Poly[[[μ3-N′-(carboxymethyl)ethylene­di­amine-N,N,N′-triacetato]dysprosium(III)] trihydrate]

Zhuang, X.; Long, Q.; Wang, J.

doi:10.1107/S1600536810041784

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 11| November 2010| Page m1436

https://doi.org/10.1107/S1600536810041784

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Poly[[[μ₃-N′-(carboxymethyl)ethylenediamine-N,N,N′-triacetato]dysprosium(III)] trihydrate]

Xiaomei Zhuang,^a Qingping Long ^a and Jun Wang ^a ^*

^aZhongshan Polytechnic, Zhongshan, Guangdong 528404, People's Republic of China
^*Correspondence e-mail: wangjun7203@126.com

(Received 9 October 2010; accepted 15 October 2010; online 23 October 2010)

In the title coordination polymer, {[Dy(C₁₀H₁₃N₂O₈)]·3H₂O}_n, the dysprosium(III) ion is coordinated by two N atoms and six O atoms from three different (carboxymethyl)ethylenediaminetriacetate ligands in a distorted square-antiprismatic geometry. The ligands connect the metal atoms, forming layers parallel to the ab plane. O—H⋯O hydrogen bonds further assemble adjacent layers into a three-dimensional supramolecular network.

Related literature

For general background to the topologies and potential applications of metal coordination polymers, see: Benelli & Gatteschi (2002 ). For related structures, see: Wang et al. (2007 ); You & Ng (2007 ); Sakagami et al. (1999 ); Templeton et al. (1985 ); Vikram & Sivasankar (2008 ).

Experimental

Crystal data

[Dy(C₁₀H₁₃N₂O₈)]·3H₂O
M_r = 505.77
Orthorhombic, P b c a
a = 13.3835 (5) Å
b = 13.0127 (4) Å
c = 18.6943 (7) Å
V = 3255.7 (2) Å³
Z = 8
Mo Kα radiation
μ = 4.65 mm⁻¹
T = 296 K
0.25 × 0.19 × 0.18 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004 ) T_min = 0.389, T_max = 0.488
19825 measured reflections
3192 independent reflections
2230 reflections with I > 2σ(I)
R_int = 0.034

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.061
S = 1.07
3192 reflections
217 parameters
H-atom parameters constrained
Δρ_max = 0.74 e Å⁻³
Δρ_min = −0.69 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯O3ⁱ	0.82	1.69	2.504 (5)	172
O1W—H2W⋯O6ⁱⁱ	0.85	2.17	2.920 (5)	148
O1W—H1W⋯O3ⁱⁱⁱ	0.84	2.10	2.925 (5)	165
O2W—H3W⋯O3W^iv	0.83	2.04	2.813 (6)	154
O2W—H4W⋯O1W^v	0.84	2.09	2.844 (6)	150
O3W—H6W⋯O2^vi	0.85	2.56	3.141 (5)	127
Symmetry codes: (i) $[-x+{\script{1\over 2}}, -y+1, z-{\script{1\over 2}}]$ ; (ii) x+1, y, z; (iii) -x+1, -y+1, -z+1; (iv) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z]$ ; (v) $[-x+2, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (vi) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ .

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: https://doi.org/10.1107/S1600536810041784/rz2501sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810041784/rz2501Isup2.hkl

checkCIF report

Comment top

The design and construction of metal coordination polymers based on metal ions and multifunctional bridging ligands is of great research interest due to their intriguing topologies and potential applications as functional materials (Benelli & Gatteschi, 2002). The flexible ethylenediaminetetraacetato ligand possessing variable coordination modes to bind to metal ions, provides unique opportunities for the construction of unusual networks. Recently, some mono- and polynuclear Dy complexes of this ligand have been reported (Wang et al., 2007; You & Ng, 2007; Sakagami et al., 1999; Templeton et al., 1985; Vikram & Sivasankar, 2008). Herein, we report the structure of the new polynuclear dysprosium complex, {[Dy(C₁₀H₉N₂O₈)].3H₂O}_n.

In the structure of the title compound, the dysprosium(III) metal displays a distorted square antiprism geometry provided by two N atoms from one (carboxymethyl)ethylenediaminetriacetato ligand (HEDTA) and six O atoms from three different HEDTA ligands (Fig. 1). The ligands connect the dysprosium centres to form layers parallel to the ab plane. O—H···O hydrogen bonds involving the interstitial water molecules assemble adjacent layers to construct a three-dimensional supramolecular network (Table 1; Fig. 2).

