Poly[aqua­(μ11-4,6-dihy­droxy­benzene-1,3-disulfonato)­dipotassium]

Xie, Z.-L.; Lai, W.-L.; Yang, R.-Q.; Xie, Y.-R.

doi:10.1107/S1600536811047210

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 12| December 2011| Page m1745

https://doi.org/10.1107/S1600536811047210

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Poly[aqua(μ₁₁-4,6-dihydroxybenzene-1,3-disulfonato)dipotassium]

Zhu-Lin Xie,^a ^* Wu-Leng Lai,^b Rui-Qing Yang ^b and Yong-Rong Xie ^b

^aSchool of Chemistry and Chemical Engineering, University of Jinan, Jinan 250022, People's Republic of China, and ^bKey Laboratory of Jiangxi University for Functional Materials Chemistry, College of Chemistry and Chemical Engineering, Gannan Normal University, Ganzhou 341000, People's Republic of China
^*Correspondence e-mail: yongrongxie@yahoo.com.cn

(Received 10 October 2011; accepted 8 November 2011; online 12 November 2011)

In the title salt, [K₂(C₆H₄O₈S₂)(H₂O)]_n, both K⁺ ions exhibit a seven-coordination with K—O bond lengths in the range 2.6600 (14) to 3.0522 (16) Å. One K⁺ ion is coordinated by seven O atoms from the sulfonate and phenolic hydroxy groups of six 4,6-dihydroxybenzene-1,3-disulfonate (L²⁻) anions while the other K⁺ ion is coordinated by six O atoms from the sulfonate and phenolic hydroxy groups of five L²⁻ anions and one water O atom. The L²⁻ anion exhibits chelating–bridging multidentate coordination to potassium, resulting in the formation of a cross-linked three-dimensional network.

Related literature

For K—O bond lengths of potassium complexes, see: Hatano et al. (2008 ); Xie et al. (2006 ); Zhang et al. (2006 ). For other complexes with seven-coordinate potassium atoms, see: Deacon et al. (1999 ).

Experimental

Crystal data

[K₂(C₆H₄O₈S₂)(H₂O)]
M_r = 364.43
Monoclinic, P 2₁ /c
a = 7.3427 (3) Å
b = 11.5194 (5) Å
c = 14.6331 (6) Å
β = 100.495 (1)°
V = 1217.01 (9) Å³
Z = 4
Mo Kα radiation
μ = 1.16 mm⁻¹
T = 292 K
0.33 × 0.20 × 0.17 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.753, T_max = 0.816
6519 measured reflections
2365 independent reflections
2164 reflections with I > 2σ(I)
R_int = 0.013

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.071
S = 1.08
2365 reflections
173 parameters
H-atom parameters constrained
Δρ_max = 0.38 e Å⁻³
Δρ_min = −0.33 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O8—H8A⋯O4	0.82	1.88	2.625 (2)	151
O7—H7A⋯O1	0.82	1.86	2.613 (2)	152
O9—H9A⋯O6ⁱ	0.85	2.29	2.916 (2)	130
O9—H9B⋯O2ⁱⁱ	0.85	2.26	2.913 (3)	134
Symmetry codes: (i) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) x+1, y, z.

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); 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: https://doi.org/10.1107/S1600536811047210/vm2127sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811047210/vm2127Isup2.hkl

