# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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. 
# 
#######################################################################

data_Zn
_database_code_depnum_ccdc_archive 'CCDC 1058697'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H48 N6 O22 S4 Zn'
_chemical_formula_weight         1182.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '

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

_cell_length_a                   22.103(3)
_cell_length_b                   19.932(3)
_cell_length_c                   15.101(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 130.848(2)
_cell_angle_gamma                90.00
_cell_volume                     5032.5(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2448
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7972
_exptl_absorpt_correction_T_max  0.8248
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14126
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         27.57
_reflns_number_total             5622
_reflns_number_gt                2478
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
The following restraints were used:
isor 0.01 0.01 O6
simu 0.01 0.01 O6
dfix 0.85 0.02 o2w h2wa o2w h2wb
dfix 1.35 0.02 h2wa h2wb
;

_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)+(0.1422P)²+10.0511P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5622
_refine_ls_number_parameters     346
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1685
_refine_ls_R_factor_gt           0.0890
_refine_ls_wR_factor_ref         0.3006
_refine_ls_wR_factor_gt          0.2462
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.047
_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
Zn1 Zn 0.2500 0.7500 0.5000 0.0701(4) Uani 1 2 d S . .
C1 C -0.1683(4) 0.5121(4) -0.1190(6) 0.078(2) Uani 1 1 d . . .
H1A H -0.1389 0.5488 -0.0709 0.094 Uiso 1 1 calc R . .
C2 C -0.2423(6) 0.5210(5) -0.2256(8) 0.099(3) Uani 1 1 d . . .
H2A H -0.2631 0.5641 -0.2508 0.119 Uiso 1 1 calc R . .
C3 C -0.2574(5) 0.4079(5) -0.2627(7) 0.087(2) Uani 1 1 d . . .
H3A H -0.2884 0.3722 -0.3122 0.105 Uiso 1 1 calc R . .
C4 C -0.1826(5) 0.3961(4) -0.1570(7) 0.079(2) Uani 1 1 d . . .
H4A H -0.1628 0.3525 -0.1357 0.095 Uiso 1 1 calc R . .
C5 C -0.1373(4) 0.4482(4) -0.0830(6) 0.0660(17) Uani 1 1 d . . .
C6 C -0.0560(4) 0.4382(3) 0.0351(6) 0.0648(17) Uani 1 1 d . . .
C7 C -0.0232(4) 0.3744(3) 0.0751(6) 0.0692(18) Uani 1 1 d . . .
H7A H -0.0519 0.3373 0.0280 0.083 Uiso 1 1 calc R . .
C8 C 0.0511(4) 0.3657(4) 0.1833(7) 0.0733(19) Uani 1 1 d . . .
C9 C 0.0912(4) 0.4218(3) 0.2481(6) 0.0707(18) Uani 1 1 d . . .
H9 H 0.1421 0.4181 0.3213 0.085 Uiso 1 1 calc R . .
C10 C 0.0553(4) 0.4853(3) 0.2039(6) 0.0684(18) Uani 1 1 d . . .
C11 C 0.0979(4) 0.5474(3) 0.2741(6) 0.0647(17) Uani 1 1 d . . .
C12 C 0.1688(4) 0.5453(4) 0.3893(6) 0.077(2) Uani 1 1 d . . .
H12A H 0.1910 0.5041 0.4259 0.093 Uiso 1 1 calc R . .
C13 C 0.2064(5) 0.6034(4) 0.4495(7) 0.086(2) Uani 1 1 d . . .
H13A H 0.2526 0.6003 0.5278 0.104 Uiso 1 1 calc R . .
C14 C 0.1109(4) 0.6674(4) 0.2918(6) 0.0719(19) Uani 1 1 d . . .
H14A H 0.0902 0.7095 0.2583 0.086 Uiso 1 1 calc R . .
C15 C 0.0684(4) 0.6124(4) 0.2256(6) 0.0723(19) Uani 1 1 d . . .
H15A H 0.0205 0.6174 0.1491 0.087 Uiso 1 1 calc R . .
C16 C 0.0829(4) 0.2966(4) 0.2349(6) 0.0723(19) Uani 1 1 d . . .
C17 C 0.0766(4) 0.2394(3) 0.1750(6) 0.0664(18) Uani 1 1 d . . .
C18 C 0.0963(4) 0.1769(4) 0.2288(6) 0.0700(18) Uani 1 1 d . . .
H18 H 0.0875 0.1386 0.1866 0.084 Uiso 1 1 calc R . .
C19 C 0.1288(4) 0.1705(4) 0.3441(7) 0.078(2) Uani 1 1 d . . .
C20 C 0.1428(5) 0.2290(5) 0.4075(7) 0.096(3) Uani 1 1 d . . .
H20A H 0.1678 0.2262 0.4863 0.115 Uiso 1 1 calc R . .
C21 C 0.1192(5) 0.2898(4) 0.3524(7) 0.094(3) Uani 1 1 d . . .
H21A H 0.1278 0.3280 0.3946 0.112 Uiso 1 1 calc R . .
N1 N -0.2853(4) 0.4688(5) -0.2941(6) 0.095(2) Uani 1 1 d . . .
H1B H -0.3324 0.4754 -0.3604 0.114 Uiso 1 1 calc R . .
N2 N -0.0171(3) 0.4932(3) 0.0983(5) 0.0672(14) Uani 1 1 d . . .
N3 N 0.1803(3) 0.6648(3) 0.4018(5) 0.0701(15) Uani 1 1 d . . .
O1W O 0.3588(3) 0.6936(2) 0.5876(4) 0.0833(14) Uani 1 1 d . . .
H1WA H 0.3895 0.7006 0.5732 0.125 Uiso 1 1 d R . .
H1WB H 0.3831 0.6680 0.6469 0.125 Uiso 1 1 d R . .
O1 O 0.0792(4) 0.1817(2) 0.0256(5) 0.0906(16) Uani 1 1 d . . .
O2 O -0.0394(3) 0.2461(2) -0.0516(5) 0.0947(17) Uani 1 1 d . . .
O2W O 0.2407(4) 0.7215(4) 0.6272(5) 0.0998(17) Uani 1 1 d D . .
H2WB H 0.277(4) 0.708(5) 0.697(4) 0.150 Uiso 1 1 d D . .
H2WA H 0.198(3) 0.721(6) 0.614(8) 0.150 Uiso 1 1 d D . .
O3 O 0.0843(3) 0.3027(2) 0.0334(5) 0.0890(15) Uani 1 1 d . . .
O3W O 0.1603(7) 0.1646(6) 0.6594(7) 0.262(7) Uani 1 1 d . . .
O4W O 0.0800(6) -0.0873(4) 0.2592(8) 0.185(4) Uani 1 1 d . . .
O4 O 0.0850(8) 0.0731(6) 0.3976(13) 0.274(8) Uani 1 1 d . . .
O5 O 0.2019(7) 0.1010(4) 0.5334(7) 0.190(4) Uani 1 1 d . . .
O5W O 0.0610(4) 0.0195(4) -0.0049(6) 0.152(3) Uani 1 1 d . . .
O6 O 0.1554(7) 0.0459(4) 0.3511(8) 0.189(4) Uani 1 1 d U . .
S1 S 0.04771(12) 0.24310(9) 0.03443(16) 0.0727(6) Uani 1 1 d . . .
S2 S 0.15460(17) 0.09146(13) 0.4122(2) 0.1029(8) Uani 1 1 d . . .


_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
Zn1 N3 2.114(6) . ?
Zn1 N3 2.114(6) 7_566 ?
Zn1 O2W 2.138(5) 7_566 ?
Zn1 O2W 2.138(5) . ?
Zn1 O1W 2.153(4) . ?
Zn1 O1W 2.153(4) 7_566 ?
C1 C2 1.362(10) . ?
C1 C5 1.379(9) . ?
C1 H1A 0.9300 . ?
C2 N1 1.331(12) . ?
C2 H2A 0.9300 . ?
C3 N1 1.302(10) . ?
C3 C4 1.373(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.366(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.503(9) . ?
C6 N2 1.333(8) . ?
C6 C7 1.390(8) . ?
C7 C8 1.374(9) . ?
C7 H7A 0.9300 . ?
C8 C9 1.364(10) . ?
C8 C16 1.510(9) . ?
C9 C10 1.410(8) . ?
C9 H9 0.9300 . ?
C10 N2 1.338(8) . ?
C10 C11 1.494(10) . ?
C11 C12 1.384(9) . ?
C11 C15 1.421(9) . ?
C12 C13 1.368(10) . ?
C12 H12A 0.9300 . ?
C13 N3 1.343(8) . ?
C13 H13A 0.9300 . ?
C14 N3 1.335(8) . ?
C14 C15 1.362(10) . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9300 . ?
C16 C21 1.394(10) . ?
C16 C17 1.406(10) . ?
C17 C18 1.393(8) . ?
C17 S1 1.774(7) . ?
C18 C19 1.389(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.409(11) . ?
C19 S2 1.759(7) . ?
C20 C21 1.367(11) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
N1 H1B 0.8600 . ?
O1W H1WA 0.8481 . ?
O1W H1WB 0.8493 . ?
O1 S1 1.457(5) . ?
O2 S1 1.459(6) . ?
O2W H2WB 0.85(2) . ?
O2W H2WA 0.84(2) . ?
O3 S1 1.444(5) . ?
O4 S2 1.452(10) . ?
O5 S2 1.405(8) . ?
O6 S2 1.302(9) . ?

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
N3 Zn1 N3 180.00 . 7_566 ?
N3 Zn1 O2W 92.1(2) . 7_566 ?
N3 Zn1 O2W 87.9(3) 7_566 7_566 ?
N3 Zn1 O2W 87.9(3) . . ?
N3 Zn1 O2W 92.1(2) 7_566 . ?
O2W Zn1 O2W 180.000 7_566 . ?
N3 Zn1 O1W 91.16(19) . . ?
N3 Zn1 O1W 88.84(19) 7_566 . ?
O2W Zn1 O1W 88.1(2) 7_566 . ?
O2W Zn1 O1W 91.9(2) . . ?
N3 Zn1 O1W 88.84(19) . 7_566 ?
N3 Zn1 O1W 91.16(19) 7_566 7_566 ?
O2W Zn1 O1W 91.9(2) 7_566 7_566 ?
O2W Zn1 O1W 88.1(2) . 7_566 ?
O1W Zn1 O1W 180.000 . 7_566 ?
C2 C1 C5 119.3(8) . . ?
C2 C1 H1A 120.4 . . ?
C5 C1 H1A 120.4 . . ?
N1 C2 C1 120.8(8) . . ?
N1 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
N1 C3 C4 120.5(8) . . ?
N1 C3 H3A 119.7 . . ?
C4 C3 H3A 119.7 . . ?
C5 C4 C3 120.1(7) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C4 C5 C1 118.1(7) . . ?
C4 C5 C6 122.6(6) . . ?
C1 C5 C6 119.3(7) . . ?
N2 C6 C7 122.1(6) . . ?
N2 C6 C5 116.9(6) . . ?
C7 C6 C5 121.0(7) . . ?
C8 C7 C6 120.7(7) . . ?
C8 C7 H7A 119.7 . . ?
C6 C7 H7A 119.7 . . ?
C9 C8 C7 117.4(6) . . ?
C9 C8 C16 120.8(7) . . ?
C7 C8 C16 121.3(7) . . ?
C8 C9 C10 119.8(7) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N2 C10 C9 122.2(7) . . ?
N2 C10 C11 117.2(6) . . ?
C9 C10 C11 120.6(6) . . ?
C12 C11 C15 115.8(7) . . ?
C12 C11 C10 122.5(6) . . ?
C15 C11 C10 121.7(6) . . ?
C13 C12 C11 120.4(6) . . ?
C13 C12 H12A 119.8 . . ?
C11 C12 H12A 119.8 . . ?
N3 C13 C12 123.6(7) . . ?
N3 C13 H13A 118.2 . . ?
C12 C13 H13A 118.2 . . ?
N3 C14 C15 124.1(6) . . ?
N3 C14 H14A 117.9 . . ?
C15 C14 H14A 117.9 . . ?
C14 C15 C11 119.5(6) . . ?
C14 C15 H15A 120.2 . . ?
C11 C15 H15A 120.2 . . ?
C21 C16 C17 118.2(6) . . ?
C21 C16 C8 115.6(7) . . ?
C17 C16 C8 126.2(6) . . ?
C18 C17 C16 119.2(6) . . ?
C18 C17 S1 117.8(5) . . ?
C16 C17 S1 122.9(5) . . ?
C19 C18 C17 121.5(7) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 118.6(7) . . ?
C18 C19 S2 121.3(6) . . ?
C20 C19 S2 120.1(6) . . ?
C21 C20 C19 119.6(7) . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C20 C21 C16 122.2(8) . . ?
C20 C21 H21A 118.9 . . ?
C16 C21 H21A 118.9 . . ?
C3 N1 C2 121.2(8) . . ?
C3 N1 H1B 119.4 . . ?
C2 N1 H1B 119.4 . . ?
C6 N2 C10 117.8(6) . . ?
C14 N3 C13 116.4(6) . . ?
C14 N3 Zn1 123.9(4) . . ?
C13 N3 Zn1 119.7(5) . . ?
Zn1 O1W H1WA 121.0 . . ?
Zn1 O1W H1WB 130.1 . . ?
H1WA O1W H1WB 107.9 . . ?
Zn1 O2W H2WB 130(6) . . ?
Zn1 O2W H2WA 124(6) . . ?
H2WB O2W H2WA 106(3) . . ?
O3 S1 O2 112.3(3) . . ?
O3 S1 O1 112.7(3) . . ?
O2 S1 O1 112.6(3) . . ?
O3 S1 C17 106.4(3) . . ?
O2 S1 C17 107.4(3) . . ?
O1 S1 C17 104.8(3) . . ?
O6 S2 O5 132.3(5) . . ?
O6 S2 O4 102.8(8) . . ?
O5 S2 O4 92.5(7) . . ?
O6 S2 C19 111.0(4) . . ?
O5 S2 C19 108.7(5) . . ?
O4 S2 C19 103.4(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
C5 C1 C2 N1 1.2(13) . . . . ?
N1 C3 C4 C5 1.0(12) . . . . ?
C3 C4 C5 C1 -1.3(11) . . . . ?
C3 C4 C5 C6 178.3(6) . . . . ?
C2 C1 C5 C4 0.2(11) . . . . ?
C2 C1 C5 C6 -179.3(7) . . . . ?
C4 C5 C6 N2 178.9(6) . . . . ?
C1 C5 C6 N2 -1.5(9) . . . . ?
C4 C5 C6 C7 -0.4(10) . . . . ?
C1 C5 C6 C7 179.1(6) . . . . ?
N2 C6 C7 C8 0.8(10) . . . . ?
C5 C6 C7 C8 -179.9(6) . . . . ?
C6 C7 C8 C9 -0.9(10) . . . . ?
C6 C7 C8 C16 171.5(6) . . . . ?
C7 C8 C9 C10 1.1(10) . . . . ?
C16 C8 C9 C10 -171.3(6) . . . . ?
C8 C9 C10 N2 -1.3(10) . . . . ?
C8 C9 C10 C11 179.4(6) . . . . ?
N2 C10 C11 C12 172.5(6) . . . . ?
C9 C10 C11 C12 -8.1(10) . . . . ?
N2 C10 C11 C15 -8.5(9) . . . . ?
C9 C10 C11 C15 170.9(6) . . . . ?
C15 C11 C12 C13 -0.2(11) . . . . ?
C10 C11 C12 C13 178.9(7) . . . . ?
C11 C12 C13 N3 -2.9(12) . . . . ?
N3 C14 C15 C11 0.5(11) . . . . ?
C12 C11 C15 C14 1.4(10) . . . . ?
C10 C11 C15 C14 -177.7(6) . . . . ?
C9 C8 C16 C21 37.0(10) . . . . ?
C7 C8 C16 C21 -135.2(8) . . . . ?
C9 C8 C16 C17 -145.2(7) . . . . ?
C7 C8 C16 C17 42.6(10) . . . . ?
C21 C16 C17 C18 8.8(11) . . . . ?
C8 C16 C17 C18 -168.9(7) . . . . ?
C21 C16 C17 S1 -168.9(6) . . . . ?
C8 C16 C17 S1 13.4(10) . . . . ?
C16 C17 C18 C19 -5.9(10) . . . . ?
S1 C17 C18 C19 172.0(5) . . . . ?
C17 C18 C19 C20 -0.8(11) . . . . ?
C17 C18 C19 S2 -179.4(5) . . . . ?
C18 C19 C20 C21 4.4(12) . . . . ?
S2 C19 C20 C21 -177.0(6) . . . . ?
C19 C20 C21 C16 -1.3(13) . . . . ?
C17 C16 C21 C20 -5.4(12) . . . . ?
C8 C16 C21 C20 172.6(8) . . . . ?
C4 C3 N1 C2 0.4(13) . . . . ?
C1 C2 N1 C3 -1.5(14) . . . . ?
C7 C6 N2 C10 -0.8(9) . . . . ?
C5 C6 N2 C10 179.9(5) . . . . ?
C9 C10 N2 C6 1.1(9) . . . . ?
C11 C10 N2 C6 -179.6(6) . . . . ?
C15 C14 N3 C13 -3.3(11) . . . . ?
C15 C14 N3 Zn1 175.4(5) . . . . ?
C12 C13 N3 C14 4.6(11) . . . . ?
C12 C13 N3 Zn1 -174.2(6) . . . . ?
N3 Zn1 N3 C14 70(100) 7_566 . . . ?
O2W Zn1 N3 C14 -57.8(6) 7_566 . . . ?
O2W Zn1 N3 C14 122.2(6) . . . . ?
O1W Zn1 N3 C14 -145.9(5) . . . . ?
O1W Zn1 N3 C14 34.1(5) 7_566 . . . ?
N3 Zn1 N3 C13 -111(100) 7_566 . . . ?
O2W Zn1 N3 C13 120.9(6) 7_566 . . . ?
O2W Zn1 N3 C13 -59.1(6) . . . . ?
O1W Zn1 N3 C13 32.8(6) . . . . ?
O1W Zn1 N3 C13 -147.2(6) 7_566 . . . ?
C18 C17 S1 O3 -139.7(5) . . . . ?
C16 C17 S1 O3 38.0(7) . . . . ?
C18 C17 S1 O2 99.8(6) . . . . ?
C16 C17 S1 O2 -82.4(7) . . . . ?
C18 C17 S1 O1 -20.1(7) . . . . ?
C16 C17 S1 O1 157.6(6) . . . . ?
C18 C19 S2 O6 13.7(9) . . . . ?
C20 C19 S2 O6 -164.9(8) . . . . ?
C18 C19 S2 O5 166.8(7) . . . . ?
C20 C19 S2 O5 -11.8(9) . . . . ?
C18 C19 S2 O4 -95.8(9) . . . . ?
C20 C19 S2 O4 85.6(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.958
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.102
####################################################################### 
# 
# 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_Cd
_database_code_depnum_ccdc_archive 'CCDC 1058698'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H17 Cd N3 O8 S2'
_chemical_formula_weight         615.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2928(16)
_cell_length_b                   11.423(2)
_cell_length_c                   12.436(2)
_cell_angle_alpha                101.262(2)
_cell_angle_beta                 103.547(2)
_cell_angle_gamma                96.798(2)
_cell_volume                     1106.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2436
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             616
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6386
_exptl_absorpt_correction_T_max  0.7088
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6113
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4245
_reflns_number_gt                3654
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0332P)²+0.6903P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4245
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0837
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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
Cd1 Cd 0.23473(3) -0.19539(2) 0.08956(2) 0.02432(10) Uani 1 1 d . . .
S1 S 0.45666(11) 0.09474(8) 0.27144(8) 0.0222(2) Uani 1 1 d . . .
S2 S 0.92389(12) -0.16858(8) 0.18761(9) 0.0297(2) Uani 1 1 d . . .
O1 O 0.4205(3) 0.1655(2) 0.3685(2) 0.0347(7) Uani 1 1 d . . .
O1W O 0.4598(4) -0.2357(3) 0.0000(3) 0.0413(7) Uani 1 1 d . . .
H1WA H 0.5426 -0.2640 0.0338 0.062 Uiso 1 1 d R . .
H1WB H 0.4717 -0.2323 -0.0654 0.062 Uiso 1 1 d R . .
O2 O 0.4276(3) 0.1486(2) 0.1726(2) 0.0342(7) Uani 1 1 d . . .
O2W O 0.2492(4) -0.0420(3) -0.0112(3) 0.0453(8) Uani 1 1 d . . .
H2WA H 0.3262 0.0109 0.0373 0.068 Uiso 1 1 d R . .
H2WB H 0.1763 -0.0048 -0.0438 0.068 Uiso 1 1 d R . .
O3 O 0.3713(3) -0.0314(2) 0.2402(2) 0.0265(6) Uani 1 1 d . . .
O4 O 1.0625(4) -0.2110(3) 0.2526(3) 0.0471(9) Uani 1 1 d . . .
O5 O 0.7696(3) -0.2554(2) 0.1432(3) 0.0456(8) Uani 1 1 d . . .
O6 O 0.9771(4) -0.1195(3) 0.0979(3) 0.0440(8) Uani 1 1 d . . .
N1 N 1.0623(4) 0.6746(3) 0.9246(3) 0.0307(8) Uani 1 1 d . . .
N2 N 0.7404(4) 0.5399(2) 0.5133(3) 0.0222(6) Uani 1 1 d . . .
N3 N 0.3790(4) 0.6890(3) 0.1999(3) 0.0267(7) Uani 1 1 d . . .
C3 C 0.9416(5) 0.7140(4) 0.8556(3) 0.0348(10) Uani 1 1 d . . .
H3A H 0.9095 0.7866 0.8840 0.042 Uiso 1 1 calc R . .
C4 C 0.8623(5) 0.6533(3) 0.7456(3) 0.0303(9) Uani 1 1 d . . .
H4A H 0.7797 0.6853 0.7015 0.036 Uiso 1 1 calc R . .
C5 C 0.9057(4) 0.5443(3) 0.7003(3) 0.0215(7) Uani 1 1 d . . .
C2 C 1.0999(6) 0.5682(4) 0.8808(4) 0.0415(11) Uani 1 1 d . . .
H2A H 1.1807 0.5372 0.9274 0.050 Uiso 1 1 calc R . .
C6 C 0.8301(4) 0.4789(3) 0.5798(3) 0.0195(7) Uani 1 1 d . . .
C7 C 0.8517(4) 0.3600(3) 0.5397(3) 0.0242(8) Uani 1 1 d . . .
H7A H 0.9143 0.3198 0.5885 0.029 Uiso 1 1 calc R . .
C8 C 0.7787(4) 0.3029(3) 0.4269(3) 0.0197(7) Uani 1 1 d . . .
C9 C 0.6874(4) 0.3676(3) 0.3579(3) 0.0233(8) Uani 1 1 d . . .
H9A H 0.6381 0.3325 0.2813 0.028 Uiso 1 1 calc R . .
C10 C 0.6701(4) 0.4853(3) 0.4040(3) 0.0206(7) Uani 1 1 d . . .
C11 C 0.5706(4) 0.5562(3) 0.3328(3) 0.0225(8) Uani 1 1 d . . .
C15 C 0.5094(6) 0.5151(4) 0.2154(3) 0.0361(10) Uani 1 1 d . . .
H15A H 0.5297 0.4413 0.1790 0.043 Uiso 1 1 calc R . .
C14 C 0.4192(5) 0.5842(4) 0.1540(4) 0.0380(10) Uani 1 1 d . . .
H14A H 0.3836 0.5565 0.0754 0.046 Uiso 1 1 calc R . .
C13 C 0.4351(5) 0.7274(3) 0.3132(3) 0.0305(9) Uani 1 1 d . . .
H13A H 0.4076 0.7994 0.3476 0.037 Uiso 1 1 calc R . .
C12 C 0.5312(5) 0.6661(3) 0.3808(3) 0.0275(8) Uani 1 1 d . . .
H12A H 0.5700 0.6979 0.4588 0.033 Uiso 1 1 calc R . .
C16 C 0.8056(4) 0.1786(3) 0.3794(3) 0.0214(7) Uani 1 1 d . . .
C21 C 0.9696(5) 0.1553(3) 0.4008(3) 0.0284(9) Uani 1 1 d . . .
H21A H 1.0556 0.2140 0.4513 0.034 Uiso 1 1 calc R . .
C20 C 1.0088(5) 0.0473(3) 0.3492(4) 0.0300(9) Uani 1 1 d . . .
H20A H 1.1195 0.0339 0.3647 0.036 Uiso 1 1 calc R . .
C19 C 0.8803(4) -0.0407(3) 0.2740(3) 0.0234(8) Uani 1 1 d . . .
C18 C 0.7160(4) -0.0224(3) 0.2569(3) 0.0233(8) Uani 1 1 d . . .
H18A H 0.6298 -0.0839 0.2107 0.028 Uiso 1 1 calc R . .
C17 C 0.6771(4) 0.0856(3) 0.3071(3) 0.0207(7) Uani 1 1 d . . .
C1 C 1.0282(5) 0.5018(3) 0.7726(3) 0.0349(10) Uani 1 1 d . . .
H1A H 1.0609 0.4284 0.7474 0.042 Uiso 1 1 calc R . .


