Tris(ethyl-enediamine)zinc(II) hexa-fluorido-silicate.

The title compound, [Zn(C(2)H(8)N(2))(3)](SiF(6)), was synthesized ionothermally using choline chloride-imidazolidone as solvent and template provider. In the crystal structure, the anions and cations are located on special positions of site symmetry 3.2 and show a typical octa-hedral geometry. The Zn(II) ion is coordinated by six N atoms from three ethyl-enediamine mol-ecules. The crystal structure displays weak hydrogen bonding between [SiF(6)](2-) anions and the ethyl-enediamine NH hydrogen atoms.

Related literature

For related structures, see: Ray et al. (1973 ▶); Bernhardt & Riley (2003 ▶); Cernak et al. (1984 ▶); Emsley et al. (1989 ▶); Cheng et al. (2008 ▶).

Experimental

Crystal data

[Zn(C2H8N2)3](SiF6)

M = 387.77

Hexagonal,

a = 9.192 (2) Å

c = 9.755 (3) Å

V = 713.8 (3) Å3

Z = 2

Mo Kα radiation

μ = 1.87 mm−1

T = 93 K

0.10 × 0.10 × 0.10 mm

Data collection

Rigaku Mercury CCD diffractometer

Absorption correction: multi-scan (CrystalClear; Rigaku, 2004 ▶) T min = 0.835, T max = 0.835

4809 measured reflections

534 independent reflections

499 reflections with I > 2σ(I)

R int = 0.045

Refinement

R[F 2 > 2σ(F 2)] = 0.027

wR(F 2) = 0.059

S = 1.11

534 reflections

32 parameters

H-atom parameters constrained

Δρmax = 0.51 e Å−3

Δρmin = −0.38 e Å−3

Absolute structure: Flack (1983 ▶), 177 Friedel pairs

Flack parameter: 0.01 (3)

Data collection: CrystalClear (Rigaku, 2004 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809045693/bt5123sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809045693/bt5123Isup2.hkl

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

[Zn(C2H8N2)3](SiF6)	Dx = 1.804 Mg m−3
Mr = 387.77	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P6322	Cell parameters from 1402 reflections
Hall symbol: P 6c 2c	θ = 6.6–54.6°
a = 9.192 (2) Å	µ = 1.87 mm−1
c = 9.755 (3) Å	T = 93 K
V = 713.8 (3) Å3	Prism, colorless
Z = 2	0.10 × 0.10 × 0.10 mm
F(000) = 400

Rigaku Mercury CCD diffractometer	534 independent reflections
Radiation source: rotating anode	499 reflections with I > 2σ(I)
confocal	Rint = 0.045
Detector resolution: 0.83 pixels mm-1	θmax = 27.4°, θmin = 3.3°
ω scans	h = −10→11
Absorption correction: multi-scan (CrystalClear; Rigaku, 2004)	k = −10→11
Tmin = 0.835, Tmax = 0.835	l = −11→9
4809 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027	H-atom parameters constrained
wR(F2) = 0.059	w = 1/[σ2(Fo2) + (0.0158P)2 + 0.5912P] where P = (Fo2 + 2Fc2)/3
S = 1.11	(Δ/σ)max < 0.001
534 reflections	Δρmax = 0.51 e Å−3
32 parameters	Δρmin = −0.38 e Å−3
0 restraints	Absolute structure: Flack (1983), 177 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.01 (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
Si1	0.3333	0.6667	0.7500	0.0135 (3)
F1	0.48288 (18)	0.6657 (2)	0.85081 (14)	0.0250 (3)
Zn1	0.6667	0.3333	0.7500	0.01508 (18)
N1	0.8544 (2)	0.5434 (2)	0.87149 (19)	0.0191 (4)
H1A	0.8277	0.5243	0.9631	0.023*
H1B	0.9584	0.5539	0.8589	0.023*
C1	0.8584 (4)	0.6997 (3)	0.8277 (2)	0.0222 (5)
H2A	0.9655	0.7986	0.8566	0.027*
H2B	0.7651	0.7070	0.8716	0.027*

