data_global 
_audit_creation_date        "2018-06-23"
_audit_creation_method CRYSTALS_ver_14.61

_oxford_structure_analysis_title  'tw1704'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
 
# Check this file using the IUCr facility at: 
# http://checkcif.iucr.org/ 
 
# The content below is held in the file 'script/refcif.dat'. This is a text 
# file which you may edit to reflect local conditions. 
# Items which need looking at are represented by a '?'. 
# Items for which there are choices are prefixed with 'choose from'. 
 
_publ_contact_letter 
; 
 Please consider this CIF submission for 
 publication as a Short Format Paper in BJOC. 
; 
_publ_contact_author_name         'Victor Nemykin' 
_publ_contact_author_address 
; 
 Department of Chemistry, 
 University of Manitoba, 
 Winnipeg, MB R3T 2N2, Canada.  
; 
 
_publ_contact_author_phone        '+1 204 4749265' 
_publ_contact_author_fax          '+1 204 4749265' 
_publ_contact_author_email        'Victor.Nemykin@umanitoba.ca' 
_publ_requested_journal           'BJOC' 
_publ_requested_category          EO # choose from: FI FM FO CI CM CO AD 
_publ_requested_coeditor_name     'Prof ' 
 
_publ_section_title 
# Title of paper - generally just the systematic or trivial name 
; ? 
; 
 
# The loop structure below should contain the names and addresses of all 
# authors, in the required order of publication. Repeat as necessary. 
loop_ 
 _publ_author_name 
 _publ_author_address 
 _publ_author_footnote 
 'Nemykin, Victor N.' # Author 1 
; 
   Department of Chemistry, 
 University of Manitoba, 
 Winnipeg, MB R3T 2N2, Canada. # Address for author 1 
; 
; 
 ? # Footnote for author 1 
; 
 'Zhdankin, V. V.' # Author 2 
; 
  Department of Chemistry & Biochemistry
University of Minnesota Duluth
Duluth, MN 55812, USA # Address 2  # Address 2 
; 
; 
 ? # Footnote 2 
; 
 
 
_publ_section_abstract 
# Text of the abstract 
# (a) The Abstract must be self-contained and comprehensible 
# without the rest of the paper. This means no references 
# to atom names or to compound numbers; compounds must be 
# identified as the title compound, or by name or by some other 
# means such as derivatives of each other (e.g. "the 
# corresponding ketone"). 
# (b) The chemical formula of "the title compound" must be given. 
# (c) Any crystallographic molecular symmetry should be 
# mentioned, and also the presence of more than one molecule 
# in the asymmetric unit (i.e. anything other than Z'=1). 
; 
? 
; 
 
_publ_section_related_literature  # Not in version 2.3.1 
############################################################### 
# Essential references (e.g. to the origin of the material studied, related 
# structural studies, and to information supporting the reported structure) 
# should be cited in this section, with appropriate very brief explanatory 
# text, for example `The synthesis of the complex is described by Jones 
# (2001). The anhydrous complex has essentially the same coordination 
# geometry (Smith, 2003).' In addition, all references included in the 
# supplementary materials, but not elsewhere in the published article, 
# should be given here. The simple text `For related literature, see:...' 
# may be used, but further details should be provided in the Comment 
# section, which forms part of the supplementary material. 
############################################################### 
; 
? 
; 
 
_publ_section_comment 
# Text of the paper 
# Note that atoms are referenced as N2, not N(2) or N~2~ 
# If text containing () occur within (), the outer ones should be [] 
# Figures should be referenced as Fig. 
; 
? 
; 
_publ_section_acknowledgements    # Acknowledgments 
; 
? 
; 
_publ_section_figure_captions 
# Captions to figures - Start each caption on a new line after a blank line 
; 
Fig. 1. 
The title compound with displacement ellipsoids drawn at the 50% 
probability level. H atoms are shown as spheres of 
arbitary radius. 
 
