Poly[[diaqua­tris[μ4-(p-phenyl­enedi­oxy)diacetato]didysprosium(III)] dihydrate]

Li, Y.-F.; Wang, D.-W.; Wang, Y.-R.; Zhang, L.

doi:10.1107/S1600536808017649

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 64| Part 7| July 2008| Page m944

doi:10.1107/S1600536808017649

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Poly[[diaquatris[μ₄-(p-phenylenedioxy)diacetato]didysprosium(III)] dihydrate]

Ya-Feng Li,^a ^* Dao-Wu Wang,^a Yuan-Rui Wang ^a and Long Zhang ^a

^aSchool of Chemical Engineering, Changchun University of Technology, Changchun 130012, People's Republic of China
^*Correspondence e-mail: fly012345@sohu.com

(Received 23 May 2008; accepted 11 June 2008; online 19 June 2008)

The title dysprosium coordination polymer, {[Dy₂(C₁₀H₈O₆)₃(H₂O)₂]·2H₂O}_n, was synthesized by reacting dysprosium(III) nitrate and the flexible ligand (p-phenylenedioxy)diacetic acid under hydrothermal conditions. Each Dy^III ion is coordinated by nine O atoms in a tricapped trigonal prismatic geometry. The DyO₉ polyhedra form layers parallel to the bc plane. The rigid benzene rings of the anions link the layers along the a axis, forming a three-dimensional framework.

Related literature

For related literature, see: Eddaoudi et al. (2001 ); Li & Han (2006 ); Michl (1995 ); Yaghi et al. (1998 ).

Experimental

Crystal data

[Dy₂(C₁₀H₈O₆)₃(H₂O)₂]·2H₂O
M_r = 1069.56
Monoclinic, P 2₁ /c
a = 12.080 (2) Å
b = 16.615 (3) Å
c = 8.8802 (18) Å
β = 109.32 (3)°
V = 1682.0 (6) Å³
Z = 2
Mo Kα radiation
μ = 4.50 mm⁻¹
T = 293 (2) K
0.19 × 0.16 × 0.13 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.437, T_max = 0.548
16183 measured reflections
3838 independent reflections
3229 reflections with I > 2σ(I)
R_int = 0.043

Refinement

R[F² > 2σ(F²)] = 0.028
wR(F²) = 0.059
S = 1.05
3838 reflections
256 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.83 e Å⁻³
Δρ_min = −0.93 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H16A⋯O6ⁱ	0.80 (3)	2.11 (5)	2.706 (4)	131 (6)
O1W—H16B⋯O2W	0.79 (3)	1.98 (4)	2.755 (6)	166 (7)
O2W—H17A⋯O3	0.82 (3)	2.41 (6)	2.952 (5)	125 (5)
Symmetry code: (i) $[x+1, -y+{\script{1\over 2}}, z+{\script{3\over 2}}]$ .

Data collection: PROCESS-AUTO (Rigaku, 1998 ); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2000 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808017649/ci2601sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808017649/ci2601Isup2.hkl

checkCIF report

Comment top

Extensive efforts have been made to construct metal-organic frameworks (MOFs) owing to the benefits they offer such as functional mesoscopic phases, modified surfaces and designed crystals (Michl, 1995). The carboxylate group can offer more solid frameworks by forming M—O—C cluster. The recent works focus on metals and rigid multidentate phenylcarboxylates to form MOFs (Yaghi et al., 1998; Eddaoudi et al., 2001). The chemistry of rare earth compounds is always an attactive research direction due to their complicated geometry and many important applications. We have constructed a MOF by using a rare earth and a flexible multidentate carboxylate ligand with rigid phenyl core, and its crystal structure is reported here.

The asymmetric unit of the title compound contains one Dy atom, one and half (p-phenylenedioxy)diacetate (BDOA) anions and two water molecules. One of the anions is loacted in a general position (say BDOA-N) and the other (say BDOA-C) lies on an inversion center. Each Dy^III cation is coordinated by two BDOA-C anions and four BDOA-N anions (Fig.1). The BDOA-C anion provides O atom from the carboxylate group, while the O atoms provided by the BDOA-N anions are from both carboxylate and phenol groups. Each Dy^III ion is coordinated by nine O atoms; seven out of the nine O atoms are from carboxylate groups of six BDOA anions, one from the phenolic O atom of one BDOA anion and one from a coordinated water molecule. The coordination environment around the Dy^III ion may be described as tricapped trigonal-prismatic, with Dy—O distances in the range 2.333 (10) Å-2.829 (4) Å and O—Dy—O angles in the range 47.86 (10)°-148.5 (1)°. A pair of Dy^III atoms are bridged by the two ligands in different coordination modes (Fig. 1). The Dy···Dy distance is 4.1404 (9) Å.

