Poly[[(μ2-di-3-pyridyl­methanone-κ2N:N′)(μ2-hexa­fluoro­silicato-κ2F:F′)copper(II)] dihydrate]

Yang, Y.-L.

doi:10.1107/S1600536812002267

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 2| February 2012| Page m209

doi:10.1107/S1600536812002267

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Poly[[(μ₂-di-3-pyridylmethanone-κ²N:N′)(μ₂-hexafluorosilicato-κ²F:F′)copper(II)] dihydrate]

Yong-Li Yang ^a ^*

^aDepartment of Chemistry, Capital Normal University, Beijing 100048, People's Republic of China
^*Correspondence e-mail: ylcnu@yahoo.cn

(Received 20 November 2011; accepted 18 January 2012; online 31 January 2012)

In the title complex, {[Cu(SiF₆)(C₁₁H₈N₂O)₂]·2H₂O}_n, the Cu^II atom adopts an N₄F₂-octahedral coordination geometry with four pyridine N atoms in the equatorial sites and two F atoms in the axial sites. The di-3-pyridylmethanone and hexafluorosilicate ligands act as bidentate ligands, linking symmetry-related Cu^II atoms. Water molecules form O—H⋯O and O—H⋯F hydrogen bonds with the di-3-pyridylmethanone and hexafluorosilicate ligands. The Cu²⁺ and SiF₆²⁻ ions are each located on a twofold axis.

Related literature

For background to the coordination chemistry of pyridyl-based derivatives, see: Manriquez et al. (1991 ); Wang et al. (2009 ). For dipyridylmethanone, see: Boudalis et al. (2003 ). For transition metal complexes of di-3-pyridylmethanone, see: Chen et al. (2005 , 2009 ); Chen & Mak (2005 ).

Experimental

Crystal data

[Cu(SiF₆)(C₁₁H₈N₂O)₂]·2H₂O
M_r = 610.05
Monoclinic, C 2/c
a = 22.276 (3) Å
b = 8.0625 (11) Å
c = 15.773 (2) Å
β = 123.757 (2)°
V = 2355.2 (5) Å³
Z = 4
Mo Kα radiation
μ = 1.07 mm⁻¹
T = 296 K
0.40 × 0.32 × 0.30 mm

Data collection

Bruker SMART APEXII CCD area-detector' diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.742, T_max = 1.000
6195 measured reflections
2082 independent reflections
1822 reflections with I > 2σ(I)
R_int = 0.031

Refinement

R[F² > 2σ(F²)] = 0.034
wR(F²) = 0.094
S = 1.02
2082 reflections
174 parameters
H-atom parameters constrained
Δρ_max = 0.54 e Å⁻³
Δρ_min = −0.31 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1B⋯F1	0.89	1.89	2.777 (6)	173
O1W—H1A⋯O1ⁱ	0.89	2.03	2.850 (3)	153
Symmetry code: (i) -x+1, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2007); cell refinement: APEX2 and SAINT (Bruker, 2007); 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 and PLATON (Spek, 2009 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812002267/aa2040sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812002267/aa2040Isup2.hkl

checkCIF report

Comment top

Pyridyl-based building blocks are widely used in construction various supramolecules of transition metal complexes (Manriquez et al. 1991; Wang et al., 2009). Among them, dipyridylmethanone derivates are famous for their versatile linkage behavior in numbers of coordination supramolecular assemblies (Boudalis et al., 2003). Di-3-pyridinylmethanone was provided to act as a flexible µ²-bridging mode in many coordination frameworks, such as one-dimensional helical and zigzag chains (Chen & Mak, 2005), two-dimensional nets (Chen et al., 2005) as well as honeycomb-like three-dimensional frameworks (Chen et al., 2009). Herein, we report a new structure derived from di-3-pyridinylmethanone, namely {[Cu(C₁₁H₈N₂O)₂SiF₆]^.2H₂O}_n.

In the title complex, the Cu^II atom adopts an N4F2-octahedral coordination geometry with four pyridyl N atoms at the equatorial sites and two F atoms at the axial sites (Fig. 1). The di-3-pyridylmethanone and hexafluorosilicate ligands act as bidentate ligands linking symmetry-related Cu^II atoms. Water molecules form hydrogen bonds with di-3-pyridylmethanone and hexafluorosilicate ligands bridging them together (Table 1). Cu²⁺ and SiF₆^2- ions are located on a twofold axis, see Fig. 2 and Fig. 3. The structure of the title complex is remarkable different from a similar complex [(CuL₂)(BF₄)₂]_n (L = di-3-pyridylmethanone, Chen et al. 2005), where the Cu^II adopts a square-plane N4-geometry with four ligands around the metal center, forming a (4,4) net structure.

