catena-Poly[[octa­aqua­bis­(μ4-benzene-1,3,5-tricarboxyl­ato)trizinc] tetra­hydrate]

Sun, L.; Qiu, T.R.; Deng, H.

doi:10.1107/S160053681101436X

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 67| Part 5| May 2011| Pages m630-m631

doi:10.1107/S160053681101436X

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catena-Poly[[octaaquabis(μ₄-benzene-1,3,5-tricarboxylato)trizinc] tetrahydrate]

Lin Sun,^a Tao Run Qiu ^a and Hong Deng ^a ^*

^aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510006, People's Republic of China
^*Correspondence e-mail: dh@scnu.edu.cn

(Received 10 March 2011; accepted 16 April 2011; online 22 April 2011)

In the title compound, {[Zn₃(C₉H₃O₆)₂(H₂O)₈]·4H₂O}_n, there are two crystallographically independent Zn^II ions. One presents a trigonal-bipyramidal coordination geometry defined by five O atoms [three from two carboxylate groups of two benzene-1,3,5-tricarboxylate (BTC) ligands and the other two deriving from three water molecules], while the other lies on an inversion centre and exists in a slightly distorted octahedral coordination geometry defined by six O atoms (two from two carboxylate groups of two BTC ligands and the others from four water molecules). A three-dimensional framework is further strengthened via O—H⋯O hydrogen-bonding interactons.

Related literature

For background to the applications of metal–organic frameworks, see: Batten & Murray (2003 ); Zhong et al. (2008 ); Qiu et al. (2010 ). For the applications of benzene-1,3,5-tricarboxylate, see: Yaghi et al. (1997 ); Xu et al. (2008 ); Xu et al. (2007 ); Liang et al. (2009 ); Wang et al. (2009 ). For compounds exhibiting similar Zn—O distances, see: Hua et al. (2010 ); Chen et al. (2010 ); Yang et al. (2008 ); Xu et al. (2007).

Experimental

Crystal data

[Zn₃(C₉H₃O₆)₂(H₂O)₈]·4H₂O
M_r = 826.59
Monoclinic, P 2₁ /n
a = 14.745 (2) Å
b = 6.7960 (12) Å
c = 15.183 (3) Å
β = 94.543 (2)°
V = 1516.7 (4) Å³
Z = 2
Mo Kα radiation
μ = 2.45 mm⁻¹
T = 296 K
0.27 × 0.24 × 0.23 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.521, T_max = 0.569
7485 measured reflections
2729 independent reflections
1990 reflections with I > 2σ(I)
R_int = 0.047

Refinement

R[F² > 2σ(F²)] = 0.064
wR(F²) = 0.225
S = 1.13
2729 reflections
205 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 1.89 e Å⁻³
Δρ_min = −0.90 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4W—H4WB⋯O6ⁱ	0.85	1.97	2.768 (9)	155
O5W—H5WA⋯O2ⁱⁱ	0.85	1.99	2.842 (9)	179
O6W—H6WB⋯O6ⁱⁱⁱ	0.84	2.29	3.058 (13)	153
O5W—H5WB⋯O6^iv	0.85	2.59	3.356 (12)	150
Symmetry codes: (i) $[x-{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (ii) -x+1, -y+1, -z+1; (iii) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iv) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT (Bruker, 2004); 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/S160053681101436X/zk2004sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053681101436X/zk2004Isup2.hkl

checkCIF report

Comment top

The exploring of metal-organic frameworks (MOFs) has attracted considerable attention not only owing to their intriguing structral architectures and topologies, but also because of their many potential applications in catalysis, ion exchange, and magnetic, optical, and porous materials (Batten & Murray, 2003; Zhong et al., 2008; Qiu et al.,2010). 1,3,5-benzenetricarboxylate with six O atoms from its three carboxylate groups is a good choice of O-donor ligand. And such ligand has been widely used to synthesize metal compounds (Yaghi et al., 1997; Xu et al., 2008; Xu et al., 2007; Liang et al., 2009; Wang et al., 2009). Thus, we synthesize a new three-dimensional Zn-BTC metal-organic compound, {[Zn₃(BTC)₂(H₂O)₈](H₂O)₄}, with achiral channels along b direction, which was generated by the reaction of zinc sulfate heptahydrate, 1,3,5-benzenetricarboxylic acid and water at 150°C for 3 days.