The adjacent DyO₉ polyhedra form edge-shared dimer, with four BDOA anions. The edge-shared DyO₉ polyhedra are connected to form layers parallel to the bc plane. The rigid phenyl cores of BDOA anions link the layers along the a axis to form a three-dimensional framework (Fig.2). The uncoordinated water molecules are trapped inside the channel formed by the DyO₉ polyhedra and phenyl core of the BDOA anions.

O—H···O hydrogen bonds are observed in the crystal structure (Table 1). The crystal structure of the title compound is similar to that of [La₂(1,4-BDOA)₃(H₂O)]₂]^.2H₂O (Li et al., 2006).

Related literature top

For related literature, see: Eddaoudi et al. (2001); Li & Han (2006); Michl (1995); Yaghi et al. (1998).

Experimental top

1,4-BDOA (0.30 g, 1.33 mmol) and Dy(NO₃)₃^.6H₂O (0.30 g, 0.67 mmol) were successively dissolved in aquous NaOH (0.13 g, 3.3 mmol NaOH/7.5 ml distilled water). The molar ratio of Dy(NO₃)₃^.6H₂O: 1,4-BDOA: NaOH: H₂O was 1:2:5:630. The solution was continuously stirred for 1 h at room temperature. Finally, the solution was sealed into 23 ml autoclave and was heated at 438 K for 6 d and then naturally cooled to room temperature, to obtain colourless crystals of the title compound.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2000); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The dinuclear unit of the title polymeric complex, showing the atomic labelling and displacement ellipsoids at the 50% probability level. H atoms have been omitted for clarity [symmetry codes: (i) -x, -y, -z; (ii) 1 + x, y, 1 + z; (iii) 1 + x, 1/2 - y, 3/2 + z; (iv) -1 - x, -y, -1 - z.]
	Fig. 2. A polyhedral and ball-stick plot of three-dimensional network in the complex, viewed along the c axis. O atoms are shown in dark gray and C atoms in light gray. H atoms have been omitted for clarity.

Poly[[diaquatris[µ₄-(p-phenylenedioxy)diacetato]didysprosium(III)] dihydrate] top

Crystal data top

[Dy₂(C₁₀H₈O₆)₃(H₂O)₂]·2H₂O	F(000) = 1040
M_r = 1069.56	D_x = 2.112 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2000 reflections
a = 12.080 (2) Å	θ = 3.0–27.5°
b = 16.615 (3) Å	µ = 4.50 mm⁻¹
c = 8.8802 (18) Å	T = 293 K
β = 109.32 (3)°	Block, grey yellow
V = 1682.0 (6) Å³	0.19 × 0.16 × 0.13 mm
Z = 2

Data collection top

Rigaku R-AXIS RAPID diffractometer	3838 independent reflections
Radiation source: fine-focus sealed tube	3229 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.043
Detector resolution: 10.00 pixels mm^-1	θ_max = 27.5°, θ_min = 3.0°
ω scans	h = −15→15
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −21→21
T_min = 0.437, T_max = 0.548	l = −11→11
16183 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)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.059	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ²(F_o²) + (0.0147P)² + 5.1969P] where P = (F_o² + 2F_c²)/3
3838 reflections	(Δ/σ)_max = 0.009
256 parameters	Δρ_max = 0.83 e Å⁻³
6 restraints	Δρ_min = −0.93 e Å⁻³

