Poly[[{μ4-2,2′-[butane-1,4-diylbis(sulfanedi­yl)]bis­(1,3,4-thia­diazole)}silver(I)] perchlorate sesquihydrate]

Li, J.-J.; Zhu, W.-M.

doi:10.1107/S1600536812022957

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 6| June 2012| Page m845

doi:10.1107/S1600536812022957

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Poly[[{μ₄-2,2′-[butane-1,4-diylbis(sulfanediyl)]bis(1,3,4-thiadiazole)}silver(I)] perchlorate sesquihydrate]

Jia-Jia Li ^a and Wei-Min Zhu ^a ^*

^aCollege of Chemistry and Molecular Engineering, Zhengzhou University, Zhengzhou 450001, People's Republic of China
^*Correspondence e-mail: zhuwm@zzu.edu.cn

(Received 30 April 2012; accepted 19 May 2012; online 31 May 2012)

In the polymeric title compound, {[Ag(C₈H₁₀N₄S₄)]ClO₄·1.5H₂O}_n, the Ag^I atom has a slightly distorted trigonal-planar coordination geometry provided by three N-atom donors from the thiadiazole rings of three symmetry-related 2,2′-[butane-1,4-diylbis(sulfanediyl)]bis(1,3,4-thiadiazole) ligands. Centrosymmetrically related Ag^I atoms are bridged by the N–N fragments of rings, forming six-membered dinuclear metallacycles, which are further linked by the alkyl spacers of the thiadiazole ligands into a layer network extending parallel to (0-21). The crystal structure is stabilized by intermolecular O—H⋯O hydrogen bonds. The O atoms of the perchlorate anion and one water molecule are disordered over two sets of sites with refined occupancy ratios of 0.640 (6):0.360 (6) and 0.663 (11):0.337 (11), respectively. The second water molecule shows half-occupancy.

Related literature

For related polymeric Ag^I complexes, see: Yu et al. (2006 ); Wang & Ma (2007 ).

Experimental

Crystal data

[Ag(C₈H₁₀N₄S₄)]ClO₄·1.5H₂O
M_r = 524.79
Triclinic, $[P \overline 1]$
a = 10.076 (12) Å
b = 10.08 (2) Å
c = 10.137 (12) Å
α = 92.02 (2)°
β = 119.727 (14)°
γ = 94.20 (2)°
V = 889 (3) Å³
Z = 2
Mo Kα radiation
μ = 1.78 mm⁻¹
T = 291 K
0.29 × 0.04 × 0.04 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1997 ) T_min = 0.624, T_max = 0.940
6708 measured reflections
3237 independent reflections
1834 reflections with I > 2σ(I)
R_int = 0.043

Refinement

R[F² > 2σ(F²)] = 0.055
wR(F²) = 0.143
S = 1.00
3237 reflections
214 parameters
236 restraints
H-atom parameters constrained
Δρ_max = 0.64 e Å⁻³
Δρ_min = −0.75 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H6W⋯O4′ⁱ	0.85	2.15	2.71 (3)	123
O6—H6W⋯O2ⁱ	0.85	1.61	2.46 (4)	178
O6—H5W⋯O1ⁱⁱ	0.85	2.47	3.02 (6)	123
O6—H5W⋯O6ⁱⁱⁱ	0.85	2.36	3.10 (4)	146
O6—H5W⋯O4′ⁱⁱ	0.85	1.98	2.62 (6)	131
O5—H2W⋯O1ⁱ	0.85	2.42	3.27 (4)	179
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x, y+1, z+1; (iii) -x+1, -y+2, -z+2.

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812022957/rz2753sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812022957/rz2753Isup2.hkl

checkCIF report

Comment top

During the last decade, a great effort has been devoted to designing ligands capable of enforcing close metal contacts during the process of assembly or crystallization to form polynuclear complexes and coordination polymers, owing to these complexes are expected to produce specific structures, properties and reactivities, not found for mononuclear complexes. In particular, N,N'-linkage ligands such as 1,2-diazines, 1,2-diazoles, 1,2,4-triazoles and 1,3,4-thiadiazole are very versatile ligands that are able to bridge a wide range of intermetallic separations through two close adjacent N donors (Yu et al., 2006; Wang & Ma, 2007).

