Bis{N,N-bis­[(diphenyl­phosphan­yl)meth­yl]aniline-κ2 P,P′}copper(I) tetra­fluoridoborate

Jing Shang; Li-Li Huang; Ting-Hong Huang; Kai Ma; Qing-Ling Ni

doi:10.1107/S160053681005186X

. 2010 Dec 18;67(Pt 1):m96. doi: 10.1107/S160053681005186X

Bis{N,N-bis[(diphenylphosphanyl)methyl]aniline-κ² P,P′}copper(I) tetrafluoridoborate

Jing Shang ^a, Li-Li Huang ^b, Ting-Hong Huang ^a, Kai Ma ^a, Qing-Ling Ni ^a,^*

PMCID: PMC3050340 PMID: 21522609

Abstract

In the cation of the title compound, [Cu(C₃₂H₂₉NP₂)₂]BF₄, the Cu^I atom is four-coordinated in a distorted tetrahedral geometry by four P atoms from two N,N-bis[(diphenylphosphanyl)methyl]aniline ligands. In the crystal, the cations are linked by C—H⋯π interactions, forming chains along the a axis. Intramolecular C—H⋯N and intermolecular C—H⋯F hydrogen bonds are also observed.

Related literature

For the structures and properties of related copper(I) complexes, see: Saravanabharathi et al. (2002 ▶); Chen et al. (2004 ▶); Sivasankar et al. (2004 ▶); Wang et al. (2008 ▶); Huang et al. (2009 ▶).

Experimental

Crystal data

[Cu(C₃₂H₂₉NP₂)₂]BF₄
M _r = 1129.35
Triclinic,
a = 11.004 (2) Å
b = 12.642 (3) Å
c = 21.725 (4) Å
α = 79.601 (3)°
β = 78.593 (3)°
γ = 76.110 (3)°
V = 2847.7 (10) Å³
Z = 2
Mo Kα radiation
μ = 0.55 mm⁻¹
T = 296 K
0.20 × 0.10 × 0.10 mm

Data collection

Bruker SMART 1000 CCD diffractometer
15689 measured reflections
9918 independent reflections
6522 reflections with I > 2σ(I)
R _int = 0.035

Refinement

R[F ² > 2σ(F ²)] = 0.059
wR(F ²) = 0.198
S = 1.06
9918 reflections
685 parameters
H-atom parameters constrained
Δρ_max = 0.73 e Å⁻³
Δρ_min = −0.47 e Å⁻³

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); data reduction: SAINT; 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 I, global. DOI: 10.1107/S160053681005186X/rz2534sup1.cif

e-67-00m96-sup1.cif^{(41.4KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S160053681005186X/rz2534Isup2.hkl

e-67-00m96-Isup2.hkl^{(485KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

Cg1 and Cg2 are the centroids of the C33–C38 and C1–C6 rings, respectively.

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C22—H22⋯N1	0.93	2.53	3.189 (6)	128
C7—H7A⋯F3ⁱ	0.97	2.25	3.181 (6)	161
C18—H18⋯Cg1ⁱ	0.93	2.72	3.653 (6)	177
C42—H42⋯Cg2ⁱⁱ	0.93	2.88	3.678 (5)	144

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

Acknowledgments

This work was supported by the Programme for Excellent Talents in Guangxi Higher Education Institutions and the Natural Science Foundation of Guangxi Province of China (No. 0832100).

supplementary crystallographic information

Comment

Copper(I) complexes containing phosphine ligands have received much attention so far due to their special structures, novel reactivity, as well as catalytic and luminescent properties (Saravanabharathi et al., 2002; Chen et al.,2004; Sivasankar et al., 2004; Wang et al., 2008; Huang et al., 2009). Herein, we report the synthesis and crystal structure of the new mononuclear copper(I) title complex.

In the cation of the title compound, the copper(I) atom adopts a distorted tetrahedral geometry provided by four P atoms from two phosphine ligands (Fig. 1). The Cu—P bond distances are in the range 2.2972 (12)–2.3153 (14) Å. An intramolecular C—H···N hydrogen bond is present (Table 1). In the crystal structure, intermolecular C—H···π interactions link adjacent cations into chains parallel to the a axis (Fig. 2). Intermolecular C—H···F hydrogen bonds involving the tetrafluoridoborate anion are also observed (Table 1).

Experimental

[Cu(CH₃CN)₄]BF₄ (0.0158 g, 0.05 mmol) was added with stirring to a solution of N,N-bis[(diphenylphosphanyl)methyl]aniline (0.0489 g, 0.10 mmol) in CH₃CN (5 ml). The resulting solution was allowed to stir for 1 h at room temperature. Slow diffusion of diethyl ether into the solution geve colourless block crystals suitable for X-ray analysis after three days.