Crystal data top

[Dy₂(C₁₀H₈O₆)₃(H₂O)₂]·2H₂O	V = 1682.0 (6) Å³
M_r = 1069.56	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 12.080 (2) Å	µ = 4.50 mm⁻¹
b = 16.615 (3) Å	T = 293 K
c = 8.8802 (18) Å	0.19 × 0.16 × 0.13 mm
β = 109.32 (3)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	3838 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	3229 reflections with I > 2σ(I)
T_min = 0.437, T_max = 0.548	R_int = 0.043
16183 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	6 restraints
wR(F²) = 0.059	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	Δρ_max = 0.83 e Å⁻³
3838 reflections	Δρ_min = −0.93 e Å⁻³
256 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	0.047406 (15)	0.117791 (10)	0.06685 (2)	0.01642 (6)
O1	−0.1292 (2)	0.11347 (17)	−0.1593 (3)	0.0272 (7)
O1W	−0.0933 (3)	0.2099 (2)	0.1170 (4)	0.0492 (11)
H16A	−0.051 (5)	0.246 (3)	0.161 (7)	0.074*
H16B	−0.145 (4)	0.228 (3)	0.046 (6)	0.074*
O2	−0.1802 (2)	−0.01721 (17)	−0.1976 (3)	0.0255 (6)
O3	−0.3483 (2)	0.15102 (17)	−0.3735 (3)	0.0252 (6)
O4	−0.7742 (2)	0.21741 (16)	−0.8419 (3)	0.0214 (6)
O5	−0.8998 (3)	0.35594 (17)	−1.1500 (3)	0.0244 (6)
O6	−0.9551 (3)	0.23500 (18)	−1.0955 (4)	0.0335 (8)
O7	0.1721 (3)	0.09109 (18)	−0.0991 (4)	0.0312 (7)
O8	0.0580 (3)	−0.0133 (2)	−0.1313 (4)	0.0362 (8)
O9	0.3019 (3)	0.0217 (2)	−0.2669 (4)	0.0417 (9)
C1	−0.1940 (3)	0.0565 (2)	−0.2298 (5)	0.0199 (8)
C2	−0.3012 (3)	0.0727 (2)	−0.3743 (5)	0.0245 (9)
H2A	−0.2803	0.0664	−0.4701	0.029*
H2B	−0.3611	0.0331	−0.3778	0.029*
C3	−0.4522 (3)	0.1666 (2)	−0.4950 (5)	0.0193 (8)
C4	−0.5023 (3)	0.1140 (2)	−0.6214 (4)	0.0211 (8)
H4	−0.4650	0.0660	−0.6286	0.025*
C5	−0.5082 (4)	0.2383 (3)	−0.4866 (5)	0.0254 (9)
H5	−0.4742	0.2739	−0.4033	0.030*
C6	−0.6087 (3)	0.1338 (2)	−0.7369 (5)	0.0216 (8)
H6	−0.6418	0.0991	−0.8222	0.026*
C7	−0.6154 (4)	0.2576 (3)	−0.6023 (5)	0.0242 (9)
H7	−0.6530	0.3058	−0.5967	0.029*
C8	−0.6648 (3)	0.2037 (2)	−0.7256 (4)	0.0176 (8)
C9	−0.7965 (3)	0.2992 (2)	−0.9002 (5)	0.0210 (8)
H9A	−0.7255	0.3229	−0.9092	0.025*
H9B	−0.8222	0.3317	−0.8272	0.025*
C10	−0.8909 (3)	0.2962 (2)	−1.0620 (4)	0.0179 (8)
C11	0.1401 (3)	0.0239 (3)	−0.1581 (5)	0.0242 (9)
C12	0.1937 (4)	−0.0131 (3)	−0.2737 (6)	0.0397 (12)
H12A	0.2054	−0.0702	−0.2510	0.048*
H12B	0.1389	−0.0075	−0.3812	0.048*
C13	0.3980 (4)	0.0092 (3)	−0.1300 (6)	0.0340 (11)