Related literature top

For background to the coordination chemistry of pyridyl-based derivatives, see: Manriquez et al. (1991); Wang et al. (2009). For dipyridylmethanone, see: Boudalis et al. (2003). For transition metal complexes of di-3-pyridylmethanone, see: Chen et al. (2005, 2009); Chen & Mak (2005).

Experimental top

The ligand was obtained according to the reported procedure (Chen & Mak, 2005). The Cu(BF₄^-)₂^.6H₂O (35 mg, 0.1 mmol) and di-3-pyridylmethanone (38 mg, 0.2 mmol) were dissolved in a mixed solvent of 1ml methanol and 3 ml acetonitrile with stirring at room temperature. The (NH₄)₂SiF₆ (18 mg, 0.1 mmol) was subsequently added to the solution. After 4 hours, the resulted clear solution was filtered and the filtrate was left to stay in air. The block crystals suitable for x-ray diffraction analysis were obtained after about one weak (29.9 mg, 49% yield).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: APEX2 and SAINT (Bruker, 2007); data reduction: SAINT (Bruker 2007); 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) and PLATON (Spek, 2009).

Figures top

	Fig. 1. The title complex showing the atom-numbering scheme, with displacement ellipsoids shown at the 30% probability level. Hydrogen atoms are omitted for clarity. Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+1, y, -z+0.5; (iii) x, -y+1, z-0.5; (iv) x, y+1, z.
	Fig. 2. Lateral view of the two-dimensional framework in the bc plane of the title complex.The O atoms of lattice water are shown as red ball mode. All H atoms except water H atoms are omitted for clarity. The Si—F are shown in a thick bond mode. The red dashed lines represent H-bonding interactions.
	Fig. 3. The packing diagram of the title complex.

Poly[[(µ₂-di-3-pyridylmethanone-κ²N:N')(µ₂- hexafluorosilicato-κ²F:F')copper(II)] dihydrate] top

Crystal data top

[Cu(SiF₆)(C₁₁H₈N₂O)₂]·2H₂O	F(000) = 1236
M_r = 610.05	D_x = 1.720 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 245 reflections
a = 22.276 (3) Å	θ = 2.2–26.1°
b = 8.0625 (11) Å	µ = 1.07 mm⁻¹
c = 15.773 (2) Å	T = 296 K
β = 123.757 (2)°	Block, blue
V = 2355.2 (5) Å³	0.40 × 0.32 × 0.30 mm
Z = 4

Data collection top

Bruker SMART APEXII CCD area-detector' diffractometer	2082 independent reflections
Radiation source: fine-focus sealed tube	1822 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.031
ω scans	θ_max = 25.0°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −22→26
T_min = 0.742, T_max = 1.000	k = −8→9
6195 measured reflections	l = −18→16

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)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.094	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.0499P)² + 3.641P] P = (F_o² + 2F_c²)/3
2082 reflections	(Δ/σ)_max < 0.001
174 parameters	Δρ_max = 0.54 e Å⁻³
0 restraints	Δρ_min = −0.31 e Å⁻³

Crystal data top

[Cu(SiF₆)(C₁₁H₈N₂O)₂]·2H₂O	V = 2355.2 (5) Å³
M_r = 610.05	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 22.276 (3) Å	µ = 1.07 mm⁻¹
b = 8.0625 (11) Å	T = 296 K
c = 15.773 (2) Å	0.40 × 0.32 × 0.30 mm
β = 123.757 (2)°

Data collection top

Bruker SMART APEXII CCD area-detector' diffractometer	2082 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	1822 reflections with I > 2σ(I)
T_min = 0.742, T_max = 1.000	R_int = 0.031
6195 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.034	0 restraints
wR(F²) = 0.094	H-atom parameters constrained
S = 1.02	Δρ_max = 0.54 e Å⁻³
2082 reflections	Δρ_min = −0.31 e Å⁻³
174 parameters

Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 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
Cu1	0.5000	0.74249 (4)	0.2500	0.02213 (16)
F1	0.41305 (11)	0.2547 (2)	0.15265 (16)	0.0656 (6)
F2	0.5000	0.4646 (2)	0.2500	0.0430 (6)
F3	0.52519 (13)	0.25362 (17)	0.16853 (16)	0.0567 (6)
F4	0.5000	0.0403 (2)	0.2500	0.0423 (5)
O1	0.71275 (11)	0.6013 (2)	0.74098 (13)	0.0495 (5)
N1	0.55932 (11)	0.2545 (2)	0.68811 (15)	0.0247 (4)
N2	0.59150 (11)	0.7466 (2)	0.39361 (16)	0.0255 (4)
C1	0.55661 (14)	0.1248 (3)	0.63175 (18)	0.0317 (5)
H1	0.5344	0.0272	0.6319	0.038*
C2	0.58540 (15)	0.1321 (3)	0.5744 (2)	0.0379 (6)
H2	0.5820	0.0409	0.5359	0.045*
C3	0.61944 (15)	0.2748 (3)	0.5736 (2)	0.0357 (6)
H3	0.6373	0.2834	0.5326	0.043*
C4	0.62620 (12)	0.4052 (3)	0.63604 (16)	0.0267 (5)
C5	0.59552 (12)	0.3905 (3)	0.69197 (17)	0.0260 (5)
H5	0.6002	0.4781	0.7336	0.031*
C7	0.66029 (13)	0.6594 (3)	0.56799 (17)	0.0271 (5)
C8	0.70977 (14)	0.7864 (3)	0.59181 (19)	0.0337 (6)
H8	0.7493	0.8005	0.6585	0.040*
C9	0.69953 (14)	0.8907 (3)	0.51563 (19)	0.0369 (6)
H9	0.7322	0.9753	0.5299	0.044*
C10	0.63992 (13)	0.8673 (3)	0.41792 (18)	0.0309 (5)
H10	0.6330	0.9382	0.3667	0.037*
C11	0.60197 (13)	0.6426 (3)	0.46786 (17)	0.0270 (5)
H11	0.5691	0.5573	0.4513	0.032*
C6	0.66989 (13)	0.5574 (3)	0.65383 (17)	0.0310 (5)
Si1	0.5000	0.25199 (9)	0.2500	0.0252 (2)
O1W	0.2808 (2)	0.1657 (6)	0.1183 (4)	0.168 (2)
H1A	0.2777	0.2089	0.1676	0.252*
H1B	0.3244	0.1856	0.1308	0.252*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0264 (2)	0.0224 (2)	0.0210 (2)	0.000	0.01529 (19)	0.000
F1	0.0410 (11)	0.0637 (13)	0.0584 (13)	−0.0046 (8)	0.0067 (10)	0.0081 (8)
F2	0.0645 (15)	0.0182 (9)	0.0684 (15)	0.000	0.0506 (13)	0.000
F3	0.1013 (17)	0.0365 (9)	0.0722 (13)	−0.0090 (8)	0.0731 (13)	−0.0082 (7)
F4	0.0658 (15)	0.0203 (9)	0.0571 (14)	0.000	0.0442 (13)	0.000
O1	0.0502 (12)	0.0604 (13)	0.0247 (10)	−0.0200 (10)	0.0126 (9)	−0.0002 (8)
N1	0.0289 (11)	0.0259 (10)	0.0233 (10)	0.0010 (7)	0.0171 (9)	0.0014 (7)
N2	0.0282 (11)	0.0240 (10)	0.0259 (10)	−0.0003 (7)	0.0160 (9)	0.0008 (7)
C1	0.0396 (14)	0.0261 (12)	0.0355 (13)	−0.0020 (10)	0.0247 (11)	−0.0023 (10)
C2	0.0507 (16)	0.0341 (13)	0.0412 (14)	−0.0035 (11)	0.0332 (13)	−0.0097 (11)
C3	0.0418 (15)	0.0406 (14)	0.0334 (14)	−0.0016 (11)	0.0264 (12)	−0.0009 (11)
C4	0.0251 (12)	0.0301 (12)	0.0221 (11)	0.0032 (9)	0.0114 (10)	0.0056 (9)
C5	0.0276 (12)	0.0264 (11)	0.0235 (11)	0.0023 (9)	0.0139 (10)	0.0010 (9)
C7	0.0287 (12)	0.0284 (11)	0.0267 (11)	−0.0012 (9)	0.0170 (10)	0.0005 (9)
C8	0.0305 (13)	0.0378 (13)	0.0284 (13)	−0.0090 (11)	0.0136 (11)	−0.0047 (10)
C9	0.0386 (14)	0.0338 (13)	0.0400 (14)	−0.0112 (11)	0.0229 (12)	−0.0023 (11)
C10	0.0372 (13)	0.0271 (11)	0.0339 (12)	−0.0031 (10)	0.0232 (11)	0.0017 (10)
C11	0.0296 (12)	0.0256 (11)	0.0278 (12)	−0.0027 (9)	0.0172 (10)	0.0010 (9)
C6	0.0284 (12)	0.0372 (13)	0.0267 (12)	−0.0014 (10)	0.0149 (11)	0.0021 (10)
Si1	0.0328 (5)	0.0179 (5)	0.0280 (5)	0.000	0.0188 (4)	0.000
O1W	0.105 (3)	0.176 (4)	0.257 (5)	−0.047 (3)	0.121 (4)	−0.145 (4)

