catena-Poly[[(3-methyl­sulfanyl-1,2,4-thia­diazole-5-thiol­ato)sodium]di-μ-aqua-κ⁴O:O]

The crystal structure of the title compound, [Na(C₃H₃N₂S₃)(H₂O)₂]_n, features polymeric chains made up of O...O edge-shared NaSN(H₂O)₄ units running along the b axis. The Na⁺ ion and all non-H atoms of the thia­diazole ligand lie on a mirror plane.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](S-N) = 0.003 Å
• R factor = 0.024
• wR factor = 0.064
• Data-to-parameter ratio = 13.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.595          5
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?
PLAT774_ALERT_1_C Suspect X-Y Bond in CIF:   NA1    --  NA1     ..       3.88 Ang.
PLAT774_ALERT_1_C Suspect X-Y Bond in CIF:   NA1    --  NA1     ..       3.88 Ang.

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C3 H7 N2 Na1 O2 S3
            Atom count from _chemical_formula_moiety:
PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.31 Ratio

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

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 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
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

---

S1. Comment

In the title compound (Fig.1), each Na⁺ ion has a six-coordinate environment formed by a S atom and a N atom of the 3-methylsulfanyl-1,2,4-thiadiazole-5-thiolate ligand, and four bridging water O atoms O1, O1A, O1B and O1C. The adjacent NaSNO₄ units share O1···O1A and O1B···O1C edges, producing chains running along the b axis (Fig. 2). Similar chains were found in the crystal structure of sodium carboxynitrobenzoate tetrahydrate (Guo, 2004). The Na—O [2.4493 (16) and 2.4736 (16) Å], Na—S [3.1271 (14) Å] and Na—N [2.467 (2) Å] distances are comparable to those observed in a related structure (Wang et al., 2007).

Related literature

For related structures, see: Guo et al. (2004); Wang et al. (2007).

S2. Experimental

To a solution of 3-methylmercapto-5-mercapto-1,2,4-thiadiazole (10 mmol) in 60 ml of doubly-distilled water, a solution of an equimolar amount (10 mmol) of sodium hydroxide in 40 ml of doubly-distilled water was added dropwise at room temperature. After vigorous stirring for 6 h, the resulting mixture was evaporated in vacuo to a volume of about 20 ml and filtered hot. The filtrate was then set aside for crystallization at room temperature. Two weeks later, colourless single crystals suitable for X-ray diffraction were obtained.

S3. Refinement

H atoms of the water molecules were initially located a difference Fourier map and later refined using a riding model with O-H = 0.85Šand U_iso(H) = 0.05 Ų. C-bound H atoms were positioned geometrically and treated as riding on their parent atoms with C-H = 0.96 Šand U_iso(H) = 1.5U_eq(C).

Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); 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

	Fig. 1. The coordination environment around the Na^+ ion. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (A) -x, -y, 2-z; (B) x, 1/2-y, z; (C) -x, 1/2+y, 2-z].
	Fig. 2. Part of the polymeric chain parallel to the b axis. H atoms have been omitted for clarity.

catena-Poly[[(3-methylsulfanyl-1,2,4-thiadiazole-5-thiolato)sodium]di- µ-aqua-κ⁴O:O]

Crystal data

[Na(C3H3N2S3)(H2O)2]	F(000) = 228
Mr = 222.28	Dx = 1.644 Mg m^−3
Monoclinic, P21/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 1437 reflections
a = 7.5794 (8) Å	θ = 2.4–27.9°
b = 6.9736 (6) Å	µ = 0.83 mm^−1
c = 8.6879 (12) Å	T = 298 K
β = 102.027 (1)°	Block, colourless
V = 449.13 (9) Å^3	0.39 × 0.27 × 0.15 mm
Z = 2

Data collection

Siemens SMART CCD area-detector diffractometer	862 independent reflections
Radiation source: fine-focus sealed tube	728 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.017
ϕ and ω scans	θmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −7→9
Tmin = 0.739, Tmax = 0.886	k = −8→8
2256 measured reflections	l = −10→10

