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

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ISSN: 2056-9890

(Tri­phenyl­phosphine-κP)[1,1,1-tris­­(di­phenyl­phosphinometh­yl)ethane-κ3P,P′,P′′]copper(I) tetra­fluoridoborate

aCollege of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming 650092, People's Republic of China
*Correspondence e-mail: quanli99@126.com

(Received 2 February 2010; accepted 26 February 2010; online 6 March 2010)

In the title mononuclear CuI complex, [Cu(C18H15P)(C41H39P3)]BF4, the cation has a basic rigid core structure reminiscent of the framework of diamond. The metal atom is coordinated by four P atoms in a distorted tetra­hedral geometry, the distortion arising from the steric hindrance of the phenyl groups. The anion is disordered over two positions, with an occupancy ratio of 0.524 (17):0.476 (17). The cations and anions are closely packed in the crystal and are in h.c.p. arrangements.

Related literature

For the synthesis of related complexes, see: Pawlowski et al. (2005[Pawlowski, V., Knor, G., Lennartz, C. & Vogler, A. (2005). Eur. J. Inorg. Chem. pp. 3167-3171.]). For the structures of related complexes, see: Kourkine et al. (1996[Kourkine, I. V., Maslennikov, S. V., Ditchfield, R., Glueck, D. S., Yap, G. P. A., Liable-Sands, L. M. & Rheingold, A. L. (1996). Inorg. Chem. 35, 6708-6716.]); Mautz et al. (2008[Mautz, J., Heinze, K., Wadepohl, H. & Huttner, G. (2008). Eur. J. Inorg. Chem. pp. 1413-1422.]).

[Scheme 1]

Experimental

Crystal data
  • [Cu(C18H15P)(C41H39P3)]BF4

  • Mr = 1037.25

  • Monoclinic, P 21 /c

  • a = 13.470 (4) Å

  • b = 14.356 (4) Å

  • c = 26.240 (7) Å

  • β = 91.338 (5)°

  • V = 5073 (2) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 0.61 mm−1

  • T = 293 K

  • 0.20 × 0.16 × 0.14 mm

Data collection
  • Bruker SMART diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.696, Tmax = 1.000

  • 29232 measured reflections

  • 10469 independent reflections

  • 5826 reflections with I > 2σ(I)

  • Rint = 0.072

Refinement
  • R[F2 > 2σ(F2)] = 0.057

  • wR(F2) = 0.138

  • S = 0.98

  • 10469 reflections

  • 660 parameters

  • H-atom parameters constrained

  • Δρmax = 0.49 e Å−3

  • Δρmin = −0.31 e Å−3

Table 1
Selected geometric parameters (Å, °)

Cu1—P4 2.2852 (11)
Cu1—P3 2.2983 (12)
Cu1—P2 2.3177 (12)
Cu1—P1 2.3314 (12)
P4—Cu1—P3 122.79 (4)
P4—Cu1—P2 124.27 (4)
P3—Cu1—P2 91.17 (4)
P4—Cu1—P1 117.67 (4)
P3—Cu1—P1 96.58 (4)
P2—Cu1—P1 97.65 (4)

Data collection: SMART (Siemens, 1996[Siemens (1996). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Siemens, 1996[Siemens (1996). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Ctyst. A63, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Ctyst. A63, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Ctyst. A63, 112-122.]).

Supporting information


Comment top

As seen in Figure 1, the copper center of the title compound can be described as having a distorted tetrahedron geometry with four of Cu—P bond lengths [2.2852 (11), 2.2983 (12), 2.3177 (12) and 2.3314 (12) Å] and P—Cu—P angles in the range 91.17 (4) to 124.27 (4)°. The average Cu—P distance is thus 2.3082 Å, slightly longer than the corresponding value, 2.2833 Å, reported for a similar compound (Kourkine et al., 1996). The P—Cu—P angles are out of the range 104.0 (1)–116.5 (1)° observed in the same complex.

Tris(diphenylphosphinomethyl)ethane and the CuI ion compose a bicyclo[2,2,2]octa core with a rigid structure similar to the basic structure of diamond. Interestingly, these rigid cations and disordered anions are connected by C—H···F weak hydrogen bonds, as shown in Figure 2, characterized by a C···F separation of 3.229 (12) Å.

Some other related complexes have been synthesized with CuI (Pawlowski et al., 2005), and Ni (Mautz et al., 2008).

Related literature top

For the synthesis of related complexes, see: Pawlowski et al. (2005). For the structures of related complexes, see: Kourkine et al. (1996); Mautz et al. (2008).

