Poly[diaqua-bis-(μ(3)-1H-imidazole-4,5-dicarboxyl-ato)(μ(2)-sulfato)-diytterbium(III)].

In the title compound, [Yb(2)(C(5)H(2)N(2)O(4))(2)(SO(4))(H(2)O)(2)](n), the Yb(III) ion is eight-coordinated by four O atoms and one N atom from three imidazole-4,5-dicarboxyl-ate ligands, two O atoms from one SO(4) (2-) anion (site symmetry 2), as well as one O atom of a water mol-ecule, giving a bicapped trigonal-prismatic coordination geometry. The metal coordination units are connected by bridging imidazole-4,5-dicarboxyl-ate and sulfate ligands, generating a heterometallic layer. The layers are stacked along the a axis via N-H⋯O, O-H⋯O, and C-H⋯O hydrogen-bonding inter-actions, generating a three-dimensional framework.

Related literature

For the application of multifunctional organic ligands containing O- and N-donors in the design of metal-organic frameworks, see: Cheng et al. (2006 ▶); Kuang et al. (2007 ▶); Sun et al. (2006 ▶); Zhu et al. (2010 ▶).

Experimental

Crystal data

[Yb2(C5H2N2O4)2(SO4)(H2O)2]

M = 786.35

Monoclinic,

a = 21.1089 (14) Å

b = 6.5584 (4) Å

c = 12.8766 (9) Å

β = 105.874 (1)°

V = 1714.7 (2) Å3

Z = 4

Mo Kα radiation

μ = 11.05 mm−1

T = 296 K

0.20 × 0.18 × 0.15 mm

Data collection

Bruker APEXII area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.126, T max = 0.191

4239 measured reflections

1534 independent reflections

1392 reflections with I > 2σ(I)

R int = 0.023

Refinement

R[F 2 > 2σ(F 2)] = 0.020

wR(F 2) = 0.047

S = 1.09

1534 reflections

150 parameters

4 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.66 e Å−3

Δρmin = −0.99 e Å−3

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.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811045673/pv2472sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811045673/pv2472Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Yb2(C5H2N2O4)2(SO4)(H2O)2]	F(000) = 1456
Mr = 786.35	Dx = 3.046 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2574 reflections
a = 21.1089 (14) Å	θ = 3.3–28.0°
b = 6.5584 (4) Å	µ = 11.05 mm−1
c = 12.8766 (9) Å	T = 296 K
β = 105.874 (1)°	Block, colorless
V = 1714.7 (2) Å3	0.20 × 0.18 × 0.15 mm
Z = 4

Bruker APEXII area-detector diffractometer	1534 independent reflections
Radiation source: fine-focus sealed tube	1392 reflections with I > 2σ(I)
graphite	Rint = 0.023
φ and ω scan	θmax = 25.2°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −25→22
Tmin = 0.126, Tmax = 0.191	k = −7→7
4239 measured reflections	l = −14→15

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) = 0.047	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ2(Fo2) + (0.0216P)2 + 5.6648P] where P = (Fo2 + 2Fc2)/3
1534 reflections	(Δ/σ)max = 0.001
150 parameters	Δρmax = 0.66 e Å−3
4 restraints	Δρmin = −0.99 e Å−3

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.

	x	y	z	Uiso*/Ueq
Yb1	0.355312 (10)	0.07841 (3)	0.714967 (16)	0.01086 (9)
S1	0.5000	0.0299 (3)	0.7500	0.0182 (4)
C1	0.3390 (2)	0.0272 (7)	0.9554 (4)	0.0134 (10)
C2	0.3697 (2)	0.2318 (7)	0.9654 (4)	0.0148 (10)
C3	0.3764 (2)	0.3838 (7)	1.0402 (4)	0.0145 (10)
C4	0.3492 (2)	0.4128 (7)	1.1340 (4)	0.0128 (10)
C5	0.4168 (2)	0.4805 (8)	0.9077 (4)	0.0179 (11)
H5	0.4371	0.5603	0.8664	0.022*
N1	0.3942 (2)	0.2930 (6)	0.8817 (3)	0.0165 (9)
N2	0.4065 (2)	0.5391 (6)	1.0009 (3)	0.0183 (10)
H1	0.420 (3)	0.648 (6)	1.039 (4)	0.027*
O1	0.32418 (19)	−0.0583 (5)	1.0318 (3)	0.0220 (9)
O2	0.32955 (18)	−0.0546 (5)	0.8633 (3)	0.0192 (8)
O3	0.33204 (18)	0.2591 (5)	1.1767 (3)	0.0219 (8)
O4	0.34067 (19)	0.5917 (5)	1.1620 (3)	0.0219 (8)
O5	0.45816 (18)	−0.0925 (5)	0.7997 (3)	0.0304 (10)
O6	0.45308 (19)	0.1572 (6)	0.6710 (3)	0.0349 (10)
O1W	0.24374 (18)	0.1038 (6)	0.6799 (3)	0.0250 (9)
H2W	0.224 (2)	0.201 (6)	0.646 (4)	0.037*
H1W	0.221 (3)	0.075 (8)	0.720 (4)	0.037*

