Tetra­aqua­tetra­kis­(4,4′-bipyridine dioxide-κO)terbium(III) octa­cyanidotungstate(V)

Shi, Y.-S.; Ran, M.-Q.; Chen, Y.-Y.; Yuan, A.-H.

doi:10.1107/S1600536812005004

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 3| March 2012| Page m288

doi:10.1107/S1600536812005004

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Tetraaquatetrakis(4,4′-bipyridine dioxide-κO)terbium(III) octacyanidotungstate(V)

Yu-Sheng Shi,^a Mao-Qian Ran,^a Ying-Ying Chen ^a ^* and Ai-Hua Yuan ^a

^aSchool of Biology and Chemical Engineering, Jiangsu University of Science and Technology, Zhenjiang 212003, People's Republic of China
^*Correspondence e-mail: aihuayuan@163.com

(Received 25 November 2011; accepted 5 February 2012; online 10 February 2012)

In the title compound, [Tb(C₁₀H₈N₂O₂)₄(H₂O)₄][W(CN)₈], both metal atoms are eight-coordinated. The Tb^III ion displays a dodecahedral geometry, while the W^v ion exhibits a distorted square-antiprismatic geometry. The Tb atoms are located on a special position of site symmetry -4, whereas the W atoms are located on a twofold rotation axis. The cations are linked by O—H⋯O hydrogen bonds. The title compound is isotypic with the corresponding and previously described Mo compound [Qian & Yuan (2011 ). Acta Cryst. E67, m845].

Related literature

For general background to octacyanometallate-based compounds, see: Sieklucka et al. (2011 ); Zhou et al. (2010 ). For related structures, see: Qian & Yuan (2011). For the preparation of the title compound, see: Bok et al. (1975 ).

Experimental

Crystal data

[Tb(C₁₀H₈N₂O₂)₄(H₂O)₄][W(CN)₈]
M_r = 1375.73
Tetragonal, P 4/n
a = 17.9222 (7) Å
c = 7.8915 (6) Å
V = 2534.8 (2) Å³
Z = 2
Mo Kα radiation
μ = 3.73 mm⁻¹
T = 291 K
0.26 × 0.23 × 0.20 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004 ) T_min = 0.444, T_max = 0.522
19073 measured reflections
2498 independent reflections
2299 reflections with I > 2σ(I)
R_int = 0.032

Refinement

R[F² > 2σ(F²)] = 0.014
wR(F²) = 0.037
S = 1.07
2498 reflections
177 parameters
H-atom parameters constrained
Δρ_max = 0.30 e Å⁻³
Δρ_min = −0.64 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1B⋯O3ⁱ	0.87	1.81	2.6695 (18)	167
O1—H1A⋯O3ⁱⁱ	0.88	1.89	2.7415 (18)	165
Symmetry codes: (i) $[y, -x+{\script{3\over 2}}, z-1]$ ; (ii) $[x-{\script{1\over 2}}, y+{\script{1\over 2}}, -z+1]$ .

Data collection: SMART (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: DIAMOND (Brandenburg, 2006 ); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812005004/bx2386sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812005004/bx2386Isup2.hkl

checkCIF report

Comment top

In the past few years, a considerable effort on crystal engineering has been devoted to the design and construction of octacyanometallates [M(CN)₈]^3-/4- (M = Mo, W)-based magnets (Sieklucka et al., 2011). The combination of [M(CN)₈]^3- as a carrier of unpaired spin with transition- or lanthanide-metal cations has produced various dimensional molecular structures, and further displayed intriguing magnetic properties (Zhou et al., 2010). Recently, we have used [W(CN)₈]^3- as the building block to react with Tb³⁺ and 4,4'-bipyridine dioxide (4,4'-dpdo), obtaining a new ionic compound, [Tb(4,4'-dpdo)₄(H₂O)₄][W(CN)₈], which is isomorphous to [Tb(4,4'-dpdo)₄(H₂O)₄][Mo(CN)₈] reported previously by our group (Qian & Yuan, 2011).

In the structure, each Tb atom is located on a special position of site symmetry 4, whereas each Mo atom is located on a twofold rotation axis. The W^v exhibits a distorted square antiprism, while the Tb^III center displays an eight-coordinated decahedron geometry with 2.386 Å of the mean Tb—O bond length. The average W—C and C—N distances are 2.174 and 1.158 Å, respectively, while the W—CN bond angles are nearly linear with a maximum deviation from linearity of 4.0°. The neighboring cations are linked through O—H···O hydrogen bonds, Table 1.

