catena-Poly[[triaqua­(pyridine-κN)nickel(II)]-μ-sulfato-κ2O:O′]

Shi, Y.-F.; Li, F.-X.; Geng, B.; Liu, Y.-C.; Chen, Z.-F.

doi:10.1107/S1600536809049605

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 12| December 2009| Page m1665

doi:10.1107/S1600536809049605

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catena-Poly[[triaqua(pyridine-κN)nickel(II)]-μ-sulfato-κ²O:O′]

Yan-Fang Shi,^a Fu-Xing Li,^a Bo Geng,^a Yan-Cheng Liu ^a and Zhen-Feng Chen ^a ^*

^aKey Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China), School of Chemistry & Chemical Engineering, Guangxi Normal University, Guilin 541004, People's Republic of China
^*Correspondence e-mail: chenzfgxnu@yahoo.com

(Received 2 November 2009; accepted 19 November 2009; online 25 November 2009)

The title compound, [Ni(SO₄)(C₅H₅N)(H₂O)₃]_n, was synthesized by the hydrothermal reaction of NiSO₄·6H₂O, pyridine and water. The central Ni^II atom is coordinated in a distorted octahedral environment by a pyridine N atom, three aqua O atoms and two O atoms of bridging sulfate anions, yielding a zigzag chain. A three-dimensional network is generated via complex hydrogen bonds involving the sulfate and aqua ligands and a pyridine C—H group.

Related literature

For the structures of related nickel(II) complexes, see: Wang et al. (2006 ); Stein et al. (2007 ).

Experimental

Crystal data

[Ni(SO₄)(C₅H₅N)(H₂O)₃]
M_r = 287.92
Monoclinic, P 2₁ /c
a = 11.868 (3) Å
b = 7.5745 (14) Å
c = 11.420 (3) Å
β = 110.724 (4)°
V = 960.2 (3) Å³
Z = 4
Mo Kα radiation
μ = 2.26 mm⁻¹
T = 193 K
0.30 × 0.20 × 0.14 mm

Data collection

Rigaku Mercury CCD diffractometer
Absorption correction: multi-scan (REQAB; Jacobson, 1998 ) T_min = 0.465, T_max = 0.729
8854 measured reflections
1746 independent reflections
1641 reflections with I > 2σ(I)
R_int = 0.040

Refinement

R[F² > 2σ(F²)] = 0.036
wR(F²) = 0.110
S = 1.16
1746 reflections
161 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.57 e Å⁻³
Δρ_min = −0.84 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5A⋯O4ⁱ	0.82 (3)	2.04 (3)	2.849 (3)	170 (4)
O5—H5B⋯O1ⁱⁱ	0.818 (10)	1.939 (12)	2.753 (3)	173 (4)
O6—H6A⋯O3ⁱ	0.821 (10)	1.949 (12)	2.764 (3)	172 (4)
O6—H6B⋯O4	0.82 (3)	2.15 (3)	2.821 (3)	139 (4)
O7—H7A⋯O2ⁱⁱ	0.82 (3)	2.00 (3)	2.817 (3)	176 (4)
O7—H7B⋯O4ⁱⁱⁱ	0.815 (10)	1.94 (2)	2.690 (3)	153 (4)
C4—H4⋯O3^iv	0.95	2.57	3.304 (5)	135
Symmetry codes: (i) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) -x+1, -y+1, -z; (iii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) x+1, y, z.

Data collection: CrystalClear (Rigaku, 1999 ); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC & Rigaku, 2000 ); 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/S1600536809049605/pk2206sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809049605/pk2206Isup2.hkl

checkCIF report

Comment top

The asymmetric unit contains one independent Ni atom, which is octahedrally coordinated by two sulfato anions, three aqua ligands and one pyridine molecule. The bond lengths and angles involving Ni—O(aqua), Ni—N are similar to those of other nickel-carboxylate coordination polymers with pyridine (Wang et al., 2006; Stein et al., 2007), with the Ni center displaying the typical distorted octahedral coordination, which can be viewed from the angles of N1—Ni1—O1 177.81 (10)°, N1—Ni1—O7 91.13 (11)°, O1—Ni1—O6 92.13 (9)°, O5—Ni1—O6 92.91 (10)° (Fig. 1). The SO₄^2- dianion acts as a µ₂ bridging ligand, linking two adjacent metal ions and generating a one-dimensional zigzag chain (Fig. 2). The aqua ligands, sulfato groups and C—H of pyridine form extensive hydrogen-bonding interactions (Table 1), resulting in a three-dimensional network (Fig. 3).