_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
Cd1 N3 2.317(3) 1_545 ?
Cd1 N1 2.322(3) 1_444 ?
Cd1 O3 2.331(2) . ?
Cd1 O2W 2.353(3) . ?
Cd1 O6 2.415(3) 1_455 ?
Cd1 O1W 2.432(3) . ?
S1 O1 1.430(3) . ?
S1 O2 1.462(3) . ?
S1 O3 1.463(2) . ?
S1 C17 1.798(3) . ?
S2 O4 1.435(3) . ?
S2 O5 1.442(3) . ?
S2 O6 1.474(3) . ?
S2 C19 1.765(3) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O6 Cd1 2.415(3) 1_655 ?
N1 C2 1.334(5) . ?
N1 C3 1.340(5) . ?
N1 Cd1 2.322(3) 1_666 ?
N2 C6 1.336(4) . ?
N2 C10 1.337(4) . ?
N3 C14 1.336(5) . ?
N3 C13 1.341(5) . ?
N3 Cd1 2.317(3) 1_565 ?
C3 C4 1.373(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.387(5) . ?
C4 H4A 0.9300 . ?
C5 C1 1.391(5) . ?
C5 C6 1.486(5) . ?
C2 C1 1.364(5) . ?
C2 H2A 0.9300 . ?
C6 C7 1.401(5) . ?
C7 C8 1.382(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.390(5) . ?
C8 C16 1.492(4) . ?
C9 C10 1.393(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.488(5) . ?
C11 C12 1.391(5) . ?
C11 C15 1.392(5) . ?
C15 C14 1.369(5) . ?
C15 H15A 0.9300 . ?
C14 H14A 0.9300 . ?
C13 C12 1.372(5) . ?
C13 H13A 0.9300 . ?
C12 H12A 0.9300 . ?
C16 C21 1.391(5) . ?
C16 C17 1.408(5) . ?
C21 C20 1.387(5) . ?
C21 H21A 0.9300 . ?
C20 C19 1.390(5) . ?
C20 H20A 0.9300 . ?
C19 C18 1.376(5) . ?
C18 C17 1.380(5) . ?
C18 H18A 0.9300 . ?
C1 H1A 0.9300 . ?

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
N3 Cd1 N1 108.12(11) 1_545 1_444 ?
N3 Cd1 O3 85.16(10) 1_545 . ?
N1 Cd1 O3 166.48(10) 1_444 . ?
N3 Cd1 O2W 147.53(11) 1_545 . ?
N1 Cd1 O2W 89.04(11) 1_444 . ?
O3 Cd1 O2W 80.50(10) . . ?
N3 Cd1 O6 129.57(11) 1_545 1_455 ?
N1 Cd1 O6 82.71(11) 1_444 1_455 ?
O3 Cd1 O6 86.85(9) . 1_455 ?
O2W Cd1 O6 78.71(11) . 1_455 ?
N3 Cd1 O1W 77.50(11) 1_545 . ?
N1 Cd1 O1W 84.24(11) 1_444 . ?
O3 Cd1 O1W 101.55(9) . . ?
O2W Cd1 O1W 77.08(11) . . ?
O6 Cd1 O1W 152.60(11) 1_455 . ?
O1 S1 O2 113.61(17) . . ?
O1 S1 O3 113.43(17) . . ?
O2 S1 O3 110.61(16) . . ?
O1 S1 C17 108.27(16) . . ?
O2 S1 C17 105.75(16) . . ?
O3 S1 C17 104.42(15) . . ?
O4 S2 O5 115.14(18) . . ?
O4 S2 O6 109.2(2) . . ?
O5 S2 O6 112.2(2) . . ?
O4 S2 C19 109.01(18) . . ?
O5 S2 C19 107.36(17) . . ?
O6 S2 C19 103.26(17) . . ?
Cd1 O1W H1WA 120.0 . . ?
Cd1 O1W H1WB 132.1 . . ?
H1WA O1W H1WB 107.7 . . ?
Cd1 O2W H2WA 100.0 . . ?
Cd1 O2W H2WB 133.4 . . ?
H2WA O2W H2WB 107.7 . . ?
S1 O3 Cd1 145.07(17) . . ?
S2 O6 Cd1 104.09(16) . 1_655 ?
C2 N1 C3 115.6(3) . . ?
C2 N1 Cd1 122.1(3) . 1_666 ?
C3 N1 Cd1 120.7(2) . 1_666 ?
C6 N2 C10 118.5(3) . . ?
C14 N3 C13 116.3(3) . . ?
C14 N3 Cd1 122.1(3) . 1_565 ?
C13 N3 Cd1 121.5(2) . 1_565 ?
N1 C3 C4 123.8(4) . . ?
N1 C3 H3A 118.1 . . ?
C4 C3 H3A 118.1 . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C1 C5 C4 116.4(3) . . ?
C1 C5 C6 121.8(3) . . ?
C4 C5 C6 121.8(3) . . ?
N1 C2 C1 124.7(4) . . ?
N1 C2 H2A 117.7 . . ?
C1 C2 H2A 117.7 . . ?
N2 C6 C7 122.5(3) . . ?
N2 C6 C5 116.1(3) . . ?
C7 C6 C5 121.4(3) . . ?
C8 C7 C6 119.2(3) . . ?
C8 C7 H7A 120.4 . . ?
C6 C7 H7A 120.4 . . ?
C7 C8 C9 117.9(3) . . ?
C7 C8 C16 121.0(3) . . ?
C9 C8 C16 121.1(3) . . ?
C8 C9 C10 119.7(3) . . ?
C8 C9 H9A 120.2 . . ?
C10 C9 H9A 120.2 . . ?
N2 C10 C9 122.2(3) . . ?
N2 C10 C11 116.8(3) . . ?
C9 C10 C11 121.0(3) . . ?
C12 C11 C15 116.5(3) . . ?
C12 C11 C10 121.5(3) . . ?
C15 C11 C10 122.0(3) . . ?
C14 C15 C11 119.5(4) . . ?
C14 C15 H15A 120.2 . . ?
C11 C15 H15A 120.2 . . ?
N3 C14 C15 124.2(4) . . ?
N3 C14 H14A 117.9 . . ?
C15 C14 H14A 117.9 . . ?
N3 C13 C12 123.4(3) . . ?
N3 C13 H13A 118.3 . . ?
C12 C13 H13A 118.3 . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C21 C16 C17 117.6(3) . . ?
C21 C16 C8 118.1(3) . . ?
C17 C16 C8 124.1(3) . . ?
C20 C21 C16 122.0(3) . . ?
C20 C21 H21A 119.0 . . ?
C16 C21 H21A 119.0 . . ?
C21 C20 C19 119.0(3) . . ?
C21 C20 H20A 120.5 . . ?
C19 C20 H20A 120.5 . . ?
C18 C19 C20 119.8(3) . . ?
C18 C19 S2 118.4(3) . . ?
C20 C19 S2 121.4(3) . . ?
C17 C18 C19 121.1(3) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 S1 114.8(3) . . ?
C16 C17 S1 125.0(3) . . ?
C2 C1 C5 119.6(3) . . ?
C2 C1 H1A 120.2 . . ?
C5 C1 H1A 120.2 . . ?

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
O1 S1 O3 Cd1 142.0(2) . . . . ?
O2 S1 O3 Cd1 13.0(3) . . . . ?
C17 S1 O3 Cd1 -100.3(3) . . . . ?
N3 Cd1 O3 S1 139.7(3) 1_545 . . . ?
N1 Cd1 O3 S1 -50.8(6) 1_444 . . . ?
O2W Cd1 O3 S1 -11.1(3) . . . . ?
O6 Cd1 O3 S1 -90.2(3) 1_455 . . . ?
O1W Cd1 O3 S1 63.5(3) . . . . ?
O4 S2 O6 Cd1 15.4(2) . . . 1_655 ?
O5 S2 O6 Cd1 -113.45(16) . . . 1_655 ?
C19 S2 O6 Cd1 131.28(15) . . . 1_655 ?
C2 N1 C3 C4 -1.9(7) . . . . ?
Cd1 N1 C3 C4 163.9(3) 1_666 . . . ?
N1 C3 C4 C5 0.4(7) . . . . ?
C3 C4 C5 C1 1.2(6) . . . . ?
C3 C4 C5 C6 -176.6(4) . . . . ?
C3 N1 C2 C1 2.0(7) . . . . ?
Cd1 N1 C2 C1 -163.7(4) 1_666 . . . ?
C10 N2 C6 C7 -0.6(5) . . . . ?
C10 N2 C6 C5 179.8(3) . . . . ?
C1 C5 C6 N2 -167.0(4) . . . . ?
C4 C5 C6 N2 10.7(5) . . . . ?
C1 C5 C6 C7 13.5(6) . . . . ?
C4 C5 C6 C7 -168.8(3) . . . . ?
N2 C6 C7 C8 0.4(5) . . . . ?
C5 C6 C7 C8 180.0(3) . . . . ?
C6 C7 C8 C9 0.4(5) . . . . ?
C6 C7 C8 C16 176.9(3) . . . . ?
C7 C8 C9 C10 -1.0(5) . . . . ?
C16 C8 C9 C10 -177.5(3) . . . . ?
C6 N2 C10 C9 0.0(5) . . . . ?
C6 N2 C10 C11 179.8(3) . . . . ?
C8 C9 C10 N2 0.8(6) . . . . ?
C8 C9 C10 C11 -178.9(3) . . . . ?
N2 C10 C11 C12 -9.5(5) . . . . ?
C9 C10 C11 C12 170.3(3) . . . . ?
N2 C10 C11 C15 171.8(4) . . . . ?
C9 C10 C11 C15 -8.4(6) . . . . ?
C12 C11 C15 C14 1.5(6) . . . . ?
C10 C11 C15 C14 -179.8(4) . . . . ?
C13 N3 C14 C15 1.2(6) . . . . ?
Cd1 N3 C14 C15 177.5(4) 1_565 . . . ?
C11 C15 C14 N3 -2.6(7) . . . . ?
C14 N3 C13 C12 1.1(6) . . . . ?
Cd1 N3 C13 C12 -175.2(3) 1_565 . . . ?
N3 C13 C12 C11 -2.0(6) . . . . ?
C15 C11 C12 C13 0.6(6) . . . . ?
C10 C11 C12 C13 -178.1(3) . . . . ?
C7 C8 C16 C21 -48.8(5) . . . . ?
C9 C8 C16 C21 127.6(4) . . . . ?
C7 C8 C16 C17 136.0(4) . . . . ?
C9 C8 C16 C17 -47.6(5) . . . . ?
C17 C16 C21 C20 3.2(6) . . . . ?
C8 C16 C21 C20 -172.2(4) . . . . ?
C16 C21 C20 C19 -0.3(6) . . . . ?
C21 C20 C19 C18 -3.7(6) . . . . ?
C21 C20 C19 S2 169.2(3) . . . . ?
O4 S2 C19 C18 -147.0(3) . . . . ?
O5 S2 C19 C18 -21.6(4) . . . . ?
O6 S2 C19 C18 97.0(3) . . . . ?
O4 S2 C19 C20 40.0(4) . . . . ?
O5 S2 C19 C20 165.3(3) . . . . ?
O6 S2 C19 C20 -76.0(4) . . . . ?
C20 C19 C18 C17 4.6(6) . . . . ?
S2 C19 C18 C17 -168.6(3) . . . . ?
C19 C18 C17 C16 -1.5(6) . . . . ?
C19 C18 C17 S1 178.1(3) . . . . ?
C21 C16 C17 C18 -2.4(5) . . . . ?
C8 C16 C17 C18 172.8(3) . . . . ?
C21 C16 C17 S1 178.1(3) . . . . ?
C8 C16 C17 S1 -6.7(5) . . . . ?
O1 S1 C17 C18 145.9(3) . . . . ?
O2 S1 C17 C18 -92.0(3) . . . . ?
O3 S1 C17 C18 24.8(3) . . . . ?
O1 S1 C17 C16 -34.6(4) . . . . ?
O2 S1 C17 C16 87.5(3) . . . . ?
O3 S1 C17 C16 -155.7(3) . . . . ?
N1 C2 C1 C5 -0.5(8) . . . . ?
C4 C5 C1 C2 -1.1(6) . . . . ?
C6 C5 C1 C2 176.7(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.098
####################################################################### 
# 
# 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_Ag1
_database_code_depnum_ccdc_archive 'CCDC 1058699'
_audit_update_record             
;
2015-06-08 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H13 Ag N3 O6 S2, 30(H2O)'
_chemical_formula_sum            'C21 H73 Ag N3 O36 S2'
_chemical_formula_weight         1115.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   36.038(12)
_cell_length_b                   19.963(7)
_cell_length_c                   8.853(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.622(6)
_cell_angle_gamma                90.00
_cell_volume                     6338(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    845
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      14.33

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4696
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7685
_exptl_absorpt_correction_T_max  0.8014
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15863
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_sigmaI/netI    0.1654
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5589
_reflns_number_gt                1684
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.
The following restraints were used:
ISOR 0.02 0.02 $O $S
simu 0.02 0.02 $O $S  
;

