Poly[hexa­aqua­bis(μ3-terephthalato)(μ2-terephthalato)diytterbium(III)]

Feng, S.

doi:10.1107/S160053680905171X

metal-organic compounds

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Volume 66| Part 1| January 2010| Page m33

doi:10.1107/S160053680905171X

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Poly[hexaaquabis(μ₃-terephthalato)(μ₂-terephthalato)diytterbium(III)]

Sun Feng ^a ^*

^aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510631, People's Republic of China
^*Correspondence e-mail: fengsun1974@yahoo.com.cn

(Received 15 November 2009; accepted 1 December 2009; online 9 December 2009)

In the title two-dimensional coordination polymer, [Yb₂(C₈H₄O₄)₃(H₂O)₆]_n, the unique Yb^III ion is eight-coordinated in a distorted dodecahedral coordination geometry by three water O atoms and five O atoms from carboxylate groups belonging to four different terephthalate ligands. One of the terephthalate ligands is located around an inversion center. The coordination polymers are parallel to (121) and are connected by O—H⋯O hydrogen bonds into a three-dimensional framework.

Related literature

For the isostructural erbium(III) and lutetium(III) complexes, see: Daiguebonne et al. (2006 ); Xie et al. (2008 ).

Experimental

Crystal data

[Yb₂(C₈H₄O₄)₃(H₂O)₆]
M_r = 473.26
Triclinic, $[P \overline 1]$
a = 7.8413 (7) Å
b = 9.5545 (8) Å
c = 10.6561 (9) Å
α = 68.827 (1)°
β = 71.024 (1)°
γ = 75.206 (1)°
V = 695.34 (10) Å³
Z = 2
Mo Kα radiation
μ = 6.77 mm⁻¹
T = 296 K
0.21 × 0.18 × 0.17 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.251, T_max = 0.316
3564 measured reflections
2444 independent reflections
2323 reflections with I > 2σ(I)
R_int = 0.015

Refinement

R[F² > 2σ(F²)] = 0.020
wR(F²) = 0.048
S = 1.04
2444 reflections
217 parameters
9 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.82 e Å⁻³
Δρ_min = −0.73 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯O2Wⁱ	0.81 (4)	2.35 (3)	3.123 (5)	158 (6)
O1W—H1W⋯O3	0.81 (4)	2.52 (4)	3.104 (5)	130 (4)
O1W—H2W⋯O5ⁱⁱ	0.82 (4)	1.91 (5)	2.714 (4)	170 (5)
O2W—H3W⋯O1ⁱⁱⁱ	0.82 (5)	1.97 (5)	2.771 (4)	167 (5)
O2W—H4W⋯O1^iv	0.82 (3)	2.17 (3)	2.900 (5)	149 (5)
O3W—H5W⋯O6^v	0.82 (3)	2.08 (2)	2.846 (4)	156 (4)
O3W—H6W⋯O1^iv	0.82 (4)	1.95 (4)	2.746 (4)	165 (5)
Symmetry codes: (i) -x, -y+1, -z+2; (ii) -x+1, -y+1, -z+2; (iii) -x, -y+1, -z+1; (iv) x, y-1, z+1; (v) -x+1, -y, -z+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: SHELXL97.

Supporting information

Crystal structure: contains datablock I. DOI: 10.1107/S160053680905171X/gk2241sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680905171X/gk2241Isup2.hkl

checkCIF report

Comment top

Terephthalic acid as a dicarboxylate ligand may exhibit various coordination modes with transition metals or lanthanide ions that result in one-, two- or three-dimensional metal-organic frameworks (MOFs). As an extension of this research we report here the structure of the title two-dimensional coordination polymer of Yb^III which is isostructural with Lu^III and Er^III complexes (Daiguebonne et al., 2006; Xie et al., 2008) .

The asymmetric unit of the title compound (Fig. 1) contains one Yb^IIIion, one and a half of terephthalate ligand, and three coordinated water molecules. The Yb^III ion is eight-coordinate with a dodecahedral coordination polyhedron made of three oxygen atoms from three coordination water molecules and five oxygen atoms from carboxylate groups of four different terephthalate ligands.

The coordination polymers are joined by O—H···O hydrogen bonds between coordinated water molecules and carboxylate groups of terephthalate ligands (Table 1).

Related literature top

Forthe isostructural erbium(III) and lutetium(III) complexes, see: Daiguebonne et al. (2006); Xie et al. (2008).