Related literature top

For the structures of related nickel(II) complexes, see: Wang et al. (2006); Stein et al. (2007).

Experimental top

Samples of NiSO₄.6H₂O (0.1 mmol) and pyridine (0.1 mmol) were placed in a thick-walled Pyrex tube (ca 20 cm long). After addition of H₂O (1 ml), the tube was frozen with liquid nitrogen, evacuated under vacuum and sealed with a torch. The tube was heated at 110°C for 2 days and then was slowly cooled down to room temperature, and light-green block-shaped crystals were obtained. Yield: 35%.

Computing details top

Data collection: CrystalClear (Rigaku, 1999); cell refinement: CrystalClear (Rigaku, 1999); data reduction: CrystalStructure (Rigaku/MSC & Rigaku, 2000); 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 molecular structure showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level.
	Fig. 2. A view of the one-dimensional chain structure that propagates along the b axis.
	Fig. 3. A packing diagram viewed approximately down the b axis.

catena-poly[[triaqua(pyridine-κN)nickel(II)]- µ-sulfato-κ²O:O'] top

Crystal data top

[Ni(SO₄)(C₅H₅N)(H₂O)₃]	F(000) = 592
M_r = 287.92	D_x = 1.992 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ybc	Cell parameters from 3550 reflections
a = 11.868 (3) Å	θ = 3.1–25.3°
b = 7.5745 (14) Å	µ = 2.26 mm⁻¹
c = 11.420 (3) Å	T = 193 K
β = 110.724 (4)°	Block, light-green
V = 960.2 (3) Å³	0.30 × 0.20 × 0.14 mm
Z = 4

Data collection top

Rigaku Mercury CCD diffractometer	1746 independent reflections
Radiation source: fine-focus sealed tube	1641 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.040
Detector resolution: 7.31 pixels mm^-1	θ_max = 25.3°, θ_min = 3.3°
ω scans	h = −14→13
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −9→9
T_min = 0.465, T_max = 0.729	l = −13→12
8854 measured reflections

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.110	H atoms treated by a mixture of independent and constrained refinement
S = 1.16	w = 1/[σ²(F_o²) + (0.0672P)² + 0.4274P] where P = (F_o² + 2F_c²)/3
1746 reflections	(Δ/σ)_max = 0.001
161 parameters	Δρ_max = 0.57 e Å⁻³
6 restraints	Δρ_min = −0.84 e Å⁻³

Crystal data top

[Ni(SO₄)(C₅H₅N)(H₂O)₃]	V = 960.2 (3) Å³
M_r = 287.92	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.868 (3) Å	µ = 2.26 mm⁻¹
b = 7.5745 (14) Å	T = 193 K
c = 11.420 (3) Å	0.30 × 0.20 × 0.14 mm
β = 110.724 (4)°

