[(–)-(1S,2S)-N,N′-Bis(2-oxidobenzyl­idene)-1,2-diphenyl­ethane-1,2-diamine]­bis­(pyridine)cobalt(III) perchlorate methanol hemisolvate hemihydrate

Yu-Ting Chen

doi:10.1107/S1600536808031887

. 2008 Oct 9;64(Pt 11):m1377–m1378. doi: 10.1107/S1600536808031887

[(–)-(1S,2S)-N,N′-Bis(2-oxidobenzylidene)-1,2-diphenylethane-1,2-diamine]bis(pyridine)cobalt(III) perchlorate methanol hemisolvate hemihydrate

Yu-Ting Chen ^a,^*

PMCID: PMC2959631 PMID: 21580833

Abstract

In the title compound, [Co(C₂₈H₂₂N₂O₂)(C₅H₅N)₂]ClO₄·0.5CH₄O·0.5H₂O, each Co^III ion is coordinated by the tetradentate N,N′-bis(2-oxidobenzylidene)-1,2-diphenylethane-1,2-diamine ligand [Co—N = 1.900 (3) and 1.903 (3) Å; Co—O = 1.885 (3) and 1.891 (3) Å] and two pyridine ligands [Co—N = 1.967 (4) and 1.977 (3) Å] in a distorted octahedral geometry. The packing of the cations and anions forms voids of 258 Å³, which are filled by methanol and solvent water molecules with half occupancies. O—H⋯O hydrogen bonds between solvent molecules, perchlorate anions and water molecules, and between water molecules and O atoms of the ligand, help to consolidate the crystal packing.

Related literature

For related crystal structures, see: Korendovych & Rybak-Akimova (2003 ▶); Shi et al. (1995 ▶). For general background, see: Amirnasr et al. (2001 ▶); Botteher et al., 1997 ▶; Cmi et al. (1998 ▶); Henson et al. (1999 ▶); Polson et al. (1997 ▶); Yamada (1999 ▶); Zhang et al. (1990 ▶).

Experimental

Crystal data

[Co(C₂₈H₂₂N₂O₂)(C₅H₅N)₂]ClO₄·0.5CH₄O·0.5H₂O
M _r = 760.09
Orthorhombic,
a = 10.8900 (3) Å
b = 18.6219 (5) Å
c = 18.6557 (6) Å
V = 3783.24 (19) Å³
Z = 4
Mo Kα radiation
μ = 0.58 mm⁻¹
T = 273 (2) K
0.18 × 0.16 × 0.14 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ▶) T _min = 0.903, T _max = 0.924
42911 measured reflections
7407 independent reflections
5476 reflections with I > 2σ(I)
R _int = 0.064

Refinement

R[F ² > 2σ(F ²)] = 0.050
wR(F ²) = 0.145
S = 1.02
7407 reflections
463 parameters
13 restraints
H-atom parameters constrained
Δρ_max = 0.48 e Å⁻³
Δρ_min = −0.37 e Å⁻³
Absolute structure: Flack (1983 ▶), with 3248 Friedel pairs
Flack parameter: 0.03 (2)

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP (Sheldrick, 1998 ▶); software used to prepare material for publication: XP.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808031887/cv2457sup1.cif

e-64-m1377-sup1.cif^{(26.3KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808031887/cv2457Isup2.hkl

e-64-m1377-Isup2.hkl^{(362.4KB, 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
O8—H8D⋯O6ⁱ	0.85	1.98	2.831 (14)	178
O8—H8C⋯O7	0.85	1.96	2.807 (19)	177
O7—H7⋯O2	0.82	2.08	2.897 (11)	171

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Symmetry code: (i) Inline graphic .

Acknowledgments

This work was supported by the Natural Science Foundation of China.

supplementary crystallographic information

Comment

The cobalt complexes with tetradentate Schiff base ligands have been extensively studied due to their important utilities in mimic cobalamin (B₁₂) coenzymes (Amirnasr et al., 2001; Cmi et al., 1998; Polson et al., 1997), and as dioxygen carriers and oxygen activators (Yamada, 1999; Henson et al., 1999) . In addition, Co^III Schiff base complexes have also been used as antimicrobial agents when their two axial positions are occupied by two amine ligands (Botteher et al., 1997). Herein, we report the new Co^III complex based on the chiral tetradentate Schiff base ligand (-)-(1S,2S)-N,N'-Bis(salicylidene)-1,2- diphenyl-1,2-ethanediamine (L), whose structure has been reported recently (Korendovych & Rybak-Akimova, 2003).

In the cation (Fig. 1), the coordination sphere of Co^III ion is a distorted octahedron, in which four equational positions come from two N atoms and two O atoms of the tetradentate Schiff base ligand and the apical positions are occupied by N atoms of two pyridine molecules. The bond lengths of Co—O(L) and Co—N(L) are 1.885 (3), 1.891 (3)A% and 1.900 (3), 1.903 (3)A%, respectively, which are in agreement with the corresponding bond lengths in the similar Co^III Schiff base complex trans-[Co(salen)(py)₂][BPh₄] (Shi et al., 1995)). The distances of Co—N_py 1.967 (4) and 1.977 (3)A% are also consistent with those distances in the same complex, but slightly longer than the distances of Co—N_{Schiff base}.

Experimental

The free Schiff base ligand L was synthesized according to the literature (Zhang et al., 1990). The synthsis of the title complex was carried out by reacting CoClO₄.6H₂O, pyridine and L (molar ratio 1:2:1 in methanol. After the stirring process was continued for about 30 min at room temperature, the mixture was filtered and the filtrate was allowed to partial evaporate in air for several days to produce crystals suitable for X-ray diffraction. Anal. Calcd for C_38.5H₃₅ClCoN₄O₇: C, 60.84; H, 4.64; N, 7.37. Found: C, 60.64; H, 4.65; N, 7.39.