_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)+(0.1000P)²+60.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5589
_refine_ls_number_parameters     328
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.2738
_refine_ls_R_factor_gt           0.1036
_refine_ls_wR_factor_ref         0.3455
_refine_ls_wR_factor_gt          0.2613
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.120
_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
Ag1 Ag 0.0000 0.0000 -0.5000 0.1126(9) Uani 1 2 d S . .
Ag2 Ag 0.2500 -0.2500 0.5000 0.1195(9) Uani 1 2 d S . .
S1 S 0.2057(3) 0.3996(4) 0.5263(13) 0.185(3) Uani 1 1 d U . .
S2 S 0.0912(2) 0.2320(3) 0.3587(10) 0.141(2) Uani 1 1 d U . .
N2 N 0.1431(3) 0.0076(6) 0.1048(14) 0.071(3) Uani 1 1 d . . .
C10 C 0.1678(4) 0.0155(7) 0.2244(18) 0.070(4) Uani 1 1 d . . .
N1 N 0.0414(3) 0.0231(8) -0.3233(16) 0.087(4) Uani 1 1 d . . .
C3 C 0.0960(4) 0.0499(8) -0.0818(19) 0.075(4) Uani 1 1 d . . .
N3 N 0.2215(4) -0.1633(6) 0.4041(16) 0.094(4) Uani 1 1 d . . .
C6 C 0.1245(4) 0.0633(8) 0.0482(17) 0.072(4) Uani 1 1 d . . .
C4 C 0.0855(4) -0.0140(7) -0.1239(18) 0.074(4) Uani 1 1 d . . .
H4A H 0.0969 -0.0504 -0.0730 0.088 Uiso 1 1 calc R . .
C11 C 0.1870(4) -0.0451(7) 0.2865(17) 0.071(4) Uani 1 1 d . . .
C12 C 0.2153(5) -0.0438(7) 0.4031(18) 0.084(5) Uani 1 1 d . . .
H12A H 0.2232 -0.0032 0.4468 0.101 Uiso 1 1 calc R . .
C16 C 0.1659(6) 0.2014(7) 0.3078(16) 0.080(5) Uani 1 1 d . . .
C15 C 0.1761(4) -0.1074(7) 0.2320(17) 0.082(4) Uani 1 1 d . . .
H15A H 0.1565 -0.1115 0.1558 0.098 Uiso 1 1 calc R . .
C8 C 0.1560(5) 0.1343(7) 0.2364(17) 0.075(4) Uani 1 1 d . . .
C7 C 0.1311(5) 0.1263(7) 0.1103(18) 0.079(4) Uani 1 1 d . . .
H7A H 0.1186 0.1633 0.0664 0.095 Uiso 1 1 calc R . .
C20 C 0.2135(6) 0.2818(9) 0.376(2) 0.108(6) Uani 1 1 d . . .
H20A H 0.2382 0.2950 0.3749 0.129 Uiso 1 1 calc R . .
C5 C 0.0586(5) -0.0241(8) -0.239(2) 0.078(4) Uani 1 1 d . . .
H5A H 0.0517 -0.0682 -0.2609 0.094 Uiso 1 1 calc R . .
C19 C 0.1902(7) 0.3229(8) 0.435(2) 0.099(6) Uani 1 1 d . . .
C2 C 0.0790(5) 0.1012(8) -0.162(2) 0.088(5) Uani 1 1 d . . .
H2A H 0.0854 0.1452 -0.1363 0.106 Uiso 1 1 calc R . .
C14 C 0.1944(5) -0.1642(8) 0.291(2) 0.095(5) Uani 1 1 d . . .
H14A H 0.1872 -0.2055 0.2497 0.113 Uiso 1 1 calc R . .
O3 O 0.0866(5) 0.1699(8) 0.415(2) 0.177(5) Uani 1 1 d U . .
C17 C 0.1401(5) 0.2453(8) 0.3604(18) 0.087(5) Uani 1 1 d . . .
C9 C 0.1749(4) 0.0794(7) 0.2980(17) 0.079(4) Uani 1 1 d . . .
H9 H 0.1918 0.0833 0.3841 0.095 Uiso 1 1 calc R . .
C1 C 0.0522(5) 0.0883(9) -0.280(2) 0.102(6) Uani 1 1 d . . .
H1A H 0.0410 0.1243 -0.3331 0.122 Uiso 1 1 calc R . .
C18 C 0.1542(7) 0.3068(7) 0.427(2) 0.116(7) Uani 1 1 d . . .
H18A H 0.1376 0.3365 0.4653 0.139 Uiso 1 1 calc R . .
C21 C 0.2031(6) 0.2200(8) 0.3145(18) 0.097(5) Uani 1 1 d . . .
H21A H 0.2207 0.1916 0.2785 0.117 Uiso 1 1 calc R . .
C13 C 0.2318(5) -0.1029(8) 0.4549(18) 0.093(5) Uani 1 1 d . . .
H13A H 0.2516 -0.1003 0.5307 0.112 Uiso 1 1 calc R . .
O2 O 0.0766(5) 0.2343(9) 0.203(2) 0.183(6) Uani 1 1 d U . .
O1 O 0.0770(4) 0.2832(8) 0.445(2) 0.176(5) Uani 1 1 d U . .
O6 O 0.1796(6) 0.4451(9) 0.497(3) 0.230(7) Uani 1 1 d U . .
O5 O 0.2205(6) 0.3852(9) 0.666(3) 0.217(7) Uani 1 1 d U . .
O4 O 0.2397(7) 0.4162(10) 0.461(3) 0.246(8) Uani 1 1 d U . .
O1W O 0.1779(6) 0.4398(9) 0.121(2) 0.218(8) Uani 1 1 d U . .
O2W O 0.0055(6) 0.1568(11) 0.076(2) 0.231(8) Uani 1 1 d U . .
O3W O 0.1784(7) 0.3292(11) 0.910(3) 0.272(10) Uani 1 1 d U . .


_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 2.103(13) . ?
Ag1 N1 2.103(13) 5_554 ?
Ag2 N3 2.144(13) . ?
Ag2 N3 2.144(13) 7_546 ?
S1 O6 1.31(2) . ?
S1 O5 1.33(2) . ?
S1 O4 1.44(2) . ?
S1 C19 1.792(17) . ?
S2 O3 1.352(16) . ?
S2 O1 1.403(14) . ?
S2 O2 1.428(19) . ?
S2 C17 1.780(18) . ?
N2 C10 1.324(17) . ?
N2 C6 1.367(16) . ?
C10 C9 1.444(18) . ?
C10 C11 1.473(19) . ?
N1 C5 1.320(18) . ?
N1 C1 1.40(2) . ?
C3 C2 1.36(2) . ?
C3 C4 1.371(19) . ?
C3 C6 1.49(2) . ?
N3 C14 1.327(19) . ?
N3 C13 1.326(18) . ?
C6 C7 1.382(19) . ?
C4 C5 1.351(19) . ?
C4 H4A 0.9300 . ?
C11 C12 1.378(19) . ?
C11 C15 1.378(18) . ?
C12 C13 1.380(19) . ?
C12 H12A 0.9300 . ?
C16 C21 1.39(2) . ?
C16 C17 1.39(2) . ?
C16 C8 1.508(19) . ?
C15 C14 1.39(2) . ?
C15 H15A 0.9300 . ?
C8 C7 1.372(19) . ?
C8 C9 1.376(19) . ?
C7 H7A 0.9300 . ?
C20 C19 1.32(2) . ?
C20 C21 1.38(2) . ?
C20 H20A 0.9300 . ?
C5 H5A 0.9300 . ?
C19 C18 1.33(2) . ?
C2 C1 1.38(2) . ?
C2 H2A 0.9300 . ?
C14 H14A 0.9300 . ?
C17 C18 1.43(2) . ?
C9 H9 0.9300 . ?
C1 H1A 0.9300 . ?
C18 H18A 0.9300 . ?
C21 H21A 0.9300 . ?
C13 H13A 0.9300 . ?

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 180.0(5) . 5_554 ?
N3 Ag2 N3 180.0(8) . 7_546 ?
O6 S1 O5 122.9(17) . . ?
O6 S1 O4 112.4(17) . . ?
O5 S1 O4 98.3(15) . . ?
O6 S1 C19 108.6(12) . . ?
O5 S1 C19 108.1(12) . . ?
O4 S1 C19 104.8(13) . . ?
O3 S2 O1 113.7(11) . . ?
O3 S2 O2 109.7(11) . . ?
O1 S2 O2 112.5(12) . . ?
O3 S2 C17 107.0(10) . . ?
O1 S2 C17 107.6(9) . . ?
O2 S2 C17 105.9(9) . . ?
C10 N2 C6 117.6(12) . . ?
N2 C10 C9 122.8(13) . . ?
N2 C10 C11 117.1(13) . . ?
C9 C10 C11 120.0(15) . . ?
C5 N1 C1 113.8(15) . . ?
C5 N1 Ag1 121.6(13) . . ?
C1 N1 Ag1 124.5(13) . . ?
C2 C3 C4 117.4(16) . . ?
C2 C3 C6 120.6(15) . . ?
C4 C3 C6 122.0(15) . . ?
C14 N3 C13 115.4(14) . . ?
C14 N3 Ag2 125.1(11) . . ?
C13 N3 Ag2 119.5(13) . . ?
N2 C6 C7 122.3(15) . . ?
N2 C6 C3 114.3(14) . . ?
C7 C6 C3 123.3(14) . . ?
C5 C4 C3 120.3(15) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
C12 C11 C15 116.4(14) . . ?
C12 C11 C10 123.4(13) . . ?
C15 C11 C10 120.2(15) . . ?
C11 C12 C13 119.8(14) . . ?
C11 C12 H12A 120.1 . . ?
C13 C12 H12A 120.1 . . ?
C21 C16 C17 119.5(14) . . ?
C21 C16 C8 116.3(16) . . ?
C17 C16 C8 124.2(17) . . ?
C14 C15 C11 119.7(15) . . ?
C14 C15 H15A 120.2 . . ?
C11 C15 H15A 120.2 . . ?
C7 C8 C9 119.2(14) . . ?
C7 C8 C16 123.6(14) . . ?
C9 C8 C16 117.0(15) . . ?
C8 C7 C6 120.2(14) . . ?
C8 C7 H7A 119.9 . . ?
C6 C7 H7A 119.9 . . ?
C19 C20 C21 123.6(19) . . ?
C19 C20 H20A 118.2 . . ?
C21 C20 H20A 118.2 . . ?
N1 C5 C4 125.6(14) . . ?
N1 C5 H5A 117.2 . . ?
C4 C5 H5A 117.2 . . ?
C20 C19 C18 118.6(17) . . ?
C20 C19 S1 121.9(18) . . ?
C18 C19 S1 119.4(16) . . ?
C3 C2 C1 120.3(16) . . ?
C3 C2 H2A 119.9 . . ?
C1 C2 H2A 119.9 . . ?
N3 C14 C15 124.2(15) . . ?
N3 C14 H14A 117.9 . . ?
C15 C14 H14A 117.9 . . ?
C16 C17 C18 117.1(17) . . ?
C16 C17 S2 126.7(13) . . ?
C18 C17 S2 116.2(15) . . ?
C8 C9 C10 117.8(15) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 H9 121.1 . . ?
C2 C1 N1 122.6(16) . . ?
C2 C1 H1A 118.7 . . ?
N1 C1 H1A 118.7 . . ?
C19 C18 C17 122.4(18) . . ?
C19 C18 H18A 118.8 . . ?
C17 C18 H18A 118.8 . . ?
C16 C21 C20 118.6(18) . . ?
C16 C21 H21A 120.7 . . ?
C20 C21 H21A 120.7 . . ?
N3 C13 C12 124.5(16) . . ?
N3 C13 H13A 117.7 . . ?
C12 C13 H13A 117.7 . . ?

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
C6 N2 C10 C9 2(2) . . . . ?
C6 N2 C10 C11 178.7(12) . . . . ?
N1 Ag1 N1 C5 70.8(9) 5_554 . . . ?
N1 Ag1 N1 C1 -106.7(15) 5_554 . . . ?
N3 Ag2 N3 C14 158(100) 7_546 . . . ?
N3 Ag2 N3 C13 -20(100) 7_546 . . . ?
C10 N2 C6 C7 1(2) . . . . ?
C10 N2 C6 C3 -177.4(12) . . . . ?
C2 C3 C6 N2 -171.4(13) . . . . ?
C4 C3 C6 N2 10(2) . . . . ?
C2 C3 C6 C7 10(2) . . . . ?
C4 C3 C6 C7 -168.4(14) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
C6 C3 C4 C5 177.7(13) . . . . ?
N2 C10 C11 C12 175.0(13) . . . . ?
C9 C10 C11 C12 -8(2) . . . . ?
N2 C10 C11 C15 -7(2) . . . . ?
C9 C10 C11 C15 169.7(14) . . . . ?
C15 C11 C12 C13 2(2) . . . . ?
C10 C11 C12 C13 179.9(14) . . . . ?
C12 C11 C15 C14 -2(2) . . . . ?
C10 C11 C15 C14 -180.0(14) . . . . ?
C21 C16 C8 C7 -120.0(18) . . . . ?
C17 C16 C8 C7 58(2) . . . . ?
C21 C16 C8 C9 56.2(19) . . . . ?
C17 C16 C8 C9 -126.2(16) . . . . ?
C9 C8 C7 C6 2(2) . . . . ?
C16 C8 C7 C6 177.7(15) . . . . ?
N2 C6 C7 C8 -2(2) . . . . ?
C3 C6 C7 C8 175.6(13) . . . . ?
C1 N1 C5 C4 -2(2) . . . . ?
Ag1 N1 C5 C4 179.8(11) . . . . ?
C3 C4 C5 N1 3(2) . . . . ?
C21 C20 C19 C18 -5(3) . . . . ?
C21 C20 C19 S1 175.2(14) . . . . ?
O6 S1 C19 C20 144(2) . . . . ?
O5 S1 C19 C20 -80(2) . . . . ?
O4 S1 C19 C20 24(2) . . . . ?
O6 S1 C19 C18 -35(2) . . . . ?
O5 S1 C19 C18 100(2) . . . . ?
O4 S1 C19 C18 -156(2) . . . . ?
C4 C3 C2 C1 0(2) . . . . ?
C6 C3 C2 C1 -178.9(14) . . . . ?
C13 N3 C14 C15 -3(3) . . . . ?
Ag2 N3 C14 C15 179.3(12) . . . . ?
C11 C15 C14 N3 3(3) . . . . ?
C21 C16 C17 C18 -3(2) . . . . ?
C8 C16 C17 C18 179.3(14) . . . . ?
C21 C16 C17 S2 178.7(12) . . . . ?
C8 C16 C17 S2 1(2) . . . . ?
O3 S2 C17 C16 47.7(17) . . . . ?
O1 S2 C17 C16 170.2(15) . . . . ?
O2 S2 C17 C16 -69.3(16) . . . . ?
O3 S2 C17 C18 -130.5(14) . . . . ?
O1 S2 C17 C18 -8.0(17) . . . . ?
O2 S2 C17 C18 112.5(14) . . . . ?
C7 C8 C9 C10 1(2) . . . . ?
C16 C8 C9 C10 -175.7(13) . . . . ?
N2 C10 C9 C8 -2(2) . . . . ?
C11 C10 C9 C8 -179.4(13) . . . . ?
C3 C2 C1 N1 0(3) . . . . ?
C5 N1 C1 C2 1(2) . . . . ?
Ag1 N1 C1 C2 178.8(12) . . . . ?
C20 C19 C18 C17 2(3) . . . . ?
S1 C19 C18 C17 -177.9(13) . . . . ?
C16 C17 C18 C19 2(3) . . . . ?
S2 C17 C18 C19 180.0(17) . . . . ?
C17 C16 C21 C20 1(2) . . . . ?
C8 C16 C21 C20 178.6(14) . . . . ?
C19 C20 C21 C16 3(3) . . . . ?
C14 N3 C13 C12 3(3) . . . . ?
Ag2 N3 C13 C12 -179.2(13) . . . . ?
C11 C12 C13 N3 -3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.317

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 0.000 0.500 -0.032 927 1070 ' '
2 0.500 0.000 0.006 927 1071 ' '
_platon_squeeze_details          
;
The disordered solvent that was removed from the asymmetric unit 
is about 27 water molecules
;
####################################################################### 
# 
# 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_Ag2
_database_code_depnum_ccdc_archive 'CCDC 1058700'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H22 Ag N3 O10 S2'
_chemical_formula_weight         648.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclnic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   7.380(5)
_cell_length_b                   20.931(13)
_cell_length_c                   16.474(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.80(2)
_cell_angle_gamma                90.00
_cell_volume                     2379(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    524
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      18.67

