# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_ox117_squeeze_NH_CCDC1028969
_database_code_depnum_ccdc_archive 'CCDC 1028969'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;
_audit_creation_date             10-03-25
_audit_creation_method           CRYSTALS_ver_12.80

_exptl_special_details           
;
The small crystal size, large unit cell and very high degree of disorder 
within the crystal gave rise to very weak scattering despite the use 
of the SRS Daresbury synchrotron radiation source. As high-angle data had negligible 
intensity, they were not measured.

Due to the low number of observed data, anisotropic atomic displacement 
parameters were only included in the model for the porphyrin core and S atoms.

There is a large number of disordered water molecules in the asymmetric unit and possibly one THF molecule (disordered over more than two sites). 
Therefore, treatment of rezidual electron density using the SQUEEZE
procedure (P. v.d. Sluis & A. L. Spek, Acta Crystallogr. 1990, A46, 194.),
implemented in PLATON (PLATON, A Multipurpose Crystallographic Tool,
Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998.) was used.
In the current model, the Platon output reports that structure Contains Solvent Accessible VOIDS of 4428.9 Ang3, electron count per cell of 1405.

Two water molecules (containing O13 and O14) are also disordered but have been retained 
as a part of the model and refined isotropically, rather than treated by the Squeeze option, since they appear to be
involved in H bonding with the main molecule. The corresponding H atoms have not been found 
with in Fourier maps and could not be placed with precision, in view of 
severe shortage of data. Hydrogen atoms on main carbon atoms were placed geometrically after each cycle. 

The N-bound H's and the H belonging to the NH groups in the main molecule could be found in a Fourier map, and their positions were 
adjusted by refinement. A further peak was found by the fourier map in proximity of 
O10: the possibility of its disorder with respect to an acetiminde /amide rearrangment cannot be ignored. 
Current assignment is supported by the spectroscopic data and, although connectivity of the porphyrin centre and peripheral substituents is proven, this cif file should only be used together with the spectroscopic evidence.
An examination of the Fourier maps indicated that each phenyl group is disordered over more than two sites: as such all phenyl rings in porphyrin core are severely disordered: these were idealised and refinement was carried out with similarity restrains.  
The sulponamide group (2 oxygen and one NH2 group) is rotationally disordered on more than two sites and the current model is tentative only. 
The discrepancies reported by PLATON/Checkcif regarding molecular formula
etc are associated with this non-standard model - correct values are reported
in this cif file.
There are several short intermolecular contacts (between O2..O13, O5 ..O13, O9..O14, O12..O14, O3..O13)
As these atoms are all parts of disordered sites which have been modelled, no great faith can be placed in
their coordinates.
Severe shortage of data made the modelling described for disordered groups listed above only tentative
;

_vrf_THETM01_ox117_squeeze_NH    
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The small crystal size, large unit cell and very high degree of disorder 
within the crystal gave rise to very weak scattering despite the use 
of the SRS Daresbury synchrotron radiation source. As high-angle data had negligible 
intensity, they were not measured.
;
_vrf_REFNR01_ox117_squeeze_NH    
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: The small crystal size, large unit cell and very high degree of disorder 
within the crystal gave rise to very weak scattering despite the use 
of the SRS Daresbury synchrotron radiation source. As high-angle data had negligible 
intensity, they were not measured.

;
_vrf_PLAT027_ox117_squeeze_NH    
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      19.73 Degree
RESPONSE: The small crystal size, large unit cell and very high degree of disorder 
within the crystal gave rise to very weak scattering despite the use 
of the SRS Daresbury synchrotron radiation source. As high-angle data had negligible 
intensity, they were not measured.

;
_vrf_PLAT201_ox117_squeeze_NH    
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         47 Report
RESPONSE: Due to the low number of observed data, anisotropic atomic displacement 
parameters were only included in the model for the porphyrin core and S atoms.
;

_vrf_PLAT601_ox117_squeeze_NH    
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .       1007 Ang3  
RESPONSE: There is a large number of disordered water molecules in the asymmetric unit. This assigment was only tentative in view of severe data shortage.
Therefore, treatment of rezidual electron density using the SQUEEZE
procedure (P. v.d. Sluis & A. L. Spek, Acta Crystallogr. 1990, A46, 194.),
implemented in PLATON (PLATON, A Multipurpose Crystallographic Tool,
Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998.) was used.
;

_vrf_PLAT430_ox117_squeeze_NH    
;
PROBLEM: Short Inter D...A Contact  O2     ..  O14     ..       2.36 Ang.  
RESPONSE: Two water molecules (containing O13 and O14) are also disordered have been retained 
as a part of the model and refined isotropically, rather than treated by the Squeeze option, since they appear to be
involved in H bonding with the main molecule. The corresponding H atoms have not been found 
with in Fourier maps and could not be placed with precision, in view of 
severe shortage of data.  
;

_vrf_PLAT026_ox117_squeeze_NH    
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         38 %     
RESPONSE: The small crystal size, large unit cell and very high degree of disorder 
within the crystal gave rise to very weak scattering despite the use 
of the SRS Daresbury synchrotron radiation source. As high-angle data had negligable 
intensity, they were not measured.
;
_vrf_PLAT306_ox117_squeeze_NH    
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check 
RESPONSE: Two water molecules (containing O13 and O14) are also disordered have been retained 
as a part of the model and refined isotropically, rather than treated by the Squeeze option, since they appear to be
involved in H bonding with the main molecule. The corresponding H atoms have not been found 
with in Fourier maps and could not be placed with precision, in view of 
severe shortage of data
;
_vrf_PLAT340_ox117_squeeze_NH    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0208 Ang.  
RESPONSE: An examination of the Fourier maps indicated that each phenyl group is disordered over more than two sites: as such all phenyl rings in porphyrin core are severely disordered: these were idealised and refinement was carried out with similarity restrains.  
;
_vrf_PLAT369_ox117_squeeze_NH    
;
PROBLEM: Long   C(sp2)-C(sp2) Bond  C42    -   C45    ...       1.60 Ang.  
RESPONSE: An examination of the Fourier maps indicated that each phenyl group is disordered over more than two sites: as such all phenyl rings in porphyrin core are severely disordered: these were idealised and refinement was carried out with similarity restrains.  
;
# end Validation Reply Form


