Bis-Triiodide von 1,2-Ethandiaminkomplexen am Beispiel des Metalls Kupfer

In bis­(1,2-ethanedi­amine-N,N')­bis­[tri­iodo(1-)-I]copper, [Cu(I₃)₂­(C₂H₈N₂)₂], the triiodide anions form chains parallel to [001]. The central metal ion (site symmetry 2/m) of the complex cation is coordinated to four N atoms and to two I atoms. The geometry of the square-bipyramidal complex is as expected, with d(Cu-N) = 2.006 (5) and d(Cu-I) = 3.3600 (9) Å.

Computing details

Data collection: IPDS-Programmsystem (Stoe & Cie 1996/97); cell refinement: IPDS-Programmsystem; data reduction: IPDS-Programmsystem (Stoe & Cie, 1996/97) and X-SHAPE and X-RED (Stoe & Cie, 1997)'; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999), PARST95 (Nardelli, 1995), PLATON96 (Spek, 1996) and CIFEDIT (Wieczorrek, 1999).

[Bis-1,2-Diaminoethan-kupfer]bis-triiodid

Crystal data

[Cu(I3)2(C2H8N2)2]	Dx = 3.356 Mg m^−3
Mr = 945.15	Melting point: 505 K
Orthorhombic, Ibam	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -I 2 2c	Cell parameters from 5000 reflections
a = 7.490 (2) Å	θ = 3.2–51.3°
b = 13.400 (3) Å	µ = 11.05 mm^−1
c = 18.639 (6) Å	T = 293 K
V = 1870.7 (9) Å^3	Kombination aus den Quader- und Pyramidenflächen (010), (001) und (101)., black
Z = 4	0.38 × 0.36 × 0.33 mm
F(000) = 1660

Data collection

Stoe & Cie IPDS diffractometer	927 independent reflections
Radiation source: fine-focus sealed tube	740 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.099
Detector resolution: 44.4 pixels mm^-1	θmax = 25.8°, θmin = 2.2°
oscillation scans	h = −9→9
Absorption correction: analytical Analytische Absorptionskorrektur über WINGX V1.61 (Alcock, 1970) über die Kristallflächen (010), (001) und (101).	k = −16→16
Tmin = 0.051, Tmax = 0.104	l = −22→22
8344 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.039	H-atom parameters constrained
wR(F^2) = 0.091	w = 1/[σ^2(Fo^2) + (0.0402P)^2 + 4.5689P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max < 0.001
927 reflections	Δρmax = 1.25 e Å^−3
43 parameters	Δρmin = −1.01 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0074 (3)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
I1	0.35115 (11)	0.15604 (5)	0.5000	0.0639 (3)
I2	0.45688 (6)	0.16005 (3)	0.32327 (4)	0.0683 (3)
Cu	0.0000	0.0000	0.5000	0.0461 (5)
N1	−0.1268 (8)	0.0721 (4)	0.4206 (3)	0.0515 (14)
H1NA	−0.240 (9)	0.0524 (15)	0.4188 (3)	0.09 (2)*
H1NB	−0.1252 (8)	0.137 (5)	0.4290 (7)	0.09 (2)*
C1	−0.0392 (10)	0.0511 (5)	0.3516 (4)	0.0544 (18)
H1A	0.061 (7)	0.103 (3)	0.3426 (7)	0.09 (2)*
H1B	−0.132 (6)	0.0570 (7)	0.310 (3)	0.09 (2)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
I1	0.0793 (5)	0.0522 (4)	0.0603 (5)	−0.0183 (3)	0.000	0.000
I2	0.0445 (4)	0.0440 (3)	0.1164 (6)	0.0000 (2)	−0.0046 (3)	−0.0006 (2)
Cu	0.0554 (10)	0.0407 (8)	0.0423 (9)	0.0174 (7)	0.000	0.000
N1	0.053 (3)	0.047 (3)	0.054 (4)	0.017 (3)	−0.001 (3)	0.002 (2)
C1	0.061 (4)	0.062 (4)	0.040 (4)	0.009 (3)	0.004 (3)	0.008 (3)

Geometric parameters (Å, º)

I1—Cu	3.3600 (10)	Cu—N1^iv	2.007 (6)
I1—I2	3.3883 (13)	Cu—N1^i	2.007 (6)
I1—I2^i	3.3883 (13)	Cu—I1^iv	3.3600 (10)
I2—I2^ii	2.8068 (16)	N1—C1	1.471 (9)
Cu—N1^iii	2.007 (6)	C1—C1^iii	1.489 (14)
Cu—N1	2.007 (6)
Cu—I1—I2	101.118 (14)	N1—Cu—I1^iv	85.92 (18)
Cu—I1—I2^i	101.118 (15)	N1^iv—Cu—I1^iv	94.08 (18)
I2—I1—I2^i	152.91 (3)	N1^i—Cu—I1^iv	85.92 (18)
I2^ii—I2—I1	179.066 (15)	N1^iii—Cu—I1	85.92 (18)
N1^iii—Cu—N1	84.9 (3)	N1—Cu—I1	94.08 (18)
N1^iii—Cu—N1^iv	95.1 (3)	N1^iv—Cu—I1	85.92 (18)
N1—Cu—N1^iv	180.0 (2)	N1^i—Cu—I1	94.08 (18)
N1^iii—Cu—N1^i	180.0 (2)	I1^iv—Cu—I1	180.0
N1—Cu—N1^i	95.1 (3)	C1—N1—Cu	110.0 (4)
N1^iv—Cu—N1^i	84.9 (3)	N1—C1—C1^iii	110.6 (4)
N1^iii—Cu—I1^iv	94.08 (18)
Cu—I1—I2—I2^ii	−37.8 (18)	I2^i—I1—Cu—N1^i	50.09 (17)
I2^i—I1—I2—I2^ii	106.9 (18)	I2—I1—Cu—I1^iv	162.248 (18)
I2—I1—Cu—N1^iii	34.51 (16)	I2^i—I1—Cu—I1^iv	−2.171 (18)
I2^i—I1—Cu—N1^iii	−129.91 (17)	N1^iii—Cu—N1—C1	−11.3 (4)
I2—I1—Cu—N1	−50.09 (17)	N1^iv—Cu—N1—C1	146 (57)
I2^i—I1—Cu—N1	145.49 (16)	N1^i—Cu—N1—C1	168.7 (4)
I2—I1—Cu—N1^iv	129.91 (17)	I1^iv—Cu—N1—C1	−105.8 (5)
I2^i—I1—Cu—N1^iv	−34.51 (16)	I1—Cu—N1—C1	74.2 (5)
I2—I1—Cu—N1^i	−145.49 (16)	Cu—N1—C1—C1^iii	31.6 (9)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1NB···I1^v	0.88	3.08 (1)	3.936 (4)	164 (1)

Symmetry code: (v) x−1/2, −y+1/2, z.