Di-μ-chlorido-bis-[bis-(ethyl-enediamine-κN,N')cadmium(II)] dichloride.

The crystal structure of the title compound, [Cd(2)Cl(2)(C(2)H(8)N(2))(4)]Cl(2), consists of binuclear centrosymmetric [Cd(2)(C(2)H(8)N(2))(4)Cl(2)](2+) cations and discrete chloride anions. The Cd(II) cation is coordinated by four N atoms of two ethyl-enediamine ligands and two symmetry-related chloride anions within a distorted CdN(4)Cl(2) octa-hedron. Two Cd(II) cations are connected by two chloride anions via μ(2)-coordination, forming a four-membered Cd(2)Cl(2) ring. The uncoordinated chloride anions are linked to the amino groups via N-H⋯Cl hydrogen bonding. Two C atoms of one of the two crystallographically independent ethyl-enediamine ligands are disordered and were refined using a split model [occupancy ratio 0.674 (9):0.326 (9)].

Related literature

For the general background to this work see: Bhosekar et al. (2006 ▶); Näther et al. (2007 ▶). For related structures, see: Cannas et al. (1980 ▶); Marsh (1999 ▶); Pauly et al. (2000 ▶); Chen et al. (2005 ▶).

Experimental

Crystal data

[Cd2Cl2(C2H8N2)4]Cl2

M = 607.02

Monoclinic,

a = 6.3869 (8) Å

b = 11.3143 (10) Å

c = 14.8255 (19) Å

β = 92.621 (13)°

V = 1070.2 (2) Å3

Z = 2

Mo Kα radiation

μ = 2.49 mm−1

T = 293 K

0.3 × 0.2 × 0.2 mm

Data collection

Stoe IPDS-1 diffractometer

Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998 ▶) T min = 0.576, T max = 0.613

6562 measured reflections

3110 independent reflections

2699 reflections with I > 2σ(I)

R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.018

wR(F 2) = 0.047

S = 1.04

3110 reflections

120 parameters

H-atom parameters constrained

Δρmax = 0.53 e Å−3

Δρmin = −0.49 e Å−3

Data collection: DIF4 (Stoe & Cie, 1992 ▶); cell refinement: DIF4; data reduction: REDU4 (Stoe & Cie, 1992 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: XCIF in SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809054804/wm2291sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809054804/wm2291Isup2.hkl

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

[Cd2Cl2(C2H8N2)4]Cl2	F(000) = 600
Mr = 607.02	Dx = 1.884 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 120 reflections
a = 6.3869 (8) Å	θ = 10–25°
b = 11.3143 (10) Å	µ = 2.49 mm−1
c = 14.8255 (19) Å	T = 293 K
β = 92.621 (13)°	Block, colourless
V = 1070.2 (2) Å3	0.3 × 0.2 × 0.2 mm
Z = 2

Stoe IPDS-1 diffractometer	3110 independent reflections
Radiation source: fine-focus sealed tube	2699 reflections with I > 2σ(I)
graphite	Rint = 0.018
φ scan	θmax = 30.0°, θmin = 2.3°
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998)	h = 0→8
Tmin = 0.576, Tmax = 0.613	k = −15→15
6562 measured reflections	l = −20→20

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)] = 0.018	H-atom parameters constrained
wR(F2) = 0.047	w = 1/[σ2(Fo2) + (0.0256P)2 + 0.1639P] where P = (Fo2 + 2Fc2)/3
S = 1.04	(Δ/σ)max = 0.002
3110 reflections	Δρmax = 0.53 e Å−3
120 parameters	Δρmin = −0.49 e Å−3
0 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: 0.0088 (4)