There are two kinds of zinc atoms in the title compound (I) (Fig. 1). One is surrounded by five O atoms (three from two carboxylate groups of two BTC ligands and the other two deriving from three water molecules), exhibiting a trigonal bipyramidal geometry, the other is coordinated with six O atoms (two from two carboxylate groups of two BTC ligands; the others from four water molecules) and displays a slightly distorted octahedral geometry. All the BTC ligands have the same coordinated modes and each ligand coordinated to three zinc atoms. The bond distances of Zn—O_{chelated carboxylate} range from 1.999 (5)Å to 2.412 (6) Å. While the bond lengthes of Zn—O_{monodentate carboxylate} fall between 1.946 (6)Å and 2.049 (5) Å. And the Zn—O_w distances are in the normal range of 1.965 (6)–2.150 (6)Å (Table 1). All the distances of Zn—O in compound (I) are comparable to those found in the literatures (Hua et al., 2010; Chen et al., 2010; Yang et al., 2008; Xu et al., 2007). And there are weak interactions between Zn1 and C1 with the distances of 2.554Å and Zn1 and H2WB with with the distances of 2.0711 Å. A three-dimensional architecture is strengthened by the extended O—H···O hydrogen-bonding interactions (Table 2, Fig. 2)

Related literature top

For background to the applications of metal–organic frameworks, see: Batten & Murray (2003); Zhong et al. (2008); Qiu et al. (2010). For the applications of benzene-1,3,5-tricarboxylate, see: Yaghi et al. (1997); Xu et al. (2008); Xu et al. (2007); Liang et al. (2009); Wang et al. (2009). For compounds exhibiting similar Zn—O distances, see: Hua et al. (2010); Chen et al. (2010); Yang et al. (2008); Xu et al. (2007).

Experimental top

A mixture of zinc sulfate heptahydrate (0.287 g; 1 mmol), benzenetricarboxylic acid (0.210 g; 1 mmol) and water (10 ml) was sealed in a 23 ml Teflon-lined stainless steel reactor and heated at 120°C under autogenous pressure for 72 h. Then the mixture was cooled down to room temperature at a rate of 5°C per hour, and colorless block crystals were obtained in a yield of 49% based on Zn

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); 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 structure of (I), showing the atomic numbering scheme. Non-H atoms are shown as 30% probability displacement ellipsoids.
	Fig. 2. A packing view of (I) along the b axis, showing the O—H···O hydrogen bonds.

catena-Poly[[octaaquabis(µ₄-benzene-1,3,5-tricarboxylato)trizinc] tetrahydrate] top

Crystal data top

[Zn₃(C₉H₃O₆)₂(H₂O)₈]·4H₂O	F(000) = 840.0
M_r = 826.59	D_x = 1.810 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2729 reflections
a = 14.745 (2) Å	θ = 2.0–25.2°
b = 6.7960 (12) Å	µ = 2.45 mm⁻¹
c = 15.183 (3) Å	T = 296 K
β = 94.543 (2)°	Block, colourless
V = 1516.7 (4) Å³	0.27 × 0.24 × 0.23 mm
Z = 2

Data collection top

Bruker SMART APEX CCD diffractometer	2729 independent reflections
Radiation source: fine-focus sealed tube	1990 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.047
ω scans	θ_max = 25.2°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −17→17
T_min = 0.521, T_max = 0.569	k = −8→8
7485 measured reflections	l = −18→11

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)] = 0.064	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.225	H-atom parameters constrained
S = 1.13	w = 1/[σ²(F_o²) + (0.124P)² + 4.534P] where P = (F_o² + 2F_c²)/3
2729 reflections	(Δ/σ)_max = 0.002
205 parameters	Δρ_max = 1.89 e Å⁻³
1 restraint	Δρ_min = −0.90 e Å⁻³