_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   43.396(15)
_cell_length_b                   8.396(3)
_cell_length_c                   39.773(14)
_cell_angle_alpha                90
_cell_angle_beta                 114.146(6)
_cell_angle_gamma                90
_cell_volume                     13223(8)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 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            8

_chemical_formula_sum            'C53 H35 N6 O14 S4'
_chemical_formula_moiety         'C53 H35 N6 O14 S4'
_chemical_compound_source        ?
_chemical_formula_weight         1108.16


_cell_measurement_reflns_used    6835
_cell_measurement_theta_min      1
_cell_measurement_theta_max      22
_cell_measurement_temperature    150

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_max          0.35

_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_meas      ?
# Non-dispersive F(000): 
_exptl_crystal_F_000             4584
_exptl_absorpt_coefficient_mu    0.202

_exptl_absorpt_process_details   
;

  Correction applied by SADABS - note that the transmission factors are
  not real since they include corrections for beam decay and possibly
  crystal decay (the two cannot be distinguished).
  The numbers listed in the CIF are those calculated by CRYSTALS.
;
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_T_max  1.00

_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD'
_diffrn_measurement_method       'fine-slice ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        5
_diffrn_radiation_wavelength     0.69440

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    Sir2000
_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_ambient_temperature      150
_diffrn_reflns_number            6829
_reflns_number_total             6829
_diffrn_reflns_av_R_equivalents  0.043
# Number of reflections with Friedels Law is 6829 
# Number of reflections without Friedels Law is 0 
# Theoretical number of reflections is about 6866 


_diffrn_reflns_theta_min         1.005
_diffrn_reflns_theta_max         20.337
_diffrn_measured_fraction_theta_max 0.983

_diffrn_reflns_theta_full        19.727
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       39
_reflns_limit_h_min              -42
_reflns_limit_h_max              39
_reflns_limit_k_min              0
_reflns_limit_k_max              8
_reflns_limit_l_min              0
_reflns_limit_l_max              39

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     direct
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.71
_refine_diff_density_max         1.09


_refine_ls_number_reflns         2620
_refine_ls_number_restraints     203
_refine_ls_number_parameters     413

#_refine_ls_R_factor_ref 0.1333 
_refine_ls_wR_factor_ref         0.1244
_refine_ls_goodness_of_fit_ref   1.1404

#_reflns_number_all 6777 
_refine_ls_R_factor_all          0.2103
_refine_ls_wR_factor_all         0.1490

# The I/u(I) cutoff below was used for refinement as 
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                2620
_refine_ls_R_factor_gt           0.1333
_refine_ls_wR_factor_gt          0.1244

_refine_ls_shift/su_max          0.017917

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


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref
_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: 
 2.50 1.82 1.97 
;

_diffrn_special_details          
;
The small crystal size, large unit cell and very high degree of disorder 
within the crystal gave rise to very weak scattering despite the use 
of the SRS Daresbury synchrotron radiation source. As high-angle data had negligable 
intensity, they were not measured.
;
_refine_special_details          
;

Due to the low number of observed data, anisotropic atomic displacement 
parameters were only included in the model for the porphyrin core and S atoms.

There is a large number of disordered water molecules in the asymmetric unit. This assigment was only tentative in view of severe data shortage.
Therefore, treatment of rezidual electron density using the SQUEEZE
procedure (P. v.d. Sluis & A. L. Spek, Acta Crystallogr. 1990, A46, 194.),
implemented in PLATON (PLATON, A Multipurpose Crystallographic Tool,
Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998.) was used.
In the current model, the structure Contains Solvent Accessible VOIDS of 4428.9 Ang3.

Two water molecules (containing O13 and O14) are also disordered have been retained 
as a part of the model and refined isotropically, rather than treated by the Squeeze option, since they appear to be
involved in H bonding with the main molecule. The corresponding H atoms have not been found 
with in Fourier maps and could not be placed with precision, in view of 
severe shortage of data. Hydrogen atoms on main carbon atoms were placed geometrically after each cycle. 

The N-bound H's and the H belonging to the NH groups in 
main molecule could be found in a Fourier map, and their positions were 
adjusted by refinement. A further peak was found by the fourier map in proximity of 
O10: the possibility of its disorder with respect to an acetiminde /amide rearrangment cannot be ignored. 
Current assigment is supported by the spectroscopic data and, although connectivity of the porphyrin centre and peripheral substituents is proven, this cif file should only be used together with the spectroscopic evidence.
 
An examination of the Fourier maps indicated that each phenyl group is disordered over more than two sites: as such all phenyl rings in porphyrin core are severely disordered: these were idealised and refinement was carried out with similarity restrains.  

The sulponamide group (2 oxygen and one NH2 group) is rotationally disordered on more than two sites and the current model is tentative only. 
The discrepancies reported by PLATON/Checkcif regarding molecular formula
etc are associated with this non-standard model - correct values are reported
in this cif file.


