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Acta Cryst. (2007). E63, m2462    [ doi:10.1107/S1600536807042390 ]

trans-Bis(ethylenediamine-[kappa]2N,N')bis(nitrato-[kappa]O)zinc(II)

Y.-Q. Liu, X.-R. Zeng and W.-T. Chen

Abstract top

In the title compound, [Zn(NO3)2(C2H8N2)2], the ZnII atom lies on a centre of inversion and is coordinated by four N atoms belonging to two ethylenediamine molecules and two O atoms belonging to two nitrate anions arranged in a trans manner. The ZnII ion displays a distorted octahedral coordination geometry. Adjacent complexes are connected by N-H...O hydrogen bonds formed between the H atoms of the amino groups and the uncoordinated O atoms of the nitrate anions.

Comment top

The title compound (Fig. 1) is a mononuclear ZnII complex. The ZnII atom lies on a centre of inversion and is coordinated to four N atoms belonging to two ethylenediamine molecules and two O atoms belonging to two nitrate anions arranged in a trans manner. In the crystal, adjacent molecules are connected by N—H···O hydrogen bonds involving the H atoms of the amino groups and the non-bonded O atoms of the nitrate ions (Fig. 2).

Related literature top

For the structure of the analogous CuII compound, see: Komiyama & Lingafelter (1964); Fronczek et al. (1995); Manriquez et al. (1996).

Experimental top

Ethylenediamine (0.120 g, 0.002 mol) and Zn(NO3)2 (0.189 g, 0.001 mol) were added to 25 ml me thanol. The mixture was heated for 5 h under reflux with stirring and the resulting solution was filtered. Single crystals suitable for X-ray diffraction were formed after a week by slow evaporation of the filtrate.

Refinement top

H atoms were placed at calculated positions and refined as riding on their parent C or N atoms, with C—H = 0.97 Å or N—H = 0.90 Å, and with Uiso(H) = 1.2Ueq(C/N).