; 
 
 
_publ_section_exptl_refinement 
# Some potentially useful phrases are donated by Bill Clegg: 
; 
In the absence of significant anomalous scattering, Friedel pairs were 
merged. 
 
The absolute configuration was arbitrarily assigned. 
 
The relatively large ratio of minimum to maximum corrections applied 
in the multiscan process (1:nnn) reflect changes in the illuminated 
volume of the crystal. 
 
Changes in illuminated volume were kept to a minimum, and were 
taken into account (Görbitz, 1999) by the multi-scan inter-frame 
scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). 
 
 
Görbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. 
 
 
 
 
The H atoms were all located in a difference map, but those 
attached to carbon atoms were repositioned geometrically. 
The H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98, 
N---H in the range 0.86--0.89 
N---H to 0.86 
O---H = 0.82 
Å) 
and 
Uiso(H) (in the range 1.2-1.5 times Ueq of the parent atom), 
after which the positions were refined with riding constraints 
(Cooper et al, 2010). 
 
Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 
43, 1100-1107. 
 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
# Hand-made tables can be put in the cif. The number of columns 
# is set in the loop header. 
# The contants of each column can either be a piece of text 
# without any spaces (eg a number) or other text enclosed in " " 
# Remove the leading # in the following example 
 
#geom_extra_table_head_A 
#; 
#Table 2. 
#Molecular parameters deviating most from MOGUL averages 
#; 
# 
#loop_ 
#_geom_extra_tableA_col_1 
#_geom_extra_tableA_col_2 
#_geom_extra_tableA_col_3 
#_geom_extra_tableA_col_4 
# 
#Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" 
#N5-C6-C4 129 124 "7 (\%)" 
#C3-O10-C2 105 109 "2 (\%)" 
#C6-O7 1.25 1.22 ".02 (\%A)" 
# 
 
data_1 
 
_exptl_special_details 
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
; 
_refine_special_details 
; 
? 
; 
#--------------------------------------------------------------- 
# _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                    12.1580(5)
_cell_length_b                    14.0099(6)
_cell_length_c                    14.3011(5)
_cell_angle_alpha                 61.355(4)
_cell_angle_beta                  65.376(4)
_cell_angle_gamma                 65.479(4)
_cell_volume                      1871.29(7)
 
_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'
 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'
 K       0.2009   0.2494   8.2186  12.7949   7.4398   0.7748   1.0519 213.1870
   0.8659  41.6841   1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 I      -0.4742   1.8119  20.1472   4.3470  18.9949   0.3814   7.5138  27.7660
   2.2735  66.8776   4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C24 H16 I4 K3 O21 S4 
# Dc =      2.47 Fooo =   1328.00 Mu =     39.72 M =   1393.55
# Found Formula = C24 H19 I4 K3 O21 S4 
# Dc =      2.48 FOOO =   1328.00 Mu =     39.72 M =   1396.58

_chemical_formula_sum             'C24 H19 I4 K3 O21 S4'
_chemical_formula_moiety          'C24 H19 I4 K3 O21 S4'
_chemical_compound_source                ?
_chemical_formula_weight           1396.58
 
 
_cell_measurement_reflns_used        12160
_cell_measurement_theta_min              3
_cell_measurement_theta_max             29
_cell_measurement_temperature          296
 
_exptl_crystal_description        'needle' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_size_min           0.086 
_exptl_crystal_size_mid           0.104 
_exptl_crystal_size_max           0.196 
 
_exptl_crystal_density_diffrn     2.478 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1328 
_exptl_absorpt_coefficient_mu     3.972 
 