Related literature top

For general background to octacyanometallate-based compounds, see: Sieklucka et al. (2011); Zhou et al. (2010). For related structures, see: Qian et al. (2011). For the preparation of the title compound, see: Bok et al., (1975).

Experimental top

Single crystals of the title compound were prepared at room temperature in the dark by slow diffusion of a H₂O solution (3 ml) containing Tb(NO₃)₃.6H₂O (0.05 mmol) and 4,4'-dpdo (0.05 mmol) into a CH₃CN solution (15 ml) of [HN(n-C₄H₉)₃]₃[W(CN)₈].4H₂O (0.05 mmol) (Bok et al., 1975). After two weeks, yellow block crystals were obtained.

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SMART (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: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. ORTEP diagram of the title compound. Hydrogen atoms have been omitted for clarity and thermal ellipsoids are presented at the 30% probability level. Symmetry codes: (i) -x + 3/2, -y + 3/2, z; (ii) -y + 3/2, x, z; (iii) y, -x + 3/2, z; (iv) y - 1/2, -x + 1, -z + 1; (v) -y + 1, x + 1/2, -z + 1; (vi) -x + 1/2, -y + 3/2, z.

Tetraaquatetrakis(4,4'-bipyridine dioxide-κO)terbium(III) octacyanidotungstate(V) top

Crystal data top

[Tb(C₁₀H₈N₂O₂)₄(H₂O)₄][W(CN)₈]	D_x = 1.802 Mg m⁻³
M_r = 1375.73	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/n	Cell parameters from 9955 reflections
Hall symbol: -P 4a	θ = 2.3–27.5°
a = 17.9222 (7) Å	µ = 3.73 mm⁻¹
c = 7.8915 (6) Å	T = 291 K
V = 2534.8 (2) Å³	Block, yellow
Z = 2	0.26 × 0.23 × 0.20 mm
F(000) = 1350

Data collection top

Bruker SMART APEX CCD diffractometer	2498 independent reflections
Radiation source: fine-focus sealed tube	2299 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.032
ϕ and ω scans	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −22→22
T_min = 0.444, T_max = 0.522	k = −22→22
19073 measured reflections	l = −9→9

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)] = 0.014	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.037	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0164P)² + 1.703P] where P = (F_o² + 2F_c²)/3
2498 reflections	(Δ/σ)_max = 0.001
177 parameters	Δρ_max = 0.30 e Å⁻³
0 restraints	Δρ_min = −0.64 e Å⁻³

Crystal data top

[Tb(C₁₀H₈N₂O₂)₄(H₂O)₄][W(CN)₈]	Z = 2
M_r = 1375.73	Mo Kα radiation
Tetragonal, P4/n	µ = 3.73 mm⁻¹
a = 17.9222 (7) Å	T = 291 K
c = 7.8915 (6) Å	0.26 × 0.23 × 0.20 mm
V = 2534.8 (2) Å³

