# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_c
_database_code_depnum_ccdc_archive 'CCDC 1470477'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 tris-(4-methylthiazolyl)cyclotriguaiacylene hydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H41 N3 O10 S3'
_chemical_formula_weight         771.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6(3)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'

_cell_length_a                   14.5223(19)
_cell_length_b                   14.5223(19)
_cell_length_c                   10.2703(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1875.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    866
_cell_measurement_theta_min      3.5180
_cell_measurement_theta_max      66.1350

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7225
_exptl_absorpt_correction_T_max  0.9551
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.3095
_diffrn_reflns_number            4447
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.1047
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         73.42
_reflns_number_total             2236
_reflns_number_gt                1394
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1467P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(7)
_refine_ls_number_reflns         2236
_refine_ls_number_parameters     158
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.0886
_refine_ls_wR_factor_ref         0.2598
_refine_ls_wR_factor_gt          0.2260
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.66746(16) -0.50074(17) -0.1047(3) 0.0648(6) Uani 1 1 d . . .
O1 O -0.1694(4) -0.3811(4) 0.0965(5) 0.0497(12) Uani 1 1 d . . .
O2 O -0.3249(4) -0.3416(4) 0.1027(5) 0.0433(11) Uani 1 1 d . . .
O3 O -0.2887(6) -0.4517(6) -0.1528(9) 0.092(3) Uani 1 1 d . . .
O4 O -0.3333 -0.6667 -0.2122(13) 0.092(4) Uani 1 3 d S . .
N1 N -0.4660(6) -0.4150(5) -0.1226(6) 0.0551(16) Uani 1 1 d . . .
C1 C -0.0582(5) -0.1571(5) 0.3321(7) 0.0413(15) Uani 1 1 d . . .
C2 C -0.0674(6) -0.2404(6) 0.2526(6) 0.0427(15) Uani 1 1 d . . .
H2 H -0.0113 -0.2561 0.2516 0.051 Uiso 1 1 calc R . .
C3 C -0.1555(6) -0.2992(5) 0.1769(6) 0.0405(14) Uani 1 1 d . . .
C4 C -0.2393(5) -0.2784(5) 0.1792(6) 0.0372(14) Uani 1 1 d . . .
C5 C -0.2318(6) -0.1964(6) 0.2566(6) 0.0411(15) Uani 1 1 d . . .
H5 H -0.2891 -0.1825 0.2585 0.049 Uiso 1 1 calc R . .
C6 C -0.1402(5) -0.1334(5) 0.3324(6) 0.0403(15) Uani 1 1 d . . .
C7 C -0.1391(6) -0.0437(6) 0.4090(7) 0.0478(16) Uani 1 1 d . . .
H7A H -0.2122 -0.0670 0.4395 0.057 Uiso 1 1 calc R . .
H7B H -0.0937 -0.0292 0.4869 0.057 Uiso 1 1 calc R . .
C8 C -0.0774(7) -0.3838(8) 0.0597(8) 0.057(2) Uani 1 1 d . . .
H8A H -0.0257 -0.3151 0.0219 0.086 Uiso 1 1 calc R . .
H8B H -0.0962 -0.4402 -0.0048 0.086 Uiso 1 1 calc R . .
H8C H -0.0463 -0.3979 0.1365 0.086 Uiso 1 1 calc R . .
C9 C -0.3990(6) -0.3064(6) 0.0804(7) 0.0511(18) Uani 1 1 d . . .
H9A H -0.3629 -0.2361 0.0371 0.061 Uiso 1 1 calc R . .
H9B H -0.4276 -0.2986 0.1647 0.061 Uiso 1 1 calc R . .
C10 C -0.4871(6) -0.3835(6) -0.0021(8) 0.0498(17) Uani 1 1 d . . .
C11 C -0.5930(7) -0.4246(7) 0.0232(9) 0.061(2) Uani 1 1 d . . .
H11 H -0.6211 -0.4126 0.1007 0.073 Uiso 1 1 calc R . .
C12 C -0.5563(7) -0.4768(7) -0.1812(10) 0.066(2) Uani 1 1 d . . .
H12 H -0.5585 -0.5068 -0.2641 0.079 Uiso 1 1 calc R . .

