Tetra­kis(pyridazine-κN)bis­(thio­cyanato-κN)nickel(II) pyridazine disolvate

Susanne Wöhlert; Mario Wriedt; Inke Jess; Christian Näther

doi:10.1107/S1600536812023306

. 2012 May 26;68(Pt 6):m793. doi: 10.1107/S1600536812023306

Tetrakis(pyridazine-κN)bis(thiocyanato-κN)nickel(II) pyridazine disolvate

Susanne Wöhlert ^a,^*, Mario Wriedt ^b, Inke Jess ^a, Christian Näther ^a

PMCID: PMC3379122 PMID: 22719343

Abstract

The reaction of nickel(II) thiocyanate with an excess of pyridazine leads to single crystals of the title compound, [Ni(NCS)₂(C₄H₄N₂)₄]·2C₄H₄N₂. The Ni^II cations are coordinated by two terminal N-bonded thiocyanate anions (trans) and four pyridazine ligands in a slightly distorted octahedral geometry. The discrete complexes are arranged into layers parallel to the ab plane which are separated by additional non-coordinated pyridazine ligands.

Related literature

For related pyridazine coordination compounds, see: Boeckmann et al. (2011 ▶); Lloret et al. (1998 ▶); Yi et al. (2006 ▶); Wriedt & Näther (2009 ▶, 2011 ▶).

Experimental

Crystal data

[Ni(NCS)₂(C₄H₄N₂)₄]·2C₄H₄N₂
M _r = 655.42
Triclinic,
a = 11.2111 (9) Å
b = 12.033 (1) Å
c = 12.5409 (10) Å
α = 62.287 (9)°
β = 88.983 (10)°
γ = 88.949 (10)°
V = 1497.4 (2) Å³
Z = 2
Mo Kα radiation
μ = 0.83 mm⁻¹
T = 200 K
0.06 × 0.04 × 0.03 mm

Data collection

Stoe IPDS-1 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T _min = 0.916, T _max = 0.973
11937 measured reflections
6400 independent reflections
4719 reflections with I > 2σ(I)
R _int = 0.029

Refinement

R[F ² > 2σ(F ²)] = 0.032
wR(F ²) = 0.084
S = 0.97
6400 reflections
389 parameters
H-atom parameters constrained
Δρ_max = 0.39 e Å⁻³
Δρ_min = −0.40 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2008 ▶); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 2011 ▶); software used to prepare material for publication: XCIF in SHELXTL and PLATON (Spek, 2009 ▶).

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812023306/bt5930sup1.cif

e-68-0m793-sup1.cif^{(22.5KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812023306/bt5930Isup2.hkl

e-68-0m793-Isup2.hkl^{(313.3KB, hkl)}

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

Acknowledgments

We gratefully acknowledge financial support by the DFG (project No. NA 720/3–1) and the State of Schleswig–Holstein. We also thank Professor Dr Wolfgang Bensch for access to his experimental facility.

supplementary crystallographic information

Comment

Currently, we are interested in the synthesis and characterization of coordination polymers based on Mn(II), Fe(II), Co(II), Ni(II) and Cd(II) thiocyanates and pyridazine as co-ligand. Only a few compounds based on Cobalt, Nickel and Cadmium are structurally characterized (Boeckmann et al., 2011; Lloret et al., 1998; Yi et al., 2006; Wriedt & Näther, 2011; Wriedt & Näther, 2009). In this context we have reported on two different modifications of a trinuclear nickel(II) complex of composition [Ni₃(NCS)₆(pyridazine)₆] (Wriedt & Näther, 2009). In our ongoing investigation in this field we have isolated light-green single-crystals of a further compound by the reaction of nickel(II) thiocyanate with an excess of pyridazine, that were characterized by single-crystal X-ray diffraction. In the crystal structure of the title compound each nickel(II) cation is coordinated by two terminal N-bonded thiocyanato anions and four pyridazine ligands in a slightly distorted octahedral geometry (Fig. 1). The NiN₆ distances are ranges from 2.0494 (15) to 2.1530 (15) Å and the angles are between 87.33 (5) ° and 179.71 (7) °. Because of sterical reasons only one of the two pyridazine nitrogen atoms is involved in metal coordination. In the crystal structure the discrete complexes are arranged in layers that are parallel to the ab plane. These layers are separated by additional pyridazine ligands that are not coordinated to the metal centers (Fig. 2). The shortest intermolecular Ni···Ni distances amounts to 8.0823 (9) Å.

Experimental

Nickel(II) thiocyanate (Ni(NCS)₂) and pyridazine were obtained from Alfa Aesar. All chemicals were used without further purification. 0.125 mmol (21.7 mg) Ni(NCS)₂ and 2.76 mmol (200 µL) pyridazine were reacted in a closed snap-vial without stirring. Light-green single crystals of the title compounds were obtained after two weeks.