In the title compound (Fig. 1), the Ag metal is coordinated by three N donors from thiadiazole rings of three distinct 2,2'-(butane-1,4-diyldithio)-bis(1,3,4-thiadiazole) ligands in a slightly distorted trigonal planar coordination geometry, with the metal protruding 0.0172 (15) Å from the N₃ coordination plane. The Ag-N bond distances fall in the range 2.232 (8)-2.311 (9) Å. Centrosymmetrically related Ag metals are doubly bridged by the N-N fragments of thiadiazole rings of two distinct ligands to form six-membered dinuclear metallacycles. The Ag···Ag separation within the rings is 3.722 (4) Å, which is longer than the summed van der Waals radii of two free Ag ions (3.44 Å). The six-membered rings are linked by the alkyl spacers of the ligand into a two-dimensional layer network extending parallel to the (0 -2 1) plane (Fig. 2). Each Ag metal in the layer shows weak interactions with one S atom from an adjacent layer (Ag···S separation of 3.116 (5) Å), and with the oxygen atoms of the disordered ClO4^- anion, the shortest Ag···O separation being 2.816 (8) Å. The crystal structure is enforced by intermolecular O—H···O hydrogen bonds (Table 1).

Related literature top

For related polymeric Ag^I complexes, see: Yu et al. (2006); Wang & Ma (2007).

Experimental top

The reaction of bis[2,2'-(butane-1,4-diyldithio)-bis(1,3,4-thiadiazole)] (0.1 mmol) with AgCl0₄ (0.1 mmol) in MeOH (10 mL) for a few minutes afforded a light white solid, which was filtered, washed with acetone, and dried in air. Single crystals of the title compound suitable for X-ray analysis were obtained by slow diffusion of Et₂O into an acetonitrile solution of the solid.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The asymmetric unit of the title compound, with displacement ellipsoids drawn at the 30% probability level. Hydrogen atoms are omitted.
	Fig. 2. Partial crystal packing of the title compound showing the two-dimensional layer structure. Hydrogen atoms, water molecules and perchlorate anions are omitted.

Poly[[{µ₄-2,2'-[butane-1,4-diylbis(sulfanediyl)]bis(1,3,4- thiadiazole)}silver(I)] perchlorate sesquihydrate] top

Crystal data top

[Ag(C₈H₁₀N₄S₄)]ClO₄·1.5H₂O	Z = 2
M_r = 524.79	F(000) = 522
Triclinic, P1	D_x = 1.961 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.076 (12) Å	Cell parameters from 954 reflections
b = 10.08 (2) Å	θ = 2.3–19.5°
c = 10.137 (12) Å	µ = 1.78 mm⁻¹
α = 92.02 (2)°	T = 291 K
β = 119.727 (14)°	Block, colourless
γ = 94.20 (2)°	0.29 × 0.04 × 0.04 mm
V = 889 (3) Å³

Data collection top

Bruker SMART CCD area-detector diffractometer	3237 independent reflections
Radiation source: fine-focus sealed tube	1834 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.043
phi and ω scans	θ_max = 25.5°, θ_min = 2.9°
Absorption correction: multi-scan (SADABS; Bruker, 1997)	h = −12→12
T_min = 0.624, T_max = 0.940	k = −12→11
6708 measured reflections	l = −12→12

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.055	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.143	H-atom parameters constrained
S = 1.00	w = 1/[σ²(F_o²) + (0.0596P)² + 0.9001P] where P = (F_o² + 2F_c²)/3
3237 reflections	(Δ/σ)_max < 0.001
214 parameters	Δρ_max = 0.64 e Å⁻³
236 restraints	Δρ_min = −0.75 e Å⁻³

Crystal data top

[Ag(C₈H₁₀N₄S₄)]ClO₄·1.5H₂O	γ = 94.20 (2)°
M_r = 524.79	V = 889 (3) Å³
Triclinic, P1	Z = 2
a = 10.076 (12) Å	Mo Kα radiation
b = 10.08 (2) Å	µ = 1.78 mm⁻¹
c = 10.137 (12) Å	T = 291 K
α = 92.02 (2)°	0.29 × 0.04 × 0.04 mm
β = 119.727 (14)°

Data collection top

Bruker SMART CCD area-detector diffractometer	3237 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 1997)	1834 reflections with I > 2σ(I)
T_min = 0.624, T_max = 0.940	R_int = 0.043
6708 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.055	236 restraints
wR(F²) = 0.143	H-atom parameters constrained
S = 1.00	Δρ_max = 0.64 e Å⁻³
3237 reflections	Δρ_min = −0.75 e Å⁻³
214 parameters

Special details top

Geometry. 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.