There are several short intermolecular contacts (between O2..O13, O5 ..O13, O9..O14, O12..O14, O3..O13)
As these atoms are all parts of disordered sites which have been modelled, no great faith can be placed in
their coordinates.

Severe shortage of data made the modelling described for disordered groups (above) only tentative

;

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

# Replace last . with number of unfound hydrogen atomsattached 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 0.33443(10) 0.6113(7) 0.58296(12) 0.0650 1.0000 Uani . . . . . .
S2 S 0.65340(13) 0.2363(9) 0.79587(12) 0.0826 1.0000 Uani . . . . . .
S3 S 0.71009(10) -0.1411(7) 0.50000(13) 0.0700 1.0000 Uani . . . . . .
S4 S 0.25756(16) -0.0490(10) 0.37627(18) 0.1051 1.0000 Uani . . . . . .
N1 N 0.4715(3) 0.3204(16) 0.5048(3) 0.0431 1.0000 Uani . U . . . .
N2 N 0.5139(3) 0.3124(16) 0.5840(3) 0.0439 1.0000 Uani . U . . . .
N3 N 0.5697(3) 0.2000(15) 0.5683(3) 0.0430 1.0000 Uani . U . . . .
N4 N 0.5266(3) 0.1866(16) 0.4895(3) 0.0428 1.0000 Uani . U . . . .
C1 C 0.4512(3) 0.397(2) 0.5163(4) 0.0433 1.0000 Uani . U . . . .
C2 C 0.4232(3) 0.459(2) 0.4854(4) 0.0437 1.0000 Uani . U . . . .
C3 C 0.4265(3) 0.417(2) 0.4548(4) 0.0436 1.0000 Uani . U . . . .
C4 C 0.4578(3) 0.327(2) 0.4669(4) 0.0436 1.0000 Uani . U . . . .
C5 C 0.4703(3) 0.256(2) 0.4442(4) 0.0436 1.0000 Uani . U . . . .
C6 C 0.5007(3) 0.179(2) 0.4550(4) 0.0429 1.0000 Uani . U . . . .
C7 C 0.5133(3) 0.080(2) 0.4321(4) 0.0427 1.0000 Uani . U . . . .
C8 C 0.5462(3) 0.043(2) 0.4536(4) 0.0423 1.0000 Uani . U . . . .
C9 C 0.5543(3) 0.105(2) 0.4895(4) 0.0426 1.0000 Uani . U . . . .
C10 C 0.5865(3) 0.098(2) 0.5194(4) 0.0431 1.0000 Uani . U . . . .
C11 C 0.5934(3) 0.148(2) 0.5564(4) 0.0430 1.0000 Uani . U . . . .
C12 C 0.6271(3) 0.158(2) 0.5874(4) 0.0430 1.0000 Uani . U . . . .
C13 C 0.6221(3) 0.196(2) 0.6159(4) 0.0432 1.0000 Uani . U . . . .
C14 C 0.5870(3) 0.225(2) 0.6063(4) 0.0429 1.0000 Uani . U . . . .
C15 C 0.5722(3) 0.257(2) 0.6308(4) 0.0434 1.0000 Uani . U . . . .
C16 C 0.5373(3) 0.286(2) 0.6203(4) 0.0436 1.0000 Uani . U . . . .
C17 C 0.5198(3) 0.322(2) 0.6430(4) 0.0440 1.0000 Uani . U . . . .
C18 C 0.4887(3) 0.367(2) 0.6226(4) 0.0437 1.0000 Uani . U . . . .
C19 C 0.4834(3) 0.361(2) 0.5849(4) 0.0436 1.0000 Uani . U . . . .
C20 C 0.4548(3) 0.411(2) 0.5530(4) 0.0438 1.0000 Uani . U . . . .
N5 N 0.3408(4) 0.2742(19) 0.2869(4) 0.069(4) 1.0000 Uiso . . . . . .
N6 N 0.2264(6) -0.146(3) 0.3612(6) 0.127(7) 1.0000 Uiso . . . . . .
C45 C 0.3702(5) 0.252(2) 0.2895(5) 0.067(5) 1.0000 Uiso . . . . . .
O10 O 0.3811(3) 0.2530(17) 0.2652(4) 0.083(4) 1.0000 Uiso . . . . . .
O11 O 0.2889(4) -0.146(2) 0.4026(5) 0.116(5) 1.0000 Uiso . . . . . .
O12 O 0.2495(4) 0.104(2) 0.3900(5) 0.128(6) 1.0000 Uiso . . . . . .
C21 C 0.4252(3) 0.4730(14) 0.5609(3) 0.043(3) 1.0000 Uiso . . . . . .
C22 C 0.3955(3) 0.3822(14) 0.5441(3) 0.047(3) 1.0000 Uiso . . . . . .
C23 C 0.3667(3) 0.4294(15) 0.5521(3) 0.054(3) 1.0000 Uiso . . . . . .
C24 C 0.3700(3) 0.5629(15) 0.5737(3) 0.043(3) 1.0000 Uiso . . . . . .
C25 C 0.4015(3) 0.6349(14) 0.5908(3) 0.037(3) 1.0000 Uiso . . . . . .
C26 C 0.4274(3) 0.5968(14) 0.5850(3) 0.037(3) 1.0000 Uiso . . . . . .
