Poly[[tetra-aquadi-μ4-fumarato-μ2-oxalato-dierbium(III)] tetra-hydrate].

The title compound, {[Er2(C4H2O4)2(C2O4)(H2O)4]·4H2O} n , was synthesized by the reaction of erbium nitrate hexa-hydrate with fumaric acid and oxalic acid under hydro-thermal conditions. The Er(3+) cation (site symmetry ..2) is eight-coordinated by six O atoms from four fumarate anions (site symmetry ..2) and one bidentate oxalate anion (site symmetry 222), and by two water mol-ecules. The complex exhibits a three-dimensional structure consisting of oxalate pillared Er-fumarate layers with channels occupied by coordinating and lattice water mol-ecules. The three-dimensional structure features by Owater-H⋯O hydrogen bonds involving both the coordinating and lattice water mol-ecules.

Related literature

For lanthanide–metal complexes containing fumarate ligands, see: Zhang et al. (2006 ▶). For lanthanide-containing structures with metal-organic frameworks and two different flexible carboxyl­ate ligands, see: Zhang et al. (2008 ▶); Zhu et al. (2007 ▶).

Experimental

Crystal data

[Er2(C4H2O4)2(C2O4)(H2O)4]·4H2O

M = 794.78

Orthorhombic,

a = 9.6016 (19) Å

b = 15.701 (3) Å

c = 26.722 (5) Å

V = 4028.5 (14) Å3

Z = 8

Mo Kα radiation

μ = 8.38 mm−1

T = 293 K

0.19 × 0.16 × 0.13 mm

Data collection

Bruker SMART APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.305, T max = 0.402

9284 measured reflections

1162 independent reflections

1088 reflections with I > 2σ(I)

R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.018

wR(F 2) = 0.045

S = 1.11

1162 reflections

74 parameters

H-atom parameters constrained

Δρmax = 0.51 e Å−3

Δρmin = −1.04 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: 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: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S160053681205026X/hg5272sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681205026X/hg5272Isup2.hkl

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

[Er2(C4H2O4)2(C2O4)(H2O)4]·4H2O	Dx = 2.621 Mg m−3
Mr = 794.78	Melting point: not measured K
Orthorhombic, Fddd	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -F 2uv 2vw	Cell parameters from 9875 reflections
a = 9.6016 (19) Å	θ = 3.0–27.5°
b = 15.701 (3) Å	µ = 8.38 mm−1
c = 26.722 (5) Å	T = 293 K
V = 4028.5 (14) Å3	Block, pink
Z = 8	0.19 × 0.16 × 0.13 mm
F(000) = 3008

Bruker SMART APEX CCD diffractometer	1162 independent reflections
Radiation source: fine-focus sealed tube	1088 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.022
Detector resolution: 9.00cm pixels mm-1	θmax = 27.5°, θmin = 3.0°
ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Bruker, 2001)	k = −20→20
Tmin = 0.305, Tmax = 0.402	l = −34→31
9284 measured reflections

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)] = 0.018	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.045	H-atom parameters constrained
S = 1.11	w = 1/[σ2(Fo2) + (0.0186P)2 + 60.2587P] where P = (Fo2 + 2Fc2)/3
1162 reflections	(Δ/σ)max = 0.003
74 parameters	Δρmax = 0.51 e Å−3
0 restraints	Δρmin = −1.04 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
C1	0.9358 (4)	0.1660 (2)	0.52974 (13)	0.0167 (6)
C2	1.0906 (4)	0.1604 (3)	0.53278 (16)	0.0268 (8)
H2	1.1407	0.2110	0.5348	0.032*
C3	0.6250	0.0756 (3)	0.6250	0.0150 (8)
Er1	0.6250	0.1250	0.508677 (7)	0.01528 (8)
O1	0.8868 (3)	0.23742 (16)	0.51740 (10)	0.0237 (5)
O2	0.8597 (3)	0.10210 (16)	0.53731 (11)	0.0239 (5)
O3	0.6164 (3)	0.04009 (15)	0.58332 (9)	0.0190 (5)
O4	0.4757 (3)	0.12267 (15)	0.43533 (9)	0.0256 (5)
H4A	0.3985	0.1447	0.4440	0.031*
H4B	0.4595	0.0706	0.4288	0.031*
O5	0.5533 (3)	0.20049 (15)	0.34370 (9)	0.0859 (16)
H5A	0.5298	0.1769	0.3711	0.103*
H5B	0.5661	0.2534	0.3485	0.129*