Refinement. 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
O5	0.5870 (14)	0.9980 (12)	0.5479 (13)	0.111 (3)	0.663 (11)
H1W	0.5826	0.9510	0.4743	0.166*	0.663 (11)
H2W	0.5493	0.9603	0.5974	0.166*	0.663 (11)
O5'	0.709 (3)	0.984 (2)	0.599 (3)	0.111 (3)	0.337 (11)
H3W	0.6772	0.9410	0.5137	0.166*	0.337 (11)
H4W	0.6737	0.9609	0.6564	0.166*	0.337 (11)
Cl1	0.6364 (2)	0.2700 (2)	0.2629 (3)	0.0868 (8)	0.640 (6)
O1	0.5621 (6)	0.1488 (5)	0.2654 (8)	0.105 (2)	0.640 (6)
O2	0.7031 (8)	0.2400 (7)	0.1638 (8)	0.107 (2)	0.640 (6)
O3	0.7646 (7)	0.3177 (6)	0.4046 (6)	0.093 (2)	0.640 (6)
O4	0.5392 (6)	0.3695 (5)	0.1966 (8)	0.098 (2)	0.640 (6)
Cl1'	0.6364 (2)	0.2700 (2)	0.2629 (3)	0.0868 (8)	0.360 (6)
O1'	0.5900 (8)	0.3025 (7)	0.3739 (8)	0.105 (2)	0.360 (6)
O2'	0.7956 (5)	0.2706 (6)	0.3363 (8)	0.107 (2)	0.360 (6)
O3'	0.5824 (7)	0.3645 (6)	0.1525 (7)	0.093 (2)	0.360 (6)
O4'	0.5605 (7)	0.1401 (5)	0.1931 (7)	0.098 (2)	0.360 (6)
Ag1	0.28732 (7)	0.49669 (7)	0.38379 (8)	0.0710 (3)
S1	0.4338 (2)	0.2152 (2)	0.7857 (2)	0.0592 (6)
S2	0.1184 (2)	0.28824 (19)	0.5359 (2)	0.0517 (5)
S3	−0.2397 (2)	0.5507 (2)	0.0592 (2)	0.0525 (5)
S4	−0.1933 (2)	0.74107 (19)	−0.1386 (2)	0.0539 (5)
N1	0.5493 (7)	0.3652 (6)	0.6644 (7)	0.0519 (16)
N2	0.3926 (6)	0.3663 (6)	0.5770 (6)	0.0464 (15)
N3	0.0497 (7)	0.5526 (6)	0.2226 (6)	0.0488 (15)
N4	0.0286 (6)	0.6374 (5)	0.1089 (6)	0.0433 (14)
C1	0.5838 (9)	0.2893 (8)	0.7730 (9)	0.057 (2)
H1	0.6850	0.2755	0.8411	0.069*
C2	0.3171 (8)	0.2935 (7)	0.6263 (8)	0.0424 (17)
C3	0.0689 (9)	0.1618 (8)	0.6326 (9)	0.054 (2)
H3A	0.1430	0.1754	0.7408	0.065*
H3B	−0.0309	0.1755	0.6198	0.065*
C4	0.0641 (9)	0.0183 (8)	0.5792 (8)	0.055 (2)
H4A	0.1607	0.0053	0.5839	0.065*
H4B	0.0524	−0.0404	0.6473	0.065*
C5	−0.0794 (9)	0.5012 (8)	0.2069 (9)	0.0518 (19)
H5	−0.0839	0.4410	0.2724	0.062*
C6	−0.1156 (8)	0.6454 (6)	0.0185 (7)	0.0401 (16)
C7	−0.0201 (9)	0.8336 (8)	−0.1127 (9)	0.060 (2)
H7A	0.0559	0.7718	−0.0924	0.072*
H7B	−0.0431	0.8718	−0.2073	0.072*
C8	0.0493 (10)	0.9440 (8)	0.0136 (10)	0.068 (2)
H8A	0.0685	0.9068	0.1077	0.082*
H8B	0.1475	0.9798	0.0268	0.082*
O6	0.337 (2)	0.974 (2)	0.981 (2)	0.169 (8)	0.50
