Tetra­aqua­bis­(2,6-dihy­droxy­benzoato-κO 1)(2,6-dihy­droxy­benzoato-κ2 O 1,O 1′)gadolinium(III) dihydrate

Juangang Wang; Jun Zhang; Tiedan Chen

doi:10.1107/S1600536811016163

. 2011 May 7;67(Pt 6):m698. doi: 10.1107/S1600536811016163

Tetraaquabis(2,6-dihydroxybenzoato-κO ¹)(2,6-dihydroxybenzoato-κ² O ¹,O ^1′)gadolinium(III) dihydrate

Juangang Wang ^a,^*, Jun Zhang ^a, Tiedan Chen ^a

PMCID: PMC3120440 PMID: 21754602

Abstract

In the title compound, [Gd(C₇H₅O₄)₃(H₂O)₄]·2H₂O, the Gd^III ion shows a distorted square antiprismatic coordination formed by four aqua ligands and four O atoms from the three 2,6-dihydroxybenzoate (L) ligands. Two L ligands coordinate the Gd^III ion in a monodentate mode, while the third coordinates it in a bidentate–chelating coordination mode. An extensive three-dimensional O—H⋯O hydrogen-bonding network consolidates the crystal packing.

Related literature

The crystal structures of related complexes with Ho and Tb were reported by Glowiak et al. (1999 ▶).

Experimental

Crystal data

[Gd(C₇H₅O₄)₃(H₂O)₄]·2H₂O
M _r = 724.68
Triclinic,
a = 10.7666 (4) Å
b = 11.3289 (4) Å
c = 12.4741 (4) Å
α = 82.270 (1)°
β = 73.066 (1)°
γ = 68.178 (1)°
V = 1350.65 (8) Å³
Z = 2
Mo Kα radiation
μ = 2.54 mm⁻¹
T = 294 K
0.24 × 0.20 × 0.18 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ▶) T _min = 0.581, T _max = 0.658
6854 measured reflections
4691 independent reflections
4301 reflections with I > 2σ(I)
R _int = 0.014

Refinement

R[F ² > 2σ(F ²)] = 0.022
wR(F ²) = 0.052
S = 1.04
4691 reflections
415 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.48 e Å⁻³
Δρ_min = −0.61 e Å⁻³

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); 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 and publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811016163/cv5069sup1.cif

e-67-0m698-sup1.cif^{(26.3KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811016163/cv5069Isup2.hkl

e-67-0m698-Isup2.hkl^{(229.8KB, 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
O13—H13A⋯O17ⁱ	0.84 (5)	1.88 (5)	2.697 (5)	161 (4)
O14—H14A⋯O17ⁱ	0.77 (5)	1.99 (7)	2.766 (5)	172 (4)
O15—H15A⋯O4ⁱⁱ	0.83 (5)	1.90 (8)	2.739 (5)	176 (5)
O16—H16A⋯O11	0.72 (4)	2.09 (5)	2.735 (5)	151 (2)
O16—H16A⋯O12ⁱⁱⁱ	0.72 (4)	2.50 (5)	2.865 (5)	113 (7)
O17—H17A⋯O18	0.86 (5)	1.81 (5)	2.668 (5)	175 (5)
O18—H18A⋯O5ⁱⁱ	0.91 (7)	1.88 (5)	2.752 (5)	161 (4)
O13—H13B⋯O1^iv	0.88 (5)	1.94 (5)	2.808 (5)	172 (5)
O14—H14B⋯O9^v	0.84 (5)	1.90 (5)	2.739 (5)	174 (5)
O15—H15B⋯O18	0.70 (4)	2.22 (5)	2.917 (5)	176 (6)
O16—H16B⋯O2	0.88 (6)	1.89 (5)	2.672 (5)	147 (5)
O17—H17B⋯O8^vi	0.82 (5)	2.03 (5)	2.713 (5)	140 (5)
O18—H18B⋯O12ⁱⁱⁱ	0.83 (5)	2.08 (5)	2.898 (5)	172 (3)
O1—H1⋯O2	0.82	1.78	2.515 (5)	148
O4—H4⋯O3	0.82	1.82	2.549 (5)	147
O5—H5⋯O6	0.82	1.83	2.566 (5)	148
O8—H8⋯O7	0.82	1.83	2.546 (5)	145
O9—H9⋯O10	0.82	1.82	2.551 (5)	147
O12—H12⋯O11	0.82	1.78	2.512 (5)	148

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

Acknowledgments

Financial support from Huaibei Normal University is gratefully acknowledged

supplementary crystallographic information

Comment

The title compound is isomorphous with the related Ho and Tb complexes (Glowiak et al., 1999). The coordinating Gd—O bond lengths are in the range 2.344 (2)–2.512 (2) Å. Intermolecular O—H···O hydrogen bonds (Table 1) form an extensive three-dimensional hydrogen-bonding network, which consolidate the crystal packing.

Experimental

The title complex was synthesized by dissolving 2,6-dihydroxybenzoic acid (10 mmol, 1.54 g) in 25 ml of ethanol. This was followed by the addition of Gadolinium nitrate (3 mmol,1.35 g), dissolved in 20 ml of distilled water. The mixture was stirred at room temperature for 5 h and the resulting white precipitate was filtered, dried and recrystallized from water.