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 0.0506(11) 0.0554(12) 0.0777(12) -0.0110(12) 0.0001(12) 0.0184(9)
O1 0.054(3) 0.040(3) 0.055(3) -0.003(2) 0.000(3) 0.024(2)
O2 0.040(2) 0.038(3) 0.050(2) 0.002(2) 0.003(2) 0.019(2)
O3 0.067(4) 0.075(5) 0.129(7) -0.017(5) -0.003(4) 0.033(4)
O4 0.091(6) 0.091(6) 0.094(9) 0.000 0.000 0.046(3)
N1 0.064(4) 0.047(3) 0.049(3) -0.009(3) 0.005(3) 0.024(3)
C1 0.044(4) 0.042(4) 0.033(3) 0.007(3) 0.006(3) 0.018(3)
C2 0.048(4) 0.040(4) 0.041(3) 0.011(3) 0.005(3) 0.023(3)
C3 0.048(4) 0.033(3) 0.039(3) 0.003(3) 0.006(3) 0.019(3)
C4 0.039(3) 0.027(3) 0.039(3) 0.005(2) 0.009(3) 0.011(3)
C5 0.045(4) 0.044(4) 0.035(3) 0.006(3) 0.008(3) 0.023(3)
C6 0.049(4) 0.040(3) 0.025(2) 0.005(3) 0.009(3) 0.017(3)
C7 0.054(4) 0.054(4) 0.036(3) 0.002(3) 0.007(3) 0.027(3)
C8 0.062(5) 0.067(5) 0.058(4) 0.003(4) 0.004(4) 0.045(5)
C9 0.052(4) 0.046(4) 0.051(4) 0.000(3) 0.004(3) 0.021(3)
C10 0.048(4) 0.045(4) 0.056(4) -0.007(3) 0.001(3) 0.023(4)
C11 0.051(5) 0.064(5) 0.072(5) -0.003(4) 0.009(4) 0.032(4)
C12 0.071(6) 0.053(5) 0.065(5) -0.017(4) -0.001(5) 0.025(4)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C12 1.668(10) . ?
S1 C11 1.709(10) . ?
O1 C3 1.377(8) . ?
O1 C8 1.408(9) . ?
O2 C4 1.366(8) . ?
O2 C9 1.422(10) . ?
N1 C12 1.308(12) . ?
N1 C10 1.405(10) . ?
C1 C6 1.395(10) . ?
C1 C2 1.410(10) . ?
C1 C7 1.514(10) 3 ?
C2 C3 1.370(10) . ?
C3 C4 1.394(9) . ?
C4 C5 1.389(9) . ?
C5 C6 1.413(10) . ?
C6 C7 1.515(10) . ?
C7 C1 1.514(10) 5 ?
C9 C10 1.475(11) . ?
C10 C11 1.368(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 S1 C11 89.7(4) . . ?
C3 O1 C8 116.9(6) . . ?
C4 O2 C9 116.7(5) . . ?
C12 N1 C10 108.7(7) . . ?
C6 C1 C2 119.2(7) . . ?
C6 C1 C7 123.8(6) . 3 ?
C2 C1 C7 117.0(6) . 3 ?
C3 C2 C1 121.4(7) . . ?
C2 C3 O1 124.6(7) . . ?
C2 C3 C4 120.0(6) . . ?
O1 C3 C4 115.5(6) . . ?
O2 C4 C5 124.1(6) . . ?
O2 C4 C3 116.4(5) . . ?
C5 C4 C3 119.5(6) . . ?
C4 C5 C6 121.0(7) . . ?
C1 C6 C5 118.8(6) . . ?
C1 C6 C7 124.7(6) . . ?
C5 C6 C7 116.4(6) . . ?
C1 C7 C6 113.7(5) 5 . ?
O2 C9 C10 110.1(6) . . ?
C11 C10 N1 114.0(7) . . ?
C11 C10 C9 125.5(8) . . ?
N1 C10 C9 120.4(7) . . ?
C10 C11 S1 110.2(6) . . ?
N1 C12 S1 117.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        73.42
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.113
####################################################################### 
# 
# 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_c
_database_code_depnum_ccdc_archive 'CCDC 1470478'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
octa[tris-(4-methylthiazolyl)cyclotriguaiacylene]dodecasilver(I)rhenate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C288 H264 Ag12 N24 O96 Re12 S24'
_chemical_formula_weight         9895.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   F432

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'

_cell_length_a                   35.7237(4)
_cell_length_b                   35.7237(4)
_cell_length_c                   35.7237(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     45590.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3087
_cell_measurement_theta_min      4.0800
_cell_measurement_theta_max      72.2730

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             19104
_exptl_absorpt_coefficient_mu    11.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9948
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.50
_diffrn_reflns_theta_max         73.74
_reflns_number_total             3794
_reflns_number_gt                2667
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

ReO4 - Re-O distances were constrained to chemically reasonable
values

One ReO4 position is not fully occupied and is sited on a 4-fold 
axis, hence O positions are also disordeerd