Crystal data top

[Zn₃(C₉H₃O₆)₂(H₂O)₈]·4H₂O	V = 1516.7 (4) Å³
M_r = 826.59	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 14.745 (2) Å	µ = 2.45 mm⁻¹
b = 6.7960 (12) Å	T = 296 K
c = 15.183 (3) Å	0.27 × 0.24 × 0.23 mm
β = 94.543 (2)°

Data collection top

Bruker SMART APEX CCD diffractometer	2729 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1990 reflections with I > 2σ(I)
T_min = 0.521, T_max = 0.569	R_int = 0.047
7485 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.064	1 restraint
wR(F²) = 0.225	H-atom parameters constrained
S = 1.13	Δρ_max = 1.89 e Å⁻³
2729 reflections	Δρ_min = −0.90 e Å⁻³
205 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
C1	0.3865 (5)	0.7336 (11)	0.2885 (5)	0.0258 (16)
C2	0.2896 (5)	0.7366 (11)	0.2512 (5)	0.0247 (16)
C3	0.2199 (5)	0.7180 (11)	0.3061 (5)	0.0229 (15)
H3	0.2334	0.7052	0.3667	0.027*
C4	0.1296 (5)	0.7180 (11)	0.2720 (5)	0.0251 (16)
C5	0.0531 (5)	0.6843 (12)	0.3308 (5)	0.0292 (17)
C6	0.1136 (4)	0.7328 (10)	0.1806 (5)	0.0266 (17)
H6	0.0539	0.7242	0.1561	0.032*
C7	0.1800 (5)	0.7589 (11)	0.1259 (5)	0.0241 (16)
C8	0.1573 (5)	0.7876 (13)	0.0286 (5)	0.0334 (19)
C9	0.2690 (5)	0.7583 (11)	0.1620 (5)	0.0240 (15)
H9	0.3160	0.7728	0.1251	0.029*
O1	0.4494 (4)	0.7356 (9)	0.2381 (4)	0.0397 (15)
O2	0.4054 (4)	0.7247 (9)	0.3705 (4)	0.0353 (13)
O3	0.0741 (4)	0.6348 (9)	0.4086 (3)	0.0358 (13)
O4	−0.0276 (4)	0.7041 (10)	0.2973 (4)	0.0398 (15)
O5	0.0728 (4)	0.7813 (10)	0.0033 (4)	0.0407 (15)
O6	0.2183 (4)	0.8087 (13)	−0.0218 (4)	0.064 (2)
O1W	0.5996 (4)	0.9590 (10)	0.3383 (4)	0.0472 (16)
H1WA	0.6200	1.0116	0.2931	0.071*
H1WB	0.5642	1.0416	0.3600	0.071*
O2W	0.6025 (4)	0.4905 (9)	0.3245 (4)	0.0504 (17)
H2WA	0.6226	0.4688	0.2739	0.076*
H2WB	0.5518	0.4334	0.3252	0.076*
O3W	0.0151 (4)	0.2213 (10)	0.4358 (4)	0.0450 (15)
H3WA	0.0380	0.2934	0.3975	0.067*
H3WB	0.0384	0.1073	0.4327	0.067*
O4W	−0.1226 (4)	0.5373 (11)	0.4216 (4)	0.0475 (17)
H4WA	−0.1203	0.6053	0.3750	0.071*
H4WB	−0.1606	0.5920	0.4533	0.071*
O5W	0.6697 (5)	0.2093 (11)	0.4653 (5)	0.062 (2)
H5WA	0.6465	0.2278	0.5141	0.092*
H5WB	0.6894	0.3201	0.4485	0.092*
O6W	0.8488 (7)	0.0366 (15)	0.4616 (8)	0.114 (4)
H6WA	0.8232	0.1311	0.4498	0.172*
H6WB	0.8175	−0.0498	0.4851	0.172*
Zn1	0.54125 (6)	0.71412 (16)	0.37644 (6)	0.0342 (4)
Zn2	0.0000	0.5000	0.5000	0.0330 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.024 (4)	0.027 (4)	0.025 (4)	−0.002 (3)	−0.004 (3)	0.004 (3)
C2	0.019 (4)	0.029 (4)	0.026 (4)	0.003 (3)	0.002 (3)	0.005 (3)
C3	0.024 (4)	0.030 (4)	0.015 (3)	0.000 (3)	0.003 (3)	0.002 (3)
C4	0.023 (4)	0.036 (4)	0.016 (4)	0.001 (3)	0.003 (3)	0.002 (3)
C5	0.023 (4)	0.044 (5)	0.020 (4)	0.001 (3)	0.002 (3)	0.000 (3)
C6	0.019 (4)	0.036 (4)	0.024 (4)	−0.004 (3)	−0.005 (3)	0.001 (3)
C7	0.021 (4)	0.034 (4)	0.016 (4)	−0.002 (3)	−0.001 (3)	0.005 (3)
C8	0.027 (4)	0.054 (5)	0.020 (4)	−0.002 (4)	0.001 (3)	0.002 (3)
C9	0.018 (3)	0.036 (4)	0.018 (4)	−0.003 (3)	0.003 (3)	0.000 (3)
O1	0.018 (3)	0.068 (4)	0.033 (3)	0.001 (3)	0.002 (2)	0.007 (3)
O2	0.024 (3)	0.057 (4)	0.024 (3)	−0.001 (3)	−0.005 (2)	0.000 (2)
O3	0.027 (3)	0.062 (4)	0.018 (3)	−0.003 (3)	0.002 (2)	0.009 (3)
O4	0.020 (3)	0.071 (4)	0.030 (3)	0.002 (3)	0.004 (2)	0.010 (3)
O5	0.020 (3)	0.077 (4)	0.024 (3)	0.000 (3)	−0.006 (2)	0.005 (3)
O6	0.030 (3)	0.139 (7)	0.022 (3)	−0.021 (4)	0.000 (3)	0.012 (4)
O1W	0.041 (3)	0.060 (4)	0.038 (4)	0.001 (3)	−0.010 (3)	0.001 (3)
O2W	0.039 (4)	0.059 (4)	0.051 (4)	0.009 (3)	−0.007 (3)	−0.017 (3)
O3W	0.045 (4)	0.056 (4)	0.035 (3)	0.003 (3)	0.013 (3)	0.001 (3)
O4W	0.029 (3)	0.080 (5)	0.034 (3)	0.006 (3)	0.004 (3)	0.006 (3)
O5W	0.073 (5)	0.064 (5)	0.048 (4)	−0.006 (4)	0.011 (4)	−0.012 (3)
O6W	0.105 (8)	0.080 (7)	0.166 (11)	−0.032 (6)	0.057 (8)	−0.003 (7)
Zn1	0.0231 (5)	0.0556 (7)	0.0228 (6)	0.0024 (4)	−0.0043 (4)	−0.0048 (4)
Zn2	0.0246 (7)	0.0539 (9)	0.0211 (7)	0.0012 (6)	0.0059 (5)	0.0050 (6)

