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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807042390/bi2235sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807042390/bi2235Isup2.hkl
Contains datablock I

CCDC reference: 1296690

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.048
  • wR factor = 0.148
  • Data-to-parameter ratio = 14.1

checkCIF/PLATON results

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Alert level C PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 7
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn1 (2) 2.09
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

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).

Structure description 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).

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

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 m3
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 mm1
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 = 99
Tmin = 0.668, Tmax = 0.823k = 1211
3715 measured reflectionsl = 99
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 Å3
0 restraintsΔρmin = 0.84 e Å3
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 mm1
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 reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0480 restraints
wR(F2) = 0.148H-atom parameters constrained
S = 1.07Δρmax = 0.71 e Å3
1116 reflectionsΔρmin = 0.84 e Å3
79 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
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, z1/2; (iii) x, y+3/2, z1/2; (iv) x, y, z1.

Experimental details

Crystal data
Chemical formula[Zn(NO3)2(C2H8N2)2]
Mr309.62
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)8.2127 (7), 9.9673 (8), 7.9733 (7)
β (°) 111.171 (1)
V3)608.63 (9)
Z2
Radiation typeMo Kα
µ (mm1)2.05
Crystal size (mm)0.24 × 0.17 × 0.09
Data collection
DiffractometerBruker APEXII CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 1997)
Tmin, Tmax0.668, 0.823
No. of measured, independent and
observed [I > 2σ(I)] reflections
3715, 1116, 811
Rint0.026
(sin θ/λ)max1)0.606
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.048, 0.148, 1.07
No. of reflections1116
No. of parameters79
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.71, 0.84

Computer programs: APEX2 (Bruker, 2006), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997).

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, z1/2; (iii) x, y+3/2, z1/2; (iv) x, y, z1.
 

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