Issue contents
Download PDF of article
Download CIF
3D view
Navigation
Highlighting
Dictionary of Crystallography reference
IUPAC Gold Book reference
more ...
Download citation
FormatBIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Plain Text
share
Previous article
Next article
Previous article
Issue contents
Download PDF of article
Download CIF
3D view
Navigation
Highlighting
Dictionary of Crystallography reference
IUPAC Gold Book reference
more ...
Download citation
FormatBIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Plain Text
share
Next article

metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 64| Part 5| May 2008| Page m607
doi:10.1107/S1600536808008386

Bis(pyridine-κN)bis­­(tri­phenyl­phosphine-κP)copper(I) tetra­fluoridoborate

Peter C. Healya*

aSchool of Biomolecular and Physical Sciences, Griffith University, Nathan, Brisbane 4111, Australia
*Correspondence e-mail: p.healy@griffith.edu.au

(Received 26 March 2008; accepted 27 March 2008; online 2 April 2008)

The title compound, [Cu(C5H5N)2(C18H15P)2]BF4, crystallizes as discrete [(PPh3)2(py)2Cu]+ cations and [BF4]− anions and is isostructural with the analogous perchlorate salt. The anion is located in close proximity to the pyridine ligands with weak C—H⋯F inter­actions apparent. The P2CuN2 coordination geometry is pseudo-tetra­hedral, with P—Cu—P and N—Cu—N angles of 116.02 (6) and 101.5 (2)°, respectively.

Related literature

For background literature on copper(I)–phosphine adducts, see: Hanna et al. (1998[Hanna, J. V., Hart, R. D., Healy, P. C., Skelton, B. W. & White, A. H. (1998). J. Chem. Soc. Dalton Trans. pp. 2321-2325.], 2005[Hanna, J. V., Boyd, S. E., Healy, P. C., Bowmaker, G. A., Skelton, B. W. & White, A. H. (2005). Dalton Trans. pp. 2547-2556.]). For isostructural [(PPh3)2(py)2Cu][ClO4], see: Engelhardt et al. (1985[Engelhardt, L. M., Pakawatchai, C., White, A. H. & Healy, P. C. (1985). J. Chem. Soc. Dalton Trans. pp. 125-133.])

[Scheme 1]

Experimental

Crystal data

  • [Cu(C5H5N)2(C18H15P)2]BF4

  • Mr = 833.10

  • Triclinic, [P \overline 1]

  • a = 10.890 (5) Å

  • b = 13.488 (6) Å

  • c = 15.547 (6) Å

  • α = 84.97 (3)°

  • β = 109.59 (3)°

  • γ = 101.93 (3)°

  • V = 2104.5 (16) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.65 mm−1

  • T = 295 (2) K

  • 0.50 × 0.30 × 0.15 mm
Data collection

  • Rigaku AFC-7R diffractometer

  • Absorption correction: ψ scan (North et al., 1968[North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.]) Tmin = 0.738, Tmax = 0.909

  • 8222 measured reflections

  • 7393 independent reflections

  • 4745 reflections with I > 2σ(I)

  • Rint = 0.035

  • 3 standard reflections every 150 reflections intensity decay: 0.6%
Refinement

  • R[F2 > 2σ(F2)] = 0.057

  • wR(F2) = 0.180

  • S = 1.03

  • 7393 reflections

  • 505 parameters

  • H-atom parameters constrained

  • Δρmax = 0.86 e Å−3

  • Δρmin = −0.63 e Å−3

Table 1
Selected geometric parameters (Å, °)

Cu1—P1 2.2712 (17)
Cu1—P2 2.2955 (16)
Cu1—N1 2.091 (4)
Cu1—N2 2.113 (5)
P1—Cu1—P2 116.02 (6)
P1—Cu1—N1 112.68 (12)
P1—Cu1—N2 113.03 (13)
P2—Cu1—N1 109.04 (12)
P2—Cu1—N2 103.22 (12)
N1—Cu1—N2 101.51 (17)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
C11—H11⋯F2 0.95 2.43 3.157 (12) 133
C22—H22⋯F1i 0.95 2.53 3.421 (11) 156
Symmetry code: (i) -x+1, -y+1, -z.

Data collection: MSC/AFC7 Diffractometer Control for Windows (Molecular Structure Corporation, 1999[Molecular Structure Corporation (1999). MSC/AFC7 Diffractometer Control for Windows. MSC, The Woodlands, Texas, USA.]); cell refinement: MSC/AFC7 Diffractometer Control for Windows; data reduction: TEXSAN for Windows (Molecular Structure Corporation, 2001[Molecular Structure Corporation. (2001). TEXSAN for Windows. MSC, The Woodlands, Texas, USA.]); program(s) used to solve structure: TEXSAN for Windows; program(s) used to refine structure: TEXSAN for Windows and SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: TEXSAN for Windows and PLATON (Spek, 2003[Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.]).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808008386/ng2437sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808008386/ng2437Isup2.hkl

checkCIF report


Comment top

The structure of (I) consists of discrete [PPh3)2(pyr)2Cu]+ cations and [BF4]- anions (Fig. 1) and is isostructural with the analogous perchlorate complex (Engelhardt et al., 1985). The anion is located in the neighbourhood of the pyridine ligands on the cation with weak C—H···F interactions apparent (Table 2). The P2CuN2 coordination geometry (Table 1) is pseudo-tetrahedral with P—Cu—P and N—Cu—N angles of 116.02 (6) and 101.51 (17)° respectively. For comparison, the P—Cu—P and N—Cu—N angles for [PPh3)2(CH3CN)2]BF4 are 127.1 (1) and 99.5 (4)° (Hanna et al., 1998). The Cu—P bond lengths of 2.271 (2), 2.296 (2)Å for (I) are similar to the values of 2.269 (1), 2.287 (2)Å recorded for [PPh3)2(CH3CN)2]BF4. The Cu—N bond lengths for (I), however, are longer with values of 2.091 (4), 2.113 (5)Å compared to 2.039 (4), 2.049 (2) Å. These differences in bond length and angular geometries are likely to a result of increased steric crowding of the 'two dimensional' pyridine ligand by comparison with the linear acetonitrile ligand.

