.30270(13) 0.0225 1.0000 Uani . . . . . .
C30 C -0.00450(17) 0.93945(17) -0.22994(16) 0.0152 1.0000 Uani . . . . . .
C31 C -0.06073(17) 0.86069(17) -0.24003(16) 0.0157 1.0000 Uani . . . . . .
C32 C -0.02656(17) 0.96826(17) -0.13475(17) 0.0158 1.0000 Uani . . . . . .
C33 C 0.19202(18) 1.00261(19) -0.46978(16) 0.0185 1.0000 Uani . . . . . .
C34 C 0.30427(18) 0.94970(18) -0.43952(16) 0.0172 1.0000 Uani . . . . . .
C35 C 0.37508(18) 0.98994(18) -0.39233(16) 0.0162 1.0000 Uani . . . . . .
O36 O 0.34705(13) 1.08110(12) -0.37296(12) 0.0206 1.0000 Uani . . . . . .
C37 C 0.47846(17) 0.94136(17) -0.36610(15) 0.0143 1.0000 Uani . . . . . .
C38 C 0.55310(17) 0.98258(17) -0.31060(16) 0.0151 1.0000 Uani . . . . . .
C39 C 0.53817(17) 0.93345(17) -0.19697(16) 0.0137 1.0000 Uani . . . . . .
C40 C 0.61172(18) 0.85327(17) -0.14625(17) 0.0147 1.0000 Uani . . . . . .
C41 C 0.45149(17) 0.96603(16) -0.13950(17) 0.0141 1.0000 Uani . . . . . .
O42 O 0.38043(13) 1.04892(12) -0.18119(12) 0.0213 1.0000 Uani . . . . . .
C43 C 0.51165(18) 0.85262(18) -0.39007(16) 0.0163 1.0000 Uani . . . . . .
C44 C 0.44176(18) 0.81085(18) -0.43516(16) 0.0181 1.0000 Uani . . . . . .
C45 C 0.33872(18) 0.85888(19) -0.45866(16) 0.0186 1.0000 Uani . . . . . .
S46 S 0.48065(5) 0.69581(5) -0.46297(5) 0.0222 1.0000 Uani . . . . . .
O47 O 0.58863(14) 0.65983(14) -0.42754(13) 0.0254 1.0000 Uani . . . . . .
O48 O 0.47889(16) 0.72286(18) -0.57124(14) 0.0372 1.0000 Uani . . . . . .
O49 O 0.39799(17) 0.62253(17) -0.40761(17) 0.0408 1.0000 Uani . . . . . .
O50 O 0.90080(13) 0.42279(13) 0.08741(12) 0.0218 1.0000 Uani . . . . . .
C51 C 0.84813(18) 0.40360(18) 0.16922(17) 0.0180 1.0000 Uani . . . . . .
O52 O 0.84579(15) 0.46300(15) 0.22586(14) 0.0287 1.0000 Uani . . . . . .
C53 C 0.78315(19) 0.30994(18) 0.21731(17) 0.0204 1.0000 Uani . . . . . .
C54 C 0.72740(19) 0.27676(19) 0.14340(19) 0.0220 1.0000 Uani . . . . . .
C55 C 0.63233(19) 0.35152(19) 0.09648(18) 0.0213 1.0000 Uani . . . . . .
C56 C 0.53504(19) 0.34832(19) 0.17379(18) 0.0200 1.0000 Uani . . . . . .
C57 C 0.43968(19) 0.42414(19) 0.13405(18) 0.0210 1.0000 Uani . . . . . .
N58 N 0.35077(16) 0.41737(17) 0.21591(17) 0.0256 1.0000 Uani . . . . . .
N63 N -0.1387(2) 0.71066(19) 0.27164(19) 0.0370 1.0000 Uani . . . . . .
C64 C -0.2268(2) 0.7036(2) 0.33628(19) 0.0273 1.0000 Uani . . . . . .
N65 N -0.32341(19) 0.7066(2) 0.30386(17) 0.0387 1.0000 Uani . . . . . .
N66 N -0.21803(19) 0.69730(19) 0.43003(17) 0.0332 1.0000 Uani . . . . . .
H61 H -0.0249 0.7806 0.0039 0.0160 1.0000 Uiso R . . . . .
H111 H 0.2622 0.7678 0.1219 0.0174 1.0000 Uiso R . . . . .