checkCIF report

Comment top

The title compound, (I), consists of a three dimensional framework of K⁺ ions coordinated to 4, 6-dihydroxybenzene-1, 3-disulfonate anions. The K⁺ ion is typically seven-coordinated (Deacon et al., 1999), in which the coordination environment around the K⁺ center in (I) is a distorted pentangular dipyramid. As shown in Fig.1, the K1 ion is coordinated by seven O atoms from six 4, 6-dihydroxybenzene-1, 3-disulfonate anions, in which the K—O bond distances range from 2.7160 (14) to 3.0206 (16) Å, with an average bond distance of 2.8460 Å, and the K2 ion is also coordinated by five 4, 6-dihydroxybenzene-1, 3-disulfonate anions and one water molecule, in which the K—O bond distances range from 2.6606 (14) to 3.0518 (16) Å, with an average bond distance of 2.791 Å. The K—O bond distances are similar to the values in other potassium complexes (Hatano et al., 2008; Xie et al., 2006; Zhang et al., 2006). The two sulfonate groups of the 4, 6-dihydroxybenzene-1, 3-disulfonate anions in (I) exhibit a chelating-bridging pentadentate or tetradentate coordination. The O1/O2 atoms and O5/O6 atoms bridge two different K⁺ ions, the other O atoms including those of the hydroxide groups chelate to one type of K⁺ ion (Fig. 2) giving a three dimensional structure (Fig. 3).

Related literature top

For K—O bond distances of potassium complexes, see: Hatano et al. (2008); Xie et al. (2006); Zhang et al. (2006). For other complexes with seven-coordinate potassium atoms, see: Deacon et al. (1999).

Experimental top

KOH (0.14 g, 2.5 mmol) and 4, 6-dihydroxybenzene-1, 3-disulfonate acid (0.91 g, 2.5 mmol) were dissolved in 10 ml of distilled water by vigorous stirring. Filtering solution was evaporated slowly at room temperature. Colorless block crystals of the tilted compound suitable for X-ray analysis were collected in 55% yield (based on potassium) after one week.

Structure description top

# Following replaced by publCIF - 12 23 16:59:45 2008

The stucture of the title compound, (I), is shown below. Dimensions are available in the archived CIF.

For related literature, see [type here to add references to related literature].

# Following replaced by publCIF - 12 23 17:42:43 2008

For related literature, see [list references here]

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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 coordination environment of the K⁺ ions showing displacement ellipsoids drawn at the 30% probability level. [Symmetry codes: (i) x, -y + 1/2, z + 1/2; (ii) -x + 1, y + 1/2, -z + 1/2; (iii) -x + 1, y - 1/2, -z + 1/2; (iv) x + 1, -y + 1/2, z + 1/2; (v) -x + 1, -y, -z + 1; (vii) x + 1, y, z; (viii) -x + 1, -y, -z].
	Fig. 2. View of chelating/bridging to K⁺ ions by the sulfonic and phenolic hydroxy groups in the L^2-anion, displacement ellipsoids are drawn at 30% probability level. [Symmetry codes: (ii) -x + 1, y + 1/2, -z + 1/2; (iii) -x + 1, y - 1/2, -z + 1/2; (v) -x + 1, -y, -z + 1; (viii) -x + 1, -y, -z (ix) x - 1, -y + 1/2, z - 1/2; (x) x, -y + 1/2, z - 1/2; (xi) x - 1, y, z].
	Fig. 3. Perspective view of crystal packing along the a axis. Hydrogen atoms are omitted for clarity.

Poly[aqua(µ₁₁-4,6-dihydroxybenzene-1,3-disulfonato)dipotassium] top

Crystal data top

[K₂(C₆H₄O₈S₂)(H₂O)]	F(000) = 736
M_r = 364.43	D_x = 1.989 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2637 reflections
a = 7.3427 (3) Å	θ = 2.3–27.4°
b = 11.5194 (5) Å	µ = 1.16 mm⁻¹
c = 14.6331 (6) Å	T = 292 K
β = 100.495 (1)°	Block, colorless
V = 1217.01 (9) Å³	0.33 × 0.20 × 0.17 mm
Z = 4

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	2365 independent reflections
Radiation source: fine-focus sealed tube	2164 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.013
φ and ω scans	θ_max = 26.0°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→8
T_min = 0.753, T_max = 0.816	k = −14→14
6519 measured reflections	l = −13→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.024	H-atom parameters constrained
wR(F²) = 0.071	w = 1/[σ²(F_o²) + (0.0436P)² + 0.4024P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max < 0.001
2365 reflections	Δρ_max = 0.38 e Å⁻³
173 parameters	Δρ_min = −0.33 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0022 (7)