Related literature top

For background literature on copper(I)–phosphine adducts, see: Hanna et al. (1998, 2005). For isostructural [(PPh3)2(py)2Cu][ClO4], see: Engelhardt et al. (1985)

Experimental top

[(PPh3)3CuBF4] (Hanna et al., 2005) (0.52 g, 0.540 mmol) was dissolved in 15 ml boiling ethanol. Pyridine (2 ml) was added and the solution allowed to cool to room temperature. Slow evaporation of solvent resulted in crystallization of colourless crystals of the complex suitable for X-ray diffraction studies.

Refinement top

H atoms were constrained as riding atoms, with C—H set to 0.95 Å. Uiso(H) values were set to 1.2Ueq of the parent atom.

Computing details top

Data collection: MSC/AFC7 Diffractometer Control for Windows (Molecular Structure Corporation, 1999); cell refinement: MSC/AFC7 Diffractometer Control for Windows (Molecular Structure Corporation, 1999); data reduction: TEXSAN for Windows (Molecular Structure Corporation, 2001); program(s) used to solve structure: TEXSAN for Windows (Molecular Structure Corporation, 2001); program(s) used to refine structure: TEXSAN for Windows (Molecular Structure Corporation, 2001) and SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: TEXSAN for Windows (Molecular Structure Corporation, 2001) and PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 30% probability level. H atoms are included with arbitrary radii.
Bis(pyridine-κN)bis(triphenylphosphine-κP)copper(I) tetrafluoridoborate top
Crystal data top
[Cu(C5H5N)2(C18H15P)2]BF4Z = 2
Mr = 833.10F(000) = 860
Triclinic, P1Dx = 1.315 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.7107 Å
a = 10.890 (5) ÅCell parameters from 23 reflections
b = 13.488 (6) Åθ = 12.5–14.9°
c = 15.547 (6) ŵ = 0.65 mm−1
α = 84.97 (3)°T = 295 K
β = 109.59 (3)°Prismatic, colourless
γ = 101.93 (3)°0.50 × 0.30 × 0.15 mm
V = 2104.5 (16) Å3
Data collection top
Rigaku AFC-7R
diffractometer		4745 reflections with I > 2σ(I)
Radiation source: Rigaku rotating anodeRint = 0.035
Graphite monochromatorθmax = 25.0°, θmin = 2.8°
ω–2θ scansh = −12→5
Absorption correction: ψ scan
(North et al., 1968)		k = −15→16
Tmin = 0.738, Tmax = 0.909l = −17→18
8222 measured reflections3 standard reflections every 150 reflections
7393 independent reflections intensity decay: 0.6%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.180H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0978P)2 + 0.8077P]
where P = (Fo2 + 2Fc2)/3
7393 reflections(Δ/σ)max = 0.003
505 parametersΔρmax = 0.86 e Å−3
0 restraintsΔρmin = −0.63 e Å−3
Crystal data top
[Cu(C5H5N)2(C18H15P)2]BF4γ = 101.93 (3)°
Mr = 833.10V = 2104.5 (16) Å3
Triclinic, P1Z = 2
a = 10.890 (5) ÅMo Kα radiation
b = 13.488 (6) ŵ = 0.65 mm−1
c = 15.547 (6) ÅT = 295 K
α = 84.97 (3)°0.50 × 0.30 × 0.15 mm
β = 109.59 (3)°
Data collection top
Rigaku AFC-7R
diffractometer		4745 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)		Rint = 0.035
Tmin = 0.738, Tmax = 0.9093 standard reflections every 150 reflections
8222 measured reflections intensity decay: 0.6%
7393 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0570 restraints
wR(F2) = 0.180H-atom parameters constrained
S = 1.03Δρmax = 0.86 e Å−3
7393 reflectionsΔρmin = −0.63 e Å−3
505 parameters
Special details top

Experimental. The scan width was (1.63 + 0.30tanθ)° with an ω scan speed of 16° per minute (up to 4 scans to achieve I/σ(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1.