C14	0.4975 (4)	0.0529 (3)	−0.1204 (6)	0.0361 (11)
H14	0.4960	0.0887	−0.2014	0.043*
C15	0.4008 (4)	−0.0437 (3)	−0.0085 (6)	0.0357 (11)
H15	0.3342	−0.0731	−0.0135	0.043*
O2W	−0.2446 (4)	0.2835 (3)	−0.1500 (5)	0.0604 (12)
H17A	−0.229 (6)	0.258 (4)	−0.219 (7)	0.091*
H17B	−0.303 (5)	0.260 (4)	−0.133 (8)	0.091*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.01428 (9)	0.01573 (9)	0.01598 (9)	0.00025 (7)	0.00061 (6)	0.00046 (7)
O1	0.0256 (15)	0.0200 (14)	0.0229 (14)	−0.0024 (12)	−0.0097 (12)	−0.0005 (12)
O1W	0.044 (2)	0.060 (3)	0.0311 (19)	0.0266 (19)	−0.0044 (16)	−0.0118 (18)
O2	0.0257 (15)	0.0170 (14)	0.0278 (15)	0.0069 (11)	0.0010 (13)	0.0013 (12)
O3	0.0199 (14)	0.0197 (14)	0.0236 (14)	0.0063 (11)	−0.0093 (12)	−0.0046 (12)
O4	0.0150 (13)	0.0162 (14)	0.0233 (14)	−0.0012 (10)	−0.0068 (11)	0.0050 (11)
O5	0.0303 (15)	0.0203 (14)	0.0180 (13)	−0.0027 (12)	0.0018 (12)	0.0078 (12)
O6	0.0304 (17)	0.0256 (17)	0.0284 (16)	−0.0090 (13)	−0.0118 (13)	0.0125 (13)
O7	0.0436 (19)	0.0238 (16)	0.0336 (17)	−0.0028 (14)	0.0226 (15)	−0.0064 (13)
O8	0.0270 (16)	0.046 (2)	0.0300 (16)	−0.0127 (15)	0.0015 (14)	0.0092 (15)
O9	0.0338 (18)	0.063 (2)	0.0360 (18)	0.0116 (17)	0.0216 (16)	0.0022 (17)
C1	0.0173 (18)	0.022 (2)	0.0179 (18)	0.0061 (15)	0.0022 (15)	−0.0016 (16)
C2	0.021 (2)	0.018 (2)	0.026 (2)	0.0061 (16)	−0.0042 (17)	−0.0026 (17)
C3	0.0142 (17)	0.019 (2)	0.0204 (18)	0.0005 (14)	0.0000 (15)	0.0004 (15)
C4	0.0196 (18)	0.0181 (19)	0.0205 (18)	0.0024 (16)	−0.0003 (15)	−0.0044 (16)
C5	0.023 (2)	0.023 (2)	0.021 (2)	0.0029 (17)	−0.0057 (17)	−0.0077 (17)
C6	0.0202 (18)	0.017 (2)	0.0211 (19)	−0.0009 (15)	−0.0024 (16)	−0.0027 (15)
C7	0.021 (2)	0.020 (2)	0.026 (2)	0.0051 (16)	0.0002 (17)	−0.0025 (17)
C8	0.0128 (17)	0.0201 (19)	0.0166 (18)	0.0003 (14)	0.0003 (15)	0.0046 (15)
C9	0.024 (2)	0.0146 (19)	0.0195 (19)	0.0001 (15)	0.0008 (16)	0.0022 (15)
C10	0.0168 (18)	0.0158 (19)	0.0178 (18)	0.0027 (14)	0.0013 (15)	0.0026 (15)
C11	0.020 (2)	0.026 (2)	0.027 (2)	−0.0014 (16)	0.0099 (17)	0.0060 (18)
C12	0.036 (3)	0.043 (3)	0.043 (3)	0.001 (2)	0.017 (2)	−0.014 (2)
C13	0.032 (2)	0.036 (3)	0.044 (3)	0.011 (2)	0.025 (2)	−0.001 (2)
C14	0.043 (3)	0.032 (3)	0.047 (3)	0.009 (2)	0.032 (2)	0.009 (2)
C15	0.033 (2)	0.033 (3)	0.050 (3)	0.003 (2)	0.026 (2)	0.001 (2)
O2W	0.055 (3)	0.060 (3)	0.051 (3)	0.016 (2)	−0.003 (2)	−0.013 (2)