Crystal data top

[K₂(C₆H₄O₈S₂)(H₂O)]	V = 1217.01 (9) Å³
M_r = 364.43	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 7.3427 (3) Å	µ = 1.16 mm⁻¹
b = 11.5194 (5) Å	T = 292 K
c = 14.6331 (6) Å	0.33 × 0.20 × 0.17 mm
β = 100.495 (1)°

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	2365 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2164 reflections with I > 2σ(I)
T_min = 0.753, T_max = 0.816	R_int = 0.013
6519 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	0 restraints
wR(F²) = 0.071	H-atom parameters constrained
S = 1.08	Δρ_max = 0.38 e Å⁻³
2365 reflections	Δρ_min = −0.33 e Å⁻³
173 parameters

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
K1	0.65409 (5)	0.13314 (3)	0.49915 (3)	0.03113 (13)
K2	0.92404 (6)	0.02144 (4)	0.28049 (3)	0.03374 (13)
S1	0.44515 (6)	0.00084 (4)	0.26286 (3)	0.02489 (13)
S2	0.13059 (5)	0.32694 (3)	0.01439 (3)	0.02338 (13)
O1	0.0057 (2)	0.32564 (11)	−0.07575 (9)	0.0390 (3)
O2	0.03127 (18)	0.35943 (11)	0.08772 (10)	0.0349 (3)
O3	0.29405 (18)	0.39641 (11)	0.01473 (10)	0.0372 (3)
O4	0.5722 (2)	−0.09468 (13)	0.25379 (10)	0.0431 (4)
O5	0.5404 (2)	0.10174 (12)	0.30606 (9)	0.0401 (3)
O6	0.29385 (19)	−0.03620 (13)	0.30678 (9)	0.0410 (3)
O7	0.0959 (2)	0.11766 (12)	−0.12326 (9)	0.0381 (3)
H7A	0.0522	0.1834	−0.1271	0.046*
O8	0.3915 (2)	−0.15510 (11)	0.08903 (10)	0.0383 (3)
H8A	0.4576	−0.1604	0.1404	0.046*
O9	0.8087 (4)	0.21939 (16)	0.19154 (15)	0.0948 (8)
H9A	0.7450	0.2678	0.2163	0.114*
H9B	0.8358	0.2336	0.1386	0.114*
C1	0.2023 (2)	0.18131 (14)	0.03585 (11)	0.0225 (3)
C2	0.1799 (2)	0.09683 (15)	−0.03415 (11)	0.0254 (4)
C3	0.2454 (2)	−0.01451 (15)	−0.01379 (12)	0.0292 (4)
H3A	0.2321	−0.0700	−0.0607	0.035*
C4	0.3303 (2)	−0.04435 (14)	0.07530 (12)	0.0258 (3)
C5	0.3490 (2)	0.03891 (14)	0.14670 (11)	0.0233 (3)
C6	0.2866 (2)	0.15100 (14)	0.12554 (12)	0.0241 (3)
H6A	0.3015	0.2069	0.1722	0.029*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
K1	0.0284 (2)	0.0278 (2)	0.0368 (2)	−0.00127 (15)	0.00475 (16)	0.00329 (15)
K2	0.0373 (2)	0.0326 (2)	0.0297 (2)	0.00037 (16)	0.00155 (17)	−0.00276 (16)
S1	0.0255 (2)	0.0254 (2)	0.0225 (2)	0.00017 (16)	0.00132 (16)	0.00241 (15)
S2	0.0237 (2)	0.0199 (2)	0.0257 (2)	0.00147 (15)	0.00221 (16)	0.00099 (15)
O1	0.0470 (8)	0.0309 (7)	0.0329 (7)	0.0074 (6)	−0.0093 (6)	0.0026 (6)
O2	0.0364 (7)	0.0305 (7)	0.0402 (8)	0.0088 (5)	0.0131 (6)	−0.0009 (5)
O3	0.0319 (7)	0.0263 (7)	0.0538 (9)	−0.0039 (5)	0.0092 (6)	0.0049 (6)
O4	0.0458 (8)	0.0437 (8)	0.0363 (7)	0.0193 (7)	−0.0020 (6)	0.0016 (6)
O5	0.0492 (8)	0.0366 (7)	0.0291 (7)	−0.0113 (6)	−0.0071 (6)	0.0010 (6)
O6	0.0364 (7)	0.0531 (9)	0.0349 (7)	−0.0057 (6)	0.0100 (6)	0.0096 (6)
O7	0.0549 (9)	0.0336 (7)	0.0219 (6)	0.0099 (6)	−0.0029 (6)	−0.0033 (5)
O8	0.0521 (8)	0.0218 (6)	0.0366 (7)	0.0081 (6)	−0.0033 (6)	−0.0020 (5)
O9	0.178 (3)	0.0389 (10)	0.0766 (14)	0.0139 (13)	0.0474 (15)	0.0119 (9)
C1	0.0222 (8)	0.0205 (8)	0.0249 (8)	0.0014 (6)	0.0041 (6)	0.0008 (6)
C2	0.0259 (8)	0.0279 (9)	0.0220 (8)	0.0002 (7)	0.0029 (6)	−0.0012 (7)
C3	0.0343 (10)	0.0250 (9)	0.0269 (9)	0.0011 (7)	0.0023 (7)	−0.0073 (7)
C4	0.0270 (8)	0.0202 (8)	0.0300 (9)	0.0001 (7)	0.0046 (7)	−0.0015 (7)
C5	0.0233 (8)	0.0236 (8)	0.0223 (8)	0.0002 (6)	0.0019 (6)	0.0007 (6)
C6	0.0256 (8)	0.0224 (8)	0.0234 (8)	−0.0004 (6)	0.0019 (6)	−0.0036 (6)