Experimental top

A mixture of AgNO₃(0.057 g, 0.33 mmol), Yb₂O₃(0.116 g, 0.33 mmol), 2-pyrazinecarboxylic acid(0.165 g, 1.33 mmol), terephthalic acid (0.166 g, 1.0 mmol), H₂O(7 ml), and HClO₄(0.257 mmol)(pH 2) was sealed in a 20 ml Teflon-lined reaction vessel at 443 K for 6 days and then slowly cooled to room temperature. The product was collected by filtration, washed with water and air-dried. Colorless block crystals were suitable for X-ray analysis were obtained.

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: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. ORTEP view of the asymmetric unit of the title compound with displacement ellipsoids drawn at the 30% probability level. Symmetry codes: (A) 1 - x, -y, 3 - z.;(B) -x, 1 - y, 2 - z; (C) 1 - x, 1 - y, 1 - z.
	Fig. 2. A view of the three-dimensional structure of the title compound. Hydrogen atoms are omitted for clarity.

Poly[hexaaquabis(µ₃-terephthalato)(µ₂-terephthalato)diytterbium(III)] top

Crystal data top

[Yb₂(C₈H₄O₄)₃(H₂O)₆]	Z = 2
M_r = 473.26	F(000) = 452
Triclinic, P1	D_x = 2.260 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.8413 (7) Å	Cell parameters from 2800 reflections
b = 9.5545 (8) Å	θ = 2.6–27.8°
c = 10.6561 (9) Å	µ = 6.77 mm⁻¹
α = 68.827 (1)°	T = 296 K
β = 71.024 (1)°	Block, colorless
γ = 75.206 (1)°	0.21 × 0.18 × 0.17 mm
V = 695.34 (10) Å³

Data collection top

Bruker APEXII area-detector diffractometer	2444 independent reflections
Radiation source: fine-focus sealed tube	2323 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.015
Detector resolution: 0 pixels mm^-1	θ_max = 25.2°, θ_min = 2.1°
ϕ and ω scan	h = −9→7
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −10→11
T_min = 0.251, T_max = 0.316	l = −12→11
3564 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)] = 0.020	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.048	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0237P)² + 0.8814P] where P = (F_o² + 2F_c²)/3
2444 reflections	(Δ/σ)_max = 0.003
217 parameters	Δρ_max = 0.82 e Å⁻³
9 restraints	Δρ_min = −0.73 e Å⁻³

Crystal data top

[Yb₂(C₈H₄O₄)₃(H₂O)₆]	γ = 75.206 (1)°
M_r = 473.26	V = 695.34 (10) Å³
Triclinic, P1	Z = 2
a = 7.8413 (7) Å	Mo Kα radiation
b = 9.5545 (8) Å	µ = 6.77 mm⁻¹
c = 10.6561 (9) Å	T = 296 K
α = 68.827 (1)°	0.21 × 0.18 × 0.17 mm
β = 71.024 (1)°