Other ReO4, O positionsrefined with group Uiso

Only Re of ReO4 were refined anisotropically
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1989P)²+179.8345P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_number_reflns         3794
_refine_ls_number_parameters     168
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0847
_refine_ls_wR_factor_ref         0.2886
_refine_ls_wR_factor_gt          0.2499
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.862804(13) 0.137196(13) 0.137196(13) 0.0674(3) Uani 1 3 d SD . .
Re2 Re 0.84830(11) 0.0000 0.5000 0.1384(10) Uani 0.67 4 d SPD . .
Ag1 Ag 0.82756(3) 0.0000 0.32756(3) 0.1012(6) Uani 1 2 d S . .
S1 S 0.7512(3) 0.03771(18) 0.42495(15) 0.163(4) Uani 1 1 d . . .
O1 O 0.8312(3) 0.0547(2) 0.2469(3) 0.068(2) Uani 1 1 d . . .
O2 O 0.7764(2) 0.04381(19) 0.29074(19) 0.0532(17) Uani 1 1 d . . .
O3 O 0.8225(6) 0.1135(6) 0.1485(6) 0.164(6) Uiso 1 1 d D . .
O4 O 0.8897(4) 0.1103(4) 0.1103(4) 0.164(6) Uiso 1 3 d SD . .
O5 O 0.8006(12) 0.0000 0.5000 0.19(2) Uiso 0.67 4 d SPD . .
O6 O 0.8482(15) -0.0372(13) 0.5218(15) 0.22(2) Uiso 0.50 1 d PD . .
N1 N 0.7861(5) 0.0208(4) 0.3660(3) 0.097(5) Uani 1 1 d . . .
C1 C 0.8209(2) 0.1921(2) 0.2537(2) 0.044(2) Uani 1 1 d . . .
H1A H 0.7993 0.2095 0.2536 0.053 Uiso 1 1 calc R . .
H1B H 0.8300 0.1898 0.2276 0.053 Uiso 1 1 calc R . .
C2 C 0.8076(3) 0.1537(3) 0.2671(3) 0.048(2) Uani 1 1 d . . .
C3 C 0.8264(3) 0.1233(3) 0.2521(3) 0.048(2) Uani 1 1 d . . .
H3 H 0.8467 0.1275 0.2355 0.058 Uiso 1 1 calc R . .
C4 C 0.8162(3) 0.0865(3) 0.2610(3) 0.049(2) Uani 1 1 d . . .
C5 C 0.7847(3) 0.0809(2) 0.2855(3) 0.0473(17) Uani 1 1 d . . .
C6 C 0.7670(3) 0.1113(3) 0.2993(3) 0.048(2) Uani 1 1 d . . .
H6 H 0.7461 0.1076 0.3154 0.057 Uiso 1 1 calc R . .
C7 C 0.7780(3) 0.1476(3) 0.2911(3) 0.044(2) Uani 1 1 d . . .
C8 C 0.7443(3) 0.0355(3) 0.3130(3) 0.056(2) Uani 1 1 d . . .
H8A H 0.7346 0.0105 0.3061 0.067 Uiso 1 1 calc R . .
H8B H 0.7245 0.0541 0.3078 0.067 Uiso 1 1 calc R . .
C9 C 0.7531(4) 0.0359(3) 0.3541(4) 0.072(3) Uani 1 1 d . . .
C10 C 0.7288(7) 0.0459(5) 0.3814(4) 0.105(7) Uani 1 1 d . . .
H10 H 0.7043 0.0555 0.3779 0.126 Uiso 1 1 calc R . .
C11 C 0.7903(9) 0.0189(7) 0.4034(5) 0.138(9) Uani 1 1 d . . .
H11 H 0.8114 0.0089 0.4160 0.166 Uiso 1 1 calc R . .
C12 C 0.8627(5) 0.0585(4) 0.2231(6) 0.093(5) Uani 1 1 d . . .
H12A H 0.8564 0.0750 0.2021 0.140 Uiso 1 1 calc R . .
H12B H 0.8700 0.0339 0.2135 0.140 Uiso 1 1 calc R . .
H12C H 0.8836 0.0693 0.2373 0.140 Uiso 1 1 calc R . .

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
Re1 0.0674(3) 0.0674(3) 0.0674(3) -0.0052(2) 0.0052(2) 0.0052(2)
Re2 0.137(2) 0.1392(15) 0.1392(15) 0.000 0.000 0.000
Ag1 0.0941(7) 0.1154(13) 0.0941(7) -0.0239(10) -0.0225(8) 0.0239(10)
S1 0.303(11) 0.118(4) 0.068(2) -0.002(3) 0.036(4) 0.062(6)
O1 0.085(6) 0.039(4) 0.080(5) -0.008(4) 0.023(4) 0.003(4)
O2 0.065(4) 0.042(3) 0.053(4) 0.003(3) 0.005(3) -0.009(3)
N1 0.156(14) 0.089(8) 0.048(5) -0.009(6) -0.010(7) 0.035(9)
C1 0.050(5) 0.046(5) 0.036(4) 0.007(3) -0.005(3) 0.006(4)
C2 0.060(6) 0.040(4) 0.044(5) 0.008(4) -0.013(4) 0.002(4)
C3 0.047(5) 0.041(4) 0.058(5) 0.000(4) -0.004(4) 0.004(4)
C4 0.050(5) 0.042(5) 0.056(6) 0.004(4) 0.003(4) -0.006(4)
C5 0.051(6) 0.049(4) 0.043(5) 0.003(5) -0.008(3) -0.003(5)
C6 0.050(5) 0.049(5) 0.044(5) 0.006(4) -0.006(4) -0.004(4)
C7 0.047(5) 0.042(4) 0.043(4) 0.005(4) -0.006(4) 0.010(3)
C8 0.053(6) 0.043(5) 0.071(7) -0.005(5) -0.004(5) -0.010(4)
C9 0.096(10) 0.041(5) 0.080(8) 0.003(5) 0.009(7) -0.005(6)
C10 0.160(18) 0.090(11) 0.065(9) 0.009(8) 0.041(10) 0.034(12)
C11 0.21(3) 0.144(19) 0.060(9) -0.015(10) -0.026(13) 0.039(17)
C12 0.072(8) 0.074(9) 0.134(14) 0.004(9) 0.053(9) 0.005(7)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
Highest residual peak is 0.24 A from RE1 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O4 1.67(3) . ?
Re1 O3 1.72(2) . ?
Re1 O3 1.72(2) 15_656 ?
Re1 O3 1.72(2) 16_665 ?
Re2 O6 1.54(3) 31_545 ?
Re2 O6 1.54(4) 6_556 ?
Re2 O6 1.54(3) . ?
Re2 O6 1.54(3) 29 ?
Re2 O5 1.70(4) . ?
Ag1 N1 2.151(15) . ?
Ag1 N1 2.151(15) 71_554 ?
S1 C11 1.73(3) . ?
S1 C10 1.77(2) . ?
O1 C4 1.355(13) . ?
O1 C12 1.417(16) . ?
O2 C5 1.370(11) . ?
O2 C8 1.427(13) . ?
N1 C11 1.34(2) . ?
N1 C9 1.37(2) . ?
C1 C2 1.529(13) . ?
C1 C7 1.544(13) 37_654 ?
C2 C7 1.380(17) . ?
C2 C3 1.383(15) . ?
C3 C4 1.403(14) . ?
C4 C5 1.438(18) . ?
C5 C6 1.349(15) . ?
C6 C7 1.387(13) . ?
C7 C1 1.544(13) 62_565 ?
C8 C9 1.499(19) . ?
C9 C10 1.35(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Re1 O3 109.6(7) . . ?
O4 Re1 O3 109.6(7) . 15_656 ?
O3 Re1 O3 109.3(7) . 15_656 ?
O4 Re1 O3 109.6(7) . 16_665 ?
O3 Re1 O3 109.3(7) . 16_665 ?
O3 Re1 O3 109.3(7) 15_656 16_665 ?
O6 Re2 O6 90.001(17) 31_545 6_556 ?
O6 Re2 O6 89.999(11) 31_545 . ?
O6 Re2 O6 180(5) 6_556 . ?
O6 Re2 O6 180(4) 31_545 29 ?
O6 Re2 O6 89.997(9) 6_556 29 ?
O6 Re2 O6 90.002(15) . 29 ?
O6 Re2 O5 90(2) 31_545 . ?
O6 Re2 O5 90(2) 6_556 . ?
O6 Re2 O5 90(2) . . ?
O6 Re2 O5 90(2) 29 . ?
N1 Ag1 N1 175.9(8) . 71_554 ?
C11 S1 C10 92.1(9) . . ?
C4 O1 C12 117.2(9) . . ?
C5 O2 C8 116.8(9) . . ?
C11 N1 C9 115.0(19) . . ?
C11 N1 Ag1 122.7(17) . . ?
C9 N1 Ag1 122.2(9) . . ?
C2 C1 C7 113.5(7) . 37_654 ?
C7 C2 C3 119.3(9) . . ?
C7 C2 C1 125.1(9) . . ?
C3 C2 C1 115.6(10) . . ?
C2 C3 C4 121.4(10) . . ?
O1 C4 C3 126.8(10) . . ?
O1 C4 C5 114.9(9) . . ?
C3 C4 C5 118.1(9) . . ?
C6 C5 O2 128.8(12) . . ?
C6 C5 C4 118.5(9) . . ?
O2 C5 C4 112.7(10) . . ?
C5 C6 C7 122.8(10) . . ?
C2 C7 C6 119.8(9) . . ?
C2 C7 C1 123.9(8) . 62_565 ?
C6 C7 C1 116.2(8) . 62_565 ?
O2 C8 C9 112.2(10) . . ?
C10 C9 N1 115.7(16) . . ?
C10 C9 C8 125.1(16) . . ?
N1 C9 C8 118.6(12) . . ?
C9 C10 S1 107.4(16) . . ?
N1 C11 S1 109.6(19) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        73.74
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         2.000
_refine_diff_density_min         -2.126
_refine_diff_density_rms         0.218