C27 C 0.5927(3) 0.2380(19) 0.6709(4) 0.035(4) 1.0000 Uiso . . . . . .
C28 C 0.5857(4) 0.128(2) 0.6928(4) 0.047(4) 1.0000 Uiso . . . . . .
C29 C 0.6049(4) 0.127(2) 0.7306(5) 0.062(5) 1.0000 Uiso . . . . . .
C30 C 0.6309(4) 0.230(2) 0.7463(4) 0.049(4) 1.0000 Uiso . . . . . .
C31 C 0.6398(4) 0.347(2) 0.7263(4) 0.053(4) 1.0000 Uiso . . . . . .
C32 C 0.6188(4) 0.351(2) 0.6866(4) 0.055(5) 1.0000 Uiso . . . . . .
C33 C 0.6166(3) 0.0415(14) 0.5148(3) 0.043(3) 1.0000 Uiso . . . . . .
C34 C 0.6347(3) -0.0877(14) 0.5336(3) 0.057(3) 1.0000 Uiso . . . . . .
C35 C 0.6620(3) -0.1434(15) 0.5282(3) 0.056(3) 1.0000 Uiso . . . . . .
C36 C 0.6723(3) -0.0750(15) 0.5058(3) 0.058(3) 1.0000 Uiso . . . . . .
C37 C 0.6528(3) 0.0548(14) 0.4833(3) 0.059(3) 1.0000 Uiso . . . . . .
C38 C 0.6256(3) 0.1078(14) 0.4873(3) 0.056(3) 1.0000 Uiso . . . . . .
C39 C 0.4465(3) 0.239(2) 0.4036(4) 0.039(4) 1.0000 Uiso . . . . . .
C40 C 0.4146(3) 0.1745(18) 0.3941(4) 0.040(4) 1.0000 Uiso . . . . . .
C41 C 0.3905(4) 0.176(2) 0.3585(4) 0.055(5) 1.0000 Uiso . . . . . .
C42 C 0.3997(4) 0.246(2) 0.3302(4) 0.045(4) 1.0000 Uiso . . . . . .
C43 C 0.4309(4) 0.3025(19) 0.3400(4) 0.045(4) 1.0000 Uiso . . . . . .
C44 C 0.4549(3) 0.3040(19) 0.3760(4) 0.041(4) 1.0000 Uiso . . . . . .
C46 C 0.3085(5) 0.277(3) 0.2510(6) 0.086(6) 1.0000 Uiso . . . . . .
C47 C 0.2902(4) 0.1240(19) 0.2458(5) 0.081(6) 1.0000 Uiso . . . . . .
C48 C 0.2811(5) 0.080(2) 0.2753(5) 0.093(7) 1.0000 Uiso . . . . . .
C49 C 0.2539(4) 0.150(2) 0.2809(5) 0.085(6) 1.0000 Uiso . . . . . .
C50 C 0.2449(5) 0.103(2) 0.3117(5) 0.091(7) 1.0000 Uiso . . . . . .
C51 C 0.2635(5) -0.008(2) 0.3355(5) 0.091(7) 1.0000 Uiso . . . . . .
C52 C 0.2918(4) -0.080(2) 0.3297(5) 0.085(6) 1.0000 Uiso . . . . . .
C53 C 0.2999(4) -0.0423(17) 0.3026(4) 0.063(5) 1.0000 Uiso . . . . . .
O1 O 0.3079(2) 0.6492(12) 0.5477(3) 0.075(3) 1.0000 Uiso . . . . . .
O2 O 0.3246(2) 0.4734(11) 0.5972(2) 0.068(3) 1.0000 Uiso . . . . . .
O3 O 0.3444(2) 0.7392(12) 0.6065(3) 0.075(3) 1.0000 Uiso . . . . . .
O4 O 0.6304(3) 0.1735(17) 0.8103(4) 0.088(4) 1.0000 Uiso . . . . . .
O5 O 0.6646(4) 0.399(2) 0.8048(4) 0.100(5) 1.0000 Uiso . . . . . .
O6 O 0.6826(3) 0.1322(17) 0.8040(4) 0.084(4) 1.0000 Uiso . . . . . .
O7 O 0.7213(2) -0.2852(12) 0.5224(3) 0.093(3) 1.0000 Uiso . . . . . .
O8 O 0.7322(2) -0.0168(11) 0.5130(2) 0.080(3) 1.0000 Uiso . . . . . .
O9 O 0.6980(2) -0.1709(12) 0.4611(3) 0.088(3) 1.0000 Uiso . . . . . .
O13 O 0.1741(3) -0.0877(14) 0.3456(3) 0.061(3) 1.0000 Uiso . . . . . .
O14 O 0.7760(2) -0.1886(12) 0.5731(2) 0.042(3) 1.0000 Uiso . . . . . .
H1 H 0.5173 0.2951 0.5653 0.0641 1.0000 Uiso . . . . . .
H2 H 0.5259 0.2324 0.5094 0.0630 1.0000 Uiso . . . . . .
H3 H 0.3388 0.2991 0.3076 0.0980 1.0000 Uiso . . . . . .
H4 H 0.2336 -0.2458 0.3513 0.1507 1.0000 Uiso . . . . . .
H5 H 0.2217 -0.1707 0.3784 0.1507 1.0000 Uiso . . . . . .
H532 H 0.4054 0.5182 0.4866 0.0629 1.0000 Uiso . . . . . .
H31 H 0.4116 0.4401 0.4305 0.0630 1.0000 Uiso . . . . . .
H71 H 0.5012 0.0492 0.4079 0.0620 1.0000 Uiso . . . . . .
H81 H 0.5606 -0.0130 0.4459 0.0620 1.0000 Uiso . . . . . .
H121 H 0.6478 0.1401 0.5863 0.0630 1.0000 Uiso . . . . . .
H131 H 0.6389 0.2037 0.6397 0.0631 1.0000 Uiso . . . . . .
H171 H 0.5290 0.3157 0.6685 0.0651 1.0000 Uiso . . . . . .