Data collection top

Bruker APEXII area-detector diffractometer	2444 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2323 reflections with I > 2σ(I)
T_min = 0.251, T_max = 0.316	R_int = 0.015
3564 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.020	9 restraints
wR(F²) = 0.048	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 0.82 e Å⁻³
2444 reflections	Δρ_min = −0.73 e Å⁻³
217 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
Yb1	0.26626 (2)	0.294523 (19)	1.006579 (16)	0.01940 (7)
C1	0.2794 (6)	0.7548 (5)	0.1682 (4)	0.0244 (9)
C2	0.2113 (6)	0.6900 (5)	0.3233 (4)	0.0231 (9)
C3	0.3017 (8)	0.5574 (6)	0.3942 (5)	0.0546 (17)
H3	0.3999	0.5039	0.3444	0.066*
C4	0.2506 (8)	0.5012 (6)	0.5381 (5)	0.0501 (15)
H4	0.3117	0.4094	0.5839	0.060*
C5	0.1094 (6)	0.5813 (5)	0.6133 (4)	0.0238 (9)
C6	0.0601 (5)	0.5283 (5)	0.7702 (4)	0.0210 (8)
C7	0.0173 (7)	0.7138 (6)	0.5423 (5)	0.0465 (14)
H7	−0.0791	0.7690	0.5917	0.056*
C8	0.0665 (7)	0.7660 (6)	0.3982 (5)	0.0435 (13)
H8	0.0001	0.8540	0.3519	0.052*
C9	0.3969 (5)	0.1538 (5)	1.2422 (4)	0.0221 (9)
C10	0.4506 (6)	0.0733 (5)	1.3751 (4)	0.0243 (9)
C11	0.5442 (8)	0.1424 (5)	1.4211 (5)	0.0406 (13)
H11	0.5754	0.2380	1.3678	0.049*
C12	0.4091 (8)	−0.0693 (6)	1.4544 (5)	0.0411 (13)
H12	0.3486	−0.1171	1.4234	0.049*
O1	0.1745 (4)	0.8546 (4)	0.1024 (3)	0.0324 (7)
O2	0.4422 (4)	0.7076 (4)	0.1137 (3)	0.0361 (8)
O3	−0.0475 (4)	0.6148 (4)	0.8340 (3)	0.0317 (7)
O4	0.1368 (5)	0.3988 (3)	0.8290 (3)	0.0336 (7)
O5	0.4165 (4)	0.2898 (3)	1.1772 (3)	0.0276 (7)
O6	0.3249 (4)	0.0831 (3)	1.1957 (3)	0.0271 (7)
O1W	0.3026 (5)	0.5482 (4)	0.9349 (4)	0.0387 (8)
H1W	0.221 (4)	0.617 (4)	0.914 (6)	0.058*
H2W	0.393 (4)	0.589 (5)	0.908 (6)	0.058*
O2W	0.0025 (5)	0.1676 (4)	1.0747 (4)	0.0358 (8)
H3W	−0.038 (7)	0.168 (5)	1.013 (4)	0.054*
H4W	0.030 (8)	0.0778 (19)	1.115 (5)	0.054*
O3W	0.3438 (5)	0.0930 (3)	0.9110 (3)	0.0329 (7)
H5W	0.451 (2)	0.065 (5)	0.877 (5)	0.049*
H6W	0.303 (5)	0.014 (3)	0.957 (5)	0.049*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Yb1	0.02266 (11)	0.02072 (11)	0.01111 (10)	−0.00012 (7)	−0.00580 (7)	−0.00153 (7)
C1	0.027 (2)	0.026 (2)	0.021 (2)	−0.0095 (19)	−0.0056 (18)	−0.0052 (18)
C2	0.026 (2)	0.028 (2)	0.015 (2)	−0.0081 (18)	−0.0059 (16)	−0.0031 (17)
C3	0.064 (4)	0.049 (3)	0.019 (2)	0.029 (3)	−0.001 (2)	−0.006 (2)
C4	0.065 (4)	0.039 (3)	0.017 (2)	0.027 (3)	−0.008 (2)	−0.002 (2)
C5	0.026 (2)	0.023 (2)	0.018 (2)	−0.0040 (18)	−0.0057 (17)	−0.0023 (17)
C6	0.023 (2)	0.022 (2)	0.018 (2)	−0.0043 (17)	−0.0086 (17)	−0.0035 (17)
C7	0.036 (3)	0.053 (3)	0.019 (2)	0.024 (2)	0.002 (2)	−0.003 (2)
C8	0.034 (3)	0.050 (3)	0.018 (2)	0.019 (2)	−0.005 (2)	0.003 (2)
C9	0.021 (2)	0.027 (2)	0.015 (2)	−0.0004 (17)	−0.0046 (16)	−0.0045 (18)
C10	0.030 (2)	0.023 (2)	0.018 (2)	0.0013 (18)	−0.0117 (17)	−0.0023 (17)
C11	0.070 (4)	0.028 (3)	0.029 (3)	−0.019 (2)	−0.028 (2)	0.007 (2)
C12	0.066 (4)	0.036 (3)	0.033 (3)	−0.020 (3)	−0.034 (3)	0.003 (2)
O1	0.0370 (18)	0.0362 (18)	0.0199 (15)	−0.0057 (15)	−0.0127 (14)	0.0009 (14)
O2	0.0302 (18)	0.046 (2)	0.0226 (16)	−0.0030 (15)	0.0006 (13)	−0.0083 (15)
O3	0.0330 (17)	0.0383 (19)	0.0170 (15)	0.0030 (14)	−0.0030 (13)	−0.0094 (14)
O4	0.054 (2)	0.0251 (17)	0.0212 (16)	0.0009 (15)	−0.0202 (15)	−0.0014 (13)
O5	0.0352 (17)	0.0276 (17)	0.0182 (15)	−0.0074 (13)	−0.0135 (13)	0.0027 (13)
O6	0.0391 (18)	0.0250 (16)	0.0196 (15)	−0.0059 (13)	−0.0179 (13)	0.0003 (13)
O1W	0.0313 (18)	0.0267 (18)	0.052 (2)	−0.0055 (14)	−0.0105 (17)	−0.0049 (16)
O2W	0.0395 (19)	0.0379 (19)	0.0327 (19)	−0.0096 (16)	−0.0140 (15)	−0.0074 (15)
O3W	0.0388 (19)	0.0277 (17)	0.0296 (18)	−0.0009 (14)	−0.0077 (15)	−0.0096 (14)