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.46141 (5)0.28505 (4)0.26070 (3)0.0484 (2)
P10.29384 (11)0.36519 (8)0.25296 (7)0.0479 (3)
P20.40161 (11)0.11504 (8)0.23049 (8)0.0474 (3)
N10.6167 (4)0.3073 (3)0.3847 (2)0.0552 (12)
N20.5606 (4)0.3441 (3)0.1662 (3)0.0567 (12)
C110.7030 (5)0.3947 (4)0.4011 (4)0.0717 (19)
C120.8051 (6)0.4137 (5)0.4833 (5)0.093 (2)
C130.8198 (6)0.3400 (7)0.5494 (4)0.095 (3)
C140.7324 (7)0.2507 (5)0.5330 (4)0.089 (2)
C150.6334 (5)0.2366 (4)0.4502 (3)0.0636 (17)
C210.4905 (5)0.3665 (4)0.0801 (4)0.0690 (17)
C220.5399 (7)0.3781 (5)0.0084 (4)0.084 (2)
C230.6672 (7)0.3692 (5)0.0249 (4)0.088 (3)
C240.7440 (6)0.3517 (5)0.1131 (5)0.087 (2)
C250.6879 (5)0.3393 (4)0.1808 (4)0.0708 (19)
C1110.2321 (5)0.3414 (4)0.3501 (3)0.0587 (17)
C1120.3261 (7)0.3485 (4)0.4363 (4)0.081 (2)
C1130.2820 (11)0.3314 (6)0.5138 (4)0.109 (4)
C1140.1482 (12)0.3075 (6)0.5017 (7)0.116 (4)
C1150.0590 (10)0.2995 (7)0.4180 (7)0.120 (4)
C1160.0997 (7)0.3173 (5)0.3443 (4)0.092 (3)
C1210.3246 (5)0.5026 (3)0.2445 (3)0.0517 (14)
C1220.2309 (5)0.5585 (4)0.2463 (3)0.0664 (17)
C1230.2574 (7)0.6627 (4)0.2386 (4)0.081 (3)
C1240.3758 (7)0.7121 (4)0.2304 (4)0.081 (2)
C1250.4710 (6)0.6597 (4)0.2285 (4)0.078 (2)
C1260.4445 (5)0.5546 (4)0.2352 (3)0.0624 (17)
C1310.1482 (4)0.3265 (3)0.1530 (3)0.0514 (14)
C1320.1208 (5)0.3868 (4)0.0746 (3)0.0652 (17)
C1330.0207 (6)0.3505 (5)−0.0047 (4)0.083 (2)
C134−0.0496 (6)0.2550 (6)−0.0061 (4)0.095 (3)
C135−0.0232 (6)0.1931 (4)0.0698 (5)0.086 (2)
C1360.0754 (5)0.2285 (4)0.1491 (4)0.0688 (17)
C2110.2640 (4)0.0412 (3)0.2632 (3)0.0497 (14)
C2120.2424 (5)0.0666 (4)0.3404 (4)0.0647 (17)
C2130.1408 (6)0.0100 (5)0.3689 (4)0.081 (2)
C2140.0599 (5)−0.0729 (5)0.3199 (5)0.080 (2)
C2150.0768 (5)−0.0978 (4)0.2436 (5)0.076 (2)
C2160.1779 (5)−0.0418 (4)0.2135 (4)0.0655 (17)
C2210.5348 (4)0.0446 (3)0.2882 (3)0.0535 (16)
C2220.5237 (5)−0.0362 (4)0.3464 (4)0.0714 (19)
C2230.6289 (7)−0.0850 (5)0.3898 (5)0.095 (3)
C2240.7473 (7)−0.0526 (6)0.3746 (5)0.099 (3)
C2250.7632 (6)0.0313 (5)0.3178 (5)0.089 (3)
C2260.6557 (5)0.0784 (4)0.2738 (4)0.073 (2)
C2310.3568 (5)0.0846 (4)0.1109 (3)0.0633 (17)
C2320.2883 (6)0.1468 (5)0.0460 (4)0.083 (2)
C2330.2507 (8)0.1311 (8)−0.0457 (5)0.114 (3)
C2340.2762 (8)0.0461 (11)−0.0741 (5)0.142 (5)
C2350.3421 (7)−0.0196 (8)−0.0116 (6)0.122 (4)
C2360.3837 (5)−0.0021 (5)0.0824 (4)0.081 (2)
F10.7323 (6)0.5919 (5)0.1749 (6)0.242 (4)
F20.8547 (13)0.5615 (6)0.2980 (6)0.353 (7)
F30.9394 (7)0.6435 (7)0.2124 (6)0.240 (5)
F40.8438 (8)0.7146 (5)0.2723 (5)0.213 (4)
B10.8395 (8)0.6264 (7)0.2351 (5)0.098 (3)
H110.694700.445500.354300.0880*
H120.864400.477900.492300.1070*
H130.888300.351800.605800.1140*
H140.739400.198500.579000.1060*
H150.575300.174000.439900.0770*
H210.400500.372400.068300.0820*
H220.484100.39180−0.051400.0960*
H230.703800.37580−0.023400.1070*
H240.835700.347800.126700.1060*
H250.741100.326800.241900.0870*
H1120.418000.363700.442400.0960*
H1130.352000.339400.572900.1320*
H1140.126700.296100.557200.1500*
H115−0.028600.283000.414600.1400*
H1160.034200.313300.285600.1120*
H1220.148500.524300.251600.0770*
H1230.193800.700500.241200.0930*
H1240.392600.783400.226000.0970*
H1250.552600.693300.222000.0920*
H1260.507500.517800.233800.0730*
H1320.169700.453600.076000.0780*
H1330.005000.39260−0.058400.1000*
H134−0.116700.23070−0.060500.1150*
H135−0.073500.126500.067900.1020*
H1360.094000.184700.202300.0820*
H2120.298300.123500.373600.0760*
H2130.127600.028400.422400.0970*
H214−0.00790−0.113000.340700.1010*
H2150.02100−0.154300.209100.0950*
H2160.18950−0.060300.160000.0760*
H2220.44130−0.059300.356700.0840*
H2230.61980−0.140400.430200.1160*
H2240.81840−0.087100.402500.1170*
H2250.847400.055500.311000.1070*