Data collection top

Rigaku Mercury CCD diffractometer	1746 independent reflections
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	1641 reflections with I > 2σ(I)
T_min = 0.465, T_max = 0.729	R_int = 0.040
8854 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	6 restraints
wR(F²) = 0.110	H atoms treated by a mixture of independent and constrained refinement
S = 1.16	Δρ_max = 0.57 e Å⁻³
1746 reflections	Δρ_min = −0.84 e Å⁻³
161 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
Ni1	0.65136 (3)	0.59664 (5)	0.21049 (4)	0.0112 (2)
S1	0.37812 (7)	0.51034 (10)	0.20733 (7)	0.0111 (2)
O1	0.4632 (2)	0.5757 (3)	0.1473 (2)	0.0144 (5)
O2	0.3600 (2)	0.3178 (3)	0.1818 (2)	0.0148 (5)
O3	0.2651 (2)	0.6067 (3)	0.1535 (2)	0.0185 (6)
O4	0.4322 (2)	0.5392 (3)	0.3441 (2)	0.0163 (5)
O5	0.6504 (2)	0.3741 (3)	0.1062 (2)	0.0139 (5)
H5A	0.626 (3)	0.283 (3)	0.128 (3)	0.017 (10)*
H5B	0.619 (4)	0.381 (6)	0.0300 (11)	0.033 (13)*
O6	0.6708 (2)	0.4525 (3)	0.3691 (2)	0.0165 (5)
H6A	0.687 (4)	0.3472 (19)	0.367 (4)	0.037 (13)*
H6B	0.611 (2)	0.435 (5)	0.387 (4)	0.028 (12)*
O7	0.6283 (2)	0.7484 (3)	0.0563 (2)	0.0212 (6)
H7A	0.632 (4)	0.724 (5)	−0.0120 (19)	0.034 (12)*
H7B	0.609 (4)	0.850 (2)	0.064 (4)	0.031 (12)*
N1	0.8352 (3)	0.6199 (4)	0.2656 (3)	0.0179 (7)
C1	0.9028 (3)	0.6672 (5)	0.3822 (3)	0.0247 (8)
H1	0.8637	0.6950	0.4394	0.030*
C2	1.0269 (3)	0.6774 (6)	0.4232 (4)	0.0325 (9)
H2	1.0718	0.7112	0.5069	0.039*
C3	1.0846 (3)	0.6379 (6)	0.3407 (4)	0.0345 (10)
H3	1.1699	0.6441	0.3664	0.041*
C4	1.0165 (4)	0.5894 (5)	0.2207 (5)	0.0331 (10)
H4	1.0539	0.5612	0.1620	0.040*
C5	0.8929 (3)	0.5822 (5)	0.1867 (4)	0.0255 (9)
H5C	0.8464	0.5490	0.1034	0.031*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0115 (3)	0.0107 (3)	0.0109 (3)	−0.00030 (14)	0.0035 (2)	0.00009 (15)
S1	0.0122 (4)	0.0103 (4)	0.0114 (4)	−0.0005 (3)	0.0050 (3)	−0.0009 (3)
O1	0.0123 (12)	0.0198 (13)	0.0129 (12)	−0.0013 (9)	0.0066 (10)	0.0014 (9)
O2	0.0222 (13)	0.0097 (12)	0.0127 (11)	−0.0012 (9)	0.0064 (10)	−0.0036 (10)
O3	0.0172 (13)	0.0147 (13)	0.0259 (14)	0.0034 (9)	0.0103 (11)	0.0035 (10)
O4	0.0226 (13)	0.0160 (12)	0.0113 (12)	−0.0048 (10)	0.0071 (10)	−0.0043 (10)
O5	0.0188 (13)	0.0144 (12)	0.0081 (12)	−0.0028 (10)	0.0042 (10)	0.0010 (10)
O6	0.0158 (13)	0.0135 (13)	0.0198 (13)	−0.0005 (11)	0.0058 (10)	0.0022 (11)
O7	0.0361 (15)	0.0135 (14)	0.0175 (14)	0.0053 (11)	0.0139 (12)	0.0009 (11)
N1	0.0154 (15)	0.0150 (15)	0.0223 (16)	−0.0002 (11)	0.0053 (12)	0.0016 (12)
C1	0.0198 (19)	0.029 (2)	0.0217 (19)	−0.0036 (16)	0.0025 (15)	−0.0012 (17)
C2	0.020 (2)	0.035 (2)	0.033 (2)	−0.0033 (17)	−0.0025 (17)	0.002 (2)
C3	0.0139 (19)	0.028 (2)	0.057 (3)	−0.0045 (16)	0.007 (2)	0.004 (2)
C4	0.024 (2)	0.028 (2)	0.056 (3)	−0.0004 (17)	0.025 (2)	0.002 (2)
C5	0.0198 (19)	0.029 (2)	0.030 (2)	−0.0035 (15)	0.0124 (17)	−0.0038 (17)