Geometric parameters (Å, º) top

Yb1—O2ⁱ	2.227 (3)	C6—O4	1.261 (5)
Yb1—O4	2.231 (3)	C7—C8	1.384 (6)
Yb1—O3ⁱⁱ	2.233 (3)	C7—H7	0.9300
Yb1—O1W	2.327 (3)	C8—H8	0.9300
Yb1—O3W	2.352 (3)	C9—O5	1.255 (5)
Yb1—O6	2.354 (3)	C9—O6	1.280 (5)
Yb1—O2W	2.438 (3)	C9—C10	1.487 (5)
Yb1—O5	2.450 (3)	C10—C12	1.376 (6)
Yb1—C9	2.773 (4)	C10—C11	1.389 (6)
C1—O1	1.252 (5)	C11—C12ⁱⁱⁱ	1.378 (6)
C1—O2	1.259 (5)	C11—H11	0.9300
C1—C2	1.502 (5)	C12—C11ⁱⁱⁱ	1.378 (6)
C2—C8	1.364 (6)	C12—H12	0.9300
C2—C3	1.370 (6)	O2—Yb1ⁱ	2.227 (3)
C3—C4	1.385 (6)	O3—Yb1ⁱⁱ	2.233 (3)
C3—H3	0.9300	O1W—H1W	0.81 (4)
C4—C5	1.373 (6)	O1W—H2W	0.82 (4)
C4—H4	0.9300	O2W—H3W	0.82 (5)
C5—C7	1.376 (6)	O2W—H4W	0.82 (3)
C5—C6	1.507 (5)	O3W—H5W	0.82 (3)
C6—O3	1.238 (5)	O3W—H6W	0.82 (4)

O2ⁱ—Yb1—O4	98.80 (12)	C5—C4—C3	119.9 (4)
O2ⁱ—Yb1—O3ⁱⁱ	144.25 (12)	C5—C4—H4	120.1
O4—Yb1—O3ⁱⁱ	98.76 (12)	C3—C4—H4	120.1
O2ⁱ—Yb1—O1W	76.69 (12)	C4—C5—C7	118.6 (4)
O4—Yb1—O1W	77.10 (12)	C4—C5—C6	120.8 (4)
O3ⁱⁱ—Yb1—O1W	77.26 (12)	C7—C5—C6	120.5 (4)
O2ⁱ—Yb1—O3W	73.41 (12)	O3—C6—O4	123.7 (4)
O4—Yb1—O3W	79.48 (11)	O3—C6—C5	118.9 (4)
O3ⁱⁱ—Yb1—O3W	140.62 (12)	O4—C6—C5	117.3 (4)
O1W—Yb1—O3W	138.30 (12)	C5—C7—C8	120.8 (4)
O2ⁱ—Yb1—O6	94.87 (11)	C5—C7—H7	119.6
O4—Yb1—O6	148.87 (11)	C8—C7—H7	119.6
O3ⁱⁱ—Yb1—O6	85.72 (11)	C2—C8—C7	120.8 (4)
O1W—Yb1—O6	133.53 (11)	C2—C8—H8	119.6
O3W—Yb1—O6	77.85 (11)	C7—C8—H8	119.6
O2ⁱ—Yb1—O2W	143.67 (12)	O5—C9—O6	119.7 (4)
O4—Yb1—O2W	74.76 (12)	O5—C9—C10	121.4 (4)
O3ⁱⁱ—Yb1—O2W	71.38 (12)	O6—C9—C10	118.8 (4)
O1W—Yb1—O2W	133.46 (12)	O5—C9—Yb1	62.0 (2)
O3W—Yb1—O2W	70.26 (12)	O6—C9—Yb1	57.76 (19)
O6—Yb1—O2W	77.66 (11)	C10—C9—Yb1	174.7 (3)
O2ⁱ—Yb1—O5	77.29 (11)	C12—C10—C11	118.9 (4)
O4—Yb1—O5	156.47 (11)	C12—C10—C9	121.2 (4)
O3ⁱⁱ—Yb1—O5	74.22 (11)	C11—C10—C9	119.9 (4)
O1W—Yb1—O5	79.44 (11)	C12ⁱⁱⁱ—C11—C10	120.0 (4)
O3W—Yb1—O5	120.37 (11)	C12ⁱⁱⁱ—C11—H11	120.0
O6—Yb1—O5	54.27 (9)	C10—C11—H11	120.0
O2W—Yb1—O5	121.90 (10)	C10—C12—C11ⁱⁱⁱ	121.1 (4)
O2ⁱ—Yb1—C9	86.23 (11)	C10—C12—H12	119.5
O4—Yb1—C9	174.57 (12)	C11ⁱⁱⁱ—C12—H12	119.5
O3ⁱⁱ—Yb1—C9	78.02 (11)	C1—O2—Yb1ⁱ	161.1 (3)
O1W—Yb1—C9	106.19 (13)	C6—O3—Yb1ⁱⁱ	162.9 (3)
O3W—Yb1—C9	100.18 (12)	C6—O4—Yb1	137.1 (3)
O6—Yb1—C9	27.39 (11)	C9—O5—Yb1	91.1 (2)
O2W—Yb1—C9	99.99 (11)	C9—O6—Yb1	94.8 (2)
O5—Yb1—C9	26.89 (11)	Yb1—O1W—H1W	121 (3)
O1—C1—O2	124.3 (4)	Yb1—O1W—H2W	132 (3)
O1—C1—C2	118.7 (4)	H1W—O1W—H2W	105 (5)
O2—C1—C2	116.9 (4)	Yb1—O2W—H3W	118 (4)
C8—C2—C3	118.3 (4)	Yb1—O2W—H4W	109 (4)
C8—C2—C1	121.2 (4)	H3W—O2W—H4W	105 (5)
C3—C2—C1	120.3 (4)	Yb1—O3W—H5W	119 (4)
C2—C3—C4	121.6 (5)	Yb1—O3W—H6W	119 (4)
C2—C3—H3	119.2	H5W—O3W—H6W	104 (4)
C4—C3—H3	119.2