H2260.665100.134900.233500.0850*
H2320.265500.204400.065100.0950*
H2330.206200.17630−0.088400.1410*
H2340.250700.03440−0.137600.1820*
H2350.36150−0.07740−0.031800.1450*
H2360.42900−0.048000.125900.1030*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0446 (3)0.0460 (3)0.0477 (3)0.0085 (2)0.0067 (2)0.0012 (2)
P10.0507 (6)0.0444 (6)0.0448 (6)0.0139 (5)0.0081 (5)0.0010 (5)
P20.0475 (6)0.0450 (6)0.0470 (6)0.0069 (5)0.0114 (5)−0.0069 (5)
N10.054 (2)0.052 (2)0.050 (2)0.0125 (18)0.0021 (17)−0.0040 (17)
N20.053 (2)0.060 (2)0.054 (2)0.0083 (18)0.0175 (18)0.0096 (18)
C110.060 (3)0.056 (3)0.079 (4)0.004 (2)−0.001 (3)−0.008 (3)
C120.058 (3)0.088 (4)0.110 (5)−0.001 (3)−0.002 (3)−0.043 (4)
C130.071 (4)0.141 (6)0.059 (3)0.035 (4)−0.010 (3)−0.026 (4)
C140.094 (4)0.102 (5)0.055 (3)0.030 (4)0.000 (3)0.006 (3)
C150.068 (3)0.066 (3)0.046 (3)0.016 (3)0.003 (2)0.001 (2)
C210.063 (3)0.075 (3)0.065 (3)0.016 (3)0.019 (3)0.019 (3)
C220.093 (4)0.089 (4)0.068 (4)0.020 (3)0.028 (3)0.022 (3)
C230.099 (5)0.095 (4)0.086 (4)0.021 (4)0.053 (4)0.015 (3)
C240.063 (3)0.110 (5)0.093 (4)0.020 (3)0.035 (3)0.014 (4)
C250.060 (3)0.082 (4)0.066 (3)0.012 (3)0.019 (3)0.012 (3)
C1110.077 (3)0.053 (3)0.053 (3)0.025 (2)0.024 (2)0.005 (2)
C1120.117 (5)0.081 (4)0.052 (3)0.049 (4)0.018 (3)0.003 (3)
C1130.185 (9)0.096 (5)0.058 (4)0.074 (6)0.032 (5)0.013 (3)
C1140.185 (9)0.095 (5)0.110 (6)0.055 (6)0.093 (7)0.023 (5)
C1150.145 (7)0.130 (7)0.115 (6)0.024 (6)0.086 (6)0.012 (5)
C1160.099 (5)0.110 (5)0.082 (4)0.025 (4)0.048 (4)0.004 (4)
C1210.059 (3)0.049 (2)0.040 (2)0.014 (2)0.0051 (19)0.0008 (18)
C1220.075 (3)0.059 (3)0.063 (3)0.024 (3)0.013 (3)0.000 (2)
C1230.117 (5)0.062 (4)0.068 (4)0.042 (4)0.019 (3)0.000 (3)
C1240.117 (5)0.042 (3)0.068 (3)0.016 (3)0.009 (3)−0.003 (2)
C1250.085 (4)0.052 (3)0.074 (4)−0.004 (3)0.007 (3)0.004 (3)
C1260.063 (3)0.057 (3)0.054 (3)0.013 (2)0.001 (2)0.000 (2)
C1310.044 (2)0.056 (3)0.052 (2)0.013 (2)0.0101 (19)−0.003 (2)
C1320.071 (3)0.069 (3)0.051 (3)0.019 (3)0.011 (2)0.001 (2)
C1330.091 (4)0.090 (4)0.053 (3)0.025 (3)−0.001 (3)−0.006 (3)
C1340.083 (4)0.096 (5)0.082 (4)0.026 (4)−0.018 (3)−0.030 (4)
C1350.063 (3)0.067 (4)0.106 (5)0.005 (3)−0.001 (3)−0.022 (3)
C1360.055 (3)0.062 (3)0.075 (3)0.011 (2)0.004 (2)0.004 (3)
C2110.047 (2)0.042 (2)0.057 (3)0.0114 (19)0.012 (2)0.0024 (19)
C2120.070 (3)0.061 (3)0.065 (3)0.008 (2)0.026 (3)−0.006 (2)
C2130.089 (4)0.084 (4)0.084 (4)0.022 (3)0.047 (3)0.010 (3)
C2140.058 (3)0.074 (4)0.112 (5)0.013 (3)0.035 (3)0.014 (3)
C2150.055 (3)0.061 (3)0.104 (5)−0.001 (2)0.021 (3)−0.001 (3)
C2160.059 (3)0.063 (3)0.072 (3)0.005 (2)0.020 (3)−0.010 (2)
C2210.053 (3)0.047 (2)0.057 (3)0.012 (2)0.009 (2)−0.013 (2)
C2220.067 (3)0.064 (3)0.083 (4)0.018 (3)0.022 (3)0.004 (3)
C2230.104 (5)0.094 (5)0.091 (5)0.053 (4)0.022 (4)0.016 (4)
C2240.096 (5)0.126 (6)0.086 (4)0.070 (5)0.018 (4)0.003 (4)
C2250.070 (4)0.109 (5)0.099 (5)0.037 (4)0.029 (3)−0.008 (4)
C2260.063 (3)0.076 (4)0.087 (4)0.021 (3)0.031 (3)0.000 (3)
C2310.052 (3)0.082 (3)0.053 (3)0.001 (2)0.016 (2)−0.018 (3)
C2320.072 (4)0.106 (5)0.054 (3)0.003 (3)0.007 (3)−0.008 (3)
C2330.094 (5)0.173 (8)0.052 (4)0.001 (5)0.006 (3)−0.005 (4)
C2340.084 (5)0.259 (13)0.059 (4)−0.031 (7)0.018 (4)−0.051 (6)
C2350.075 (4)0.187 (9)0.107 (6)−0.020 (5)0.038 (4)−0.089 (6)
C2360.066 (3)0.100 (4)0.081 (4)−0.004 (3)0.031 (3)−0.038 (3)
F10.112 (4)0.207 (6)0.317 (9)0.049 (4)−0.087 (5)−0.127 (6)
F20.499 (17)0.195 (7)0.194 (8)−0.134 (9)0.028 (9)0.070 (6)
F30.150 (5)0.316 (10)0.282 (9)−0.008 (6)0.122 (6)−0.071 (8)
F40.261 (8)0.156 (5)0.207 (6)−0.070 (5)0.103 (6)−0.079 (5)
B10.081 (5)0.103 (6)0.079 (5)−0.050 (4)0.025 (4)0.000 (4)
Geometric parameters (Å, º) top
Cu1—P12.2712 (17)C133—C1341.353 (10)
Cu1—P22.2955 (16)C134—C1351.368 (9)
