Poly[diaqua­(μ3-succinato)cadmium(II)]

Liu, X.-W.

doi:10.1107/S1600536809011593

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 65| Part 5| May 2009| Page m574

doi:10.1107/S1600536809011593

Open

access

Poly[diaqua(μ₃-succinato)cadmium(II)]

Xuan-Wen Liu ^a ^*

^aDepartment of Materials Science and Engineering, Northeastern University at Qinhuangdao, Qinhuangdao, Hebei 066000, People's Republic of China
^*Correspondence e-mail: liuxuanwen2009@163.com

(Received 6 March 2009; accepted 29 March 2009; online 25 April 2009)

The title compound, [Cd(C₄H₄O₄)(H₂O)₂]_n, has been synthesized under hydrothermal conditions. The asymmetric unit consists of one Cd²⁺ cation, one succinate anion and two aqua ligands. The Cd atoms present a distorted pentagonal bipyramidal coordination and are bridged into layers parallel to (201) by succinate ligands.

Related literature

For different bridging modes in succinato complexes, see: Ng (1998 ); Rastsvetaeva et al. (1996 ); Brusau et al. (2000 ); He et al. (2006 ); He et al. (2007 ). For geometrical comparisons with related compounds, see Huo et al. (2005 ); Zhuo et al. (2006 ).

Experimental

Crystal data

[Cd(C₄H₄O₄)(H₂O)₂]
M_r = 264.51
Monoclinic, P 2₁ /c
a = 7.7130 (15) Å
b = 12.231 (2) Å
c = 8.0560 (16) Å
β = 94.71 (3)°
V = 757.4 (2) Å³
Z = 4
Mo Kα radiation
μ = 2.87 mm⁻¹
T = 293 K
0.40 × 0.30 × 0.21 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1998 ) T_min = 0.35, T_max = 0.55
6371 measured reflections
1409 independent reflections
1335 reflections with I > 2σ(I)
R_int = 0.028

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.053
S = 1.05
1409 reflections
116 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.40 e Å⁻³
Δρ_min = −0.68 e Å⁻³

Table 1
Selected bond lengths (Å)

Cd1—O4ⁱ	2.255 (2)
Cd1—O2	2.284 (2)
Cd1—O6	2.302 (3)
Cd1—O4ⁱⁱ	2.316 (2)
Cd1—O5	2.329 (3)
Cd1—O1	2.389 (2)
Cd1—O3ⁱ	2.690 (2)
Symmetry codes: (i) $[x-1, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); 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.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809011593/bg2243sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809011593/bg2243Isup2.hkl

checkCIF report

Comment top

The succinate dianion has been used as a bridging ligand in the preparation of multinuclear metal complexes. A variety of bridging modes have been found (Ng,1998; Rastsvetaeva et al., 1996; Brusau et al., 2000; He et al., 2006; He et al., 2007). We report herein the synthesis and crystal stucture of a new succinate complex [Cd(C₄H₄O₄)(H₂O)₂] (I).

The asymmetric unit consists of one Cd²⁺ cation, one succinate anion and two aqua ligands (Fig. 1). The Cd atom is coordinated by seven O atoms of three succinate anions and two aqua ligand, forming a distorted pentagonal bipyramidal coordination geometry (Table 1), with Cd—O bond lengths which agree well with those observed in analogous complexes (Huo et al., 2005; Zhuo et al., 2006). Cd atoms are bridged by succinate ligands into a two-dimensional layer (Fig. 2).

Related literature top

For different bridging modes in succinato complexes, see: Ng, (1998); Rastsvetaeva et al. (1996); Brusau et al. (2000); He et al. (2006); He et al. (2007). For geometrical comparisons with related compounds, see Huo et al. (2005); Zhuo et al. (2006).

Experimental top

Cd(NO₃)₂.4H₂O (0.5 mmol, 0.154 g), succinic acid (0.5 mmol, 0.059 g), sodium hydroxide (1 mmol, 0.04 g) and water (12 ml) were placed in a 23-ml Teflon-lined Parr bomb. The bomb was heated at 453 K for 3 d. The colourless block-shapped crystals were filtered off and washed with water and acetone (yield 45%, based on Cd).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); 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. A view of the molecular structure of (I) with the atom-numbering scheme and 30% displacement ellipsoids. Atoms with the suffix A and B are generated by the symmetry operations x + 1, -y + 3/2, z + 1/2 and -x + 2, -y + 1, -z + 2, respectively.
	Fig. 2. The 2-D layer structure of compound (I) (H atoms of methylenes are omitted for clarity).

