cis-(Dimethyl sulfoxide-κO)[N′-(3-eth­oxy-2-oxidobenzyl­idene-κO)-2-hy­droxy­benzohydrazidato-κ2 N′,O]dioxido­molybdenum(VI)

Ngui Khiong Ngan; Kong Mun Lo; Chee Seng Richard Wong

doi:10.1107/S1600536811020290

. 2011 Jun 4;67(Pt 7):m857. doi: 10.1107/S1600536811020290

cis-(Dimethyl sulfoxide-κO)[N′-(3-ethoxy-2-oxidobenzylidene-κO)-2-hydroxybenzohydrazidato-κ² N′,O]dioxidomolybdenum(VI)

Ngui Khiong Ngan ^a, Kong Mun Lo ^a,^*, Chee Seng Richard Wong ^a

PMCID: PMC3152017 PMID: 21836856

Abstract

The coordination geometry at the Mo^VI atom in the title compound, [Mo(C₁₆H₁₄N₂O₄)O₂(C₂H₆OS)], is distorted octahedral. The phenolate O, imino N, oxide O from the enolized carbonyl group and one of the terminal O atoms form the equatorial plane; the axial positions are occupied by the other terminal O atom of the dioxidomolybdenum group and the donor O atom of DMSO. The O=Mo=O angle is 105.31 (6)°. An intramolecular O—H⋯N hydrogen bond and weak intermolecular C—H⋯O hydrogen bonds are present in the structure.

Related literature

For related Schiff base complexes of molybdenum, see: Rajan & Chakravorty (1981 ▶). For Mo=O bond lengths in cis-dioxidomolybdenum(VI) complexes, see: Dinda et al. (2006 ▶); Rao et al. (1999 ▶); Syamal & Maurya (1986 ▶).

Experimental

Crystal data

[Mo(C₁₆H₁₄N₂O₄)O₂(C₂H₆OS)]
M _r = 504
Monoclinic,
a = 7.7527 (1) Å
b = 20.6173 (4) Å
c = 12.6506 (2) Å
β = 100.931 (1)°
V = 1985.38 (6) Å³
Z = 4
Mo Kα radiation
μ = 0.81 mm⁻¹
T = 100 K
0.37 × 0.30 × 0.30 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.752, T _max = 0.788
18375 measured reflections
4556 independent reflections
4485 reflections with I > 2σ(I)
R _int = 0.017

Refinement

R[F ² > 2σ(F ²)] = 0.024
wR(F ²) = 0.120
S = 1.15
4556 reflections
266 parameters
H-atom parameters constrained
Δρ_max = 0.47 e Å⁻³
Δρ_min = −1.68 e Å⁻³

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811020290/xu5215sup1.cif

e-67-0m857-sup1.cif^{(21.9KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811020290/xu5215Isup2.hkl

e-67-0m857-Isup2.hkl^{(223.2KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Mo1—N1	2.2343 (13)
Mo1—O1	1.9197 (11)
Mo1—O2	1.7132 (11)
Mo1—O3	1.7055 (12)
Mo1—O4	2.0297 (11)
Mo1—O6	2.2928 (11)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7⋯N2	0.82	1.87	2.5859 (19)	145
C9—H9⋯O3ⁱ	0.93	2.54	3.217 (2)	130
C18—H18C⋯O3ⁱⁱ	0.96	2.56	3.438 (2)	152

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Symmetry codes: (i) Inline graphic ; (ii) .

Acknowledgments

We thank the University of Malaya (grant Nos. PS378/2010B and RG020/09AFR) for supporting this study.

supplementary crystallographic information

Comment

The coordination chemistry of molybdenum has taken cognizance of by the scientific community in the last 20 years is because of its ability to achieve multiple common oxidation states ranging from +4 to +6 as well as to form stable complexes with Schiff base ligands (Rajan & Chakravorty, 1981). The title compound represents one of the stable molybdenum complex containing a tridentate O,N,O' Schiff base ligand. This molybdenum complex consists of a discrete mononuclear unit (Scheme 1). The overall geometry at molybdenum is a six coordinate octahedron with the bonds formed by the dibasic tridentate ligands together with the two terminal oxygen atoms and the donor oxygen atom of DMSO. The relatively long bond length between Mo and O6 from the DMSO molecule [2.293 (1) Å] shows that the coordination site is labile. The Mo = O bond distances are 1.706 (1) and 1.713 (1) Å, which fall in the expected range for most of the cis-dioxomolybdenum(VI) complexes (Dinda, et al., 2006; Syamal & Maurya, 1986 and Rao, et al., 1999).

Experimental

The Schiff base ligand was prepared by the condensation reaction of salicylic acid hydrazide with 3-ethoxysalicylaldehyde. The title compound was prepared from the equimolar amount of the prepared Schiff base (0.30 g, 1.0 mmol) and bis(acetylacetonato)dioxomolybdenum(VI), [MoO₂(acac)₂] (0.328 g, 1.0 mmol) in refluxing ethanol (100 ml). The solution was then added with a few drops of DMSO and refluxed for another 1 h. The solution was left for recrystallizaton at room temperature during which orange colour crystals were obtained.