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL (Bruker, 1997).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound with displacement ellipsoids drawn at 50% probability for non-H atoms.
[Figure 2] Fig. 2. Unit-cell contents viewed along the c axis. H bonds are shown as dashed lines.
trans-Bis(ethylenediamine-κ2N,N')bis(nitrato-κO) zinc(II) top
Crystal data top
[Zn(NO3)2(C2H8N2)2]F(000) = 320
Mr = 309.62Dx = 1.689 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2202 reflections
a = 8.2127 (7) Åθ = 2.7–27.8°
b = 9.9673 (8) ŵ = 2.05 mm−1
c = 7.9733 (7) ÅT = 293 K
β = 111.171 (1)°Block, colourless
V = 608.63 (9) Å30.24 × 0.17 × 0.09 mm
Z = 2
Data collection top
Bruker APEXII CCD
diffractometer		1116 independent reflections
Radiation source: fine-focus sealed tube811 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
φ and ω scansθmax = 25.5°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Bruker, 1997)		h = −9→9
Tmin = 0.668, Tmax = 0.823k = −12→11
3715 measured reflectionsl = −9→9
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.148H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0901P)2 + 0.4042P]
where P = (Fo2 + 2Fc2)/3
1116 reflections(Δ/σ)max < 0.001
79 parametersΔρmax = 0.71 e Å−3
0 restraintsΔρmin = −0.84 e Å−3
Crystal data top
[Zn(NO3)2(C2H8N2)2]V = 608.63 (9) Å3
Mr = 309.62Z = 2
Monoclinic, P21/cMo Kα radiation
a = 8.2127 (7) ŵ = 2.05 mm−1
b = 9.9673 (8) ÅT = 293 K
c = 7.9733 (7) Å0.24 × 0.17 × 0.09 mm
β = 111.171 (1)°
Data collection top
Bruker APEXII CCD
diffractometer		1116 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1997)		811 reflections with I > 2σ(I)
Tmin = 0.668, Tmax = 0.823Rint = 0.026
3715 measured reflectionsθmax = 25.5°
Refinement top
R[F2 > 2σ(F2)] = 0.048H-atom parameters constrained
wR(F2) = 0.148Δρmax = 0.71 e Å−3
S = 1.07Δρmin = −0.84 e Å−3
1116 reflectionsAbsolute structure: ?
79 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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
xyzUiso*/Ueq
Zn11.00000.50000.50000.0411 (3)
N30.8252 (6)0.5573 (4)0.8297 (6)0.0547 (11)
O10.7756 (5)0.6261 (4)0.9285 (5)0.0637 (10)
O20.9006 (5)0.6110 (3)0.7375 (5)0.0600 (10)
O30.7984 (5)0.4342 (4)0.8202 (6)0.0675 (11)
C20.6379 (8)0.5160 (5)0.3000 (9)0.0620 (15)
H2A0.54730.53320.18400.074*
H2B0.59680.54740.39290.074*
N10.8360 (5)0.3461 (4)0.4743 (6)0.0544 (11)
H3B0.88560.26960.45630.065*
H3A0.81250.33700.57550.065*
N20.7978 (5)0.5876 (4)0.3128 (6)0.0515 (11)
H4A0.79040.67390.34230.062*
H4B0.81200.58530.20610.062*
C10.6745 (7)0.3712 (5)0.3217 (8)0.0649 (15)
H1A0.57840.32560.34080.078*
H1B0.68510.33560.21280.078*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O20.090 (3)0.044 (2)0.062 (2)−0.0035 (18)0.045 (2)−0.0026 (16)
O30.095 (3)0.039 (2)0.075 (3)−0.0047 (19)0.039 (2)0.0023 (19)
Zn10.0495 (5)0.0314 (5)0.0439 (5)0.0007 (3)0.0187 (3)0.0030 (3)
N30.082 (3)0.037 (2)0.056 (3)−0.001 (2)0.039 (2)0.000 (2)
O10.093 (3)0.052 (2)0.060 (2)0.0047 (19)0.044 (2)−0.0022 (17)
C20.058 (3)0.052 (3)0.069 (4)−0.001 (2)0.014 (3)0.002 (2)
N10.057 (2)0.037 (2)0.069 (3)−0.0039 (18)0.021 (2)−0.0027 (19)
N20.054 (2)0.044 (2)0.054 (3)0.0043 (18)0.0172 (19)0.0036 (18)
C10.061 (3)0.049 (3)0.076 (4)−0.004 (2)0.014 (3)−0.003 (3)
Geometric parameters (Å, º) top
O2—N31.241 (5)C2—H2A0.970
O2—Zn12.568 (3)C2—H2B0.970
O3—N31.243 (6)N1—C11.462 (6)
Zn1—N2i1.989 (4)N1—H3B0.900
Zn1—N21.989 (4)N1—H3A0.900
Zn1—N12.002 (4)N2—H4A0.900
Zn1—N1i2.002 (4)N2—H4B0.900
N3—O11.221 (5)C1—H1A0.970
C2—N21.466 (7)C1—H1B0.970
C2—C11.472 (7)
N3—O2—Zn1127.6 (3)H2A—C2—H2B108.3
N2i—Zn1—N2180.0C1—N1—Zn1109.2 (3)
N2i—Zn1—N195.11 (16)C1—N1—H3B109.8
N2—Zn1—N184.89 (16)Zn1—N1—H3B109.8
N2i—Zn1—N1i84.89 (16)C1—N1—H3A109.8
N2—Zn1—N1i95.11 (16)Zn1—N1—H3A109.8
N1—Zn1—N1i180.00 (14)H3B—N1—H3A108.3
N2i—Zn1—O292.14 (15)C2—N2—Zn1108.9 (3)
N2—Zn1—O287.86 (15)C2—N2—H4A109.9
N1—Zn1—O291.40 (15)Zn1—N2—H4A109.9
N1i—Zn1—O288.60 (15)C2—N2—H4B109.9
O1—N3—O2119.6 (4)Zn1—N2—H4B109.9
O1—N3—O3120.0 (4)H4A—N2—H4B108.3
O2—N3—O3120.3 (4)N1—C1—C2110.6 (4)
N2—C2—C1109.2 (5)N1—C1—H1A109.5
N2—C2—H2A109.8C2—C1—H1A109.5
C1—C2—H2A109.8N1—C1—H1B109.5
N2—C2—H2B109.8C2—C1—H1B109.5
C1—C2—H2B109.8H1A—C1—H1B108.1
Symmetry code: (i) −x+2, −y+1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H3B···O3ii0.902.293.023 (6)138
N1—H3A···O30.902.223.015 (6)147
N2—H4A···O1iii0.902.133.025 (5)176
N2—H4A···O2iii0.902.583.235 (5)130
N2—H4B···O1iv0.902.163.027 (6)161
Symmetry codes: (ii) x, −y+1/2, z−1/2; (iii) x, −y+3/2, z−1/2; (iv) x, y, z−1.
Selected geometric parameters (Å, º) top
O2—Zn12.568 (3)Zn1—N12.002 (4)
Zn1—N21.989 (4)
N2i—Zn1—N2180.0N2i—Zn1—O292.14 (15)
N2i—Zn1—N195.11 (16)N2—Zn1—O287.86 (15)
N2—Zn1—N184.89 (16)N1—Zn1—O291.40 (15)
N1—Zn1—N1i180.00 (14)N1i—Zn1—O288.60 (15)
Symmetry code: (i) −x+2, −y+1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H3B···O3ii0.902.293.023 (6)138.1
N1—H3A···O30.902.223.015 (6)147.3
N2—H4A···O1iii0.902.133.025 (5)176.4
N2—H4A···O2iii0.902.583.235 (5)130.2
N2—H4B···O1iv0.902.163.027 (6)161.1
Symmetry codes: (ii) x, −y+1/2, z−1/2; (iii) x, −y+3/2, z−1/2; (iv) x, y, z−1.
Acknowledgements top

The authors are grateful to the Natural Science Foundation of Jiangxi Province (grant Nos. 0520036 and 0620029) for support of this work.

references
References top

Bruker (1997). SADABS, SAINT and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA. [Note SMART cannot be used with an APEXII machine, so it has been removed]

Bruker (2006). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA. [Please check added reference and correct as necessary]

Fronczek, F. R., Brown, L. A. & Maverick, A. W. (1995). Private communication [Refcode ???]. CCDC, Union Road, Cambridge, England.

Komiyama, Y. & Lingafelter, E. C. (1964). Acta Cryst. 17, 1145–1148.

Manriquez, V., Campos-Vallette, M., Lara, N., Gonzalez-Tejeda, N., Wittke, O., Diaz, G., Diez, S., Munoz, R. & Kriskovic, L. (1996). J. Chem. Crystallogr. 26, 15–22.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.