# start Validation Reply Form
_vrf_PLAT308_c__users_           
;
PROBLEM: Single Bonded Metal Atom in Structure  (Unusual)        Re2 Check 
RESPONSE: Disordered ReO4, Re2-O bonds are given in cif
;
_vrf_PLAT430_c__users_           
;
PROBLEM: Short Inter D...A Contact  O5     ..  O6      ..       2.29 Ang.  
RESPONSE: Oxygen of disordered ReO4
;
_vrf_PLAT602_c__users_           
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: ...
;
# end Validation Reply Form

####################################################################### 
# 
# 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_c
_database_code_depnum_ccdc_archive 'CCDC 1470479'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
octa[tris-(4-methylthiazolyl)cyclotriguaiacylene]dodecasilver(I)tetrafluoroborate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C288 H264 Ag12 B12 F48 N24 O48 S24'
_chemical_formula_weight         7934.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   F432

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'

_cell_length_a                   35.4548(7)
_cell_length_b                   35.4548(7)
_cell_length_c                   35.4548(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     44568.2(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1977
_cell_measurement_theta_min      4.1250
_cell_measurement_theta_max      4.777

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             15936
_exptl_absorpt_coefficient_mu    5.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37596
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4858
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.53
_diffrn_reflns_theta_max         73.63
_reflns_number_total             2572
_reflns_number_gt                1639
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

BF4- could not be refined and are excluded from refinement though 
included in formula. Data was squeezed, R1 fell from ca. 17% to 7%