Related literature top

For general background to the topologies and potential applications of metal coordination polymers, see: Benelli & Gatteschi (2002). For related structures, see: Wang et al. (2007); You & Ng (2007); Sakagami et al. (1999); Templeton et al. (1985); Vikram & Sivasankar (2008).

Experimental top

A mixture of Dy₂O₃ (0.189 g, 0.5 mmol), ethylenediaminetetraacetic acid (0.146 g, 0.5 mmol), and H₂O (10 mL) was sealed in a 20 mL Teflon-lined reactor, which was heated in an oven to 423 K for 36 h and then cooled to room temperature at a rate of 5 K h^-1. Colourless crystals were obtained in a yield of 46% based on Dy.

Structure description top

For general background to the topologies and potential applications of metal coordination polymers, see: Benelli & Gatteschi (2002). For related structures, see: Wang et al. (2007); You & Ng (2007); Sakagami et al. (1999); Templeton et al. (1985); Vikram & Sivasankar (2008).

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 asymmetric unit of the title compound, with displacement ellipsoids drawn at the 50% probability level. Symmetry codes: (ii) 1/2-x, -1/2+y, z; (iii) 1/2+x, y, 1/2-z.
	Fig. 2. Crystal packing of the title compound viewed along the b axis. Intermolecular hydrogen bonds are shown as dashed lines.

Poly[[[µ₃-N'-(carboxymethyl)ethylenediamine- N,N,N'-triacetato]dysprosium(III)] trihydrate] top

Crystal data top

[Dy(C₁₀H₁₃N₂O₈)]·3H₂O	F(000) = 1976
M_r = 505.77	D_x = 2.064 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 4800 reflections
a = 13.3835 (5) Å	θ = 1.4–28.0°
b = 13.0127 (4) Å	µ = 4.65 mm⁻¹
c = 18.6943 (7) Å	T = 296 K
V = 3255.7 (2) Å³	Block, colourless
Z = 8	0.25 × 0.19 × 0.18 mm

Data collection top

Bruker APEXII area-detector diffractometer	3192 independent reflections
Radiation source: fine-focus sealed tube	2230 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.034
φ and ω scan	θ_max = 26.0°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)	h = −13→16
T_min = 0.389, T_max = 0.488	k = −16→16
19825 measured reflections	l = −22→20

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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.061	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0239P)² + 3.1993P] where P = (F_o² + 2F_c²)/3
3192 reflections	(Δ/σ)_max = 0.001
217 parameters	Δρ_max = 0.74 e Å⁻³
0 restraints	Δρ_min = −0.69 e Å⁻³

Crystal data top

[Dy(C₁₀H₁₃N₂O₈)]·3H₂O	V = 3255.7 (2) Å³
M_r = 505.77	Z = 8
Orthorhombic, Pbca	Mo Kα radiation
a = 13.3835 (5) Å	µ = 4.65 mm⁻¹
b = 13.0127 (4) Å	T = 296 K
c = 18.6943 (7) Å	0.25 × 0.19 × 0.18 mm