H122 H 0.3260 1.0270 -0.0016 0.0160 1.0000 Uiso R . . . . .
H121 H 0.3489 0.9296 0.0946 0.0157 1.0000 Uiso R . . . . .
H141 H 0.4972 0.8049 0.0819 0.0144 1.0000 Uiso R . . . . .
H261 H 0.0541 0.8569 -0.4567 0.0209 1.0000 Uiso R . . . . .
H311 H -0.1136 0.8281 -0.1904 0.0187 1.0000 Uiso R . . . . .
H322 H -0.0248 1.0436 -0.1519 0.0192 1.0000 Uiso R . . . . .
H321 H -0.0990 0.9482 -0.1061 0.0191 1.0000 Uiso R . . . . .
H331 H 0.1920 1.0760 -0.4804 0.0219 1.0000 Uiso R . . . . .
H332 H 0.1792 0.9922 -0.5323 0.0208 1.0000 Uiso R . . . . .
H381 H 0.5399 1.0573 -0.3288 0.0170 1.0000 Uiso R . . . . .
H382 H 0.6286 0.9667 -0.3309 0.0187 1.0000 Uiso R . . . . .
H401 H 0.6723 0.8318 -0.1828 0.0178 1.0000 Uiso R . . . . .
H431 H 0.5816 0.8202 -0.3749 0.0196 1.0000 Uiso R . . . . .
H451 H 0.2918 0.8288 -0.4891 0.0219 1.0000 Uiso R . . . . .
H532 H 0.8351 0.2537 0.2499 0.0254 1.0000 Uiso R . . . . .
H531 H 0.7304 0.3223 0.2688 0.0242 1.0000 Uiso R . . . . .
H542 H 0.7822 0.2714 0.0905 0.0262 1.0000 Uiso R . . . . .
H541 H 0.7012 0.2088 0.1769 0.0262 1.0000 Uiso R . . . . .
H552 H 0.6568 0.4211 0.0709 0.0261 1.0000 Uiso R . . . . .
H551 H 0.6098 0.3334 0.0423 0.0264 1.0000 Uiso R . . . . .
H562 H 0.5587 0.3632 0.2307 0.0232 1.0000 Uiso R . . . . .
H561 H 0.5089 0.2791 0.1957 0.0243 1.0000 Uiso R . . . . .
H571 H 0.4634 0.4945 0.1090 0.0253 1.0000 Uiso R . . . . .
H572 H 0.4092 0.4098 0.0805 0.0253 1.0000 Uiso R . . . . .
H361 H 0.2804 1.0871 -0.3649 0.0311 1.0000 Uiso R . . . . .
H652 H -0.3834 0.7066 0.3433 0.0458 1.0000 Uiso R . . . . .
H661 H -0.2766 0.6910 0.4700 0.0395 1.0000 Uiso R . . . . .
H291 H 0.1308 1.0680 -0.2459 0.0338 1.0000 Uiso R . . . . .
H582 H 0.3223 0.3564 0.2363 0.0383 1.0000 Uiso R . . . . .
H91 H 0.2230 1.0760 -0.1171 0.0308 1.0000 Uiso R . . . . .
H421 H 0.3822 1.0608 -0.2411 0.0323 1.0000 Uiso R . . . . .
H632 H -0.0765 0.7016 0.2944 0.0439 1.0000 Uiso R . . . . .
H583 H 0.2963 0.4655 0.1958 0.0380 1.0000 Uiso R . . . . .
H662 H -0.1568 0.7026 0.4500 0.0400 1.0000 Uiso R . . . . .
H651 H -0.3267 0.7060 0.2441 0.0462 1.0000 Uiso R . . . . .
H631 H -0.1453 0.7103 0.2123 0.0445 1.0000 Uiso R . . . . .
H581 H 0.3786 0.4260 0.2676 0.0390 1.0000 Uiso R . . . . .