DELU restraints used on displacement parameters

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1359P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(3)
_refine_ls_number_reflns         2572
_refine_ls_number_parameters     152
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_ref         0.2256
_refine_ls_wR_factor_gt          0.2054
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.5000 0.33014(2) 0.33014(2) 0.0933(6) Uani 1 2 d SU . .
S1 S 0.46238(11) 0.42451(9) 0.24863(17) 0.1314(16) Uani 1 1 d U . .
O1 O 0.44465(15) 0.24483(18) 0.33232(19) 0.0624(17) Uani 1 1 d U . .
O2 O 0.45689(14) 0.28998(15) 0.27824(15) 0.0495(14) Uani 1 1 d U . .
N1 N 0.4800(3) 0.3681(2) 0.2860(3) 0.082(2) Uani 1 1 d U . .
C1 C 0.3073(2) 0.2538(2) 0.3214(2) 0.0429(18) Uani 1 1 d U . .
H1A H 0.2898 0.2547 0.2996 0.051 Uiso 1 1 calc R . .
H1B H 0.3089 0.2273 0.3298 0.051 Uiso 1 1 calc R . .
C2 C 0.3464(2) 0.2664(2) 0.3079(2) 0.0375(16) Uani 1 1 d U . .
C3 C 0.3787(2) 0.2512(2) 0.3270(2) 0.0408(16) Uani 1 1 d U . .
H3 H 0.3752 0.2344 0.3477 0.049 Uiso 1 1 calc R . .
C4 C 0.41248(19) 0.2601(2) 0.3163(2) 0.0421(18) Uani 1 1 d U . .
C5 C 0.41970(19) 0.2842(3) 0.2866(3) 0.0451(16) Uani 1 1 d U . .
C6 C 0.3890(2) 0.2992(2) 0.2670(2) 0.0422(18) Uani 1 1 d U . .
H6 H 0.3932 0.3155 0.2462 0.051 Uiso 1 1 calc R . .
C7 C 0.3533(2) 0.29075(18) 0.27737(19) 0.0389(17) Uani 1 1 d U . .
C8 C 0.4660(2) 0.3139(3) 0.2465(3) 0.058(2) Uani 1 1 d U . .
H8A H 0.4918 0.3076 0.2379 0.069 Uiso 1 1 calc R . .
H8B H 0.4484 0.3079 0.2256 0.069 Uiso 1 1 calc R . .
C9 C 0.4642(2) 0.3535(3) 0.2537(3) 0.066(2) Uani 1 1 d U . .
C10 C 0.4540(3) 0.3812(3) 0.2289(4) 0.092(3) Uani 1 1 d U . .
H10 H 0.4439 0.3771 0.2045 0.111 Uiso 1 1 calc R . .
C11 C 0.4817(3) 0.4038(3) 0.2872(5) 0.112(4) Uani 1 1 d U . .
H11 H 0.4926 0.4175 0.3075 0.134 Uiso 1 1 calc R . .
C12 C 0.4383(3) 0.2180(4) 0.3628(3) 0.110(6) Uani 1 1 d U . .
H12A H 0.4287 0.2314 0.3850 0.165 Uiso 1 1 calc R . .
H12B H 0.4621 0.2055 0.3692 0.165 Uiso 1 1 calc R . .
H12C H 0.4198 0.1991 0.3548 0.165 Uiso 1 1 calc R . .