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7363
_exptl_absorpt_correction_T_max  0.7960
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11966
_diffrn_reflns_av_R_equivalents  0.1294
_diffrn_reflns_av_sigmaI/netI    0.1866
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4189
_reflns_number_gt                1812
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0789P)²+0.8387P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4189
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1779
_refine_ls_R_factor_gt           0.0870
_refine_ls_wR_factor_ref         0.2569
_refine_ls_wR_factor_gt          0.1999
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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
Ag1 Ag 0.70980(15) 0.33042(5) 0.73775(6) 0.0733(5) Uani 1 1 d . . .
S1 S 1.7262(5) 0.33529(13) 1.25261(19) 0.0582(9) Uani 1 1 d . . .
S2 S 1.9030(4) 0.38610(13) 1.59334(17) 0.0496(8) Uani 1 1 d . . .
O3 O 1.8463(13) 0.2842(3) 1.3000(5) 0.078(3) Uani 1 1 d . . .
O2 O 1.5310(14) 0.3132(4) 1.2028(6) 0.094(3) Uani 1 1 d . . .
O1 O 1.8130(14) 0.3712(4) 1.2034(5) 0.076(3) Uani 1 1 d . . .
O6 O 1.8713(15) 0.4338(4) 1.6475(5) 0.094(3) Uani 1 1 d . . .
O5 O 1.8216(11) 0.3256(3) 1.6025(5) 0.060(2) Uani 1 1 d . . .
O4 O 2.1051(12) 0.3810(4) 1.6034(5) 0.082(3) Uani 1 1 d . . .
O1W O 0.4213(11) 0.3011(3) 0.6457(5) 0.067(2) Uani 1 1 d . . .
H1WA H 0.3613 0.2727 0.6085 0.101 Uiso 1 1 d R . .
H1WB H 0.3485 0.3338 0.6362 0.101 Uiso 1 1 d R . .
N1 N 1.5983(13) 0.7526(4) 1.0615(6) 0.049(2) Uani 1 1 d . . .
H1A H 1.6177 0.7914 1.0492 0.059 Uiso 1 1 calc R . .
N2 N 1.3651(11) 0.5328(4) 1.0590(5) 0.038(2) Uani 1 1 d . . .
N3 N 0.9111(12) 0.3785(4) 0.8530(5) 0.043(2) Uani 1 1 d . . .
C1 C 1.4392(14) 0.6550(5) 1.0182(7) 0.049(3) Uani 1 1 d . . .
H1 H 1.3549 0.6292 0.9753 0.058 Uiso 1 1 calc R . .
C2 C 1.4755(17) 0.7155(5) 0.9989(7) 0.056(3) Uani 1 1 d . . .
H2 H 1.4162 0.7314 0.9430 0.067 Uiso 1 1 calc R . .
C3 C 1.6896(18) 0.7312(6) 1.1411(8) 0.065(4) Uani 1 1 d . . .
H3 H 1.7758 0.7582 1.1814 0.078 Uiso 1 1 calc R . .
C4 C 1.6620(15) 0.6706(4) 1.1665(7) 0.046(3) Uani 1 1 d . . .
H4 H 1.7276 0.6563 1.2227 0.055 Uiso 1 1 calc R . .
C5 C 1.5294(14) 0.6309(4) 1.1033(6) 0.032(2) Uani 1 1 d . . .
C6 C 1.4908(13) 0.5646(4) 1.1246(6) 0.035(2) Uani 1 1 d . . .
C7 C 1.5768(14) 0.5391(4) 1.2064(7) 0.040(3) Uani 1 1 d . . .
H7 H 1.6661 0.5629 1.2503 0.048 Uiso 1 1 calc R . .
C8 C 1.5282(13) 0.4770(4) 1.2227(6) 0.036(2) Uani 1 1 d . . .
C9 C 1.3886(14) 0.4457(4) 1.1543(6) 0.040(3) Uani 1 1 d . . .
H9 H 1.3447 0.4057 1.1635 0.048 Uiso 1 1 calc R . .
C10 C 1.3153(15) 0.4727(4) 1.0740(6) 0.039(3) Uani 1 1 d . . .
C11 C 1.1741(14) 0.4394(4) 0.9985(6) 0.033(2) Uani 1 1 d . . .
C12 C 1.1118(15) 0.3784(5) 1.0021(6) 0.044(3) Uani 1 1 d . . .
H12 H 1.1583 0.3559 1.0542 0.053 Uiso 1 1 calc R . .
C13 C 0.9815(16) 0.3497(5) 0.9301(7) 0.047(3) Uani 1 1 d . . .
H13 H 0.9406 0.3084 0.9352 0.056 Uiso 1 1 calc R . .
C14 C 0.9688(16) 0.4381(5) 0.8497(7) 0.049(3) Uani 1 1 d . . .
H14 H 0.9178 0.4599 0.7973 0.059 Uiso 1 1 calc R . .
C15 C 1.0970(13) 0.4690(5) 0.9178(6) 0.036(2) Uani 1 1 d . . .
H15 H 1.1342 0.5105 0.9109 0.043 Uiso 1 1 calc R . .
C16 C 1.6156(14) 0.4503(5) 1.3115(6) 0.040(3) Uani 1 1 d . . .
C17 C 1.7067(14) 0.3890(4) 1.3332(6) 0.038(3) Uani 1 1 d . . .
C18 C 1.7847(15) 0.3712(5) 1.4183(7) 0.044(3) Uani 1 1 d . . .
H18 H 1.8391 0.3307 1.4312 0.053 Uiso 1 1 calc R . .
C19 C 1.7869(14) 0.4099(5) 1.4854(6) 0.040(3) Uani 1 1 d . . .
C20 C 1.6959(14) 0.4683(5) 1.4643(6) 0.042(3) Uani 1 1 d . . .
H20 H 1.6891 0.4948 1.5084 0.051 Uiso 1 1 calc R . .
C21 C 1.6156(14) 0.4881(5) 1.3800(6) 0.042(3) Uani 1 1 d . . .
H21 H 1.5590 0.5284 1.3685 0.050 Uiso 1 1 calc R . .
O4W O 0.2958(13) 0.3715(3) 0.4643(5) 0.073(3) Uani 1 1 d . . .
O3W O 0.1398(14) 0.4379(4) 0.3140(6) 0.089(3) Uani 1 1 d . . .
O2W O 0.0719(14) 0.2814(4) 0.1527(7) 0.098(3) Uani 1 1 d . . .


_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 N3 2.196(8) . ?
Ag1 O1W 2.218(7) . ?
S1 O1 1.415(10) . ?
S1 O3 1.431(8) . ?
S1 O2 1.457(9) . ?
S1 C17 1.785(10) . ?
S2 O6 1.412(9) . ?
S2 O5 1.433(7) . ?
S2 O4 1.445(9) . ?
S2 C19 1.749(10) . ?
O1W H1WA 0.8553 . ?
O1W H1WB 0.8496 . ?
N1 C3 1.321(14) . ?
N1 C2 1.351(13) . ?
N1 H1A 0.8600 . ?
N2 C6 1.326(11) . ?
N2 C10 1.358(12) . ?
N3 C14 1.327(12) . ?
N3 C13 1.332(12) . ?
C1 C2 1.355(14) . ?
C1 C5 1.415(13) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.373(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.417(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.482(13) . ?
C6 C7 1.378(13) . ?
C7 C8 1.400(13) . ?
C7 H7 0.9300 . ?
C8 C9 1.392(12) . ?
C8 C16 1.482(12) . ?
C9 C10 1.361(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.483(12) . ?
C11 C12 1.366(12) . ?
C11 C15 1.391(12) . ?
C12 C13 1.372(13) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.349(13) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C21 1.378(13) . ?
C16 C17 1.435(13) . ?
C17 C18 1.364(13) . ?
C18 C19 1.366(14) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(13) . ?
C20 C21 1.366(13) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?

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
N3 Ag1 O1W 155.3(3) . . ?
O1 S1 O3 113.0(6) . . ?
O1 S1 O2 113.8(6) . . ?
O3 S1 O2 111.6(6) . . ?
O1 S1 C17 105.3(5) . . ?
O3 S1 C17 105.2(5) . . ?
O2 S1 C17 107.1(5) . . ?
O6 S2 O5 112.9(6) . . ?
O6 S2 O4 112.0(6) . . ?
O5 S2 O4 112.2(5) . . ?
O6 S2 C19 108.1(5) . . ?
O5 S2 C19 106.6(4) . . ?
O4 S2 C19 104.5(5) . . ?
Ag1 O1W H1WA 144.0 . . ?
Ag1 O1W H1WB 107.0 . . ?
H1WA O1W H1WB 107.2 . . ?
C3 N1 C2 121.9(9) . . ?
C3 N1 H1A 119.0 . . ?
C2 N1 H1A 119.0 . . ?
C6 N2 C10 118.3(8) . . ?
C14 N3 C13 116.3(9) . . ?
C14 N3 Ag1 121.6(7) . . ?
C13 N3 Ag1 122.2(7) . . ?
C2 C1 C5 120.2(10) . . ?
C2 C1 H1 119.9 . . ?
C5 C1 H1 119.9 . . ?
N1 C2 C1 119.6(10) . . ?
N1 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
N1 C3 C4 122.5(11) . . ?
N1 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C5 117.2(10) . . ?
C3 C4 H4 121.4 . . ?
C5 C4 H4 121.4 . . ?
C1 C5 C4 118.5(9) . . ?
C1 C5 C6 120.4(9) . . ?
C4 C5 C6 121.1(9) . . ?
N2 C6 C7 123.2(9) . . ?
N2 C6 C5 114.5(8) . . ?
C7 C6 C5 122.3(9) . . ?
C6 C7 C8 119.2(9) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C9 C8 C7 116.6(9) . . ?
C9 C8 C16 124.0(9) . . ?
C7 C8 C16 119.2(9) . . ?
C10 C9 C8 121.1(9) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
N2 C10 C9 121.4(9) . . ?
N2 C10 C11 116.0(8) . . ?
C9 C10 C11 122.6(9) . . ?
C12 C11 C15 115.4(9) . . ?
C12 C11 C10 123.3(8) . . ?
C15 C11 C10 121.3(8) . . ?
C13 C12 C11 120.9(9) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
N3 C13 C12 122.9(10) . . ?
N3 C13 H13 118.5 . . ?
C12 C13 H13 118.5 . . ?
N3 C14 C15 123.8(10) . . ?
N3 C14 H14 118.1 . . ?
C15 C14 H14 118.1 . . ?
C14 C15 C11 120.7(10) . . ?
C14 C15 H15 119.7 . . ?
C11 C15 H15 119.7 . . ?
C21 C16 C17 116.4(8) . . ?
C21 C16 C8 117.8(9) . . ?
C17 C16 C8 125.8(9) . . ?
C18 C17 C16 119.4(9) . . ?
C18 C17 S1 118.5(8) . . ?
C16 C17 S1 122.1(7) . . ?
C17 C18 C19 123.3(9) . . ?
C17 C18 H18 118.3 . . ?
C19 C18 H18 118.3 . . ?
C20 C19 C18 117.2(9) . . ?
C20 C19 S2 121.8(8) . . ?
C18 C19 S2 121.0(8) . . ?
C21 C20 C19 121.4(9) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C20 C21 C16 122.2(9) . . ?
C20 C21 H21 118.9 . . ?
C16 C21 H21 118.9 . . ?

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
O1W Ag1 N3 C14 -90.2(11) . . . . ?
O1W Ag1 N3 C13 89.6(10) . . . . ?
C3 N1 C2 C1 2.0(18) . . . . ?
C5 C1 C2 N1 0.1(17) . . . . ?
C2 N1 C3 C4 -2.0(19) . . . . ?
N1 C3 C4 C5 -0.1(18) . . . . ?
C2 C1 C5 C4 -2.0(15) . . . . ?
C2 C1 C5 C6 -179.7(10) . . . . ?
C3 C4 C5 C1 2.0(15) . . . . ?
C3 C4 C5 C6 179.7(10) . . . . ?
C10 N2 C6 C7 1.6(15) . . . . ?
C10 N2 C6 C5 -177.2(9) . . . . ?
C1 C5 C6 N2 -1.7(13) . . . . ?
C4 C5 C6 N2 -179.3(9) . . . . ?
C1 C5 C6 C7 179.4(10) . . . . ?
C4 C5 C6 C7 1.8(15) . . . . ?
N2 C6 C7 C8 -1.2(15) . . . . ?
C5 C6 C7 C8 177.6(9) . . . . ?
C6 C7 C8 C9 -2.1(15) . . . . ?
C6 C7 C8 C16 -178.0(9) . . . . ?
C7 C8 C9 C10 4.9(15) . . . . ?
C16 C8 C9 C10 -179.4(10) . . . . ?
C6 N2 C10 C9 1.2(15) . . . . ?
C6 N2 C10 C11 180.0(9) . . . . ?
C8 C9 C10 N2 -4.6(16) . . . . ?
C8 C9 C10 C11 176.7(9) . . . . ?
N2 C10 C11 C12 178.7(10) . . . . ?
C9 C10 C11 C12 -2.6(16) . . . . ?
N2 C10 C11 C15 -0.8(14) . . . . ?
C9 C10 C11 C15 177.9(10) . . . . ?
C15 C11 C12 C13 -0.2(16) . . . . ?
C10 C11 C12 C13 -179.7(10) . . . . ?
C14 N3 C13 C12 -2.2(15) . . . . ?
Ag1 N3 C13 C12 178.0(8) . . . . ?
C11 C12 C13 N3 1.1(17) . . . . ?
C13 N3 C14 C15 2.5(16) . . . . ?
Ag1 N3 C14 C15 -177.7(8) . . . . ?
N3 C14 C15 C11 -1.7(17) . . . . ?
C12 C11 C15 C14 0.5(15) . . . . ?
C10 C11 C15 C14 180.0(10) . . . . ?
C9 C8 C16 C21 -128.6(11) . . . . ?
C7 C8 C16 C21 46.9(14) . . . . ?
C9 C8 C16 C17 53.5(15) . . . . ?
C7 C8 C16 C17 -131.0(11) . . . . ?
C21 C16 C17 C18 0.8(15) . . . . ?
C8 C16 C17 C18 178.7(10) . . . . ?
C21 C16 C17 S1 -178.0(8) . . . . ?
C8 C16 C17 S1 -0.1(15) . . . . ?
O1 S1 C17 C18 -125.8(9) . . . . ?
O3 S1 C17 C18 -6.2(10) . . . . ?
O2 S1 C17 C18 112.7(9) . . . . ?
O1 S1 C17 C16 53.0(10) . . . . ?
O3 S1 C17 C16 172.6(9) . . . . ?
O2 S1 C17 C16 -68.6(10) . . . . ?
C16 C17 C18 C19 -2.3(17) . . . . ?
S1 C17 C18 C19 176.5(9) . . . . ?
C17 C18 C19 C20 3.5(16) . . . . ?
C17 C18 C19 S2 -175.9(8) . . . . ?
O6 S2 C19 C20 4.1(11) . . . . ?
O5 S2 C19 C20 125.7(9) . . . . ?
O4 S2 C19 C20 -115.4(9) . . . . ?
O6 S2 C19 C18 -176.6(9) . . . . ?
O5 S2 C19 C18 -55.0(10) . . . . ?
O4 S2 C19 C18 63.9(10) . . . . ?
C18 C19 C20 C21 -3.3(15) . . . . ?
S2 C19 C20 C21 176.1(8) . . . . ?
C19 C20 C21 C16 2.0(16) . . . . ?
C17 C16 C21 C20 -0.6(15) . . . . ?
C8 C16 C21 C20 -178.7(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.139
####################################################################### 
# 
# 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_Ag3
_database_code_depnum_ccdc_archive 'CCDC 1058701'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H13 Ag2 N3 O6 S2'
_chemical_formula_weight         683.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.538(3)
_cell_length_b                   10.962(5)
_cell_length_c                   12.083(5)
_cell_angle_alpha                87.664(7)
_cell_angle_beta                 85.159(8)
_cell_angle_gamma                81.961(8)
_cell_volume                     1115.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    832
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      19.67

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             668
_exptl_absorpt_coefficient_mu    1.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6060
_exptl_absorpt_correction_T_max  0.6919
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5693
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3898
_reflns_number_gt                2380
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1000P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3898
_refine_ls_number_parameters     322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0638
_refine_ls_wR_factor_ref         0.2000
_refine_ls_wR_factor_gt          0.1680
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
Ag1 Ag 1.5000 1.5000 1.0000 0.0678(4) Uani 1 2 d S . .
Ag2 Ag 1.33084(10) 0.42184(7) 1.45015(7) 0.0587(3) Uani 1 1 d . . .
Ag3 Ag 0.4529(2) 0.91191(17) 0.55167(18) 0.0752(6) Uani 0.50 1 d P . .
C1 C 1.3635(11) 1.1372(9) 1.0613(8) 0.044(2) Uani 1 1 d . . .
H1A H 1.3880 1.0750 1.1142 0.053 Uiso 1 1 calc R . .
C2 C 1.4135(12) 1.2488(10) 1.0683(8) 0.054(3) Uani 1 1 d . . .
H2A H 1.4697 1.2614 1.1286 0.064 Uiso 1 1 calc R . .
C3 C 1.3032(12) 1.3192(9) 0.9130(8) 0.051(3) Uani 1 1 d . . .
H3A H 1.2834 1.3826 0.8604 0.061 Uiso 1 1 calc R . .
C4 C 1.2446(11) 1.2146(8) 0.8996(8) 0.044(2) Uani 1 1 d . . .
H4A H 1.1835 1.2077 0.8406 0.052 Uiso 1 1 calc R . .
C5 C 1.2748(10) 1.1174(8) 0.9734(7) 0.035(2) Uani 1 1 d . . .
C6 C 1.2233(10) 0.9942(8) 0.9623(7) 0.0338(19) Uani 1 1 d . . .
C7 C 1.1649(10) 0.9666(8) 0.8630(7) 0.037(2) Uani 1 1 d . . .
H7A H 1.1547 1.0258 0.8058 0.044 Uiso 1 1 calc R . .
C8 C 1.1229(10) 0.8525(8) 0.8501(7) 0.0330(19) Uani 1 1 d . . .
C9 C 1.1394(10) 0.7672(8) 0.9386(7) 0.0334(19) Uani 1 1 d . . .
H9A H 1.1141 0.6881 0.9325 0.040 Uiso 1 1 calc R . .
C10 C 1.1944(10) 0.8024(8) 1.0368(7) 0.034(2) Uani 1 1 d . . .
C11 C 1.2181(10) 0.7141(8) 1.1336(7) 0.036(2) Uani 1 1 d . . .
C12 C 1.1528(12) 0.6049(8) 1.1431(7) 0.046(2) Uani 1 1 d . . .
H12A H 1.0917 0.5838 1.0885 0.055 Uiso 1 1 calc R . .
C13 C 1.1799(12) 0.5282(9) 1.2346(8) 0.049(3) Uani 1 1 d . . .
H13A H 1.1318 0.4569 1.2421 0.059 Uiso 1 1 calc R . .
C14 C 1.3335(13) 0.6552(9) 1.3027(8) 0.054(3) Uani 1 1 d . . .
H14A H 1.3940 0.6731 1.3589 0.065 Uiso 1 1 calc R . .
C15 C 1.3141(12) 0.7391(9) 1.2142(8) 0.049(3) Uani 1 1 d . . .
H15A H 1.3639 0.8096 1.2093 0.059 Uiso 1 1 calc R . .
C16 C 1.0588(10) 0.8245(8) 0.7452(6) 0.0322(19) Uani 1 1 d . . .
C17 C 1.1272(10) 0.7423(8) 0.6681(7) 0.034(2) Uani 1 1 d . . .
C18 C 1.0560(10) 0.7307(9) 0.5693(7) 0.042(2) Uani 1 1 d . . .
H18A H 1.1036 0.6742 0.5172 0.050 Uiso 1 1 calc R . .
C19 C 0.9180(11) 0.8019(10) 0.5502(7) 0.046(2) Uani 1 1 d . A .
C20 C 0.8475(12) 0.8885(10) 0.6244(8) 0.057(3) Uani 1 1 d . . .
H20A H 0.7541 0.9390 0.6098 0.069 Uiso 1 1 calc R . .
C21 C 0.9202(12) 0.8987(10) 0.7224(8) 0.051(3) Uani 1 1 d . . .
H21A H 0.8740 0.9569 0.7735 0.062 Uiso 1 1 calc R . .
N1 N 1.3877(10) 1.3390(7) 0.9961(7) 0.047(2) Uani 1 1 d . . .
N2 N 1.2369(8) 0.9140(6) 1.0469(5) 0.0336(16) Uani 1 1 d . . .
N3 N 1.2709(9) 0.5511(7) 1.3120(6) 0.046(2) Uani 1 1 d . . .
S1 S 1.3202(3) 0.6581(2) 0.68237(19) 0.0429(6) Uani 1 1 d . . .
S2 S 0.8263(3) 0.7944(4) 0.4230(2) 0.0719(10) Uani 1 1 d . . .
O1 O 1.4211(8) 0.7525(6) 0.6889(6) 0.0548(18) Uani 1 1 d . . .
O2 O 1.3124(9) 0.5842(7) 0.7829(6) 0.068(2) Uani 1 1 d . . .
O3 O 1.3624(8) 0.5909(7) 0.5805(5) 0.062(2) Uani 1 1 d . . .
O4 O 0.9294(19) 0.742(3) 0.3475(12) 0.176(11) Uani 0.75 1 d P A 1
O4' O 0.903(4) 0.649(3) 0.383(3) 0.047(8) Uani 0.25 1 d P A 2
O5 O 0.6733(8) 0.7535(6) 0.4543(6) 0.059(2) Uani 1 1 d . . .
O6 O 0.7946(13) 0.9220(11) 0.3795(8) 0.128(5) Uani 1 1 d . A .


