Poly[μ₃-1,3-dithiol­ane-2-methanol-κ³S:S:S′-μ-nitrato-silver(I)]

The title compound, [Ag(NO₃)(C₄H₈OS₂)]_n, is a polymeric complex in which each Ag atom is coordinated by three S atoms from three different dithiol­ane ligands, forming a T-shaped coordination configuration. The Ag atoms and dithiol­ane ligands construct a linear backbone via the Ag—S bonds. The backbones are linked into a three-dimensional network by bridging nitrate groups and O—H...O hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.033
• wR factor = 0.079
• Data-to-parameter ratio = 18.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.96
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.80
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N1
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.29 Ratio

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

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

Poly[µ₃-1,3-dithiolane-2-methanol-κ₃S:S:S'-µ-nitrato-silver(I)]

Crystal data

[Ag(NO3)(C4H8OS2)]	F(000) = 600
Mr = 306.10	Dx = 2.386 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 9.4659 (7) Å	Cell parameters from 3583 reflections
b = 6.6555 (5) Å	θ = 3.0–27.7°
c = 13.9767 (10) Å	µ = 2.83 mm^−1
β = 104.597 (1)°	T = 296 K
V = 852.11 (11) Å^3	Thin-plate, colorless
Z = 4	0.32 × 0.27 × 0.02 mm

Data collection

Bruker APEX diffractometer	2039 independent reflections
Radiation source: fine-focus sealed tube	1870 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.017
Detector resolution: 83.33 pixels mm^-1	θmax = 28.3°, θmin = 2.4°
φ and ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Bruker, 1997)	k = −8→8
Tmin = 0.415, Tmax = 0.945	l = −18→18
7522 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.079	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0363P)^2 + 1.5745P] where P = (Fo^2 + 2Fc^2)/3
2039 reflections	(Δ/σ)max = 0.001
110 parameters	Δρmax = 1.45 e Å^−3
0 restraints	Δρmin = −0.52 e Å^−3

Special details

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

	x	y	z	Uiso*/Ueq
Ag1	0.63194 (3)	0.20899 (4)	0.33123 (2)	0.04569 (12)
C1	0.5138 (4)	0.7103 (5)	0.2533 (2)	0.0349 (7)
H1	0.5111	0.6328	0.1933	0.042*
S2	0.68952 (9)	0.84145 (12)	0.28994 (6)	0.03357 (18)
C3	0.7608 (4)	0.7233 (5)	0.4093 (3)	0.0382 (7)
H3A	0.8171	0.6049	0.4023	0.046*
H3B	0.8238	0.8159	0.4542	0.046*
C4	0.6323 (4)	0.6654 (5)	0.4492 (2)	0.0366 (7)
H4A	0.5878	0.7844	0.4692	0.044*
H4B	0.6637	0.5782	0.5062	0.044*
S5	0.50275 (9)	0.53613 (11)	0.35123 (6)	0.03304 (18)
C6	0.3864 (4)	0.8592 (6)	0.2308 (3)	0.0545 (10)
H6A	0.3921	0.9401	0.1742	0.065*
H6B	0.2955	0.7846	0.2131	0.065*
O7	0.3841 (3)	0.9871 (4)	0.3100 (3)	0.0612 (8)
H7	0.3474	0.9282	0.3494	0.092*
N1	0.8387 (4)	0.1954 (4)	0.5396 (2)	0.0463 (7)
O1	0.7037 (3)	0.1576 (5)	0.5224 (2)	0.0633 (8)
O2	0.8892 (4)	0.2376 (6)	0.4687 (3)	0.0711 (9)
O3	0.9156 (4)	0.1854 (5)	0.6244 (2)	0.0711 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ag1	0.0566 (2)	0.02957 (16)	0.04904 (19)	0.00501 (11)	0.00982 (13)	−0.00315 (11)
C1	0.0409 (17)	0.0282 (15)	0.0339 (16)	−0.0053 (13)	0.0062 (13)	0.0006 (12)
S2	0.0378 (4)	0.0266 (4)	0.0403 (4)	−0.0035 (3)	0.0172 (3)	0.0002 (3)
C3	0.0371 (17)	0.0326 (16)	0.0422 (18)	−0.0001 (13)	0.0046 (14)	0.0000 (14)
C4	0.0466 (18)	0.0331 (16)	0.0320 (15)	−0.0004 (14)	0.0134 (14)	−0.0006 (13)
S5	0.0348 (4)	0.0247 (3)	0.0418 (4)	−0.0023 (3)	0.0138 (3)	0.0025 (3)
C6	0.0407 (19)	0.0370 (19)	0.074 (3)	−0.0019 (16)	−0.0070 (18)	0.0151 (19)
O7	0.0517 (17)	0.0358 (14)	0.100 (2)	0.0099 (12)	0.0257 (17)	0.0076 (15)
N1	0.0554 (19)	0.0318 (15)	0.0447 (17)	0.0061 (13)	−0.0007 (15)	−0.0023 (13)
O1	0.0561 (18)	0.072 (2)	0.0610 (19)	0.0048 (16)	0.0126 (15)	−0.0060 (16)
O2	0.064 (2)	0.092 (3)	0.0556 (19)	−0.0078 (18)	0.0105 (16)	0.0148 (18)
O3	0.087 (2)	0.069 (2)	0.0434 (16)	0.0067 (18)	−0.0097 (16)	−0.0001 (15)