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
Ag1 0.1061(10) 0.0870(6) 0.0870(6) -0.0134(6) -0.0152(7) 0.0152(7)
S1 0.110(3) 0.0591(18) 0.225(5) 0.021(3) -0.039(3) 0.0030(18)
O1 0.025(3) 0.071(4) 0.091(5) 0.006(3) 0.004(3) 0.001(3)
O2 0.038(3) 0.057(3) 0.053(3) 0.006(3) 0.009(2) -0.003(2)
N1 0.065(5) 0.049(4) 0.132(7) -0.001(4) -0.002(5) 0.004(4)
C1 0.052(4) 0.031(4) 0.046(5) -0.002(3) 0.008(3) -0.001(3)
C2 0.043(4) 0.042(5) 0.028(4) -0.008(3) 0.008(3) 0.011(3)
C3 0.045(4) 0.036(4) 0.041(4) 0.004(3) 0.008(3) 0.015(3)
C4 0.007(3) 0.051(5) 0.069(5) -0.001(3) 0.010(3) 0.002(3)
C5 0.035(4) 0.050(5) 0.050(5) -0.010(3) 0.016(3) -0.010(3)
C6 0.033(4) 0.032(4) 0.062(5) -0.009(3) 0.010(3) 0.001(3)
C7 0.042(4) 0.029(4) 0.046(4) 0.001(3) -0.005(3) 0.011(3)
C8 0.025(4) 0.067(5) 0.081(6) 0.011(4) 0.018(4) -0.015(4)
C9 0.031(5) 0.059(4) 0.107(7) 0.003(4) -0.008(5) -0.004(4)
C10 0.038(6) 0.082(6) 0.158(9) 0.038(6) -0.012(6) -0.008(5)
C11 0.095(9) 0.037(5) 0.204(11) -0.021(6) -0.039(9) 0.010(6)
C12 0.029(5) 0.218(16) 0.083(8) 0.085(9) 0.000(5) 0.008(7)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N1 2.182(10) 21_655 ?
Ag1 N1 2.182(10) . ?
S1 C11 1.696(16) . ?
S1 C10 1.711(14) . ?
O1 C4 1.385(9) . ?
O1 C12 1.457(12) . ?
O2 C5 1.367(8) . ?
O2 C8 1.445(10) . ?
N1 C11 1.270(14) . ?
N1 C9 1.375(14) . ?
C1 C7 1.525(9) 12 ?
C1 C2 1.530(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.408(10) . ?
C2 C3 1.435(10) . ?
C3 C4 1.298(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(13) . ?
C5 C6 1.397(12) . ?
C6 C7 1.350(11) . ?
C6 H6 0.9500 . ?
C7 C1 1.525(9) 11 ?
C8 C9 1.428(14) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.368(15) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ag1 N1 171.8(5) 21_655 . ?
C11 S1 C10 90.6(6) . . ?
C4 O1 C12 115.7(6) . . ?
C5 O2 C8 118.2(7) . . ?
C11 N1 C9 115.0(12) . . ?
C11 N1 Ag1 125.2(10) . . ?
C9 N1 Ag1 119.8(7) . . ?
C7 C1 C2 114.9(6) 12 . ?
C7 C1 H1A 108.5 12 . ?
C2 C1 H1A 108.5 . . ?
C7 C1 H1B 108.5 12 . ?
C2 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
C7 C2 C3 117.1(7) . . ?
C7 C2 C1 125.1(7) . . ?
C3 C2 C1 117.8(7) . . ?
C4 C3 C2 120.5(7) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 123.2(8) . . ?
C3 C4 O1 123.0(7) . . ?
C5 C4 O1 113.7(6) . . ?
O2 C5 C4 116.0(8) . . ?
O2 C5 C6 126.0(9) . . ?
C4 C5 C6 118.0(7) . . ?
C7 C6 C5 120.8(8) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C2 120.5(7) . . ?
C6 C7 C1 117.5(7) . 11 ?
C2 C7 C1 121.9(7) . 11 ?
C9 C8 O2 115.4(9) . . ?
C9 C8 H8A 108.4 . . ?
O2 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
O2 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
C10 C9 N1 111.8(10) . . ?
C10 C9 C8 127.2(11) . . ?
N1 C9 C8 120.1(9) . . ?
C9 C10 S1 109.8(11) . . ?
C9 C10 H10 125.1 . . ?
S1 C10 H10 125.1 . . ?
N1 C11 S1 112.6(11) . . ?
N1 C11 H11 123.7 . . ?
S1 C11 H11 123.7 . . ?
O1 C12 H12A 109.5 . . ?
O1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ag1 N1 C11 -160.9(11) 21_655 . . . ?
N1 Ag1 N1 C9 18.7(7) 21_655 . . . ?
C7 C1 C2 C7 -94.7(9) 12 . . . ?
C7 C1 C2 C3 87.6(8) 12 . . . ?
C7 C2 C3 C4 0.5(11) . . . . ?
C1 C2 C3 C4 178.3(7) . . . . ?
C2 C3 C4 C5 0.1(12) . . . . ?
C2 C3 C4 O1 -176.6(7) . . . . ?
C12 O1 C4 C3 -0.7(13) . . . . ?
C12 O1 C4 C5 -177.6(9) . . . . ?
C8 O2 C5 C4 177.8(7) . . . . ?
C8 O2 C5 C6 0.4(11) . . . . ?
C3 C4 C5 O2 -178.4(7) . . . . ?
O1 C4 C5 O2 -1.5(10) . . . . ?
C3 C4 C5 C6 -0.9(11) . . . . ?
O1 C4 C5 C6 176.1(7) . . . . ?
O2 C5 C6 C7 178.4(7) . . . . ?
C4 C5 C6 C7 1.1(11) . . . . ?
C5 C6 C7 C2 -0.6(11) . . . . ?
C5 C6 C7 C1 -178.2(6) . . . 11 ?
C3 C2 C7 C6 -0.2(11) . . . . ?
C1 C2 C7 C6 -177.9(7) . . . . ?
C3 C2 C7 C1 177.3(6) . . . 11 ?
C1 C2 C7 C1 -0.4(11) . . . 11 ?
C5 O2 C8 C9 80.2(9) . . . . ?
C11 N1 C9 C10 0.9(15) . . . . ?
Ag1 N1 C9 C10 -178.8(7) . . . . ?
C11 N1 C9 C8 170.4(10) . . . . ?
Ag1 N1 C9 C8 -9.2(13) . . . . ?
O2 C8 C9 C10 -147.0(10) . . . . ?
O2 C8 C9 N1 45.2(12) . . . . ?
N1 C9 C10 S1 -3.3(12) . . . . ?
C8 C9 C10 S1 -171.9(8) . . . . ?
C11 S1 C10 C9 3.7(10) . . . . ?
C9 N1 C11 S1 2.1(15) . . . . ?
Ag1 N1 C11 S1 -178.3(6) . . . . ?
C10 S1 C11 N1 -3.4(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.750
_diffrn_reflns_theta_full        73.63
_diffrn_measured_fraction_theta_full 0.749
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.084
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 -0.081 -0.121 -0.103 20339 6558 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
# start Validation Reply Form
_vrf_CHEMW03_c__users_           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: BF4 anions not located in strcuture are included in formula
;
# end Validation Reply Form
####################################################################### 
# 
# 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_c
_database_code_depnum_ccdc_archive 'CCDC 1478562'
_audit_update_record             
;
2016-05-06 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 tris-(4-methylthiazolyl)cyclotriguaiacylene nitromethane clathrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H42 N6 O12 S3'
_chemical_formula_weight         882.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   28.138(3)
_cell_length_b                   28.138(3)
_cell_length_c                   4.4445(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3047.4(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    864
_cell_measurement_theta_min      5.4200
_cell_measurement_theta_max      73.6040