H181 H 0.4726 0.3985 0.6312 0.0640 1.0000 Uiso . . . . . .
H221 H 0.3945 0.2955 0.5289 0.0680 1.0000 Uiso . . . . . .
H231 H 0.3466 0.3706 0.5428 0.0771 1.0000 Uiso . . . . . .
H251 H 0.4037 0.7178 0.6072 0.0540 1.0000 Uiso . . . . . .
H261 H 0.4476 0.6520 0.5971 0.0538 1.0000 Uiso . . . . . .
H281 H 0.5682 0.0546 0.6821 0.0671 1.0000 Uiso . . . . . .
H291 H 0.5999 0.0531 0.7455 0.0889 1.0000 Uiso . . . . . .
H311 H 0.6578 0.4170 0.7377 0.0771 1.0000 Uiso . . . . . .
H321 H 0.6228 0.4264 0.6717 0.0810 1.0000 Uiso . . . . . .
H341 H 0.6286 -0.1402 0.5506 0.0820 1.0000 Uiso . . . . . .
H351 H 0.6733 -0.2331 0.5410 0.0801 1.0000 Uiso . . . . . .
H371 H 0.6592 0.1017 0.4659 0.0850 1.0000 Uiso . . . . . .
H381 H 0.6127 0.1896 0.4723 0.0799 1.0000 Uiso . . . . . .
H401 H 0.4092 0.1286 0.4123 0.0579 1.0000 Uiso . . . . . .
H411 H 0.3691 0.1335 0.3527 0.0801 1.0000 Uiso . . . . . .
H431 H 0.4368 0.3433 0.3216 0.0651 1.0000 Uiso . . . . . .
H441 H 0.4763 0.3482 0.3820 0.0589 1.0000 Uiso . . . . . .
H461 H 0.3148 0.2906 0.2305 0.1221 1.0000 Uiso . . . . . .
H462 H 0.2940 0.3632 0.2517 0.1220 1.0000 Uiso . . . . . .
H491 H 0.2412 0.2298 0.2645 0.1190 1.0000 Uiso . . . . . .
H501 H 0.2267 0.1511 0.3143 0.1320 1.0000 Uiso . . . . . .
H521 H 0.3047 -0.1582 0.3462 0.1250 1.0000 Uiso . . . . . .
H531 H 0.3177 -0.0940 0.3002 0.0932 1.0000 Uiso . . . . . .
H471 H 0.3040 0.0387 0.2426 0.1171 1.0000 Uiso . . . . . .
H472 H 0.2695 0.1324 0.2234 0.1171 1.0000 Uiso . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.044(2) 0.103(5) 0.054(3) -0.004(3) 0.027(2) 0.003(3)
S2 0.080(3) 0.122(6) 0.034(2) 0.006(3) 0.012(2) 0.026(4)
S3 0.031(2) 0.121(5) 0.061(3) -0.033(3) 0.021(2) -0.009(3)
S4 0.093(4) 0.143(7) 0.101(4) 0.006(4) 0.063(4) 0.009(4)
N1 0.031(2) 0.066(3) 0.035(2) 0.000(3) 0.015(2) 0.002(2)
N2 0.034(2) 0.067(3) 0.034(2) 0.000(3) 0.0170(19) 0.002(2)
N3 0.031(2) 0.066(3) 0.036(2) 0.000(2) 0.0170(19) 0.001(2)
N4 0.029(2) 0.067(3) 0.034(2) -0.001(3) 0.0156(19) 0.001(2)
C1 0.031(2) 0.066(3) 0.035(2) 0.000(2) 0.0156(19) 0.002(2)
C2 0.031(2) 0.066(3) 0.035(2) 0.000(3) 0.015(2) 0.002(2)
C3 0.031(2) 0.066(3) 0.035(2) 0.000(3) 0.015(2) 0.002(2)
C4 0.031(2) 0.066(3) 0.035(2) 0.000(2) 0.0143(19) 0.002(2)
C5 0.030(2) 0.067(3) 0.035(2) 0.000(2) 0.0143(19) 0.001(2)
C6 0.030(2) 0.067(3) 0.035(2) -0.001(2) 0.0152(18) 0.001(2)
C7 0.029(2) 0.067(3) 0.035(2) -0.001(3) 0.015(2) 0.001(2)
C8 0.029(2) 0.067(3) 0.034(2) -0.001(3) 0.016(2) 0.000(3)
C9 0.030(2) 0.067(3) 0.035(2) -0.001(2) 0.0164(18) 0.001(2)
C10 0.030(2) 0.067(3) 0.035(2) 0.000(2) 0.0166(19) 0.001(2)
C11 0.030(2) 0.067(3) 0.036(2) 0.000(2) 0.0170(18) 0.001(2)
C12 0.030(2) 0.066(3) 0.036(2) 0.001(3) 0.017(2) 0.001(3)
C13 0.031(2) 0.066(3) 0.035(2) 0.001(3) 0.016(2) 0.000(3)
C14 0.031(2) 0.066(3) 0.035(2) 0.001(2) 0.0170(18) 0.000(2)
C15 0.033(2) 0.066(3) 0.035(2) 0.001(2) 0.0169(18) 0.001(2)
C16 0.033(2) 0.066(3) 0.034(2) 0.001(2) 0.0171(18) 0.001(2)
C17 0.034(2) 0.067(3) 0.034(2) 0.000(3) 0.017(2) 0.002(3)
C18 0.034(2) 0.067(3) 0.034(2) 0.000(3) 0.018(2) 0.002(3)
C19 0.033(2) 0.067(3) 0.034(2) 0.000(2) 0.0172(18) 0.002(2)
C20 0.033(2) 0.066(3) 0.035(2) 0.000(2) 0.0164(19) 0.002(2)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.0508(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 . C24 . 1.775(11) yes
