supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers buy article online

hg2353 scheme

Acta Cryst. (2007). E63, m3061    [ doi:10.1107/S1600536807058874 ]

Carbonylchlorido[tris(2-aminoethyl)amine]ruthenium(II) chloride

P. Klüfers and A. Zangl

Abstract top

In the monocationic octahedral complex, [RuCl(C6H18N4)(CO)]Cl, the ruthenium(II) centre is coordinated by a chloride and a carbonyl ligand and by the tetradentate tris(2-aminoethyl)amine (tren) chelator. The complex has approximate non-crystallographic Cs symmetry. In the crystal structure, N-H...Cl hydrogen bonds are found, mainly with the chloride counter-ion as the acceptor.

Comment top

The title compound, C7H18Cl2N4ORu, was obtained on the attempted preparation of [RuCl2(tren)] by refluxing RuCl3 with an equimolar amount of tris(2-aminoethyl)amine (tren) in DMF.

The molecular structure is shown in Fig. 1. The complex features three 5-membered rings: Ru–N1–C2–C3–N4 adopts a twist conformation on N1–C2 (Q2 = 0.444 (2) Å, φ2 = 241.5 (2)°), whereas Ru–N1–C5–C6–N7 (Q2 = 0.359 (2) Å, φ2 = 294.6 (3)°) shows an envelope conformation on C6. Ru–N1–C8–C9–N10 is twisted on N1–C8 (Q2 = 0.459 (2) Å, φ2 = 55.6 (2)°). Ring puckering parameters (Cremer & Pople, 1975) were calculated with PLATON (Spek, 2007).

Bond lengths and angles are normal.

The molecular packing including the hydrogen bond system is shown in Fig. 2. The search for hydrogen bonded molecular aggregates provided an infinite two-dimensional network (base vectors = [0 1 0], [2 0 1]) along the (1 0 − 2)-plane.

Related literature top

For related literature, see: Sullivan et al. (1978; Cremer & Pople (1975).

Experimental top

The title compound was obtained accidentally on the attempted preparation of [RuCl2(tren)] by refluxing RuCl3 * 3 H2O with an equimolar amount of tris(2-aminoethyl)amine (tren) and 7 equivalents of LiCl in DMF in analogy to a published procedure (Sullivan et al., 1978).

Refinement top

All H atoms were constructed and refined as riding on their parent atoms with one common isotropic displacement parameter.

Computing details top

Data collection: COLLECT (Hooft, 1997–2004); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with atom labels and anisotropic displacement ellipsoids (drawn at 50% probability level) for non-H atoms.
[Figure 2] Fig. 2. The packing of (I), viewed along [0 1 0].
Carbonylchlorido[tris(2-aminoethyl)amine]ruthenium(II) chloride top
Crystal data top
[RuCl(C6H18N4)(CO)]ClF000 = 696
Mr = 346.22Dx = 1.840 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3049 reflections
a = 10.1514 (2) Åθ = 3.1–27.5º
b = 8.52680 (10) ŵ = 1.66 mm−1
c = 14.7413 (3) ÅT = 200 (2) K
β = 101.6790 (7)ºBlock, yellow
V = 1249.58 (4) Å30.17 × 0.12 × 0.07 mm
Z = 4
Data collection top
KappaCCD
diffractometer		2863 independent reflections
Radiation source: rotating anode2562 reflections with I > 2σ(I)
Monochromator: MONTEL, graded multilayered X-ray opticsRint = 0.031
T = 200(2) Kθmax = 27.5º
φ and ω scansθmin = 3.1º
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)		h = −13→13
Tmin = 0.800, Tmax = 0.890k = −11→10
23413 measured reflectionsl = −19→19
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.020H-atom parameters constrained
wR(F2) = 0.048  w = 1/[σ2(Fo2) + (0.0181P)2 + 1.1292P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
2863 reflectionsΔρmax = 0.56 e Å−3
137 parametersΔρmin = −0.53 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[RuCl(C6H18N4)(CO)]ClV = 1249.58 (4) Å3
Mr = 346.22Z = 4
Monoclinic, P21/cMo Kα
a = 10.1514 (2) ŵ = 1.66 mm−1
b = 8.52680 (10) ÅT = 200 (2) K
c = 14.7413 (3) Å0.17 × 0.12 × 0.07 mm
β = 101.6790 (7)º
Data collection top
KappaCCD
diffractometer		2863 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)		2562 reflections with I > 2σ(I)
Tmin = 0.800, Tmax = 0.890Rint = 0.031
23413 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.020137 parameters
wR(F2) = 0.048H-atom parameters constrained
S = 1.06Δρmax = 0.56 e Å−3
2863 reflectionsΔρmin = −0.53 e Å−3
Special details top