	U11	U22	U33	U12	U13	U23
Si1	0.0151 (4)	0.0151 (4)	0.0102 (7)	0.0076 (2)	0.000	0.000
F1	0.0260 (7)	0.0352 (8)	0.0183 (7)	0.0186 (7)	−0.0057 (6)	−0.0011 (7)
Zn1	0.0169 (2)	0.0169 (2)	0.0115 (3)	0.00843 (11)	0.000	0.000
N1	0.0185 (10)	0.0240 (11)	0.0137 (11)	0.0097 (9)	−0.0018 (8)	0.0003 (8)
C1	0.0234 (13)	0.0195 (11)	0.0225 (12)	0.0099 (13)	−0.0031 (12)	−0.0037 (8)

Si1—F1i	1.6938 (13)	Zn1—N1v	2.186 (2)
Si1—F1ii	1.6938 (13)	Zn1—N1viii	2.1863 (19)
Si1—F1iii	1.6938 (14)	Zn1—N1ix	2.1863 (19)
Si1—F1iv	1.6938 (14)	N1—C1	1.482 (3)
Si1—F1	1.6938 (13)	N1—H1A	0.9200
Si1—F1v	1.6938 (13)	N1—H1B	0.9200
Zn1—N1vi	2.1863 (19)	C1—C1viii	1.523 (4)
Zn1—N1vii	2.1863 (19)	C1—H2A	0.9900
Zn1—N1	2.186 (2)	C1—H2B	0.9900
F1i—Si1—F1ii	90.69 (10)	N1vi—Zn1—N1viii	93.40 (7)
F1i—Si1—F1iii	89.68 (7)	N1vii—Zn1—N1viii	170.67 (11)
F1ii—Si1—F1iii	89.95 (10)	N1—Zn1—N1viii	80.19 (10)
F1i—Si1—F1iv	89.95 (10)	N1v—Zn1—N1viii	93.40 (7)
F1ii—Si1—F1iv	89.68 (7)	N1vi—Zn1—N1ix	170.67 (11)
F1iii—Si1—F1iv	179.47 (11)	N1vii—Zn1—N1ix	93.40 (7)
F1i—Si1—F1	179.47 (11)	N1—Zn1—N1ix	93.40 (7)
F1ii—Si1—F1	89.68 (7)	N1v—Zn1—N1ix	80.19 (10)
F1iii—Si1—F1	90.69 (10)	N1viii—Zn1—N1ix	93.74 (11)
F1iv—Si1—F1	89.68 (7)	C1—N1—Zn1	109.01 (14)
F1i—Si1—F1v	89.68 (7)	C1—N1—H1A	109.9
F1ii—Si1—F1v	179.47 (11)	Zn1—N1—H1A	109.9
F1iii—Si1—F1v	89.68 (7)	C1—N1—H1B	109.9
F1iv—Si1—F1v	90.69 (10)	Zn1—N1—H1B	109.9
F1—Si1—F1v	89.95 (10)	H1A—N1—H1B	108.3
N1vi—Zn1—N1vii	80.19 (10)	N1—C1—C1viii	109.52 (17)
N1vi—Zn1—N1	93.74 (11)	N1—C1—H2A	109.8
N1vii—Zn1—N1	93.40 (7)	C1viii—C1—H2A	109.8
N1vi—Zn1—N1v	93.40 (7)	N1—C1—H2B	109.8
N1vii—Zn1—N1v	93.74 (11)	C1viii—C1—H2B	109.8
N1—Zn1—N1v	170.67 (11)	H2A—C1—H2B	108.2
N1vi—Zn1—N1—C1	106.99 (17)	N1ix—Zn1—N1—C1	−79.03 (19)
N1vii—Zn1—N1—C1	−172.64 (16)	Zn1—N1—C1—C1viii	−39.9 (3)
N1viii—Zn1—N1—C1	14.19 (13)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···F1x	0.92	2.26	3.113 (3)	155
N1—H1A···F1xi	0.92	2.49	3.239 (3)	139
N1—H1B···F1vii	0.92	2.25	3.153 (3)	166

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯F1i	0.92	2.26	3.113 (3)	155
N1—H1A⋯F1ii	0.92	2.49	3.239 (3)	139
N1—H1B⋯F1iii	0.92	2.25	3.153 (3)	166

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