H521 H 0.8921 0.5074 0.1964 0.0451 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.5763(18)
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 . Na20 2_665 3.1547(11) yes
S1 . O2 . 1.4509(18) yes
S1 . O3 . 1.4473(17) yes
S1 . O4 . 1.4569(19) yes
S1 . C5 . 1.761(2) yes
O2 . Na20 2_665 2.529(2) yes
O3 . Na20 2_665 2.757(2) yes
C5 . C6 . 1.385(3) yes
C5 . C11 . 1.389(3) yes
C6 . C7 . 1.391(3) yes
C6 . H61 . 0.931 no
C7 . C8 . 1.398(3) yes
C7 . C32 . 1.521(3) yes
C8 . O9 . 1.375(3) yes
C8 . C10 . 1.407(3) yes
O9 . H91 . 0.809 no
C10 . C11 . 1.376(3) yes
C10 . C12 . 1.522(3) yes
C11 . H111 . 0.941 no
C12 . C13 . 1.519(3) yes
C12 . H122 . 0.974 no
C12 . H121 . 0.986 no
C13 . C14 . 1.392(3) yes
C13 . C41 . 1.397(3) yes
C14 . C15 . 1.389(3) yes
C14 . H141 . 0.934 no
C15 . S16 . 1.776(2) yes
C15 . C40 . 1.386(3) yes
S16 . O17 . 1.444(2) yes
S16 . O18 . 1.439(2) yes
S16 . O19 . 1.4398(19) yes
O19 . Na20 . 2.301(2) yes
Na20 . O21 1_655 2.3241(19) yes
Na20 . O50 2_765 2.4499(19) yes
Na20 . Na20 2_765 3.2965(18) yes
Na20 . O50 . 2.4011(18) yes
O21 . S22 . 1.4498(17) yes
S22 . O23 . 1.4524(18) yes
S22 . O24 . 1.4540(19) yes
S22 . C25 . 1.769(2) yes
C25 . C26 . 1.388(3) yes
C25 . C31 . 1.390(3) yes
C26 . C27 . 1.393(3) yes
C26 . H261 . 0.928 no
C27 . C28 . 1.387(3) yes
C27 . C33 . 1.526(3) yes
C28 . O29 . 1.374(3) yes
C28 . C30 . 1.403(3) yes
O29 . H291 . 0.814 no
C30 . C31 . 1.391(3) yes
C30 . C32 . 1.518(3) yes
C31 . H311 . 0.926 no
C32 . H322 . 0.981 no
C32 . H321 . 0.960 no
C33 . C34 . 1.528(3) yes
C33 . H331 . 0.966 no
C33 . H332 . 0.974 no
C34 . C35 . 1.405(3) yes
C34 . C45 . 1.381(3) yes
C35 . O36 . 1.374(3) yes
C35 . C37 . 1.402(3) yes
O36 . H361 . 0.814 no
C37 . C38 . 1.528(3) yes
C37 . C43 . 1.385(3) yes
C38 . C39 . 1.517(3) yes
C38 . H381 . 0.971 no
C38 . H382 . 0.966 no
C39 . C40 . 1.400(3) yes
C39 . C41 . 1.399(3) yes
C40 . H401 . 0.940 no
C41 . O42 . 1.368(3) yes
O42 . H421 . 0.806 no
C43 . C44 . 1.390(3) yes
C43 . H431 . 0.939 no
C44 . C45 . 1.388(3) yes
C44 . S46 . 1.763(2) yes
C45 . H451 . 0.952 no
S46 . O47 . 1.4502(19) yes
S46 . O48 . 1.452(2) yes
S46 . O49 . 1.464(2) yes
O50 . C51 . 1.221(3) yes
C51 . O52 . 1.319(3) yes
C51 . C53 . 1.496(3) yes
O52 . H521 . 0.842 no
C53 . C54 . 1.519(3) yes
C53 . H532 . 0.971 no
C53 . H531 . 0.968 no
C54 . C55 . 1.528(3) yes
C54 . H542 . 0.968 no
C54 . H541 . 0.962 no
C55 . C56 . 1.522(3) yes
C55 . H552 . 0.965 no
C55 . H551 . 0.957 no
C56 . C57 . 1.511(3) yes
C56 . H562 . 0.974 no
C56 . H561 . 0.969 no
C57 . N58 . 1.487(3) yes
C57 . H571 . 0.971 no
C57 . H572 . 0.965 no
N58 . H582 . 0.881 no
N58 . H583 . 0.891 no
N58 . H581 . 0.887 no