Poly[diaqua(µ₃-succinato)cadmium(II)] top

Crystal data top

[Cd(C₄H₄O₄)(H₂O)₂]	F(000) = 512.0
M_r = 264.51	D_x = 2.32 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2567 reflections
a = 7.7130 (15) Å	θ = 2.6–25.5°
b = 12.231 (2) Å	µ = 2.87 mm⁻¹
c = 8.0560 (16) Å	T = 293 K
β = 94.71 (3)°	Block, colorless
V = 757.4 (2) Å³	0.40 × 0.30 × 0.21 mm
Z = 4

Data collection top

Bruker SMART CD area-detector diffractometer	1409 independent reflections
Radiation source: fine-focus sealed tube	1335 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.028
ϕ and ω scans	θ_max = 25.5°, θ_min = 3.0°
Absorption correction: multi-scan (SADABS; Bruker, 1998)	h = −9→9
T_min = 0.35, T_max = 0.55	k = −14→14
6371 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)] = 0.023	Hydrogen site location: constr
wR(F²) = 0.053	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.0207P)² + 1.5P] where P = (F_o² + 2F_c²)/3
1409 reflections	(Δ/σ)_max < 0.001
116 parameters	Δρ_max = 0.40 e Å⁻³
6 restraints	Δρ_min = −0.68 e Å⁻³

Crystal data top

[Cd(C₄H₄O₄)(H₂O)₂]	V = 757.4 (2) Å³
M_r = 264.51	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 7.7130 (15) Å	µ = 2.87 mm⁻¹
b = 12.231 (2) Å	T = 293 K
c = 8.0560 (16) Å	0.40 × 0.30 × 0.21 mm
β = 94.71 (3)°

Data collection top

Bruker SMART CD area-detector diffractometer	1409 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 1998)	1335 reflections with I > 2σ(I)
T_min = 0.35, T_max = 0.55	R_int = 0.028
6371 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	6 restraints
wR(F²) = 0.053	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	Δρ_max = 0.40 e Å⁻³
1409 reflections	Δρ_min = −0.68 e Å⁻³
116 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
Cd1	0.17614 (3)	0.587427 (19)	0.08353 (3)	0.02570 (10)
C1	0.4820 (4)	0.6353 (3)	0.2526 (4)	0.0274 (7)
C2	0.6501 (5)	0.6626 (3)	0.3501 (6)	0.0454 (10)
H2A	0.6471	0.6327	0.4613	0.055*
H2B	0.7436	0.6262	0.2983	0.055*
C3	0.6922 (4)	0.7799 (3)	0.3648 (5)	0.0349 (9)
H3A	0.6046	0.8150	0.4262	0.042*
H3B	0.6840	0.8113	0.2538	0.042*
C4	0.8675 (4)	0.8072 (3)	0.4482 (4)	0.0252 (7)
O1	0.4603 (3)	0.5387 (2)	0.2005 (3)	0.0367 (6)
O2	0.3664 (3)	0.70570 (19)	0.2216 (3)	0.0352 (6)
O3	0.9815 (3)	0.7385 (2)	0.4838 (3)	0.0399 (6)
O4	0.8946 (3)	0.90780 (18)	0.4832 (3)	0.0307 (6)
O5	0.0710 (4)	0.5424 (2)	0.3376 (3)	0.0402 (6)
H5A	−0.012 (5)	0.499 (3)	0.325 (6)	0.072 (18)*
H5B	0.047 (5)	0.598 (2)	0.392 (5)	0.056 (15)*
O6	0.2576 (3)	0.5909 (2)	−0.1850 (3)	0.0332 (6)
H6A	0.348 (4)	0.553 (3)	−0.197 (5)	0.044 (12)*
H6B	0.278 (5)	0.6562 (17)	−0.213 (5)	0.051 (13)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.01635 (14)	0.02632 (15)	0.03318 (16)	−0.00248 (9)	−0.00550 (10)	−0.00305 (10)
C1	0.0181 (16)	0.0294 (18)	0.0342 (18)	−0.0041 (14)	−0.0016 (14)	−0.0046 (15)
C2	0.032 (2)	0.034 (2)	0.065 (3)	−0.0035 (17)	−0.0250 (19)	0.0000 (19)
C3	0.0231 (18)	0.0299 (19)	0.049 (2)	−0.0034 (15)	−0.0132 (16)	−0.0034 (16)
C4	0.0213 (16)	0.0263 (18)	0.0278 (18)	−0.0025 (14)	−0.0003 (13)	−0.0029 (14)
O1	0.0220 (12)	0.0292 (14)	0.0572 (17)	0.0006 (10)	−0.0056 (11)	−0.0134 (12)
O2	0.0245 (13)	0.0274 (13)	0.0512 (16)	0.0008 (10)	−0.0117 (11)	−0.0102 (11)
O3	0.0264 (13)	0.0286 (13)	0.0619 (18)	0.0039 (11)	−0.0132 (12)	−0.0085 (12)
O4	0.0229 (12)	0.0228 (12)	0.0448 (15)	−0.0029 (9)	−0.0078 (11)	−0.0017 (10)
O5	0.0414 (16)	0.0419 (17)	0.0377 (16)	0.0015 (14)	0.0054 (12)	−0.0026 (13)
O6	0.0306 (14)	0.0266 (14)	0.0432 (15)	0.0036 (11)	0.0070 (11)	0.0052 (11)

