Poly[[tris­(μ2-4,4′-bipyridine N,N′-di­oxide)hexa­nitratodigadolinium(III)] dichloro­methane disolvate]

Adam J Dillner; Cassandra P Lilly; Jacqueline M Knaust

doi:10.1107/S1600536810033258

. 2010 Aug 21;66(Pt 9):m1158–m1159. doi: 10.1107/S1600536810033258

Poly[[tris(μ₂-4,4′-bipyridine N,N′-dioxide)hexanitratodigadolinium(III)] dichloromethane disolvate]

Adam J Dillner ^a, Cassandra P Lilly ^a, Jacqueline M Knaust ^a,^*

PMCID: PMC3008111 PMID: 21588551

Abstract

The title one-dimensional coordination network, {[Gd₂(NO₃)₆(C₁₀H₈N₂O₂)₃]·2CH₂Cl₂}_n, is isostructural with the previously reported Tb and Tl coordination networks and to its Eu analog. The Gd^III cation is coordinated in a distorted tricapped trigonal-prismatic fashion by nine O atoms from three bridging 4,4′-bipyridine N,N′-dioxide ligands and three chelating nitrate anions. None of the atoms lie on a special position, but there is an inversion center located between the rings of one of the ligands. The network topology is ladder-like, and each ladder interacts with six neighboring ladders through C—H⋯O hydrogen bonds. The packing motif of the ladders allows for the formation of channels that run parallel to the a axis; these channels are filled with CH₂Cl₂ solvent molecules that interact with the ladders through C—H⋯O hydrogen bonds

Related literature

For the isostructural Tb and Tl, coordination networks, see: Long et al. (2002 ▶); Moitsheki et al. (2006 ▶). For the isostructural Eu coordination network and detailed background to this study, see: Dillner et al. (2010 ▶).

Experimental

Crystal data

[Gd₂(NO₃)₆(C₁₀H₈N₂O₂)₃]·2CH₂Cl₂
M _r = 1420.96
Triclinic,
a = 7.9917 (5) Å
b = 11.5668 (7) Å
c = 13.0347 (8) Å
α = 86.059 (1)°
β = 80.134 (1)°
γ = 78.255 (1)°
V = 1161.52 (12) Å³
Z = 1
Mo Kα radiation
μ = 3.16 mm⁻¹
T = 100 K
0.51 × 0.48 × 0.25 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2009 ▶) T _min = 0.529, T _max = 0.746
13791 measured reflections
6990 independent reflections
6776 reflections with I > 2σ(I)
R _int = 0.019

Refinement

R[F ² > 2σ(F ²)] = 0.020
wR(F ²) = 0.051
S = 1.06
6990 reflections
334 parameters
H-atom parameters constrained
Δρ_max = 1.34 e Å⁻³
Δρ_min = −1.26 e Å⁻³

Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT (Bruker, 2009 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: X-SEED.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810033258/zl2303sup1.cif

e-66-m1158-sup1.cif^{(22KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810033258/zl2303Isup2.hkl

e-66-m1158-Isup2.hkl^{(342KB, 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
C5—H5⋯O7ⁱ	0.95	2.41	3.082 (2)	127
C9—H9⋯O9ⁱⁱ	0.95	2.57	3.287 (2)	132
C12—H12⋯O2ⁱⁱⁱ	0.95	2.43	3.300 (2)	152
C16—H16B⋯O12ⁱⁱ	0.99	2.43	3.246 (3)	139
C16—H16A⋯O8	0.99	2.56	3.302 (3)	132
C16—H16A⋯O9	0.99	2.50	3.084 (3)	117

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

Acknowledgments

The authors are thankful to Allegheny College for providing funding in support of this research. The diffractometer was funded by the NSF (grant No. 0087210), the Ohio Board of Regents (grant No. CAP-491) and by Youngstown State University. The authors would like to acknowledge Youngstown State University and the STaRBURSTT CyberInstrumentation Consortium for assistance with the crystallography.

supplementary crystallographic information

Comment

The description of the structure of the title compound is part of a set of consecutive papers on one-dimensional ladder-like coordination networks of the type [Ln₂(NO₃)₆(C₁₀H₈N₂O₂)₃]_n, with Ln = Eu (Dillner et al., 2010) and Gd (this publication), respectively. Both compounds are also isostructural to the previously reported Tb and Tl, coordination networks (Long et al., 2002 and Moitsheki et al., 2006). The background to this study is given in Dillner et al. (2010).

Experimental

Gd(NO₃)₃ (0.051 g 0.15 mmol) was placed in the bottom of a test tube and covered with CH₂Cl₂ (5 ml). 4,4'-bipyridine-N,N'-dioxide^.H₂O (0.0376 g, 0.182 mmol) was dissolved in methanol (8 ml), and this solution was layered over the CH₂Cl₂. The two solutions were allowed to slowly mix. Over a period of several weeks the Gd(NO₃)₃ dissolved, and yellow plate-like crystals of the title compound formed.