Cu1—N12.091 (4)C135—C1361.380 (9)
Cu1—N22.113 (5)C211—C2161.401 (7)
P1—C1111.828 (5)C211—C2121.381 (7)
P1—C1211.815 (4)C112—H1120.9500
P1—C1311.830 (5)C212—C2131.387 (9)
P2—C2111.817 (5)C113—H1130.9800
P2—C2211.833 (5)C213—C2141.378 (9)
P2—C2311.818 (5)C114—H1140.9600
F1—B11.255 (12)C214—C2151.340 (10)
F2—B11.246 (12)C115—H1150.9200
F3—B11.225 (13)C215—C2161.393 (8)
F4—B11.353 (11)C116—H1160.9500
N1—C151.325 (6)C221—C2221.366 (7)
N1—C111.331 (7)C221—C2261.387 (8)
N2—C211.344 (7)C222—C2231.384 (10)
N2—C251.342 (8)C122—H1220.9500
C11—C121.386 (9)C223—C2241.365 (11)
C12—C131.359 (10)C123—H1230.9500
C13—C141.356 (11)C224—C2251.392 (10)
C14—C151.372 (8)C124—H1240.9400
C21—C221.376 (9)C225—C2261.392 (9)
C22—C231.352 (11)C125—H1250.9400
C23—C241.375 (10)C126—H1260.9300
C24—C251.366 (9)C231—C2321.373 (8)
C111—C1161.385 (10)C231—C2361.403 (8)
C11—H110.9500C132—H1320.9500
C111—C1121.384 (8)C232—C2331.368 (10)
C112—C1131.425 (11)C233—C2341.374 (16)
C12—H120.9600C133—H1330.9500
C113—C1141.377 (18)C234—C2351.374 (15)
C13—H130.9400C134—H1340.9400
C114—C1151.335 (15)C135—H1350.9500
C14—H140.9500C235—C2361.403 (11)
C15—H150.9300C136—H1360.9600
C115—C1161.347 (13)C212—H2120.9400
C121—C1261.396 (8)C213—H2130.9500
C21—H210.9500C214—H2140.9500
C121—C1221.397 (8)C215—H2150.9500
C22—H220.9500C216—H2160.9400
C122—C1231.378 (7)C222—H2220.9500
C23—H230.9500C223—H2230.9400
C123—C1241.365 (11)C224—H2240.9400
C124—C1251.379 (10)C225—H2250.9500
C24—H240.9600C226—H2260.9500
C25—H250.9500C232—H2320.9600
C125—C1261.389 (7)C233—H2330.9400
C131—C1321.385 (6)C234—H2340.9500
C131—C1361.389 (7)C235—H2350.9500
C132—C1331.390 (8)C236—H2360.9600
Cu1···H1123.3100C221···H152.9200
Cu1···H1263.0900C222···H124xi3.0100
Cu1···H2123.2900C224···H213vii3.0100
Cu1···H2263.4400C225···H234x2.9600
Cu1···H2323.2000C226···H2363.0700
P2···N23.457 (5)C231···H2162.6300
F1···C253.338 (9)C232···H213.0400
F2···C113.157 (12)C234···H135xii2.8800
F3···C123i3.306 (12)C235···H135xii2.8600
F4···C215ii3.309 (10)C235···H235x3.0900
F4···C214ii3.274 (10)C236···H235x3.0900
F1···H22iii2.5300C236···H2162.7200
F1···H1262.8600H11···F22.4300
F2···H13iv2.7500H11···H1262.5600
F2···H112.4300H12···C114v2.9400
F3···H133iii2.7600H13···F2iv2.7500
F3···H123i2.6100H13···F3iv2.8200
F3···H215ii2.6900H14···C214vii2.9800
F3···H13iv2.8200H15···C2212.9200
F4···H215ii2.7200H21···C2323.0400
F4···H214ii2.6200H21···H2322.4300
F4···H114v2.5600H22···F1iii2.5300
N1···N23.255 (6)H25···N12.9300
N2···N13.255 (6)H25···C112.8900
N2···P23.457 (5)H25···H2262.5500
N1···H252.9300H112···Cu13.3100
N1···H1122.8600H112···N12.8600
N2···H1262.8900H113···C125v3.0400
C11···C253.512 (8)H114···F4v2.5600
C11···F23.157 (12)H116···H1362.5600
C15···C2213.519 (7)H116···C1312.7200
C21···C2323.272 (9)H116···C1362.7000
C22···C22iii3.538 (10)H122···C1163.0600
C25···C113.512 (8)H122···C1112.9300
C25···F13.338 (9)H123···F3vi2.6100
C11···H252.8900H124···C222xiii3.0100
C116···C1363.268 (9)H126···Cu13.0900
C21···H2322.8900H126···F12.8600
C122···C1323.423 (7)H126···H112.5600
C123···F3vi3.306 (12)H126···N22.8900
C25···H2262.7900H132···C1212.6500
C132···C1223.423 (7)H132···C1222.9200
C136···C2113.559 (7)H133···F3iii2.7600
C136···C1163.268 (9)H134···C123ix3.0700
C111···H1363.0400H135···C234xii2.8800
C211···C1363.559 (7)H135···C235xii2.8600
C111···H1222.9300H136···C1113.0400
C212···C2223.586 (8)H136···C1162.9400
C113···H223vii2.9400H136···C2112.8400
C114···H12v2.9400H136···C2122.8100
C214···F4viii3.274 (10)H136···H1162.5600
C215···F4viii3.309 (10)H212···Cu13.2900
C116···H1223.0600H213···C224vii3.0100
C116···H1362.9400H214···F4viii2.6200
C216···C2363.441 (9)H214···H224vi2.4800
C221···C153.519 (7)H215···F3viii2.6900
C121···H1322.6500H215···F4viii2.7200