N63 . C64 . 1.326(3) yes
N63 . H632 . 0.843 no
N63 . H631 . 0.855 no
C64 . N65 . 1.309(4) yes
C64 . N66 . 1.316(4) yes
N65 . H652 . 0.873 no
N65 . H651 . 0.854 no
N66 . H661 . 0.856 no
N66 . H662 . 0.849 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
Na20 2_665 S1 . O2 . 51.78(8) yes
Na20 2_665 S1 . O3 . 60.89(8) yes
O2 . S1 . O3 . 112.39(11) yes
Na20 2_665 S1 . O4 . 128.03(8) yes
O2 . S1 . O4 . 112.28(12) yes
O3 . S1 . O4 . 112.34(11) yes
Na20 2_665 S1 . C5 . 125.32(8) yes
O2 . S1 . C5 . 106.39(10) yes
O3 . S1 . C5 . 106.52(10) yes
O4 . S1 . C5 . 106.37(11) yes
Na20 2_665 O2 . S1 . 101.42(10) yes
S1 . O3 . Na20 2_665 91.82(9) yes
S1 . C5 . C6 . 120.38(17) yes
S1 . C5 . C11 . 118.85(17) yes
C6 . C5 . C11 . 120.7(2) yes
C5 . C6 . C7 . 119.8(2) yes
C5 . C6 . H61 . 120.0 no
C7 . C6 . H61 . 120.1 no
C6 . C7 . C8 . 118.58(19) yes
C6 . C7 . C32 . 119.49(19) yes
C8 . C7 . C32 . 121.9(2) yes
C7 . C8 . O9 . 115.97(19) yes
C7 . C8 . C10 . 122.1(2) yes
O9 . C8 . C10 . 121.93(19) yes
C8 . O9 . H91 . 111.2 no
C8 . C10 . C11 . 117.52(19) yes
C8 . C10 . C12 . 123.19(19) yes
C11 . C10 . C12 . 119.29(19) yes
C5 . C11 . C10 . 121.3(2) yes
C5 . C11 . H111 . 119.9 no
C10 . C11 . H111 . 118.8 no
C10 . C12 . C13 . 112.73(17) yes
C10 . C12 . H122 . 110.9 no
C13 . C12 . H122 . 108.4 no
C10 . C12 . H121 . 108.1 no
C13 . C12 . H121 . 108.9 no
H122 . C12 . H121 . 107.7 no
C12 . C13 . C14 . 121.22(19) yes
C12 . C13 . C41 . 120.46(19) yes
C14 . C13 . C41 . 118.3(2) yes
C13 . C14 . C15 . 120.3(2) yes
C13 . C14 . H141 . 119.4 no
C15 . C14 . H141 . 120.3 no
C14 . C15 . S16 . 118.02(16) yes
C14 . C15 . C40 . 120.6(2) yes
S16 . C15 . C40 . 121.24(17) yes
C15 . S16 . O17 . 106.16(11) yes
C15 . S16 . O18 . 105.95(11) yes
O17 . S16 . O18 . 112.09(15) yes
C15 . S16 . O19 . 106.61(11) yes
O17 . S16 . O19 . 111.80(15) yes
O18 . S16 . O19 . 113.61(14) yes
S16 . O19 . Na20 . 143.27(12) yes
O19 . Na20 . O21 1_655 91.49(7) yes
O19 . Na20 . O50 2_765 124.90(9) yes
O21 1_655 Na20 . O50 2_765 85.33(6) yes
O19 . Na20 . Na20 2_765 128.92(7) yes
O21 1_655 Na20 . Na20 2_765 128.04(6) yes
O50 2_765 Na20 . Na20 2_765 46.57(4) yes
O19 . Na20 . O2 2_665 108.26(8) yes
O21 1_655 Na20 . O2 2_665 79.54(7) yes
O50 2_765 Na20 . O2 2_665 124.92(7) yes
Na20 2_765 Na20 . O2 2_665 109.61(6) yes
O19 . Na20 . O3 2_665 161.62(8) yes
O21 1_655 Na20 . O3 2_665 81.06(6) yes
O50 2_765 Na20 . O3 2_665 71.51(6) yes
Na20 2_765 Na20 . O3 2_665 67.45(5) yes
O2 2_665 Na20 . O3 2_665 53.99(6) yes
O19 . Na20 . S1 2_665 134.62(7) yes
O21 1_655 Na20 . S1 2_665 77.43(5) yes
O50 2_765 Na20 . S1 2_665 98.24(5) yes
Na20 2_765 Na20 . S1 2_665 89.67(4) yes
