catena-Poly[[[diaqua­(2-fluoro­benzoato-κ2O,O′)strontium]-μ3-2-fluoro­benzoato-κ5O:O,O′:O′,F] monohydrate]

Jin, Z.-N.

doi:10.1107/S1600536811008397

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 4| April 2011| Page m440

doi:10.1107/S1600536811008397

Open

access

catena-Poly[[[diaqua(2-fluorobenzoato-κ²O,O′)strontium]-μ₃-2-fluorobenzoato-κ⁵O:O,O′:O′,F] monohydrate]

Zhu-Nian Jin ^a ^*

^aCollege of Materials Science and Chemical Engineering, Jinhua College of Profession and Technology, Jinhua, Zhejiang 321017, People's Republic of China
^*Correspondence e-mail: jzn@chem.jhc.cn

(Received 20 February 2011; accepted 5 March 2011; online 12 March 2011)

In the title compound, {[Sr(C₇H₄FO₂)₂(H₂O)₂]·H₂O}_n, the Sr^II atom is coordinated by six O atoms and one F atom from four 2-fluorobenzoate ligands and two water molecules, resulting in an irregular SrFO₈ coordination environment. The μ₃-2-fluorobenzoate ligand bridges three symmetry-related Sr^II atoms, giving rise to a chain structure extending along [010]. The polymeric chains are connected via O—H⋯O hydrogen bonds into a two-dimensional supramolecular structure parallel to (100).

Related literature

For metal complexes with 2-fluorobenzoate ligands, see: Zhang et al. (2005a ,b ); Zhang (2006 ). For related structures, see: Zhang (2008 , 2009 ).

Experimental

Crystal data

[Sr(C₇H₄FO₂)₂(H₂O)₂]·H₂O
M_r = 419.87
Monoclinic, P 2₁ /c
a = 12.515 (3) Å
b = 6.8232 (14) Å
c = 19.489 (4) Å
β = 93.71 (3)°
V = 1660.7 (6) Å³
Z = 4
Mo Kα radiation
μ = 3.30 mm⁻¹
T = 290 K
0.22 × 0.16 × 0.12 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.535, T_max = 0.674
12414 measured reflections
2912 independent reflections
2351 reflections with I > 2σ(I)
R_int = 0.043

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.097
S = 1.28
2912 reflections
218 parameters
H-atom parameters constrained
Δρ_max = 0.67 e Å⁻³
Δρ_min = −0.68 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5A⋯O7ⁱ	0.82	2.11	2.854 (5)	152
O5—H5B⋯O7ⁱⁱ	0.82	2.14	2.914 (6)	158
O6—H6A⋯O1ⁱⁱⁱ	0.82	2.10	2.791 (5)	142
O6—H6B⋯O2ⁱⁱ	0.82	2.22	2.901 (5)	140
O7—H7A⋯O2ⁱⁱ	0.82	2.01	2.800 (5)	161
Symmetry codes: (i) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: RAPID-AUTO (Rigaku, 1998 ); cell refinement: RAPID-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: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811008397/hy2410sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811008397/hy2410Isup2.hkl

checkCIF report

Comment top

Metal ions with 2-fluorobenzoate ligands can form, among others, mononuclear and dinuclear complexes (Zhang, 2006; Zhang et al., 2005a,b). However, very few complexes of 2-fluorobenzoate ligands with one-dimensional chain structure have been reported. In this paper, we report the synthesis and crystal structure of a one-dimensional chain strontium(II) complex with 2-fluorobenzoate.