# Sheldrick geometric approximatio 0.66 0.71 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' 
_exptl_absorpt_correction_T_min   0.53 
_exptl_absorpt_correction_T_max   0.71 
_diffrn_measurement_device_type   'Unknown' 
_diffrn_measurement_device        'Serial' 
_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        'USER DEFINED DATA COLLECTION' 
_computing_cell_refinement        'USER DEFINED CELL REFINEMENT' 
_computing_data_reduction         'USER DEFINED DATA REDUCTION' 
_computing_structure_solution     'SHELXS 86 (Sheldrick, 1986)' 
_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   2 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          12160 
_diffrn_standards_decay_%         0.00 
 
_diffrn_ambient_temperature        296
_diffrn_reflns_number             31392 
_reflns_number_total              9038 
_diffrn_reflns_av_R_equivalents   0.065 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9038 
# Theoretical number of reflections is about 21109 
 
 
_diffrn_reflns_theta_min          2.898 
_diffrn_reflns_theta_max          29.631 
_diffrn_measured_fraction_theta_max 0.856 
 
_diffrn_reflns_theta_full         25.186 
_diffrn_measured_fraction_theta_full 0.945 
 
 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        19 
_reflns_limit_h_min               -14 
_reflns_limit_h_max               16 
_reflns_limit_k_min               -16 
_reflns_limit_k_max               19 
_reflns_limit_l_min               0 
_reflns_limit_l_max               19 
 
_oxford_diffrn_Wilson_B_factor    0.00 
_oxford_diffrn_Wilson_scale       0.00 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -1.97 
_refine_diff_density_max          2.14 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-3.0\s(I)
_refine_ls_number_reflns          9020 
_refine_ls_number_restraints      3 
_refine_ls_number_parameters      514 
_oxford_refine_ls_R_factor_ref    0.0581 
_refine_ls_wR_factor_ref          0.0698 
_refine_ls_goodness_of_fit_ref    0.8944 
_refine_ls_shift/su_max           0.0024182 
_refine_ls_shift/su_mean          0.0000576 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         9020 
_refine_ls_R_factor_all           0.0581 
_refine_ls_wR_factor_all          0.0698 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 6397 
_refine_ls_R_factor_gt            0.0304 
_refine_ls_wR_factor_gt           0.0636 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     mixed          #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 0.00P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined data collection reference 
 
User defined data reduction 
 
User defined cell refinement 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, 
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. 
New York: Academic Press. 
 
Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# 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
I1 I 0.38171(2) 0.98958(2) 0.256299(19) 0.0181 1.0000 Uani . . . . . . 
O1 O 0.3999(3) 0.8427(2) 0.3387(2) 0.0309 1.0000 Uani . . . . . . 
O2 O 0.3377(3) 1.0041(2) 0.1425(2) 0.0292 1.0000 Uani . . . . . . 
I2 I 0.37590(2) 0.87543(2) 0.054784(19) 0.0207 1.0000 Uani . . . . . . 
O6 O 0.3688(3) 0.8147(2) -0.0338(2) 0.0257 1.0000 Uani D . . . . . 
O7 O 0.3422(3) 0.7638(2) 0.1883(2) 0.0266 1.0000 Uani . . . . . . 
C7 C 0.1871(4) 0.9725(3) 0.0658(3) 0.0189 1.0000 Uani . . . . . . 
C8 C 0.1542(4) 1.0709(3) -0.0209(3) 0.0192 1.0000 Uani . . . . . . 
S2 S 0.26796(10) 1.12074(9) -0.14667(8) 0.0227 1.0000 Uani . . . . . . 
O9 O 0.2725(4) 1.0791(3) -0.2227(2) 0.0464 1.0000 Uani . . . . . . 
O10 O 0.2334(3) 1.2409(3) -0.1825(3) 0.0423 1.0000 Uani . . . . . . 
O8 O 0.3849(3) 1.0667(3) -0.1123(2) 0.0403 1.0000 Uani . . . . . . 
C9 C 0.0275(4) 1.1293(4) -0.0093(4) 0.0270 1.0000 Uani . . . . . . 
C10 C -0.0613(4) 1.0890(4) 0.0872(4) 0.0310 1.0000 Uani . . . . . . 
C11 C -0.0252(4) 0.9910(4) 0.1724(4) 0.0310 1.0000 Uani . . . . . . 
C12 C 0.0988(4) 0.9319(4) 0.1630(3) 0.0248 1.0000 Uani . . . . . . 
C1 C 0.1949(4) 1.0605(3) 0.3377(3) 0.0200 1.0000 Uani . . . . . . 
C2 C 0.1687(4) 1.0691(3) 0.4378(3) 0.0205 1.0000 Uani . . . . . . 
S1 S 0.28724(10) 1.01664(9) 0.50454(8) 0.0218 1.0000 Uani . . . . . . 
O5 O 0.2684(3) 1.0988(3) 0.5473(2) 0.0362 1.0000 Uani . . . . . . 
O4 O 0.2735(3) 0.9086(3) 0.5912(2) 0.0338 1.0000 Uani . . . . . . 
O3 O 0.4048(3) 1.0058(3) 0.4162(2) 0.0285 1.0000 Uani . . . . . . 
C3 C 0.0470(4) 1.1198(4) 0.4858(3) 0.0288 1.0000 Uani . . . . . . 
C4 C -0.0466(4) 1.1619(4) 0.4332(4) 0.0326 1.0000 Uani . . . . . . 
C5 C -0.0182(4) 1.1525(4) 0.3335(4) 0.0321 1.0000 Uani . . . . . . 
C6 C 0.1029(4) 1.1026(4) 0.2842(3) 0.0270 1.0000 Uani . . . . . . 
I3 I 0.32752(3) 0.57090(2) 0.21303(2) 0.0224 1.0000 Uani . . . . . . 
O11 O 0.3101(3) 0.4388(2) 0.2371(2) 0.0319 1.0000 Uani . . . . . . 
O12 O 0.2485(3) 0.6616(3) 0.0988(2) 0.0383 1.0000 Uani . . . . . . 
C13 C 0.1646(4) 0.6076(3) 0.3388(3) 0.0199 1.0000 Uani . . . . . . 
C14 C 0.1727(4) 0.5802(3) 0.4423(3) 0.0214 1.0000 Uani . . . . . . 
S3 S 0.31863(10) 0.52480(9) 0.47412(8) 0.0262 1.0000 Uani . . . . . . 
O15 O 0.3363(4) 0.6093(4) 0.4908(4) 0.0679 1.0000 Uani . . . . . . 
O14 O 0.3169(3) 0.4202(3) 0.5661(3) 0.0555 1.0000 Uani . . . . . . 