O2 2_665 Na20 . S1 2_665 26.80(4) yes
O19 . Na20 . O50 . 106.18(7) yes
O21 1_655 Na20 . O50 . 158.28(7) yes
O50 2_765 Na20 . O50 . 94.39(6) yes
Na20 2_765 Na20 . O50 . 47.82(5) yes
O2 2_665 Na20 . O50 . 82.91(6) yes
O3 2_665 Na20 . S1 2_665 27.29(4) yes
O3 2_665 Na20 . O50 . 78.29(6) yes
S1 2_665 Na20 . O50 . 81.13(5) yes
Na20 1_455 O21 . S22 . 149.19(11) yes
O21 . S22 . O23 . 111.95(11) yes
O21 . S22 . O24 . 112.59(11) yes
O23 . S22 . O24 . 113.07(12) yes
O21 . S22 . C25 . 106.49(10) yes
O23 . S22 . C25 . 106.40(11) yes
O24 . S22 . C25 . 105.71(11) yes
S22 . C25 . C26 . 121.42(18) yes
S22 . C25 . C31 . 117.95(17) yes
C26 . C25 . C31 . 120.6(2) yes
C25 . C26 . C27 . 120.1(2) yes
C25 . C26 . H261 . 119.7 no
C27 . C26 . H261 . 120.2 no
C26 . C27 . C28 . 118.7(2) yes
C26 . C27 . C33 . 120.7(2) yes
C28 . C27 . C33 . 120.6(2) yes
C27 . C28 . O29 . 116.8(2) yes
C27 . C28 . C30 . 122.1(2) yes
O29 . C28 . C30 . 121.1(2) yes
C28 . O29 . H291 . 112.7 no
C28 . C30 . C31 . 118.1(2) yes
C28 . C30 . C32 . 122.3(2) yes
C31 . C30 . C32 . 119.5(2) yes
C30 . C31 . C25 . 120.4(2) yes
C30 . C31 . H311 . 120.3 no
C25 . C31 . H311 . 119.3 no
C7 . C32 . C30 . 111.86(17) yes
C7 . C32 . H322 . 110.2 no
C30 . C32 . H322 . 109.6 no
C7 . C32 . H321 . 108.9 no
C30 . C32 . H321 . 107.4 no
H322 . C32 . H321 . 108.7 no
C27 . C33 . C34 . 112.06(17) yes
C27 . C33 . H331 . 109.8 no
C34 . C33 . H331 . 109.9 no
C27 . C33 . H332 . 108.0 no
C34 . C33 . H332 . 107.4 no
H331 . C33 . H332 . 109.7 no
C33 . C34 . C35 . 122.4(2) yes
C33 . C34 . C45 . 119.6(2) yes
C35 . C34 . C45 . 118.0(2) yes
C34 . C35 . O36 . 121.1(2) yes
C34 . C35 . C37 . 121.9(2) yes
O36 . C35 . C37 . 117.0(2) yes
C35 . O36 . H361 . 107.8 no
C35 . C37 . C38 . 121.8(2) yes
C35 . C37 . C43 . 118.3(2) yes
C38 . C37 . C43 . 119.91(19) yes
C37 . C38 . C39 . 113.38(17) yes
C37 . C38 . H381 . 109.4 no
C39 . C38 . H381 . 109.5 no
C37 . C38 . H382 . 108.6 no
C39 . C38 . H382 . 106.8 no
H381 . C38 . H382 . 109.0 no
C38 . C39 . C40 . 120.44(19) yes
C38 . C39 . C41 . 121.74(19) yes
C40 . C39 . C41 . 117.82(19) yes
C39 . C40 . C15 . 120.5(2) yes
C39 . C40 . H401 . 119.5 no
C15 . C40 . H401 . 119.9 no
C39 . C41 . C13 . 122.2(2) yes
C39 . C41 . O42 . 122.08(19) yes
C13 . C41 . O42 . 115.67(19) yes
C41 . O42 . H421 . 110.0 no
C37 . C43 . C44 . 120.4(2) yes
C37 . C43 . H431 . 119.5 no
C44 . C43 . H431 . 120.1 no
C43 . C44 . C45 . 120.4(2) yes
C43 . C44 . S46 . 121.24(18) yes
C45 . C44 . S46 . 118.39(18) yes
C44 . C45 . C34 . 120.9(2) yes
C44 . C45 . H451 . 119.1 no
C34 . C45 . H451 . 119.9 no
C44 . S46 . O47 . 107.24(11) yes
C44 . S46 . O48 . 106.24(12) yes