Data collection top

Bruker SMART APEX CCD diffractometer	2498 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2004)	2299 reflections with I > 2σ(I)
T_min = 0.444, T_max = 0.522	R_int = 0.032
19073 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.014	0 restraints
wR(F²) = 0.037	H-atom parameters constrained
S = 1.07	Δρ_max = 0.30 e Å⁻³
2498 reflections	Δρ_min = −0.64 e Å⁻³
177 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
W1	0.7500	0.7500	0.24882 (2)	0.01913 (5)
Tb1	0.2500	0.7500	0.5000	0.01051 (5)
O1	0.29389 (7)	0.81662 (7)	0.25409 (15)	0.0171 (3)
H1B	0.3287	0.8015	0.1848	0.021*
H1A	0.2637	0.8394	0.1839	0.021*
N1	0.68065 (11)	0.89541 (11)	0.0386 (3)	0.0393 (5)
C1	0.70418 (11)	0.84317 (11)	0.1061 (3)	0.0284 (5)
O2	0.35045 (7)	0.67744 (8)	0.39890 (16)	0.0239 (3)
N2	0.59625 (11)	0.79552 (11)	0.4621 (3)	0.0374 (5)
C2	0.65117 (11)	0.78032 (11)	0.3929 (3)	0.0278 (4)
O3	0.72018 (7)	0.38740 (8)	1.00441 (16)	0.0212 (3)
N3	0.39907 (9)	0.63844 (9)	0.49170 (19)	0.0194 (3)
C7	0.46983 (11)	0.66305 (11)	0.5066 (3)	0.0248 (4)
H7	0.4843	0.7066	0.4515	0.030*
C6	0.52093 (11)	0.62425 (11)	0.6029 (3)	0.0234 (4)
H6	0.5695	0.6420	0.6125	0.028*
C5	0.50060 (10)	0.55836 (10)	0.6866 (2)	0.0171 (4)
C4	0.42720 (10)	0.53429 (11)	0.6643 (2)	0.0200 (4)
H4	0.4114	0.4903	0.7157	0.024*
C3	0.37781 (11)	0.57476 (11)	0.5672 (2)	0.0226 (4)
H3	0.3291	0.5578	0.5538	0.027*
C8	0.55622 (10)	0.51442 (10)	0.7837 (2)	0.0158 (4)
C12	0.62818 (10)	0.54238 (10)	0.8120 (2)	0.0194 (4)
H12	0.6399	0.5906	0.7774	0.023*
C11	0.68155 (10)	0.49949 (10)	0.8903 (2)	0.0202 (4)
H11	0.7290	0.5189	0.9089	0.024*
N4	0.66553 (8)	0.42914 (8)	0.94064 (19)	0.0163 (3)
C10	0.59602 (10)	0.40097 (10)	0.9223 (2)	0.0178 (4)
H10	0.5854	0.3532	0.9613	0.021*
C9	0.54087 (10)	0.44284 (10)	0.8461 (2)	0.0171 (4)
H9	0.4930	0.4234	0.8360	0.021*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
W1	0.01293 (6)	0.01293 (6)	0.03153 (10)	0.000	0.000	0.000
Tb1	0.01091 (6)	0.01091 (6)	0.00970 (8)	0.000	0.000	0.000
O1	0.0165 (6)	0.0216 (7)	0.0134 (6)	0.0015 (5)	0.0022 (5)	0.0030 (5)
N1	0.0269 (10)	0.0294 (10)	0.0617 (14)	−0.0036 (8)	−0.0126 (9)	0.0106 (10)
C1	0.0180 (10)	0.0236 (10)	0.0435 (12)	−0.0035 (8)	−0.0054 (9)	0.0016 (10)
O2	0.0219 (7)	0.0334 (8)	0.0165 (6)	0.0156 (6)	−0.0023 (5)	0.0007 (6)
N2	0.0276 (10)	0.0317 (10)	0.0528 (12)	−0.0001 (8)	0.0092 (9)	−0.0084 (9)
C2	0.0233 (10)	0.0178 (9)	0.0422 (12)	−0.0016 (8)	0.0001 (9)	−0.0039 (9)
O3	0.0184 (7)	0.0235 (7)	0.0217 (7)	0.0064 (5)	−0.0021 (5)	0.0064 (5)
N3	0.0183 (8)	0.0235 (8)	0.0163 (8)	0.0101 (7)	−0.0004 (6)	−0.0014 (6)
C7	0.0223 (10)	0.0201 (10)	0.0322 (11)	0.0039 (8)	0.0008 (8)	0.0060 (8)
C6	0.0164 (9)	0.0200 (9)	0.0337 (11)	0.0009 (7)	−0.0031 (8)	0.0037 (8)
C5	0.0190 (9)	0.0165 (9)	0.0159 (8)	0.0048 (7)	0.0009 (7)	−0.0032 (7)
C4	0.0186 (9)	0.0199 (9)	0.0216 (9)	0.0009 (7)	−0.0002 (8)	0.0014 (8)
C3	0.0171 (9)	0.0268 (10)	0.0238 (10)	0.0021 (8)	−0.0004 (8)	−0.0016 (8)
C8	0.0170 (9)	0.0166 (9)	0.0137 (8)	0.0032 (7)	0.0022 (7)	−0.0039 (7)
C12	0.0218 (9)	0.0144 (9)	0.0220 (9)	−0.0014 (7)	−0.0017 (8)	0.0015 (7)
C11	0.0182 (9)	0.0201 (9)	0.0222 (9)	−0.0031 (7)	−0.0024 (8)	0.0019 (8)
N4	0.0167 (7)	0.0188 (8)	0.0133 (7)	0.0048 (6)	−0.0001 (6)	0.0008 (6)
C10	0.0202 (9)	0.0163 (9)	0.0169 (9)	0.0004 (7)	0.0037 (7)	0.0008 (7)
C9	0.0164 (9)	0.0180 (9)	0.0170 (9)	0.0005 (7)	0.0027 (7)	−0.0013 (7)