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1386
_exptl_absorpt_coefficient_mu    2.277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.48073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;
_diffrn_ambient_temperature      120(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.3095
_diffrn_reflns_number            4449
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1148
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         5.45
_diffrn_reflns_theta_max         73.82
_reflns_number_total             2150
_reflns_number_gt                1635
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0537P)²+7.5716P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_number_reflns         2150
_refine_ls_number_parameters     183
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0719
_refine_ls_wR_factor_ref         0.1873
_refine_ls_wR_factor_gt          0.1663
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.59394(9) 0.59957(8) -0.0148(5) 0.0504(5) Uani 1 1 d . . .
O1 O 0.75098(17) 0.53308(17) 0.4594(10) 0.0328(10) Uani 1 1 d . . .
O2 O 0.64682(17) 0.49948(17) 0.4874(11) 0.0340(10) Uani 1 1 d . . .
C6 C 0.6639(2) 0.4689(2) 0.6464(14) 0.0271(12) Uani 1 1 d . . .
C5 C 0.7208(2) 0.4881(3) 0.6389(13) 0.0288(13) Uani 1 1 d . . .
N1 N 0.5317(2) 0.5173(3) 0.3088(15) 0.0476(16) Uani 1 1 d . . .
C2 C 0.6520(3) 0.3960(2) 0.9842(12) 0.0278(13) Uani 1 1 d . . .
C7 C 0.6308(2) 0.4240(2) 0.8201(14) 0.0286(12) Uani 1 1 d . . .
H7 H 0.5926 0.4115 0.8297 0.034 Uiso 1 1 calc R . .
C10 C 0.5816(3) 0.5207(3) 0.3035(14) 0.0332(14) Uani 1 1 d . . .
C4 C 0.7414(3) 0.4614(2) 0.8053(14) 0.0309(13) Uani 1 1 d . . .
H4 H 0.7798 0.4746 0.8016 0.037 Uiso 1 1 calc R . .
C3 C 0.7072(3) 0.4148(3) 0.9823(13) 0.0290(13) Uani 1 1 d . . .
C9 C 0.5907(3) 0.4804(3) 0.4836(16) 0.0335(13) Uani 1 1 d . . .
H9A H 0.5769 0.4777 0.6913 0.040 Uiso 1 1 calc R . .
H9B H 0.5709 0.4436 0.3901 0.040 Uiso 1 1 calc R . .
C1 C 0.6110(2) 0.3457(3) 1.1597(13) 0.0289(12) Uani 1 1 d . . .
H1A H 0.6297 0.3416 1.3378 0.035 Uiso 1 1 calc R . .
H1B H 0.5814 0.3520 1.2334 0.035 Uiso 1 1 calc R . .
C11 C 0.6207(3) 0.5624(3) 0.1426(16) 0.0387(15) Uani 1 1 d . . .
H11 H 0.6575 0.5701 0.1197 0.046 Uiso 1 1 calc R . .
C8 C 0.8075(3) 0.5504(3) 0.4191(16) 0.0378(15) Uani 1 1 d . . .
H8A H 0.8241 0.5817 0.2811 0.057 Uiso 1 1 calc R . .
H8B H 0.8111 0.5201 0.3348 0.057 Uiso 1 1 calc R . .
H8C H 0.8264 0.5612 0.6138 0.057 Uiso 1 1 calc R . .
C12 C 0.5330(4) 0.5567(4) 0.154(2) 0.059(2) Uani 1 1 d . . .
H12 H 0.5019 0.5615 0.1352 0.071 Uiso 1 1 calc R . .
N2 N 0.4445(4) 0.3737(3) 0.963(2) 0.077(3) Uani 1 1 d . . .
O3 O 0.4344(5) 0.4136(5) 0.822(4) 0.159(5) Uani 1 1 d . . .
C13 C 0.4881(3) 0.3763(3) 0.941(3) 0.062(3) Uani 1 1 d . . .
H13A H 0.5030 0.3891 0.7388 0.093 Uiso 1 1 calc R . .
H13B H 0.4836 0.3398 0.9742 0.093 Uiso 1 1 calc R . .
H13C H 0.5134 0.4019 1.0910 0.093 Uiso 1 1 calc R . .
O4 O 0.4081(6) 0.3362(6) 1.087(5) 0.241(11) Uani 1 1 d . . .