Geometric parameters (Å, º) top

Dy1—O8ⁱ	2.333 (3)	C3—O3	1.382 (4)
Dy1—O2ⁱ	2.341 (3)	C3—C5	1.385 (5)
Dy1—O1	2.399 (3)	C3—C4	1.392 (5)
Dy1—O6ⁱⁱ	2.417 (3)	C4—C6	1.392 (5)
Dy1—O5ⁱⁱⁱ	2.421 (3)	C4—H4	0.93
Dy1—O1W	2.435 (4)	C5—C7	1.399 (5)
Dy1—O7	2.471 (3)	C5—H5	0.93
Dy1—O4ⁱⁱ	2.624 (3)	C6—C8	1.366 (5)
Dy1—O8	2.830 (4)	C6—H6	0.93
O1—C1	1.255 (5)	C7—C8	1.387 (5)
O1W—H16A	0.80 (3)	C7—H7	0.93
O1W—H16B	0.79 (3)	C9—C10	1.512 (5)
O2—C1	1.256 (5)	C9—H9A	0.97
O3—C3	1.382 (4)	C9—H9B	0.97
O3—C2	1.421 (5)	C11—C12	1.514 (6)
O4—C8	1.400 (4)	C12—H12A	0.97
O4—C9	1.448 (4)	C12—H12B	0.97
O5—C10	1.246 (5)	C13—C14	1.382 (7)
O6—C10	1.253 (5)	C13—C15	1.384 (7)
O7—C11	1.240 (5)	C14—C15^iv	1.383 (7)
O8—C11	1.257 (5)	C14—H14	0.93
O9—C13	1.391 (6)	C15—C14^iv	1.383 (7)
O9—C12	1.413 (6)	C15—H15	0.93
C1—C2	1.516 (5)	O2W—H17A	0.82 (3)
C2—H2A	0.97	O2W—H17B	0.86 (3)
C2—H2B	0.97