Geometric parameters (Å, º) top

Cu1—N1ⁱ	2.033 (2)	C2—H2	0.9300
Cu1—N1ⁱⁱ	2.033 (2)	C3—C4	1.390 (3)
Cu1—N2	2.038 (2)	C3—H3	0.9300
Cu1—N2ⁱⁱⁱ	2.038 (2)	C4—C5	1.389 (3)
Cu1—F2	2.241 (2)	C4—C6	1.493 (3)
Cu1—F4^iv	2.401 (2)	C5—H5	0.9300
F1—Si1	1.6747 (19)	C7—C11	1.386 (3)
F2—Si1	1.714 (2)	C7—C8	1.394 (3)
F3—Si1	1.6636 (17)	C7—C6	1.494 (3)
F4—Si1	1.707 (2)	C8—C9	1.378 (4)
F4—Cu1^v	2.401 (2)	C8—H8	0.9300
O1—C6	1.212 (3)	C9—C10	1.378 (4)
N1—C5	1.342 (3)	C9—H9	0.9300
N1—C1	1.352 (3)	C10—H10	0.9300
N1—Cu1ⁱⁱ	2.033 (2)	C11—H11	0.9300
N2—C10	1.341 (3)	Si1—F3ⁱⁱⁱ	1.6636 (17)
N2—C11	1.351 (3)	Si1—F1ⁱⁱⁱ	1.6747 (19)
C1—C2	1.371 (4)	O1W—H1A	0.8900
C1—H1	0.9300	O1W—H1B	0.8901
C2—C3	1.382 (4)

N1ⁱ—Cu1—N1ⁱⁱ	178.65 (9)	N1—C5—H5	118.8
N1ⁱ—Cu1—N2	91.03 (8)	C4—C5—H5	118.8
N1ⁱⁱ—Cu1—N2	88.95 (8)	C11—C7—C8	118.6 (2)
N1ⁱ—Cu1—N2ⁱⁱⁱ	88.95 (8)	C11—C7—C6	123.4 (2)
N1ⁱⁱ—Cu1—N2ⁱⁱⁱ	91.03 (8)	C8—C7—C6	117.8 (2)
N2—Cu1—N2ⁱⁱⁱ	178.15 (9)	C9—C8—C7	119.4 (2)
N1ⁱ—Cu1—F2	90.68 (5)	C9—C8—H8	120.3
N1ⁱⁱ—Cu1—F2	90.68 (5)	C7—C8—H8	120.3
N2—Cu1—F2	90.93 (5)	C8—C9—C10	118.8 (2)
N2ⁱⁱⁱ—Cu1—F2	90.93 (5)	C8—C9—H9	120.6
N1ⁱ—Cu1—F4^iv	89.32 (5)	C10—C9—H9	120.6
N1ⁱⁱ—Cu1—F4^iv	89.32 (5)	N2—C10—C9	122.8 (2)
N2—Cu1—F4^iv	89.07 (5)	N2—C10—H10	118.6
N2ⁱⁱⁱ—Cu1—F4^iv	89.07 (5)	C9—C10—H10	118.6
F2—Cu1—F4^iv	180.0	N2—C11—C7	121.9 (2)
Si1—F2—Cu1	180.000 (1)	N2—C11—H11	119.1
Si1—F4—Cu1^v	180.000 (1)	C7—C11—H11	119.1
C5—N1—C1	117.9 (2)	O1—C6—C4	118.3 (2)
C5—N1—Cu1ⁱⁱ	120.21 (15)	O1—C6—C7	119.5 (2)
C1—N1—Cu1ⁱⁱ	121.42 (16)	C4—C6—C7	122.1 (2)
C10—N2—C11	118.6 (2)	F3—Si1—F3ⁱⁱⁱ	179.09 (11)
C10—N2—Cu1	118.57 (16)	F3—Si1—F1ⁱⁱⁱ	89.62 (12)
C11—N2—Cu1	122.52 (15)	F3ⁱⁱⁱ—Si1—F1ⁱⁱⁱ	90.36 (12)
N1—C1—C2	122.3 (2)	F3—Si1—F1	90.36 (12)
N1—C1—H1	118.8	F3ⁱⁱⁱ—Si1—F1	89.62 (12)
C2—C1—H1	118.8	F1ⁱⁱⁱ—Si1—F1	178.52 (13)
C1—C2—C3	120.2 (2)	F3—Si1—F4	90.45 (5)
C1—C2—H2	119.9	F3ⁱⁱⁱ—Si1—F4	90.45 (5)
C3—C2—H2	119.9	F1ⁱⁱⁱ—Si1—F4	90.74 (6)
C2—C3—C4	117.8 (2)	F1—Si1—F4	90.74 (6)
C2—C3—H3	121.1	F3—Si1—F2	89.55 (5)
C4—C3—H3	121.1	F3ⁱⁱⁱ—Si1—F2	89.55 (5)
C5—C4—C3	119.2 (2)	F1ⁱⁱⁱ—Si1—F2	89.26 (6)
C5—C4—C6	116.8 (2)	F1—Si1—F2	89.26 (6)
C3—C4—C6	123.9 (2)	F4—Si1—F2	180.0
N1—C5—C4	122.4 (2)	H1A—O1W—H1B	109.8

