Tris(ethyl-enediamine-κ(2)N,N')cadmium hexa-fluoridogermanate.

In the title compound, [Cd(C(2)H(8)N(2))(3)](GeF(6)), the Cd(II) atom, lying on a 32 symmetry site, is coordinated by six N atoms from three ethyl-enediamine (en) ligands in a distorted octa-hedral geometry. The Ge atom also lies on a 32 symmetry site and is coordinated by six F atoms. The en ligand has a twofold rotation axis passing through the mid-point of the C-C bond. The F atom is disordered over two sites with equal occupancy factors. In the crystal, the [Cd(en)(3)](2+) cations and [GeF(6)](2-) anions are connected through N-H⋯F hydrogen bonds, forming a three-dimensional supra-molecular network.

Related literature

For background to the structures and applications of microporous materials, see: Cheetham et al. (1999 ▶); Jiang et al. (2010 ▶); Liang et al. (2006 ▶); Yu & Xu (2003 ▶); Zou et al. (2005 ▶). For related fluorides, see: Brauer et al. (1980 ▶, 1986 ▶); Dadachov et al. (2001 ▶); Lukevics et al. (1997 ▶); Tang et al. (2001a ▶,b ▶,c ▶,d ▶,e ▶,f ▶); Wang et al. (2004 ▶); Wang & Wang (2011 ▶); Zhang et al. (2003 ▶). For related structures containing chiral metal complexes, see: Stalder & Wilkinson (1997 ▶); Wang et al. (2003 ▶); Yu et al. (2001 ▶).

Experimental

Crystal data

[Cd(C2H8N2)3](GeF6)

M = 479.33

Trigonal,

a = 9.5422 (3) Å

c = 9.9977 (5) Å

V = 788.37 (7) Å3

Z = 2

Mo Kα radiation

μ = 3.32 mm−1

T = 293 K

0.20 × 0.18 × 0.12 mm

Data collection

Bruker APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.557, T max = 0.692

7348 measured reflections

549 independent reflections

496 reflections with I > 2σ(I)

R int = 0.038

Refinement

R[F 2 > 2σ(F 2)] = 0.024

wR(F 2) = 0.038

S = 1.16

549 reflections

42 parameters

12 restraints

H-atom parameters constrained

Δρmax = 0.23 e Å−3

Δρmin = −0.23 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 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S160053681200983X/hy2520sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681200983X/hy2520Isup2.hkl

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

[Cd(C2H8N2)3](GeF6)	Dx = 2.019 Mg m−3
Mr = 479.33	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P31c	Cell parameters from 549 reflections
Hall symbol: -P 3 2c	θ = 4.1–26.5°
a = 9.5422 (3) Å	µ = 3.32 mm−1
c = 9.9977 (5) Å	T = 293 K
V = 788.37 (7) Å3	Block, colorless
Z = 2	0.20 × 0.18 × 0.12 mm
F(000) = 472

Bruker APEX CCD diffractometer	549 independent reflections
Radiation source: fine-focus sealed tube	496 reflections with I > 2σa(I)
Graphite monochromator	Rint = 0.038
φ and ω scans	θmax = 26.5°, θmin = 4.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→11
Tmin = 0.557, Tmax = 0.692	k = −11→11
7348 measured reflections	l = −12→12

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)] = 0.024	H-atom parameters constrained
wR(F2) = 0.038	w = 1/[σ2(Fo2) + (0.0048P)2 + 0.9629P] where P = (Fo2 + 2Fc2)/3
S = 1.16	(Δ/σ)max < 0.001
549 reflections	Δρmax = 0.23 e Å−3
42 parameters	Δρmin = −0.23 e Å−3
12 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0045 (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	Occ. (<1)
Cd1	0.3333	0.6667	0.2500	0.03249 (17)
Ge1	0.6667	0.3333	0.2500	0.02960 (19)
N1	0.2829 (3)	0.4387 (3)	0.1196 (2)	0.0444 (6)
H1C	0.2637	0.4538	0.0341	0.053*
H1D	0.3698	0.4254	0.1212	0.053*
C1	0.1425 (4)	0.2956 (4)	0.1743 (3)	0.0504 (8)
H1A	0.1381	0.1989	0.1388	0.060*
H1B	0.0443	0.2949	0.1479	0.060*
F1	0.5391 (11)	0.3708 (8)	0.1387 (10)	0.065 (2)	0.50
F1'	0.5004 (11)	0.2974 (8)	0.1521 (10)	0.064 (2)	0.50