_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 2.127(7) . ?
Ag1 N1 2.127(7) 2_887 ?
Ag2 N3 2.192(7) . ?
Ag2 O5 2.205(7) 2_767 ?
Ag2 O3 2.537(6) 1_556 ?
Ag2 O3 2.599(7) 2_867 ?
Ag3 O1 2.387(7) 1_455 ?
Ag3 Ag3 2.451(4) 2_676 ?
C1 C2 1.359(13) . ?
C1 C5 1.396(11) . ?
C2 N1 1.299(12) . ?
C3 N1 1.327(12) . ?
C3 C4 1.334(13) . ?
C4 C5 1.372(12) . ?
C5 C6 1.492(11) . ?
C6 N2 1.323(10) . ?
C6 C7 1.397(11) . ?
C7 C8 1.367(12) . ?
C8 C9 1.394(11) . ?
C8 C16 1.482(11) . ?
C9 C10 1.400(11) . ?
C10 N2 1.337(11) . ?
C10 C11 1.496(11) . ?
C11 C15 1.385(12) . ?
C11 C12 1.387(12) . ?
C12 C13 1.377(12) . ?
C13 N3 1.319(12) . ?
C14 N3 1.322(12) . ?
C14 C15 1.387(13) . ?
C16 C17 1.361(12) . ?
C16 C21 1.380(13) . ?
C17 C18 1.402(11) . ?
C17 S1 1.790(9) . ?
C18 C19 1.351(13) . ?
C19 C20 1.373(14) . ?
C19 S2 1.793(9) . ?
C20 C21 1.398(13) . ?
S1 O2 1.434(7) . ?
S1 O1 1.445(7) . ?
S1 O3 1.454(6) . ?
S2 O4 1.306(17) . ?
S2 O5 1.455(7) . ?
S2 O6 1.470(11) . ?
S2 O4' 1.71(4) . ?
O1 Ag3 2.387(7) 1_655 ?
O3 Ag2 2.537(6) 1_554 ?
O3 Ag2 2.599(7) 2_867 ?
O5 Ag2 2.205(6) 2_767 ?

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 180.0 . 2_887 ?
N3 Ag2 O5 154.2(3) . 2_767 ?
N3 Ag2 O3 93.7(3) . 1_556 ?
O5 Ag2 O3 109.3(3) 2_767 1_556 ?
N3 Ag2 O3 97.6(3) . 2_867 ?
O5 Ag2 O3 96.8(3) 2_767 2_867 ?
O3 Ag2 O3 82.7(2) 1_556 2_867 ?
O1 Ag3 Ag3 162.3(2) 1_455 2_676 ?
C2 C1 C5 119.0(9) . . ?
N1 C2 C1 124.1(9) . . ?
N1 C3 C4 124.5(9) . . ?
C3 C4 C5 119.7(9) . . ?
C4 C5 C1 116.2(8) . . ?
C4 C5 C6 124.0(8) . . ?
C1 C5 C6 119.7(8) . . ?
N2 C6 C7 122.3(8) . . ?
N2 C6 C5 118.4(7) . . ?
C7 C6 C5 119.3(8) . . ?
C8 C7 C6 119.9(8) . . ?
C7 C8 C9 117.9(8) . . ?
C7 C8 C16 119.6(8) . . ?
C9 C8 C16 122.5(8) . . ?
C8 C9 C10 119.1(8) . . ?
N2 C10 C9 121.9(8) . . ?
N2 C10 C11 116.4(7) . . ?
C9 C10 C11 121.5(8) . . ?
C15 C11 C12 118.5(8) . . ?
C15 C11 C10 119.2(8) . . ?
C12 C11 C10 122.3(8) . . ?
C13 C12 C11 119.0(8) . . ?
N3 C13 C12 123.0(9) . . ?
N3 C14 C15 123.9(9) . . ?
C11 C15 C14 117.6(9) . . ?
C17 C16 C21 118.4(8) . . ?
C17 C16 C8 127.2(8) . . ?
C21 C16 C8 114.2(8) . . ?
C16 C17 C18 120.7(8) . . ?
C16 C17 S1 121.1(6) . . ?
C18 C17 S1 117.9(7) . . ?
C19 C18 C17 119.8(9) . . ?
C18 C19 C20 121.3(8) . . ?
C18 C19 S2 121.4(7) . . ?
C20 C19 S2 117.2(8) . . ?
C19 C20 C21 118.1(10) . . ?
C16 C21 C20 121.7(9) . . ?
C2 N1 C3 116.4(8) . . ?
C2 N1 Ag1 121.4(7) . . ?
C3 N1 Ag1 121.8(7) . . ?
C6 N2 C10 118.9(7) . . ?
C13 N3 C14 117.9(8) . . ?
C13 N3 Ag2 123.1(6) . . ?
C14 N3 Ag2 118.9(6) . . ?
O2 S1 O1 111.8(5) . . ?
O2 S1 O3 115.9(5) . . ?
O1 S1 O3 110.3(4) . . ?
O2 S1 C17 107.8(4) . . ?
O1 S1 C17 104.2(4) . . ?
O3 S1 C17 106.0(4) . . ?
O4 S2 O5 123.6(11) . . ?
O4 S2 O6 102.9(13) . . ?
O5 S2 O6 107.1(5) . . ?
O4 S2 O4' 41.6(14) . . ?
O5 S2 O4' 90.3(12) . . ?
O6 S2 O4' 141.9(11) . . ?
O4 S2 C19 109.9(7) . . ?
O5 S2 C19 105.9(4) . . ?
O6 S2 C19 106.3(5) . . ?
O4' S2 C19 100.7(11) . . ?
S1 O1 Ag3 125.0(4) . 1_655 ?
S1 O3 Ag2 152.2(5) . 1_554 ?
S1 O3 Ag2 104.7(4) . 2_867 ?
Ag2 O3 Ag2 97.3(2) 1_554 2_867 ?
S2 O5 Ag2 118.3(4) . 2_767 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.800
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.151
####################################################################### 
# 
# 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_Ag4
_database_code_depnum_ccdc_archive 'CCDC 1058702'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H36 Ag4 N6 O17 S4'
_chemical_formula_weight         1456.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8904(7)
_cell_length_b                   12.8137(9)
_cell_length_c                   17.3860(11)
_cell_angle_alpha                105.159(1)
_cell_angle_beta                 94.273(1)
_cell_angle_gamma                94.113(1)
_cell_volume                     2324.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2880
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      22.91

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1436
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_T_max  0.6151
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12764
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.22
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8940
_reflns_number_gt                6154
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1200P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8940
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.2007
_refine_ls_wR_factor_gt          0.1697
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Ag1 Ag 0.18943(6) 0.11946(6) -0.47207(5) 0.0641(2) Uani 1 1 d . . .
Ag2 Ag -0.77686(9) -0.12793(8) -0.38271(5) 0.0881(4) Uani 1 1 d . . .
Ag3 Ag 0.29475(5) 0.49965(5) 0.23345(3) 0.04255(19) Uani 1 1 d . . .
Ag4 Ag 0.23917(9) 0.14363(8) 0.84104(7) 0.0976(4) Uani 1 1 d . . .
C1 C 0.1308(6) 0.6645(6) -0.2261(4) 0.0355(16) Uani 1 1 d . . .
H1A H 0.1406 0.6760 -0.1709 0.043 Uiso 1 1 calc R . .
C2 C 0.1684(7) 0.7450(6) -0.2591(5) 0.0441(19) Uani 1 1 d . . .
H2A H 0.2037 0.8107 -0.2251 0.053 Uiso 1 1 calc R . .
C3 C 0.1061(7) 0.6383(6) -0.3853(4) 0.0389(17) Uani 1 1 d . . .
H3A H 0.0978 0.6283 -0.4404 0.047 Uiso 1 1 calc R . .
C4 C 0.0654(7) 0.5533(6) -0.3559(4) 0.0356(16) Uani 1 1 d . . .
H4A H 0.0296 0.4883 -0.3906 0.043 Uiso 1 1 calc R . .
C5 C 0.0784(6) 0.5659(5) -0.2741(4) 0.0270(13) Uani 1 1 d . . .
C6 C 0.0379(6) 0.4775(5) -0.2385(4) 0.0262(13) Uani 1 1 d . . .
C7 C -0.0512(6) 0.3938(5) -0.2780(4) 0.0290(14) Uani 1 1 d . . .
H7A H -0.0886 0.3925 -0.3282 0.035 Uiso 1 1 calc R . .
C8 C -0.0844(6) 0.3119(5) -0.2423(4) 0.0263(13) Uani 1 1 d . . .
C9 C -0.0261(6) 0.3193(6) -0.1661(4) 0.0308(15) Uani 1 1 d . . .
H9A H -0.0433 0.2652 -0.1407 0.037 Uiso 1 1 calc R . .
C10 C 0.0585(6) 0.4093(5) -0.1286(4) 0.0275(14) Uani 1 1 d . . .
C11 C 0.1203(6) 0.4245(5) -0.0465(4) 0.0265(13) Uani 1 1 d . . .
C12 C 0.0899(7) 0.3591(6) 0.0020(4) 0.0396(17) Uani 1 1 d . . .
H12A H 0.0303 0.3004 -0.0170 0.047 Uiso 1 1 calc R . .
C13 C 0.1475(7) 0.3803(6) 0.0787(4) 0.0421(18) Uani 1 1 d . . .
H13A H 0.1253 0.3350 0.1103 0.050 Uiso 1 1 calc R . .
C14 C 0.2645(6) 0.5277(6) 0.0623(4) 0.0339(15) Uani 1 1 d . . .
H14A H 0.3245 0.5857 0.0829 0.041 Uiso 1 1 calc R . .
C15 C 0.2100(6) 0.5111(5) -0.0157(4) 0.0309(14) Uani 1 1 d . . .
H15A H 0.2334 0.5572 -0.0465 0.037 Uiso 1 1 calc R . .
C16 C -0.1922(5) 0.2300(5) -0.2771(4) 0.0251(13) Uani 1 1 d . . .
C17 C -0.2165(6) 0.1695(5) -0.3577(4) 0.0275(14) Uani 1 1 d . . .
C18 C -0.3287(6) 0.1095(5) -0.3852(4) 0.0289(14) Uani 1 1 d . . .
H18A H -0.3443 0.0706 -0.4387 0.035 Uiso 1 1 calc R . .
C19 C -0.4187(6) 0.1071(5) -0.3324(4) 0.0277(14) Uani 1 1 d . . .
C20 C -0.3946(6) 0.1599(6) -0.2530(4) 0.0346(15) Uani 1 1 d . . .
H20A H -0.4533 0.1551 -0.2176 0.041 Uiso 1 1 calc R . .
C21 C -0.2831(6) 0.2203(6) -0.2260(4) 0.0334(15) Uani 1 1 d . . .
H21A H -0.2674 0.2559 -0.1718 0.040 Uiso 1 1 calc R . .
C22 C 0.3056(7) 0.3815(6) 0.7055(4) 0.0396(17) Uani 1 1 d . . .
H22A H 0.2778 0.3822 0.6537 0.048 Uiso 1 1 calc R . .
C23 C 0.2701(7) 0.2969(6) 0.7330(4) 0.0434(18) Uani 1 1 d . . .
H23A H 0.2168 0.2407 0.6994 0.052 Uiso 1 1 calc R . .
C24 C 0.3811(8) 0.3710(7) 0.8525(5) 0.047(2) Uani 1 1 d . . .
H24A H 0.4079 0.3672 0.9037 0.057 Uiso 1 1 calc R . .
C25 C 0.4210(7) 0.4614(6) 0.8304(4) 0.0361(16) Uani 1 1 d . . .
H25A H 0.4722 0.5173 0.8659 0.043 Uiso 1 1 calc R . .
C26 C 0.3836(6) 0.4684(6) 0.7535(4) 0.0312(14) Uani 1 1 d . . .
C27 C 0.4210(6) 0.5641(5) 0.7237(4) 0.0279(14) Uani 1 1 d . . .
C28 C 0.4826(6) 0.6605(6) 0.7741(4) 0.0326(15) Uani 1 1 d . . .
H28A H 0.4978 0.6686 0.8288 0.039 Uiso 1 1 calc R . .
C29 C 0.5204(6) 0.7432(6) 0.7411(4) 0.0310(14) Uani 1 1 d . . .
C30 C 0.4963(6) 0.7275(6) 0.6595(4) 0.0344(15) Uani 1 1 d . . .
H30A H 0.5217 0.7813 0.6356 0.041 Uiso 1 1 calc R . .
C31 C 0.4337(6) 0.6305(5) 0.6139(4) 0.0288(14) Uani 1 1 d . . .
C32 C 0.4004(6) 0.6068(5) 0.5258(4) 0.0293(14) Uani 1 1 d . . .
C33 C 0.4467(6) 0.6730(6) 0.4790(4) 0.0340(15) Uani 1 1 d . . .
H33A H 0.4981 0.7361 0.5027 0.041 Uiso 1 1 calc R . .
C34 C 0.4144(7) 0.6425(6) 0.3983(4) 0.0345(15) Uani 1 1 d . . .
H34A H 0.4460 0.6866 0.3682 0.041 Uiso 1 1 calc R . .
C35 C 0.2974(7) 0.4908(6) 0.4040(4) 0.0372(16) Uani 1 1 d . . .
H35A H 0.2466 0.4281 0.3780 0.045 Uiso 1 1 calc R . .
C36 C 0.3234(7) 0.5132(6) 0.4854(4) 0.0362(16) Uani 1 1 d . . .
H36A H 0.2903 0.4669 0.5133 0.043 Uiso 1 1 calc R . .
C37 C 0.5766(7) 0.8486(6) 0.7962(4) 0.0345(16) Uani 1 1 d . . .
C38 C 0.7001(6) 0.8892(6) 0.8020(4) 0.0330(15) Uani 1 1 d . . .
C39 C 0.7447(6) 0.9859(6) 0.8575(4) 0.0340(15) Uani 1 1 d . . .
H39A H 0.8277 1.0114 0.8615 0.041 Uiso 1 1 calc R . .
C40 C 0.6646(6) 1.0444(6) 0.9070(4) 0.0320(15) Uani 1 1 d . . .
C41 C 0.5415(7) 1.0052(6) 0.8999(4) 0.0425(18) Uani 1 1 d . . .
H41A H 0.4875 1.0445 0.9326 0.051 Uiso 1 1 calc R . .
C42 C 0.4986(7) 0.9103(6) 0.8462(4) 0.0419(18) Uani 1 1 d . . .
H42A H 0.4153 0.8856 0.8424 0.050 Uiso 1 1 calc R . .
N1 N 0.2334(5) 0.4628(5) 0.1092(3) 0.0342(13) Uani 1 1 d . . .
N2 N 0.0900(5) 0.4847(4) -0.1643(3) 0.0276(12) Uani 1 1 d . . .
N3 N 0.1571(5) 0.7347(5) -0.3387(4) 0.0393(14) Uani 1 1 d . . .
N4 N 0.3072(6) 0.2886(5) 0.8065(4) 0.0446(15) Uani 1 1 d . . .
N5 N 0.3966(5) 0.5506(4) 0.6452(3) 0.0291(12) Uani 1 1 d . . .
N6 N 0.3410(5) 0.5539(5) 0.3599(3) 0.0332(13) Uani 1 1 d . . .
S1 S -0.10488(15) 0.16305(15) -0.42875(9) 0.0316(4) Uani 1 1 d . . .
S2 S -0.56987(16) 0.04501(15) -0.37136(12) 0.0390(4) Uani 1 1 d . . .
S3 S 0.81117(17) 0.81302(16) 0.74534(11) 0.0407(4) Uani 1 1 d . . .
S4 S 0.72239(18) 1.16483(15) 0.98169(11) 0.0404(4) Uani 1 1 d . . .
O1 O 0.0092(4) 0.1448(5) -0.3884(3) 0.0455(13) Uani 1 1 d . . .
O1W O 0.2156(10) 0.0737(8) 0.9442(7) 0.145(5) Uani 1 1 d . . .
H1WB H 0.2093 0.1077 0.9926 0.217 Uiso 1 1 d R . .
H1WA H 0.2184 0.0069 0.9422 0.217 Uiso 1 1 d R . .
O2 O -0.0982(5) 0.2637(4) -0.4525(3) 0.0434(12) Uani 1 1 d . . .
O2W O 0.1479(6) 0.2695(6) -0.5145(4) 0.0714(19) Uani 1 1 d . . .
H2WA H 0.0771 0.2934 -0.5126 0.107 Uiso 1 1 d R . .
H2WB H 0.1715 0.2680 -0.5602 0.107 Uiso 1 1 d R . .
O3 O -0.1524(5) 0.0714(4) -0.4974(3) 0.0423(12) Uani 1 1 d . . .
O3W O 0.0781(8) 0.0198(8) 0.7252(7) 0.129(4) Uani 1 1 d . . .
H3WA H 0.0449 0.0503 0.6923 0.193 Uiso 1 1 d R . .
H3WB H 0.0236 -0.0258 0.7337 0.193 Uiso 1 1 d R . .
O4 O -0.5589(5) -0.0619(4) -0.4220(3) 0.0492(14) Uani 1 1 d . . .
O4W O 0.4044(9) 1.2781(9) 1.0239(5) 0.117(4) Uani 1 1 d . . .
H4WA H 0.4671 1.2864 0.9990 0.175 Uiso 1 1 d R . .
H4WB H 0.3619 1.3313 1.0251 0.175 Uiso 1 1 d R . .
O5 O -0.6158(5) 0.1201(5) -0.4150(4) 0.0617(17) Uani 1 1 d . . .
O5W O 1.0436(7) 1.1249(7) 1.0468(5) 0.092(2) Uani 1 1 d . . .
H5WA H 0.9792 1.1350 1.0199 0.138 Uiso 1 1 d R . .
H5WB H 1.0235 1.1243 1.0932 0.138 Uiso 1 1 d R . .
O6 O -0.6387(5) 0.0409(5) -0.3035(4) 0.0622(17) Uani 1 1 d . . .
O7 O 0.7817(7) 0.8144(6) 0.6639(4) 0.073(2) Uani 1 1 d . . .
O8 O 0.7968(5) 0.7050(4) 0.7570(3) 0.0523(14) Uani 1 1 d . . .
O9 O 0.9306(5) 0.8707(5) 0.7781(4) 0.0609(17) Uani 1 1 d . . .
O10 O 0.8422(5) 1.1956(5) 0.9610(3) 0.0609(17) Uani 1 1 d . . .
O11 O 0.7312(6) 1.1333(5) 1.0559(3) 0.0602(17) Uani 1 1 d . . .
O12 O 0.6347(7) 1.2423(5) 0.9786(5) 0.081(2) Uani 1 1 d . . .