Geometric parameters (Å, º) top

W1—C2ⁱ	2.174 (2)	N3—C3	1.343 (3)
W1—C2ⁱⁱ	2.174 (2)	N3—C7	1.348 (3)
W1—C2ⁱⁱⁱ	2.174 (2)	C7—C6	1.378 (3)
W1—C2	2.174 (2)	C7—H7	0.9300
W1—C1ⁱ	2.175 (2)	C6—C5	1.401 (3)
W1—C1ⁱⁱ	2.175 (2)	C6—H6	0.9300
W1—C1	2.175 (2)	C5—C4	1.396 (3)
W1—C1ⁱⁱⁱ	2.175 (2)	C5—C8	1.484 (3)
Tb1—O2^iv	2.3598 (13)	C4—C3	1.377 (3)
Tb1—O2^v	2.3598 (13)	C4—H4	0.9300
Tb1—O2	2.3598 (13)	C3—H3	0.9300
Tb1—O2^vi	2.3598 (13)	C8—C9	1.401 (3)
Tb1—O1^vi	2.4104 (12)	C8—C12	1.402 (3)
Tb1—O1^iv	2.4104 (12)	C12—C11	1.374 (3)
Tb1—O1	2.4104 (12)	C12—H12	0.9300
Tb1—O1^v	2.4104 (12)	C11—N4	1.353 (2)
O1—H1B	0.8724	C11—H11	0.9300
O1—H1A	0.8755	N4—C10	1.352 (2)
N1—C1	1.157 (3)	C10—C9	1.379 (3)
O2—N3	1.336 (2)	C10—H10	0.9300
N2—C2	1.158 (3)	C9—H9	0.9300
O3—N4	1.3312 (19)

C2ⁱ—W1—C2ⁱⁱ	74.13 (6)	O2^iv—Tb1—O1^v	72.77 (5)
C2ⁱ—W1—C2ⁱⁱⁱ	116.94 (12)	O2^v—Tb1—O1^v	75.63 (5)
C2ⁱⁱ—W1—C2ⁱⁱⁱ	74.13 (6)	O2—Tb1—O1^v	146.09 (4)
C2ⁱ—W1—C2	74.13 (6)	O2^vi—Tb1—O1^v	73.41 (4)
C2ⁱⁱ—W1—C2	116.94 (12)	O1^vi—Tb1—O1^v	130.40 (4)
C2ⁱⁱⁱ—W1—C2	74.13 (6)	O1^iv—Tb1—O1^v	72.76 (6)
C2ⁱ—W1—C1ⁱ	76.77 (8)	O1—Tb1—O1^v	130.40 (4)
C2ⁱⁱ—W1—C1ⁱ	143.32 (7)	Tb1—O1—H1B	125.7
C2ⁱⁱⁱ—W1—C1ⁱ	140.38 (7)	Tb1—O1—H1A	122.6
C2—W1—C1ⁱ	74.90 (8)	H1B—O1—H1A	101.0
C2ⁱ—W1—C1ⁱⁱ	74.90 (8)	N1—C1—W1	175.9 (2)
C2ⁱⁱ—W1—C1ⁱⁱ	76.77 (8)	N3—O2—Tb1	126.92 (10)
C2ⁱⁱⁱ—W1—C1ⁱⁱ	143.32 (7)	N2—C2—W1	176.3 (2)
C2—W1—C1ⁱⁱ	140.38 (7)	O2—N3—C3	120.20 (16)
C1ⁱ—W1—C1ⁱⁱ	74.45 (6)	O2—N3—C7	119.38 (16)
C2ⁱ—W1—C1	143.32 (7)	C3—N3—C7	120.42 (16)
C2ⁱⁱ—W1—C1	140.38 (7)	N3—C7—C6	120.54 (18)
C2ⁱⁱⁱ—W1—C1	74.90 (8)	N3—C7—H7	119.7
C2—W1—C1	76.77 (8)	C6—C7—H7	119.7
C1ⁱ—W1—C1	74.45 (6)	C7—C6—C5	120.81 (18)
C1ⁱⁱ—W1—C1	117.63 (12)	C7—C6—H6	119.6
C2ⁱ—W1—C1ⁱⁱⁱ	140.38 (7)	C5—C6—H6	119.6
C2ⁱⁱ—W1—C1ⁱⁱⁱ	74.90 (8)	C4—C5—C6	116.52 (17)
C2ⁱⁱⁱ—W1—C1ⁱⁱⁱ	76.77 (8)	C4—C5—C8	122.29 (17)
C2—W1—C1ⁱⁱⁱ	143.32 (7)	C6—C5—C8	121.07 (17)
C1ⁱ—W1—C1ⁱⁱⁱ	117.63 (12)	C3—C4—C5	120.87 (18)
C1ⁱⁱ—W1—C1ⁱⁱⁱ	74.45 (6)	C3—C4—H4	119.6
C1—W1—C1ⁱⁱⁱ	74.45 (6)	C5—C4—H4	119.6
O2^iv—Tb1—O2^v	140.48 (6)	N3—C3—C4	120.81 (18)
O2^iv—Tb1—O2	96.56 (2)	N3—C3—H3	119.6
O2^v—Tb1—O2	96.56 (2)	C4—C3—H3	119.6
O2^iv—Tb1—O2^vi	96.56 (2)	C9—C8—C12	116.87 (17)
O2^v—Tb1—O2^vi	96.56 (2)	C9—C8—C5	122.38 (17)
O2—Tb1—O2^vi	140.48 (6)	C12—C8—C5	120.72 (17)
O2^iv—Tb1—O1^vi	73.41 (4)	C11—C12—C8	120.82 (17)
O2^v—Tb1—O1^vi	146.09 (4)	C11—C12—H12	119.6
O2—Tb1—O1^vi	72.77 (5)	C8—C12—H12	119.6
O2^vi—Tb1—O1^vi	75.63 (5)	N4—C11—C12	120.38 (17)
O2^iv—Tb1—O1^iv	75.63 (5)	N4—C11—H11	119.8
O2^v—Tb1—O1^iv	72.77 (5)	C12—C11—H11	119.8
O2—Tb1—O1^iv	73.41 (4)	O3—N4—C10	120.56 (15)
O2^vi—Tb1—O1^iv	146.09 (4)	O3—N4—C11	118.59 (15)
O1^vi—Tb1—O1^iv	130.40 (4)	C10—N4—C11	120.83 (16)
O2^iv—Tb1—O1	146.09 (4)	N4—C10—C9	120.25 (17)
O2^v—Tb1—O1	73.41 (4)	N4—C10—H10	119.9
O2—Tb1—O1	75.63 (5)	C9—C10—H10	119.9
O2^vi—Tb1—O1	72.77 (5)	C10—C9—C8	120.71 (17)
O1^vi—Tb1—O1	72.76 (6)	C10—C9—H9	119.6
O1^iv—Tb1—O1	130.40 (4)	C8—C9—H9	119.6