Geometric parameters (Å, º) top

C1—O1	1.248 (9)	O1W—Zn1	1.981 (7)
C1—O2	1.256 (9)	O1W—H1WA	0.8505
C1—C2	1.495 (10)	O1W—H1WB	0.8502
C2—C9	1.372 (11)	O2W—Zn1	1.965 (6)
C2—C3	1.380 (10)	O2W—H2WA	0.8584
C3—C4	1.390 (10)	O2W—H2WB	0.8429
C3—H3	0.9300	O3W—Zn2	2.150 (6)
C4—C6	1.392 (10)	O3W—H3WA	0.8498
C4—C5	1.511 (10)	O3W—H3WB	0.8494
C5—O3	1.244 (9)	O4W—Zn2	2.099 (6)
C5—O4	1.263 (9)	O4W—H4WA	0.8483
C6—C7	1.344 (10)	O4W—H4WB	0.8518
C6—H6	0.9300	O5W—H5WA	0.8487
C7—C9	1.382 (10)	O5W—H5WB	0.8538
C7—C8	1.501 (10)	O6W—H6WA	0.7595
C8—O6	1.235 (10)	O6W—H6WB	0.8431
C8—O5	1.275 (10)	Zn1—O5ⁱⁱ	1.946 (6)
C9—H9	0.9300	Zn1—H2WB	2.0711
O1—Zn1	2.412 (6)	Zn2—O3ⁱⁱⁱ	2.049 (5)
O2—Zn1	1.999 (5)	Zn2—O4Wⁱⁱⁱ	2.099 (6)
O3—Zn2	2.049 (5)	Zn2—O3Wⁱⁱⁱ	2.150 (6)
O5—Zn1ⁱ	1.946 (6)

