Bis[O-propan-2-yl (4-eth­oxy­phen­yl)dithio­phospho­nato-κ2S,S′]nickel(II)

Sewpersad, S.; Van Zyl, W.E.

doi:10.1107/S1600536812045114

Volume 68
Part 12
Page m1457
December 2012

Received 19 October 2012
Accepted 31 October 2012
Online 3 November 2012

Key indicators
Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.003 Å
R = 0.030
wR = 0.065
Data-to-parameter ratio = 19.9
Details

Bis[O-propan-2-yl (4-ethoxyphenyl)dithiophosphonato-²S,S']nickel(II)

Shirveen Sewpersad ^a and Werner E. Van Zyl ^a ^*

^aSchool of Chemistry and Physics, University of KwaZulu-Natal, Westville Campus, Private Bag X54001, Durban 4000, South Africa
Correspondence e-mail: vanzylw@ukzn.ac.za

The title compound, [Ni(C₁₁H₁₆O₂PS₂)₂], is a neutral four-coordinate mononuclear complex with a square-planar geometry. The complex lies on an inversion center. The metal atom is surrounded by two chelating isobidentate O-propan-2-yl (4-ethoxyphenyl)dithiophosphonate ligands in a trans configuration binding through the S-donor atoms. The Ni-S bond lengths are 2.2328 (5) and 2.2369 (5) Å, an insignificant difference to be considered anisobidentate. The NiP separation is 2.8224 (5) Å and the S-P bond lengths are 2.0035 (7) and 2.0053 (7) Å. The S-Ni-S (chelating) and S-Ni-S (trans) bond angles are 88.321 (18) and 180°. The Ni-S-P bond angles are 83.26 (2) and 83.33 (2)°, indicating a very minor distortion from ideal square-planar geometry for the Ni atom. The P atom, however, is distorted quite significantly from an ideal tetrahedral geometry, as reflected by the S-P-S and O-P-C bond angles of 101.93 (3) and 100.70 (7)°, respectively.

Related literature

For information on dithiophosphonate compounds, see: Van Zyl & Fackler (2000); Van Zyl (2010). For examples of nickel(II) dithiophosphonate complexes, see: Liu et al. (2004); Gray et al. (2004); Aragoni et al. (2007); Arca et al. (1997); Malatesta & Pizzotti (1945); Hartung (1967).

Experimental

Crystal data

[Ni(C₁₁H₁₆O₂PS₂)₂]
M_r = 609.37
Triclinic, $[P \overline 1]$
a = 7.8893 (6) Å
b = 8.4178 (7) Å
c = 11.4825 (10) Å
= 109.530 (4)°
= 101.959 (4)°
= 93.913 (5)°
V = 695.22 (10) Å³
Z = 1
Mo K radiation
= 1.14 mm^-1
T = 173 K
0.39 × 0.26 × 0.14 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.665, T_max = 0.857
14410 measured reflections
3062 independent reflections
2381 reflections with I > 2(I)
R_int = 0.035

Refinement

R[F² > 2(F²)] = 0.030
wR(F²) = 0.065
S = 1.02
3062 reflections
154 parameters
H-atom parameters constrained
_max = 0.27 e Å^-3
_min = -0.31 e Å^-3

Data collection: COLLECT (Nonius, 2000); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; 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: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BH2460 ).

Acknowledgements

The authors thank the National Research Foundation (NRF) and UKZN for financial support.

References

Aragoni, M. C., Arca, M., Devillanova, F. A., Hursthouse, M. B., Huth, S. L., Isaia, F., Lippolis, V., Mancini, A., Soddu, S. & Verani, G. (2007). Dalton Trans. pp. 2127-2134.
Arca, M., Cornia, A., Devillanova, F. A., Fabretti, A. C., Isaia, F., Lippolis, V. & Verani, G. (1997). Inorg. Chim. Acta, 262, 81-84.
Gray, I. P., Slawin, A. M. Z. & Woollins, J. D. (2004). Dalton Trans. pp. 2477-2486.
Hartung, H. (1967). Z. Chem. 7, 241.
Liu, H.-L., Mao, H.-Y., Xu, C., Zhang, H.-Y., Hou, H.-W., Wu, Q., Zhu, Y., Ye, B.-X. & Yuan, L.-J. (2004). Polyhedron, 23, 1799-1804.
Malatesta, L. & Pizzotti, R. (1945). Chim. Ind. (Milan), 27, 6-9.
Nonius (2000). COLLECT. 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. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Van Zyl, W. E. (2010). Comments Inorg. Chem. 31, 13-45.
Van Zyl, W. E. & Fackler, J. P. (2000). Phosphorus Sulfur Silicon Relat. Elem. 167, 117-132.

metal-organic compounds

Bis[O-propan-2-yl (4-ethoxyphenyl)dithiophosphonato-2S,S']nickel(II)