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···O3^vii	0.87	1.81	2.6695 (18)	167
O1—H1A···O3^viii	0.88	1.89	2.7415 (18)	165

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

Experimental details

Crystal data
Chemical formula	[Tb(C₁₀H₈N₂O₂)₄(H₂O)₄][W(CN)₈]
M_r	1375.73
Crystal system, space group	Tetragonal, P4/n
Temperature (K)	291
a, c (Å)	17.9222 (7), 7.8915 (6)
V (Å³)	2534.8 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	3.73
Crystal size (mm)	0.26 × 0.23 × 0.20

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2004)
T_min, T_max	0.444, 0.522
No. of measured, independent and observed [I > 2σ(I)] reflections	19073, 2498, 2299
R_int	0.032
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.014, 0.037, 1.07
No. of reflections	2498
No. of parameters	177
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.30, −0.64

Computer programs: SMART (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2006), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···O3ⁱ	0.87	1.81	2.6695 (18)	166.8
O1—H1A···O3ⁱⁱ	0.88	1.89	2.7415 (18)	165.2

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

Acknowledgements

This work was supported by the Project of Undergraduate Innovative Plan of Jiangsu University of Science and Technology, and the Project of the Priority Academic Program Development of Jiangsu Higher Education Institutions.

References

Bok, L. D. C., Leipoldt, J. G. & Basson, S. S. (1975). Z. Anorg. Allg. Chem. 415, 81–83. CrossRef CAS Web of Science Google Scholar
Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2004). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Qian, S.-Y. & Yuan, A.-H. (2011). Acta Cryst. E67, m845. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sieklucka, B., Podgajny, R., Korzeniak, T., Nowicka, B., Pinkowicz, D. & Kozieł, M. (2011). Eur. J. Inorg. Chem. pp. 305–326. Web of Science CrossRef Google Scholar
Zhou, H., Yuan, A. H., Qian, S. Y., Song, Y. & Diao, G. W. (2010). Inorg. Chem. 49, 5971–5976. Web of Science CSD CrossRef CAS PubMed Google Scholar

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Volume 68| Part 3| March 2012| Page m288

doi:10.1107/S1600536812005004

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Tetra­aqua­tetra­kis­(4,4′-bi­pyridine dioxide-κO)terbium(III) octa­cyanidotungstate(V)

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Tetraaquatetrakis(4,4′-bipyridine dioxide-κO)terbium(III) octacyanidotungstate(V)