_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 O5 2.272(5) 1_655 ?
Ag1 O2W 2.294(6) . ?
Ag1 O3 2.361(5) 2_554 ?
Ag1 O1 2.518(5) . ?
Ag2 N3 2.193(6) 1_445 ?
Ag2 O3 2.468(5) 2_454 ?
Ag2 O6 2.551(6) . ?
Ag3 N1 2.131(5) . ?
Ag3 N6 2.134(5) . ?
Ag4 N4 2.195(6) . ?
Ag4 O1W 2.228(8) . ?
C1 C2 1.358(10) . ?
C1 C5 1.375(9) . ?
C2 N3 1.350(9) . ?
C3 N3 1.342(9) . ?
C3 C4 1.378(10) . ?
C4 C5 1.384(9) . ?
C5 C6 1.483(9) . ?
C6 N2 1.347(8) . ?
C6 C7 1.390(9) . ?
C7 C8 1.392(9) . ?
C8 C9 1.403(9) . ?
C8 C16 1.494(8) . ?
C9 C10 1.403(9) . ?
C10 N2 1.318(8) . ?
C10 C11 1.491(8) . ?
C11 C12 1.376(10) . ?
C11 C15 1.389(9) . ?
C12 C13 1.381(9) . ?
C13 N1 1.329(9) . ?
C14 N1 1.350(9) . ?
C14 C15 1.396(9) . ?
C16 C21 1.398(9) . ?
C16 C17 1.409(9) . ?
C17 C18 1.377(9) . ?
C17 S1 1.787(6) . ?
C18 C19 1.395(9) . ?
C19 C20 1.366(9) . ?
C19 S2 1.780(6) . ?
C20 C21 1.373(9) . ?
C22 C23 1.340(10) . ?
C22 C26 1.389(10) . ?
C23 N4 1.344(10) . ?
C24 N4 1.320(11) . ?
C24 C25 1.366(11) . ?
C25 C26 1.396(9) . ?
C26 C27 1.494(9) . ?
C27 N5 1.333(8) . ?
C27 C28 1.404(9) . ?
C28 C29 1.382(9) . ?
C29 C30 1.382(9) . ?
C29 C37 1.495(9) . ?
C30 C31 1.386(9) . ?
C31 N5 1.332(8) . ?
C31 C32 1.492(9) . ?
C32 C36 1.401(9) . ?
C32 C33 1.412(9) . ?
C33 C34 1.366(9) . ?
C34 N6 1.330(9) . ?
C35 N6 1.338(9) . ?
C35 C36 1.371(9) . ?
C37 C38 1.393(10) . ?
C37 C42 1.396(10) . ?
C38 C39 1.385(9) . ?
C38 S3 1.797(7) . ?
C39 C40 1.390(10) . ?
C40 C41 1.383(10) . ?
C40 S4 1.776(7) . ?
C41 C42 1.352(10) . ?
N3 Ag2 2.193(6) 1_665 ?
S1 O1 1.445(5) . ?
S1 O2 1.452(5) . ?
S1 O3 1.469(5) . ?
S2 O4 1.440(6) . ?
S2 O6 1.454(6) . ?
S2 O5 1.465(6) . ?
S3 O7 1.433(7) . ?
S3 O9 1.447(6) . ?
S3 O8 1.450(6) . ?
S4 O10 1.434(6) . ?
S4 O12 1.434(7) . ?
S4 O11 1.448(6) . ?
O3 Ag1 2.361(5) 2_554 ?
O3 Ag2 2.468(5) 2_454 ?
O5 Ag1 2.272(5) 1_455 ?

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
O5 Ag1 O2W 116.4(2) 1_655 . ?
O5 Ag1 O3 92.99(19) 1_655 2_554 ?
O2W Ag1 O3 144.3(2) . 2_554 ?
O5 Ag1 O1 120.9(2) 1_655 . ?
O2W Ag1 O1 90.1(2) . . ?
O3 Ag1 O1 91.61(18) 2_554 . ?
N3 Ag2 O3 131.0(2) 1_445 2_454 ?
N3 Ag2 O6 126.7(2) 1_445 . ?
O3 Ag2 O6 100.89(19) 2_454 . ?
N1 Ag3 N6 172.4(2) . . ?
N4 Ag4 O1W 144.4(4) . . ?
C2 C1 C5 120.3(7) . . ?
N3 C2 C1 123.4(7) . . ?
N3 C3 C4 123.6(7) . . ?
C3 C4 C5 119.1(6) . . ?
C1 C5 C4 117.5(6) . . ?
C1 C5 C6 120.5(6) . . ?
C4 C5 C6 122.0(6) . . ?
N2 C6 C7 121.8(6) . . ?
N2 C6 C5 116.0(5) . . ?
C7 C6 C5 122.2(6) . . ?
C6 C7 C8 119.8(6) . . ?
C7 C8 C9 117.4(6) . . ?
C7 C8 C16 121.2(6) . . ?
C9 C8 C16 120.6(6) . . ?
C10 C9 C8 119.3(6) . . ?
N2 C10 C9 122.1(6) . . ?
N2 C10 C11 115.7(6) . . ?
C9 C10 C11 122.1(6) . . ?
C12 C11 C15 117.9(6) . . ?
C12 C11 C10 123.3(6) . . ?
C15 C11 C10 118.8(6) . . ?
C11 C12 C13 120.3(6) . . ?
N1 C13 C12 122.7(7) . . ?
N1 C14 C15 122.6(6) . . ?
C11 C15 C14 118.8(6) . . ?
C21 C16 C17 117.1(5) . . ?
C21 C16 C8 116.4(5) . . ?
C17 C16 C8 126.3(5) . . ?
C18 C17 C16 120.7(6) . . ?
C18 C17 S1 116.5(5) . . ?
C16 C17 S1 122.7(5) . . ?
C17 C18 C19 119.8(6) . . ?
C20 C19 C18 120.6(6) . . ?
C20 C19 S2 120.1(5) . . ?
C18 C19 S2 119.1(5) . . ?
C19 C20 C21 119.4(6) . . ?
C20 C21 C16 122.3(6) . . ?
C23 C22 C26 120.6(7) . . ?
C22 C23 N4 123.6(7) . . ?
N4 C24 C25 124.7(7) . . ?
C24 C25 C26 118.8(7) . . ?
C22 C26 C25 116.2(6) . . ?
C22 C26 C27 120.8(6) . . ?
C25 C26 C27 123.0(6) . . ?
N5 C27 C28 122.0(6) . . ?
N5 C27 C26 115.6(6) . . ?
C28 C27 C26 122.4(6) . . ?
C29 C28 C27 118.9(6) . . ?
C28 C29 C30 118.6(6) . . ?
C28 C29 C37 118.4(6) . . ?
C30 C29 C37 122.9(6) . . ?
C29 C30 C31 119.1(6) . . ?
N5 C31 C30 122.7(6) . . ?
N5 C31 C32 114.1(6) . . ?
C30 C31 C32 123.2(6) . . ?
C36 C32 C33 117.0(6) . . ?
C36 C32 C31 119.9(6) . . ?
C33 C32 C31 123.0(6) . . ?
C34 C33 C32 118.7(6) . . ?
N6 C34 C33 124.4(7) . . ?
N6 C35 C36 123.8(7) . . ?
C35 C36 C32 119.1(7) . . ?
C38 C37 C42 117.9(6) . . ?
C38 C37 C29 125.3(6) . . ?
C42 C37 C29 116.9(6) . . ?
C39 C38 C37 120.9(6) . . ?
C39 C38 S3 117.0(5) . . ?
C37 C38 S3 121.8(5) . . ?
C38 C39 C40 119.6(6) . . ?
C41 C40 C39 119.3(7) . . ?
C41 C40 S4 120.6(5) . . ?
C39 C40 S4 119.9(5) . . ?
C42 C41 C40 120.9(7) . . ?
C41 C42 C37 121.3(7) . . ?
C13 N1 C14 117.7(6) . . ?
C13 N1 Ag3 118.4(5) . . ?
C14 N1 Ag3 123.2(5) . . ?
C10 N2 C6 119.6(5) . . ?
C3 N3 C2 116.1(6) . . ?
C3 N3 Ag2 124.8(5) . 1_665 ?
C2 N3 Ag2 119.1(5) . 1_665 ?
C24 N4 C23 116.1(7) . . ?
C24 N4 Ag4 125.5(5) . . ?
C23 N4 Ag4 118.4(5) . . ?
C31 N5 C27 118.7(6) . . ?
C34 N6 C35 117.0(6) . . ?
C34 N6 Ag3 125.6(5) . . ?
C35 N6 Ag3 117.3(5) . . ?
O1 S1 O2 113.7(3) . . ?
O1 S1 O3 113.0(3) . . ?
O2 S1 O3 110.3(3) . . ?
O1 S1 C17 105.3(3) . . ?
O2 S1 C17 108.7(3) . . ?
O3 S1 C17 105.4(3) . . ?
O4 S2 O6 111.8(4) . . ?
O4 S2 O5 113.6(4) . . ?
O6 S2 O5 112.8(4) . . ?
O4 S2 C19 108.3(3) . . ?
O6 S2 C19 107.3(3) . . ?
O5 S2 C19 102.2(3) . . ?
O7 S3 O9 111.9(4) . . ?
O7 S3 O8 113.2(4) . . ?
O9 S3 O8 113.0(4) . . ?
O7 S3 C38 106.1(3) . . ?
O9 S3 C38 105.6(3) . . ?
O8 S3 C38 106.4(3) . . ?
O10 S4 O12 113.6(5) . . ?
O10 S4 O11 111.4(4) . . ?
O12 S4 O11 114.0(4) . . ?
O10 S4 C40 106.0(3) . . ?
O12 S4 C40 106.0(4) . . ?
O11 S4 C40 105.1(3) . . ?
S1 O1 Ag1 115.4(3) . . ?
S1 O3 Ag1 138.7(3) . 2_554 ?
S1 O3 Ag2 113.3(3) . 2_454 ?
Ag1 O3 Ag2 107.94(18) 2_554 2_454 ?
S2 O5 Ag1 127.9(3) . 1_455 ?
S2 O6 Ag2 93.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.911
_refine_diff_density_min         -2.308
_refine_diff_density_rms         0.149
####################################################################### 
# 
# 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_Pb1
_database_code_depnum_ccdc_archive 'CCDC 1058703'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H17 N3 O8 Pb S2'
_chemical_formula_weight         710.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3520(11)
_cell_length_b                   11.7428(16)
_cell_length_c                   12.3408(16)
_cell_angle_alpha                100.670(2)
_cell_angle_beta                 101.093(2)
_cell_angle_gamma                97.040(2)
_cell_volume                     1151.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3894
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      27.61

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    7.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1519
_exptl_absorpt_correction_T_max  0.1772
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5825
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4010
_reflns_number_gt                3731
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.
The following restrains were used:
dfix 0.85 0.02 o1w h1wa o1w h1wb
dfix 1.37 0.02 h1wa h1wb 
;

_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)+(0.0322P)²+2.3113P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4010
_refine_ls_number_parameters     322
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0677
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.003
_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
Pb1 Pb 0.75895(2) 1.189096(17) 0.402349(16) 0.03106(8) Uani 1 1 d . . .
C1 C 0.0602(9) 0.3006(6) -0.3504(5) 0.0570(18) Uani 1 1 d . . .
H1A H 0.0919 0.2293 -0.3770 0.068 Uiso 1 1 calc R . .
C2 C 0.1341(8) 0.3603(5) -0.2421(5) 0.0416(14) Uani 1 1 d . . .
H2A H 0.2141 0.3297 -0.1978 0.050 Uiso 1 1 calc R . .
C3 C 0.0893(6) 0.4652(4) -0.1996(4) 0.0281(11) Uani 1 1 d . . .
C4 C -0.0255(7) 0.5077(5) -0.2717(5) 0.0386(13) Uani 1 1 d . . .
H4A H -0.0565 0.5800 -0.2480 0.046 Uiso 1 1 calc R . .
C5 C -0.0929(8) 0.4426(6) -0.3777(5) 0.0495(16) Uani 1 1 d . . .
H5A H -0.1712 0.4722 -0.4242 0.059 Uiso 1 1 calc R . .
C6 C 0.1634(6) 0.5304(4) -0.0812(4) 0.0268(11) Uani 1 1 d . . .
C7 C 0.1438(6) 0.6461(4) -0.0422(4) 0.0300(11) Uani 1 1 d . . .
H7A H 0.0830 0.6855 -0.0901 0.036 Uiso 1 1 calc R . .
C8 C 0.2160(6) 0.7015(4) 0.0691(4) 0.0263(11) Uani 1 1 d . . .
C9 C 0.3018(7) 0.6379(4) 0.1365(4) 0.0315(12) Uani 1 1 d . . .
H9A H 0.3486 0.6715 0.2121 0.038 Uiso 1 1 calc R . .
C10 C 0.3188(6) 0.5233(4) 0.0916(4) 0.0259(10) Uani 1 1 d . . .
C11 C 0.4163(6) 0.4539(4) 0.1617(4) 0.0291(11) Uani 1 1 d . . .
C12 C 0.4459(7) 0.3457(5) 0.1121(5) 0.0383(13) Uani 1 1 d . . .
H12A H 0.4027 0.3147 0.0355 0.046 Uiso 1 1 calc R . .
C13 C 0.5407(8) 0.2833(5) 0.1771(5) 0.0430(14) Uani 1 1 d . . .
H13A H 0.5605 0.2107 0.1423 0.052 Uiso 1 1 calc R . .
C14 C 0.5739(8) 0.4264(6) 0.3336(5) 0.0492(16) Uani 1 1 d . . .
H14A H 0.6173 0.4549 0.4106 0.059 Uiso 1 1 calc R . .
C15 C 0.4822(8) 0.4943(5) 0.2755(5) 0.0434(14) Uani 1 1 d . . .
H15A H 0.4649 0.5667 0.3126 0.052 Uiso 1 1 calc R . .
C16 C 0.1926(6) 0.8231(4) 0.1166(4) 0.0282(11) Uani 1 1 d . . .
C17 C 0.3217(6) 0.9111(4) 0.1831(4) 0.0293(11) Uani 1 1 d . . .
C18 C 0.2856(7) 1.0174(5) 0.2320(5) 0.0334(12) Uani 1 1 d . . .
H18A H 0.3713 1.0760 0.2750 0.040 Uiso 1 1 calc R . .
C19 C 0.1258(7) 1.0386(5) 0.2185(4) 0.0331(12) Uani 1 1 d . . .
C20 C -0.0013(7) 0.9562(5) 0.1496(5) 0.0391(13) Uani 1 1 d . . .
H20A H -0.1091 0.9719 0.1370 0.047 Uiso 1 1 calc R . .
C21 C 0.0338(7) 0.8488(5) 0.0987(5) 0.0364(13) Uani 1 1 d . . .
H21A H -0.0518 0.7929 0.0514 0.044 Uiso 1 1 calc R . .
N1 N -0.0535(7) 0.3384(5) -0.4193(4) 0.0521(14) Uani 1 1 d . . .
N2 N 0.2489(5) 0.4699(4) -0.0157(3) 0.0279(9) Uani 1 1 d . . .
N3 N 0.6039(6) 0.3224(4) 0.2861(4) 0.0419(12) Uani 1 1 d . . .
S1 S 0.53670(17) 0.89760(12) 0.21413(12) 0.0346(3) Uani 1 1 d . . .
S2 S 0.08954(18) 1.16601(12) 0.30675(13) 0.0391(3) Uani 1 1 d . . .
O1 O 0.5613(6) 0.8476(4) 0.3150(4) 0.0557(12) Uani 1 1 d . . .
O1W O 0.7304(9) 1.0222(5) 0.5085(6) 0.0868(18) Uani 1 1 d D . .
H1WA H 0.826(6) 1.004(8) 0.530(9) 0.130 Uiso 1 1 d D . .
H1WB H 0.674(10) 0.963(6) 0.459(7) 0.130 Uiso 1 1 d D . .
O2W O 0.5219(6) 1.2485(5) 0.5036(4) 0.0616(13) Uani 1 1 d . . .
H2WA H 0.4364 1.2664 0.4652 0.092 Uiso 1 1 d R . .
H2WB H 0.5015 1.2406 0.5670 0.092 Uiso 1 1 d R . .
O2 O 0.5712(5) 0.8252(4) 0.1186(4) 0.0580(13) Uani 1 1 d . . .
O3 O 0.6235(5) 1.0181(3) 0.2388(3) 0.0424(10) Uani 1 1 d . . .
O4 O 0.2380(6) 1.2515(4) 0.3347(5) 0.0643(14) Uani 1 1 d . . .
O5 O 0.0540(6) 1.1244(4) 0.4058(3) 0.0520(11) Uani 1 1 d . . .
O6 O -0.0561(5) 1.2038(3) 0.2481(3) 0.0432(10) Uani 1 1 d . . .


_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
Pb1 O3 2.539(4) . ?
Pb1 O1W 2.564(6) . ?
Pb1 N3 2.608(5) 1_565 ?
Pb1 N1 2.635(5) 1_666 ?
Pb1 O2W 2.634(5) . ?
Pb1 O5 2.661(4) 1_655 ?
Pb1 O6 2.689(4) 1_655 ?
C1 N1 1.324(8) . ?
C1 C2 1.375(8) . ?
C1 H1A 0.9300 . ?
C2 C3 1.372(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.383(7) . ?
C3 C6 1.493(7) . ?
C4 C5 1.361(8) . ?
C4 H4A 0.9300 . ?
C5 N1 1.341(8) . ?
C5 H5A 0.9300 . ?
C6 N2 1.335(6) . ?
C6 C7 1.395(7) . ?
C7 C8 1.388(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.377(7) . ?
C8 C16 1.491(7) . ?
C9 C10 1.392(7) . ?
C9 H9A 0.9300 . ?
C10 N2 1.339(6) . ?
C10 C11 1.493(7) . ?
C11 C15 1.375(7) . ?
C11 C12 1.378(7) . ?
C12 C13 1.387(8) . ?
C12 H12A 0.9300 . ?
C13 N3 1.318(7) . ?
C13 H13A 0.9300 . ?
C14 N3 1.329(8) . ?
C14 C15 1.373(8) . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9300 . ?
C16 C21 1.381(8) . ?
C16 C17 1.406(7) . ?
C17 C18 1.377(7) . ?
C17 S1 1.796(5) . ?
C18 C19 1.373(7) . ?
C18 H18A 0.9300 . ?
C19 C20 1.372(8) . ?
C19 S2 1.775(5) . ?
C20 C21 1.393(8) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
N1 Pb1 2.635(5) 1_444 ?
N3 Pb1 2.608(5) 1_545 ?
S1 O2 1.420(4) . ?
S1 O3 1.458(4) . ?
S1 O1 1.462(5) . ?
S2 O4 1.438(5) . ?
S2 O6 1.454(4) . ?
S2 O5 1.465(5) . ?
O1W H1WA 0.85(2) . ?
O1W H1WB 0.86(2) . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8499 . ?
O5 Pb1 2.661(4) 1_455 ?
O6 Pb1 2.689(4) 1_455 ?