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 0.0662(13) 0.0438(10) 0.0482(9) 0.0014(9) -0.0116(9) 0.0326(10)
O1 0.030(2) 0.023(2) 0.043(3) 0.0009(18) 0.0019(18) 0.0121(18)
O2 0.028(2) 0.030(2) 0.045(3) 0.0076(19) 0.0060(19) 0.0149(19)
C6 0.027(3) 0.027(3) 0.029(3) -0.007(2) -0.005(2) 0.015(2)
C5 0.026(3) 0.033(3) 0.027(3) -0.007(2) -0.002(2) 0.014(2)
N1 0.032(3) 0.053(4) 0.062(4) 0.002(3) -0.008(3) 0.025(3)
C2 0.035(3) 0.027(3) 0.021(3) -0.002(2) -0.004(2) 0.015(3)
C7 0.026(3) 0.029(3) 0.031(3) -0.003(2) 0.004(2) 0.014(2)
C10 0.034(3) 0.035(3) 0.033(3) -0.005(3) -0.006(3) 0.019(3)
C4 0.026(3) 0.028(3) 0.033(3) -0.006(2) -0.001(2) 0.009(2)
C3 0.033(3) 0.031(3) 0.021(3) -0.004(2) 0.001(2) 0.014(3)
C9 0.030(3) 0.033(3) 0.038(3) -0.007(3) -0.008(3) 0.016(3)
C1 0.025(3) 0.038(3) 0.028(3) -0.002(2) 0.003(2) 0.018(3)
C11 0.044(4) 0.038(4) 0.039(4) 0.000(3) -0.004(3) 0.023(3)
C8 0.031(3) 0.032(3) 0.043(4) 0.007(3) 0.009(3) 0.011(3)
C12 0.053(5) 0.055(5) 0.081(6) -0.019(4) -0.034(5) 0.036(4)
N2 0.062(5) 0.042(4) 0.115(7) 0.015(4) 0.014(5) 0.018(4)
O3 0.146(10) 0.132(9) 0.223(14) 0.028(9) -0.051(10) 0.088(8)
C13 0.042(5) 0.048(4) 0.109(8) 0.019(5) 0.004(4) 0.032(4)
O4 0.150(12) 0.193(14) 0.43(3) 0.214(17) 0.167(15) 0.126(12)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C12 1.700(10) . ?
S1 C11 1.714(7) . ?
O1 C5 1.373(8) . ?
O1 C8 1.424(8) . ?
O2 C6 1.372(7) . ?
O2 C9 1.390(8) . ?
C6 C7 1.372(9) . ?
C6 C5 1.412(8) . ?
C5 C4 1.372(9) . ?
N1 C12 1.291(11) . ?
N1 C10 1.361(9) . ?
C2 C3 1.368(9) . ?
C2 C7 1.406(9) . ?
C2 C1 1.520(8) . ?
C7 H7 0.9500 . ?
C10 C11 1.345(10) . ?
C10 C9 1.510(9) . ?
C4 C3 1.415(9) . ?
C4 H4 0.9500 . ?
C3 C1 1.519(9) 3_665 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C1 C3 1.519(9) 2_655 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C11 H11 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C12 H12 0.9500 . ?
N2 O4 1.178(13) . ?
N2 C13 1.195(12) . ?
N2 O3 1.432(13) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 S1 C11 89.0(4) . . ?
C5 O1 C8 117.3(5) . . ?
C6 O2 C9 116.7(5) . . ?
C7 C6 O2 125.4(5) . . ?
C7 C6 C5 118.8(6) . . ?
O2 C6 C5 115.7(5) . . ?
C4 C5 O1 125.6(5) . . ?
C4 C5 C6 119.2(6) . . ?
O1 C5 C6 115.3(5) . . ?
C12 N1 C10 110.2(7) . . ?
C3 C2 C7 119.8(6) . . ?
C3 C2 C1 123.4(5) . . ?
C7 C2 C1 116.8(5) . . ?
C6 C7 C2 121.8(6) . . ?
C6 C7 H7 119.1 . . ?
C2 C7 H7 119.1 . . ?
C11 C10 N1 115.8(6) . . ?
C11 C10 C9 124.5(6) . . ?
N1 C10 C9 119.7(6) . . ?
C5 C4 C3 122.0(6) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C2 C3 C4 118.4(6) . . ?
C2 C3 C1 124.3(5) . 3_665 ?
C4 C3 C1 117.3(5) . 3_665 ?
O2 C9 C10 107.6(5) . . ?
O2 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
O2 C9 H9B 110.2 . . ?
C10 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C3 C1 C2 114.7(5) 2_655 . ?
C3 C1 H1A 108.6 2_655 . ?
C2 C1 H1A 108.6 . . ?
C3 C1 H1B 108.6 2_655 . ?
C2 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C10 C11 S1 109.5(6) . . ?
C10 C11 H11 125.3 . . ?
S1 C11 H11 125.3 . . ?
O1 C8 H8A 109.5 . . ?
O1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C12 S1 115.4(6) . . ?
N1 C12 H12 122.3 . . ?
S1 C12 H12 122.3 . . ?
O4 N2 C13 119.9(10) . . ?
O4 N2 O3 118.8(11) . . ?
C13 N2 O3 121.2(9) . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 O2 C6 C7 -5.6(8) . . . . ?
C9 O2 C6 C5 178.0(5) . . . . ?
C8 O1 C5 C4 6.4(9) . . . . ?
C8 O1 C5 C6 -173.5(5) . . . . ?
C7 C6 C5 C4 -0.1(8) . . . . ?
O2 C6 C5 C4 176.6(5) . . . . ?
C7 C6 C5 O1 179.8(5) . . . . ?
O2 C6 C5 O1 -3.5(8) . . . . ?
O2 C6 C7 C2 -177.9(6) . . . . ?
C5 C6 C7 C2 -1.6(9) . . . . ?
C3 C2 C7 C6 2.7(9) . . . . ?
C1 C2 C7 C6 -178.0(5) . . . . ?
C12 N1 C10 C11 -0.5(10) . . . . ?
C12 N1 C10 C9 176.8(6) . . . . ?
O1 C5 C4 C3 -179.3(6) . . . . ?
C6 C5 C4 C3 0.6(9) . . . . ?
C7 C2 C3 C4 -2.0(9) . . . . ?
C1 C2 C3 C4 178.6(5) . . . . ?
C7 C2 C3 C1 177.8(6) . . . 3_665 ?
C1 C2 C3 C1 -1.6(9) . . . 3_665 ?
C5 C4 C3 C2 0.4(9) . . . . ?
C5 C4 C3 C1 -179.4(5) . . . 3_665 ?
C6 O2 C9 C10 178.7(5) . . . . ?
C11 C10 C9 O2 8.8(9) . . . . ?
N1 C10 C9 O2 -168.2(6) . . . . ?
C3 C2 C1 C3 -92.9(7) . . . 2_655 ?
C7 C2 C1 C3 87.8(7) . . . 2_655 ?
N1 C10 C11 S1 -0.5(8) . . . . ?
C9 C10 C11 S1 -177.6(5) . . . . ?
C12 S1 C11 C10 1.0(6) . . . . ?
C10 N1 C12 S1 1.3(9) . . . . ?
C11 S1 C12 N1 -1.4(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        73.82
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.073