O13 O 0.4096(3) 0.5076(3) 0.3728(2) 0.0393 1.0000 Uani . . . . . . 
C15 C 0.0614(4) 0.5988(4) 0.5244(4) 0.0351 1.0000 Uani . . . . . . 
C16 C -0.0525(5) 0.6438(4) 0.5005(4) 0.0413 1.0000 Uani . . . . . . 
C17 C -0.0576(5) 0.6710(4) 0.3949(4) 0.0428 1.0000 Uani . . . . . . 
C18 C 0.0514(4) 0.6532(4) 0.3134(4) 0.0322 1.0000 Uani . . . . . . 
I4 I 0.61044(2) 0.66293(2) -0.07035(2) 0.0214 1.0000 Uani . . . . . . 
O16 O 0.5935(3) 0.7104(3) 0.0339(2) 0.0351 1.0000 Uani . . . . . . 
O17 O 0.6529(3) 0.7769(2) -0.1970(2) 0.0362 1.0000 Uani . . . . . . 
C19 C 0.7930(4) 0.5518(3) -0.0673(3) 0.0209 1.0000 Uani . . . . . . 
C20 C 0.8123(4) 0.4510(3) 0.0203(3) 0.0217 1.0000 Uani . . . . . . 
S4 S 0.68526(11) 0.40789(9) 0.13611(8) 0.0277 1.0000 Uani . . . . . . 
O19 O 0.6818(4) 0.4381(3) 0.2210(3) 0.0502 1.0000 Uani . . . . . . 
O20 O 0.7086(3) 0.2885(3) 0.1677(3) 0.0487 1.0000 Uani . . . . . . 
O18 O 0.5759(3) 0.4746(3) 0.0921(2) 0.0360 1.0000 Uani . . . . . . 
C21 C 0.9336(4) 0.3822(4) 0.0183(4) 0.0319 1.0000 Uani . . . . . . 
C22 C 1.0324(4) 0.4165(4) -0.0709(4) 0.0356 1.0000 Uani . . . . . . 
C23 C 1.0120(4) 0.5178(4) -0.1580(4) 0.0373 1.0000 Uani . . . . . . 
C24 C 0.8912(4) 0.5865(4) -0.1572(3) 0.0311 1.0000 Uani . . . . . . 
K2 K 0.58194(10) 0.28722(8) 0.44652(8) 0.0344 1.0000 Uani . . . . . . 
K3 K 0.42233(10) 0.34509(9) 0.73977(8) 0.0357 1.0000 Uani . . . . . . 
K1 K 0.39793(10) 0.88909(9) -0.27013(7) 0.0305 1.0000 Uani . . . . . . 
O21 O 0.4296(3) 0.2428(3) 0.3917(3) 0.0425 1.0000 Uani D . . . . . 
H161 H 0.1294 0.8643 0.2222 0.0302 1.0000 Uiso R . . . . . 
H3 H 0.377(4) 0.210(4) 0.439(3) 0.0498 1.0000 Uiso D . . . . . 
H2 H 0.388(4) 0.293(3) 0.350(4) 0.0498 1.0000 Uiso D . . . . . 
H1 H 0.310(3) 0.788(4) 0.013(3) 0.0313 1.0000 Uiso D . . . . . 
H242 H 0.8761 0.6545 -0.2161 0.0385 1.0000 Uiso R . . . . . 
H232 H 1.0794 0.5401 -0.2171 0.0445 1.0000 Uiso R . . . . . 
H221 H 1.1138 0.3702 -0.0720 0.0426 1.0000 Uiso R . . . . . 
H211 H 0.9486 0.3137 0.0766 0.0385 1.0000 Uiso R . . . . . 
H152 H 0.0642 0.5803 0.5953 0.0428 1.0000 Uiso R . . . . . 
H162 H -0.1264 0.6568 0.5550 0.0498 1.0000 Uiso R . . . . . 
H171 H -0.1348 0.7010 0.3794 0.0510 1.0000 Uiso R . . . . . 
H181 H 0.0488 0.6716 0.2425 0.0386 1.0000 Uiso R . . . . . 
H31 H 0.0277 1.1260 0.5531 0.0345 1.0000 Uiso R . . . . . 
H41 H -0.1283 1.1963 0.4653 0.0394 1.0000 Uiso R . . . . . 
H51 H -0.0812 1.1799 0.2991 0.0385 1.0000 Uiso R . . . . . 
