Two-dimensional dysprosium(III) triiodate(V) dihydrate, Dy(IO3)3(H2O)·H2O

Chai, W.; Song, L.; Shi, H.; Qin, L.; Shu, K.

doi:10.1107/S1600536809027068

inorganic compounds

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ISSN: 2056-9890

Volume 65| Part 8| August 2009| Pages i61-i62

doi:10.1107/S1600536809027068

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Two-dimensional dysprosium(III) triiodate(V) dihydrate, Dy(IO₃)₃(H₂O)·H₂O

Wenxiang Chai,^a ^* Li Song,^b Hongsheng Shi,^a Laishun Qin ^a and Kangying Shu ^a

^aCollege of Materials Science and Engineering, China Jiliang University, Hangzhou 310018, People's Republic of China, and ^bDepartment of Chemistry, Key Laboratory of Advanced Textile Materials and Manufacturing Technology of the Education Ministry, Zhejiang Sci-Tech University, Hangzhou 310018, People's Republic of China
^*Correspondence e-mail: wxchai_cm@yahoo.com.cn

(Received 1 July 2009; accepted 10 July 2009; online 15 July 2009)

During our research into novel nonlinear optical materials using 1,10-phenanthroline as an appending ligand on lanthanide iodates, crystals of an infinite layered Dy^III iodate compound, Dy(IO₃)₃(H₂O)·H₂O, were obtained under hydrothermal conditions. The Dy^III cation has a dicapped trigonal prismatic coordination environment consisting of one water O atom and seven other O atoms from seven iodate anions. These iodate anions bridge the Dy^III cations into a two-dimensional structure. Through O—H⋯O hydrogen bonds, all of these layers stack along [111], giving a supramolecular channel, with the solvent water molecules filling the voids.

Related literature

For related materials with non-linear optical propertie, see: Rosenzweig & Morosin (1966 ); Liminga et al. (1977 ); Ok & Halasyamani (2005 ). The method of preparation was based on HIO₃, which is different to the previous method of obtaining periodates (Douglas et al., 2004 ; Assefa et al., 2006 ). For noncentrosymmetric inorganic–organic framework structures synthesized from organic ligands, see: Sun et al. (2009 ). For related structrues, see: Sun et al. (2009); Assefa et al. (2006); Douglas et al. (2004); Ok & Halasyamani (2005); Chen et al. (2005 ).

Experimental

Crystal data

Dy(IO₃)₃H₂O·H₂O
M_r = 723.23
Triclinic, $[P \overline 1]$
a = 7.15990 (10) Å
b = 7.4292 (1) Å
c = 10.64430 (10) Å
α = 95.161 (12)°
β = 104.858 (7)°
γ = 110.081 (8)°
V = 504.00 (5) Å³
Z = 2
Mo Kα radiation
μ = 16.65 mm⁻¹
T = 293 K
0.16 × 0.12 × 0.06 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.136, T_max = 0.435 (expected range = 0.115–0.368)
3819 measured reflections
2260 independent reflections
2067 reflections with I > 2σ(I)
R_int = 0.027

Refinement

R[F² > 2σ(F²)] = 0.038
wR(F²) = 0.109
S = 1.06
2260 reflections
141 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 2.79 e Å⁻³
Δρ_min = −3.20 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O10—H10A⋯O3ⁱ	0.80	2.29	2.873 (10)	131
O10—H10B⋯O9ⁱ	0.80	2.33	2.753 (11)	114
O11—H11A⋯O8ⁱⁱ	0.80	2.22	2.954 (11)	153
O11—H11B⋯O7ⁱⁱⁱ	0.80	2.26	2.946 (11)	145
Symmetry codes: (i) x, y-1, z; (ii) x, y-1, z+1; (iii) -x, -y-1, -z.

Data collection: PROCESS-AUTO (Rigaku, 1998 ); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004 ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009 ; van der Sluis & Spek, 1990 ); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809027068/br2111sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809027068/br2111Isup2.hkl

checkCIF report

Comment top

In the 1970s, metal iodates have been extensively studied by Bell Laboratories not only for their nonlinear optical (NLO) properties but also for ferroelectric, piezoelectric and pyroelectric properties (Rosenzweig & Morosin, 1966; Liminga et al., 1977). In attempts to prepare noncentrosymmetric structures of lanthanide iodates, about six anhydrous structure types have been reported, in addition to numerous hydrated structures ranging from hemihydrates to pentahydrates. (Assefa et al., 2006). After comparing these structure types, herein, we find that the hydrated structures favor of adopting centrosymmetric structures. Then organic ligands are come into our view because they could form noncentrosymmetric inorganic–organic framework structures with metal ion. (Sun et al., 2009). Here, we firstly report a infinite layered Dy^III iodate dihydrate synthesized from the hydrothermal reaction of Dy₂O₃, HIO₃ and 1,10-phenanthroline.

In the title compound, the Dy^III cation has dicapped trigonal prismatic coordination sphere. The coordination enciroments of the rare earth Dy^III cation consist of eight O atoms derived from seven iodate anions and one water molecule (see Fig. 1). And these seven iodates are classed two types, one is three 3-connected iodates (of I2) through three O atoms, and the other is four iodates 2-connected (of I1 or I3) through two O atoms. Then these iodate anions bridge Dy atoms into two dimensional structure. And between the adjacent layers, there are two types of hydrogen bonds, one is O10—H10A···O3 bond, the other is O10—H10B···O9 bond. Then through these hydrogen bonds, all of these layers stacking along [111] axis to give out of a supramolecular channel. And the solvent water molecules fill in the channels, and stick on the channel with two hydrogen bonds of O11—H11A···O8 and O11—H11B···O7. (see Fig. 2) The hydrogen bonding data of lengths and angles are in the range of ordinary examples and have been examined by the PLATON program (Spek, 2009; van der Sluis & Spek, 1990).

Related literature top

For related NLO materials, see: Rosenzweig & Morosin (1966); Liminga et al. (1977); Ok & Halasyamani (2005). The method of preparation was based on HIO₃, which is different to the previous method of obtaining periodates (Douglas et al., 2004; Assefa et al., 2006). For noncentrosymmetric inorganic–organic framework structures synthesized from organic ligands, see: Sun et al. (2009). For related structrues, see: Sun et al. (2009); Assefa et al. (2006); Douglas et al. (2004); Ok & Halasyamani (2005); Chen et al. (2005).

Experimental top

All chemicals were obtained from commercial sources and were used as received. The title compound was handily synthesized by a hydrothermal reaction from iodic acid. To a 25 ml stainless steal Teflon-lined reaction vessel, Dy₂O₃ (0.2 mmol, 75 mg), HIO₃ (0.8 mmol, 141 mg), 1,10-phenanthroline (0.4 mmol, 80 mg) and 13 ml H₂O were added and stirred thoroughly for 1 h, then heated at 393 K for 2 d. After cooling down to room temperature, some colorless crystalline product (I) was obtained.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009; van der Sluis & Spek, 1990); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. Structure and labeling of the title compound, with displacement ellipsoids drawn at the 30% probability level and H atoms shown as small spheres of arbitrary radii.
	Fig. 2. The packing diagram viewed along the a-direction, Dy: green diagonal; I: purple inner dot; O: red; and H: small blue circles. And hydrogen bonds are denoted as dash lines.

dysprosium(III) triiodate(V) dihydrate top

Crystal data top

Dy(IO₃)₃H₂O·H₂O	Z = 2
M_r = 723.23	F(000) = 634
Triclinic, P1	D_x = 4.766 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71075 Å
a = 7.1599 (1) Å	Cell parameters from 1561 reflections
b = 7.4292 (1) Å	θ = 2.0–27.5°
c = 10.6443 (1) Å	µ = 16.65 mm⁻¹
α = 95.161 (12)°	T = 293 K
β = 104.858 (7)°	Block, colourless
γ = 110.081 (8)°	0.16 × 0.12 × 0.06 mm
V = 504.00 (5) Å³

Data collection top

Rigaku R-AXIS RAPID diffractometer	2260 independent reflections
Radiation source: fine-focus sealed tube	2067 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
Detector resolution: 14.6306 pixels mm^-1	θ_max = 27.5°, θ_min = 3.2°
CCD profile fitting scans	h = −9→9
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −7→9
T_min = 0.136, T_max = 0.435	l = −13→13
3819 measured reflections

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)] = 0.038	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.109	w = 1/[σ²(F_o²) + (0.0647P)² + 5.3292P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max < 0.001
2260 reflections	Δρ_max = 2.79 e Å⁻³
141 parameters	Δρ_min = −3.20 e Å⁻³
2 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: 0.0126 (8)

