Chlorido{4-ethyl-1-[1-(pyrazin-2-yl)ethyl­idene]thio­semicabazidato-κS}bis­(triphenyl­phosphane-κP)silver(I)

Venkatraman, R.; Ruddock, K.D.; Das, H.S.; Hossain, M.A.; Fronczek, F.R.

doi:10.1107/S1600536813003152

Volume 69
Part 3
Pages m137-m138
March 2013

Received 6 November 2012
Accepted 30 January 2013
Online 6 February 2013

Key indicators
Single-crystal X-ray study
T = 90 K
Mean (C-C) = 0.005 Å
R = 0.042
wR = 0.103
Data-to-parameter ratio = 27.4
Details

Chlorido{4-ethyl-1-[1-(pyrazin-2-yl)ethylidene]thiosemicabazidato-S}bis(triphenylphosphane-P)silver(I)

Ramaiyer Venkatraman,^a ^* Kleopatra D. Ruddock,^a Himangshu S. Das,^b Md. Alamgir Hossain ^a and Frank R. Fronczek ^c

^aDepartment of Chemistry and Biochemistry, Jackson State University, Jackson, MS 39217-0510, USA,^bDepartment of Civil and Env. Engineering, Jackson State University, Jackson, MS 39217-0510, USA, and ^cDepartment of Chemistry, Louisiana State University, Baton Rouge, LA 70803, USA
Correspondence e-mail: ramaiyer.venkatraman@jsums.edu

The title compound, [Ag(C₉H₁₃N₅S)Cl(C₁₈H₁₅P)₂], crystallizes with four independent molecules in the asymmetric unit, in each of which the Ag atom is in a distorted tetrahedral coordination, defined by the chloride ligand, the S atom of the neutral ligand and two P atoms derived from the triphenyl phosphine ligands. The thiosemicarbazone acts as a monodentate ligand through its thione S atom. An intramolecular N-HCl hydrogen bond occurs in two of the independent molecules. In the crystal, the molecules are assembled through N-HCl hydrogen bonds, forming chains along [101].

Related literature

For general background to thiosemicarbazones, see: Akinchan et al. (2002); Ali & Livingstone (1974); Bermejo et al. (2003); Blanz & French (1968); Campbell (1975); Casas et al. (2000); Grecu & Neamtu (1967); Hossain et al. (2002); Huheey et al. (1993); Lobana et al. (1998, 2008); Pellerito & Negy (2002); Raper (1985); Venkatraman et al. (2009); Zhou et al. (2008).

Experimental

Crystal data

[Ag(C₉H₁₃N₅S)Cl(C₁₈H₁₅P)₂]
M_r = 891.17
Monoclinic, P 2₁
a = 12.0640 (5) Å
b = 31.810 (2) Å
c = 21.9207 (15) Å
= 98.029 (5)°
V = 8329.7 (9) Å³
Z = 8
Mo K radiation
= 0.71 mm^-1
T = 90 K
0.27 × 0.22 × 0.20 mm

Data collection

Nonius KappaCCD diffractometer with Oxford Cryostream system
Absorption correction: multi-scan (DENZO and SCALEPACK; Otwinowski & Minor, 1997) T_min = 0.831, T_max = 0.870
138032 measured reflections
54942 independent reflections
44399 reflections with I > 2(I)
R_int = 0.055

Refinement

R[F² > 2(F²)] = 0.042
wR(F²) = 0.103
S = 1.03
54942 reflections
2007 parameters
9 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 1.03 e Å^-3
_min = -0.85 e Å^-3
Absolute structure: Flack (1983), 25,519 Friedel pairs
Flack parameter: 0.382 (11)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1NCl1	0.88 (2)	2.54 (2)	3.381 (3)	163 (3)
N3-H3NCl3	0.87 (2)	2.68 (3)	3.406 (3)	142 (3)
N6-H6NCl2	0.88 (2)	2.53 (2)	3.370 (3)	162 (3)
N8-H8NCl4	0.86 (2)	2.68 (3)	3.411 (3)	143 (3)
N11-H11NCl3	0.88 (2)	2.52 (2)	3.363 (3)	161 (3)
N13-H13NCl2	0.88 (2)	2.65 (2)	3.423 (3)	147 (3)
N16-H16NCl4	0.86 (2)	2.50 (2)	3.338 (3)	164 (3)
N18-H18NCl1ⁱ	0.86 (2)	2.70 (3)	3.425 (3)	143 (3)
Symmetry code: (i) x-1, y, z-1.

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXH (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: SHELXH.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RK2386 ).

Acknowledgements

The National Science Foundation is acknowledged for a CAREER award (CHE-1056927) to MAH. Purchase of the diffractometer was made possible by grant No. LEQSF (1999-2000)-ENH-TR-13, administered by the Louisiana Board of Regents.

References

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metal-organic compounds