The crystal structure of the title compound is similar to those of the reported complexes (Zhang, 2008, 2009). The Sr^II atom is coordinated by six O atoms and one F atom from four 2-fluorobenzoate ligands and two water molecules in an irregular SrFO₈ coordination geometry. The µ₃-2-fluorobenzoate ligand bridges three symmetry-related Sr^II atoms, giving rise to a chain structure extending along [0 1 0], with Sr—O bond lengths in the range of 2.463 (3) to 2.705 (3) Å and the Sr—F bond length being 2.908 (4) Å. Separation between Sr1 and Sr1ⁱ [symmetry code: (i) -x+1, y+1/2, -z+1/2] is 4.1869 (8)Å (Fig. 1). The polymeric chains are connected via O—H···O intermolecular hydrogen bonds (Table 2) between the coordinated and uncoordinated water molecules and the carboxylate groups of the 2-fluorobenzoate ligands into a two-dimensional supramolecular structure (Fig. 2).

Related literature top

For metal complexes with 2-fluorobenzoate ligands, see: Zhang et al. (2005a,b); Zhang (2006). For related structures, see: Zhang (2008, 2009).

Experimental top

Sr(NO₃)₂ (0.109 g, 0.50 mmol) was dissolved in appropriate amount of water and then 1M Na₂CO₃ solution was added. SrCO₃ was obtained by filtration, which was washed with distilled water for 5 times. The freshly prepared SrCO₃, 2-fluorobenzoic acid (0.036 g, 0.25 mmol), 2,2'-bipyridine (0.039 g, 0.25 mmol) and CH₃OH/H₂O (v/v = 1:2, 15 ml) were mixed and stirred for 2 h. Subsequently, the resulting cream suspension was heated in a 23 ml Teflon-lined stainless steel autoclave at 433 K for 97 h. After the autoclave was cooled to room temperature in a procedure of 43 h, the solid was filtered off. The resulting filtrate was allowed to stand at room temperature, and slow evaporation for 6 weeks afforded colorless block single crystals.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-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: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The one-dimensional chain structure of the title compound. Displacement ellipsoids are drawn at the 40% probability level. H atoms have been omitted for clarity. Hydrogen bonds are shown as dashed lines. [Symmetry codes: (i) -x+1, y+1/2, -z+1/2; (ii) -x+1, y-1/2, -z+1/2.]
	Fig. 2. A packing diagram of the title compound, viewed along the b axis. Hydrogen bonds are shown as dashed lines.

catena-Poly[[[diaqua(2-fluorobenzoato- κ²O,O')strontium]-µ₃-2-fluorobenzoato- κ⁵O:O,O':O',F] monohydrate] top

Crystal data top

[Sr(C₇H₄FO₂)₂(H₂O)₂]·H₂O	F(000) = 840
M_r = 419.87	D_x = 1.679 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2912 reflections
a = 12.515 (3) Å	θ = 3.2–25.0°
b = 6.8232 (14) Å	µ = 3.30 mm⁻¹
c = 19.489 (4) Å	T = 290 K
β = 93.71 (3)°	Block, colorless
V = 1660.7 (6) Å³	0.22 × 0.16 × 0.12 mm
Z = 4

Data collection top

Rigaku R-AXIS RAPID diffractometer	2912 independent reflections
Radiation source: rotation anode	2351 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.043
ω scans	θ_max = 25.0°, θ_min = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −14→14
T_min = 0.535, T_max = 0.674	k = −7→8
12414 measured reflections	l = −23→23

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)] = 0.032	H-atom parameters constrained
wR(F²) = 0.097	w = 1/[σ²(F_o²) + (0.P)² + 5.2938P] where P = (F_o² + 2F_c²)/3
S = 1.28	(Δ/σ)_max = 0.001
2912 reflections	Δρ_max = 0.67 e Å⁻³
218 parameters	Δρ_min = −0.68 e Å⁻³
0 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: 0.0066 (5)