Experimental. µ × r = 0.116, Tmin/Tmax = 0.899

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru0.263803 (15)0.685462 (18)0.091163 (10)0.01895 (6)
Cl10.09940 (5)0.70362 (7)−0.05312 (3)0.03170 (13)
O10.3830 (2)0.3964 (2)0.02630 (15)0.0593 (5)
N10.18612 (16)0.8875 (2)0.14884 (11)0.0220 (3)
N40.37625 (18)0.8578 (2)0.03603 (12)0.0285 (4)
H410.46670.84100.05770.0381 (16)*
H420.35930.8499−0.02750.0381 (16)*
N70.39797 (17)0.6894 (2)0.21966 (12)0.0247 (4)
H710.41620.58840.24030.0381 (16)*
H720.47750.73520.21300.0381 (16)*
N100.11750 (16)0.5702 (2)0.15115 (11)0.0240 (4)
H1010.06250.51100.10680.0381 (16)*
H1020.15950.50380.19720.0381 (16)*
C10.3369 (2)0.5085 (3)0.04993 (16)0.0343 (5)
C20.1995 (2)1.0192 (3)0.08523 (16)0.0310 (5)
H210.18451.12020.11470.0381 (16)*
H220.13101.00880.02730.0381 (16)*
C30.3396 (2)1.0170 (3)0.06317 (16)0.0329 (5)
H310.34281.09130.01200.0381 (16)*
H320.40601.05210.11820.0381 (16)*
C50.2655 (2)0.9209 (3)0.24410 (14)0.0300 (5)
H510.20380.95820.28360.0381 (16)*
H520.33081.00570.24050.0381 (16)*
C60.3403 (2)0.7782 (3)0.28834 (14)0.0307 (5)
H610.41330.81140.34000.0381 (16)*
H620.27790.71000.31410.0381 (16)*
C80.0435 (2)0.8471 (3)0.14896 (16)0.0299 (5)
H81−0.00930.84820.08470.0381 (16)*
H820.00470.92640.18510.0381 (16)*
C90.0346 (2)0.6870 (3)0.19081 (15)0.0292 (5)
H910.06680.69300.25880.0381 (16)*
H92−0.06040.65220.17850.0381 (16)*
Cl20.32744 (5)0.36408 (7)0.31352 (4)0.03583 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru0.01829 (9)0.02010 (9)0.01801 (9)−0.00241 (6)0.00263 (6)−0.00132 (6)
Cl10.0317 (3)0.0424 (3)0.0181 (2)−0.0134 (2)−0.0020 (2)0.0007 (2)
O10.0670 (13)0.0386 (11)0.0765 (14)0.0085 (10)0.0243 (11)−0.0213 (10)
N10.0230 (8)0.0200 (8)0.0226 (8)0.0004 (7)0.0039 (7)0.0014 (7)
N40.0253 (9)0.0384 (11)0.0225 (8)−0.0102 (8)0.0060 (7)0.0013 (8)
N70.0212 (8)0.0261 (9)0.0247 (9)−0.0008 (7)0.0001 (7)0.0038 (7)
N100.0228 (8)0.0243 (9)0.0233 (8)−0.0079 (7)0.0007 (7)0.0025 (7)
C10.0345 (12)0.0319 (12)0.0371 (12)−0.0037 (10)0.0082 (10)−0.0065 (10)
C20.0319 (11)0.0236 (11)0.0352 (12)0.0013 (9)0.0017 (9)0.0087 (9)
C30.0351 (12)0.0275 (12)0.0348 (12)−0.0104 (9)0.0045 (9)0.0082 (10)