S1 . O1 . 1.439(10) yes
S1 . O2 . 1.430(10) yes
S1 . O3 . 1.375(10) yes
S2 . C30 . 1.808(16) yes
S2 . O4 . 1.441(14) yes
S2 . O5 . 1.449(17) yes
S2 . O6 . 1.464(14) yes
S3 . C36 . 1.834(11) yes
S3 . O7 . 1.463(11) yes
S3 . O8 . 1.367(10) yes
S3 . O9 . 1.438(10) yes
S4 . N6 . 1.48(2) yes
S4 . O11 . 1.564(18) yes
S4 . O12 . 1.49(2) yes
S4 . C51 . 1.78(2) yes
N1 . C1 . 1.314(17) yes
N1 . C4 . 1.376(17) yes
N2 . C16 . 1.402(17) yes
N2 . C19 . 1.398(16) yes
N2 . H1 . 0.828 no
N3 . C11 . 1.369(16) yes
N3 . C14 . 1.401(17) yes
N4 . C6 . 1.373(17) yes
N4 . C9 . 1.384(17) yes
N4 . H2 . 0.892 no
C1 . C2 . 1.43(2) yes
C1 . C20 . 1.408(19) yes
C2 . C3 . 1.328(19) yes
C2 . H532 . 0.936 no
C3 . C4 . 1.46(2) yes
C3 . H31 . 0.937 no
C4 . C5 . 1.366(19) yes
C5 . C6 . 1.366(19) yes
C5 . C39 . 1.526(19) yes
C6 . C7 . 1.50(2) yes
C7 . C8 . 1.366(19) yes
C7 . H71 . 0.923 no
C8 . C9 . 1.422(19) yes
C8 . H81 . 0.928 no
C9 . C10 . 1.419(19) yes
C10 . C11 . 1.439(19) yes
C10 . C33 . 1.470(16) yes
C11 . C12 . 1.48(2) yes
C12 . C13 . 1.278(18) yes
C12 . H121 . 0.928 no
C13 . C14 . 1.433(18) yes
C13 . H131 . 0.930 no
C14 . C15 . 1.395(18) yes
C15 . C16 . 1.417(19) yes
C15 . C27 . 1.482(19) yes
C16 . C17 . 1.433(19) yes
C17 . C18 . 1.315(18) yes
C17 . H171 . 0.926 no
C18 . C19 . 1.422(19) yes
C18 . H181 . 0.931 no
C19 . C20 . 1.43(2) yes
C20 . C21 . 1.532(17) yes
N5 . C45 . 1.25(2) yes
N5 . C46 . 1.54(2) yes
N5 . H3 . 0.884 no
N6 . H4 . 1.025 no
N6 . H5 . 0.813 no
C45 . O10 . 1.235(19) yes
C45 . C42 . 1.60(2) yes
C21 . C22 . 1.408(15) yes
C21 . C26 . 1.392(15) yes
C22 . C23 . 1.468(14) yes
C22 . H221 . 0.936 no
C23 . C24 . 1.383(16) yes
C23 . H231 . 0.936 no
C24 . C25 . 1.389(15) yes
C25 . C26 . 1.278(13) yes
C25 . H251 . 0.931 no
C26 . H261 . 0.932 no
C27 . C28 . 1.39(2) yes
C27 . C32 . 1.41(2) yes
C28 . C29 . 1.39(2) yes
C28 . H281 . 0.932 no
C29 . C30 . 1.36(2) yes
C29 . H291 . 0.941 no
C30 . C31 . 1.41(2) yes
C31 . C32 . 1.47(2) yes
C31 . H311 . 0.932 no
C32 . H321 . 0.930 no
C33 . C34 . 1.369(16) yes
C33 . C38 . 1.417(14) yes
C34 . C35 . 1.368(14) yes
C34 . H341 . 0.933 no
C35 . C36 . 1.284(15) yes
C35 . H351 . 0.930 no
C36 . C37 . 1.444(16) yes
C37 . C38 . 1.331(13) yes
C37 . H371 . 0.930 no
C38 . H381 . 0.932 no
C39 . C40 . 1.389(19) yes
C39 . C44 . 1.401(19) yes
C40 . C41 . 1.37(2) yes
C40 . H401 . 0.932 no
C41 . C42 . 1.46(2) yes
C41 . H411 . 0.929 no
C42 . C43 . 1.336(19) yes
C43 . C44 . 1.38(2) yes
C43 . H431 . 0.932 no
C44 . H441 . 0.935 no
C46 . C47 . 1.48(2) yes
C46 . H461 . 0.970 no
C46 . H462 . 0.970 no
C47 . C48 . 1.43(3) yes
C47 . H471 . 0.976 no
C47 . H472 . 0.973 no
C48 . C49 . 1.42(3) yes
C48 . C53 . 1.47(3) yes
C49 . C50 . 1.48(3) yes
C49 . H491 . 0.939 no
C50 . C51 . 1.34(3) yes
C50 . H501 . 0.927 no
C51 . C52 . 1.47(3) yes
C52 . C53 . 1.30(2) yes
C52 . H521 . 0.935 no
C53 . H531 . 0.928 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
C24 . S1 . O1 . 105.4(5) yes
C24 . S1 . O2 . 108.9(6) yes
O1 . S1 . O2 . 108.4(6) yes
C24 . S1 . O3 . 105.3(6) yes
O1 . S1 . O3 . 113.3(7) yes
O2 . S1 . O3 . 115.0(6) yes
C30 . S2 . O4 . 105.7(8) yes
C30 . S2 . O5 . 105.8(9) yes