H5W	0.4339	0.9960	1.0303	0.254*	0.50
H6W	0.3215	0.9007	0.9296	0.254*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O5	0.104 (6)	0.128 (6)	0.102 (6)	0.027 (5)	0.051 (5)	0.015 (5)
O5'	0.104 (6)	0.128 (6)	0.102 (6)	0.027 (5)	0.051 (5)	0.015 (5)
Cl1	0.0565 (13)	0.0827 (16)	0.0970 (17)	0.0042 (11)	0.0195 (12)	0.0245 (14)
O1	0.099 (4)	0.099 (4)	0.109 (4)	−0.007 (4)	0.048 (3)	0.013 (4)
O2	0.084 (4)	0.116 (5)	0.110 (4)	0.006 (3)	0.041 (3)	0.010 (4)
O3	0.079 (4)	0.104 (4)	0.087 (4)	0.023 (3)	0.033 (3)	0.010 (3)
O4	0.084 (4)	0.092 (4)	0.105 (5)	0.018 (3)	0.035 (3)	0.011 (3)
Cl1'	0.0565 (13)	0.0827 (16)	0.0970 (17)	0.0042 (11)	0.0195 (12)	0.0245 (14)
O1'	0.099 (4)	0.099 (4)	0.109 (4)	−0.007 (4)	0.048 (3)	0.013 (4)
O2'	0.084 (4)	0.116 (5)	0.110 (4)	0.006 (3)	0.041 (3)	0.010 (4)
O3'	0.079 (4)	0.104 (4)	0.087 (4)	0.023 (3)	0.033 (3)	0.010 (3)
O4'	0.084 (4)	0.092 (4)	0.105 (5)	0.018 (3)	0.035 (3)	0.011 (3)
Ag1	0.0421 (4)	0.0867 (5)	0.0724 (5)	0.0093 (3)	0.0171 (3)	0.0441 (4)
S1	0.0534 (12)	0.0638 (14)	0.0507 (12)	0.0034 (10)	0.0179 (10)	0.0237 (10)
S2	0.0405 (10)	0.0521 (12)	0.0588 (12)	0.0008 (9)	0.0218 (9)	0.0155 (10)
S3	0.0385 (10)	0.0540 (12)	0.0567 (12)	0.0057 (9)	0.0173 (9)	0.0089 (10)
S4	0.0499 (11)	0.0509 (12)	0.0459 (11)	0.0124 (9)	0.0111 (9)	0.0139 (10)
N1	0.043 (4)	0.051 (4)	0.055 (4)	0.004 (3)	0.019 (3)	0.016 (3)
N2	0.037 (3)	0.047 (4)	0.048 (4)	0.003 (3)	0.015 (3)	0.017 (3)
N3	0.045 (4)	0.051 (4)	0.045 (4)	0.016 (3)	0.017 (3)	0.011 (3)
N4	0.037 (3)	0.039 (3)	0.050 (4)	0.009 (3)	0.018 (3)	0.011 (3)
C1	0.045 (4)	0.058 (5)	0.057 (5)	0.002 (4)	0.016 (4)	0.013 (4)
C2	0.043 (4)	0.043 (4)	0.040 (4)	0.005 (3)	0.020 (3)	0.007 (3)
C3	0.050 (5)	0.060 (5)	0.055 (5)	−0.007 (4)	0.029 (4)	0.009 (4)
C4	0.058 (5)	0.054 (5)	0.051 (4)	−0.001 (4)	0.027 (4)	0.012 (4)
C5	0.052 (5)	0.048 (5)	0.053 (5)	0.011 (4)	0.024 (4)	0.014 (4)
C6	0.039 (4)	0.034 (4)	0.038 (4)	0.004 (3)	0.013 (3)	0.005 (3)
C7	0.073 (6)	0.054 (5)	0.053 (5)	0.019 (4)	0.029 (4)	0.020 (4)
C8	0.067 (6)	0.051 (5)	0.076 (6)	0.008 (4)	0.028 (5)	0.021 (5)
O6	0.162 (11)	0.181 (11)	0.168 (11)	0.007 (8)	0.087 (8)	0.007 (8)