Geometric parameters (Å, º) top

Cd1—O4ⁱ	2.255 (2)	C2—H2A	0.9700
Cd1—O2	2.284 (2)	C2—H2B	0.9700
Cd1—O6	2.302 (3)	C3—C4	1.498 (4)
Cd1—O4ⁱⁱ	2.316 (2)	C3—H3A	0.9700
Cd1—O5	2.329 (3)	C3—H3B	0.9700
Cd1—O1	2.389 (2)	C4—O3	1.233 (4)
Cd1—O3ⁱ	2.690 (2)	C4—O4	1.275 (4)
C1—O2	1.250 (4)	O5—H5B	0.84 (3)
C1—O1	1.260 (4)	O5—H5A	0.84 (3)
C1—C2	1.498 (5)	O6—H6A	0.85 (3)
C2—C3	1.474 (5)	O6—H6B	0.85 (3)

O4ⁱ—Cd1—O2	136.02 (8)	C1—C2—H2B	108.3
O4ⁱ—Cd1—O6	89.54 (10)	H2A—C2—H2B	107.4
O2—Cd1—O6	103.41 (10)	C2—C3—C4	116.0 (3)
O4ⁱ—Cd1—O4ⁱⁱ	74.92 (9)	C2—C3—H3A	108.3
O2—Cd1—O4ⁱⁱ	147.52 (8)	C4—C3—H3A	108.3
O6—Cd1—O4ⁱⁱ	82.91 (9)	C2—C3—H3B	108.3
O4ⁱ—Cd1—O5	85.77 (10)	C4—C3—H3B	108.3
O2—Cd1—O5	88.74 (10)	H3A—C3—H3B	107.4
O6—Cd1—O5	166.39 (10)	O3—C4—O4	120.4 (3)
O4ⁱⁱ—Cd1—O5	83.54 (10)	O3—C4—C3	123.5 (3)
O4ⁱ—Cd1—O1	166.71 (8)	O4—C4—C3	116.1 (3)
O2—Cd1—O1	55.52 (8)	C1—O1—Cd1	89.42 (19)
O6—Cd1—O1	93.60 (10)	C1—O2—Cd1	94.6 (2)
O4ⁱⁱ—Cd1—O1	92.64 (8)	C4—O4—Cd1ⁱⁱⁱ	103.8 (2)
O5—Cd1—O1	88.23 (10)	C4—O4—Cd1^iv	146.3 (2)
O2—C1—O1	120.4 (3)	Cd1ⁱⁱⁱ—O4—Cd1^iv	105.08 (9)
O2—C1—C2	121.6 (3)	Cd1—O5—H5B	112 (3)
O1—C1—C2	118.0 (3)	Cd1—O5—H5A	111 (3)
C3—C2—C1	115.8 (3)	H5B—O5—H5A	112 (3)
C3—C2—H2A	108.3	Cd1—O6—H6A	113 (3)
C1—C2—H2A	108.3	Cd1—O6—H6B	110 (3)
C3—C2—H2B	108.3	H6A—O6—H6B	108 (3)