N1ⁱ—Cu1—N2—C10	54.16 (18)	C11—C7—C8—C9	−0.2 (4)
N1ⁱⁱ—Cu1—N2—C10	−124.49 (18)	C6—C7—C8—C9	−175.2 (2)
F2—Cu1—N2—C10	144.85 (17)	C7—C8—C9—C10	0.7 (4)
F4^iv—Cu1—N2—C10	−35.15 (17)	C11—N2—C10—C9	−0.6 (4)
N1ⁱ—Cu1—N2—C11	−132.42 (18)	Cu1—N2—C10—C9	173.0 (2)
N1ⁱⁱ—Cu1—N2—C11	48.93 (18)	C8—C9—C10—N2	−0.3 (4)
F2—Cu1—N2—C11	−41.73 (17)	C10—N2—C11—C7	1.2 (3)
F4^iv—Cu1—N2—C11	138.27 (17)	Cu1—N2—C11—C7	−172.22 (17)
C5—N1—C1—C2	−4.1 (4)	C8—C7—C11—N2	−0.8 (4)
Cu1ⁱⁱ—N1—C1—C2	167.9 (2)	C6—C7—C11—N2	173.9 (2)
N1—C1—C2—C3	0.8 (4)	C5—C4—C6—O1	45.3 (3)
C1—C2—C3—C4	3.0 (4)	C3—C4—C6—O1	−129.8 (3)
C2—C3—C4—C5	−3.4 (4)	C5—C4—C6—C7	−132.4 (2)
C2—C3—C4—C6	171.6 (2)	C3—C4—C6—C7	52.6 (3)
C1—N1—C5—C4	3.7 (3)	C11—C7—C6—O1	−164.2 (2)
Cu1ⁱⁱ—N1—C5—C4	−168.43 (17)	C8—C7—C6—O1	10.6 (4)
C3—C4—C5—N1	0.0 (3)	C11—C7—C6—C4	13.4 (4)
C6—C4—C5—N1	−175.3 (2)	C8—C7—C6—C4	−171.8 (2)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1B···F1	0.89	1.89	2.777 (6)	173
O1W—H1A···O1ⁱⁱ	0.89	2.03	2.850 (3)	153

Symmetry code: (ii) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Cu(SiF₆)(C₁₁H₈N₂O)₂]·2H₂O
M_r	610.05
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	296
a, b, c (Å)	22.276 (3), 8.0625 (11), 15.773 (2)
β (°)	123.757 (2)
V (Å³)	2355.2 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.07
Crystal size (mm)	0.40 × 0.32 × 0.30

Data collection
Diffractometer	Bruker SMART APEXII CCD area-detector' diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.742, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	6195, 2082, 1822
R_int	0.031
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.034, 0.094, 1.02
No. of reflections	2082
No. of parameters	174
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.54, −0.31

Computer programs: APEX2 (Bruker, 2007), APEX2 and SAINT (Bruker, 2007), SAINT (Bruker 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1B···F1	0.89	1.89	2.777 (6)	173
O1W—H1A···O1ⁱ	0.89	2.03	2.850 (3)	153

Symmetry code: (i) −x+1, −y+1, −z+1.

Acknowledgements

The author is grateful for financial support from the Beijing Municipal Education Commission.

References

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