	U11	U22	U33	U12	U13	U23
Yb1	0.01712 (13)	0.00743 (13)	0.00944 (13)	0.00016 (8)	0.00604 (9)	0.00022 (8)
S1	0.0156 (9)	0.0145 (9)	0.0250 (10)	0.000	0.0063 (8)	0.000
C1	0.017 (2)	0.010 (2)	0.012 (3)	0.0000 (19)	0.001 (2)	0.001 (2)
C2	0.021 (2)	0.012 (3)	0.011 (2)	−0.003 (2)	0.0040 (19)	0.000 (2)
C3	0.021 (3)	0.013 (2)	0.011 (2)	0.002 (2)	0.006 (2)	0.001 (2)
C4	0.017 (2)	0.010 (3)	0.010 (2)	−0.0018 (19)	0.002 (2)	−0.0017 (19)
C5	0.025 (3)	0.015 (3)	0.015 (3)	−0.005 (2)	0.008 (2)	0.003 (2)
N1	0.024 (2)	0.012 (2)	0.016 (2)	−0.0023 (17)	0.0082 (18)	−0.0010 (17)
N2	0.027 (2)	0.014 (2)	0.016 (2)	−0.0064 (19)	0.0084 (19)	−0.0018 (18)
O1	0.042 (2)	0.0151 (19)	0.0107 (19)	−0.0090 (16)	0.0095 (17)	−0.0001 (15)
O2	0.033 (2)	0.0155 (19)	0.0110 (18)	−0.0084 (15)	0.0090 (15)	−0.0058 (15)
O3	0.037 (2)	0.0144 (19)	0.0182 (18)	0.0042 (16)	0.0134 (16)	0.0061 (16)
O4	0.039 (2)	0.0103 (19)	0.018 (2)	0.0028 (16)	0.0105 (17)	−0.0009 (14)
O5	0.021 (2)	0.030 (2)	0.041 (3)	0.0019 (16)	0.0104 (18)	0.0155 (19)
O6	0.023 (2)	0.044 (2)	0.041 (3)	0.0071 (19)	0.0135 (19)	0.027 (2)
O1W	0.024 (2)	0.023 (2)	0.031 (2)	0.0066 (17)	0.0129 (18)	0.0083 (17)