O4 . S2 . O5 . 117.8(9) yes
C30 . S2 . O6 . 104.9(8) yes
O4 . S2 . O6 . 111.9(9) yes
O5 . S2 . O6 . 109.7(9) yes
C36 . S3 . O7 . 105.4(6) yes
C36 . S3 . O8 . 104.2(6) yes
O7 . S3 . O8 . 113.2(6) yes
C36 . S3 . O9 . 103.7(5) yes
O7 . S3 . O9 . 113.3(6) yes
O8 . S3 . O9 . 115.5(6) yes
N6 . S4 . O11 . 112.4(12) yes
N6 . S4 . O12 . 108.2(11) yes
O11 . S4 . O12 . 118.3(10) yes
N6 . S4 . C51 . 100.9(10) yes
O11 . S4 . C51 . 107.6(10) yes
O12 . S4 . C51 . 108.0(10) yes
C1 . N1 . C4 . 108.1(11) yes
C16 . N2 . C19 . 108.3(10) yes
C16 . N2 . H1 . 125.0 no
C19 . N2 . H1 . 126.5 no
C11 . N3 . C14 . 105.9(10) yes
C6 . N4 . C9 . 109.6(11) yes
C6 . N4 . H2 . 126.2 no
C9 . N4 . H2 . 124.1 no
N1 . C1 . C2 . 109.6(12) yes
N1 . C1 . C20 . 126.5(13) yes
C2 . C1 . C20 . 123.8(13) yes
C1 . C2 . C3 . 108.6(12) yes
C1 . C2 . H532 . 125.3 no
C3 . C2 . H532 . 126.1 no
C2 . C3 . C4 . 105.7(12) yes
C2 . C3 . H31 . 127.0 no
C4 . C3 . H31 . 127.2 no
C3 . C4 . N1 . 108.0(12) yes
C3 . C4 . C5 . 125.4(13) yes
N1 . C4 . C5 . 126.6(13) yes
C4 . C5 . C6 . 126.1(13) yes
C4 . C5 . C39 . 117.2(12) yes
C6 . C5 . C39 . 116.1(13) yes
N4 . C6 . C5 . 125.8(13) yes
N4 . C6 . C7 . 106.1(11) yes
C5 . C6 . C7 . 128.0(13) yes
C6 . C7 . C8 . 107.1(12) yes
C6 . C7 . H71 . 126.5 no
C8 . C7 . H71 . 126.4 no
C7 . C8 . C9 . 108.1(12) yes
C7 . C8 . H81 . 125.4 no
C9 . C8 . H81 . 126.4 no
C8 . C9 . N4 . 108.9(11) yes
C8 . C9 . C10 . 125.5(12) yes
N4 . C9 . C10 . 125.3(13) yes
C9 . C10 . C11 . 124.5(12) yes
C9 . C10 . C33 . 122.0(12) yes
C11 . C10 . C33 . 113.4(11) yes
C10 . C11 . N3 . 125.2(11) yes
C10 . C11 . C12 . 126.2(11) yes
N3 . C11 . C12 . 108.6(11) yes
C11 . C12 . C13 . 106.6(11) yes
C11 . C12 . H121 . 126.5 no
C13 . C12 . H121 . 126.9 no
C12 . C13 . C14 . 110.7(13) yes
C12 . C13 . H131 . 124.8 no
C14 . C13 . H131 . 124.5 no
C13 . C14 . N3 . 107.8(11) yes
C13 . C14 . C15 . 126.1(12) yes
N3 . C14 . C15 . 125.9(12) yes
C14 . C15 . C16 . 124.5(12) yes
C14 . C15 . C27 . 119.1(12) yes
C16 . C15 . C27 . 115.8(11) yes
C15 . C16 . N2 . 124.7(11) yes
C15 . C16 . C17 . 128.8(12) yes
N2 . C16 . C17 . 105.6(11) yes
C16 . C17 . C18 . 110.3(12) yes
C16 . C17 . H171 . 125.2 no
C18 . C17 . H171 . 124.5 no
C17 . C18 . C19 . 108.8(12) yes
C17 . C18 . H181 . 126.1 no
C19 . C18 . H181 . 125.1 no
C18 . C19 . N2 . 107.0(11) yes
C18 . C19 . C20 . 129.2(12) yes
N2 . C19 . C20 . 123.3(11) yes
C19 . C20 . C1 . 125.7(12) yes
C19 . C20 . C21 . 114.5(11) yes
C1 . C20 . C21 . 119.6(12) yes
C45 . N5 . C46 . 126.1(15) yes
C45 . N5 . H3 . 116.3 no
C46 . N5 . H3 . 117.4 no
S4 . N6 . H4 . 103.5 no
S4 . N6 . H5 . 107.4 no
H4 . N6 . H5 . 109.8 no
N5 . C45 . O10 . 129.6(17) yes
N5 . C45 . C42 . 116.9(15) yes
O10 . C45 . C42 . 112.8(15) yes
C20 . C21 . C22 . 113.6(11) yes
C20 . C21 . C26 . 124.6(10) yes
C22 . C21 . C26 . 121.5(10) yes
C21 . C22 . C23 . 116.6(10) yes
C21 . C22 . H221 . 121.4 no
C23 . C22 . H221 . 122.1 no
C22 . C23 . C24 . 118.1(10) yes
C22 . C23 . H231 . 120.6 no
C24 . C23 . H231 . 121.2 no
S1 . C24 . C23 . 115.7(8) yes
S1 . C24 . C25 . 124.3(9) yes
C23 . C24 . C25 . 119.3(10) yes
C24 . C25 . C26 . 124.4(11) yes
C24 . C25 . H251 . 118.0 no
C26 . C25 . H251 . 117.6 no
C21 . C26 . C25 . 119.5(10) yes
C21 . C26 . H261 . 120.9 no
