Bis(di-2-pyridylmethane­diol-κ3 N,O,N′)copper(II) bis­(tetra­fluorido­borate) dihydrate

Krystal L Brown; Guy Crundwell; Barry L Westcott

doi:10.1107/S1600536809016973

. 2009 May 14;65(Pt 6):m642. doi: 10.1107/S1600536809016973

Bis(di-2-pyridylmethanediol-κ³ N,O,N′)copper(II) bis(tetrafluoridoborate) dihydrate

Krystal L Brown ^a, Guy Crundwell ^a, Barry L Westcott ^a,^*

PMCID: PMC2969716 PMID: 21583009

Abstract

The title complex, [Cu(C₁₁H₁₀N₂O₂)₂](BF₄)₂·2H₂O, was isolated as a dihydrate from a 1:2 molar mixture of copper(II) tetrafluoridoborate hexahydrate with di-2-pyridyl ketone in aqueous solution. The centrosymmetric complex cation is structurally similar to that found in previously reported salts and exhibits Cu—O bonds deviating by 25 degrees from an octahedral geometry by the so-called ‘off-axis angle’ distortion. The BF₄ ⁻ anion exhibits a two site disorder of the fluorine atoms [ratio 0.210 (8):0.790 (8)].

Related literature

For related structures, see: Wang et al. (1986 ▶); Tangoulis et al. (1997 ▶); Yang et al. (1998 ▶); Tong et al. (1998 ▶); Serna et al. (1999 ▶); Reinoso et al. (2003 ▶); Li et al. (2005 ▶).

Experimental

Crystal data

[Cu(C₁₁H₁₀N₂O₂)₂](BF₄)₂·2H₂O
M _r = 677.61
Monoclinic,
a = 7.8147 (2) Å
b = 14.4225 (4) Å
c = 12.1840 (3) Å
β = 101.160 (3)°
V = 1347.26 (6) Å³
Z = 2
Mo Kα radiation
μ = 0.91 mm⁻¹
T = 293 K
0.8 × 0.6 × 0.6 mm

Data collection

Oxford Diffraction Sapphire CCD diffractometer
Absorption correction: multi-scan SCALE3 ABSPACK in CrysAlis RED (Oxford Diffraction, 2006 ▶) T _min = 0.474, T _max = 0.579
25175 measured reflections
5349 independent reflections
4145 reflections with I > 2σ(I)
R _int = 0.036

Refinement

R[F ² > 2σ(F ²)] = 0.055
wR(F ²) = 0.192
S = 1.21
5349 reflections
219 parameters
10 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.72 e Å⁻³
Δρ_min = −1.03 e Å⁻³

Data collection: CrysAlis CCD (Oxford Diffraction, 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809016973/fj2210sup1.cif

e-65-0m642-sup1.cif^{(18.2KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809016973/fj2210Isup2.hkl

e-65-0m642-Isup2.hkl^{(261.9KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Cu1—N1ⁱ	2.0099 (19)
Cu1—N1	2.0099 (19)
Cu1—N2	2.0146 (19)
Cu1—N2ⁱ	2.0147 (19)
Cu1—O1	2.4312 (17)
Cu1—O1ⁱ	2.4312 (17)

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Symmetry code: (i) Inline graphic .

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2⋯O3	0.82	1.87	2.686 (3)	172

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Symmetry codes: .

Acknowledgments

The diffractometer was purchased with funding from the National Science Foundation (NSF # 0420322). Additional funding is from a CSUAAUP research grant.

supplementary crystallographic information

Experimental

All chemicals and reagents were purchased from Aldrich and used as received. di-2-pyridyl ketone (2 mmol) and copper(II) tetrafluorborate hexahydrate (1 mmol) were combined in 40 ml of water and stirred for 30 minutes. The resulting violet crystals were isolated after 48 h by slow evaporation of the solution.