O8ⁱ—Dy1—O2ⁱ	71.77 (11)	O3—C2—C1	113.0 (3)
O8ⁱ—Dy1—O1	77.10 (10)	O3—C2—H2A	109.0
O2ⁱ—Dy1—O1	131.87 (10)	C1—C2—H2A	109.0
O8ⁱ—Dy1—O6ⁱⁱ	147.73 (10)	O3—C2—H2B	109.0
O2ⁱ—Dy1—O6ⁱⁱ	137.92 (11)	C1—C2—H2B	109.0
O1—Dy1—O6ⁱⁱ	72.10 (10)	H2A—C2—H2B	107.8
O8ⁱ—Dy1—O5ⁱⁱⁱ	81.77 (11)	O3—C3—C5	116.9 (3)
O2ⁱ—Dy1—O5ⁱⁱⁱ	73.24 (10)	O3—C3—C5	116.9 (3)
O1—Dy1—O5ⁱⁱⁱ	136.95 (11)	O3—C3—C4	123.6 (3)
O6ⁱⁱ—Dy1—O5ⁱⁱⁱ	114.92 (10)	O3—C3—C4	123.6 (3)
O8ⁱ—Dy1—O1W	87.26 (14)	C5—C3—C4	119.5 (3)
O2ⁱ—Dy1—O1W	139.73 (12)	C3—C4—C6	119.7 (4)
O1—Dy1—O1W	71.98 (11)	C3—C4—H4	120.1
O6ⁱⁱ—Dy1—O1W	74.39 (14)	C6—C4—H4	120.1
O5ⁱⁱⁱ—Dy1—O1W	69.93 (11)	C3—C5—C7	120.5 (4)
O8ⁱ—Dy1—O7	120.17 (11)	C3—C5—H5	119.7
O2ⁱ—Dy1—O7	73.43 (11)	C7—C5—H5	119.7
O1—Dy1—O7	92.54 (11)	C8—C6—C4	120.4 (4)
O6ⁱⁱ—Dy1—O7	71.26 (11)	C8—C6—H6	119.8
O5ⁱⁱⁱ—Dy1—O7	130.44 (10)	C4—C6—H6	119.8
O1W—Dy1—O7	145.27 (13)	C8—C7—C5	119.0 (4)
O8ⁱ—Dy1—O4ⁱⁱ	148.49 (9)	C8—C7—H7	120.5
O2ⁱ—Dy1—O4ⁱⁱ	86.51 (9)	C5—C7—H7	120.5
O1—Dy1—O4ⁱⁱ	133.60 (9)	C6—C8—C7	120.8 (3)
O6ⁱⁱ—Dy1—O4ⁱⁱ	61.51 (9)	C6—C8—O4	117.0 (3)
O5ⁱⁱⁱ—Dy1—O4ⁱⁱ	70.01 (10)	C7—C8—O4	122.2 (3)
O1W—Dy1—O4ⁱⁱ	95.66 (12)	O4—C9—C10	107.5 (3)
O7—Dy1—O4ⁱⁱ	72.37 (10)	O4—C9—H9A	110.2
O8ⁱ—Dy1—O8	73.76 (13)	C10—C9—H9A	110.2
O2ⁱ—Dy1—O8	66.07 (10)	O4—C9—H9B	110.2
O1—Dy1—O8	70.55 (10)	C10—C9—H9B	110.2
O6ⁱⁱ—Dy1—O8	104.10 (10)	H9A—C9—H9B	108.5
O5ⁱⁱⁱ—Dy1—O8	137.24 (9)	O5—C10—O6	125.5 (3)
O1W—Dy1—O8	140.83 (11)	O5—C10—C9	116.8 (3)
O7—Dy1—O8	47.87 (9)	O6—C10—C9	117.8 (3)
O4ⁱⁱ—Dy1—O8	118.45 (9)	O7—C11—O8	121.3 (4)
C1—O1—Dy1	132.4 (2)	O7—C11—C12	120.6 (4)
Dy1—O1W—H16A	101 (5)	O8—C11—C12	118.0 (4)
Dy1—O1W—H16B	121 (5)	O9—C12—C11	113.7 (4)
H16A—O1W—H16B	108 (4)	O9—C12—H12A	108.8
C1—O2—Dy1ⁱ	145.7 (3)	C11—C12—H12A	108.8
C3—O3—C2	115.4 (3)	O9—C12—H12B	108.8
C8—O4—C9	115.7 (3)	C11—C12—H12B	108.8
C8—O4—Dy1^v	127.1 (2)	H12A—C12—H12B	107.7
C9—O4—Dy1^v	116.5 (2)	C14—C13—C15	119.3 (5)
C10—O5—Dy1^vi	137.2 (3)	C14—C13—O9	115.6 (4)
C10—O6—Dy1^v	128.9 (2)	C15—C13—O9	125.0 (5)
C11—O7—Dy1	104.3 (3)	C13—C14—C15^iv	120.6 (4)
C11—O8—Dy1ⁱ	160.3 (3)	C13—C14—H14	119.7
C11—O8—Dy1	86.5 (3)	C15^iv—C14—H14	119.7
Dy1ⁱ—O8—Dy1	106.24 (12)	C14^iv—C15—C13	120.0 (5)
C13—O9—C12	118.0 (4)	C14^iv—C15—H15	120.0
O1—C1—O2	127.4 (3)	C13—C15—H15	120.0
O1—C1—C2	120.3 (3)	H17A—O2W—H17B	108 (4)
O2—C1—C2	112.2 (3)

