Dicarbonyl­dichlorido(N,N,N′,N′-tetra­methyl­ethylenediamine)­ruthenium(II)

Ahmad O Baghlaf; Muhammad Ishaq; Salih S Al-Juaid; Abdullah M Asiri; Muhammad Nadeem Arshad

doi:10.1107/S1600536811022227

. 2011 Jun 18;67(Pt 7):m925. doi: 10.1107/S1600536811022227

Dicarbonyldichlorido(N,N,N′,N′-tetramethylethylenediamine)ruthenium(II)

Ahmad O Baghlaf ^a, Muhammad Ishaq ^a, Salih S Al-Juaid ^a, Abdullah M Asiri ^b,^‡, Muhammad Nadeem Arshad ^c,^*

PMCID: PMC3152070 PMID: 21836909

Abstract

In the title compound, [RuCl₂(C₆H₁₆N₂)(CO)₂], the geometry around the Ru^II atom is a distorted RuC₂N₂Cl₂ octahedron, with pairs of C and Cl atoms trans to each other and the N atoms of the bidentate ligand in a cis conformation. The five-membered chelate ring is puckered on the C—C bond.

Related literature

For background to ruthenium carbonyl derivatives, see: Manchot & Konig (1924 ▶); Stephenson & Wilkinson (1966 ▶); Kingston et al. (1967 ▶); Baghlaf et al. (2007 ▶); Campbell (1975 ▶); Padhey & Kaufman (1985 ▶). For a related structure, see: Bakar et al. (1993 ▶).

Experimental

Crystal data

[RuCl₂(C₆H₁₆N₂)(CO)₂]
M _r = 344.20
Monoclinic,
a = 7.463 (6) Å
b = 14.579 (6) Å
c = 12.718 (12) Å
β = 106.37 (8)°
V = 1327.7 (17) Å³
Z = 4
Mo Kα radiation
μ = 1.57 mm⁻¹
T = 160 K
0.38 × 0.38 × 0.25 mm

Data collection

Enraf–Nonius CAD-4 diffractometer
Absorption correction: ψ scan (North et al., 1968 ▶) T _min = 0.591, T _max = 0.69
3153 measured reflections
2877 independent reflections
2644 reflections with I > 2σ(I)
R _int = 0.015
2 standard reflections every 100 reflections intensity decay: 5%

Refinement

R[F ² > 2σ(F ²)] = 0.023
wR(F ²) = 0.061
S = 1.07
2877 reflections
184 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.06 e Å⁻³
Δρ_min = −0.48 e Å⁻³

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995 ▶); program(s) used to solve structure: DIRDIF99 (Beurskens et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶) and PLATON (Spek, 2009 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811022227/hb5901sup1.cif

e-67-0m925-sup1.cif^{(17.7KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811022227/hb5901Isup2.hkl

e-67-0m925-Isup2.hkl^{(138.3KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Ru1—C1	1.872 (3)
Ru1—C2	1.872 (2)
Ru1—N2	2.211 (2)
Ru1—N1	2.220 (2)
Ru1—Cl1	2.413 (2)
Ru1—Cl2	2.408 (2)

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N2—Ru1—N1

82.75 (9)

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Acknowledgments

The authors would like to thank the Chemistry Department, King Abdul Aziz University, Jeddah, Saudi Arabia, for providing the research facilities.

supplementary crystallographic information

Comment

The salt [Ru(CO)2Cl2]n was first reported by (Manchot & Konig, 1924) but its importance and chemistry was shown in late 1960's by (Stephenson & Wilkinson, 1966), (Kingston et al., 1967) who have reported several compounds of the type [Ru(CO)2Cl2L2] where L=monodentate ligand. This was due to the fact that the salt [Ru(CO)2Cl2]n has proved a useful precursor for the synthesis of a variety of organometallic compounds. We have also reported from our laboratories compounds with ligands containing N, O and S atom as electron donor (e.g. Baghlaf et al., 2007). However (Campbell (1975) and Padhey & Kaufman (1985) have reported about remarkable biological activities of such compounds against microbes, viruses and tumours. This has been the main reason for our research activity in the field of bio-inorganic chemistry of transition metal complexes. The metal atom Ru in the salt [Ru(CO)2Cl2]n being electron deficient acts as electron acceptor. This enhances its ability to coordinate with electron donor ligand (TMEDA) to give a stable octahedral electron rich compound of low ionization energy [Ru(CO)2Cl2TMEDA]. The bidentate nature of the ligand (TMEDA) has also been reported in the X-ray structure of the complex [Mo(CO)₄TMEDA] by (Bakar et al., 1993).

In the crystal structure of title compound, ruthenium atom is almost octahedrally coordinated to the two nitrogen-donors atoms of tetramethyl ethylene-1,2-diamine (TMEDA), two chloro and two carbonyl groups. A five membered non-planer ring formed through Ru1/N1/C5/C6/N2 as both of the carbon atoms are sp³ hybridized. The root mean square deniavtion for the ring measure 0.2149Å with the maximum deviation from C5 and C6 measures -0.2999 (19) Å and 0.3144 (19)Å respectively.

Experimental

In a 100-ml round bottom flask fitted with nitrogen gas inlet, water condenser and magnetic stirrer was added 0.2 g of [Ru(CO)₂ Cl₂]n and 0.5 ml of tetramethylethylene diamine (TMEDA) in 15 ml MeOH. The reaction mixture was heated at about 70 °C for 1 h. The yellow green solution was reduced in volume and passed through a small alumina column (15 g. Al₂O₃). The yellow band was eluted with MeOH. The solvent was reduced in volume and on cooling it gave yellow blocks of (I). Yield 70%.