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	0.658581 (17)	0.626379 (10)	0.561674 (7)	0.03352 (5)
Cl1	0.70739 (6)	0.39404 (4)	0.52416 (3)	0.04109 (9)
Cl2	0.67265 (8)	0.63867 (4)	0.20632 (4)	0.05032 (11)
N1	0.5276 (2)	0.61258 (13)	0.70697 (10)	0.0382 (3)
H1N1	0.4337	0.6703	0.7155	0.046*
H2N1	0.4645	0.5423	0.7142	0.046*
C1	0.7084 (3)	0.62488 (17)	0.77133 (11)	0.0475 (4)
H1A	0.6709	0.5970	0.8303	0.057*
H1B	0.7471	0.7076	0.7768	0.057*
C2	0.8923 (3)	0.55455 (18)	0.73977 (13)	0.0491 (4)
H2A	1.0072	0.5586	0.7848	0.059*
H2B	0.8523	0.4723	0.7322	0.059*
N2	0.9601 (2)	0.60183 (13)	0.65389 (10)	0.0394 (3)
H1N2	1.0487	0.5512	0.6284	0.047*
H2N2	1.0259	0.6715	0.6627	0.047*
N3	0.8018 (2)	0.70351 (15)	0.43233 (10)	0.0447 (3)
H1N3	0.9427	0.7019	0.4377	0.054*	0.326 (9)
H2N3	0.7598	0.6610	0.3835	0.054*	0.326 (9)
H3N3	0.9223	0.6660	0.4214	0.054*	0.674 (9)
H4N3	0.7121	0.6933	0.3844	0.054*	0.674 (9)
C3	0.7267 (15)	0.8259 (6)	0.4236 (4)	0.0468 (19)	0.326 (9)
H3C	0.7886	0.8641	0.3726	0.056*	0.326 (9)
H3D	0.5754	0.8271	0.4139	0.056*	0.326 (9)
C4	0.7884 (17)	0.8874 (6)	0.5075 (5)	0.054 (2)	0.326 (9)
H4C	0.7632	0.9716	0.5009	0.065*	0.326 (9)
H4D	0.9365	0.8753	0.5221	0.065*	0.326 (9)
C3'	0.8423 (7)	0.8322 (3)	0.4474 (3)	0.0536 (10)	0.674 (9)
H3A	0.8603	0.8708	0.3899	0.064*	0.674 (9)
H3B	0.9708	0.8421	0.4841	0.064*	0.674 (9)
C4'	0.6641 (8)	0.8893 (3)	0.4939 (3)	0.0557 (10)	0.674 (9)
H4A	0.6870	0.9738	0.4989	0.067*	0.674 (9)
H4B	0.5333	0.8760	0.4595	0.067*	0.674 (9)
N4	0.6547 (3)	0.83613 (14)	0.58432 (12)	0.0531 (4)
H1N4	0.5228	0.8642	0.5798	0.064*	0.326 (9)
H2N4	0.7120	0.8550	0.6390	0.064*	0.326 (9)
H3N4	0.5368	0.8583	0.6107	0.064*	0.674 (9)
H4N4	0.7658	0.8588	0.6197	0.064*	0.674 (9)

	U11	U22	U33	U12	U13	U23
Cd1	0.03410 (7)	0.03660 (7)	0.02973 (6)	−0.00457 (4)	0.00013 (4)	−0.00078 (4)
Cl1	0.02885 (16)	0.04039 (19)	0.0533 (2)	0.00407 (14)	−0.00646 (15)	−0.01037 (16)
Cl2	0.0504 (2)	0.0410 (2)	0.0597 (3)	0.00376 (17)	0.0042 (2)	0.01005 (18)
N1	0.0337 (6)	0.0439 (7)	0.0374 (6)	−0.0007 (5)	0.0052 (5)	0.0035 (5)
C1	0.0458 (9)	0.0665 (12)	0.0302 (7)	0.0017 (8)	0.0017 (6)	−0.0002 (7)
C2	0.0439 (9)	0.0571 (10)	0.0455 (9)	0.0089 (8)	−0.0067 (7)	0.0085 (8)
N2	0.0303 (6)	0.0422 (7)	0.0458 (7)	0.0000 (5)	0.0008 (5)	−0.0061 (6)
N3	0.0360 (7)	0.0607 (9)	0.0378 (7)	0.0050 (6)	0.0062 (5)	0.0027 (6)
C3	0.045 (4)	0.051 (3)	0.044 (3)	−0.003 (3)	0.002 (3)	0.019 (2)
C4	0.063 (5)	0.038 (3)	0.062 (4)	−0.008 (3)	0.008 (4)	0.013 (3)
C3'	0.047 (2)	0.0619 (19)	0.0529 (19)	−0.0065 (14)	0.0122 (16)	0.0177 (14)
C4'	0.059 (3)	0.0456 (15)	0.063 (2)	0.0064 (15)	0.0113 (17)	0.0172 (13)
N4	0.0788 (12)	0.0383 (7)	0.0430 (8)	0.0001 (8)	0.0106 (8)	−0.0019 (7)

Cd1—N2	2.3268 (15)	N3—H1N3	0.9000
Cd1—N3	2.3314 (15)	N3—H2N3	0.9000
Cd1—N1	2.3513 (14)	N3—H3N3	0.9000
Cd1—N4	2.3971 (16)	N3—H4N3	0.9000
Cd1—Cl1i	2.6200 (5)	C3—C4	1.464 (12)
Cd1—Cl1	2.7078 (5)	C3—H3C	0.9700
Cl1—Cd1i	2.6200 (5)	C3—H3D	0.9700
N1—C1	1.471 (2)	C4—N4	1.566 (7)
N1—H1N1	0.9000	C4—H4C	0.9700
N1—H2N1	0.9000	C4—H4D	0.9700
C1—C2	1.511 (3)	C3'—C4'	1.503 (6)
C1—H1A	0.9700	C3'—H3A	0.9700
C1—H1B	0.9700	C3'—H3B	0.9700
C2—N2	1.465 (2)	C4'—N4	1.473 (4)
C2—H2A	0.9700	C4'—H4A	0.9700
C2—H2B	0.9700	C4'—H4B	0.9700
N2—H1N2	0.9000	N4—H1N4	0.9000
N2—H2N2	0.9000	N4—H2N4	0.9000
N3—C3	1.469 (7)	N4—H3N4	0.9000
N3—C3'	1.494 (4)	N4—H4N4	0.9000
N2—Cd1—N3	100.53 (6)	H1N3—N3—H3N3	31.4
N2—Cd1—N1	76.90 (5)	H2N3—N3—H3N3	80.1
N3—Cd1—N1	161.39 (5)	C3—N3—H4N3	81.8
N2—Cd1—N4	92.83 (6)	C3'—N3—H4N3	110.0
N3—Cd1—N4	75.61 (6)	Cd1—N3—H4N3	110.0
N1—Cd1—N4	86.05 (5)	H1N3—N3—H4N3	131.6
N2—Cd1—Cl1i	166.14 (4)	H2N3—N3—H4N3	30.7
N3—Cd1—Cl1i	90.48 (4)	H3N3—N3—H4N3	108.4
N1—Cd1—Cl1i	95.29 (4)	C4—C3—N3	107.4 (7)
N4—Cd1—Cl1i	98.09 (5)	C4—C3—H3C	110.2
N2—Cd1—Cl1	84.54 (4)	N3—C3—H3C	110.2
N3—Cd1—Cl1	98.12 (4)	C4—C3—H3D	110.2
N1—Cd1—Cl1	99.95 (4)	N3—C3—H3D	110.2
N4—Cd1—Cl1	172.69 (5)	H3C—C3—H3D	108.5
Cl1i—Cd1—Cl1	85.593 (13)	C3—C4—N4	107.9 (6)
Cd1i—Cl1—Cd1	94.407 (13)	C3—C4—H4C	110.1
C1—N1—Cd1	106.64 (10)	N4—C4—H4C	110.1
C1—N1—H1N1	110.4	C3—C4—H4D	110.1
Cd1—N1—H1N1	110.4	N4—C4—H4D	110.1
C1—N1—H2N1	110.4	H4C—C4—H4D	108.4
Cd1—N1—H2N1	110.4	N3—C3'—C4'	111.0 (3)
H1N1—N1—H2N1	108.6	N3—C3'—H3A	109.4
N1—C1—C2	110.35 (15)	C4'—C3'—H3A	109.4
N1—C1—H1A	109.6	N3—C3'—H3B	109.4
C2—C1—H1A	109.6	C4'—C3'—H3B	109.4
N1—C1—H1B	109.6	H3A—C3'—H3B	108.0
C2—C1—H1B	109.6	N4—C4'—C3'	107.7 (3)
H1A—C1—H1B	108.1	N4—C4'—H4A	110.2
N2—C2—C1	109.99 (14)	C3'—C4'—H4A	110.2
N2—C2—H2A	109.7	N4—C4'—H4B	110.2
C1—C2—H2A	109.7	C3'—C4'—H4B	110.2
N2—C2—H2B	109.7	H4A—C4'—H4B	108.5
C1—C2—H2B	109.7	C4'—N4—C4	30.7 (3)
H2A—C2—H2B	108.2	C4'—N4—Cd1	106.00 (17)
C2—N2—Cd1	106.55 (10)	C4—N4—Cd1	104.8 (3)
C2—N2—H1N2	110.4	C4'—N4—H1N4	82.3
Cd1—N2—H1N2	110.4	C4—N4—H1N4	110.8
C2—N2—H2N2	110.4	Cd1—N4—H1N4	110.8
Cd1—N2—H2N2	110.4	C4'—N4—H2N4	133.7
H1N2—N2—H2N2	108.6	C4—N4—H2N4	110.8
C3—N3—C3'	31.6 (3)	Cd1—N4—H2N4	110.8
C3—N3—Cd1	106.7 (2)	H1N4—N4—H2N4	108.9
C3'—N3—Cd1	108.26 (14)	C4'—N4—H3N4	110.5
C3—N3—H1N3	110.4	C4—N4—H3N4	135.0
C3'—N3—H1N3	80.9	Cd1—N4—H3N4	110.5
Cd1—N3—H1N3	110.4	H1N4—N4—H3N4	30.0
C3—N3—H2N3	110.4	H2N4—N4—H3N4	81.8
C3'—N3—H2N3	133.2	C4'—N4—H4N4	110.5
Cd1—N3—H2N3	110.4	C4—N4—H4N4	83.0
H1N3—N3—H2N3	108.6	Cd1—N4—H4N4	110.5
C3—N3—H3N3	135.0	H1N4—N4—H4N4	130.7
C3'—N3—H3N3	110.0	H2N4—N4—H4N4	29.5
Cd1—N3—H3N3	110.0	H3N4—N4—H4N4	108.7