O1—C1—O2	119.4 (7)	Zn2—O3W—H3WB	152.2
O1—C1—C2	120.1 (7)	H3WA—O3W—H3WB	107.8
O2—C1—C2	120.5 (7)	Zn2—O4W—H4WA	116.8
C9—C2—C3	119.3 (7)	Zn2—O4W—H4WB	108.0
C9—C2—C1	120.4 (6)	H4WA—O4W—H4WB	107.7
C3—C2—C1	120.4 (7)	H5WA—O5W—H5WB	107.5
C2—C3—C4	120.8 (7)	H6WA—O6W—H6WB	114.2
C2—C3—H3	119.6	O5ⁱⁱ—Zn1—O2W	109.2 (3)
C4—C3—H3	119.6	O5ⁱⁱ—Zn1—O1W	101.6 (3)
C3—C4—C6	116.9 (6)	O2W—Zn1—O1W	108.0 (3)
C3—C4—C5	121.2 (6)	O5ⁱⁱ—Zn1—O2	101.8 (2)
C6—C4—C5	121.7 (6)	O2W—Zn1—O2	120.0 (2)
O3—C5—O4	124.5 (7)	O1W—Zn1—O2	114.4 (2)
O3—C5—C4	117.4 (7)	O5ⁱⁱ—Zn1—O1	159.2 (2)
O4—C5—C4	118.0 (7)	O2W—Zn1—O1	86.6 (2)
C7—C6—C4	123.5 (7)	O1W—Zn1—O1	85.5 (2)
C7—C6—H6	118.3	O2—Zn1—O1	57.8 (2)
C4—C6—H6	118.3	O5ⁱⁱ—Zn1—H2WB	111.6
C6—C7—C9	118.0 (7)	O2W—Zn1—H2WB	23.9
C6—C7—C8	120.6 (7)	O1W—Zn1—H2WB	128.1
C9—C7—C8	121.4 (7)	O2—Zn1—H2WB	96.9
O6—C8—O5	124.0 (7)	O1—Zn1—H2WB	77.4
O6—C8—C7	120.6 (7)	O3ⁱⁱⁱ—Zn2—O3	180.000 (1)
O5—C8—C7	115.4 (7)	O3ⁱⁱⁱ—Zn2—O4W	87.5 (2)
C2—C9—C7	121.4 (7)	O3—Zn2—O4W	92.5 (2)
C2—C9—H9	119.3	O3ⁱⁱⁱ—Zn2—O4Wⁱⁱⁱ	92.5 (2)
C7—C9—H9	119.3	O3—Zn2—O4Wⁱⁱⁱ	87.5 (2)
C1—O1—Zn1	81.8 (4)	O4W—Zn2—O4Wⁱⁱⁱ	180.000 (1)
C1—O2—Zn1	100.9 (5)	O3ⁱⁱⁱ—Zn2—O3Wⁱⁱⁱ	90.4 (2)
C5—O3—Zn2	131.1 (5)	O3—Zn2—O3Wⁱⁱⁱ	89.6 (2)
C8—O5—Zn1ⁱ	116.7 (5)	O4W—Zn2—O3Wⁱⁱⁱ	92.0 (3)
Zn1—O1W—H1WA	141.2	O4Wⁱⁱⁱ—Zn2—O3Wⁱⁱⁱ	88.0 (3)
Zn1—O1W—H1WB	98.5	O3ⁱⁱⁱ—Zn2—O3W	89.6 (2)
H1WA—O1W—H1WB	107.6	O3—Zn2—O3W	90.4 (2)
Zn1—O2W—H2WA	134.0	O4W—Zn2—O3W	88.0 (3)
Zn1—O2W—H2WB	85.1	O4Wⁱⁱⁱ—Zn2—O3W	92.0 (3)
H2WA—O2W—H2WB	107.6	O3Wⁱⁱⁱ—Zn2—O3W	180.000 (1)
Zn2—O3W—H3WA	82.1

