Aqua­(4,5-dihydroxy­benzene-1,3-disulfonato-κO)bis­(1,10-phenanthroline-κ2 N,N’)cadmium(II) monohydrate

Xiangdong Zhang; Chunhua Ge; Lei Guan; Zhimin Sun

doi:10.1107/S1600536807067918

. 2008 Jan 23;64(Pt 2):m396–m397. doi: 10.1107/S1600536807067918

Aqua(4,5-dihydroxybenzene-1,3-disulfonato-κO)bis(1,10-phenanthroline-κ² N,N’)cadmium(II) monohydrate

Xiangdong Zhang ^a,^*, Chunhua Ge ^a, Lei Guan ^a, Zhimin Sun ^a

PMCID: PMC2960182 PMID: 21201347

Abstract

In the title compound, [Cd(C₆H₄O₈S₂)(C₁₂H₈N₂)₂(H₂O)]·H₂O, each Cd^II ion is coordinated by four N atoms [Cd—N = 2.310 (7)–2.341 (7) Å] from two 1,10-phenanthroline ligands, one O atom [Cd—O = 2.300 (6) Å] from a 4,5-dihydroxybenzene-1,3-disulfonate ligand and one aqua O atom [Cd—O = 2.288 (7) Å] in a distorted octahedral geometry. The crystal packing exhibits intermolecular O—H⋯O and C—H⋯O hydrogen bonds and π–π interactions evidenced by relatively short distances [3.525 (5)–3.937 (6) Å] between the centroids of the six-membered rings of neighbouring molecules.

Related literature

For related literature, see: Haddad & Raymond (1986 ▶); Riley et al. (1983 ▶); Sheriff et al. (2003 ▶); Sun et al. (1995 ▶).

Experimental

Crystal data

[Cd(C₆H₄O₈S₂)(C₁₂H₈N₂)₂(H₂O)]·H₂O
M _r = 777.05
Monoclinic,
a = 16.570 (5) Å
b = 9.330 (3) Å
c = 24.585 (6) Å
β = 127.199 (16)°
V = 3027.5 (15) Å³
Z = 4
Mo Kα radiation
μ = 0.93 mm⁻¹
T = 293 (2) K
0.30 × 0.20 × 0.18 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.816, T _max = 0.851
6494 measured reflections
5155 independent reflections
3318 reflections with I > 2σ(I)
R _int = 0.031

Refinement

R[F ² > 2σ(F ²)] = 0.067
wR(F ²) = 0.223
S = 1.16
5155 reflections
426 parameters
H-atom parameters constrained
Δρ_max = 1.32 e Å⁻³
Δρ_min = −2.31 e Å⁻³

Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT (Bruker, 2001 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a ▶); molecular graphics: SHELXTL (Sheldrick, 1997b ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807067918/cv2375sup1.cif

e-64-0m396-sup1.cif^{(29.4KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807067918/cv2375Isup2.hkl

e-64-0m396-Isup2.hkl^{(252.5KB, hkl)}

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

Table 1. Centroid-to-centroid distances (Å).

Cg1, Cg2, Cg3, Cg4, Cg5 and Cg6 are the centroids of N2/C6/C9–C12, N3/C13–C17, N4/C18/C21–C24, C4–C9, C16–C21 and C25–C30, respectively

Cg1⋯Cg4ⁱ	3.734 (7)
Cg1⋯Cg6ⁱⁱ	3.937 (6)
Cg2⋯Cg6ⁱⁱⁱ	3.525 (5)
Cg3⋯Cg3^iv	3.900 (7)
Cg4⋯Cg4ⁱ	3.533 (7)
Cg5⋯Cg5^v	3.606 (7)

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

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯O3	0.82	2.15	2.790 (10)	135
O1—H1B⋯O5^vi	0.82	1.93	2.735 (10)	167
O10—H10A⋯O6^vii	0.82	2.22	2.737 (19)	121
O10—H10B⋯O7	0.82	2.18	2.876 (15)	143
O8—H8⋯O7	0.82	1.87	2.614 (11)	150
O9—H9⋯O4^viii	0.82	1.90	2.690 (9)	160
C23—H23⋯O8^ix	0.93	2.57	3.465 (15)	163
C23—H23⋯O9^ix	0.93	2.40	3.112 (17)	134

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Symmetry codes: (vi) Inline graphic ; (vii) ; (viii) ; (ix) .

Acknowledgments

This project was supported by the Natural Science Foundation of the Education Bureau of Liaoning Province (grant No. 05L159).

supplementary crystallographic information

Comment

As a multi-group compound, 4,5-dihydroxybenzene-1,3-disulfonic acid (H₂dhds) is a good candidate for investigation of supramolecular assemblies (Haddad & Raymond, 1986; Riley et al., 1983; Sheriff et al., 2003; Sun et al., 1995). Herewith we present the title compound, (I), containing dhds anion as a coordinating ligand.

In (I) (Fig. 1), the dhds anion undoubtedly plays an important role in the formation and stabilization of the three dimesional supramolecular network (Fig.1). Each complex connects with six other complexes by inter-molecular O—H···O and C—H···O hydrogen bonds (Table 2). Significant π···π interactions between pairs of dhds and 1,10-phenanthroline or pairs of 1,10-phenanthrolines exist in (I) (Table 1).

Experimental

In a typical synthesis, hydrated nitrate (0.5 mmol), phen (1 mmol), 4,5-dihydroxybenzene-1,3-disulfonic acid (0.5 mmol) and NaOH (1 mmol) were mixed in ethanol:H₂O (v: v = 1:1, 20 ml) solution. The resulting mixture was stirred for 4 h and the solution was filtered. By slow evaporation of the solvent, block-shape single crystals suitable for X-ray analysis were obtained after several weeks.