C122···H1322.9200H215···H233xii2.5300
C222···C2123.586 (8)H216···C2312.6300
C123···H134ix3.0700H216···C2362.7200
C125···H113v3.0400H222···C2112.5600
C226···C2363.483 (8)H222···C2122.9500
C131···H2322.9400H222···C2163.0200
C131···H1162.7200H223···C113vii2.9400
C232···C213.272 (9)H224···H214i2.4800
C235···C236x3.464 (11)H226···C252.7900
C235···C235x3.269 (12)H226···H252.5500
C136···H2322.8700H226···Cu13.4400
C236···C235x3.464 (11)H232···Cu13.2000
C236···C2163.441 (9)H232···C1312.9400
C136···H1162.7000H232···C1362.8700
C236···C2263.483 (8)H232···C212.8900
C211···H2222.5600H232···H212.4300
C211···H1362.8400H233···H215xii2.5300
C212···H2222.9500H234···C225x2.9600
C212···H1362.8100H235···C235x3.0900
C214···H14vii2.9800H235···C236x3.0900
C216···H2223.0200H236···C2212.6900
C221···H2362.6900H236···C2263.0700
P1—Cu1—P2116.02 (6)C112—C113—H113115.00
P1—Cu1—N1112.68 (12)C212—C213—C214119.9 (6)
P1—Cu1—N2113.03 (13)C114—C113—H113125.00
P2—Cu1—N1109.04 (12)C113—C114—H114115.00
P2—Cu1—N2103.22 (12)C115—C114—H114125.00
N1—Cu1—N2101.51 (17)C213—C214—C215120.4 (6)
Cu1—P1—C111115.25 (18)C214—C215—C216120.7 (6)
Cu1—P1—C121117.97 (19)C114—C115—H115116.00
Cu1—P1—C131111.42 (15)C116—C115—H115124.00
C111—P1—C121102.0 (2)C211—C216—C215120.2 (5)
C111—P1—C131105.0 (2)C111—C116—H116119.00
C121—P1—C131103.8 (2)C115—C116—H116118.00
Cu1—P2—C211118.50 (15)C222—C221—C226118.4 (5)
Cu1—P2—C221113.17 (14)P2—C221—C222124.3 (4)
Cu1—P2—C231114.85 (18)P2—C221—C226117.3 (3)
C211—P2—C221101.9 (2)C121—C122—H122120.00
C211—P2—C231102.9 (2)C221—C222—C223121.7 (6)
C221—P2—C231103.6 (2)C123—C122—H122120.00
Cu1—N1—C11120.6 (3)C222—C223—C224119.9 (6)
Cu1—N1—C15122.2 (3)C124—C123—H123120.00
C11—N1—C15117.2 (4)C122—C123—H123120.00
Cu1—N2—C21120.0 (4)C223—C224—C225119.9 (7)
Cu1—N2—C25122.5 (4)C125—C124—H124120.00
C21—N2—C25115.8 (5)C123—C124—H124119.00
N1—C11—C12122.5 (5)C126—C125—H125120.00
C11—C12—C13119.1 (6)C124—C125—H125122.00
C12—C13—C14118.6 (6)C224—C225—C226119.3 (7)
C13—C14—C15119.5 (6)C121—C126—H126119.00
N1—C15—C14123.1 (5)C221—C226—C225120.8 (5)
N2—C21—C22123.8 (6)C125—C126—H126120.00
C21—C22—C23118.8 (6)C232—C231—C236118.7 (5)
C22—C23—C24118.9 (6)P2—C231—C236122.9 (4)
C23—C24—C25119.1 (7)P2—C231—C232118.4 (4)
N2—C25—C24123.4 (6)C133—C132—H132120.00
P1—C111—C112116.9 (5)C231—C232—C233123.0 (7)
P1—C111—C116125.4 (4)C131—C132—H132119.00
C112—C111—C116117.7 (5)C134—C133—H133121.00
C12—C11—H11119.00C132—C133—H133119.00
N1—C11—H11119.00C232—C233—C234118.5 (8)
C13—C12—H12121.00C135—C134—H134120.00
C11—C12—H12120.00C133—C134—H134119.00
C111—C112—C113118.6 (7)C233—C234—C235120.5 (8)
C12—C13—H13120.00C234—C235—C236120.9 (9)
C112—C113—C114119.8 (7)C134—C135—H135120.00
C14—C13—H13121.00C136—C135—H135120.00
C13—C14—H14120.00C231—C236—C235118.2 (6)
C15—C14—H14120.00C131—C136—H136120.00
C113—C114—C115120.7 (10)C135—C136—H136120.00
C114—C115—C116119.9 (11)C211—C212—H212119.00
C14—C15—H15118.00C213—C212—H212120.00
N1—C15—H15119.00C212—C213—H213120.00
C111—C116—C115123.2 (7)C214—C213—H213120.00
P1—C121—C122121.9 (4)C213—C214—H214120.00
N2—C21—H21117.00C215—C214—H214120.00
C22—C21—H21119.00C214—C215—H215121.00
P1—C121—C126119.6 (4)C216—C215—H215118.00
C122—C121—C126118.6 (4)C211—C216—H216120.00
C121—C122—C123120.1 (6)C215—C216—H216120.00
C21—C22—H22120.00C221—C222—H222119.00
C23—C22—H22122.00C223—C222—H222120.00
C22—C23—H23121.00C222—C223—H223121.00
C122—C123—C124120.4 (6)C224—C223—H223119.00
C24—C23—H23120.00C223—C224—H224120.00
C123—C124—C125121.3 (5)C225—C224—H224120.00
C23—C24—H24120.00C224—C225—H225119.00
C25—C24—H24121.00C226—C225—H225122.00
C124—C125—C126118.7 (6)C221—C226—H226119.00
C24—C25—H25119.00C225—C226—H226120.00
N2—C25—H25118.00C231—C232—H232119.00
C121—C126—C125121.0 (5)C233—C232—H232118.00