H61 H 0.1224 1.0974 0.2163 0.0327 1.0000 Uiso R . . . . . 
H111 H -0.0857 0.9647 0.2371 0.0375 1.0000 Uiso R . . . . . 
H101 H -0.1459 1.1280 0.0949 0.0373 1.0000 Uiso R . . . . . 
H91 H 0.0028 1.1954 -0.0665 0.0323 1.0000 Uiso R . . . . . 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 1.611(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
I1 . O1 . 1.786(3)    yes
I1 . O2 . 1.814(3)    yes
I1 . C1 . 2.129(4)    yes
I1 . O3 . 2.539(3)    yes
O2 . I2 . 2.456(3)    yes
I2 . O6 . 1.876(3)    yes
I2 . O7 . 1.810(3)    yes
I2 . C7 . 2.111(4)    yes
I2 . O8 . 2.606(3)    yes
I2 . O16 . 2.713(3)    yes
O6 . H1 . 0.826(18)    no
O7 . I3 . 2.626(3)    yes
C7 . C8 . 1.384(5)    yes
C7 . C12 . 1.383(5)    yes
C8 . S2 . 1.777(4)    yes
C8 . C9 . 1.393(6)    yes
S2 . O9 . 1.434(3)    yes
S2 . O10 . 1.427(3)    yes
S2 . O8 . 1.473(3)    yes
C9 . C10 . 1.381(6)    yes
C9 . H91 . 0.930    no
C10 . C11 . 1.380(6)    yes
C10 . H101 . 0.930    no
C11 . C12 . 1.370(6)    yes
C11 . H111 . 0.930    no
C12 . H161 . 0.977    no
C1 . C2 . 1.385(5)    yes
C1 . C6 . 1.385(5)    yes
C2 . S1 . 1.767(4)    yes
C2 . C3 . 1.383(6)    yes
S1 . O5 . 1.447(3)    yes
S1 . O4 . 1.447(3)    yes
S1 . O3 . 1.470(3)    yes
C3 . C4 . 1.393(6)    yes
C3 . H31 . 0.930    no
C4 . C5 . 1.378(6)    yes
C4 . H41 . 0.930    no
C5 . C6 . 1.381(6)    yes
C5 . H51 . 0.930    no
C6 . H61 . 0.930    no
I3 . O11 . 1.800(3)    yes
I3 . O12 . 1.874(3)    yes
I3 . C13 . 2.120(4)    yes
I3 . O13 . 2.495(3)    yes
C13 . C14 . 1.377(5)    yes
C13 . C18 . 1.377(6)    yes
C14 . S3 . 1.774(4)    yes
C14 . C15 . 1.398(6)    yes
S3 . O15 . 1.425(4)    yes
S3 . O14 . 1.425(3)    yes
S3 . O13 . 1.469(3)    yes
C15 . C16 . 1.377(7)    yes
C15 . H152 . 0.930    no
C16 . C17 . 1.391(7)    yes
C16 . H162 . 0.930    no
C17 . C18 . 1.376(7)    yes
C17 . H171 . 0.930    no
C18 . H181 . 0.930    no
I4 . O16 . 1.814(3)    yes
I4 . O17 . 1.797(3)    yes
I4 . C19 . 2.121(4)    yes
I4 . O18 . 2.601(3)    yes
C19 . C20 . 1.375(5)    yes
C19 . C24 . 1.386(6)    yes
C20 . S4 . 1.783(4)    yes
C20 . C21 . 1.384(6)    yes
S4 . O19 . 1.446(4)    yes
S4 . O20 . 1.440(3)    yes
S4 . O18 . 1.463(3)    yes
C21 . C22 . 1.384(6)    yes
C21 . H211 . 0.930    no
C22 . C23 . 1.377(7)    yes
C22 . H221 . 0.930    no
C23 . C24 . 1.380(7)    yes
C23 . H232 . 0.930    no
C24 . H242 . 0.930    no
O21 . H3 . 0.811(19)    no
O21 . H2 . 0.812(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
O1 . I1 . O2 . 101.98(13)    yes