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O4W—H4WB···O6^iv	0.85	1.97	2.768 (9)	155
O5W—H5WA···O2^v	0.85	1.99	2.842 (9)	179
O6W—H6WB···O6^vi	0.84	2.29	3.058 (13)	153
O5W—H5WB···O6ⁱⁱ	0.85	2.59	3.356 (12)	150

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

Experimental details

Crystal data
Chemical formula	[Zn₃(C₉H₃O₆)₂(H₂O)₈]·4H₂O
M_r	826.59
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	296
a, b, c (Å)	14.745 (2), 6.7960 (12), 15.183 (3)
β (°)	94.543 (2)
V (Å³)	1516.7 (4)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.45
Crystal size (mm)	0.27 × 0.24 × 0.23

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.521, 0.569
No. of measured, independent and observed [I > 2σ(I)] reflections	7485, 2729, 1990
R_int	0.047
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.064, 0.225, 1.13
No. of reflections	2729
No. of parameters	205
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.89, −0.90

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), 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
O4W—H4WB···O6ⁱ	0.85	1.97	2.768 (9)	154.6
O5W—H5WA···O2ⁱⁱ	0.85	1.99	2.842 (9)	178.7
O6W—H6WB···O6ⁱⁱⁱ	0.84	2.29	3.058 (13)	152.5
O5W—H5WB···O6^iv	0.85	2.59	3.356 (12)	149.5

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

Acknowledgements

The authors acknowledge South China Normal University and the National Natural Science Foundation of China, grant No. 20871048, for supporting this work.

References

Batten, S. R. & Murray, K. S. (2003). Coord. Chem. Rev. 246, 103–130. Web of Science CrossRef CAS Google Scholar
Bruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Chen, S. S., Fan, J., Okamura, T. A., Chen, M. S., Su, Z., Sun, W. Y. & Ueyama, N. (2010). Cryst. Growth Des. 10, 812–822. CrossRef CAS Google Scholar
Hua, Q., Zhao, Y., Xu, G. C., Chen, M. S., Su, Z., Cai, K. & Sun, W. Y. (2010). Cryst. Growth Des. 10, 2553–2562. CrossRef CAS Google Scholar
Liang, X. Q., Zhou, X. H., Chen, C., Xiao, H. P., Li, Y. Z. & Zuo, J. L. (2009). Cryst. Growth Des. 9, 1041–1053. CrossRef CAS Google Scholar
Qiu, Y. C., Li, Y. H., Peng, G., Cai, J. B., Jin, L. M., Ma, L., Deng, H., Zeller, M. & Batten, S. R. (2010). Cryst. Growth Des. 10, 1332–13401. CrossRef CAS Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wang, X., Wang, W. Y., Liu, S. M., Hou, H. W. & Fan, Y. T. (2009). J. Mol. Struct. 938, 185–191. CrossRef CAS Google Scholar
Xu, L., Choi, E. Y. & Kwon, Y. U. (2007). Inorg. Chem. 46, 10670–10680. Web of Science CSD CrossRef PubMed CAS Google Scholar
Xu, L., Choi, E. Y. & Kwon, Y. U. (2008). Inorg. Chem. Commun. 11, 1190–1193. CrossRef CAS Google Scholar
Yaghi, O. M., Davis, C. E., Li, G. M. & Li, H. L. (1997). J. Am. Chem. Soc. 119, 2861–2868. CSD CrossRef CAS Web of Science Google Scholar
Yang, E. C., Liu, Z. Y., Wang, X. G., Batten, S. R. & Zhao, X. J. (2008). CrystEngComm, 10, 1140–1143. CrossRef CAS Google Scholar
Zhong, R. Q., Zou, R. Q., Du, M., Takeichi, N. & Xu, Q. (2008). CrystEngComm, 10, 1175–1179. CrossRef CAS Google Scholar

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