(O,O′-Diethyl dithio­phosphato-κ2S,S′)(hydridotripyrazol-1-ylborato-κ3N2,N2′,N2′′)(triphenyl­phosphine-κP)ruthenium(II)

Tong, H.-C.; Chen Hsu, C.-Y.; Liang, Y.-R.; Lo, Y.H.; Lin, C.-H.

doi:10.1107/S160053680803170X

Volume 64
Part 11
Pages m1372-m1373
November 2008

Received 16 September 2008
Accepted 1 October 2008
Online 9 October 2008

Key indicators
Single-crystal X-ray study
T = 200 K
Mean (C-C) = 0.005 Å
Disorder in main residue
R = 0.036
wR = 0.093
Data-to-parameter ratio = 14.0
Details

(O,O'-Diethyl dithiophosphato-²S,S')(hydridotripyrazol-1-ylborato-³N²,N^2',N^2'')(triphenylphosphine-P)ruthenium(II)

Hung-Chun Tong,^a Chih-Yung Chen Hsu,^a Yao-Ren Liang,^a Yih Hsing Lo ^a ^* and Chia-Her Lin ^b

^aDepartment of Chemical Engineering, Tatung University, Taipei 104, Taiwan, and ^bDepartment of Chemistry, Chung-Yuan Christian University, Chung-Li 320, Taiwan
Correspondence e-mail: yhlo@ttu.edu.tw

Reaction of [Ru(Tp)Cl(PPh₃)₂] {where Tp is hydridotripyrazolylborate, BH[C₃H₃N₂)₃)]} with NH₄[S₂P(OEt)₂] in methanol afforded the title compound, [Ru(C₉H₁₀BN₆)(C₄H₁₀O₂PS₂)(C₁₈H₁₅P)], in which the Ru^II ion is in a slightly disorted octahedral coordination environment. The [S₂P(OEt)₂]^- ligand coordinates in a chelating mode with two similar Ru-S bond lengths and a slightly acute S-Ru-S angle. The atoms of both -OCH₂CH₃ groups of the diethyl dithiophosphate ligand are disordered over two sites with approximate occupancies of 0.76 and 0.24.

Related literature

For related structures, see: Alock et al. (1992); Burrows (2001); Hidai et al. (2000); Gemel et al. (1996); Jain & Jakkal (1996); Meno et al. (1995); Pavlik et al. (2005); Sellmann et al. (1999); Slugovc et al. (1998); Vit & Zdrazil (1989).

Experimental

Crystal data

[Ru(C₉H₁₀BN₆)(C₄H₁₀O₂PS₂)(C₁₈H₁₅P)]
M_r = 761.59
Monoclinic, P 2₁ /c
a = 12.4408 (2) Å
b = 13.7386 (2) Å
c = 20.3775 (3) Å
= 99.676 (1)°
V = 3433.36 (9) Å³
Z = 4
Mo K radiation
= 0.71 mm^-1
T = 200 (2) K
0.42 × 0.3 × 0.15 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: multi-scan (SORTAV; Blessing, 1995) T_min = 0.755, T_max = 0.901
24009 measured reflections
6265 independent reflections
5601 reflections with I > 2(I)
R_int = 0.051

Refinement

R[F² > 2(F²)] = 0.036
wR(F²) = 0.093
S = 1.05
6265 reflections
449 parameters
42 restraints
H-atom parameters constrained
_max = 1.43 e Å^-3
_min = -0.62 e Å^-3

Table 1
Selected geometric parameters (Å, °)

Ru1-N3	2.086 (2)
Ru1-N1	2.088 (2)
Ru1-N5	2.144 (3)
Ru1-P1	2.3171 (8)
Ru1-S1	2.4540 (8)
Ru1-S2	2.4635 (8)

N3-Ru1-N1	90.09 (9)
N3-Ru1-N5	83.57 (10)
N1-Ru1-N5	84.88 (10)
N3-Ru1-P1	90.07 (7)
N1-Ru1-P1	90.63 (7)
N5-Ru1-P1	172.20 (7)
N3-Ru1-S1	170.14 (7)
N1-Ru1-S1	93.07 (7)
N5-Ru1-S1	87.41 (7)
P1-Ru1-S1	99.23 (3)
N3-Ru1-S2	94.61 (7)
N1-Ru1-S2	169.78 (7)
N5-Ru1-S2	86.63 (7)
P1-Ru1-S2	98.42 (3)
S1-Ru1-S2	80.86 (3)

Data collection: COLLECT (Nonius, 1999); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: LH2697 ).

Acknowledgements

This research was supported by the National Science Council, Taiwan (NSC 97-2113-M-036-001-MY2), and in part by the project of the specific research fields in Tatung University, Taiwan (B96-C07-081), and the project of the specific research fields in Chung Yuan Christian University, Taiwan, under grant No. CYCU-97-CR-CH. We also thank Mr Ting Shen Kuo (Department of Chemistry, National Taiwan Normal University) for his assistance in X-ray single-crystal structure analysis.

References

Alock, N. W., Burns, I. D., Claire, K. S. & Hill, A. F. (1992). Inorg. Chem. 31, 2906-2908.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Burrows, A. D. (2001). CrystEngComm, 46, 1-5.
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Hidai, M., Kuwata, S. & Mizobe, Y. (2000). Acc. Chem. Res. 33, 46-52.
Jain, V. K. & Jakkal, V. S. (1996). J. Organomet. Chem. 515, 81-87.
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Nonius (1999). COLLECT. Nonius BV, Delft, The Netherlands.
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Pavlik, S., Mereiter, K., Puchberger, M. & Kirchner, K. (2005). Organometallics, 24, 3561-3575.
Sellmann, D., Utz, J. & Heineman, F. W. (1999). Eur. J. Inorg. Chem. 2, 341-346.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Slugovc, C., Mereiter, K., Schmidt, R. & Kirchner, K. (1998). Organometallics, 17, 827-831.
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metal-organic compounds

(O,O'-Diethyl dithiophosphato-2S,S')(hydridotripyrazol-1-ylborato-3N2,N2',N2'')(triphenylphosphine-P)ruthenium(II)