Geometric parameters (Å, º) top

K1—O3ⁱ	2.7160 (14)	O1—K2^viii	2.7256 (13)
K1—O8ⁱⁱ	2.7514 (13)	O1—K1^viii	3.0207 (16)
K1—O3ⁱⁱⁱ	2.7660 (14)	O2—K2ⁱⁱ	2.6607 (14)
K1—O5	2.8200 (14)	O2—K1^viii	2.8372 (14)
K1—O2^iv	2.8372 (14)	O3—K1^ix	2.7160 (14)
K1—O6^v	3.0104 (14)	O3—K1ⁱⁱ	2.7660 (14)
K1—O1^iv	3.0207 (16)	O6—K2^x	2.7535 (15)
K1—O9ⁱ	3.307 (2)	O6—K1^v	3.0104 (14)
K1—S2^iv	3.4954 (6)	O7—C2	1.359 (2)
K2—O2ⁱⁱⁱ	2.6607 (14)	O7—K2^vii	2.7856 (13)
K2—O9	2.6851 (19)	O7—H7A	0.8204
K2—O1^iv	2.7256 (13)	O8—C4	1.356 (2)
K2—O6^vi	2.7535 (15)	O8—K1ⁱⁱⁱ	2.7514 (13)
K2—O7^vii	2.7856 (13)	O8—H8A	0.8194
K2—O4	2.8720 (16)	O9—K1^ix	3.307 (2)
K2—O5	3.0521 (16)	O9—H9A	0.8500
K2—S1	3.4867 (6)	O9—H9B	0.8502
S1—O5	1.4417 (13)	C1—C6	1.390 (2)
S1—O6	1.4455 (14)	C1—C2	1.401 (2)
S1—O4	1.4641 (14)	C2—C3	1.383 (2)
S1—C5	1.7729 (16)	C3—C4	1.382 (2)
S2—O3	1.4418 (13)	C3—H3A	0.9300
S2—O2	1.4519 (13)	C4—C5	1.406 (2)
S2—O1	1.4628 (13)	C5—C6	1.386 (2)
S2—C1	1.7691 (16)	C6—H6A	0.9300
S2—K1^viii	3.4954 (6)