O8ⁱ—Dy1—O1—C1	−35.1 (4)	C2—O3—C3—C5	172.1 (4)
O2ⁱ—Dy1—O1—C1	15.4 (4)	O3—O3—C3—C4	0.0 (3)
O6ⁱⁱ—Dy1—O1—C1	154.7 (4)	C2—O3—C3—C4	−7.1 (6)
O5ⁱⁱⁱ—Dy1—O1—C1	−97.7 (4)	O3—C3—C4—C6	178.5 (4)
O1W—Dy1—O1—C1	−126.4 (4)	O3—C3—C4—C6	178.5 (4)
O7—Dy1—O1—C1	85.3 (4)	C5—C3—C4—C6	−0.6 (6)
O4ⁱⁱ—Dy1—O1—C1	153.2 (3)	O3—C3—C5—C7	−178.1 (4)
O8—Dy1—O1—C1	42.0 (4)	O3—C3—C5—C7	−178.1 (4)
O8ⁱ—Dy1—O7—C11	14.8 (3)	C4—C3—C5—C7	1.1 (7)
O2ⁱ—Dy1—O7—C11	71.4 (3)	C3—C4—C6—C8	−0.9 (6)
O1—Dy1—O7—C11	−61.7 (3)	C3—C5—C7—C8	0.1 (7)
O6ⁱⁱ—Dy1—O7—C11	−131.9 (3)	C4—C6—C8—C7	2.1 (6)
O5ⁱⁱⁱ—Dy1—O7—C11	121.0 (3)	C4—C6—C8—O4	−176.8 (4)
O1W—Dy1—O7—C11	−123.1 (3)	C5—C7—C8—C6	−1.6 (6)
O4ⁱⁱ—Dy1—O7—C11	163.0 (3)	C5—C7—C8—O4	177.2 (4)
O8—Dy1—O7—C11	−1.0 (2)	C9—O4—C8—C6	−139.9 (4)
O8ⁱ—Dy1—O8—C11	−164.8 (3)	Dy1^v—O4—C8—C6	49.9 (5)
O2ⁱ—Dy1—O8—C11	−87.9 (2)	C9—O4—C8—C7	41.2 (5)
O1—Dy1—O8—C11	113.5 (3)	Dy1^v—O4—C8—C7	−129.0 (3)
O6ⁱⁱ—Dy1—O8—C11	48.6 (2)	C8—O4—C9—C10	158.0 (3)
O5ⁱⁱⁱ—Dy1—O8—C11	−107.1 (3)	Dy1^v—O4—C9—C10	−30.8 (4)
O1W—Dy1—O8—C11	131.1 (3)	Dy1^vi—O5—C10—O6	−34.7 (7)
O7—Dy1—O8—C11	1.0 (2)	Dy1^vi—O5—C10—C9	146.8 (3)
O4ⁱⁱ—Dy1—O8—C11	−16.3 (3)	Dy1^v—O6—C10—O5	−177.4 (3)
O8ⁱ—Dy1—O8—Dy1ⁱ	0.0	Dy1^v—O6—C10—C9	1.1 (6)
O2ⁱ—Dy1—O8—Dy1ⁱ	76.87 (12)	O4—C9—C10—O5	−160.8 (3)
O1—Dy1—O8—Dy1ⁱ	−81.74 (12)	O4—C9—C10—O6	20.5 (5)
O6ⁱⁱ—Dy1—O8—Dy1ⁱ	−146.60 (11)	Dy1—O7—C11—O8	2.0 (5)
O5ⁱⁱⁱ—Dy1—O8—Dy1ⁱ	57.68 (18)	Dy1—O7—C11—C12	177.9 (3)
O1W—Dy1—O8—Dy1ⁱ	−64.1 (2)	Dy1ⁱ—O8—C11—O7	−133.2 (8)
O7—Dy1—O8—Dy1ⁱ	165.76 (18)	Dy1—O8—C11—O7	−1.7 (4)
O4ⁱⁱ—Dy1—O8—Dy1ⁱ	148.44 (9)	Dy1ⁱ—O8—C11—C12	50.8 (10)
Dy1—O1—C1—O2	−0.9 (7)	Dy1—O8—C11—C12	−177.7 (4)
Dy1—O1—C1—C2	−179.0 (3)	C13—O9—C12—C11	68.3 (6)
Dy1ⁱ—O2—C1—O1	−18.9 (8)	O7—C11—C12—O9	18.6 (6)
Dy1ⁱ—O2—C1—C2	159.4 (4)	O8—C11—C12—O9	−165.4 (4)
O3—O3—C2—C1	0.00 (8)	C12—O9—C13—C14	−172.0 (4)
C3—O3—C2—C1	−174.5 (4)	C12—O9—C13—C15	9.4 (7)
O1—C1—C2—O3	−27.4 (6)	C15—C13—C14—C15^iv	0.4 (8)
O2—C1—C2—O3	154.2 (4)	O9—C13—C14—C15^iv	−178.4 (4)
C2—O3—C3—O3	0 (43)	C14—C13—C15—C14^iv	−0.4 (8)
O3—O3—C3—C5	0.00 (12)	O9—C13—C15—C14^iv	178.3 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H16A···O6ⁱⁱⁱ	0.80 (3)	2.11 (5)	2.706 (4)	131 (6)
O1W—H16B···O2W	0.79 (3)	1.98 (4)	2.755 (6)	166 (7)
O2W—H17A···O3	0.82 (3)	2.41 (6)	2.952 (5)	125 (5)

Symmetry code: (iii) x+1, −y+1/2, z+3/2.

Experimental details

Crystal data
Chemical formula	[Dy₂(C₁₀H₈O₆)₃(H₂O)₂]·2H₂O
M_r	1069.56
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	12.080 (2), 16.615 (3), 8.8802 (18)
β (°)	109.32 (3)
V (Å³)	1682.0 (6)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	4.50
Crystal size (mm)	0.19 × 0.16 × 0.13

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.437, 0.548
No. of measured, independent and observed [I > 2σ(I)] reflections	16183, 3838, 3229
R_int	0.043
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.028, 0.059, 1.06
No. of reflections	3838
No. of parameters	256
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)	0.83, −0.93

Computer programs: PROCESS-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2000).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H16A···O6ⁱ	0.80 (3)	2.11 (5)	2.706 (4)	131 (6)
O1W—H16B···O2W	0.79 (3)	1.98 (4)	2.755 (6)	166 (7)
O2W—H17A···O3	0.82 (3)	2.41 (6)	2.952 (5)	125 (5)

Symmetry code: (i) x+1, −y+1/2, z+3/2.

Acknowledgements

This work was supported by the Scientific Research Foundation for Returned Overseas Chinese Scholars, Chinese Education Ministry (20071108).

References

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