	U11	U22	U33	U12	U13	U23
C1	0.0141 (15)	0.0186 (16)	0.0173 (16)	0.0032 (13)	−0.0010 (13)	0.0001 (13)
C2	0.0159 (17)	0.0232 (18)	0.041 (2)	−0.0021 (14)	0.0015 (15)	−0.0025 (17)
C3	0.0133 (19)	0.013 (2)	0.019 (2)	0.000	−0.0012 (19)	0.000
Er1	0.01765 (12)	0.01422 (11)	0.01396 (11)	0.00560 (8)	0.000	0.000
O1	0.0239 (13)	0.0200 (12)	0.0270 (13)	0.0067 (10)	0.0003 (11)	0.0045 (10)
O2	0.0168 (12)	0.0205 (12)	0.0344 (14)	0.0009 (10)	0.0001 (11)	0.0027 (11)
O3	0.0269 (13)	0.0139 (11)	0.0161 (11)	−0.0003 (10)	−0.0015 (10)	−0.0010 (9)
O4	0.0296 (13)	0.0215 (12)	0.0256 (13)	−0.0017 (11)	−0.0040 (11)	0.0002 (11)
O5	0.099 (4)	0.076 (3)	0.082 (3)	−0.011 (3)	0.012 (3)	0.037 (3)

C1—O2	1.258 (4)	Er1—O3	2.401 (2)
C1—O1	1.260 (4)	Er1—O2	2.407 (3)
C1—C2	1.491 (5)	Er1—O2iii	2.407 (3)
C2—C2i	1.294 (8)	Er1—O4	2.428 (2)
C2—H2	0.9300	Er1—O4iii	2.428 (2)
C3—O3	1.249 (3)	O1—Er1iv	2.273 (3)
C3—O3ii	1.249 (3)	O4—H4A	0.8500
C3—C3iii	1.550 (9)	O4—H4B	0.8499
Er1—O1iv	2.273 (3)	O5—H5A	0.8500
Er1—O1v	2.273 (3)	O5—H5B	0.8500
Er1—O3iii	2.401 (2)
O2—C1—O1	122.4 (3)	O3—Er1—O2iii	77.67 (9)
O2—C1—C2	121.5 (3)	O2—Er1—O2iii	142.93 (13)
O1—C1—C2	116.0 (3)	O1iv—Er1—O4	74.78 (9)
C2i—C2—C1	124.0 (5)	O1v—Er1—O4	76.55 (9)
C2i—C2—H2	118.0	O3iii—Er1—O4	134.38 (9)
C1—C2—H2	118.0	O3—Er1—O4	129.93 (8)
O3—C3—O3ii	126.9 (4)	O2—Er1—O4	143.80 (9)
O3—C3—C3iii	116.6 (2)	O2iii—Er1—O4	72.91 (9)
O3ii—C3—C3iii	116.6 (2)	O1iv—Er1—O4iii	76.55 (9)
O1iv—Er1—O1v	144.28 (13)	O1v—Er1—O4iii	74.78 (9)
O1iv—Er1—O3iii	74.25 (9)	O3iii—Er1—O4iii	129.93 (8)
O1v—Er1—O3iii	141.35 (9)	O3—Er1—O4iii	134.38 (9)
O1iv—Er1—O3	141.35 (9)	O2—Er1—O4iii	72.91 (9)
O1v—Er1—O3	74.25 (9)	O2iii—Er1—O4iii	143.80 (9)
O3iii—Er1—O3	67.62 (11)	O4—Er1—O4iii	72.38 (12)
O1iv—Er1—O2	106.62 (9)	C1—O1—Er1iv	160.8 (3)
O1v—Er1—O2	84.78 (9)	C1—O2—Er1	111.9 (2)
O3iii—Er1—O2	77.67 (9)	C3—O3—Er1	119.4 (2)
O3—Er1—O2	71.66 (9)	Er1—O4—H4A	106.7
O1iv—Er1—O2iii	84.78 (9)	Er1—O4—H4B	106.7
O1v—Er1—O2iii	106.62 (9)	H4A—O4—H4B	106.7
O3iii—Er1—O2iii	71.66 (9)	H5A—O5—H5B	109.5

D—H···A	D—H	H···A	D···A	D—H···A
O4—H4A···O5vi	0.85	2.35	3.045 (5)	139
O4—H4B···O3vii	0.85	1.91	2.750 (3)	168
O5—H5A···O4	0.85	1.99	2.836	180
O5—H5B···O2viii	0.85	2.36	2.938 (4)	125

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H4A⋯O5i	0.85	2.35	3.045 (5)	139
O4—H4B⋯O3ii	0.85	1.91	2.750 (3)	168
O5—H5A⋯O4	0.85	1.99	2.836	180
O5—H5B⋯O2iii	0.85	2.36	2.938 (4)	125

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