Crystal data top

[Sr(C₇H₄FO₂)₂(H₂O)₂]·H₂O	V = 1660.7 (6) Å³
M_r = 419.87	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 12.515 (3) Å	µ = 3.30 mm⁻¹
b = 6.8232 (14) Å	T = 290 K
c = 19.489 (4) Å	0.22 × 0.16 × 0.12 mm
β = 93.71 (3)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	2912 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	2351 reflections with I > 2σ(I)
T_min = 0.535, T_max = 0.674	R_int = 0.043
12414 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	0 restraints
wR(F²) = 0.097	H-atom parameters constrained
S = 1.28	Δρ_max = 0.67 e Å⁻³
2912 reflections	Δρ_min = −0.68 e Å⁻³
218 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Sr1	0.49560 (4)	0.13650 (6)	0.18761 (2)	0.02804 (17)
F1	0.8456 (3)	−0.2517 (6)	0.1198 (2)	0.0793 (13)
F2	0.6409 (3)	0.4689 (5)	0.4237 (2)	0.0751 (12)
O1	0.6953 (3)	0.2536 (5)	0.1848 (2)	0.0513 (11)
O2	0.6718 (3)	−0.0557 (5)	0.15556 (19)	0.0398 (9)
O3	0.5848 (3)	−0.0267 (4)	0.30415 (18)	0.0366 (8)
O4	0.4430 (3)	−0.2113 (5)	0.18799 (19)	0.0386 (9)
O5	0.5122 (3)	0.2790 (6)	0.0668 (2)	0.0581 (11)
H5A	0.4729	0.2551	0.0325	0.087*
H5B	0.5570	0.3656	0.0634	0.087*
O6	0.3191 (3)	0.1157 (5)	0.24982 (19)	0.0414 (9)
H6A	0.3064	0.0463	0.2827	0.062*
H6B	0.3006	0.2265	0.2602	0.062*
O7	0.3815 (3)	0.1569 (6)	0.4433 (2)	0.0602 (12)
H7A	0.3644	0.2184	0.4082	0.090*
H7B	0.3370	0.1511	0.4723	0.090*
C1	0.8510 (4)	0.0722 (8)	0.1647 (3)	0.0356 (12)
C2	0.9161 (5)	0.2282 (10)	0.1858 (3)	0.0525 (16)
H2	0.8851	0.3423	0.2014	0.063*
C3	1.0267 (5)	0.2175 (12)	0.1841 (4)	0.069 (2)
H3	1.0689	0.3235	0.1989	0.082*
C4	1.0738 (5)	0.0520 (13)	0.1607 (4)	0.069 (2)
H4	1.1478	0.0459	0.1593	0.083*
C5	1.0123 (4)	−0.1044 (11)	0.1394 (3)	0.0595 (18)
H5	1.0439	−0.2176	0.1235	0.071*
C6	0.9030 (4)	−0.0920 (9)	0.1419 (3)	0.0472 (14)
C7	0.7313 (4)	0.0909 (7)	0.1680 (2)	0.0340 (12)
C8	0.6861 (4)	0.1429 (7)	0.3916 (2)	0.0301 (11)
C9	0.7526 (4)	−0.0162 (8)	0.4058 (3)	0.0406 (13)
H9	0.7459	−0.1266	0.3779	0.049*
C10	0.8289 (5)	−0.0148 (10)	0.4606 (3)	0.0572 (17)
H10	0.8724	−0.1236	0.4694	0.069*
C11	0.8399 (5)	0.1477 (12)	0.5016 (3)	0.0640 (19)
H11	0.8915	0.1485	0.5382	0.077*
C12	0.7760 (5)	0.3100 (10)	0.4897 (3)	0.0594 (18)
H12	0.7830	0.4197	0.5180	0.071*
C13	0.7012 (4)	0.3044 (8)	0.4344 (3)	0.0429 (13)
C14	0.6027 (3)	0.1360 (7)	0.3328 (2)	0.0241 (10)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sr1	0.0313 (3)	0.0191 (2)	0.0333 (3)	−0.00040 (19)	−0.00080 (18)	0.0008 (2)
F1	0.050 (2)	0.060 (2)	0.128 (4)	0.0046 (19)	0.008 (2)	−0.038 (2)
F2	0.105 (3)	0.046 (2)	0.069 (3)	0.020 (2)	−0.030 (2)	−0.0262 (19)
O1	0.043 (2)	0.030 (2)	0.082 (3)	−0.0060 (18)	0.011 (2)	−0.015 (2)
O2	0.037 (2)	0.0299 (19)	0.052 (2)	−0.0019 (16)	0.0028 (17)	−0.0079 (17)
O3	0.049 (2)	0.0202 (17)	0.039 (2)	−0.0012 (16)	−0.0090 (17)	−0.0037 (15)
O4	0.044 (2)	0.0245 (18)	0.045 (2)	−0.0049 (16)	−0.0090 (17)	−0.0026 (16)
O5	0.063 (3)	0.068 (3)	0.043 (2)	−0.017 (2)	−0.001 (2)	0.013 (2)
O6	0.0369 (19)	0.0283 (19)	0.060 (2)	−0.0018 (16)	0.0105 (17)	0.0053 (18)
O7	0.072 (3)	0.064 (3)	0.045 (2)	0.014 (2)	0.004 (2)	0.013 (2)
C1	0.030 (3)	0.043 (3)	0.033 (3)	−0.002 (2)	0.000 (2)	0.001 (2)
C2	0.044 (3)	0.062 (4)	0.051 (4)	−0.012 (3)	0.001 (3)	−0.012 (3)
C3	0.040 (4)	0.097 (6)	0.069 (5)	−0.027 (4)	0.000 (3)	−0.012 (4)
C4	0.028 (3)	0.112 (6)	0.068 (5)	−0.001 (4)	0.005 (3)	−0.003 (4)
C5	0.032 (3)	0.085 (5)	0.061 (4)	0.016 (3)	0.007 (3)	−0.007 (4)
C6	0.036 (3)	0.057 (4)	0.048 (3)	−0.007 (3)	−0.001 (3)	−0.006 (3)
C7	0.039 (3)	0.035 (3)	0.026 (3)	−0.003 (2)	−0.009 (2)	−0.001 (2)
C8	0.032 (3)	0.029 (2)	0.030 (3)	−0.003 (2)	0.007 (2)	0.002 (2)
C9	0.038 (3)	0.041 (3)	0.042 (3)	0.006 (2)	−0.004 (2)	0.005 (3)
C10	0.042 (3)	0.073 (5)	0.055 (4)	0.016 (3)	−0.006 (3)	0.013 (4)
C11	0.049 (4)	0.098 (6)	0.043 (4)	−0.005 (4)	−0.011 (3)	0.000 (4)
C12	0.069 (4)	0.071 (5)	0.037 (4)	−0.005 (4)	−0.009 (3)	−0.012 (3)
C13	0.044 (3)	0.042 (3)	0.041 (3)	0.002 (3)	−0.003 (3)	−0.006 (3)
C14	0.021 (2)	0.023 (2)	0.029 (2)	0.000 (2)	0.0043 (18)	0.000 (2)

Geometric parameters (Å, º) top

Sr1—O4	2.463 (3)	C1—C6	1.384 (8)
Sr1—O3ⁱ	2.518 (3)	C1—C2	1.387 (7)
Sr1—O5	2.568 (4)	C1—C7	1.509 (7)
Sr1—O6	2.591 (3)	C2—C3	1.388 (8)
Sr1—O1	2.627 (4)	C2—H2	0.9300
Sr1—O2	2.674 (3)	C3—C4	1.365 (10)
Sr1—O4ⁱ	2.703 (4)	C3—H3	0.9300
Sr1—O3	2.705 (3)	C4—C5	1.364 (9)
Sr1—F2ⁱⁱ	2.908 (4)	C4—H4	0.9300
F1—C6	1.359 (6)	C5—C6	1.375 (7)
F2—C13	1.361 (6)	C5—H5	0.9300
F2—Sr1ⁱ	2.908 (4)	C8—C9	1.385 (7)
O1—C7	1.250 (6)	C8—C13	1.387 (7)
O2—C7	1.261 (6)	C8—C14	1.500 (6)
O3—C14	1.256 (5)	C9—C10	1.386 (8)
O3—Sr1ⁱⁱ	2.518 (3)	C9—H9	0.9300
O4—C14ⁱⁱ	1.244 (5)	C10—C11	1.369 (9)
O4—Sr1ⁱⁱ	2.703 (4)	C10—H10	0.9300
O5—H5A	0.8200	C11—C12	1.377 (9)
O5—H5B	0.8200	C11—H11	0.9300
O6—H6A	0.8200	C12—C13	1.382 (8)
O6—H6B	0.8200	C12—H12	0.9300
O7—H7A	0.8200	C14—O4ⁱ	1.244 (5)
O7—H7B	0.8200

O4—Sr1—O3ⁱ	140.48 (11)	H6A—O6—H6B	105.5
O4—Sr1—O5	113.89 (13)	H7A—O7—H7B	116.6
O3ⁱ—Sr1—O5	76.65 (13)	C6—C1—C2	115.9 (5)
O4—Sr1—O6	73.14 (11)	C6—C1—C7	124.8 (5)
O3ⁱ—Sr1—O6	70.37 (11)	C2—C1—C7	119.3 (5)
O5—Sr1—O6	124.86 (13)	C1—C2—C3	121.4 (6)
O4—Sr1—O1	123.21 (12)	C1—C2—H2	119.3
O3ⁱ—Sr1—O1	96.20 (11)	C3—C2—H2	119.3
O5—Sr1—O1	74.49 (14)	C4—C3—C2	120.2 (6)
O6—Sr1—O1	150.09 (12)	C4—C3—H3	119.9
O4—Sr1—O2	75.68 (11)	C2—C3—H3	119.9
O3ⁱ—Sr1—O2	143.25 (11)	C5—C4—C3	120.1 (6)
O5—Sr1—O2	81.65 (13)	C5—C4—H4	119.9
O6—Sr1—O2	145.41 (11)	C3—C4—H4	119.9
O1—Sr1—O2	49.04 (11)	C4—C5—C6	119.0 (6)
O4—Sr1—O4ⁱ	115.34 (9)	C4—C5—H5	120.5
O3ⁱ—Sr1—O4ⁱ	71.56 (10)	C6—C5—H5	120.5
O5—Sr1—O4ⁱ	129.93 (12)	F1—C6—C5	116.5 (6)
O6—Sr1—O4ⁱ	78.62 (11)	F1—C6—C1	120.0 (5)
O1—Sr1—O4ⁱ	71.71 (12)	C5—C6—C1	123.4 (6)
O2—Sr1—O4ⁱ	101.95 (11)	O1—C7—O2	122.4 (5)
O4—Sr1—O3	72.34 (10)	O1—C7—C1	117.5 (4)
O3ⁱ—Sr1—O3	117.84 (8)	O2—C7—C1	120.0 (5)
O5—Sr1—O3	150.73 (12)	O1—C7—Sr1	60.2 (3)
O6—Sr1—O3	84.40 (11)	O2—C7—Sr1	62.3 (3)
O1—Sr1—O3	78.54 (12)	C1—C7—Sr1	175.0 (3)
O2—Sr1—O3	72.10 (11)	C9—C8—C13	116.5 (5)
O4ⁱ—Sr1—O3	47.70 (10)	C9—C8—C14	120.5 (4)
O4—Sr1—F2ⁱⁱ	58.61 (10)	C13—C8—C14	123.1 (4)
O3ⁱ—Sr1—F2ⁱⁱ	100.89 (11)	C8—C9—C10	121.6 (6)
O5—Sr1—F2ⁱⁱ	62.81 (12)	C8—C9—H9	119.2
O6—Sr1—F2ⁱⁱ	81.40 (12)	C10—C9—H9	119.2
O1—Sr1—F2ⁱⁱ	128.15 (13)	C11—C10—C9	119.6 (6)
O2—Sr1—F2ⁱⁱ	94.95 (12)	C11—C10—H10	120.2
O4ⁱ—Sr1—F2ⁱⁱ	160.00 (12)	C9—C10—H10	120.2
O3—Sr1—F2ⁱⁱ	130.94 (9)	C10—C11—C12	121.1 (6)
C13—F2—Sr1ⁱ	137.0 (3)	C10—C11—H11	119.4
C7—O1—Sr1	95.5 (3)	C12—C11—H11	119.4
C7—O2—Sr1	93.0 (3)	C11—C12—C13	117.8 (6)
C14—O3—Sr1ⁱⁱ	147.1 (3)	C11—C12—H12	121.1
C14—O3—Sr1	93.5 (3)	C13—C12—H12	121.1
Sr1ⁱⁱ—O3—Sr1	106.53 (12)	F2—C13—C12	116.0 (5)
C14ⁱⁱ—O4—Sr1	157.5 (3)	F2—C13—C8	120.7 (5)
C14ⁱⁱ—O4—Sr1ⁱⁱ	93.9 (3)	C12—C13—C8	123.3 (5)
Sr1—O4—Sr1ⁱⁱ	108.21 (12)	O4ⁱ—C14—O3	122.0 (4)
Sr1—O5—H5A	126.3	O4ⁱ—C14—C8	120.3 (4)
Sr1—O5—H5B	116.3	O3—C14—C8	117.6 (4)
H5A—O5—H5B	117.0	O4ⁱ—C14—Sr1	62.1 (2)
Sr1—O6—H6A	127.7	O3—C14—Sr1	62.2 (2)
Sr1—O6—H6B	109.2	C8—C14—Sr1	162.0 (3)