O3ⁱ—K1—O8ⁱⁱ	96.50 (4)	O1^iv—K2—S1	100.27 (3)
O3ⁱ—K1—O3ⁱⁱⁱ	91.82 (4)	O6^vi—K2—S1	161.72 (4)
O8ⁱⁱ—K1—O3ⁱⁱⁱ	147.81 (5)	O7^vii—K2—S1	89.95 (3)
O3ⁱ—K1—O5	87.31 (5)	O4—K2—S1	24.24 (3)
O8ⁱⁱ—K1—O5	69.84 (4)	O5—K2—S1	24.33 (3)
O3ⁱⁱⁱ—K1—O5	79.60 (4)	O2ⁱⁱⁱ—K2—K1	71.35 (3)
O3ⁱ—K1—O2^iv	148.16 (4)	O9—K2—K1	87.63 (5)
O8ⁱⁱ—K1—O2^iv	102.29 (4)	O1^iv—K2—K1	44.92 (3)
O3ⁱⁱⁱ—K1—O2^iv	85.83 (4)	O6^vi—K2—K1	123.37 (3)
O5—K1—O2^iv	123.22 (4)	O7^vii—K2—K1	146.39 (3)
O3ⁱ—K1—O6^v	80.36 (4)	O4—K2—K1	73.30 (3)
O8ⁱⁱ—K1—O6^v	139.02 (4)	O5—K2—K1	41.41 (3)
O3ⁱⁱⁱ—K1—O6^v	73.03 (4)	S1—K2—K1	58.329 (11)
O5—K1—O6^v	149.45 (4)	O2ⁱⁱⁱ—K2—K1^xi	37.90 (3)
O2^iv—K1—O6^v	68.57 (4)	O9—K2—K1^xi	144.42 (6)
O3ⁱ—K1—O1^iv	163.66 (4)	O1^iv—K2—K1^xi	70.77 (3)
O8ⁱⁱ—K1—O1^iv	74.31 (4)	O6^vi—K2—K1^xi	42.14 (3)
O3ⁱⁱⁱ—K1—O1^iv	89.44 (4)	O7^vii—K2—K1^xi	107.18 (3)
O5—K1—O1^iv	76.90 (4)	O4—K2—K1^xi	113.91 (3)
O2^iv—K1—O1^iv	48.18 (4)	O5—K2—K1^xi	124.94 (3)
O6^v—K1—O1^iv	115.50 (4)	S1—K2—K1^xi	126.161 (14)
O3ⁱ—K1—O9ⁱ	100.44 (5)	K1—K2—K1^xi	86.205 (11)
O8ⁱⁱ—K1—O9ⁱ	86.41 (5)	O5—S1—O6	113.19 (9)
O3ⁱⁱⁱ—K1—O9ⁱ	122.58 (5)	O5—S1—O4	112.30 (9)
O5—K1—O9ⁱ	155.78 (5)	O6—S1—O4	111.87 (9)
O2^iv—K1—O9ⁱ	55.98 (6)	O5—S1—C5	107.31 (8)
O6^v—K1—O9ⁱ	54.73 (5)	O6—S1—C5	107.16 (8)
O1^iv—K1—O9ⁱ	92.56 (5)	O4—S1—C5	104.37 (8)
O3ⁱ—K1—S2^iv	171.66 (4)	O5—S1—K2	60.70 (6)
O8ⁱⁱ—K1—S2^iv	87.03 (3)	O6—S1—K2	146.47 (6)
O3ⁱⁱⁱ—K1—S2^iv	89.13 (3)	O4—S1—K2	53.65 (6)
O5—K1—S2^iv	101.01 (3)	C5—S1—K2	105.92 (6)
O2^iv—K1—S2^iv	23.71 (3)	O3—S2—O2	112.60 (8)
O6^v—K1—S2^iv	92.00 (3)	O3—S2—O1	113.16 (9)
O1^iv—K1—S2^iv	24.59 (2)	O2—S2—O1	110.63 (8)
O9ⁱ—K1—S2^iv	72.17 (5)	O3—S2—C1	107.76 (8)
O3ⁱ—K1—K1^v	46.45 (3)	O2—S2—C1	106.66 (8)
O8ⁱⁱ—K1—K1^v	133.97 (3)	O1—S2—C1	105.53 (8)
O3ⁱⁱⁱ—K1—K1^v	45.37 (3)	O3—S2—K1^viii	138.60 (6)
O5—K1—K1^v	80.54 (3)	O2—S2—K1^viii	51.80 (6)
O2^iv—K1—K1^v	123.52 (3)	O1—S2—K1^viii	59.22 (6)
O6^v—K1—K1^v	70.68 (3)	C1—S2—K1^viii	113.46 (6)
O1^iv—K1—K1^v	132.54 (3)	S2—O1—K2^viii	134.67 (8)
O9ⁱ—K1—K1^v	121.30 (4)	S2—O1—K1^viii	96.20 (7)
