Diaqua­sodium(I) perchlorate bis­[μ-2-(carboxyl­atomethyl­imino­meth­yl)phenolato]bis­[(3-methyl­pyridine)copper(II)]

Xiangru Wen; Yongmin Liu; Zhengyi Li

doi:10.1107/S1600536808039561

. 2008 Nov 29;64(Pt 12):m1634. doi: 10.1107/S1600536808039561

Diaquasodium(I) perchlorate bis[μ-2-(carboxylatomethyliminomethyl)phenolato]bis[(3-methylpyridine)copper(II)]

Xiangru Wen ^a, Yongmin Liu ^a, Zhengyi Li ^a,^*

PMCID: PMC2960105 PMID: 21581223

Abstract

In the title compound, [Na(H₂O)₂]ClO₄·[Cu₂(C₉H₇NO₃)₂(C₆H₇N)₂], the Cu^II atom is coordinated by one N atom and two O atoms from a tridentate N-salicylideneglycinate Schiff base dianion and one N atom from a 3-methylpyridine ligand. Longer Cu⋯O contacts [2.680 (2) Å] complete an approximate square-based pyramidal coordination geometry around Cu^II, forming a dimeric complex across a centre of inversion. The dimeric complexes form stacks along the a axis, with Cu⋯O contacts of 3.332 (2) Å between them. The Na⁺ cations and perchlorate anions lie on twofold rotation axes between the stacks. The former are coordinated by two disordered water molecules (each with half-occupancy), and form Na⋯O contacts of 3.698 (3) Å to the perchlorate anions and Na⋯π contacts to neighbouring salicylideneglycinate ligands [shortest Na⋯C = 3.516 (3) Å].

Related literature

For related structures, see: Warda (1998a ▶,b ▶,c ▶,d ▶). For synthesis details, see: Ueki et al. (1967 ▶); Warda (1994 ▶).

Experimental

Crystal data

[Na(H₂O)₂]ClO₄·[Cu₂(C₉H₇NO₃)₂(C₆H₇N)₂]
M _r = 826.12
Monoclinic,
a = 7.4677 (5) Å
b = 13.2402 (9) Å
c = 19.3937 (12) Å
β = 109.165 (2)°
V = 1811.3 (2) Å³
Z = 2
Mo Kα radiation
μ = 1.32 mm⁻¹
T = 292 (2) K
0.30 × 0.26 × 0.24 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T _min = 0.68, T _max = 0.73
18486 measured reflections
3558 independent reflections
2926 reflections with I > 2σ(I)
R _int = 0.047

Refinement

R[F ² > 2σ(F ²)] = 0.045
wR(F ²) = 0.100
S = 1.13
3558 reflections
237 parameters
H-atom parameters constrained
Δρ_max = 0.29 e Å⁻³
Δρ_min = −0.59 e Å⁻³

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808039561/bi2318sup1.cif

e-64-m1634-sup1.cif^{(18.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808039561/bi2318Isup2.hkl

e-64-m1634-Isup2.hkl^{(174.5KB, hkl)}

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

supplementary crystallographic information

Comment

Copper(II) complexes with tridentate Schiff-base dianions of the N-salicylideneaminoacidato type (TSB^2-) have been reported recently (1998a–d). These complexes are pyridine adducts. In this paper, we present the structure of the related title compound.

The Cu^II atom is coordinated by the tridentate N-salicylideneglycinato dianion and the 2-methylpyridine ligand in an approximately square-planar geometry. The pyridine ring is inclined with respect to the mean plane (through O1, O2, N1 and N2) at an angle of 11.5 (2) ° and the Cu^II atom lies 0.042 (1) Å out of this plane. The Cu—N and Cu—O bond distances [Cu—N 1.919 (2) and 2.018 (2) Å; Cu—O 1.922 (2) and 1.966 (2) Å] do not differ significantly when compared to the 2-ethylpyridine compound (Warda, 1998c). These units are associated into dimers through Cu···O interactions (2.680 (2) Å), and these dimers are associated into stacks along the a axis of the monoclinic unit cell by longer Cu···O contacts (3.332 (2) Å) (Fig. 2). The Na⁺ cations and perchlorate anions lie between stacks, both on 2-fold axes, forming Na···O contacts of 3.698 (2) Å. The Na⁺ cation is also coordinated by two water molecules in a bent geometry.

Experimental

The title compound was synthesized from aqua(N-salicylideneglycinato)copper(II) hemihydrate according to the methods of Ueki et al. (1967) and Warda (1994), with 3-methylpyridine and sodium perchlorate in a 4:3 ethanol-water mixture at room temperature. Dark-green prismatic crystals grew within a few days.