Crystal data top

Dy(IO₃)₃H₂O·H₂O	γ = 110.081 (8)°
M_r = 723.23	V = 504.00 (5) Å³
Triclinic, P1	Z = 2
a = 7.1599 (1) Å	Mo Kα radiation
b = 7.4292 (1) Å	µ = 16.65 mm⁻¹
c = 10.6443 (1) Å	T = 293 K
α = 95.161 (12)°	0.16 × 0.12 × 0.06 mm
β = 104.858 (7)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	2260 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	2067 reflections with I > 2σ(I)
T_min = 0.136, T_max = 0.435	R_int = 0.027
3819 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.038	2 restraints
wR(F²) = 0.109	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	Δρ_max = 2.79 e Å⁻³
2260 reflections	Δρ_min = −3.20 e Å⁻³
141 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
Dy1	0.11491 (7)	−0.58338 (7)	−0.21096 (4)	0.01105 (18)
I1	0.30890 (8)	−0.14149 (8)	0.07303 (5)	0.00659 (18)
I2	0.28110 (8)	−0.63445 (8)	0.16834 (5)	0.00652 (18)
I3	0.27848 (9)	−0.26870 (9)	−0.45631 (6)	0.00862 (19)
O1	0.1496 (11)	−0.2711 (12)	−0.0929 (7)	0.0178 (15)
O2	0.0966 (11)	−0.1450 (11)	0.1365 (7)	0.0144 (14)
O3	0.3778 (11)	0.1033 (10)	0.0380 (7)	0.0134 (14)
O4	0.2940 (11)	−0.5350 (11)	0.0209 (7)	0.0155 (15)
O5	0.2291 (10)	−0.4405 (11)	0.2502 (7)	0.0131 (14)
O6	0.5556 (10)	−0.5510 (11)	0.2555 (7)	0.0121 (14)
O7	0.0908 (11)	−0.3710 (11)	−0.3699 (7)	0.0130 (14)
O8	0.1065 (11)	−0.1986 (11)	−0.5813 (7)	0.0125 (14)
O9	0.4335 (11)	−0.0352 (12)	−0.3515 (8)	0.0187 (16)
O10	0.2235 (12)	−0.8611 (12)	−0.2319 (8)	0.0185 (16)
H10A	0.198 (15)	−0.928 (9)	−0.179 (7)	0.028*
H10B	0.346 (4)	−0.8277 (13)	−0.221 (10)	0.028*
O11	0.2419 (13)	−0.7837 (13)	0.3943 (9)	0.0257 (18)
H11A	0.225 (3)	−0.897 (15)	0.3811 (19)	0.039*
H11B	0.144 (13)	−0.7725 (18)	0.412 (2)	0.039*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.0094 (3)	0.0136 (3)	0.0131 (3)	0.00658 (19)	0.00455 (18)	0.00444 (19)
I1	0.0048 (3)	0.0061 (3)	0.0105 (3)	0.0031 (2)	0.0028 (2)	0.0041 (2)
I2	0.0040 (3)	0.0067 (3)	0.0111 (3)	0.0040 (2)	0.0027 (2)	0.0039 (2)
I3	0.0076 (3)	0.0109 (3)	0.0101 (3)	0.0063 (2)	0.0032 (2)	0.0026 (2)
O1	0.014 (3)	0.023 (4)	0.012 (3)	0.010 (3)	−0.004 (3)	−0.002 (3)
O2	0.011 (3)	0.014 (4)	0.022 (4)	0.006 (3)	0.009 (3)	0.007 (3)
O3	0.020 (3)	0.006 (3)	0.020 (4)	0.007 (3)	0.011 (3)	0.006 (3)
O4	0.019 (4)	0.013 (4)	0.014 (3)	0.006 (3)	0.005 (3)	0.006 (3)
O5	0.006 (3)	0.014 (4)	0.021 (4)	0.005 (3)	0.007 (3)	0.002 (3)
O6	0.001 (3)	0.016 (4)	0.018 (3)	0.002 (3)	0.003 (3)	0.007 (3)
O7	0.014 (3)	0.020 (4)	0.013 (3)	0.012 (3)	0.007 (3)	0.013 (3)
O8	0.014 (3)	0.013 (4)	0.013 (3)	0.005 (3)	0.007 (3)	0.006 (3)
O9	0.011 (3)	0.018 (4)	0.022 (4)	0.005 (3)	0.000 (3)	−0.002 (3)
O10	0.022 (4)	0.023 (4)	0.025 (4)	0.019 (3)	0.013 (3)	0.011 (3)
O11	0.022 (4)	0.022 (4)	0.034 (5)	0.007 (4)	0.012 (4)	0.005 (4)