C50.0385 (12)0.0267 (11)0.0239 (10)−0.0036 (9)0.0041 (9)−0.0065 (9)
C60.0337 (12)0.0374 (13)0.0180 (10)−0.0053 (10)−0.0020 (9)−0.0018 (9)
C80.0207 (10)0.0337 (12)0.0364 (12)0.0040 (9)0.0089 (9)0.0010 (10)
C90.0234 (10)0.0375 (12)0.0282 (11)−0.0055 (9)0.0087 (8)0.0010 (9)
Cl20.0257 (3)0.0361 (3)0.0443 (3)0.0040 (2)0.0038 (2)0.0146 (3)
Geometric parameters (Å, °) top
Ru—C11.838 (2)N10—H1010.9200
Ru—N72.0975 (17)N10—H1020.9200
Ru—N102.1176 (16)C2—C31.522 (3)
Ru—N42.1208 (17)C2—H210.9900
Ru—N12.1409 (17)C2—H220.9900
Ru—Cl12.4281 (5)C3—H310.9900
O1—C11.149 (3)C3—H320.9900
N1—C21.487 (3)C5—C61.510 (3)
N1—C81.489 (3)C5—H510.9900
N1—C51.498 (3)C5—H520.9900
N4—C31.484 (3)C6—H610.9900
N4—H410.9200C6—H620.9900
N4—H420.9200C8—C91.508 (3)
N7—C61.477 (3)C8—H810.9900
N7—H710.9200C8—H820.9900
N7—H720.9200C9—H910.9900
N10—C91.497 (3)C9—H920.9900
C1—Ru—N794.58 (9)H101—N10—H102108.1
C1—Ru—N1096.99 (8)O1—C1—Ru178.3 (2)
N7—Ru—N1090.72 (6)N1—C2—C3109.53 (17)
C1—Ru—N499.04 (9)N1—C2—H21109.8
N7—Ru—N491.91 (7)C3—C2—H21109.8
N10—Ru—N4163.50 (7)N1—C2—H22109.8
C1—Ru—N1175.95 (9)C3—C2—H22109.8
N7—Ru—N181.51 (6)H21—C2—H22108.2
N10—Ru—N182.04 (6)N4—C3—C2111.40 (17)
N4—Ru—N182.24 (7)N4—C3—H31109.3
C1—Ru—Cl190.85 (7)C2—C3—H31109.3
N7—Ru—Cl1174.57 (5)N4—C3—H32109.3
N10—Ru—Cl188.83 (5)C2—C3—H32109.3
N4—Ru—Cl187.02 (5)H31—C3—H32108.0
N1—Ru—Cl193.06 (5)N1—C5—C6112.32 (17)
C2—N1—C8112.88 (16)N1—C5—H51109.1
C2—N1—C5110.32 (16)C6—C5—H51109.1
C8—N1—C5112.42 (16)N1—C5—H52109.1
C2—N1—Ru105.61 (12)C6—C5—H52109.1
C8—N1—Ru104.53 (12)H51—C5—H52107.9
C5—N1—Ru110.72 (12)N7—C6—C5110.56 (17)
C3—N4—Ru110.29 (12)N7—C6—H61109.5
C3—N4—H41109.6C5—C6—H61109.5
Ru—N4—H41109.6N7—C6—H62109.5
C3—N4—H42109.6C5—C6—H62109.5
Ru—N4—H42109.6H61—C6—H62108.1
H41—N4—H42108.1N1—C8—C9110.39 (17)
C6—N7—Ru110.62 (12)N1—C8—H81109.6
C6—N7—H71109.5C9—C8—H81109.6
Ru—N7—H71109.5N1—C8—H82109.6
C6—N7—H72109.5C9—C8—H82109.6
Ru—N7—H72109.5H81—C8—H82108.1
H71—N7—H72108.1N10—C9—C8110.95 (16)
C9—N10—Ru110.59 (12)N10—C9—H91109.4
C9—N10—H101109.5C8—C9—H91109.4
Ru—N10—H101109.5N10—C9—H92109.4
C9—N10—H102109.5C8—C9—H92109.4
Ru—N10—H102109.5H91—C9—H92108.0
N7—Ru—N1—C2119.66 (13)C1—Ru—N10—C9−178.62 (14)
N10—Ru—N1—C2−148.41 (13)N7—Ru—N10—C986.67 (13)