P1—C131—C132121.3 (3)C232—C233—H233121.00
P1—C131—C136119.7 (4)C234—C233—H233121.00
C132—C131—C136118.1 (4)C233—C234—H234119.00
C131—C132—C133120.5 (5)C235—C234—H234120.00
C132—C133—C134120.0 (6)C234—C235—H235120.00
C133—C134—C135120.8 (6)C236—C235—H235119.00
C134—C135—C136119.8 (6)C231—C236—H236121.00
C131—C136—C135120.8 (5)C235—C236—H236121.00
P2—C211—C212119.4 (4)F1—B1—F2106.0 (9)
P2—C211—C216122.8 (4)F1—B1—F3116.6 (8)
C212—C211—C216117.8 (5)F1—B1—F4115.8 (8)
C211—C212—C213120.9 (5)F2—B1—F3107.9 (10)
C111—C112—H112120.00F2—B1—F4106.9 (7)
C113—C112—H112122.00F3—B1—F4103.2 (9)
P2—Cu1—P1—C11176.07 (19)C231—P2—C211—C21619.4 (5)
P2—Cu1—P1—C121−163.25 (17)Cu1—P2—C221—C222122.9 (4)
P2—Cu1—P1—C131−43.36 (16)Cu1—P2—C221—C226−54.7 (4)
N1—Cu1—P1—C111−50.6 (2)C211—P2—C221—C222−5.4 (5)
N1—Cu1—P1—C12170.1 (2)C211—P2—C221—C226176.9 (4)
N1—Cu1—P1—C131−170.05 (19)C231—P2—C221—C222−112.0 (5)
N2—Cu1—P1—C111−165.0 (2)C231—P2—C221—C22670.3 (4)
N2—Cu1—P1—C121−44.3 (2)Cu1—P2—C231—C232−37.2 (5)
N2—Cu1—P1—C13175.6 (2)Cu1—P2—C231—C236145.9 (4)
P1—Cu1—P2—C211−33.12 (18)C211—P2—C231—C23293.0 (5)
P1—Cu1—P2—C221−152.24 (16)C211—P2—C231—C236−83.9 (5)
P1—Cu1—P2—C23189.0 (2)C221—P2—C231—C232−161.2 (5)
N1—Cu1—P2—C21195.4 (2)C221—P2—C231—C23621.9 (5)
N1—Cu1—P2—C221−23.8 (2)Cu1—N1—C11—C12178.1 (5)
N1—Cu1—P2—C231−142.5 (2)C15—N1—C11—C12−1.4 (8)
N2—Cu1—P2—C211−157.3 (2)Cu1—N1—C15—C14−178.1 (5)
N2—Cu1—P2—C22183.6 (2)C11—N1—C15—C141.4 (8)
N2—Cu1—P2—C231−35.2 (2)Cu1—N2—C21—C22−161.4 (5)
P1—Cu1—N1—C11−76.4 (4)C25—N2—C21—C224.0 (8)
P1—Cu1—N1—C15103.0 (4)Cu1—N2—C25—C24162.2 (5)
P2—Cu1—N1—C11153.2 (4)C21—N2—C25—C24−2.8 (8)
P2—Cu1—N1—C15−27.3 (4)N1—C11—C12—C131.2 (10)
N2—Cu1—N1—C1144.8 (4)C11—C12—C13—C14−1.0 (11)
N2—Cu1—N1—C15−135.8 (4)C12—C13—C14—C151.0 (11)
P1—Cu1—N2—C21−42.9 (4)C13—C14—C15—N1−1.2 (10)
P1—Cu1—N2—C25152.8 (4)N2—C21—C22—C23−1.8 (9)
P2—Cu1—N2—C2183.2 (4)C21—C22—C23—C24−1.8 (10)
P2—Cu1—N2—C25−81.1 (4)C22—C23—C24—C252.9 (10)
N1—Cu1—N2—C21−163.9 (4)C23—C24—C25—N2−0.6 (9)
N1—Cu1—N2—C2531.8 (4)P2—C211—C212—C213−178.0 (5)
Cu1—P1—C111—C11246.7 (5)C216—C211—C212—C2131.6 (8)
Cu1—P1—C111—C116−133.5 (5)P2—C211—C216—C215177.8 (4)
C121—P1—C111—C112−82.3 (5)C212—C211—C216—C215−1.9 (8)
C121—P1—C111—C11697.5 (5)C211—C212—C213—C2140.0 (9)
C131—P1—C111—C112169.7 (4)C212—C213—C214—C215−1.6 (10)
C131—P1—C111—C116−10.5 (6)C213—C214—C215—C2161.4 (10)
Cu1—P1—C121—C122−175.1 (3)C214—C215—C216—C2110.4 (9)
Cu1—P1—C121—C1265.4 (4)P2—C221—C222—C223−178.4 (5)
C111—P1—C121—C122−47.8 (4)C226—C221—C222—C223−0.8 (8)
C111—P1—C121—C126132.7 (4)P2—C221—C226—C225177.6 (5)
C131—P1—C121—C12261.1 (4)C222—C221—C226—C225−0.2 (8)
C131—P1—C121—C126−118.4 (4)C221—C222—C223—C224−0.2 (10)
Cu1—P1—C131—C132−100.7 (4)C222—C223—C224—C2252.0 (11)
Cu1—P1—C131—C13668.7 (4)C223—C224—C225—C226−2.9 (11)
C111—P1—C131—C132133.9 (4)C224—C225—C226—C2212.0 (10)
C111—P1—C131—C136−56.7 (5)P2—C231—C232—C233179.5 (6)
C121—P1—C131—C13227.3 (5)C236—C231—C232—C233−3.4 (10)
C121—P1—C131—C136−163.4 (4)P2—C231—C236—C235178.6 (6)
Cu1—P2—C211—C212−33.0 (5)C232—C231—C236—C2351.6 (9)
Cu1—P2—C211—C216147.4 (4)C231—C232—C233—C2343.7 (13)
C221—P2—C211—C21291.8 (4)C232—C233—C234—C235−2.2 (15)
C221—P2—C211—C216−87.8 (4)C233—C234—C235—C2360.6 (15)
C231—P2—C211—C212−161.0 (4)C234—C235—C236—C231−0.3 (12)
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1, z; (iii) −x+1, −y+1, −z; (iv) −x+2, −y+1, −z+1; (v) −x+1, −y+1, −z+1; (vi) x−1, y, z; (vii) −x+1, −y, −z+1; (viii) x−1, y−1, z; (ix) −x, −y+1, −z; (x) −x+1, −y, −z; (xi) x, y−1, z; (xii) −x, −y, −z; (xiii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C11—H11···F20.95002.43003.157 (12)133.00
C22—H22···F1iii0.95002.53003.421 (11)156.00
Symmetry code: (iii) −x+1, −y+1, −z.