Yb1—O4i	2.264 (3)	C1—C2	1.481 (6)
Yb1—O1ii	2.272 (3)	C2—C3	1.367 (7)
Yb1—O1W	2.280 (4)	C2—N1	1.377 (6)
Yb1—O3ii	2.291 (3)	C3—N2	1.369 (6)
Yb1—O2	2.297 (3)	C3—C4	1.485 (7)
Yb1—O6	2.342 (4)	C4—O3	1.249 (6)
Yb1—O5	2.421 (4)	C4—O4	1.255 (5)
Yb1—N1	2.510 (4)	C5—N1	1.328 (6)
Yb1—S1	2.9798 (3)	C5—N2	1.334 (7)
S1—O5iii	1.464 (4)	C5—H5	0.9300
S1—O5	1.464 (4)	N2—H1	0.87 (5)
S1—O6iii	1.470 (4)	O1—Yb1iv	2.272 (3)
S1—O6	1.470 (4)	O3—Yb1iv	2.291 (3)
S1—Yb1iii	2.9798 (3)	O4—Yb1v	2.264 (3)
C1—O1	1.244 (6)	O1W—H2W	0.82 (2)
C1—O2	1.266 (6)	O1W—H1W	0.82 (6)
O4i—Yb1—O1ii	76.46 (12)	O6iii—S1—O6	110.8 (4)
O4i—Yb1—O1W	79.74 (14)	O5iii—S1—Yb1	135.09 (15)
O1ii—Yb1—O1W	78.99 (15)	O5—S1—Yb1	53.75 (14)
O4i—Yb1—O3ii	148.74 (13)	O6iii—S1—Yb1	120.86 (16)
O1ii—Yb1—O3ii	74.75 (12)	O6—S1—Yb1	50.65 (15)
O1W—Yb1—O3ii	83.05 (14)	O5iii—S1—Yb1iii	53.75 (14)
O4i—Yb1—O2	124.73 (12)	O5—S1—Yb1iii	135.09 (15)
O1ii—Yb1—O2	140.73 (13)	O6iii—S1—Yb1iii	50.65 (15)
O1W—Yb1—O2	74.07 (14)	O6—S1—Yb1iii	120.86 (16)
O3ii—Yb1—O2	74.10 (12)	Yb1—S1—Yb1iii	167.75 (7)
O4i—Yb1—O6	76.89 (14)	O1—C1—O2	122.7 (4)
O1ii—Yb1—O6	77.64 (14)	O1—C1—C2	122.6 (4)
O1W—Yb1—O6	150.11 (14)	O2—C1—C2	114.7 (4)
O3ii—Yb1—O6	108.21 (14)	C3—C2—N1	110.6 (4)
O2—Yb1—O6	135.20 (13)	C3—C2—C1	132.9 (5)
O4i—Yb1—O5	127.57 (13)	N1—C2—C1	116.5 (4)
O1ii—Yb1—O5	114.21 (14)	C2—C3—N2	104.5 (4)
O1W—Yb1—O5	150.85 (13)	C2—C3—C4	132.8 (4)
O3ii—Yb1—O5	76.28 (13)	N2—C3—C4	121.8 (4)
O2—Yb1—O5	80.58 (13)	O3—C4—O4	123.2 (5)
O6—Yb1—O5	58.02 (13)	O3—C4—C3	118.5 (4)
O4i—Yb1—N1	72.99 (13)	O4—C4—C3	118.1 (4)
O1ii—Yb1—N1	148.68 (12)	N1—C5—N2	111.0 (4)
O1W—Yb1—N1	101.95 (14)	N1—C5—H5	124.5
O3ii—Yb1—N1	136.57 (13)	N2—C5—H5	124.5
O2—Yb1—N1	66.31 (12)	C5—N1—C2	105.0 (4)
O6—Yb1—N1	88.79 (15)	C5—N1—Yb1	138.2 (3)
O5—Yb1—N1	80.25 (14)	C2—N1—Yb1	113.6 (3)
O4i—Yb1—S1	101.39 (10)	C5—N2—C3	109.0 (4)
O1ii—Yb1—S1	98.30 (10)	C5—N2—H1	130 (4)
O1W—Yb1—S1	176.78 (11)	C3—N2—H1	121 (4)
O3ii—Yb1—S1	94.59 (10)	C1—O1—Yb1iv	141.5 (3)
O2—Yb1—S1	107.44 (9)	C1—O2—Yb1	127.3 (3)
O6—Yb1—S1	29.03 (9)	C4—O3—Yb1iv	143.5 (3)
O5—Yb1—S1	29.18 (9)	C4—O4—Yb1v	164.1 (3)
N1—Yb1—S1	81.27 (10)	S1—O5—Yb1	97.06 (18)
O5iii—S1—O5	113.5 (3)	S1—O6—Yb1	100.32 (19)
O5iii—S1—O6iii	103.9 (2)	Yb1—O1W—H2W	121 (4)
O5—S1—O6iii	112.4 (2)	Yb1—O1W—H1W	128 (4)
O5iii—S1—O6	112.4 (2)	H2W—O1W—H1W	102 (3)
O5—S1—O6	103.9 (2)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H1···O6v	0.87 (5)	2.09 (3)	2.925 (6)	161 (5)
O1W—H2W···O2vi	0.82 (2)	1.94 (3)	2.693 (5)	151 (5)
O1W—H1W···O3vii	0.82 (6)	2.24 (4)	2.896 (5)	138 (5)
O1W—H1W···O4vii	0.82 (6)	2.51 (6)	3.308 (5)	167 (5)
C5—H5···O5viii	0.93	2.52	3.347 (6)	149.

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H1⋯O6i	0.87 (5)	2.09 (3)	2.925 (6)	161 (5)
O1W—H2W⋯O2ii	0.82 (2)	1.94 (3)	2.693 (5)	151 (5)
O1W—H1W⋯O3iii	0.82 (6)	2.24 (4)	2.896 (5)	138 (5)
O1W—H1W⋯O4iii	0.82 (6)	2.51 (6)	3.308 (5)	167 (5)
C5—H5⋯O5iv	0.93	2.52	3.347 (6)	149

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .