cis-Diiodido(N,N,N',N'-tetra-methyl-ethylenediamine-κ(2)N,N')palladium(II).

In the title complex, cis-[PdI(2)(C(6)H(16)N(2))], the Pd(II) atom lies on a crystallographic twofold rotation axis and is four-coordinated by the two N atoms of a chelating N,N,N',N'-tetra-methyl-ethylenediamine ligand [Pd-N = 2.125 (3) Å] and two I atoms [Pd-I = 2.5833 (4) Å], displaying a distorted square-planar geometry (r.m.s. deviation = 0.005 Å), imposed by the small bite of the chelating ligand [N-Pd-N angle = 84.68 (18)°].

Related literature

For related diiodido complexes, see: Jones et al. (2007 ▶); Wursche et al. (1999 ▶); Dodd et al. (2006 ▶); Alsters et al. (1993 ▶); Bhattacharyya et al. (2009 ▶); Ha (2009 ▶, 2010 ▶). For mol­ecular parameters in related dichlorido complexes, see: Boyle et al. (2004 ▶); Iball et al. (1975 ▶). For a description of the Cambridge Structural Database, see: Allen (2002 ▶).

Experimental

Crystal data

[PdI2(n class="CellLine">C6H16N2)]

M = 476.41

Monoclinic,

a = 7.9266 (4) Å

b = 14.6911 (7) Å

c = 10.5309 (5) Å

β = 107.262 (2)°

V = 1171.09 (10) Å3

Z = 4

Mo Kα radiation

μ = 6.81 mm−1

T = 100 K

0.22 × 0.15 × 0.03 mm

Data collection

Bruker SMART APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2003 ▶) T min = 0.581, T max = 0.822

6502 measured reflections

1351 independent reflections

1326 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.060

S = 1.14

1351 reflections

53 parameters

H-atom parameters constrained

Δρmax = 1.23 e Å−3

Δρmin = −0.73 e Å−3

Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT (Bruker, 2003 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812033004/lr2073sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812033004/lr2073Isup2.hkl

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

[PdI2(C6H16N2)]	F(000) = 872
Mr = 476.41	Dx = 2.702 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 4971 reflections
a = 7.9266 (4) Å	θ = 2.8–28.1°
b = 14.6911 (7) Å	µ = 6.81 mm−1
c = 10.5309 (5) Å	T = 100 K
β = 107.262 (2)°	Needle, red
V = 1171.09 (10) Å3	0.22 × 0.15 × 0.03 mm
Z = 4

Bruker SMART APEX CCD diffractometer	1351 independent reflections
Radiation source: fine-focus sealed tube	1326 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
Detector resolution: 8.26 pixels mm-1	θmax = 28.1°, θmin = 2.8°
ω scan	h = −10→10
Absorption correction: multi-scan (SADABS; Bruker, 2003)	k = −18→18
Tmin = 0.581, Tmax = 0.822	l = −13→13
6502 measured reflections

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.060	H-atom parameters constrained
S = 1.14	w = 1/[σ2(Fo2) + (0.025P)2 + 10.9315P] where P = (Fo2 + 2Fc2)/3
1351 reflections	(Δ/σ)max = 0.001
53 parameters	Δρmax = 1.23 e Å−3
0 restraints	Δρmin = −0.73 e Å−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.Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)- 0.3294 (0.0368) x + 14.6093 (0.0042) y + 1.1036 (0.0293) z = 6.0620 (0.0112)* 0.0000 (0.0000) N1 * 0.0000 (0.0000) C2 * 0.0000 (0.0000) C3Rms deviation of fitted atoms = 0.00000.3294 (0.0369) x + 14.6093 (0.0042) y - 1.1036 (0.0293) z = 5.8396 (0.0312)Angle to previous plane (with approximate e.s.d.) = 12.10 (0.08)* 0.0000 (0.0000) N1_$1 * 0.0000 (0.0000) C2_$1 * 0.0000 (0.0000) C3_$1Rms deviation of fitted atoms = 0.00005.5219 (0.0048) x - 0.0000 (0.0000) y - 9.3919 (0.0040) z = 0.4130 (0.0034)Angle to previous plane (with approximate e.s.d.) = 84.35 (0.22)* 0.0000 (0.0000) Pd1 * 0.0062 (0.0019) N1 * 0.0050 (0.0015) I1 * -0.0062 (0.0019) N1_$1 * -0.0050 (0.0015) I1_$1Rms deviation of fitted atoms = 0.0050

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
Pd1	0.5000	0.51798 (3)	0.2500	0.01073 (10)
I1	0.71154 (4)	0.644568 (18)	0.37384 (3)	0.02349 (10)
N1	0.3317 (4)	0.4111 (2)	0.1504 (3)	0.0136 (6)
C1	0.4427 (5)	0.3275 (3)	0.1794 (4)	0.0191 (8)
H1A	0.5175	0.3246	0.1192	0.023*
H1B	0.3656	0.2731	0.1632	0.023*
C2	0.1807 (5)	0.4035 (3)	0.2057 (4)	0.0209 (8)
H2A	0.1129	0.4603	0.1896	0.031*
H2B	0.2251	0.3922	0.3016	0.031*
H2C	0.1045	0.3529	0.1625	0.031*
C3	0.2605 (6)	0.4205 (3)	0.0038 (4)	0.0216 (8)
H3A	0.1947	0.3654	−0.0336	0.032*
H3B	0.3584	0.4291	−0.0341	0.032*
H3C	0.1816	0.4733	−0.0176	0.032*

	U11	U22	U33	U12	U13	U23
Pd1	0.01163 (18)	0.01133 (18)	0.00958 (18)	0.000	0.00366 (13)	0.000
I1	0.02803 (17)	0.02164 (16)	0.01984 (16)	−0.01018 (10)	0.00561 (11)	−0.00239 (10)
N1	0.0124 (14)	0.0169 (15)	0.0119 (14)	−0.0017 (12)	0.0040 (11)	−0.0028 (12)
C1	0.0214 (19)	0.0140 (17)	0.022 (2)	−0.0004 (15)	0.0073 (16)	−0.0038 (15)
C2	0.0145 (18)	0.029 (2)	0.022 (2)	−0.0052 (15)	0.0090 (15)	−0.0034 (17)
C3	0.024 (2)	0.025 (2)	0.0134 (18)	−0.0046 (16)	0.0033 (15)	−0.0043 (16)

Pd1—N1	2.125 (3)	C1—H1A	0.9900
Pd1—N1i	2.125 (3)	C1—H1B	0.9900
Pd1—I1	2.5833 (4)	C2—H2A	0.9800
Pd1—I1i	2.5833 (4)	C2—H2B	0.9800
N1—C2	1.483 (5)	C2—H2C	0.9800
N1—C3	1.484 (5)	C3—H3A	0.9800
N1—C1	1.488 (5)	C3—H3B	0.9800
C1—C1i	1.494 (8)	C3—H3C	0.9800
N1—Pd1—N1i	84.68 (18)	N1—C1—H1B	109.5
N1—Pd1—I1	178.36 (9)	C1i—C1—H1B	109.5
N1i—Pd1—I1	93.71 (9)	H1A—C1—H1B	108.1
N1—Pd1—I1i	93.71 (9)	N1—C2—H2A	109.5
N1i—Pd1—I1i	178.36 (9)	N1—C2—H2B	109.5
I1—Pd1—I1i	87.906 (18)	H2A—C2—H2B	109.5
C2—N1—C3	108.3 (3)	N1—C2—H2C	109.5
C2—N1—C1	110.7 (3)	H2A—C2—H2C	109.5
C3—N1—C1	108.1 (3)	H2B—C2—H2C	109.5
C2—N1—Pd1	108.9 (2)	N1—C3—H3A	109.5
C3—N1—Pd1	115.7 (2)	N1—C3—H3B	109.5
C1—N1—Pd1	105.2 (2)	H3A—C3—H3B	109.5
N1—C1—C1i	110.6 (3)	N1—C3—H3C	109.5
N1—C1—H1A	109.5	H3A—C3—H3C	109.5
C1i—C1—H1A	109.5	H3B—C3—H3C	109.5
N1i—Pd1—N1—C2	104.9 (3)	I1i—Pd1—N1—C1	166.5 (2)
I1i—Pd1—N1—C2	−74.8 (2)	C2—N1—C1—C1i	−77.3 (4)
N1i—Pd1—N1—C3	−133.0 (3)	C3—N1—C1—C1i	164.2 (4)
I1i—Pd1—N1—C3	47.3 (3)	Pd1—N1—C1—C1i	40.1 (4)
N1i—Pd1—N1—C1	−13.83 (18)	N1—C1—C1i—N1i	−56.4 (6)