O1 . I1 . C1 . 101.22(14)    yes
O2 . I1 . C1 . 94.03(14)    yes
O1 . I1 . O3 . 86.30(12)    yes
O2 . I1 . O3 . 167.96(12)    yes
C1 . I1 . O3 . 75.62(12)    yes
I1 . O2 . I2 . 134.34(15)    yes
O2 . I2 . O6 . 162.34(11)    yes
O2 . I2 . O7 . 91.46(11)    yes
O6 . I2 . O7 . 99.04(13)    yes
O2 . I2 . C7 . 73.66(12)    yes
O6 . I2 . C7 . 91.15(14)    yes
O7 . I2 . C7 . 95.31(14)    yes
O2 . I2 . O8 . 77.22(10)    yes
O6 . I2 . O8 . 90.26(12)    yes
O7 . I2 . O8 . 166.48(12)    yes
C7 . I2 . O8 . 74.58(12)    yes
O2 . I2 . O16 . 122.25(9)    yes
O6 . I2 . O16 . 73.98(11)    yes
O7 . I2 . O16 . 79.43(11)    yes
C7 . I2 . O16 . 163.04(13)    yes
O8 . I2 . O16 . 112.79(10)    yes
I2 . O6 . H1 . 95(3)    no
I2 . O7 . I3 . 123.30(13)    yes
I2 . C7 . C8 . 121.2(3)    yes
I2 . C7 . C12 . 116.7(3)    yes
C8 . C7 . C12 . 122.1(4)    yes
C7 . C8 . S2 . 121.8(3)    yes
C7 . C8 . C9 . 118.2(4)    yes
S2 . C8 . C9 . 119.9(3)    yes
C8 . S2 . O9 . 107.77(19)    yes
C8 . S2 . O10 . 107.33(19)    yes
O9 . S2 . O10 . 115.0(2)    yes
C8 . S2 . O8 . 102.47(17)    yes
O9 . S2 . O8 . 110.9(2)    yes
O10 . S2 . O8 . 112.5(2)    yes
I2 . O8 . S2 . 111.31(17)    yes
C8 . C9 . C10 . 120.0(4)    yes
C8 . C9 . H91 . 120.0    no
C10 . C9 . H91 . 120.0    no
C9 . C10 . C11 . 120.3(4)    yes
C9 . C10 . H101 . 119.9    no
C11 . C10 . H101 . 119.8    no
C10 . C11 . C12 . 120.9(4)    yes
C10 . C11 . H111 . 119.6    no
C12 . C11 . H111 . 119.5    no
C7 . C12 . C11 . 118.5(4)    yes
C7 . C12 . H161 . 117.5    no
C11 . C12 . H161 . 123.9    no
I1 . C1 . C2 . 120.7(3)    yes
I1 . C1 . C6 . 117.5(3)    yes
C2 . C1 . C6 . 121.7(4)    yes
C1 . C2 . S1 . 121.3(3)    yes
C1 . C2 . C3 . 118.9(4)    yes
S1 . C2 . C3 . 119.9(3)    yes
C2 . S1 . O5 . 107.14(19)    yes
C2 . S1 . O4 . 106.99(18)    yes
O5 . S1 . O4 . 112.60(19)    yes
C2 . S1 . O3 . 103.91(17)    yes
O5 . S1 . O3 . 113.14(19)    yes
O4 . S1 . O3 . 112.35(19)    yes
I1 . O3 . S1 . 113.64(15)    yes
C2 . C3 . C4 . 120.1(4)    yes
C2 . C3 . H31 . 120.0    no
C4 . C3 . H31 . 120.0    no
C3 . C4 . C5 . 120.0(4)    yes
C3 . C4 . H41 . 120.0    no
C5 . C4 . H41 . 120.0    no
C4 . C5 . C6 . 120.7(4)    yes
C4 . C5 . H51 . 119.7    no
C6 . C5 . H51 . 119.6    no
C1 . C6 . C5 . 118.7(4)    yes
C1 . C6 . H61 . 120.6    no
C5 . C6 . H61 . 120.7    no
O7 . I3 . O11 . 176.68(11)    yes
O7 . I3 . O12 . 83.63(11)    yes
O11 . I3 . O12 . 97.15(14)    yes
O7 . I3 . C13 . 80.88(12)    yes
