catena-Poly[[(tetra­aqua­cadmium)-μ-4,4′-bipyridine-κ2 N:N′] 4-hy­droxy-3-sulfonato­benzoate monohydrate]

Shan Gao; Seik Weng Ng

doi:10.1107/S1600536812018727

. 2012 May 2;68(Pt 6):m715. doi: 10.1107/S1600536812018727

catena-Poly[[(tetraaquacadmium)-μ-4,4′-bipyridine-κ² N:N′] 4-hydroxy-3-sulfonatobenzoate monohydrate]

Shan Gao ^a, Seik Weng Ng ^b,^c,^*

PMCID: PMC3379062 PMID: 22719283

Abstract

The two independent Cd^II atoms in the polymeric title compound, [Cd(C₁₀H₈N₂)(H₂O)₄](C₇H₄O₆S)·H₂O, lie on twofold rotation axes, and each is coordinated by four water molecules and the N atoms of two 4,4′-bipyridine molecules in an octahedral geometry. Bridging gives rise to chains along [101] and [-101]. The 4-hydroxy-3-sulfonatobenzoate dianions are not connected to the Cd^II atoms, but form hydrogen bonds to the coordinated water molecules as well as the lattice water molecule, generating a three-dimensional network.

Related literature

For the 1,10-phenanthroline-chelated Mn^II derivative of 4-hydroxy-3-sulfonatobenzoic acid, see: Fang et al. (2011 ▶). graphic file with name e-68-0m715-scheme1.jpg

Experimental

Crystal data

[Cd(C₁₀H₈N₂)(H₂O)₄](C₇H₄O₆S)·H₂O
M _r = 574.83
Orthorhombic,
a = 16.3246 (10) Å
b = 15.3063 (11) Å
c = 16.5084 (10) Å
V = 4124.9 (5) Å³
Z = 8
Mo Kα radiation
μ = 1.23 mm⁻¹
T = 293 K
0.18 × 0.16 × 0.12 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.810, T _max = 0.867
61947 measured reflections
4705 independent reflections
3503 reflections with I > 2σ(I)
R _int = 0.057

Refinement

R[F ² > 2σ(F ²)] = 0.033
wR(F ²) = 0.090
S = 1.04
4705 reflections
334 parameters
11 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.84 e Å⁻³
Δρ_min = −0.87 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002 ▶); 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: publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812018727/bt5895sup1.cif

e-68-0m715-sup1.cif^{(23.5KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812018727/bt5895Isup2.hkl

e-68-0m715-Isup2.hkl^{(230.6KB, 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
O1w—H11⋯O5ⁱ	0.84 (1)	1.93 (1)	2.762 (4)	171 (5)
O1w—H12⋯O1	0.84 (1)	1.99 (2)	2.805 (3)	163 (5)
O2w—H21⋯O6ⁱⁱ	0.84 (1)	2.36 (2)	3.136 (3)	154 (4)
O2w—H22⋯O5wⁱⁱ	0.84 (1)	1.85 (1)	2.685 (4)	173 (5)
O3w—H31⋯O2ⁱⁱⁱ	0.84 (1)	2.08 (2)	2.858 (3)	155 (3)
O3w—H32⋯O6^iv	0.84 (1)	1.99 (1)	2.812 (3)	167 (4)
O4w—H41⋯O1^v	0.84 (1)	1.84 (1)	2.675 (3)	178 (4)
O4w—H42⋯O4^vi	0.84 (1)	2.10 (2)	2.869 (3)	154 (4)
O5w—H51⋯O2	0.84 (1)	1.96 (2)	2.779 (3)	166 (5)
O5w—H52⋯O6^vii	0.84 (1)	2.06 (2)	2.850 (4)	157 (6)
O3—H3⋯O2^viii	0.84 (1)	1.91 (1)	2.746 (3)	176 (4)

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

Acknowledgments

This work was supported by the Key Project of the Natural Science Foundation of Heilongjiang Province (No. ZD200903), the Key Project of the Education Bureau of Heilongjiang Province (Nos. 12511z023 and 2011CJHB006), the Innovation Team of the Education Bureau of Heilongjiang Province (No. 2010 t d03), Heilongjiang University (Hdtd2010–04) and the Ministry of Higher Education of Malaysia (grant No. UM.C/HIR/MOHE/SC/12).

supplementary crystallographic information

Comment

The doubly-deprotonated 4-hydroxy-3-sulfonatobenzoic acid ion functions in a chelating mode to connect Mn^II atoms into a chain motif. In this coordination polymer, the metal atom is chelated by 1,10-phenanthroline. When the N-heterocycle is replaced by 4,4'-bipyridine in the present synthesis (and with Cd replacing Mn), the dianion is now connected only indirectly, in an outer-sphere type of coordination. The two independent Cd atoms in polymeric [Cd(H₂O)₄(C₁₀H₈N₂)]^2+.(C₇H₄O₆S)^2–.H₂O lie on twofold rotation axes, and each is coordinated by four water molecules and the N atoms of two 4,4'-bipyridine molecules in an octahedral geometry (Fig. 1). µ-Bridging gives rise to a chain along [-1 0 1]. The C₇H₄O₆S^2– dianion interacts indirectly through the coordinated water molecules as well as through the lattice water molecule to generate a three-dimensional network (Table 1).

Experimental

A methanol solution (5 ml) of 4,4'-bipyridine (1 mmol) was added to an aqueous solution (10 ml) of cadium(II) dichloride (1 mmol), 2-hydroxy-5-carboxybenzenesulfonic acid (2 mmol) and lithium hydroxide (4 mmol). Colorless crystals were isolated from the solution after several days.