O47 . S46 . O48 . 113.44(11) yes
C44 . S46 . O49 . 105.82(11) yes
O47 . S46 . O49 . 111.45(13) yes
O48 . S46 . O49 . 112.08(13) yes
Na20 . O50 . Na20 2_765 85.61(6) yes
Na20 . O50 . C51 . 136.33(16) yes
Na20 2_765 O50 . C51 . 120.90(14) yes
O50 . C51 . O52 . 122.7(2) yes
O50 . C51 . C53 . 124.3(2) yes
O52 . C51 . C53 . 113.0(2) yes
C51 . O52 . H521 . 105.1 no
C51 . C53 . C54 . 114.09(19) yes
C51 . C53 . H532 . 106.3 no
C54 . C53 . H532 . 107.7 no
C51 . C53 . H531 . 109.0 no
C54 . C53 . H531 . 111.2 no
H532 . C53 . H531 . 108.3 no
C53 . C54 . C55 . 113.7(2) yes
C53 . C54 . H542 . 108.0 no
C55 . C54 . H542 . 109.1 no
C53 . C54 . H541 . 109.2 no
C55 . C54 . H541 . 109.4 no
H542 . C54 . H541 . 107.2 no
C54 . C55 . C56 . 111.27(19) yes
C54 . C55 . H552 . 108.9 no
C56 . C55 . H552 . 108.5 no
C54 . C55 . H551 . 109.4 no
C56 . C55 . H551 . 109.4 no
H552 . C55 . H551 . 109.4 no
C55 . C56 . C57 . 114.3(2) yes
C55 . C56 . H562 . 109.5 no
C57 . C56 . H562 . 107.8 no
C55 . C56 . H561 . 107.3 no
C57 . C56 . H561 . 107.7 no
H562 . C56 . H561 . 110.2 no
C56 . C57 . N58 . 110.11(19) yes
C56 . C57 . H571 . 110.1 no
N58 . C57 . H571 . 108.3 no
C56 . C57 . H572 . 111.5 no
N58 . C57 . H572 . 107.8 no
H571 . C57 . H572 . 108.9 no
C57 . N58 . H582 . 110.9 no
C57 . N58 . H583 . 111.7 no
H582 . N58 . H583 . 107.4 no
C57 . N58 . H581 . 109.0 no
H582 . N58 . H581 . 108.7 no
H583 . N58 . H581 . 109.0 no
C64 . N63 . H632 . 117.8 no
C64 . N63 . H631 . 119.8 no
H632 . N63 . H631 . 120.9 no
N63 . C64 . N65 . 118.4(3) yes
N63 . C64 . N66 . 120.9(3) yes
N65 . C64 . N66 . 120.6(2) yes
C64 . N65 . H652 . 120.8 no
C64 . N65 . H651 . 118.8 no
H652 . N65 . H651 . 120.4 no
C64 . N66 . H661 . 118.2 no
C64 . N66 . H662 . 121.4 no
H661 . N66 . H662 . 120.4 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C43 . H431 . O23 1_655 169.66(7) 0.939 2.473 3.401(3) yes
O36 . H361 . O29 . 160.46(7) 0.814 1.935 2.716(3) yes
N65 . H652 . O48 1_456 174.01(11) 0.873 2.008 2.878(3) yes
N66 . H661 . O47 1_456 173.95(8) 0.856 2.053 2.905(3) yes
O29 . H291 . O9 . 166.66(7) 0.814 1.904 2.702(3) yes
N58 . H582 . O23 2_565 156.97(8) 0.881 2.090 2.921(3) yes
O9 . H91 . O42 . 139.04(6) 0.809 2.097 2.760(3) yes
O42 . H421 . O36 . 164.92(7) 0.806 1.884 2.671(3) yes
N63 . H632 . O4 . 134.36(8) 0.843 2.352 3.003(3) yes
N58 . H583 . O2 . 166.99(9) 0.891 1.910 2.785(3) yes
N66 . H662 . O24 1_556 146.25(8) 0.849 2.183 2.927(3) yes
N65 . H651 . O18 1_455 146.28(9) 0.854 2.274 3.022(3) yes
N63 . H631 . O18 1_455 145.53(8) 0.855 2.265 3.009(3) yes
N58 . H581 . O47 2_665 140.95(7) 0.887 2.233 2.974(3) yes
O52 . H521 . O3 1_655 177.11(8) 0.842 1.857 2.699(3) yes