Geometric parameters (Å, º)

Ag1—S5	2.5468 (8)	C3—C4	1.510 (5)
Ag1—S2^i	2.6024 (9)	C3—H3A	0.9700
Ag1—O1	2.609 (3)	C3—H3B	0.9700
Ag1—O2	2.702 (4)	C4—S5	1.809 (3)
Ag1—S2^ii	2.8185 (8)	C4—H4A	0.9700
Ag1—O3^iii	3.171 (3)	C4—H4B	0.9700
C1—C6	1.531 (5)	C6—O7	1.401 (6)
C1—S5	1.816 (3)	C6—H6A	0.9700
C1—S2	1.833 (3)	C6—H6B	0.9700
C1—H1	0.9800	O7—H7	0.8200
S2—C3	1.814 (4)	N1—O3	1.227 (5)
S2—Ag1^iv	2.6024 (8)	N1—O2	1.236 (5)
S2—Ag1^v	2.8185 (8)	N1—O1	1.265 (4)
S5—Ag1—S2^i	163.97 (3)	C4—C3—H3B	110.2
S5—Ag1—O1	90.45 (8)	S2—C3—H3B	110.2
S2^i—Ag1—O1	95.10 (8)	H3A—C3—H3B	108.5
S5—Ag1—O2	103.49 (9)	C3—C4—S5	107.3 (2)
S2^i—Ag1—O2	91.29 (9)	C3—C4—H4A	110.3
O1—Ag1—O2	47.57 (10)	S5—C4—H4A	110.3
S5—Ag1—S2^ii	100.12 (3)	C3—C4—H4B	110.3
S2^i—Ag1—S2^ii	88.279 (17)	S5—C4—H4B	110.3
O1—Ag1—S2^ii	128.02 (7)	H4A—C4—H4B	108.5
O2—Ag1—S2^ii	80.56 (8)	C4—S5—C1	96.32 (15)
C6—C1—S5	112.1 (3)	C4—S5—Ag1	103.72 (12)
C6—C1—S2	111.2 (2)	C1—S5—Ag1	110.03 (11)
S5—C1—S2	108.30 (17)	O7—C6—C1	113.5 (3)
C6—C1—H1	108.4	O7—C6—H6A	108.9
S5—C1—H1	108.4	C1—C6—H6A	108.9
S2—C1—H1	108.4	O7—C6—H6B	108.9
C3—S2—C1	98.70 (16)	C1—C6—H6B	108.9
C3—S2—Ag1^iv	104.69 (12)	H6A—C6—H6B	107.7
C1—S2—Ag1^iv	106.47 (11)	C6—O7—H7	109.5
C3—S2—Ag1^v	106.08 (12)	O3—N1—O2	122.1 (4)
C1—S2—Ag1^v	108.81 (11)	O3—N1—O1	119.9 (4)
Ag1^iv—S2—Ag1^v	128.17 (3)	O2—N1—O1	118.0 (3)
C4—C3—S2	107.6 (2)	N1—O1—Ag1	99.1 (2)
C4—C3—H3A	110.2	N1—O2—Ag1	95.3 (2)
S2—C3—H3A	110.2

Symmetry codes: (i) x, y−1, z; (ii) −x+3/2, y−1/2, −z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) x, y+1, z; (v) −x+3/2, y+1/2, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7···O1^vi	0.82	2.05	2.843 (5)	162

Symmetry code: (vi) −x+1, −y+1, −z+1.