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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 [sigma](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
Open access

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

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 RuII 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[Chomitz, W. A. & Arnold, J. (2009). Chem. Eur. J. 15, 2020-2030.]). 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[Chomitz, W. A., Minasian, S. G., Sutton, A. D. & Arnold, J. (2007). Inorg. Chem. 46, 7199-7209.]; Marinescu et al., 2007[Marinescu, S. C., Agapie, T., Day, M. W. & Bercaw, J. E. (2007). Organometallics, 26, 1178-1190.]) 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[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.]; Bratsos et al., 2007[Bratsos, I., Serli, B., Zangrando, E., Katsaros, N. & Alessio, E. (2007). Inorg. Chem., 46, 975-992.]). Substitution mechanisms for related complexes have been studied, see: Mola et al. (2007[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.]).

[Scheme 1]

Experimental

Crystal data
  • [RuCl2(C30H43N3OSi)(C2H6OS)]·2CH2Cl2

  • Mr = 909.71

  • Triclinic, [P \overline 1]

  • a = 10.913 (2) Å

  • b = 18.435 (4) Å

  • c = 22.413 (5) Å

  • [alpha] = 82.039 (3)°

  • [beta] = 76.212 (3)°

  • [gamma] = 89.148 (3)°

  • V = 4336.4 (15) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 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[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.769, Tmax = 0.988

  • 52307 measured reflections

  • 15775 independent reflections

  • 8958 reflections with I > 2[sigma](I)

  • Rint = 0.085

Refinement
  • R[F2 > 2[sigma](F2)] = 0.049

  • wR(F2) = 0.124

  • S = 0.98

  • 15775 reflections

  • 861 parameters

  • 24 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.70 e Å-3

  • [Delta][rho]min = -0.57 e Å-3

Data collection: SMART (Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).


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.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Chomitz, W. A. & Arnold, J. (2009). Chem. Eur. J. 15, 2020-2030.  [CrossRef] [ChemPort]
Chomitz, W. A., Minasian, S. G., Sutton, A. D. & Arnold, J. (2007). Inorg. Chem. 46, 7199-7209.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Marinescu, S. C., Agapie, T., Day, M. W. & Bercaw, J. E. (2007). Organometallics, 26, 1178-1190.  [CSD] [CrossRef] [ChemPort]
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.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [ISI] [CrossRef] [details]
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.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]


Acta Cryst (2009). E65, m1371-m1372   [ doi:10.1107/S1600536809041324 ]

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