catena-Poly[[[aqua­copper(II)]bis­[μ-bis(3,5-dimethyl-1H-pyrazol-4-yl) selenide]] bis­(tetra­fluorido­borate) bis­(triphenyl­phosphine oxide) monohydrate]

Maksym Seredyuk; Kateryna O Znovjyak; Yurii S Moroz; Vadim A Pavlenko; Igor O Fritsky

doi:10.1107/S1600536810012997

. 2010 Apr 17;66(Pt 5):m527. doi: 10.1107/S1600536810012997

catena-Poly[[[aquacopper(II)]bis[μ-bis(3,5-dimethyl-1H-pyrazol-4-yl) selenide]] bis(tetrafluoridoborate) bis(triphenylphosphine oxide) monohydrate]

Maksym Seredyuk ^a,^*, Kateryna O Znovjyak ^a, Yurii S Moroz ^a, Vadim A Pavlenko ^a, Igor O Fritsky ^a

PMCID: PMC2979014 PMID: 21579021

Abstract

The title compound, {[Cu(C₁₀H₁₄N₄Se)₂(H₂O)](BF₄)₂·2C₁₈H₁₅PO·H₂O}_n, has a polymeric structure where each Cu^II ion adopts a square-pyramidal coordination constituted by four N atoms of pyrazole moieties in the equatorial plane and an axial O atom of a water molecule. A pair of bis(3,5-dimethyl-1H-pyrazol-4-yl) selenide ligands bridges the Cu^II centres into a chain extending along the c axis. The water molecules, anions and triphenylphosphine oxide molecules are involved in intermolecular hydrogen bonding, which links the chains into a three-dimensional network.

Related literature

For general background, see: Farha et al. (2009 ▶); Shibahara et al. (2007 ▶); Zhang et al. (2009 ▶). For related structures, see: Seredyuk et al. (2007 ▶, 2009 ▶).

Experimental

Crystal data

[Cu(C₁₀H₁₄N₄Se)₂(H₂O)](BF₄)₂·2C₁₈H₁₅OP·H₂O
M _r = 1386.17
Monoclinic,
a = 21.4560 (4) Å
b = 15.3590 (4) Å
c = 18.4910 (6) Å
β = 97.74 (2)°
V = 6038.0 (3) Å³
Z = 4
Mo Kα radiation
μ = 1.70 mm⁻¹
T = 100 K
0.09 × 0.07 × 0.04 mm

Data collection

Kuma KM4 CCD area-detector diffractometer
34362 measured reflections
6876 independent reflections
6210 reflections with I > 2σ(I)
R _int = 0.045

Refinement

R[F ² > 2σ(F ²)] = 0.043
wR(F ²) = 0.082
S = 1.16
6876 reflections
384 parameters
H-atom parameters constrained
Δρ_max = 0.63 e Å⁻³
Δρ_min = −0.38 e Å⁻³

Data collection: KM-4-CCD (Kuma, 1999 ▶); cell refinement: KM-4-CCD; data reduction: KM-4-CCD; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810012997/ds2023sup1.cif

e-66-0m527-sup1.cif^{(28.5KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810012997/ds2023Isup2.hkl

e-66-0m527-Isup2.hkl^{(329.8KB, 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
O1W—H1W⋯F2	0.90	2.14	3.002 (3)	161
O1W—H1W⋯F3	0.90	2.51	3.115 (3)	125
O1W—H2W⋯O2	0.95	1.90	2.785 (3)	155
O1—H1O⋯O2	0.81	1.95	2.752 (2)	173
N1—H1N⋯F4ⁱ	0.88	2.06	2.861 (3)	152
N4—H4N⋯O1Wⁱⁱ	0.88	1.86	2.730 (3)	170

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

Acknowledgments

The authors thank the Ministry of Education and Science of Ukraine for financial support (grant No. M/263-2008)

supplementary crystallographic information

Comment

Study of organometallic polymers is a well elaborated research area in coordination chemistry. Infinite molecular polymeric arrays are potentially applicable as specifically ordered crystalline substances with reversible selective sorption (Farha et al., 2009; Zhang et al., 2009), electrical conductivity (Zhang et al., 2009) and molecular magnetism functionality (Shibahara et al., 2007).

The title compound, [Cu(H₂O)(C₁₀H₁₄N₄Se)₂][(BF₄)₂.(Ph₃PO)₂.H₂O, was prepared in a water–methanolic medium by mixing solutions of Cu(BF₄)₂.6H₂O and the mixture of the ligand bis(3,5-dimethyl-1H-pyrazolyl)selenide (L) and trisphenylphosphine oxide. It has similar structure to the copper compounds reported recently (Seredyuk et al., 2007, 2009). A pyramidal environment of the Cu^II ion is constituted by four non-coplanar N atoms of pyrazolyl cycles (distances Cu—N are 1.997 (2) and 2.040 (2) Å, distance Cu—O is 2.222 (2) Å). Symmetrically equivalent ligand molecules in cis-bonding configuration are linked to Cu^II ion in a double-stranded bridge fashion (Fig. 1). Formed one-dimensional linear chain is running along the c axis where each Cu atom deviates from the average position by a value of ±0.279 (0) Å (Fig. 2). One of the pyrazole cycles of the ligand molecule is involved in hydrogen bonding with F atom of the tetrafluoroborate anion (N···F 2.861 (3) Å) which additionally forms a hydrogen bond with the free water molecule (F···OW 3.002 (3) Å). Further, the coordinated water molecule is connected through hydrogen bonds with the free water molecule (O···OW 2.785 (3) Å) and the Ph₃PO molecule (O···O 3.115 (3) Å).

Experimental

Bis(3,5-dimethyl-1H-pyrazolyl)selenide was prepared according to early reported method (Seredyuk et al., 2007). Copper(II) tetrafluoroborate hexahydrate (0.065 g, 0.19 mmol) in water (5 ml) was added to 5 ml of hot methanol solution of the ligand (0.100 g, 0.37 mmol) and thisphenylphosphine oxide (0.052 g, 0.19 mmol). After several days green crystals of the title compound suitable for X-ray analysis were isolated. Found: C 49.06, H 4.43, N 8.22; C₅₆H₆₂B₂CuF₈N₈O₄P₂Se₂ requires: C 49.16, H 4.57, N 8.19.