C25 . C26 . H261 . 119.6 no
C15 . C27 . C28 . 123.8(13) yes
C15 . C27 . C32 . 115.1(14) yes
C28 . C27 . C32 . 120.9(13) yes
C27 . C28 . C29 . 119.5(15) yes
C27 . C28 . H281 . 119.9 no
C29 . C28 . H281 . 120.6 no
C28 . C29 . C30 . 120.9(16) yes
C28 . C29 . H291 . 119.4 no
C30 . C29 . H291 . 119.8 no
S2 . C30 . C29 . 119.7(13) yes
S2 . C30 . C31 . 116.4(12) yes
C29 . C30 . C31 . 123.7(15) yes
C30 . C31 . C32 . 115.4(14) yes
C30 . C31 . H311 . 122.0 no
C32 . C31 . H311 . 122.6 no
C31 . C32 . C27 . 119.6(15) yes
C31 . C32 . H321 . 120.4 no
C27 . C32 . H321 . 120.0 no
C10 . C33 . C34 . 122.0(11) yes
C10 . C33 . C38 . 120.6(11) yes
C34 . C33 . C38 . 117.0(10) yes
C33 . C34 . C35 . 121.7(11) yes
C33 . C34 . H341 . 119.9 no
C35 . C34 . H341 . 118.4 no
C34 . C35 . C36 . 121.7(11) yes
C34 . C35 . H351 . 119.3 no
C36 . C35 . H351 . 119.0 no
S3 . C36 . C35 . 122.3(10) yes
S3 . C36 . C37 . 118.5(8) yes
C35 . C36 . C37 . 119.1(10) yes
C36 . C37 . C38 . 120.0(10) yes
C36 . C37 . H371 . 120.4 no
C38 . C37 . H371 . 119.7 no
C33 . C38 . C37 . 120.1(10) yes
C33 . C38 . H381 . 119.9 no
C37 . C38 . H381 . 120.0 no
C5 . C39 . C40 . 119.5(12) yes
C5 . C39 . C44 . 120.8(12) yes
C40 . C39 . C44 . 119.3(13) yes
C39 . C40 . C41 . 122.1(13) yes
C39 . C40 . H401 . 119.4 no
C41 . C40 . H401 . 118.5 no
C40 . C41 . C42 . 117.6(14) yes
C40 . C41 . H411 . 121.0 no
C42 . C41 . H411 . 121.4 no
C45 . C42 . C41 . 115.7(13) yes
C45 . C42 . C43 . 125.5(14) yes
C41 . C42 . C43 . 118.8(13) yes
C42 . C43 . C44 . 123.4(14) yes
C42 . C43 . H431 . 118.1 no
C44 . C43 . H431 . 118.5 no
C39 . C44 . C43 . 118.7(13) yes
C39 . C44 . H441 . 120.3 no
C43 . C44 . H441 . 120.9 no
N5 . C46 . C47 . 110.7(16) yes
N5 . C46 . H461 . 108.6 no
C47 . C46 . H461 . 107.9 no
N5 . C46 . H462 . 109.8 no
C47 . C46 . H462 . 109.6 no
H461 . C46 . H462 . 110.2 no
C46 . C47 . C48 . 114.9(13) yes
C46 . C47 . H471 . 109.3 no
C48 . C47 . H471 . 107.9 no
C46 . C47 . H472 . 108.0 no
C48 . C47 . H472 . 107.8 no
H471 . C47 . H472 . 108.8 no
C47 . C48 . C49 . 123.1(20) yes
C47 . C48 . C53 . 122.0(19) yes
C49 . C48 . C53 . 114.9(18) yes
C48 . C49 . C50 . 122.4(20) yes
C48 . C49 . H491 . 118.4 no
C50 . C49 . H491 . 119.2 no
C49 . C50 . C51 . 119(2) yes
C49 . C50 . H501 . 120.0 no
C51 . C50 . H501 . 121.2 no
S4 . C51 . C50 . 120.6(17) yes
S4 . C51 . C52 . 120.4(17) yes
C50 . C51 . C52 . 119(2) yes
C51 . C52 . C53 . 123.6(20) yes
C51 . C52 . H521 . 118.4 no
C53 . C52 . H521 . 117.9 no
C48 . C53 . C52 . 121.7(18) yes
C48 . C53 . H531 . 118.9 no
C52 . C53 . H531 . 119.4 no
# SQUEEZE RESULTS (APPEND TO CIF)
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
1 0.500 -0.039 0.250 1101.8 351.4
2 1.000 0.461 0.250 1101.8 351.3
3 0.500 1.037 0.750 1102.1 350.9
4 1.000 0.537 0.750 1102.1 350.9
_platon_squeeze_details          
;  
There is a large number of disordered water molecules in the asymmetric unit and possibly one THF molecule (disordered over more than two sites). 
Therefore, treatment of rezidual electron density using the SQUEEZE
procedure (P. v.d. Sluis & A. L. Spek, Acta Crystallogr. 1990, A46, 194.),
implemented in PLATON (PLATON, A Multipurpose Crystallographic Tool,
Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998.) was used.
;
#end