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
O3 Pb1 O1W 79.60(19) . . ?
O3 Pb1 N3 86.93(15) . 1_565 ?
O1W Pb1 N3 146.04(19) . 1_565 ?
O3 Pb1 N1 168.01(15) . 1_666 ?
O1W Pb1 N1 93.5(2) . 1_666 ?
N3 Pb1 N1 103.95(17) 1_565 1_666 ?
O3 Pb1 O2W 106.02(14) . . ?
O1W Pb1 O2W 80.38(19) . . ?
N3 Pb1 O2W 73.59(15) 1_565 . ?
N1 Pb1 O2W 82.24(17) 1_666 . ?
O3 Pb1 O5 91.28(13) . 1_655 ?
O1W Pb1 O5 80.66(19) . 1_655 ?
N3 Pb1 O5 131.06(15) 1_565 1_655 ?
N1 Pb1 O5 77.83(15) 1_666 1_655 ?
O2W Pb1 O5 151.45(14) . 1_655 ?
O3 Pb1 O6 75.63(13) . 1_655 ?
O1W Pb1 O6 125.84(18) . 1_655 ?
N3 Pb1 O6 79.46(13) 1_565 1_655 ?
N1 Pb1 O6 101.11(16) 1_666 1_655 ?
O2W Pb1 O6 152.80(14) . 1_655 ?
O5 Pb1 O6 52.99(12) 1_655 1_655 ?
N1 C1 C2 124.0(6) . . ?
N1 C1 H1A 118.0 . . ?
C2 C1 H1A 118.0 . . ?
C3 C2 C1 119.6(5) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 117.0(5) . . ?
C2 C3 C6 121.0(5) . . ?
C4 C3 C6 122.0(5) . . ?
C5 C4 C3 119.4(5) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
N1 C5 C4 124.2(6) . . ?
N1 C5 H5A 117.9 . . ?
C4 C5 H5A 117.9 . . ?
N2 C6 C7 122.7(4) . . ?
N2 C6 C3 115.1(4) . . ?
C7 C6 C3 122.1(4) . . ?
C8 C7 C6 119.2(5) . . ?
C8 C7 H7A 120.4 . . ?
C6 C7 H7A 120.4 . . ?
C9 C8 C7 117.7(4) . . ?
C9 C8 C16 120.8(4) . . ?
C7 C8 C16 121.4(4) . . ?
C8 C9 C10 120.1(5) . . ?
C8 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
N2 C10 C9 122.0(5) . . ?
N2 C10 C11 116.8(4) . . ?
C9 C10 C11 121.2(4) . . ?
C15 C11 C12 117.4(5) . . ?
C15 C11 C10 122.7(5) . . ?
C12 C11 C10 119.9(5) . . ?
C11 C12 C13 119.5(5) . . ?
C11 C12 H12A 120.2 . . ?
C13 C12 H12A 120.2 . . ?
N3 C13 C12 122.8(5) . . ?
N3 C13 H13A 118.6 . . ?
C12 C13 H13A 118.6 . . ?
N3 C14 C15 123.6(6) . . ?
N3 C14 H14A 118.2 . . ?
C15 C14 H14A 118.2 . . ?
C14 C15 C11 119.2(5) . . ?
C14 C15 H15A 120.4 . . ?
C11 C15 H15A 120.4 . . ?
C21 C16 C17 118.3(5) . . ?
C21 C16 C8 118.0(5) . . ?
C17 C16 C8 123.7(5) . . ?
C18 C17 C16 119.4(5) . . ?
C18 C17 S1 115.0(4) . . ?
C16 C17 S1 125.6(4) . . ?
C19 C18 C17 121.3(5) . . ?
C19 C18 H18A 119.4 . . ?
C17 C18 H18A 119.4 . . ?
C18 C19 C20 120.3(5) . . ?
C18 C19 S2 117.2(4) . . ?
C20 C19 S2 122.0(4) . . ?
C19 C20 C21 118.8(5) . . ?
C19 C20 H20A 120.6 . . ?
C21 C20 H20A 120.6 . . ?
C16 C21 C20 121.7(5) . . ?
C16 C21 H21A 119.1 . . ?
C20 C21 H21A 119.2 . . ?
C1 N1 C5 115.7(5) . . ?
C1 N1 Pb1 119.3(4) . 1_444 ?
C5 N1 Pb1 122.8(4) . 1_444 ?
C6 N2 C10 118.2(4) . . ?
C13 N3 C14 117.3(5) . . ?
C13 N3 Pb1 119.8(4) . 1_545 ?
C14 N3 Pb1 122.6(4) . 1_545 ?
O2 S1 O3 113.4(3) . . ?
O2 S1 O1 113.3(3) . . ?
O3 S1 O1 111.0(3) . . ?
O2 S1 C17 108.4(3) . . ?
O3 S1 C17 104.3(2) . . ?
O1 S1 C17 105.5(3) . . ?
O4 S2 O6 114.6(3) . . ?
O4 S2 O5 112.1(3) . . ?
O6 S2 O5 109.7(3) . . ?
O4 S2 C19 107.7(3) . . ?
O6 S2 C19 108.2(3) . . ?
O5 S2 C19 103.8(3) . . ?
Pb1 O1W H1WA 109(8) . . ?
Pb1 O1W H1WB 105(8) . . ?
H1WA O1W H1WB 106(3) . . ?
Pb1 O2W H2WA 118.9 . . ?
Pb1 O2W H2WB 132.0 . . ?
H2WA O2W H2WB 107.7 . . ?
S1 O3 Pb1 141.8(3) . . ?
S2 O5 Pb1 98.7(2) . 1_455 ?
S2 O6 Pb1 97.8(2) . 1_455 ?

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 C1 C2 C3 0.6(11) . . . . ?
C1 C2 C3 C4 -2.5(9) . . . . ?
C1 C2 C3 C6 178.1(6) . . . . ?
C2 C3 C4 C5 2.7(9) . . . . ?
C6 C3 C4 C5 -177.9(5) . . . . ?
C3 C4 C5 N1 -1.1(10) . . . . ?
C2 C3 C6 N2 -12.1(7) . . . . ?
C4 C3 C6 N2 168.6(5) . . . . ?
C2 C3 C6 C7 168.1(5) . . . . ?
C4 C3 C6 C7 -11.2(8) . . . . ?
N2 C6 C7 C8 0.2(8) . . . . ?
C3 C6 C7 C8 180.0(5) . . . . ?
C6 C7 C8 C9 -1.2(7) . . . . ?
C6 C7 C8 C16 -177.2(5) . . . . ?
C7 C8 C9 C10 2.2(8) . . . . ?
C16 C8 C9 C10 178.2(5) . . . . ?
C8 C9 C10 N2 -2.3(8) . . . . ?
C8 C9 C10 C11 177.8(5) . . . . ?
N2 C10 C11 C15 -174.2(5) . . . . ?
C9 C10 C11 C15 5.7(8) . . . . ?
N2 C10 C11 C12 7.1(7) . . . . ?
C9 C10 C11 C12 -173.0(5) . . . . ?
C15 C11 C12 C13 -0.7(8) . . . . ?
C10 C11 C12 C13 178.1(5) . . . . ?
C11 C12 C13 N3 0.6(9) . . . . ?
N3 C14 C15 C11 0.2(10) . . . . ?
C12 C11 C15 C14 0.3(9) . . . . ?
C10 C11 C15 C14 -178.4(6) . . . . ?
C9 C8 C16 C21 -127.9(6) . . . . ?
C7 C8 C16 C21 48.0(7) . . . . ?
C9 C8 C16 C17 49.0(7) . . . . ?
C7 C8 C16 C17 -135.1(5) . . . . ?
C21 C16 C17 C18 2.8(8) . . . . ?
C8 C16 C17 C18 -174.0(5) . . . . ?
C21 C16 C17 S1 -178.4(4) . . . . ?
C8 C16 C17 S1 4.8(7) . . . . ?
C16 C17 C18 C19 1.0(8) . . . . ?
S1 C17 C18 C19 -177.9(4) . . . . ?
C17 C18 C19 C20 -4.2(9) . . . . ?
C17 C18 C19 S2 167.8(4) . . . . ?
C18 C19 C20 C21 3.4(9) . . . . ?
S2 C19 C20 C21 -168.3(4) . . . . ?
C17 C16 C21 C20 -3.6(8) . . . . ?
C8 C16 C21 C20 173.4(5) . . . . ?
C19 C20 C21 C16 0.5(9) . . . . ?
C2 C1 N1 C5 1.1(11) . . . . ?
C2 C1 N1 Pb1 -162.4(6) . . . 1_444 ?
C4 C5 N1 C1 -0.9(11) . . . . ?
C4 C5 N1 Pb1 162.0(5) . . . 1_444 ?
C7 C6 N2 C10 -0.3(7) . . . . ?
C3 C6 N2 C10 179.9(4) . . . . ?
C9 C10 N2 C6 1.3(7) . . . . ?
C11 C10 N2 C6 -178.8(4) . . . . ?
C12 C13 N3 C14 -0.1(9) . . . . ?
C12 C13 N3 Pb1 174.9(5) . . . 1_545 ?
C15 C14 N3 C13 -0.3(10) . . . . ?
C15 C14 N3 Pb1 -175.1(5) . . . 1_545 ?
C18 C17 S1 O2 -146.8(4) . . . . ?
C16 C17 S1 O2 34.3(5) . . . . ?
C18 C17 S1 O3 -25.7(5) . . . . ?
C16 C17 S1 O3 155.5(5) . . . . ?
C18 C17 S1 O1 91.4(5) . . . . ?
C16 C17 S1 O1 -87.4(5) . . . . ?
C18 C19 S2 O4 28.6(5) . . . . ?
C20 C19 S2 O4 -159.5(5) . . . . ?
C18 C19 S2 O6 153.0(4) . . . . ?
C20 C19 S2 O6 -35.1(6) . . . . ?
C18 C19 S2 O5 -90.4(5) . . . . ?
C20 C19 S2 O5 81.4(5) . . . . ?
O2 S1 O3 Pb1 -145.6(4) . . . . ?
O1 S1 O3 Pb1 -16.6(5) . . . . ?
C17 S1 O3 Pb1 96.7(4) . . . . ?
O1W Pb1 O3 S1 14.0(4) . . . . ?
N3 Pb1 O3 S1 -134.7(4) 1_565 . . . ?
N1 Pb1 O3 S1 69.8(9) 1_666 . . . ?
O2W Pb1 O3 S1 -62.7(4) . . . . ?
O5 Pb1 O3 S1 94.3(4) 1_655 . . . ?
O6 Pb1 O3 S1 145.4(4) 1_655 . . . ?
O4 S2 O5 Pb1 120.3(2) . . . 1_455 ?
O6 S2 O5 Pb1 -8.2(3) . . . 1_455 ?
C19 S2 O5 Pb1 -123.7(2) . . . 1_455 ?
O4 S2 O6 Pb1 -119.1(3) . . . 1_455 ?
O5 S2 O6 Pb1 8.1(3) . . . 1_455 ?
C19 S2 O6 Pb1 120.8(2) . . . 1_455 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.733
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.109
####################################################################### 
# 
# 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_Pb2
_database_code_depnum_ccdc_archive 'CCDC 1058704'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H25 N3 O12 Pb S2'
_chemical_formula_weight         782.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   13.784(3)
_cell_length_b                   14.323(3)
_cell_length_c                   13.791(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.018(4)
_cell_angle_gamma                90.00
_cell_volume                     2722.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    6.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1942
_exptl_absorpt_correction_T_max  0.2259
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13145
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_sigmaI/netI    0.1136
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4781
_reflns_number_gt                2686
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0404P)²+1.7792P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4781
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1019
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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
Pb1 Pb 1.28856(3) 0.60159(3) -0.40939(3) 0.04859(18) Uani 1 1 d . . .
S1 S 0.7662(2) 0.8521(2) 0.1685(2) 0.0509(8) Uani 1 1 d . . .
S2 S 0.4162(2) 0.6885(2) 0.0823(2) 0.0493(8) Uani 1 1 d . . .
C1 C 1.0783(9) 0.6033(8) -0.2609(8) 0.055(3) Uani 1 1 d . . .
H1A H 1.0479 0.5964 -0.3212 0.066 Uiso 1 1 calc R . .
C2 C 1.0217(8) 0.6111(8) -0.1806(8) 0.054(3) Uani 1 1 d . . .
H2A H 0.9545 0.6088 -0.1873 0.064 Uiso 1 1 calc R . .
C3 C 1.0647(7) 0.6228(7) -0.0875(8) 0.040(3) Uani 1 1 d . . .
C4 C 1.1631(8) 0.6226(8) -0.0858(8) 0.051(3) Uani 1 1 d . . .
H4A H 1.1958 0.6287 -0.0266 0.061 Uiso 1 1 calc R . .
C5 C 1.2163(8) 0.6138(9) -0.1693(9) 0.061(4) Uani 1 1 d . . .
H5A H 1.2837 0.6139 -0.1640 0.073 Uiso 1 1 calc R . .
C6 C 1.0067(8) 0.6341(7) -0.0001(7) 0.037(3) Uani 1 1 d . . .
C7 C 0.9102(8) 0.6492(8) -0.0057(8) 0.045(3) Uani 1 1 d . . .
H7A H 0.8786 0.6516 -0.0658 0.054 Uiso 1 1 calc R . .
C8 C 0.8578(7) 0.6615(8) 0.0795(8) 0.042(3) Uani 1 1 d . . .
C9 C 0.9077(7) 0.6559(8) 0.1681(8) 0.046(3) Uani 1 1 d . . .
H9A H 0.8749 0.6624 0.2260 0.055 Uiso 1 1 calc R . .
C10 C 1.0073(8) 0.6405(8) 0.1684(8) 0.043(3) Uani 1 1 d . . .
C11 C 1.0616(8) 0.6331(7) 0.2616(8) 0.042(3) Uani 1 1 d . . .
C12 C 1.1597(9) 0.6409(8) 0.2616(9) 0.056(3) Uani 1 1 d . . .
H12A H 1.1921 0.6495 0.2037 0.067 Uiso 1 1 calc R . .
C13 C 1.2116(9) 0.6359(8) 0.3492(10) 0.057(3) Uani 1 1 d . . .
H13A H 1.2787 0.6411 0.3474 0.068 Uiso 1 1 calc R . .
C14 C 1.0752(9) 0.6175(9) 0.4356(8) 0.059(4) Uani 1 1 d . . .
H14A H 1.0434 0.6096 0.4939 0.071 Uiso 1 1 calc R . .
C15 C 1.0203(8) 0.6220(8) 0.3495(7) 0.050(3) Uani 1 1 d . . .
H15A H 0.9531 0.6171 0.3526 0.060 Uiso 1 1 calc R . .
C16 C 0.7502(7) 0.6751(8) 0.0795(7) 0.037(3) Uani 1 1 d . . .
C17 C 0.7027(7) 0.7551(7) 0.1171(7) 0.038(3) Uani 1 1 d . . .
C18 C 0.6021(8) 0.7575(8) 0.1170(7) 0.047(3) Uani 1 1 d . . .
H18A H 0.5716 0.8094 0.1430 0.056 Uiso 1 1 calc R . .
C19 C 0.5451(8) 0.6855(8) 0.0794(8) 0.043(3) Uani 1 1 d . . .
C20 C 0.5920(8) 0.6097(8) 0.0381(8) 0.051(3) Uani 1 1 d . . .
H20A H 0.5555 0.5613 0.0112 0.062 Uiso 1 1 calc R . .
C21 C 0.6946(8) 0.6053(8) 0.0363(8) 0.051(3) Uani 1 1 d . . .
H21A H 0.7248 0.5553 0.0062 0.061 Uiso 1 1 calc R . .
N1 N 1.1756(7) 0.6052(7) -0.2564(7) 0.054(3) Uani 1 1 d . . .
N2 N 1.0564(6) 0.6293(6) 0.0845(6) 0.040(2) Uani 1 1 d . . .
N3 N 1.1702(8) 0.6240(6) 0.4367(7) 0.052(3) Uani 1 1 d . . .
O1 O 0.7947(5) 0.8260(6) 0.2664(5) 0.059(2) Uani 1 1 d . . .
O2 O 0.8481(5) 0.8721(5) 0.1063(5) 0.058(2) Uani 1 1 d . . .
O3 O 0.6961(6) 0.9273(5) 0.1671(6) 0.065(2) Uani 1 1 d . . .
O4 O 0.3824(6) 0.5931(6) 0.0772(7) 0.081(3) Uani 1 1 d . . .
O5 O 0.3925(5) 0.7361(6) 0.1714(5) 0.061(2) Uani 1 1 d . . .
O6 O 0.3837(5) 0.7450(6) -0.0004(5) 0.069(3) Uani 1 1 d . . .
O1W O 1.4068(6) 0.5287(7) -0.5310(6) 0.091(3) Uani 1 1 d . . .
H1WA H 1.4601 0.5177 -0.5589 0.137 Uiso 1 1 d R . .
H1WB H 1.3610 0.5111 -0.5689 0.137 Uiso 1 1 d R . .
O2W O 1.3866(7) 0.5027(7) -0.2937(6) 0.106(4) Uani 1 1 d . . .
H2WA H 1.3760 0.4603 -0.2520 0.159 Uiso 1 1 d R . .
H2WB H 1.4326 0.4841 -0.3291 0.159 Uiso 1 1 d R . .
O3W O 1.2083(5) 0.4493(5) -0.4316(5) 0.061(2) Uani 1 1 d . . .
H3WA H 1.1696 0.4364 -0.4784 0.092 Uiso 1 1 d R . .
H3WB H 1.1778 0.4415 -0.3792 0.092 Uiso 1 1 d R . .
O4W O 1.4883(7) 0.6890(8) -0.6508(6) 0.106(4) Uani 1 1 d . . .
H4WA H 1.5357 0.7271 -0.6492 0.160 Uiso 1 1 d R . .
H4WB H 1.4557 0.6994 -0.7026 0.160 Uiso 1 1 d R . .
O5W O 1.5466(8) 0.5487(9) -0.2010(8) 0.137(5) Uani 1 1 d . . .
H5WA H 1.5860 0.5939 -0.1936 0.205 Uiso 1 1 d R . .
H5WB H 1.5703 0.5019 -0.1710 0.205 Uiso 1 1 d R . .
O6W O 1.3098(7) 0.3106(6) -0.3588(6) 0.098(3) Uani 1 1 d . . .
H6WA H 1.3330 0.2862 -0.4096 0.148 Uiso 1 1 d R . .
H6WB H 1.2884 0.2667 -0.3237 0.148 Uiso 1 1 d R . .


_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
Pb1 O3W 2.462(7) . ?
Pb1 O2W 2.511(9) . ?
Pb1 O1W 2.580(8) . ?
Pb1 N1 2.645(9) . ?
Pb1 N3 2.673(9) 1_554 ?
S1 O1 1.448(7) . ?
S1 O2 1.459(8) . ?
S1 O3 1.446(8) . ?
S1 C17 1.783(10) . ?
S2 O4 1.445(8) . ?
S2 O5 1.449(8) . ?
S2 O6 1.462(8) . ?
S2 C19 1.778(11) . ?
C1 N1 1.342(13) . ?
C1 C2 1.371(14) . ?
C2 C3 1.414(14) . ?
C3 C4 1.356(14) . ?
C3 C6 1.467(13) . ?
C4 C5 1.382(14) . ?
C5 N1 1.323(13) . ?
C6 N2 1.344(12) . ?
C6 C7 1.349(13) . ?
C7 C8 1.401(13) . ?
C8 C9 1.394(13) . ?
C8 C16 1.497(14) . ?
C9 C10 1.389(14) . ?
C10 N2 1.361(12) . ?
C10 C11 1.480(14) . ?
C11 C15 1.358(13) . ?
C11 C12 1.357(14) . ?
C12 C13 1.395(15) . ?
C13 N3 1.354(14) . ?
C14 N3 1.313(13) . ?
C14 C15 1.398(14) . ?
C16 C21 1.388(13) . ?
C16 C17 1.422(13) . ?
C17 C18 1.387(13) . ?
C18 C19 1.392(14) . ?
C19 C20 1.390(14) . ?
C20 C21 1.416(14) . ?
N3 Pb1 2.673(9) 1_556 ?

