cis,fac-Dichlorido{N-[3,5-di-tert-butyl-2-(trimethyl­silyl­oxy)benz­yl]-N,N-bis­(2-pyridylmeth­yl)amine}(dimethyl sulfoxide)ruthenium(II) dichloro­methane disolvate

Fischer, P.J.; Minasian, S.G.; Arnold, J.

doi:10.1107/S1600536809041324

Volume 65
Part 11
Pages m1371-m1372
November 2009

Received 7 October 2009
Accepted 9 October 2009
Online 17 October 2009

Key indicators
Single-crystal X-ray study
T = 126 K
Mean (C-C) = 0.008 Å
Some non-H atoms missing,
Disorder in solvent or counterion
R = 0.049
wR = 0.124
Data-to-parameter ratio = 18.3
Details

cis,fac-Dichlorido{N-[3,5-di-tert-butyl-2-(trimethylsilyloxy)benzyl]-N,N-bis(2-pyridylmethyl)amine}(dimethyl sulfoxide)ruthenium(II) dichloromethane disolvate

Paul J. Fischer,^a ^* Stefan G. Minasian ^b and John Arnold ^b

^aChemistry Department, Macalester College, 1600 Grand Avenue, Saint Paul, MN 55105, USA, and ^bChemistry Department, University of California, Berkeley, CA 94720-1460, USA
Correspondence e-mail: fischer@macalester.edu

Reaction of dichloridotetrakis(dimethyl sulfoxide)ruthenium(II) and N-[3,5-di-tert-butyl-2-(trimethylsilyloxy)benzyl]-N,N-bis(2-pyridylmethyl)amine (BPPA-TMS) affords the thermodynamic product cis,fac-[RuCl₂(BPPA-TMS)(DMSO)] and kinetic product trans,mer-[RuCl₂(BPPA-TMS)(DMSO)]. The title complex, [RuCl₂(C₃₀H₄₃N₃OSi)(C₂H₆OS)]·2CH₂Cl₂, crystallizes as a dichloromethane disolvate, with two formula units in the asymmetric unit. The complex exhibits a distorted-octahedral geometry about the low spin d⁶ Ru^II center. The BPPA-TMS ligand is coordinated in a facial fashion, with the DMSO ligand cis to the aliphatic nitrogen atom of the BPPA-TMS ligand. One of the two dichloromethane solvate molecules is disordered over two positions in a 0.695:0.305 ratio.

Related literature

The application of tetradentate monoanionic (TDMA) ligands for stabilizing reactive metal complexes motivates ligand design efforts (Chomitz & Arnold, 2009). The TDMA precursor N,N-bis-(2-pyridylmethyl)(2-hydroxy-3,5-di-tert-butylbenzyl)amine (HBPPA) has been employed to prepare main group, transition metal and actinide BPPA complexes (Chomitz et al., 2007; Marinescu et al., 2007) but Ru(BPPA) complexes have not been reported. Coordination complexes of ruthenium that contain chlorido, DMSO, and pyridylic ligands demonstrate promising applications as chemotherapeutic agents (Velders et al., 2004; Bratsos et al., 2007). Substitution mechanisms for related complexes have been studied, see: Mola et al. (2007).

Experimental

Crystal data

[RuCl₂(C₃₀H₄₃N₃OSi)(C₂H₆OS)]·2CH₂Cl₂
M_r = 909.71
Triclinic, $[P \overline 1]$
a = 10.913 (2) Å
b = 18.435 (4) Å
c = 22.413 (5) Å
= 82.039 (3)°
= 76.212 (3)°
= 89.148 (3)°
V = 4336.4 (15) Å³
Z = 4
Mo K radiation
= 0.84 mm^-1
T = 126 K
0.33 × 0.31 × 0.02 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001) T_min = 0.769, T_max = 0.988
52307 measured reflections
15775 independent reflections
8958 reflections with I > 2(I)
R_int = 0.085

Refinement

R[F² > 2(F²)] = 0.049
wR(F²) = 0.124
S = 0.98
15775 reflections
861 parameters
24 restraints
H-atom parameters constrained
_max = 0.70 e Å^-3
_min = -0.57 e Å^-3

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); 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 and PLATON (Spek, 2009).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT5088 ).

Acknowledgements

The donors of the Petroleum Research Fund, administered by the American Chemical Society (ACS-PRF 48003-UFS), supported this research. PJF is grateful to Henry S. LaPierre and Victor G. Young, Jr for their expertise, and to the John Arnold research group for their hospitality.

References

Bratsos, I., Serli, B., Zangrando, E., Katsaros, N. & Alessio, E. (2007). Inorg. Chem., 46, 975-992.
Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Chomitz, W. A. & Arnold, J. (2009). Chem. Eur. J. 15, 2020-2030.
Chomitz, W. A., Minasian, S. G., Sutton, A. D. & Arnold, J. (2007). Inorg. Chem. 46, 7199-7209.
Marinescu, S. C., Agapie, T., Day, M. W. & Bercaw, J. E. (2007). Organometallics, 26, 1178-1190.
Mola, J., Romero, I., Rodriguez, M., Bozoglian, F., Poater, A., Sola, M., Parella, T., Benet-Buchholz, J., Fontrodona, X. & Llobet, A. (2007). Inorg. Chem. 46, 10707-10716.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.
Velders, A. H., Bergamo, A., Alessio, E., Zangrando, E., Haasnoot, J. G., Casarsa, C., Cocchietto, M., Zorzet, S. & Sava, G. (2004). J. Med. Chem. 47, 1110-1121.

metal-organic compounds