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O2Wⁱⁱ	0.81 (4)	2.35 (3)	3.123 (5)	158 (6)
O1W—H1W···O3	0.81 (4)	2.52 (4)	3.104 (5)	130 (4)
O1W—H2W···O5^iv	0.82 (4)	1.91 (5)	2.714 (4)	170 (5)
O2W—H3W···O1^v	0.82 (5)	1.97 (5)	2.771 (4)	167 (5)
O2W—H4W···O1^vi	0.82 (3)	2.17 (3)	2.900 (5)	149 (5)
O3W—H5W···O6^vii	0.82 (3)	2.08 (2)	2.846 (4)	156 (4)
O3W—H6W···O1^vi	0.82 (4)	1.95 (4)	2.746 (4)	165 (5)

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

Experimental details

Crystal data
Chemical formula	[Yb₂(C₈H₄O₄)₃(H₂O)₆]
M_r	473.26
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	7.8413 (7), 9.5545 (8), 10.6561 (9)
α, β, γ (°)	68.827 (1), 71.024 (1), 75.206 (1)
V (Å³)	695.34 (10)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	6.77
Crystal size (mm)	0.21 × 0.18 × 0.17

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.251, 0.316
No. of measured, independent and observed [I > 2σ(I)] reflections	3564, 2444, 2323
R_int	0.015
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.020, 0.048, 1.04
No. of reflections	2444
No. of parameters	217
No. of restraints	9
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.82, −0.73

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
O1W—H1W···O2Wⁱ	0.81 (4)	2.35 (3)	3.123 (5)	158 (6)
O1W—H1W···O3	0.81 (4)	2.52 (4)	3.104 (5)	130 (4)
O1W—H2W···O5ⁱⁱ	0.82 (4)	1.91 (5)	2.714 (4)	170 (5)
O2W—H3W···O1ⁱⁱⁱ	0.82 (5)	1.97 (5)	2.771 (4)	167 (5)
O2W—H4W···O1^iv	0.82 (3)	2.17 (3)	2.900 (5)	149 (5)
O3W—H5W···O6^v	0.82 (3)	2.08 (2)	2.846 (4)	156 (4)
O3W—H6W···O1^iv	0.82 (4)	1.95 (4)	2.746 (4)	165 (5)

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

Acknowledgements

The author acknowledges South China Normal University for supporting this work.

References

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