Geometric parameters (Å, º) top

O5—O5ⁱ	1.53 (2)	S4—C6	1.750 (7)
O5—H1W	0.8502	S4—C7	1.810 (8)
O5—H2W	0.8498	N1—C1	1.280 (9)
O5—H3W	1.2854	N1—N2	1.376 (8)
O5—H4W	1.1129	N1—Ag1ⁱⁱ	2.323 (6)
O5'—H1W	1.2852	N2—C2	1.300 (8)
O5'—H3W	0.8500	N3—C5	1.296 (9)
O5'—H4W	0.8500	N3—N4	1.398 (8)
Cl1—O1	1.393 (5)	N4—C6	1.288 (8)
Cl1—O4	1.398 (5)	C1—H1	0.9300
Cl1—O3	1.408 (4)	C3—C4	1.516 (11)
Cl1—O2	1.494 (5)	C3—H3A	0.9700
Cl1'—O2'	1.394 (4)	C3—H3B	0.9700
Cl1'—O3'	1.415 (5)	C4—C4ⁱⁱⁱ	1.487 (14)
Cl1'—O4'	1.433 (5)	C4—H4A	0.9700
Cl1'—O1'	1.452 (4)	C4—H4B	0.9700
Ag1—N2	2.239 (6)	C5—H5	0.9300
Ag1—N3	2.259 (6)	C7—C8	1.505 (11)
Ag1—N1ⁱⁱ	2.323 (6)	C7—H7A	0.9700
S1—C1	1.701 (8)	C7—H7B	0.9700
S1—C2	1.720 (7)	C8—C8^iv	1.501 (15)
S2—C2	1.736 (7)	C8—H8A	0.9700
S2—C3	1.821 (7)	C8—H8B	0.9700
S3—C5	1.695 (8)	O6—H5W	0.8500
S3—C6	1.735 (7)	O6—H6W	0.8498

O5ⁱ—O5—H1W	88.4	C6—N4—N3	110.5 (5)
O5ⁱ—O5—H2W	74.1	N1—C1—S1	116.1 (6)
H1W—O5—H2W	116.5	N1—C1—H1	122.0
O5ⁱ—O5—H3W	129.1	S1—C1—H1	122.0
H2W—O5—H3W	121.9	N2—C2—S1	113.4 (5)
O5ⁱ—O5—H4W	139.9	N2—C2—S2	119.8 (5)
H1W—O5—H4W	108.3	S1—C2—S2	126.8 (4)
H2W—O5—H4W	65.8	C4—C3—S2	115.7 (6)
H3W—O5—H4W	75.3	C4—C3—H3A	108.4
H1W—O5'—H4W	94.7	S2—C3—H3A	108.4
H3W—O5'—H4W	120.0	C4—C3—H3B	108.4
O1—Cl1—O4	114.6	S2—C3—H3B	108.4
O1—Cl1—O3	114.0	H3A—C3—H3B	107.4
O4—Cl1—O3	111.4	C4ⁱⁱⁱ—C4—C3	112.3 (8)
O1—Cl1—O2	105.0	C4ⁱⁱⁱ—C4—H4A	109.1
O4—Cl1—O2	106.5	C3—C4—H4A	109.1
O3—Cl1—O2	104.3	C4ⁱⁱⁱ—C4—H4B	109.1
O2'—Cl1'—O3'	112.2	C3—C4—H4B	109.1
O2'—Cl1'—O4'	111.4	H4A—C4—H4B	107.9
O3'—Cl1'—O4'	109.7	N3—C5—S3	115.6 (6)
O2'—Cl1'—O1'	109.6	N3—C5—H5	122.2
O3'—Cl1'—O1'	107.8	S3—C5—H5	122.2
O4'—Cl1'—O1'	105.9	N4—C6—S3	115.6 (5)
N2—Ag1—N3	136.8 (2)	N4—C6—S4	125.7 (5)
N2—Ag1—N1ⁱⁱ	118.1 (2)	S3—C6—S4	118.7 (4)
N3—Ag1—N1ⁱⁱ	104.8 (2)	C8—C7—S4	115.0 (6)
C1—S1—C2	86.5 (4)	C8—C7—H7A	108.5
C2—S2—C3	102.5 (3)	S4—C7—H7A	108.5
C5—S3—C6	86.1 (4)	C8—C7—H7B	108.5
C6—S4—C7	100.3 (3)	S4—C7—H7B	108.5
C1—N1—N2	111.0 (6)	H7A—C7—H7B	107.5
C1—N1—Ag1ⁱⁱ	128.6 (5)	C8^iv—C8—C7	114.0 (9)
N2—N1—Ag1ⁱⁱ	120.1 (4)	C8^iv—C8—H8A	108.8
C2—N2—N1	113.0 (6)	C7—C8—H8A	108.8
C2—N2—Ag1	125.1 (5)	C8^iv—C8—H8B	108.8
N1—N2—Ag1	121.7 (4)	C7—C8—H8B	108.8
C5—N3—N4	112.3 (6)	H8A—C8—H8B	107.6
C5—N3—Ag1	127.3 (5)	H5W—O6—H6W	107.3
N4—N3—Ag1	119.7 (4)