Data collection top

Bruker APEXII area-detector diffractometer	3192 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)	2230 reflections with I > 2σ(I)
T_min = 0.389, T_max = 0.488	R_int = 0.034
19825 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	0 restraints
wR(F²) = 0.061	H-atom parameters constrained
S = 1.07	Δρ_max = 0.74 e Å⁻³
3192 reflections	Δρ_min = −0.69 e Å⁻³
217 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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	0.195820 (13)	0.546220 (11)	0.248589 (10)	0.01538 (8)
N1	0.1266 (2)	0.6990 (2)	0.32682 (16)	0.0170 (7)
N2	0.0619 (2)	0.6517 (2)	0.17784 (16)	0.0167 (7)
C4	0.1889 (3)	0.5806 (3)	0.4196 (2)	0.0220 (10)
C3	0.1109 (3)	0.6609 (3)	0.4002 (2)	0.0219 (9)
H3A	0.0448	0.6310	0.4040	0.026*
H3B	0.1149	0.7178	0.4335	0.026*
C2	0.1622 (3)	0.5832 (3)	0.0792 (2)	0.0245 (10)
C1	0.0980 (3)	0.6704 (3)	0.1040 (2)	0.0231 (10)
H1A	0.1362	0.7337	0.1027	0.028*
H1B	0.0414	0.6779	0.0721	0.028*
C6	0.0396 (3)	0.7507 (3)	0.2145 (2)	0.0187 (9)
H6A	−0.0229	0.7778	0.1964	0.022*
H6B	0.0918	0.7998	0.2033	0.022*
C5	0.0323 (3)	0.7387 (3)	0.2951 (2)	0.0195 (9)
H5A	0.0166	0.8048	0.3163	0.023*
H5B	−0.0217	0.6918	0.3064	0.023*
O2	0.1990 (2)	0.5221 (2)	0.12204 (15)	0.0305 (8)
O4	0.2355 (2)	0.5364 (2)	0.36996 (14)	0.0258 (7)
O3	0.2014 (2)	0.5610 (2)	0.48468 (15)	0.0375 (8)
O1	0.1763 (3)	0.5794 (3)	0.01143 (16)	0.0444 (9)
H1	0.2118	0.5300	0.0018	0.067*
C8	0.2652 (3)	0.7845 (3)	0.2596 (2)	0.0187 (9)
C7	0.2041 (3)	0.7799 (3)	0.3277 (2)	0.0204 (9)
H7A	0.2487	0.7677	0.3677	0.024*
H7B	0.1722	0.8459	0.3352	0.024*
O5	0.2750 (2)	0.70278 (19)	0.22414 (15)	0.0228 (6)
C10	−0.0465 (3)	0.5264 (3)	0.2434 (2)	0.0180 (9)
C9	−0.0296 (3)	0.5873 (3)	0.1748 (2)	0.0219 (9)
H9A	−0.0243	0.5399	0.1349	0.026*
H9B	−0.0870	0.6312	0.1663	0.026*
O6	0.03078 (19)	0.4997 (2)	0.27769 (15)	0.0218 (6)
O7	0.30708 (18)	0.86679 (19)	0.24311 (14)	0.0243 (7)
O8	−0.13277 (19)	0.50137 (19)	0.26058 (14)	0.0216 (6)
O1W	0.9746 (4)	0.4386 (3)	0.4225 (2)	0.0840 (14)
H2W	0.9668	0.4475	0.3780	0.126*
H1W	0.9200	0.4478	0.4441	0.126*
O2W	0.8853 (3)	0.7777 (3)	0.0541 (2)	0.0798 (13)
H3W	0.8606	0.7769	0.0133	0.096*
H4W	0.9063	0.8364	0.0649	0.096*
O3W	0.3282 (4)	0.7889 (3)	0.0831 (2)	0.0966 (16)
H6W	0.2814	0.8319	0.0909	0.145*
H5W	0.3833	0.8247	0.0785	0.145*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.01199 (11)	0.01112 (10)	0.02303 (12)	0.00043 (6)	0.00005 (9)	−0.00001 (9)
N1	0.0157 (17)	0.0155 (15)	0.0197 (18)	0.0009 (14)	−0.0011 (14)	0.0026 (14)
N2	0.0193 (18)	0.0153 (16)	0.0156 (17)	0.0010 (14)	0.0044 (14)	0.0002 (14)
C4	0.023 (2)	0.020 (2)	0.022 (2)	0.0000 (18)	−0.0041 (19)	0.0008 (18)
C3	0.025 (2)	0.025 (2)	0.016 (2)	−0.0007 (19)	0.0048 (18)	−0.0006 (18)
C2	0.024 (2)	0.029 (2)	0.020 (2)	0.002 (2)	0.005 (2)	−0.0044 (19)
C1	0.024 (2)	0.023 (2)	0.022 (2)	0.0052 (19)	0.0024 (18)	0.0024 (18)
C6	0.015 (2)	0.0148 (19)	0.027 (2)	0.0073 (17)	−0.0028 (18)	0.0023 (17)
C5	0.017 (2)	0.0167 (19)	0.025 (2)	0.0043 (17)	0.0026 (18)	−0.0020 (17)
O2	0.042 (2)	0.0291 (16)	0.0204 (16)	0.0182 (14)	0.0014 (14)	−0.0032 (13)
O4	0.0253 (17)	0.0287 (16)	0.0233 (16)	0.0092 (14)	−0.0022 (14)	0.0028 (13)
O3	0.046 (2)	0.048 (2)	0.0180 (16)	0.0207 (16)	−0.0026 (14)	0.0043 (15)
O1	0.059 (2)	0.048 (2)	0.0260 (18)	0.0262 (18)	0.0108 (16)	0.0033 (16)
C8	0.0086 (18)	0.0125 (18)	0.035 (3)	0.0022 (15)	−0.0059 (18)	0.0031 (18)
C7	0.023 (2)	0.0147 (19)	0.023 (2)	−0.0004 (17)	−0.0021 (18)	−0.0029 (17)
O5	0.0212 (15)	0.0139 (14)	0.0332 (16)	−0.0004 (12)	0.0088 (13)	−0.0013 (12)
C10	0.017 (2)	0.0103 (16)	0.026 (2)	0.0009 (15)	−0.0007 (19)	−0.0050 (17)
C9	0.017 (2)	0.025 (2)	0.023 (2)	−0.0019 (18)	−0.0044 (18)	0.0021 (18)
O6	0.0114 (14)	0.0188 (13)	0.0352 (16)	0.0000 (12)	−0.0021 (13)	0.0088 (13)
O7	0.0177 (15)	0.0116 (12)	0.0437 (18)	−0.0019 (11)	0.0034 (14)	0.0005 (14)
O8	0.0077 (14)	0.0187 (12)	0.0383 (18)	−0.0011 (11)	0.0011 (12)	0.0039 (13)
O1W	0.109 (4)	0.097 (3)	0.046 (3)	−0.014 (3)	0.024 (3)	0.002 (2)
O2W	0.062 (3)	0.113 (4)	0.064 (3)	0.018 (3)	−0.004 (2)	0.017 (3)
O3W	0.127 (5)	0.084 (3)	0.079 (3)	0.007 (3)	0.011 (3)	−0.003 (3)

