(1H-Pyrazole-κN)bis­(tri-tert-but­oxy­silane­thiol­ato-κ2O,S)cadmium

Baranowska, K.; Bulman, M.; Dołęga, A.

doi:10.1107/S1600536812047186

Volume 68
Part 12
Page m1515
December 2012

Received 14 November 2012
Accepted 16 November 2012
Online 24 November 2012

Key indicators
Single-crystal X-ray study
T = 120 K
Mean (C-C) = 0.005 Å
Disorder in main residue
R = 0.039
wR = 0.103
Data-to-parameter ratio = 17.1
Details

(1H-Pyrazole-N)bis(tri-tert-butoxysilanethiolato-²O,S)cadmium

Katarzyna Baranowska,^a Mateusz Bulman ^a and Anna Dolega ^a ^*

^aDepartment of Inorganic Chemistry, Faculty of Chemistry, Gdansk University of Technology, 11/12 G. Narutowicz St., 80233 - PL Gdansk, Poland
Correspondence e-mail: anndoleg@pg.gda.pl

The Cd^II atom in the title complex, [Cd(C₁₂H₂₇O₃SSi)₂(C₃H₄N₂)], is penta-coordinated by two O and two S atoms from the O,S-chelating silanethiolate residue and one pyrazole N atom in a distorted geometry that is slightly closer to trigonal-bipyramidal than to square-based pyramidal. The pyrazole ligand is stabilized within the complex by an intramolecular N-HO hydrogen bond. One of the tert-butyl groups is disordered over two orientations with occupancy ratio of 0.534 (6):0.466 (6).

Related literature

For similar compounds, see: Dolega et al. (2005, 2006, 2008, 2009); Dolega (2010). For the synthetic procedure, see: Pladzyk et al. (2011). For a description of the geometry of complexes with five-coordinate metal atoms, see: Addison et al. (1984).

Experimental

Crystal data

[Cd(C₁₂H₂₇O₃SSi)₂(C₃H₄N₂)]
M_r = 739.45
Triclinic, $[P \overline 1]$
a = 9.4445 (4) Å
b = 12.7322 (4) Å
c = 16.9153 (5) Å
= 109.098 (3)°
= 92.905 (3)°
= 96.050 (3)°
V = 1903.53 (12) Å³
Z = 2
Mo K radiation
= 0.78 mm^-1
T = 120 K
0.2 × 0.18 × 0.08 mm

Data collection

Agilent Xcalibur Sapphire2 diffractometer
11378 measured reflections
7083 independent reflections
5935 reflections with I > 2(I)
R_int = 0.025

Refinement

R[F² > 2(F²)] = 0.039
wR(F²) = 0.103
S = 1.06
7083 reflections
414 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 1.11 e Å^-3
_min = -0.65 e Å^-3

Table 1
Selected bond lengths (Å)

Cd1-N1	2.298 (3)
Cd1-O1	2.536 (2)
Cd1-O4	2.649 (2)
Cd1-S1	2.4438 (8)
Cd1-S2	2.4503 (8)
Si1-S1	2.0917 (11)
Si2-S2	2.0781 (12)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-H2O5	0.83 (4)	2.14 (4)	2.959 (3)	167 (4)

Data collection: CrysAlis PRO (Agilent, 2010); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: VN2060 ).

References

Addison, A. W., Rao, T. N., Reedijk, J., van Rijn, J. & Verschoor, G. C. (1984). J. Chem. Soc. Dalton Trans. pp. 1349-1356.
Agilent (2010). CrysAlis PRO. Agilent Technologies, Yarnton, England.
Dolega, A. (2010). Coord. Chem. Rev. 254, 916-937.
Dolega, A., Baranowska, K., Gudat, D., Herman, A., Stangret, J., Konitz, A., Smiechowski, M. & Godlewska, S. J. (2009). Eur. J. Inorg. Chem. pp. 3644-3660.
Dolega, A., Baranowska, K. & Jarzabek, Z. (2008). Acta Cryst. E64, m1515.
Dolega, A., Chojnacki, J., Konitz, A., Komuda, W. & Wojnowski, W. (2006). Acta Cryst. E62, m636-m639.
Dolega, A., Ciborska, A., Chojnacki, J., Walewski, M. & Wojnowski, W. (2005). Thermochim. Acta, 429, 103-109.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Pladzyk, A., Baranowska, K., Gudat, D., Godlewska, S., Wieczerzak, M., Chojnacki, J., Bulman, M., Januszewicz, K. & Dolega, A. (2011). Polyhedron, 30, 2400-2405.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds

(1H-Pyrazole-N)bis(tri-tert-butoxysilanethiolato-2O,S)cadmium