Geometric parameters (Å, º) top

Ni1—O7	2.039 (2)	O6—H6B	0.82 (3)
Ni1—N1	2.053 (3)	O7—H7A	0.82 (3)
Ni1—O6	2.056 (2)	O7—H7B	0.815 (10)
Ni1—O5	2.062 (2)	N1—C1	1.337 (5)
Ni1—O1	2.096 (2)	N1—C5	1.342 (5)
Ni1—O2ⁱ	2.110 (2)	C1—C2	1.380 (5)
S1—O3	1.458 (2)	C1—H1	0.9500
S1—O4	1.479 (2)	C2—C3	1.380 (6)
S1—O2	1.488 (2)	C2—H2	0.9500
S1—O1	1.491 (2)	C3—C4	1.372 (6)
O2—Ni1ⁱⁱ	2.110 (2)	C3—H3	0.9500
O5—H5A	0.82 (3)	C4—C5	1.379 (6)
O5—H5B	0.818 (10)	C4—H4	0.9500
O6—H6A	0.821 (10)	C5—H5C	0.9500

O7—Ni1—N1	91.13 (11)	H5A—O5—H5B	108 (4)
O7—Ni1—O6	177.36 (10)	Ni1—O6—H6A	117 (3)
N1—Ni1—O6	89.97 (11)	Ni1—O6—H6B	118 (3)
O7—Ni1—O5	89.45 (9)	H6A—O6—H6B	94 (4)
N1—Ni1—O5	92.04 (11)	Ni1—O7—H7A	131 (3)
O6—Ni1—O5	92.91 (10)	Ni1—O7—H7B	113 (3)
O7—Ni1—O1	86.80 (10)	H7A—O7—H7B	115 (4)
N1—Ni1—O1	177.81 (10)	C1—N1—C5	117.1 (3)
O6—Ni1—O1	92.13 (9)	C1—N1—Ni1	121.8 (2)
O5—Ni1—O1	87.23 (9)	C5—N1—Ni1	121.1 (3)
O7—Ni1—O2ⁱ	92.22 (9)	N1—C1—C2	123.1 (4)
N1—Ni1—O2ⁱ	91.89 (10)	N1—C1—H1	118.5
O6—Ni1—O2ⁱ	85.33 (9)	C2—C1—H1	118.5
O5—Ni1—O2ⁱ	175.69 (9)	C3—C2—C1	118.9 (4)
O1—Ni1—O2ⁱ	88.90 (9)	C3—C2—H2	120.5
O3—S1—O4	111.21 (14)	C1—C2—H2	120.5
O3—S1—O2	111.13 (13)	C4—C3—C2	118.8 (4)
O4—S1—O2	109.26 (13)	C4—C3—H3	120.6
O3—S1—O1	108.13 (14)	C2—C3—H3	120.6
O4—S1—O1	108.95 (13)	C3—C4—C5	118.9 (4)
O2—S1—O1	108.08 (12)	C3—C4—H4	120.6
S1—O1—Ni1	132.76 (14)	C5—C4—H4	120.6
S1—O2—Ni1ⁱⁱ	134.32 (13)	N1—C5—C4	123.2 (4)
Ni1—O5—H5A	116 (3)	N1—C5—H5C	118.4
Ni1—O5—H5B	118 (3)	C4—C5—H5C	118.4

