{(+)-(1R,2R)-1,2-Diphenyl-2,2′-[ethane-1,2-diylbis(nitrilo­methyl­idyne)]­di­phenol­ato}dipyridine­cobalt(III) perchlorate sesquihydrate

Lian-Wen Zhou

doi:10.1107/S1600536809002293

. 2009 Jan 23;65(Pt 2):m226. doi: 10.1107/S1600536809002293

{(+)-(1R,2R)-1,2-Diphenyl-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}dipyridinecobalt(III) perchlorate sesquihydrate

Lian-Wen Zhou ^a,^*

PMCID: PMC2968403 PMID: 21581817

Abstract

In title complex, [Co(C₂₈H₂₂N₂O₂)(C₅H₅N)₂]ClO₄·1.5H₂O, the Co^III ion is in a slightly distorted octahedral coordination environment with the pyridine ligands in a trans arrangement. In addition to the cation and anion, the asymmetric unit also contains three half-occupancy solvent water molecules and all components are connected via intermolecular O—H⋯O hydrogen bonds.

Related literature

For background information, see: Amirnasr et al. (2001 ▶); Cmi et al. (1998 ▶); Polson et al. (1997 ▶); Yamada (1999 ▶); Henson et al. (1999 ▶). For the synthethis of the parent Schiff base ligand, see: Zhang et al. (1990 ▶). For a related structure, see: Shi et al. (1995 ▶).

Experimental

Crystal data

[Co(C₂₈H₂₂N₂O₂)(C₅H₅N)₂]ClO₄·1.5H₂O
M _r = 762.08
Orthorhombic,
a = 10.9214 (6) Å
b = 18.3856 (10) Å
c = 18.6714 (11) Å
V = 3749.2 (4) Å³
Z = 4
Mo Kα radiation
μ = 0.58 mm⁻¹
T = 293 (2) K
0.21 × 0.16 × 0.13 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.887, T _max = 0.928
20101 measured reflections
7290 independent reflections
4733 reflections with I > 2σ(I)
R _int = 0.059

Refinement

R[F ² > 2σ(F ²)] = 0.050
wR(F ²) = 0.127
S = 0.99
7290 reflections
480 parameters
H-atom parameters constrained
Δρ_max = 0.51 e Å⁻³
Δρ_min = −0.29 e Å⁻³
Absolute structure: Flack (1983 ▶), with 3227 Friedel pairs
Flack parameter: 0.02 (2)

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809002293/lh2754sup1.cif

e-65-0m226-sup1.cif^{(26.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809002293/lh2754Isup2.hkl

e-65-0m226-Isup2.hkl^{(356.7KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Co1—O2	1.881 (3)
Co1—O1	1.889 (3)
Co1—N2	1.897 (3)
Co1—N1	1.904 (3)
Co1—N4	1.973 (4)
Co1—N3	1.978 (4)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7C⋯O8	0.85	1.85	2.701 (12)	176
O7—H7D⋯O1ⁱ	0.85	2.04	2.888 (8)	176
O8—H8C⋯O9	0.85	1.73	2.575 (14)	177
O8—H8D⋯O4ⁱⁱ	0.85	1.99	2.835 (10)	176
O9—H9C⋯O3ⁱⁱ	0.85	2.36	3.175 (11)	161

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

supplementary crystallographic information

Comment

Cobalt complexes with tetradentate Schiff base ligands have been extensively used to mimic cobalamin (B₁₂) coenzymes (Amirnasr et al., 2001; Cmi et al., 1998; Polson et al., 1997) and dioxygen carriers and oxygen activators (Yamada, 1999; Henson et al., 1999). Here, we report the crystal structure of a Co^III complex containing the chiral tetradentate Schiff base ligand (+)-(1R,2R)-N,N'-Bis(salicylidene)-1,2-diphenyl-1,2-ethanediamine.

The molecular structure of the title cation is shown in Fig. 1. The Co^III ion is six coordinated. The four equational sites are occupied by two N atoms and two O atoms of the tetradentate Schiff base ligand and the two axial sites are occupied by the N atoms of two pyridine ligands, forming a slightly distorted octahedral coordination environment. The Co—O and Co—N_{Schiff base} bond lengths are consistent with the corresponding bond lengths in the Co^III Schiff base complex trans-[Co(salen)(py)₂][BPh₄] (Shi et al., 1995) as are the Co—N_py distances.

Experimental

The free Schiff base ligand (L), it was prepared according to the method reported previously (Zhang et al., 1990). The synthesis of the title complex was carried out by mixing CoClO₄.6H₂O, pyridine and L with a molar ratio 1:2:1 in methanol. After the mixture was stirred for about 30 min at room temperature in air, it was filtered to remove any undissolved material. The filtrate was allowed to partially evaporate in air for several days to produce crystals suitable for X-ray diffraction with a yield about 40%.