O2—C1—C2—C3	−16.9 (6)	O1—C1—O2—Cd1	2.1 (4)
O1—C1—C2—C3	162.3 (4)	C2—C1—O2—Cd1	−178.7 (3)
C1—C2—C3—C4	−174.5 (3)	O4ⁱ—Cd1—O2—C1	170.1 (2)
C2—C3—C4—O3	9.5 (6)	O6—Cd1—O2—C1	−86.3 (2)
C2—C3—C4—O4	−170.0 (4)	O4ⁱⁱ—Cd1—O2—C1	11.7 (3)
O2—C1—O1—Cd1	−2.0 (3)	O5—Cd1—O2—C1	87.5 (2)
C2—C1—O1—Cd1	178.7 (3)	O1—Cd1—O2—C1	−1.2 (2)
O4ⁱ—Cd1—O1—C1	−151.7 (4)	O3—C4—O4—Cd1ⁱⁱⁱ	5.3 (4)
O2—Cd1—O1—C1	1.2 (2)	C3—C4—O4—Cd1ⁱⁱⁱ	−175.2 (3)
O6—Cd1—O1—C1	105.0 (2)	O3—C4—O4—Cd1^iv	153.9 (3)
O4ⁱⁱ—Cd1—O1—C1	−172.0 (2)	C3—C4—O4—Cd1^iv	−26.5 (6)
O5—Cd1—O1—C1	−88.5 (2)

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

Experimental details

Crystal data
Chemical formula	[Cd(C₄H₄O₄)(H₂O)₂]
M_r	264.51
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	7.7130 (15), 12.231 (2), 8.0560 (16)
β (°)	94.71 (3)
V (Å³)	757.4 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.87
Crystal size (mm)	0.40 × 0.30 × 0.21

Data collection
Diffractometer	Bruker SMART CD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 1998)
T_min, T_max	0.35, 0.55
No. of measured, independent and observed [I > 2σ(I)] reflections	6371, 1409, 1335
R_int	0.028
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.053, 1.05
No. of reflections	1409
No. of parameters	116
No. of restraints	6
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.40, −0.68

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Cd1—O4ⁱ	2.255 (2)	Cd1—O5	2.329 (3)
Cd1—O2	2.284 (2)	Cd1—O1	2.389 (2)
Cd1—O6	2.302 (3)	Cd1—O3ⁱ	2.690 (2)
Cd1—O4ⁱⁱ	2.316 (2)

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

References

Bruker (1998). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Brusau, E. V., Pedregosa, J. C. G., Narda, E., Echeverria, G. & Punte, G. (2000). J. Solid State Chem. 153, 1–8. Web of Science CSD CrossRef CAS Google Scholar
He, Y.-K., Wang, X.-F., Zhang, L.-T., Han, Z.-B. & Ng, S. W. (2007). Acta Cryst. E63, m3019. Web of Science CSD CrossRef IUCr Journals Google Scholar
He, Q., Zi, J.-F. & Zhang, F.-J. (2006). Acta Cryst. E62, m1266–m1267. Web of Science CSD CrossRef IUCr Journals Google Scholar
Huo, L.-H., Gao, S. & Ng, S. W. (2005). Acta Cryst. E61, m2357–m2358. Web of Science CSD CrossRef IUCr Journals Google Scholar
Ng, S. W. (1998). Acta Cryst. C54, 745–750. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
Rastsvetaeva, R. K., Pushcharovsky, D. Yu., Furmanova, N. G. & Sharp, H. (1996). Z. Kristallogr. 211, 808–810. CSD CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zhuo, X., Pan, Z.-R., Wang, Z.-W., Li, Y.-Z. & Zheng, H.-G. (2006). Chin. J. Inorg. Chem. 22, 1847–1851. CAS Google Scholar