Geometric parameters (Å, º) top

Dy1—O4	2.334 (3)	C6—C5	1.518 (6)
Dy1—O7ⁱ	2.337 (3)	C6—H6A	0.9700
Dy1—O5	2.342 (3)	C6—H6B	0.9700
Dy1—O6	2.354 (3)	C5—H5A	0.9700
Dy1—O8ⁱⁱ	2.373 (3)	C5—H5B	0.9700
Dy1—O2	2.387 (3)	O1—H1	0.8200
Dy1—N2	2.617 (3)	C8—O7	1.248 (4)
Dy1—N1	2.636 (3)	C8—O5	1.260 (4)
N1—C3	1.473 (4)	C8—C7	1.513 (5)
N1—C7	1.477 (5)	C7—H7A	0.9700
N1—C5	1.487 (5)	C7—H7B	0.9700
N2—C1	1.482 (5)	C10—O8	1.243 (4)
N2—C9	1.485 (5)	C10—O6	1.265 (4)
N2—C6	1.488 (5)	C10—C9	1.524 (5)
C4—O4	1.257 (5)	C9—H9A	0.9700
C4—O3	1.254 (5)	C9—H9B	0.9700
C4—C3	1.521 (5)	O7—Dy1ⁱⁱⁱ	2.337 (3)
C3—H3A	0.9700	O8—Dy1^iv	2.373 (2)
C3—H3B	0.9700	O1W—H2W	0.8462
C2—O2	1.231 (5)	O1W—H1W	0.8429
C2—O1	1.282 (5)	O2W—H3W	0.8322
C2—C1	1.496 (5)	O2W—H4W	0.8371
C1—H1A	0.9700	O3W—H6W	0.8515
C1—H1B	0.9700	O3W—H5W	0.8763

