(5-Amino­isophthalato-κN)triaqua­(1,10-phenanthroline-κ2 N,N′)nickel(II) trihydrate

Han Huang; Kou-Lin Zhang; Seik Weng Ng

doi:10.1107/S1600536811008919

. 2011 Mar 15;67(Pt 4):m444–m445. doi: 10.1107/S1600536811008919

(5-Aminoisophthalato-κN)triaqua(1,10-phenanthroline-κ² N,N′)nickel(II) trihydrate

Han Huang ^a, Kou-Lin Zhang ^a, Seik Weng Ng ^b,^*

PMCID: PMC3099854 PMID: 21753965

Abstract

The Ni^II atom in the title compound, [Ni(C₈H₅NO₄)(C₁₂H₈N₂)(H₂O)₃]·3H₂O, is six-coordinated in an NiN₃O₃ octahedral geometry. The triply water-coordinated Ni^II atom is chelated by the phenantroline ligand and is additionally coordinated by the amino group of the 5-aminoisophtalate anion. The anion, the coordinated and the uncoordinated water molecules interact through an extensive O—H⋯O and N—H⋯O hydrogen-bonding network, generating a three-dimensional cage-like network.

Related literature

For the isotypic Co^II analog, see: Zhang et al. (2010 ▶).

Experimental

Crystal data

[Ni(C₈H₅NO₄)(C₁₂H₈N₂)(H₂O)₃]·3H₂O
M _r = 526.14
Monoclinic,
a = 10.1039 (10) Å
b = 13.9448 (14) Å
c = 16.4237 (16) Å
β = 95.522 (1)°
V = 2303.3 (4) Å³
Z = 4
Mo Kα radiation
μ = 0.90 mm⁻¹
T = 295 K
0.13 × 0.12 × 0.10 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.892, T _max = 0.915
20080 measured reflections
5258 independent reflections
3702 reflections with I > 2σ(I)
R _int = 0.092

Refinement

R[F ² > 2σ(F ²)] = 0.037
wR(F ²) = 0.081
S = 0.89
5258 reflections
363 parameters
14 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.35 e Å⁻³
Δρ_min = −0.55 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; method used to solve structure: atomic coordinates taken from an isotypic structure (Zhang et al., 2010 ▶); 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 datablocks global, I. DOI: 10.1107/S1600536811008919/wm2464sup1.cif

e-67-0m444-sup1.cif^{(25KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811008919/wm2464Isup2.hkl

e-67-0m444-Isup2.hkl^{(257.5KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Ni1—O1w	2.0408 (16)
Ni1—N2	2.0800 (16)
Ni1—O2w	2.0797 (14)
Ni1—N3	2.0883 (16)
Ni1—O3w	2.0965 (15)
Ni1—N1	2.1409 (18)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H1w1⋯O6wⁱ	0.84 (1)	1.91 (1)	2.747 (2)	177 (3)
O1w—H1w2⋯O2ⁱⁱ	0.84 (1)	1.82 (1)	2.654 (2)	180 (2)
O2w—H2w1⋯O5wⁱ	0.85 (1)	1.94 (1)	2.781 (2)	173 (3)
O2w—H2w2⋯O4ⁱⁱⁱ	0.85 (1)	1.98 (1)	2.832 (2)	178 (3)
O3w—H3w1⋯O5w^iv	0.84 (1)	2.16 (2)	2.914 (3)	148 (3)
O3w—H3w2⋯O3ⁱⁱ	0.85 (1)	1.88 (1)	2.721 (2)	173 (3)
O4w—H4w1⋯O6w^v	0.85 (1)	1.97 (1)	2.817 (3)	171 (3)
O4w—H4w2⋯O2^iv	0.85 (1)	2.16 (2)	2.915 (3)	149 (3)
O5w—H5w1⋯O1	0.85 (1)	1.90 (1)	2.726 (3)	163 (3)
O5w—H5w2⋯O3^vi	0.84 (1)	1.91 (1)	2.716 (2)	159 (3)
O6w—H6w1⋯O1	0.85 (1)	1.83 (1)	2.678 (2)	177 (3)
O6w—H6w2⋯O4ⁱⁱⁱ	0.85 (1)	1.95 (1)	2.791 (2)	176 (3)
N1—H1⋯O4w	0.85 (1)	2.08 (1)	2.928 (3)	173 (2)
N1—H2⋯O4ⁱⁱⁱ	0.85 (1)	2.30 (1)	3.116 (2)	162 (2)

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

Acknowledgments

We thank the Key Laboratory of Environmental Material and Environmental Engineering of Jiangsu Province, Yangzhou University, and the University of Malaya for supporting this study.

supplementary crystallographic information

Comment

We reported the structure of [Co(C₈H₅NO₄)(C₁₂H₈N₂)(H₂O)₃]^.3H₂O], whose 5-aminoisophthlate dianion binds only through the neutral amino donor site. The coordinated water molecules comprise the fac points of the NiN₃O₃ octahedron (Zhang et al., 2010). The nickel analog (Scheme I) is isotypic. The dianion, the coordinated and the lattice water molecules interact through hydrogen bonds (Table 1) to furnish a tightly-held, three-dimensional network. Pairs of phenanthroline units show π···π interactions about a center-of-inversion at a distance of ca 3.5 Å.

Experimental

Nickel nitrate hexahydrate (0.048 g, 0.165 mmol) dissolved in water (5 ml) was added to a mixture of 5-aminoisophthalic acid (0.030 g, 0.165 mmol) and sodium hydroxide (0.013 g, 0.330 mmol) dissolved in water (5 ml). To this solution was added 1,10-phenanthroline (0.033 g, 0.165 mmol) dissolved in methanol (10 ml). The mixture was filtered and set aside for the growth of green crystals.