O3—S1—O1—Ni1	150.13 (18)	O2ⁱ—Ni1—N1—C1	37.9 (3)
O4—S1—O1—Ni1	29.1 (2)	O7—Ni1—N1—C5	−52.1 (3)
O2—S1—O1—Ni1	−89.5 (2)	O6—Ni1—N1—C5	130.3 (3)
O7—Ni1—O1—S1	−167.8 (2)	O5—Ni1—N1—C5	37.4 (3)
O6—Ni1—O1—S1	9.8 (2)	O2ⁱ—Ni1—N1—C5	−144.4 (3)
O5—Ni1—O1—S1	102.64 (19)	C5—N1—C1—C2	−0.3 (5)
O2ⁱ—Ni1—O1—S1	−75.47 (19)	Ni1—N1—C1—C2	177.5 (3)
O3—S1—O2—Ni1ⁱⁱ	−103.2 (2)	N1—C1—C2—C3	0.2 (6)
O4—S1—O2—Ni1ⁱⁱ	19.9 (2)	C1—C2—C3—C4	−0.1 (6)
O1—S1—O2—Ni1ⁱⁱ	138.29 (18)	C2—C3—C4—C5	0.1 (6)
O7—Ni1—N1—C1	130.2 (3)	C1—N1—C5—C4	0.3 (5)
O6—Ni1—N1—C1	−47.4 (3)	Ni1—N1—C5—C4	−177.5 (3)
O5—Ni1—N1—C1	−140.3 (3)	C3—C4—C5—N1	−0.3 (6)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O4ⁱⁱ	0.82 (3)	2.04 (3)	2.849 (3)	170 (4)
O5—H5A···S1ⁱⁱ	0.82 (3)	2.81 (2)	3.571 (3)	157 (3)
O5—H5B···O1ⁱⁱⁱ	0.82 (1)	1.94 (1)	2.753 (3)	173 (4)
O5—H5B···S1ⁱⁱⁱ	0.82 (1)	2.85 (2)	3.584 (3)	151 (4)
O6—H6A···O3ⁱⁱ	0.82 (1)	1.95 (1)	2.764 (3)	172 (4)
O6—H6A···S1ⁱⁱ	0.82 (1)	2.71 (2)	3.458 (3)	152 (4)
O6—H6B···O4	0.82 (3)	2.15 (3)	2.821 (3)	139 (4)
O6—H6B···S1	0.82 (3)	2.85 (4)	3.336 (3)	120 (3)
O7—H7A···O2ⁱⁱⁱ	0.82 (3)	2.00 (3)	2.817 (3)	176 (4)
O7—H7A···S1ⁱⁱⁱ	0.82 (3)	2.82 (2)	3.571 (3)	154 (4)
O7—H7B···O4ⁱ	0.82 (1)	1.94 (2)	2.690 (3)	153 (4)
O7—H7B···S1ⁱ	0.82 (1)	2.84 (4)	3.372 (3)	125 (4)
C4—H4···O3^iv	0.95	2.57	3.304 (5)	135

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

Experimental details

Crystal data
Chemical formula	[Ni(SO₄)(C₅H₅N)(H₂O)₃]
M_r	287.92
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	193
a, b, c (Å)	11.868 (3), 7.5745 (14), 11.420 (3)
β (°)	110.724 (4)
V (Å³)	960.2 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.26
Crystal size (mm)	0.30 × 0.20 × 0.14

Data collection
Diffractometer	Rigaku Mercury CCD diffractometer
Absorption correction	Multi-scan (REQAB; Jacobson, 1998)
T_min, T_max	0.465, 0.729
No. of measured, independent and observed [I > 2σ(I)] reflections	8854, 1746, 1641
R_int	0.040
(sin θ/λ)_max (Å⁻¹)	0.602

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.110, 1.16
No. of reflections	1746
No. of parameters	161
No. of restraints	6
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.57, −0.84

Computer programs: CrystalClear (Rigaku, 1999), CrystalStructure (Rigaku/MSC & Rigaku, 2000), 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
O5—H5A···O4ⁱ	0.82 (3)	2.04 (3)	2.849 (3)	170 (4)
O5—H5A···S1ⁱ	0.82 (3)	2.805 (18)	3.571 (3)	157 (3)
O5—H5B···O1ⁱⁱ	0.818 (10)	1.939 (12)	2.753 (3)	173 (4)
O5—H5B···S1ⁱⁱ	0.818 (10)	2.85 (2)	3.584 (3)	151 (4)
O6—H6A···O3ⁱ	0.821 (10)	1.949 (12)	2.764 (3)	172 (4)
O6—H6A···S1ⁱ	0.821 (10)	2.71 (2)	3.458 (3)	152 (4)
O6—H6B···O4	0.82 (3)	2.15 (3)	2.821 (3)	139 (4)
O6—H6B···S1	0.82 (3)	2.85 (4)	3.336 (3)	120 (3)
O7—H7A···O2ⁱⁱ	0.82 (3)	2.00 (3)	2.817 (3)	176 (4)
O7—H7A···S1ⁱⁱ	0.82 (3)	2.82 (2)	3.571 (3)	154 (4)
O7—H7B···O4ⁱⁱⁱ	0.815 (10)	1.94 (2)	2.690 (3)	153 (4)
O7—H7B···S1ⁱⁱⁱ	0.815 (10)	2.84 (4)	3.372 (3)	125 (4)
C4—H4···O3^iv	0.95	2.57	3.304 (5)	134.6

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

Acknowledgements

The authors thank the National Natural Science Foundation of China (No. 20861002), the 973 Plan of China (2009CB526503), the Natural Science Foundation of Guangxi, China (Nos. 0991003, 0991012Z) and the Open Foundation of the Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China) for financial support.

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