Bis(6-meth­oxy-2-{[tris­(hydroxy­meth­yl)methyl-κO]imino­meth­yl}phenolato-κ2 N,O 1)nickel(II) dihydrate

Tian Zhou; Ru-Jin Zhou; Zhe An

doi:10.1107/S1600536809022028

. 2009 Jun 17;65(Pt 7):m779. doi: 10.1107/S1600536809022028

Bis(6-methoxy-2-{[tris(hydroxymethyl)methyl-κO]iminomethyl}phenolato-κ² N,O ¹)nickel(II) dihydrate

Tian Zhou ^a,^*, Ru-Jin Zhou ^a, Zhe An ^a

PMCID: PMC2969396 PMID: 21582708

Abstract

In the title compound, [Ni(C₁₂H₁₆NO₅)₂]·2H₂O, the Ni^II atom is coordinated by four O atoms and two N atoms from the two 6-methoxy-2-{[tris(hydroxymethyl)methyl]iminomethyl}phenolate ligands in a distorted octahedral coordination geometry. O—H⋯O hydrogen bonds link the complexes and uncoordinated water molecules into two-dimensional networks parallel to (001).

Related literature

For the applications of Schiff-base complexes, see: Kritagawa & Kondo (1998 ▶); Zhang et al. (1998 ▶); Yaghi et al. (1996 ▶).

Experimental

Crystal data

[Ni(C₁₂H₁₆NO₅)₂]·2H₂O
M _r = 603.26
Monoclinic,
a = 12.0142 (10) Å
b = 10.9876 (10) Å
c = 20.324 (2) Å
β = 97.501 (1)°
V = 2660.0 (4) Å³
Z = 4
Mo Kα radiation
μ = 0.80 mm⁻¹
T = 293 K
0.44 × 0.29 × 0.20 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ▶) T _min = 0.721, T _max = 0.857
13321 measured reflections
4933 independent reflections
4436 reflections with I > 2σ(I)
R _int = 0.043

Refinement

R[F ² > 2σ(F ²)] = 0.039
wR(F ²) = 0.117
S = 1.00
4933 reflections
376 parameters
8 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.38 e Å⁻³
Δρ_min = −0.44 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; 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/S1600536809022028/bi2378sup1.cif

e-65-0m779-sup1.cif^{(24KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809022028/bi2378Isup2.hkl

e-65-0m779-Isup2.hkl^{(241.6KB, 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
O1—H1⋯O2ⁱ	0.82	1.85	2.670 (3)	179
O2—H2A⋯O11ⁱⁱ	0.82	1.91	2.666 (3)	152
O2—H2A⋯O12ⁱⁱ	0.82	2.37	3.010 (3)	135
O5—H5⋯O6ⁱⁱⁱ	0.82	1.87	2.691 (3)	174
O6—H6⋯O3^iv	0.82	1.89	2.671 (2)	159
O10—H10A⋯O5^iv	0.82 (3)	1.93 (3)	2.751 (3)	175 (5)
O8—H1AA⋯O7ⁱ	0.82 (2)	1.972 (11)	2.775 (4)	166 (4)
O4—H4AA⋯O8^v	0.82 (3)	1.88 (4)	2.686 (3)	170 (4)
O8—H1BB⋯O2^vi	0.82 (3)	2.16 (3)	2.962 (3)	167 (4)
O7—H2BB⋯O9ⁱⁱ	0.82 (2)	2.055 (10)	2.862 (4)	168 (4)
O7—H2AA⋯O1	0.81 (3)	1.84 (3)	2.641 (3)	169 (4)

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .

Acknowledgments

The authors acknowledge financial support from the Science Foundation of Maoming University (grant No. 208033).

supplementary crystallographic information

Comment

Polymeric metal complexes containing Schiff-base ligands are of interest because of their useful chemical or physical properties (Zhang et al., 1998; Kritagawa & Kondo, 1998; Yaghi et al., 1996). Herein, we report a new crystal structure containing the Schiff-base ligand 6-methoxy-2-{[tris(hydroxymethyl)methyl]iminomethyl}phenol (denoted HL).

As shown in Figure 1, the asymmetric unit of the complex comprises two L^- ligands, one Ni^II atom and two lattice water molecules. The Ni^II atom is hexa-coordinated by four O atoms and two N atoms from the two L^- ligands, giving a distorted octahedral coordination geometry. The Ni—O and Ni—N bond distances are within normal ranges. The [NiL₂] complexes form an extensive network of O—H···O interactions involving the lattice water molecules, giving 2-D networks parallel to the (001) planes (Fig. 2).

Experimental

The complex was synthesized by refluxing HL (0.050 g, 0.2 mmol) and NiCl₂.6H₂O (0.048 g, 0.2 mmol) in the mixed solution (CH₃OH:H₂O = 4:1) until all solid was dissolved. The solution was then cooled to room temperature and filtered. Green crystals for X-ray diffraction analysis were obtained by slow evaporation of the filtrate. Elemental analysis calculated: C 47.74, H 5.97, N 4.64 %; found: C 47.69, H 5.51, N 4.58 %.