Bis{2-[3-(dimethyl­amino)­propyl­imino­meth­yl]-6-meth­oxy­phenolato}-κ3 N,N′,O 1;κ2 N,O 1-zinc(II) dihydrate

Hong Lin; Xiao-Juan Wang

doi:10.1107/S1600536810052438

. 2010 Dec 18;67(Pt 1):m90. doi: 10.1107/S1600536810052438

Bis{2-[3-(dimethylamino)propyliminomethyl]-6-methoxyphenolato}-κ³ N,N′,O ¹;κ² N,O ¹-zinc(II) dihydrate

Hong Lin ^a,^*, Xiao-Juan Wang ^b

PMCID: PMC3050366 PMID: 21522605

Abstract

In the title mononuclear Zn^II complex, [Zn(C₁₃H₁₉N₂O₂)₂]·2H₂O, the Zn^II atom is coordinated by two O atoms and three N atoms from two crystallographically different Schiff base ligands in a distorted trigonal–bipyramidal environment. One O and two N atoms constitute the base of the pyramid, and one O and one N atoms occupy the apical positions. Intermolecular O—H⋯O and O—H⋯N hydrogen bonds between the lattice water molecules and N/O atoms of the Schiff base ligands stabilize the conformation, whereas intermolecular O—H⋯O hydrogen bonds between the two lattice water molecules lead to a chain structure in [001].

Related literature

For related structures, see: Choudhury et al. (2001 ▶); Guo & Lin (2008 ▶); Lin et al. (2009 ▶).

Experimental

Crystal data

[Zn(C₁₃H₁₉N₂O₂)₂]·2H₂O
M _r = 572.01
Orthorhombic,
a = 14.982 (3) Å
b = 9.4411 (19) Å
c = 20.384 (4) Å
V = 2883.2 (10) Å³
Z = 4
Mo Kα radiation
μ = 0.90 mm⁻¹
T = 293 K
0.33 × 0.24 × 0.09 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.773, T _max = 0.923
14801 measured reflections
6371 independent reflections
4666 reflections with I > 2σ(I)
R _int = 0.027

Refinement

R[F ² > 2σ(F ²)] = 0.031
wR(F ²) = 0.072
S = 1.00
6371 reflections
352 parameters
7 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.23 e Å⁻³
Δρ_min = −0.30 e Å⁻³
Absolute structure: Flack (1983 ▶), 2935 Friedel pairs
Flack parameter: −0.002 (11)

Data collection: APEX2 (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); 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 I, global. DOI: 10.1107/S1600536810052438/bq2261sup1.cif

e-67-00m90-sup1.cif^{(27.8KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810052438/bq2261Isup2.hkl

e-67-00m90-Isup2.hkl^{(311.8KB, 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
O1W—H1WA⋯O3	0.82 (2)	2.02 (2)	2.805 (3)	161 (3)
O1W—H1WA⋯O4	0.82 (2)	2.49 (3)	3.067 (3)	129 (3)
O1W—H1WB⋯O1	0.83 (2)	2.39 (3)	3.019 (3)	133 (3)
O1W—H1WB⋯O2	0.83 (2)	2.58 (2)	3.379 (3)	162 (3)
O2W—H2WA⋯N4	0.85 (2)	2.05 (2)	2.894 (4)	178 (4)
O2W—H2WB⋯O1Wⁱ	0.84 (2)	2.06 (2)	2.900 (3)	175 (5)

Open in a new tab

Symmetry code: (i) Inline graphic .

supplementary crystallographic information

Comment

Transition metal complexes with multidentate Schiff base ligands have been extensively studied recently for their various crystallographic features, enzymatic reactions, catalysis, electrochemical and magnetic properties. Metal complexes with tridentate N₂O Schiff base ligands derived from salicylaldehyde have been well studied in the past, such as [NiMe₂NCH₂CH₂CH₂N=CHC₆H₄O)₂] (Choudhury et al., 2001), [Ni(C₁₃H₁₉N₂O₂]₂] (Guo et al., 2008) and [Cd(C₁₃H₂₀N₂O₂)₂X₂] (Lin et al., 2009). Molecule of the title complex (I) (Fig. 1) comprises one zinc(II) ion, two 2-[3-(dimethylamino)propyliminomethyl]-6-methoxyphenolato anions and two lattice water molecules. The center Zn^II atom is coordinated by two O atoms and three N atoms from two different Schiff base ligands in a distorted trigonal dipyramidal environment. Three coordinated atoms of O(1), N(2), and N(3) constitute the base of the pyramid, whereas N(1) and O(3) atoms occupy the apical position. The O and N atoms together with lattice water molecules are involved in hydrogen-bonding interactions (Fig.2). In detail, the structure is stabilized by intramolecular O—H···O and O—H···N hydrogen bonds between the lattice water molecules and N and O atoms from Schiff base ligands. The other intermolecular O—H···O hydrogen bonds between two lattice water molecules lead to a one-dimensional chain structure running along c direction.

Experimental

3-methoxysalicylaldehyde (2.0 mmol) and 3-dimethylaminopropylamine (2.0 mmol) in 15 ml of methyl alcohol were stirred for 4 h. ZnSO₄.7H₂O (1.0 mmol) was added and stirred for 10 h. The resulting solution was placed in a refrigerator at 263 K for 7 days, and the crystals were filtered off, giving colorless cystals of the title complex for x-ray analysis.