O11 . I3 . C13 . 95.83(14)    yes
O12 . I3 . C13 . 94.47(15)    yes
O7 . I3 . O13 . 79.80(10)    yes
O11 . I3 . O13 . 99.00(13)    yes
O12 . I3 . O13 . 161.98(13)    yes
C13 . I3 . O13 . 76.02(12)    yes
I3 . C13 . C14 . 120.7(3)    yes
I3 . C13 . C18 . 116.7(3)    yes
C14 . C13 . C18 . 122.4(4)    yes
C13 . C14 . S3 . 122.5(3)    yes
C13 . C14 . C15 . 118.3(4)    yes
S3 . C14 . C15 . 119.2(3)    yes
C14 . S3 . O15 . 107.5(2)    yes
C14 . S3 . O14 . 108.1(2)    yes
O15 . S3 . O14 . 115.4(3)    yes
C14 . S3 . O13 . 102.90(18)    yes
O15 . S3 . O13 . 110.7(3)    yes
O14 . S3 . O13 . 111.3(2)    yes
I3 . O13 . S3 . 117.58(17)    yes
C14 . C15 . C16 . 119.9(4)    yes
C14 . C15 . H152 . 120.1    no
C16 . C15 . H152 . 120.0    no
C15 . C16 . C17 . 120.4(4)    yes
C15 . C16 . H162 . 119.8    no
C17 . C16 . H162 . 119.8    no
C16 . C17 . C18 . 120.2(4)    yes
C16 . C17 . H171 . 119.9    no
C18 . C17 . H171 . 119.9    no
C13 . C18 . C17 . 118.7(4)    yes
C13 . C18 . H181 . 120.6    no
C17 . C18 . H181 . 120.7    no
O16 . I4 . O17 . 102.40(15)    yes
O16 . I4 . C19 . 96.05(14)    yes
O17 . I4 . C19 . 98.50(15)    yes
O16 . I4 . O18 . 86.38(13)    yes
O17 . I4 . O18 . 169.47(13)    yes
C19 . I4 . O18 . 74.54(12)    yes
I4 . O16 . I2 . 109.96(13)    yes
I4 . C19 . C20 . 121.4(3)    yes
I4 . C19 . C24 . 116.6(3)    yes
C20 . C19 . C24 . 122.0(4)    yes
C19 . C20 . S4 . 121.5(3)    yes
C19 . C20 . C21 . 118.9(4)    yes
S4 . C20 . C21 . 119.5(3)    yes
C20 . S4 . O19 . 106.6(2)    yes
C20 . S4 . O20 . 107.4(2)    yes
O19 . S4 . O20 . 113.8(2)    yes
C20 . S4 . O18 . 103.13(18)    yes
O19 . S4 . O18 . 112.5(2)    yes
O20 . S4 . O18 . 112.6(2)    yes
I4 . O18 . S4 . 111.84(16)    yes
C20 . C21 . C22 . 119.5(4)    yes
C20 . C21 . H211 . 120.2    no
C22 . C21 . H211 . 120.3    no
C21 . C22 . C23 . 121.1(4)    yes
C21 . C22 . H221 . 119.4    no
C23 . C22 . H221 . 119.6    no
C22 . C23 . C24 . 119.8(4)    yes
C22 . C23 . H232 . 120.1    no
C24 . C23 . H232 . 120.0    no
C19 . C24 . C23 . 118.7(4)    yes
C19 . C24 . H242 . 120.7    no
C23 . C24 . H242 . 120.6    no
H3 . O21 . H2 . 99(5)    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
O21 . H3 . O5 1_545 168(6) 0.811 2.068 2.865(7)    yes
O21 . H2 . O11 . 166(5) 0.812 2.047 2.843(7)    yes
O6 . H1 . O12 . 148(5) 0.826 1.855 2.594(7)    yes
C22 . H221 . O10 1_645 124.57(13) 0.930 2.556 3.177(7)    yes
C10 . H101 . O20 1_465 133.84(13) 0.930 2.584 3.297(7)    yes


