Tetra­kis[1-phenyl-3-(1H-1,2,4-triazol-1-yl)propan-1-one-κN 4]bis­(thio­cyanato-κN)nickel(II)

Jian-Hua Guo

doi:10.1107/S1600536810049081

. 2010 Nov 27;66(Pt 12):m1687. doi: 10.1107/S1600536810049081

Tetrakis[1-phenyl-3-(1H-1,2,4-triazol-1-yl)propan-1-one-κN ⁴]bis(thiocyanato-κN)nickel(II)

Jian-Hua Guo ^a,^*

PMCID: PMC3011655 PMID: 21589343

Abstract

In the centrosymmetric mononuclear title complex, [Ni(NCS)₂(C₁₁H₁₁N₃O)₄], the Ni^II atom, located on an inversion centre, is hexacoordinated in a distorted octahedral geometry comprising four N atoms of four monodentate 1-phenyl-3-(1H-1,2,4-triazol-1-yl)propan-1-one ligands and two N atoms from thiocyanate anions.

Related literature

Pseudohalide anions N₃ ⁻, NCS⁻ and NCO⁻ are versatile ligands in coordination chemistry because of their multiple bridging modes, see: Yue et al. (2008 ▶). For a related structure, see: Guo & Cai (2007 ▶).

Experimental

Crystal data

[Ni(NCS)₂(C₁₁H₁₁N₃O)₄]
M _r = 979.78
Triclinic,
a = 7.8067 (10) Å
b = 11.8539 (15) Å
c = 13.8179 (17) Å
α = 68.907 (2)°
β = 74.765 (2)°
γ = 81.687 (2)°
V = 1149.3 (3) Å³
Z = 1
Mo Kα radiation
μ = 0.57 mm⁻¹
T = 293 K
0.32 × 0.28 × 0.22 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.838, T _max = 0.884
6289 measured reflections
4016 independent reflections
3540 reflections with I > 2σ(I)
R _int = 0.015

Refinement

R[F ² > 2σ(F ²)] = 0.029
wR(F ²) = 0.080
S = 1.06
4016 reflections
304 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 0.38 e Å⁻³
Δρ_min = −0.34 e Å⁻³

Data collection: APEX2 (Bruker, 2003 ▶); cell refinement: SAINT (Bruker, 2003 ▶); data reduction: SAINT; 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: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810049081/pk2286sup1.cif

e-66-m1687-sup1.cif^{(23.5KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810049081/pk2286Isup2.hkl

e-66-m1687-Isup2.hkl^{(196.8KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The author gratefully acknowledges financial support from the Youthful Foundation of Tianjin Normal University (Natural Science, grant No. 52 L J44)

supplementary crystallographic information

Comment

Pseudohalide anions N₃^-, NCS^- and NCO^- are known as extremely versatile ligands in coordination chemistry because of their multiple bridging modes (Yue et al., 2008). Recently, we have initiated a research program of synthesizing supramolecules based on pseudohalide and flexible ligands that consist of a propanone unit substituted with an imidazole and a phenyl group (Guo et al., 2007). To further explore this series, we synthesized the title compound, a new Ni^II complex based on the mixed ligands thiocyanato and 3-(1H-1,2,4-triazol-1-yl)-1-phenylpropan-1-one (L), which consists of a propanone unit substituted with an triazole and a phenyl group. The crystal structure of the compound consists of a neutral mononuclear [Ni(L)₄(SCN)₂] molecule. As shown in Fig. 1, the Ni^II centre is coordinated by four N atoms from four L ligands, with Ni—N bond lengths in the range 2.103 (1)–2.135 (1) Å, two additional N donor from SCN anion, with a Ni—N bond distance of 2.078 (2) Å. Thus, the coordination polyhedron around the Ni^II cation could be best described as a distorted octahedral geometry. Analysis of the crystal packing indicates that there were no hydrogen bond or πi-πi stacking interactions in the crystal structure. (see Fig. 2).

Experimental

Ni(NO₃)₂.6H₂O (29.1 mg, 0.1 mmol), 3-(1H-1,2,4-triazol-1-yl)-1-phenylpropan-1-one (22.3 mg, 0.1 mmol) and NH₄SCN (7.6 mg, 0.1 mmol) were mixed in a CH₃CN—H₂O (20 ml, 1:1 v/v) solution with vigorous stirring for ca 30 min. The resulting solution was filtered and left to stand at room temperature. Green block crystals suitable for X-ray analysis were obtained in 60% yield by slow evaporation of the solvent over a period of 1 week. Analysis, calculated for NiC₄₆H₄₄N₁₄O₄S₂: C 56.39, H 4.53, N 20.01; found: C 56.44, H 4.64, N 20.05.