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···O7ⁱⁱⁱ	0.82	2.11	2.854 (5)	152
O5—H5B···O7ⁱ	0.82	2.14	2.914 (6)	158
O6—H6A···O1ⁱⁱ	0.82	2.10	2.791 (5)	142
O6—H6B···O2ⁱ	0.82	2.22	2.901 (5)	140
O7—H7A···O2ⁱ	0.82	2.01	2.800 (5)	161

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

Experimental details

Crystal data
Chemical formula	[Sr(C₇H₄FO₂)₂(H₂O)₂]·H₂O
M_r	419.87
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	290
a, b, c (Å)	12.515 (3), 6.8232 (14), 19.489 (4)
β (°)	93.71 (3)
V (Å³)	1660.7 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.30
Crystal size (mm)	0.22 × 0.16 × 0.12

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.535, 0.674
No. of measured, independent and observed [I > 2σ(I)] reflections	12414, 2912, 2351
R_int	0.043
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.097, 1.28
No. of reflections	2912
No. of parameters	218
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.67, −0.68

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), 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···O7ⁱ	0.82	2.11	2.854 (5)	152
O5—H5B···O7ⁱⁱ	0.82	2.14	2.914 (6)	158
O6—H6A···O1ⁱⁱⁱ	0.82	2.10	2.791 (5)	142
O6—H6B···O2ⁱⁱ	0.82	2.22	2.901 (5)	140
O7—H7A···O2ⁱⁱ	0.82	2.01	2.800 (5)	161

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

Acknowledgements

The author gratefully acknowledges financial support by the Education Office of Zhejiang Province (grant No. 20051316).

References

Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku/MSC (2002). CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zhang, B.-S. (2006). Z. Kristallogr. New Cryst. Struct. 221, 355–356. CAS Google Scholar
Zhang, B.-S. (2008). Acta Cryst. E64, m1055–m1056. Web of Science CSD CrossRef IUCr Journals Google Scholar
Zhang, B.-S. (2009). Acta Cryst. E65, m1500. Web of Science CSD CrossRef IUCr Journals Google Scholar
Zhang, B.-S., Zeng, X.-R., Fang, X.-N. & Huang, C.-F. (2005a). Z. Kristallogr. New Cryst. Struct. 220, 141–142. CAS Google Scholar
Zhang, B.-S., Zeng, X.-R., Yu, Y.-Y., Fang, X.-N. & Huang, C.-F. (2005b). Z. Kristallogr. New Cryst. Struct. 220, 75–76. CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.