	U11	U22	U33	U12	U13	U23
Cd1	0.0326 (2)	0.0326 (2)	0.0323 (3)	0.01630 (10)	0.000	0.000
Ge1	0.0312 (3)	0.0312 (3)	0.0264 (4)	0.01559 (13)	0.000	0.000
N1	0.0559 (17)	0.0475 (16)	0.0364 (13)	0.0309 (14)	−0.0008 (12)	−0.0037 (12)
C1	0.056 (2)	0.0397 (18)	0.0518 (18)	0.0214 (16)	−0.0092 (16)	−0.0112 (14)
F1	0.074 (5)	0.092 (5)	0.051 (3)	0.058 (4)	−0.012 (3)	0.001 (4)
F1'	0.049 (4)	0.098 (5)	0.049 (3)	0.040 (4)	−0.021 (3)	−0.010 (4)

Cd1—N1i	2.370 (2)	Ge1—F1vi	1.812 (9)
Cd1—N1ii	2.370 (2)	Ge1—F1viii	1.812 (9)
Cd1—N1iii	2.370 (2)	Ge1—F1ix	1.812 (9)
Cd1—N1	2.370 (2)	Ge1—F1v	1.812 (9)
Cd1—N1iv	2.370 (2)	Ge1—F1	1.812 (9)
Cd1—N1v	2.370 (2)	N1—C1	1.459 (4)
Ge1—F1'vi	1.746 (9)	N1—H1C	0.9000
Ge1—F1'vii	1.746 (9)	N1—H1D	0.9000
Ge1—F1'viii	1.746 (9)	C1—C1iii	1.518 (6)
Ge1—F1'v	1.746 (9)	C1—H1A	0.9700
Ge1—F1'ix	1.746 (9)	C1—H1B	0.9700
Ge1—F1'	1.746 (9)	F1—F1'	0.621 (10)
Ge1—F1vii	1.812 (9)
N1i—Cd1—N1ii	74.72 (12)	F1'ix—Ge1—F1viii	176.1 (7)
N1i—Cd1—N1iii	92.62 (8)	F1'—Ge1—F1viii	91.4 (3)
N1ii—Cd1—N1iii	103.54 (12)	F1vii—Ge1—F1viii	86.2 (5)
N1i—Cd1—N1	159.72 (12)	F1vi—Ge1—F1viii	82.4 (6)
N1ii—Cd1—N1	92.62 (8)	F1'vi—Ge1—F1ix	73.7 (3)
N1iii—Cd1—N1	74.72 (12)	F1'vii—Ge1—F1ix	90.6 (2)
N1i—Cd1—N1iv	103.54 (12)	F1'viii—Ge1—F1ix	176.1 (7)
N1ii—Cd1—N1iv	92.62 (8)	F1'v—Ge1—F1ix	91.4 (3)
N1iii—Cd1—N1iv	159.72 (12)	F1'—Ge1—F1ix	100.8 (2)
N1—Cd1—N1iv	92.62 (8)	F1vii—Ge1—F1ix	82.4 (6)
N1i—Cd1—N1v	92.62 (8)	F1vi—Ge1—F1ix	86.2 (5)
N1ii—Cd1—N1v	159.72 (12)	F1viii—Ge1—F1ix	160.3 (5)
N1iii—Cd1—N1v	92.62 (8)	F1'vi—Ge1—F1v	176.1 (7)
N1—Cd1—N1v	103.54 (12)	F1'vii—Ge1—F1v	100.8 (2)
N1iv—Cd1—N1v	74.72 (12)	F1'viii—Ge1—F1v	73.7 (3)
F1'vi—Ge1—F1'vii	76.2 (6)	F1'ix—Ge1—F1v	91.4 (3)