O4—Dy1—O7ⁱ	89.53 (9)	O2—C2—O1	124.0 (4)
O4—Dy1—O5	97.72 (10)	O2—C2—C1	121.2 (4)
O7ⁱ—Dy1—O5	150.23 (9)	O1—C2—C1	114.8 (4)
O4—Dy1—O6	88.56 (10)	N2—C1—C2	110.6 (3)
O7ⁱ—Dy1—O6	74.80 (9)	N2—C1—H1A	109.5
O5—Dy1—O6	133.90 (9)	C2—C1—H1A	109.5
O4—Dy1—O8ⁱⁱ	80.61 (10)	N2—C1—H1B	109.5
O7ⁱ—Dy1—O8ⁱⁱ	76.54 (8)	C2—C1—H1B	109.5
O5—Dy1—O8ⁱⁱ	76.25 (9)	H1A—C1—H1B	108.1
O6—Dy1—O8ⁱⁱ	149.38 (9)	N2—C6—C5	112.4 (3)
O4—Dy1—O2	162.25 (10)	N2—C6—H6A	109.1
O7ⁱ—Dy1—O2	79.94 (10)	C5—C6—H6A	109.1
O5—Dy1—O2	85.01 (10)	N2—C6—H6B	109.1
O6—Dy1—O2	102.22 (10)	C5—C6—H6B	109.1
O8ⁱⁱ—Dy1—O2	83.05 (9)	H6A—C6—H6B	107.9
O4—Dy1—N2	132.53 (9)	N1—C5—C6	112.1 (3)
O7ⁱ—Dy1—N2	119.38 (9)	N1—C5—H5A	109.2
O5—Dy1—N2	75.81 (10)	C6—C5—H5A	109.2
O6—Dy1—N2	66.98 (9)	N1—C5—H5B	109.2
O8ⁱⁱ—Dy1—N2	138.99 (9)	C6—C5—H5B	109.2
O2—Dy1—N2	65.17 (9)	H5A—C5—H5B	107.9
O4—Dy1—N1	65.28 (9)	C2—O2—Dy1	123.5 (3)
O7ⁱ—Dy1—N1	140.53 (9)	C4—O4—Dy1	125.5 (3)
O5—Dy1—N1	67.10 (9)	C2—O1—H1	109.5
O6—Dy1—N1	74.70 (10)	O7—C8—O5	123.1 (4)
O8ⁱⁱ—Dy1—N1	124.40 (9)	O7—C8—C7	119.0 (3)
O2—Dy1—N1	130.94 (9)	O5—C8—C7	117.8 (3)
N2—Dy1—N1	69.15 (9)	N1—C7—C8	113.4 (3)
C3—N1—C7	109.2 (3)	N1—C7—H7A	108.9
C3—N1—C5	111.5 (3)	C8—C7—H7A	108.9
C7—N1—C5	110.7 (3)	N1—C7—H7B	108.9
C3—N1—Dy1	108.2 (2)	C8—C7—H7B	108.9
C7—N1—Dy1	107.3 (2)	H7A—C7—H7B	107.7
C5—N1—Dy1	109.8 (2)	C8—O5—Dy1	125.7 (2)
C1—N2—C9	109.0 (3)	O8—C10—O6	123.8 (4)
C1—N2—C6	110.6 (3)	O8—C10—C9	119.4 (3)
C9—N2—C6	109.9 (3)	O6—C10—C9	116.7 (3)
C1—N2—Dy1	109.4 (2)	N2—C9—C10	112.5 (3)
C9—N2—Dy1	106.7 (2)	N2—C9—H9A	109.1
C6—N2—Dy1	111.0 (2)	C10—C9—H9A	109.1
O4—C4—O3	123.9 (4)	N2—C9—H9B	109.1
O4—C4—C3	118.5 (4)	C10—C9—H9B	109.1
O3—C4—C3	117.6 (4)	H9A—C9—H9B	107.8
N1—C3—C4	110.9 (3)	C10—O6—Dy1	125.4 (2)
N1—C3—H3A	109.5	C8—O7—Dy1ⁱⁱⁱ	147.0 (2)
C4—C3—H3A	109.5	C10—O8—Dy1^iv	144.6 (2)
N1—C3—H3B	109.5	H2W—O1W—H1W	110.2
C4—C3—H3B	109.5	H3W—O2W—H4W	111.4
H3A—C3—H3B	108.1	H6W—O3W—H5W	106.7

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O3^v	0.82	1.69	2.504 (5)	172
O1W—H2W···O6^vi	0.85	2.17	2.920 (5)	148
O1W—H1W···O3^vii	0.84	2.10	2.925 (5)	165
O2W—H3W···O3W^viii	0.83	2.04	2.813 (6)	154
O2W—H4W···O1W^ix	0.84	2.09	2.844 (6)	150
O3W—H6W···O2ⁱⁱⁱ	0.85	2.56	3.141 (5)	127

Symmetry codes: (iii) −x+1/2, y+1/2, z; (v) −x+1/2, −y+1, z−1/2; (vi) x+1, y, z; (vii) −x+1, −y+1, −z+1; (viii) x+1/2, −y+3/2, −z; (ix) −x+2, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	[Dy(C₁₀H₁₃N₂O₈)]·3H₂O
M_r	505.77
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	296
a, b, c (Å)	13.3835 (5), 13.0127 (4), 18.6943 (7)
V (Å³)	3255.7 (2)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	4.65
Crystal size (mm)	0.25 × 0.19 × 0.18

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2008)
T_min, T_max	0.389, 0.488
No. of measured, independent and observed [I > 2σ(I)] reflections	19825, 3192, 2230
R_int	0.034
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.061, 1.07
No. of reflections	3192
No. of parameters	217
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.74, −0.69

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
O1—H1···O3ⁱ	0.82	1.69	2.504 (5)	172.0
O1W—H2W···O6ⁱⁱ	0.85	2.17	2.920 (5)	147.5
O1W—H1W···O3ⁱⁱⁱ	0.84	2.10	2.925 (5)	164.7
O2W—H3W···O3W^iv	0.83	2.04	2.813 (6)	154.1
O2W—H4W···O1W^v	0.84	2.09	2.844 (6)	149.6
O3W—H6W···O2^vi	0.85	2.56	3.141 (5)	126.8

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

Acknowledgements

The authors acknowledge Zhongshan Polytechnic for supporting this work.

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