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N1···Cl2ii	0.90	2.73	3.6137 (15)	168
N1—H2N1···Cl2i	0.90	2.54	3.3941 (15)	159
N2—H2N2···Cl2iii	0.90	2.42	3.3123 (15)	171
N3—H1N3···Cl1iv	0.90	2.53	3.3581 (16)	154
N3—H2N3···Cl2	0.90	2.67	3.4919 (17)	152
N4—H3N4···Cl2ii	0.90	2.78	3.653 (2)	164
N4—H4N4···Cl2iii	0.90	2.85	3.708 (2)	161

Table 1

Selected bond lengths (Å)

Cd1—N2	2.3268 (15)
Cd1—N3	2.3314 (15)
Cd1—N1	2.3513 (14)
Cd1—N4	2.3971 (16)
Cd1—Cl1i	2.6200 (5)
Cd1—Cl1	2.7078 (5)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1N1⋯Cl2ii	0.90	2.73	3.6137 (15)	168
N1—H2N1⋯Cl2i	0.90	2.54	3.3941 (15)	159
N2—H2N2⋯Cl2iii	0.90	2.42	3.3123 (15)	171
N3—H1N3⋯Cl1iv	0.90	2.53	3.3581 (16)	154
N3—H2N3⋯Cl2	0.90	2.67	3.4919 (17)	152
N4—H3N4⋯Cl2ii	0.90	2.78	3.653 (2)	164
N4—H4N4⋯Cl2iii	0.90	2.85	3.708 (2)	161

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