C1—N1—N2—C2	1.4 (9)	N1—N2—C2—S2	177.2 (5)
Ag1ⁱⁱ—N1—N2—C2	−173.9 (5)	Ag1—N2—C2—S2	2.4 (9)
C1—N1—N2—Ag1	176.4 (5)	C1—S1—C2—N2	−0.4 (6)
Ag1ⁱⁱ—N1—N2—Ag1	1.1 (7)	C1—S1—C2—S2	−177.8 (5)
N3—Ag1—N2—C2	1.4 (8)	C3—S2—C2—N2	174.1 (6)
N1ⁱⁱ—Ag1—N2—C2	173.3 (6)	C3—S2—C2—S1	−8.6 (6)
N3—Ag1—N2—N1	−173.0 (4)	C2—S2—C3—C4	−80.2 (6)
N1ⁱⁱ—Ag1—N2—N1	−1.0 (7)	S2—C3—C4—C4ⁱⁱⁱ	−67.4 (10)
N2—Ag1—N3—C5	−8.1 (8)	N4—N3—C5—S3	−1.7 (8)
N1ⁱⁱ—Ag1—N3—C5	179.3 (6)	Ag1—N3—C5—S3	−172.0 (3)
N2—Ag1—N3—N4	−177.8 (4)	C6—S3—C5—N3	1.0 (6)
N1ⁱⁱ—Ag1—N3—N4	9.6 (5)	N3—N4—C6—S3	−0.8 (8)
C5—N3—N4—C6	1.6 (8)	N3—N4—C6—S4	179.6 (5)
Ag1—N3—N4—C6	172.7 (5)	C5—S3—C6—N4	0.0 (6)
N2—N1—C1—S1	−1.8 (9)	C5—S3—C6—S4	179.6 (5)
Ag1ⁱⁱ—N1—C1—S1	173.0 (4)	C7—S4—C6—N4	−7.9 (7)
C2—S1—C1—N1	1.3 (7)	C7—S4—C6—S3	172.5 (4)
N1—N2—C2—S1	−0.5 (8)	C6—S4—C7—C8	−74.4 (6)
Ag1—N2—C2—S1	−175.2 (3)	S4—C7—C8—C8^iv	−65.6 (11)

Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x, −y, −z+1; (iv) −x, −y+2, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6W···O4′ⁱⁱ	0.85	2.15	2.71 (3)	123
O6—H6W···O2ⁱⁱ	0.85	1.61	2.46 (4)	178
O6—H5W···O1^v	0.85	2.47	3.02 (6)	123
O6—H5W···O6^vi	0.85	2.36	3.10 (4)	146
O6—H5W···O4′^v	0.85	1.98	2.62 (6)	131
O5—H2W···O1ⁱⁱ	0.85	2.42	3.27 (4)	179

Symmetry codes: (ii) −x+1, −y+1, −z+1; (v) x, y+1, z+1; (vi) −x+1, −y+2, −z+2.

Experimental details

Crystal data
Chemical formula	[Ag(C₈H₁₀N₄S₄)]ClO₄·1.5H₂O
M_r	524.79
Crystal system, space group	Triclinic, P1
Temperature (K)	291
a, b, c (Å)	10.076 (12), 10.08 (2), 10.137 (12)
α, β, γ (°)	92.02 (2), 119.727 (14), 94.20 (2)
V (Å³)	889 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.78
Crystal size (mm)	0.29 × 0.04 × 0.04

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 1997)
T_min, T_max	0.624, 0.940
No. of measured, independent and observed [I > 2σ(I)] reflections	6708, 3237, 1834
R_int	0.043
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.055, 0.143, 1.00
No. of reflections	3237
No. of parameters	214
No. of restraints	236
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.64, −0.75

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6W···O4'ⁱ	0.85	2.15	2.71 (3)	123
O6—H6W···O2ⁱ	0.85	1.61	2.46 (4)	178
O6—H5W···O1ⁱⁱ	0.85	2.47	3.02 (6)	123
O6—H5W···O6ⁱⁱⁱ	0.85	2.36	3.10 (4)	146
O6—H5W···O4'ⁱⁱ	0.85	1.98	2.62 (6)	131
O5—H2W···O1ⁱ	0.85	2.42	3.27 (4)	179

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y+1, z+1; (iii) −x+1, −y+2, −z+2.

References

Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wang, C. C. & Ma, H. Y. (2007). Z. Kristallogr. New Cryst. Struct. 222, 101–104. CAS Google Scholar
Yu, J. H., Ding, C. J., Han, K. F., Zhang, S. W. & Guo, H. Y. (2006). Chin. J. Inorg. Chem. 22, 607–611. CAS Google Scholar

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