S2^iv—K1—K1^v	133.906 (18)	K2^viii—O1—K1^viii	95.50 (4)
O3ⁱ—K1—K2	128.22 (3)	S2—O2—K2ⁱⁱ	134.76 (8)
O8ⁱⁱ—K1—K2	87.08 (3)	S2—O2—K1^viii	104.48 (7)
O3ⁱⁱⁱ—K1—K2	63.75 (3)	K2ⁱⁱ—O2—K1^viii	106.93 (4)
O5—K1—K2	45.71 (3)	S2—O3—K1^ix	138.81 (8)
O2^iv—K1—K2	78.64 (3)	S2—O3—K1ⁱⁱ	132.27 (8)
O6^v—K1—K2	126.89 (3)	K1^ix—O3—K1ⁱⁱ	88.18 (4)
O1^iv—K1—K2	39.58 (2)	S1—O4—K2	102.11 (8)
O9ⁱ—K1—K2	131.33 (5)	S1—O5—K1	125.04 (8)
S2^iv—K1—K2	59.350 (11)	S1—O5—K2	94.98 (7)
K1^v—K1—K2	96.882 (15)	K1—O5—K2	92.88 (4)
O3ⁱ—K1—K2^xi	116.87 (3)	S1—O6—K2^x	133.23 (8)
O8ⁱⁱ—K1—K2^xi	135.14 (3)	S1—O6—K1^v	123.58 (7)
O3ⁱⁱⁱ—K1—K2^xi	64.45 (3)	K2^x—O6—K1^v	100.01 (4)
O5—K1—K2^xi	136.03 (3)	C2—O7—K2^vii	129.60 (11)
O2^iv—K1—K2^xi	35.17 (3)	C2—O7—H7A	109.4
O6^v—K1—K2^xi	37.85 (3)	K2^vii—O7—H7A	120.9
O1^iv—K1—K2^xi	78.24 (3)	C4—O8—K1ⁱⁱⁱ	139.13 (11)
O9ⁱ—K1—K2^xi	59.97 (4)	C4—O8—H8A	109.4
S2^iv—K1—K2^xi	56.355 (10)	K1ⁱⁱⁱ—O8—H8A	111.4
K1^v—K1—K2^xi	90.518 (14)	K2—O9—K1^ix	151.40 (8)
K2—K1—K2^xi	93.795 (11)	K2—O9—H9A	120.0
O2ⁱⁱⁱ—K2—O9	158.97 (6)	K1^ix—O9—H9A	84.0
O2ⁱⁱⁱ—K2—O1^iv	85.02 (4)	K2—O9—H9B	120.0
O9—K2—O1^iv	80.27 (6)	K1^ix—O9—H9B	39.3
O2ⁱⁱⁱ—K2—O6^vi	75.01 (4)	H9A—O9—H9B	120.0
O9—K2—O6^vi	119.25 (7)	C6—C1—C2	119.26 (15)
O1^iv—K2—O6^vi	88.58 (5)	C6—C1—S2	118.21 (12)
O2ⁱⁱⁱ—K2—O7^vii	100.15 (4)	C2—C1—S2	122.52 (13)
O9—K2—O7^vii	97.10 (5)	O7—C2—C3	116.73 (15)
O1^iv—K2—O7^vii	168.61 (5)	O7—C2—C1	123.46 (15)
O6^vi—K2—O7^vii	83.04 (4)	C3—C2—C1	119.80 (15)
O2ⁱⁱⁱ—K2—O4	76.18 (4)	C4—C3—C2	120.87 (16)
O9—K2—O4	97.64 (7)	C4—C3—H3A	119.6
O1^iv—K2—O4	118.17 (5)	C2—C3—H3A	119.6
O6^vi—K2—O4	138.28 (4)	O8—C4—C3	117.02 (15)
O7^vii—K2—O4	73.09 (4)	O8—C4—C5	123.15 (15)
O2ⁱⁱⁱ—K2—O5	96.80 (4)	C3—C4—C5	119.83 (15)
O9—K2—O5	65.50 (6)	C6—C5—C4	119.06 (15)
O1^iv—K2—O5	77.75 (4)	C6—C5—S1	120.16 (13)
O6^vi—K2—O5	164.73 (4)	C4—C5—S1	120.76 (13)
O7^vii—K2—O5	111.39 (4)	C5—C6—C1	121.14 (15)
O4—K2—O5	47.96 (4)	C5—C6—H6A	119.4
O2ⁱⁱⁱ—K2—S1	89.74 (3)	C1—C6—H6A	119.4
O9—K2—S1	78.29 (6)

Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x+1, y+1/2, −z+1/2; (iii) −x+1, y−1/2, −z+1/2; (iv) x+1, −y+1/2, z+1/2; (v) −x+1, −y, −z+1; (vi) x+1, y, z; (vii) −x+1, −y, −z; (viii) x−1, −y+1/2, z−1/2; (ix) x, −y+1/2, z−1/2; (x) x−1, y, z; (xi) −x+2, −y, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8A···O4	0.82	1.88	2.625 (2)	151
O7—H7A···O1	0.82	1.86	2.613 (2)	152
O9—H9A···O6ⁱⁱ	0.85	2.29	2.916 (2)	130
O9—H9B···O2^vi	0.85	2.26	2.913 (3)	134

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

Experimental details

Crystal data
Chemical formula	[K₂(C₆H₄O₈S₂)(H₂O)]
M_r	364.43
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	292
a, b, c (Å)	7.3427 (3), 11.5194 (5), 14.6331 (6)
β (°)	100.495 (1)
V (Å³)	1217.01 (9)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.16
Crystal size (mm)	0.33 × 0.20 × 0.17

Data collection
Diffractometer	Bruker SMART APEXII CCD area-detector
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.753, 0.816
No. of measured, independent and observed [I > 2σ(I)] reflections	6519, 2365, 2164
R_int	0.013
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.071, 1.08
No. of reflections	2365
No. of parameters	173
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.38, −0.33

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), 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
O8—H8A···O4	0.82	1.88	2.625 (2)	151
O7—H7A···O1	0.82	1.86	2.613 (2)	152
O9—H9A···O6ⁱ	0.85	2.29	2.916 (2)	130
O9—H9B···O2ⁱⁱ	0.85	2.26	2.913 (3)	134

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

Acknowledgements

This work was supported financially by the National Natural Science Foundation of China (grant No. 20861001) and the Natural Science Foundation of Jiangxi Provincial Education Department (grant Nos. GJJ11587 and GJJ08505).

References

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