N4—Ru—N1—C226.54 (12)N4—Ru—N10—C9−12.5 (3)
Cl1—Ru—N1—C2−60.03 (12)N1—Ru—N10—C95.35 (13)
N7—Ru—N1—C8−121.04 (13)Cl1—Ru—N10—C9−87.91 (12)
N10—Ru—N1—C8−29.11 (12)C8—N1—C2—C3−160.53 (18)
N4—Ru—N1—C8145.84 (13)C5—N1—C2—C372.8 (2)
Cl1—Ru—N1—C859.28 (12)Ru—N1—C2—C3−46.91 (19)
N7—Ru—N1—C50.25 (13)Ru—N4—C3—C2−23.8 (2)
N10—Ru—N1—C592.17 (13)N1—C2—C3—N448.3 (2)
N4—Ru—N1—C5−92.87 (13)C2—N1—C5—C6−138.18 (19)
Cl1—Ru—N1—C5−179.44 (12)C8—N1—C5—C694.9 (2)
C1—Ru—N4—C3−177.75 (15)Ru—N1—C5—C6−21.6 (2)
N7—Ru—N4—C3−82.80 (14)Ru—N7—C6—C5−39.3 (2)
N10—Ru—N4—C316.2 (3)N1—C5—C6—N740.3 (2)
N1—Ru—N4—C3−1.64 (13)C2—N1—C8—C9163.23 (18)
Cl1—Ru—N4—C391.87 (13)C5—N1—C8—C9−71.2 (2)
C1—Ru—N7—C6−157.49 (15)Ru—N1—C8—C948.95 (19)
N10—Ru—N7—C6−60.42 (14)Ru—N10—C9—C820.0 (2)
N4—Ru—N7—C6103.28 (14)N1—C8—C9—N10−47.2 (2)
N1—Ru—N7—C621.42 (13)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N4—H41···Cl2i0.922.533.3569 (19)150
N7—H71···Cl20.922.463.2442 (18)144
N7—H72···Cl2i0.922.363.2830 (18)176
N10—H101···Cl1ii0.922.483.3319 (17)154
N10—H102···Cl20.922.473.3609 (18)164
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x, −y+1, −z.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N4—H41···Cl2i0.922.533.3569 (19)150
N7—H71···Cl20.922.463.2442 (18)144
N7—H72···Cl2i0.922.363.2830 (18)176
N10—H101···Cl1ii0.922.483.3319 (17)154
N10—H102···Cl20.922.473.3609 (18)164
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x, −y+1, −z.
Acknowledgements top

The authors thank Dr Peter Mayer for professional support.

references
References top

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115–119.

Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.

Cremer, D. & Pople, J. A. (1975). J. Am. Chem. Soc. 97, 1354–1358.

Hooft, R. W. W. (1997–2004). COLLECT. Bruker–Nonius BV, Delft, The Netherlands.

Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press.

Sheldrick, G. M. (1997). SHELXL97. University of Göttingen, Germany.

Sheldrick, G. M. (2001). SADABS. Version 2. University of Göttingen, Germany.

Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13.

Sullivan, B. P., Salmon, D. J. & Meyer, T. J. (1978). Inorg. Chem. 17, 3334–3341.