catena-Poly[[[bis­(O,O′-diisobutyl dithio­phosphato-κ2 S,S′)nickel(II)]-μ-1,2-bis­(4-pyridylmethyl­ene)hydrazine-κ2 N:N′] toluene disolvate]

Erick Berdugo; Edward R T Tiekink

doi:10.1107/S1600536808017121

. 2008 Jun 13;64(Pt 7):m911. doi: 10.1107/S1600536808017121

catena-Poly[[[bis(O,O′-diisobutyl dithiophosphato-κ² S,S′)nickel(II)]-μ-1,2-bis(4-pyridylmethylene)hydrazine-κ² N:N′] toluene disolvate]

Erick Berdugo ^a, Edward R T Tiekink ^a,^*

PMCID: PMC2961896 PMID: 21202772

Abstract

The polymeric title compound, {[Ni(C₈H₁₈O₂PS₂)₂(C₁₂H₁₀N₄)]·2C₇H₇}_n, has a linear topology and features octahedrally coordinated Ni atoms with a trans-N₂S₄ donor set. The toluene solvent molecules occupy channels defined by the three-dimensional stacking of the polymeric chains. The Ni atom is located at a centre of inversion and the bridging 1,2-bis(4-pyridylmethylene)hydrazine4-pyridine molecule is also disposed about a centre of inversion. One isobutoxy group is disordered equally over two positions.

Related literature

For a related structure, see: Berdugo et al. (2007 ▶). For related literature, see: Lai et al. (2004 ▶); Chen et al. (2006 ▶); Tiekink (2006 ▶); Benson et al. (2007 ▶).

Experimental

Crystal data

[Ni(C₈H₁₈O₂PS₂)₂(C₁₂H₁₀N₄)]·2C₇H₇
M _r = 935.85
Triclinic,
a = 8.7132 (15) Å
b = 12.089 (2) Å
c = 12.293 (2) Å
α = 82.662 (10)°
β = 86.528 (10)°
γ = 69.321 (6)°
V = 1201.4 (4) Å³
Z = 1
Mo Kα radiation
μ = 0.69 mm⁻¹
T = 98 (2) K
0.30 × 0.20 × 0.10 mm

Data collection

Rigaku AFC12K/SATURN724 diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.795, T _max = 1 (expected range = 0.742–0.934)
8239 measured reflections
5457 independent reflections
4980 reflections with I > 2σ(I)
R _int = 0.033

Refinement

R[F ² > 2σ(F ²)] = 0.054
wR(F ²) = 0.142
S = 1.08
5457 reflections
279 parameters
H-atom parameters constrained
Δρ_max = 0.64 e Å⁻³
Δρ_min = −0.78 e Å⁻³

Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPII (Johnson, 1976 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808017121/ng2459sup1.cif

e-64-0m911-sup1.cif^{(26.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808017121/ng2459Isup2.hkl

e-64-0m911-Isup2.hkl^{(267.2KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C12—H12⋯S1ⁱ	0.95	2.76	3.694 (3)	169

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Symmetry code: (i) Inline graphic .

Acknowledgments

The authors gratefully thank the MBRS–RISE program (GM60655) for support and Cheminova is thanked for the gift of the dithiophosphate used in this study.

supplementary crystallographic information

Comment

Interest in examining structures related to the title compound (I), Fig. 1, relates in the main to attempts to control polymer formation and when formed topology (Lai et al., 2004; Chen et al. 2006; Tiekink, 2006; Benson et al., 2007 & Berdugo et al., 2007). A linear polymer is found in (I), Fig. 2, in which the Ni atom is located on a centre of inversion and the bridging 4-pyridinealdazine ligand is disposed about another centre of inversion. The Ni atom exists in a trans-N₂S₄ octahedral coordination geommetry. The polymers are aligned along the c-direction and form layers in the ac-plane that are stabilized by C—H···S contacts, Table 1. Layers stack along the b axis and define approximate squares with Ni···Ni edges 12.1 and 12.3 Å. Despite the fact that the isobutyl residues protrude into the resulting channels, the toluene molecules are accommodated in these as seen in Fig. 3.

Experimental

The title compound was prepared by refluxing equimolar amounts of the parent nickel dithiophosphate with 4-pyridinealdazine (Sigma-Aldrich) in toluene (30 ml) for 30 min following a literature procedure (Berdugo et al., 2007). Brown crystals of (I) were isolated by the slow evaporation (3 days) of this toluene solution. The crystals lost crystallinity with standing in air after a few minutes. IR (cm^-1): v(C—O) 1126, v(P—O) 951, v(P—S)_asymm 672, v(P—S)_sym 593.