Geometric parameters (Å, º) top

Dy1—O4	2.401 (7)	I2—O6	1.798 (6)
Dy1—O2ⁱ	2.408 (7)	I2—O4	1.804 (7)
Dy1—O8ⁱⁱ	2.412 (7)	I2—O5	1.812 (7)
Dy1—O6ⁱⁱⁱ	2.415 (6)	I3—O9	1.783 (8)
Dy1—O7	2.429 (6)	I3—O8	1.812 (7)
Dy1—O1	2.438 (8)	I3—O7	1.813 (7)
Dy1—O10	2.453 (7)	O2—Dy1ⁱ	2.408 (7)
Dy1—O5ⁱ	2.461 (6)	O5—Dy1ⁱ	2.461 (6)
I1—O1	1.804 (7)	O6—Dy1ⁱⁱⁱ	2.415 (6)
I1—O2	1.809 (7)	O8—Dy1ⁱⁱ	2.412 (7)
I1—O3	1.814 (7)

O4—Dy1—O2ⁱ	75.1 (2)	O7—Dy1—O10	126.1 (2)
O4—Dy1—O8ⁱⁱ	149.7 (2)	O1—Dy1—O10	151.9 (2)
O2ⁱ—Dy1—O8ⁱⁱ	78.5 (2)	O4—Dy1—O5ⁱ	112.2 (2)
O4—Dy1—O6ⁱⁱⁱ	90.6 (2)	O2ⁱ—Dy1—O5ⁱ	73.6 (2)
O2ⁱ—Dy1—O6ⁱⁱⁱ	142.8 (2)	O8ⁱⁱ—Dy1—O5ⁱ	73.6 (2)
O8ⁱⁱ—Dy1—O6ⁱⁱⁱ	101.7 (2)	O6ⁱⁱⁱ—Dy1—O5ⁱ	142.8 (2)
O4—Dy1—O7	135.1 (3)	O7—Dy1—O5ⁱ	72.9 (2)
O2ⁱ—Dy1—O7	141.9 (2)	O1—Dy1—O5ⁱ	69.4 (2)
O8ⁱⁱ—Dy1—O7	75.1 (2)	O10—Dy1—O5ⁱ	132.9 (3)
O6ⁱⁱⁱ—Dy1—O7	70.3 (2)	O1—I1—O2	96.8 (3)
O4—Dy1—O1	69.2 (2)	O1—I1—O3	97.2 (3)
O2ⁱ—Dy1—O1	111.8 (3)	O2—I1—O3	97.7 (3)
O8ⁱⁱ—Dy1—O1	136.0 (2)	O6—I2—O4	99.6 (3)
O6ⁱⁱⁱ—Dy1—O1	93.9 (3)	O6—I2—O5	97.8 (3)
O7—Dy1—O1	72.0 (2)	O4—I2—O5	95.5 (3)
O4—Dy1—O10	84.5 (3)	O9—I3—O8	99.4 (3)
O2ⁱ—Dy1—O10	68.8 (3)	O9—I3—O7	101.4 (3)
O8ⁱⁱ—Dy1—O10	72.1 (2)	O8—I3—O7	96.1 (3)
O6ⁱⁱⁱ—Dy1—O10	75.9 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O10—H10A···O3^iv	0.80	2.29	2.873 (10)	131
O10—H10B···O9^iv	0.80	2.33	2.753 (11)	114
O11—H11A···O8^v	0.80	2.22	2.954 (11)	153
O11—H11B···O7ⁱ	0.80	2.26	2.946 (11)	145

Symmetry codes: (i) −x, −y−1, −z; (iv) x, y−1, z; (v) x, y−1, z+1.

Experimental details

Crystal data
Chemical formula	Dy(IO₃)₃H₂O·H₂O
M_r	723.23
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	7.1599 (1), 7.4292 (1), 10.6443 (1)
α, β, γ (°)	95.161 (12), 104.858 (7), 110.081 (8)
V (Å³)	504.00 (5)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	16.65
Crystal size (mm)	0.16 × 0.12 × 0.06

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.136, 0.435
No. of measured, independent and observed [I > 2σ(I)] reflections	3819, 2260, 2067
R_int	0.027
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.038, 0.109, 1.06
No. of reflections	2260
No. of parameters	141
No. of restraints	2
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	2.79, −3.20

Computer programs: PROCESS-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009; van der Sluis & Spek, 1990), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O10—H10A···O3ⁱ	0.80	2.29	2.873 (10)	131.2
O10—H10B···O9ⁱ	0.80	2.33	2.753 (11)	114.0
O11—H11A···O8ⁱⁱ	0.80	2.22	2.954 (11)	152.6
O11—H11B···O7ⁱⁱⁱ	0.80	2.26	2.946 (11)	145.0

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

Acknowledgements

The authors are grateful for financial support from the National Natural Science Foundation of China (project Nos. 50702054 and 20803070) and the Analysis and Testing Foundation of Zhejiang Province (project Nos. 2008F70034 and 2008F70053).

References

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