Experimental details

Crystal data
Chemical formula[Cu(C5H5N)2(C18H15P)2]BF4
Mr833.10
Crystal system, space groupTriclinic, P1
Temperature (K)295
a, b, c (Å)10.890 (5), 13.488 (6), 15.547 (6)
α, β, γ (°)84.97 (3), 109.59 (3), 101.93 (3)
V (Å3)2104.5 (16)
Z2
Radiation typeMo Kα
µ (mm−1)0.65
Crystal size (mm)0.50 × 0.30 × 0.15
Data collection
DiffractometerRigaku AFC-7R
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.738, 0.909
No. of measured, independent and
observed [I > 2σ(I)] reflections		8222, 7393, 4745
Rint0.035
(sin θ/λ)max (Å−1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.057, 0.180, 1.03
No. of reflections7393
No. of parameters505
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.86, −0.63

Computer programs: MSC/AFC7 Diffractometer Control for Windows (Molecular Structure Corporation, 1999), MSC/AFC7 Diffractometer Control for Windows (Molecular Structure Corporation, 1999), TEXSAN for Windows (Molecular Structure Corporation, 2001) and SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997), TEXSAN for Windows (Molecular Structure Corporation, 2001) and PLATON (Spek, 2003).

Selected geometric parameters (Å, º) top
Cu1—P12.2712 (17)Cu1—N12.091 (4)
Cu1—P22.2955 (16)Cu1—N22.113 (5)
P1—Cu1—P2116.02 (6)P2—Cu1—N1109.04 (12)
P1—Cu1—N1112.68 (12)P2—Cu1—N2103.22 (12)
P1—Cu1—N2113.03 (13)N1—Cu1—N2101.51 (17)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C11—H11···F20.95002.43003.157 (12)133.00
C22—H22···F1i0.95002.53003.421 (11)156.00
Symmetry code: (i) −x+1, −y+1, −z.
 

Acknowledgements

Financial support of this work by the Eskitis Institute for Cell and Molecular Therapies, Griffith University is acknowledged.

References

First citationEngelhardt, L. M., Pakawatchai, C., White, A. H. & Healy, P. C. (1985). J. Chem. Soc. Dalton Trans. pp. 125–133.  CSD CrossRef Web of Science Google Scholar
 First citationFarrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  CrossRef IUCr Journals Google Scholar
 First citationHanna, J. V., Boyd, S. E., Healy, P. C., Bowmaker, G. A., Skelton, B. W. & White, A. H. (2005). Dalton Trans. pp. 2547–2556.  Web of Science CSD CrossRef Google Scholar
 First citationHanna, J. V., Hart, R. D., Healy, P. C., Skelton, B. W. & White, A. H. (1998). J. Chem. Soc. Dalton Trans. pp. 2321–2325.  Web of Science CSD CrossRef Google Scholar
 First citationMolecular Structure Corporation (1999). MSC/AFC7 Diffractometer Control for Windows. MSC, The Woodlands, Texas, USA.  Google Scholar
 First citationMolecular Structure Corporation. (2001). TEXSAN for Windows. MSC, The Woodlands, Texas, USA.  Google Scholar
 First citationNorth, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351–359.  CrossRef IUCr Journals Web of Science Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationSpek, A. L. (2003). J. Appl. Cryst. 36, 7–13.  Web of Science CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 64| Part 5| May 2008| Page m607
doi:10.1107/S1600536808008386
Follow Acta Cryst. E
Sign up for e-alerts
E-alerts
Follow Acta Cryst. on Twitter
Twitter
Follow us on facebook
Facebook
Sign up for RSS feeds
RSS