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
O3W Pb1 O2W 79.3(3) . . ?
O3W Pb1 O1W 81.3(3) . . ?
O2W Pb1 O1W 81.1(3) . . ?
O3W Pb1 N1 81.2(3) . . ?
O2W Pb1 N1 79.7(3) . . ?
O1W Pb1 N1 156.1(3) . . ?
O3W Pb1 N3 75.0(3) . 1_554 ?
O2W Pb1 N3 152.4(3) . 1_554 ?
O1W Pb1 N3 85.2(3) . 1_554 ?
N1 Pb1 N3 105.8(3) . 1_554 ?
O1 S1 O2 113.5(5) . . ?
O1 S1 O3 112.0(5) . . ?
O2 S1 O3 111.7(5) . . ?
O1 S1 C17 107.0(5) . . ?
O2 S1 C17 107.4(5) . . ?
O3 S1 C17 104.6(5) . . ?
O4 S2 O5 114.1(5) . . ?
O4 S2 O6 113.0(5) . . ?
O5 S2 O6 109.3(5) . . ?
O4 S2 C19 107.3(5) . . ?
O5 S2 C19 105.7(5) . . ?
O6 S2 C19 106.8(5) . . ?
N1 C1 C2 123.0(11) . . ?
C1 C2 C3 120.5(10) . . ?
C4 C3 C2 114.7(10) . . ?
C4 C3 C6 123.1(10) . . ?
C2 C3 C6 122.2(9) . . ?
C3 C4 C5 122.1(10) . . ?
N1 C5 C4 122.8(10) . . ?
N2 C6 C7 123.1(10) . . ?
N2 C6 C3 115.5(9) . . ?
C7 C6 C3 121.5(9) . . ?
C6 C7 C8 119.6(10) . . ?
C9 C8 C7 118.4(9) . . ?
C9 C8 C16 118.8(10) . . ?
C7 C8 C16 122.8(9) . . ?
C8 C9 C10 118.9(10) . . ?
N2 C10 C9 121.5(9) . . ?
N2 C10 C11 118.6(9) . . ?
C9 C10 C11 119.9(10) . . ?
C15 C11 C12 116.4(10) . . ?
C15 C11 C10 124.8(10) . . ?
C12 C11 C10 118.8(10) . . ?
C11 C12 C13 119.4(11) . . ?
N3 C13 C12 124.1(11) . . ?
N3 C14 C15 122.1(11) . . ?
C11 C15 C14 122.3(10) . . ?
C21 C16 C17 118.9(10) . . ?
C21 C16 C8 116.5(9) . . ?
C17 C16 C8 124.6(10) . . ?
C18 C17 C16 119.1(10) . . ?
C18 C17 S1 117.7(9) . . ?
C16 C17 S1 123.2(8) . . ?
C17 C18 C19 122.7(11) . . ?
C20 C19 C18 117.9(10) . . ?
C20 C19 S2 120.0(9) . . ?
C18 C19 S2 122.1(9) . . ?
C19 C20 C21 120.9(11) . . ?
C16 C21 C20 120.3(10) . . ?
C5 N1 C1 116.8(10) . . ?
C5 N1 Pb1 118.7(7) . . ?
C1 N1 Pb1 124.4(7) . . ?
C6 N2 C10 118.6(8) . . ?
C14 N3 C13 115.7(10) . . ?
C14 N3 Pb1 126.5(8) . 1_556 ?
C13 N3 Pb1 117.5(8) . 1_556 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.150
####################################################################### 
# 
# 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_Pb3
_database_code_depnum_ccdc_archive 'CCDC 1058705'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H19 K N4 O12 Pb S2'
_chemical_formula_weight         829.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I4(1)/a  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   13.770(2)
_cell_length_b                   13.770(2)
_cell_length_c                   59.621(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11306(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4351
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      21.81

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6432
_exptl_absorpt_coefficient_mu    6.331
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.3641
_exptl_absorpt_correction_T_max  0.4502
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32869
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.63
_reflns_number_total             6518
_reflns_number_gt                3586
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
The following restraints were used:
DFIX 1.25 0.05 N4 O7 N4 O8 N4 O9
DFIX 2.2 0.05 O7 O8 O8 O9 O9 O7
ISOR 0.02 0.02 N4 O7 O8 O9 
SIMU 0.02 0.02 N4 O7 O8 O9 
;

_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)+(0.1094P)²+205.4492P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6518
_refine_ls_number_parameters     371
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0801
_refine_ls_wR_factor_ref         0.2468
_refine_ls_wR_factor_gt          0.2108
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.003
_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
Pb1 Pb 0.74310(5) 0.73654(4) 1.097741(9) 0.0656(3) Uani 1 1 d . . .
K1 K 1.5252(4) 0.5715(6) 0.97283(11) 0.143(2) Uani 1 1 d . . .
S1 S 0.7489(3) 0.4520(2) 0.94061(5) 0.0520(8) Uani 1 1 d . . .
S2 S 0.7192(3) 0.6301(4) 0.85976(5) 0.0711(12) Uani 1 1 d . . .
C1 C 0.8898(10) 0.6638(10) 1.05498(19) 0.052(3) Uani 1 1 d . . .
H1A H 0.9315 0.6599 1.0672 0.062 Uiso 1 1 calc R . .
C2 C 0.9282(9) 0.6475(9) 1.03376(18) 0.044(3) Uani 1 1 d . . .
H2A H 0.9932 0.6310 1.0320 0.052 Uiso 1 1 calc R . .
C3 C 0.8676(9) 0.6563(8) 1.01509(17) 0.038(3) Uani 1 1 d . . .
C4 C 0.7699(9) 0.6761(10) 1.01939(19) 0.050(3) Uani 1 1 d . . .
H4A H 0.7261 0.6802 1.0075 0.060 Uiso 1 1 calc R . .
C5 C 0.7381(10) 0.6897(10) 1.0409(2) 0.058(3) Uani 1 1 d . . .
H5A H 0.6727 0.7032 1.0432 0.069 Uiso 1 1 calc R . .
C6 C 0.9065(9) 0.6384(8) 0.99226(17) 0.041(3) Uani 1 1 d . . .
C7 C 0.8471(10) 0.6397(9) 0.97321(18) 0.047(3) Uani 1 1 d . . .
H7A H 0.7806 0.6509 0.9743 0.057 Uiso 1 1 calc R . .
C8 C 0.8922(9) 0.6236(8) 0.95256(17) 0.042(3) Uani 1 1 d . . .
C9 C 0.9912(9) 0.6066(8) 0.95182(18) 0.041(3) Uani 1 1 d . . .
H9A H 1.0220 0.5950 0.9382 0.049 Uiso 1 1 calc R . .
C10 C 1.0441(9) 0.6071(8) 0.97165(18) 0.040(3) Uani 1 1 d . . .
C11 C 1.1523(10) 0.5947(8) 0.97172(19) 0.046(3) Uani 1 1 d . . .
C12 C 1.2042(11) 0.5746(11) 0.9523(2) 0.061(4) Uani 1 1 d . . .
H12A H 1.1717 0.5714 0.9387 0.073 Uiso 1 1 calc R . .
C13 C 1.3013(13) 0.5596(14) 0.9529(3) 0.084(5) Uani 1 1 d . . .
H13A H 1.3343 0.5436 0.9398 0.101 Uiso 1 1 calc R . .
C14 C 1.3030(11) 0.5841(14) 0.9918(3) 0.075(4) Uani 1 1 d . . .
H14A H 1.3364 0.5862 1.0053 0.090 Uiso 1 1 calc R . .
C15 C 1.2041(10) 0.5981(11) 0.9916(2) 0.056(3) Uani 1 1 d . . .
H15A H 1.1716 0.6101 1.0050 0.068 Uiso 1 1 calc R . .
C16 C 0.8394(9) 0.6260(9) 0.93069(17) 0.044(3) Uani 1 1 d . . .
C17 C 0.7780(9) 0.5527(8) 0.92335(18) 0.042(3) Uani 1 1 d . . .
C18 C 0.7398(10) 0.5557(10) 0.90150(18) 0.050(3) Uani 1 1 d . . .
H18A H 0.6983 0.5068 0.8966 0.060 Uiso 1 1 calc R . .
C19 C 0.7637(10) 0.6306(10) 0.8873(2) 0.053(3) Uani 1 1 d . . .
C20 C 0.8236(12) 0.7046(11) 0.8942(2) 0.065(4) Uani 1 1 d . . .
H20A H 0.8406 0.7545 0.8845 0.078 Uiso 1 1 calc R . .
C21 C 0.8586(10) 0.7028(10) 0.9165(2) 0.059(4) Uani 1 1 d . . .
H21A H 0.8956 0.7546 0.9217 0.070 Uiso 1 1 calc R . .
N1 N 0.7970(8) 0.6845(7) 1.05888(16) 0.049(3) Uani 1 1 d . . .
N2 N 1.0031(7) 0.6235(7) 0.99154(15) 0.042(2) Uani 1 1 d . . .
N3 N 1.3517(10) 0.5677(13) 0.9728(3) 0.092(5) Uani 1 1 d . . .
O1 O 0.8401(7) 0.4146(7) 0.94838(17) 0.069(3) Uani 1 1 d . . .
O1W O 0.8997(10) 0.8342(11) 1.0931(3) 0.119(5) Uani 1 1 d . . .
O2 O 0.6888(8) 0.4906(8) 0.95869(16) 0.075(3) Uani 1 1 d . . .
O3 O 0.6941(7) 0.3849(7) 0.92615(15) 0.061(2) Uani 1 1 d . . .
O3W O 1.5019(12) 0.437(4) 0.9560(5) 0.39(3) Uani 1 1 d . . .
O4 O 0.7224(19) 0.5329(14) 0.8523(2) 0.176(9) Uani 1 1 d . . .
O5 O 0.6202(10) 0.6444(13) 0.86085(19) 0.119(5) Uani 1 1 d . . .
O6 O 0.7682(13) 0.6949(17) 0.8473(2) 0.149(8) Uani 1 1 d . . .
N4 N 0.569(3) 0.582(2) 1.1010(5) 0.200(7) Uani 1 1 d DU . .
O7 O 0.5868(17) 0.6418(19) 1.0847(4) 0.196(8) Uani 1 1 d DU . .
O8 O 0.533(2) 0.4963(18) 1.1037(5) 0.211(9) Uani 1 1 d DU . .
O9 O 0.5992(15) 0.6219(15) 1.1217(3) 0.175(7) Uani 1 1 d DU . .
O2W O 1.5000 0.7500 1.0085(7) 0.30(3) Uani 1 2 d S . .
O4W O 1.5000 0.7500 0.9207(15) 0.52(6) Uani 1 2 d S . .


_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
Pb1 N1 2.536(10) . ?
Pb1 O1W 2.557(15) . ?
Pb1 O3 2.580(10) 14_557 ?
Pb1 O7 2.64(2) . ?
Pb1 O5 2.667(16) 8_454 ?
K1 O3W 2.13(4) . ?
K1 N3 2.390(15) . ?
K1 O2 2.651(13) 1_655 ?
K1 O2W 3.27(3) . ?
K1 C14 3.266(16) . ?
K1 C13 3.31(2) . ?
K1 K1 3.855(14) 9_867 ?
K1 K1 4.964(16) 6_764 ?
S1 O1 1.434(10) . ?
S1 O2 1.459(10) . ?
S1 O3 1.472(9) . ?
S1 C17 1.773(12) . ?
S2 O6 1.345(14) . ?
S2 O5 1.378(14) . ?
S2 O4 1.411(19) . ?
S2 C19 1.752(12) . ?
C1 N1 1.330(16) . ?
C1 C2 1.389(16) . ?
C2 C3 1.396(15) . ?
C3 C4 1.396(17) . ?
C3 C6 1.484(14) . ?
C4 C5 1.369(17) . ?
C5 N1 1.344(17) . ?
C6 N2 1.347(15) . ?
C6 C7 1.400(16) . ?
C7 C8 1.397(16) . ?
C8 C9 1.385(17) . ?
C8 C16 1.493(15) . ?
C9 C10 1.388(15) . ?
C10 N2 1.332(14) . ?
C10 C11 1.499(18) . ?
C11 C12 1.387(17) . ?
C11 C15 1.384(17) . ?
C12 C13 1.35(2) . ?
C13 N3 1.38(2) . ?
C14 N3 1.33(2) . ?
C14 C15 1.38(2) . ?
C16 C17 1.386(17) . ?
C16 C21 1.381(18) . ?
C17 C18 1.406(15) . ?
C18 C19 1.375(18) . ?
C19 C20 1.374(19) . ?
C20 C21 1.412(17) . ?
O2 K1 2.651(12) 1_455 ?
O3 Pb1 2.580(10) 14_547 ?
O5 Pb1 2.667(16) 7_544 ?
N4 O8 1.29(3) . ?
N4 O7 1.30(3) . ?
N4 O9 1.41(3) . ?
O2W K1 3.27(3) 6_764 ?

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 Pb1 O1W 78.7(5) . . ?
N1 Pb1 O3 78.2(3) . 14_557 ?
O1W Pb1 O3 75.2(4) . 14_557 ?
N1 Pb1 O7 80.1(6) . . ?
O1W Pb1 O7 156.6(6) . . ?
O3 Pb1 O7 90.9(6) 14_557 . ?
N1 Pb1 O5 83.3(4) . 8_454 ?
O1W Pb1 O5 70.3(5) . 8_454 ?
O3 Pb1 O5 143.4(4) 14_557 8_454 ?
O7 Pb1 O5 116.9(7) . 8_454 ?
O3W K1 N3 80.2(7) . . ?
O3W K1 O2 67.2(5) . 1_655 ?
N3 K1 O2 147.2(6) . 1_655 ?
O3W K1 O2W 160.7(9) . . ?
N3 K1 O2W 84.9(4) . . ?
O2 K1 O2W 127.8(3) 1_655 . ?
O3W K1 C14 93.9(7) . . ?
N3 K1 C14 20.7(5) . . ?
O2 K1 C14 158.2(5) 1_655 . ?
O2W K1 C14 68.6(3) . . ?
O3W K1 C13 69.3(7) . . ?
N3 K1 C13 21.1(4) . . ?
O2 K1 C13 131.1(5) 1_655 . ?
O2W K1 C13 99.9(4) . . ?
C14 K1 C13 41.7(4) . . ?
O3W K1 K1 85.7(12) . 9_867 ?
N3 K1 K1 79.0(5) . 9_867 ?
O2 K1 K1 101.9(4) 1_655 9_867 ?
O2W K1 K1 79.6(6) . 9_867 ?
C14 K1 K1 64.4(3) . 9_867 ?
C13 K1 K1 96.2(4) . 9_867 ?
O3W K1 K1 147.1(11) . 6_764 ?
N3 K1 K1 83.2(5) . 6_764 ?
O2 K1 K1 122.4(3) 1_655 6_764 ?
O2W K1 K1 40.6(6) . 6_764 ?
C14 K1 K1 79.4(4) . 6_764 ?
C13 K1 K1 85.3(4) . 6_764 ?
K1 K1 K1 118.7(2) 9_867 6_764 ?
O1 S1 O2 112.9(7) . . ?
O1 S1 O3 114.4(6) . . ?
O2 S1 O3 111.8(6) . . ?
O1 S1 C17 105.7(6) . . ?
O2 S1 C17 105.8(6) . . ?
O3 S1 C17 105.5(5) . . ?
O6 S2 O5 115.3(12) . . ?
O6 S2 O4 116.0(14) . . ?
O5 S2 O4 100.5(13) . . ?
O6 S2 C19 109.9(8) . . ?
O5 S2 C19 107.5(7) . . ?
O4 S2 C19 106.8(8) . . ?
N1 C1 C2 124.0(11) . . ?
C1 C2 C3 119.0(11) . . ?
C4 C3 C2 116.5(10) . . ?
C4 C3 C6 123.3(10) . . ?
C2 C3 C6 120.1(11) . . ?
C5 C4 C3 120.4(11) . . ?
N1 C5 C4 123.2(13) . . ?
N2 C6 C7 123.6(10) . . ?
N2 C6 C3 114.3(10) . . ?
C7 C6 C3 122.1(11) . . ?
C6 C7 C8 116.9(12) . . ?
C9 C8 C7 119.5(10) . . ?
C9 C8 C16 117.1(10) . . ?
C7 C8 C16 123.3(12) . . ?
C8 C9 C10 119.2(10) . . ?
N2 C10 C9 122.5(11) . . ?
N2 C10 C11 115.9(10) . . ?
C9 C10 C11 121.5(10) . . ?
C12 C11 C15 117.0(13) . . ?
C12 C11 C10 122.2(11) . . ?
C15 C11 C10 120.7(11) . . ?
C13 C12 C11 121.2(14) . . ?
N3 C13 C12 120.5(14) . . ?
N3 C13 K1 38.6(8) . . ?
C12 C13 K1 157.3(12) . . ?
N3 C14 C15 121.0(14) . . ?
N3 C14 K1 39.3(8) . . ?
C15 C14 K1 158.8(11) . . ?
C14 C15 C11 120.8(13) . . ?
C17 C16 C21 118.7(10) . . ?
C17 C16 C8 123.8(10) . . ?
C21 C16 C8 117.4(11) . . ?
C16 C17 C18 120.0(11) . . ?
C16 C17 S1 121.6(8) . . ?
C18 C17 S1 118.4(10) . . ?
C19 C18 C17 120.2(12) . . ?
C18 C19 C20 121.0(11) . . ?
C18 C19 S2 119.4(10) . . ?
C20 C19 S2 119.6(10) . . ?
C19 C20 C21 118.3(11) . . ?
C16 C21 C20 121.7(12) . . ?
C1 N1 C5 116.8(11) . . ?
C1 N1 Pb1 120.1(8) . . ?
C5 N1 Pb1 122.4(9) . . ?
C10 N2 C6 118.2(10) . . ?
C14 N3 C13 119.3(14) . . ?
C14 N3 K1 119.9(12) . . ?
C13 N3 K1 120.3(11) . . ?
S1 O2 K1 150.5(7) . 1_455 ?
S1 O3 Pb1 133.4(6) . 14_547 ?
S2 O5 Pb1 114.8(10) . 7_544 ?
O8 N4 O7 138(3) . . ?
O8 N4 O9 111(3) . . ?
O7 N4 O9 111(3) . . ?
N4 O7 Pb1 104(2) . . ?
K1 O2W K1 98.9(12) 6_764 . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         3.861
_refine_diff_density_min         -1.993
_refine_diff_density_rms         0.192
####################################################################