F1'vi—Ge1—F1'viii	103.8 (6)	F1'—Ge1—F1v	90.6 (2)
F1'vii—Ge1—F1'viii	91.7 (5)	F1vii—Ge1—F1v	86.2 (5)
F1'vi—Ge1—F1'v	160.4 (5)	F1vi—Ge1—F1v	160.3 (5)
F1'vii—Ge1—F1'v	91.7 (5)	F1viii—Ge1—F1v	86.2 (5)
F1'viii—Ge1—F1'v	91.7 (5)	F1ix—Ge1—F1v	108.8 (5)
F1'vi—Ge1—F1'ix	91.7 (5)	F1'vi—Ge1—F1	100.8 (2)
F1'vii—Ge1—F1'ix	103.8 (6)	F1'vii—Ge1—F1	176.1 (7)
F1'viii—Ge1—F1'ix	160.4 (5)	F1'viii—Ge1—F1	91.4 (3)
F1'v—Ge1—F1'ix	76.2 (6)	F1'v—Ge1—F1	90.6 (2)
F1'vi—Ge1—F1'	91.7 (5)	F1'ix—Ge1—F1	73.7 (3)
F1'vii—Ge1—F1'	160.4 (5)	F1vii—Ge1—F1	160.3 (5)
F1'viii—Ge1—F1'	76.2 (6)	F1vi—Ge1—F1	86.2 (5)
F1'v—Ge1—F1'	103.8 (6)	F1viii—Ge1—F1	108.8 (5)
F1'ix—Ge1—F1'	91.7 (5)	F1ix—Ge1—F1	86.2 (5)
F1'vi—Ge1—F1vii	91.4 (3)	F1v—Ge1—F1	82.4 (6)
F1'viii—Ge1—F1vii	100.8 (2)	C1—N1—Cd1	108.83 (17)
F1'v—Ge1—F1vii	73.7 (3)	C1—N1—H1C	109.9
F1'ix—Ge1—F1vii	90.6 (2)	Cd1—N1—H1C	109.9
F1'—Ge1—F1vii	176.1 (7)	C1—N1—H1D	109.9
F1'vii—Ge1—F1vi	91.4 (3)	Cd1—N1—H1D	109.9
F1'viii—Ge1—F1vi	90.6 (2)	H1C—N1—H1D	108.3
F1'v—Ge1—F1vi	176.1 (7)	N1—C1—C1iii	110.1 (2)
F1'ix—Ge1—F1vi	100.8 (2)	N1—C1—H1A	109.6
F1'—Ge1—F1vi	73.7 (3)	C1iii—C1—H1A	109.6
F1vii—Ge1—F1vi	108.8 (5)	N1—C1—H1B	109.6
F1'vi—Ge1—F1viii	90.6 (2)	C1iii—C1—H1B	109.6
F1'vii—Ge1—F1viii	73.7 (3)	H1A—C1—H1B	108.2
F1'v—Ge1—F1viii	100.8 (2)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1C···F1x	0.90	2.28	3.135 (11)	158
N1—H1C···F1′x	0.90	2.06	2.959 (11)	173
N1—H1D···F1	0.90	1.94	2.831 (11)	172
N1—H1D···F1′	0.90	2.16	3.005 (11)	156

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1C⋯F1i	0.90	2.28	3.135 (11)	158
N1—H1C⋯F1′i	0.90	2.06	2.959 (11)	173
N1—H1D⋯F1	0.90	1.94	2.831 (11)	172
N1—H1D⋯F1′	0.90	2.16	3.005 (11)	156

Symmetry code: (i) .