Poly[[μ2-aqua-aqua­(μ3-3,5-dinitro­salicylato)barium(II)] monohydrate]

Wen-Dong Song; Run-Zhen Fan; Chang-Sheng Gu; Xiao-Min Hao

doi:10.1107/S1600536808006338

. 2008 Mar 14;64(Pt 4):m551. doi: 10.1107/S1600536808006338

Poly[[μ₂-aqua-aqua(μ₃-3,5-dinitrosalicylato)barium(II)] monohydrate]

Wen-Dong Song ^a,^*, Run-Zhen Fan ^a, Chang-Sheng Gu ^a, Xiao-Min Hao ^a

PMCID: PMC2960902 PMID: 21202008

Abstract

In the title coordination polymer, {[Ba(C₇H₂N₂O₇)(H₂O)₂]·H₂O}_n, the Ba^II atom is ten-coordinated by seven O atoms from four 3,5-dinitrosalicylatate ligands, two μ₂-bridging aqua ligands and one water molecule. The coordination mode is best described as a bicapped square-antiprismatic geometry. The 3,5-dinitrosalicylatate ligands bridge three Ba atoms. Centrosymmetrically related dinuclear barium units, with a Ba⋯Ba separation of 4.767 (5) Å, form infinite chains, which are further self-assembled into a supramolecular network through intermolecular O—H⋯O hydrogen-bonding interactions between O atoms of 3,5-dinitrosalicylatate ligands and water molecules.

Related literature

For related literature, see: Song et al. (2007 ▶).

Experimental

Crystal data

[Ba(C₇H₂N₂O₇)(H₂O)₂]·H₂O
M _r = 417.49
Monoclinic,
a = 11.9649 (6) Å
b = 4.1866 (2) Å
c = 26.121 (1) Å
β = 109.332 (3)°
V = 1234.7 (1) Å³
Z = 4
Mo Kα radiation
μ = 3.27 mm⁻¹
T = 296 (2) K
0.30 × 0.26 × 0.23 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.392, T _max = 0.471
8615 measured reflections
2374 independent reflections
2189 reflections with I > 2σ(I)
R _int = 0.041

Refinement

R[F ² > 2σ(F ²)] = 0.026
wR(F ²) = 0.067
S = 1.05
2374 reflections
199 parameters
9 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.03 e Å⁻³
Δρ_min = −1.30 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808006338/im2052sup1.cif

e-64-0m551-sup1.cif^{(19.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808006338/im2052Isup2.hkl

e-64-0m551-Isup2.hkl^{(116.7KB, 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
O3W—H6W⋯O7ⁱ	0.82 (3)	2.27 (3)	2.916 (4)	135 (4)
O3W—H5W⋯O5ⁱⁱ	0.82 (4)	2.60 (4)	2.985 (4)	110 (3)
O3W—H5W⋯O2Wⁱⁱⁱ	0.82 (4)	2.04 (3)	2.755 (4)	145 (4)
O2W—H4W⋯N1^iv	0.83 (3)	2.69 (4)	3.340 (4)	137 (4)
O2W—H4W⋯O4^iv	0.83 (3)	2.55 (4)	3.080 (4)	123 (3)
O2W—H4W⋯O5^iv	0.83 (3)	2.25 (3)	2.993 (4)	150 (5)
O2W—H3W⋯O3^v	0.83 (3)	2.01 (2)	2.730 (4)	145 (4)
O1W—H1W⋯O3W^v	0.83 (3)	1.991 (16)	2.798 (4)	164 (4)
O1W—H2W⋯O3W^vi	0.83 (3)	1.90 (3)	2.725 (4)	171 (4)

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

Acknowledgments

The authors acknowledge Guang Dong Ocean University for supporting this work.

supplementary crystallographic information

Comment

In the structural investigation of 3,5-dinitrosalicylatato complexes, it has been found that the 3,5-dinitrosalicylatato moiety functions as a multidentate ligand (Song et al., 2007) with versatile binding and coordination modes. In this paper, we report the crystal structure of the title compound, (I), a new Ba complex obtained by the reaction of 3,5-dinitrosalicylic acid and barium chloride in alkaline aqueous solution.

As illustrated in Figure 1, the Ba^II atom displays a bicapped square antiprismatic coordination environment, defined by seven O atoms from four 3,5-dinitrosalicylatato ligands, two µ₂-bridging aqua ligands and one water molecule. The 3,5-dinitrosalicylatato ligands link barium ions to form infinite chains, which are further self-assembled into a supramolecular network through intermolecular O—H···O hydrogen bonding interactions (Table 1) involving the uncoordinating water molecules, coordinating water molecules as donors and O atoms of 3,5-dinitrosalicylatato ligands as acceptors (Fig. 2).

Experimental

A mixture of barium chloride (1 mmol), 3,5-dinitrosalicylic acid (1 mmol), NaOH (1.5 mmol) and H₂O (12 ml) was placed in a 23 ml Teflon reactor, which was heated to 433 K for three days and then cooled to room temperature at a rate of 10 K h^-1. The obtained crystals obtained were washed with water and dryed in air.