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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.064	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.027P)^2 + 0.2249P] where P = (Fo^2 + 2Fc^2)/3
862 reflections	(Δ/σ)max = 0.001
64 parameters	Δρmax = 0.28 e Å^−3
0 restraints	Δρmin = −0.21 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	Occ. (<1)
Na1	0.07064 (15)	0.2500	0.93636 (13)	0.0400 (3)
N1	0.1651 (3)	0.2500	0.4084 (3)	0.0339 (5)
N2	0.1364 (3)	0.2500	0.6700 (2)	0.0291 (5)
O1	0.16585 (17)	−0.0019 (2)	1.13259 (15)	0.0413 (4)
H1A	0.1666	0.0502	1.2212	0.050*
H1B	0.2701	−0.0493	1.1374	0.050*
S1	0.37894 (9)	0.2500	0.51077 (9)	0.0386 (2)
S2	−0.17326 (9)	0.2500	0.46612 (9)	0.0378 (2)
S3	0.46031 (10)	0.2500	0.86933 (9)	0.0448 (2)
C1	0.0626 (3)	0.2500	0.5131 (3)	0.0283 (6)
C2	0.3165 (3)	0.2500	0.6910 (3)	0.0310 (6)
C3	−0.2220 (4)	0.2500	0.2548 (3)	0.0470 (8)
H3A	−0.3503	0.2500	0.2163	0.071*
H3B	−0.1709	0.1376	0.2175	0.071*	0.50
H3C	−0.1709	0.3624	0.2175	0.071*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Na1	0.0488 (7)	0.0382 (7)	0.0350 (6)	0.000	0.0134 (5)	0.000
N1	0.0315 (12)	0.0391 (14)	0.0321 (13)	0.000	0.0085 (10)	0.000
N2	0.0261 (11)	0.0318 (12)	0.0302 (12)	0.000	0.0074 (9)	0.000
O1	0.0393 (8)	0.0461 (9)	0.0374 (8)	0.0029 (6)	0.0054 (6)	−0.0041 (7)
S1	0.0274 (4)	0.0514 (5)	0.0394 (4)	0.000	0.0122 (3)	0.000
S2	0.0256 (4)	0.0444 (5)	0.0423 (4)	0.000	0.0043 (3)	0.000
S3	0.0319 (4)	0.0626 (6)	0.0364 (4)	0.000	−0.0009 (3)	0.000
C1	0.0286 (13)	0.0214 (13)	0.0350 (15)	0.000	0.0067 (11)	0.000
C2	0.0280 (13)	0.0295 (15)	0.0358 (15)	0.000	0.0070 (11)	0.000
C3	0.0439 (17)	0.0468 (19)	0.0426 (18)	0.000	−0.0088 (14)	0.000

Geometric parameters (Å, º)

Na1—O1^i	2.4493 (16)	N2—C1	1.361 (3)
Na1—O1	2.4493 (16)	O1—Na1^ii	2.4736 (16)
Na1—N2	2.467 (2)	O1—H1A	0.85
Na1—O1^ii	2.4736 (16)	O1—H1B	0.85
Na1—O1^iii	2.4736 (16)	S1—C2	1.727 (3)
Na1—S3	3.1271 (14)	S2—C1	1.749 (3)
Na1—Na1^ii	3.8756 (10)	S2—C3	1.796 (3)
Na1—Na1^iv	3.8756 (10)	S3—C2	1.698 (3)
N1—C1	1.314 (3)	C3—H3A	0.96
N1—S1	1.679 (2)	C3—H3B	0.96
N2—C2	1.340 (3)	C3—H3C	0.96
O1^i—Na1—O1	91.62 (8)	Na1^ii—Na1—Na1^iv	128.23 (6)
O1^i—Na1—N2	124.42 (5)	C1—N1—S1	106.14 (18)
O1—Na1—N2	124.42 (5)	C2—N2—C1	109.3 (2)
O1^i—Na1—O1^ii	139.79 (5)	C2—N2—Na1	105.76 (16)
O1—Na1—O1^ii	76.14 (5)	C1—N2—Na1	144.92 (16)
N2—Na1—O1^ii	92.90 (6)	Na1—O1—Na1^ii	103.86 (5)
O1^i—Na1—O1^iii	76.14 (5)	Na1—O1—H1A	105.7
O1—Na1—O1^iii	139.79 (5)	Na1^ii—O1—H1A	112.7
N2—Na1—O1^iii	92.90 (6)	Na1—O1—H1B	116.7
O1^ii—Na1—O1^iii	88.79 (7)	Na1^ii—O1—H1B	111.0
O1^i—Na1—S3	88.68 (4)	H1A—O1—H1B	106.9
O1—Na1—S3	88.68 (4)	N1—S1—C2	93.66 (12)
N2—Na1—S3	56.09 (5)	C1—S2—C3	102.79 (14)
O1^ii—Na1—S3	128.30 (4)	C2—S3—Na1	73.65 (9)
O1^iii—Na1—S3	128.30 (4)	N1—C1—N2	121.0 (2)
O1^i—Na1—Na1^ii	120.36 (6)	N1—C1—S2	124.2 (2)
O1—Na1—Na1^ii	38.29 (3)	N2—C1—S2	114.86 (18)
N2—Na1—Na1^ii	112.92 (3)	N2—C2—S3	124.5 (2)
O1^ii—Na1—Na1^ii	37.85 (3)	N2—C2—S1	109.90 (19)
O1^iii—Na1—Na1^ii	117.98 (6)	S3—C2—S1	125.60 (16)
S3—Na1—Na1^ii	112.39 (3)	S2—C3—H3A	109.5
O1^i—Na1—Na1^iv	38.29 (3)	S2—C3—H3B	109.5
O1—Na1—Na1^iv	120.36 (6)	H3A—C3—H3B	109.5
N2—Na1—Na1^iv	112.92 (3)	S2—C3—H3C	109.5
O1^ii—Na1—Na1^iv	117.98 (6)	H3A—C3—H3C	109.5
O1^iii—Na1—Na1^iv	37.85 (4)	H3B—C3—H3C	109.5
S3—Na1—Na1^iv	112.39 (3)

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