Experimental top

A mixture of [Cu(CH3CN)4]BF4 (0.1258 g, 0.40 mmol) and 1,1,1-tris(diphenylphosphinomethyl)ethane (triphos, 0.25 g, 0.40 mmol) in dichloromethane (20 mL) was stirred for 3 hours at room temperature under nitrogen atmosphere, and triphenylphosphine (0.1048 g, 0.4 mmol) was then added to the solution. The resulting colorless solution was further stirred for 2 hours and then filtered. The reaction mixture was concentrated in vacuum and the crude product was recrystallized from CH2Cl2/diethyl ether, to give white crystals (Yield: 82%).

Refinement top

All H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C) for aromatic CH, C—H = 0.96 Å and Uiso(H) = 1.5Ueq(C) for the methyl group, and C—H = 0.97 Å and Uiso(H) = 1.2Ueq(C) for the methylene groups. The F atoms in the aion are disordered over two positions, and occupancies were refined with the sum of two disordered sites constrained to unity. The occupation factors converged to 0.476 (17) and 0.524 (17).

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); 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).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound. For clarity, all phenyl groups and H atoms are omitted. A single position for the anion is represented.
[Figure 2] Fig. 2. Interactions between cations and anions in the crystal structure of the title compound.
(Triphenylphosphine-κP)[1,1,1-tris(diphenylphosphinomethyl)ethane- κ3P,P',P'']copper(I) tetrafluoridoborate top
Crystal data top
[Cu(C18H15P)(C41H39P3)]BF4F(000) = 2152
Mr = 1037.25Dx = 1.358 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 904 reflections
a = 13.470 (4) Åθ = 2.8–23.1°
b = 14.356 (4) ŵ = 0.61 mm1
c = 26.240 (7) ÅT = 293 K
β = 91.338 (5)°Block, white
V = 5073 (2) Å30.20 × 0.16 × 0.14 mm
Z = 4
Data collection top
Bruker SMART
diffractometer
10469 independent reflections
Radiation source: fine-focus sealed tube5826 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.072
ϕ and ω scansθmax = 26.5°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 916
Tmin = 0.696, Tmax = 1.000k = 1718
29232 measured reflectionsl = 2932
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) = 0.138H-atom parameters constrained
S = 0.98 w = 1/[σ2(Fo2) + (0.0633P)2]
where P = (Fo2 + 2Fc2)/3
10469 reflections(Δ/σ)max < 0.001
660 parametersΔρmax = 0.49 e Å3
0 restraintsΔρmin = 0.31 e Å3
0 constraints
Crystal data top
[Cu(C18H15P)(C41H39P3)]BF4V = 5073 (2) Å3
Mr = 1037.25Z = 4
Monoclinic, P21/cMo Kα radiation
a = 13.470 (4) ŵ = 0.61 mm1
b = 14.356 (4) ÅT = 293 K
c = 26.240 (7) Å0.20 × 0.16 × 0.14 mm
β = 91.338 (5)°
Data collection top
Bruker SMART
diffractometer
10469 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5826 reflections with I > 2σ(I)
Tmin = 0.696, Tmax = 1.000Rint = 0.072
29232 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0570 restraints
wR(F2) = 0.138H-atom parameters constrained
S = 0.98Δρmax = 0.49 e Å3
10469 reflectionsΔρmin = 0.31 e Å3
660 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cu10.24249 (3)0.75782 (3)0.396487 (17)0.03077 (13)
P10.41107 (7)0.73412 (7)0.41402 (4)0.0339 (2)
P20.25203 (7)0.77281 (7)0.30879 (4)0.0335 (2)
P30.24433 (7)0.91686 (6)0.40649 (4)0.0324 (2)
P40.13205 (7)0.66350 (7)0.43651 (4)0.0338 (2)
C10.4799 (3)0.6276 (3)0.39782 (16)0.0401 (10)
C20.4919 (4)0.6035 (3)0.34792 (18)0.0666 (14)
H20.46600.64190.32230.080*
C30.5416 (4)0.5238 (4)0.3349 (2)0.0859 (18)
H30.54930.50880.30070.103*
C40.5797 (4)0.4666 (4)0.3719 (2)0.0820 (17)
H40.61250.41200.36310.098*
C50.5693 (4)0.4898 (3)0.4216 (2)0.0736 (15)
H50.59600.45130.44690.088*
C60.5202 (3)0.5692 (3)0.43494 (18)0.0558 (12)
H60.51390.58410.46920.067*
C70.4547 (3)0.7550 (2)0.47942 (15)0.0388 (9)
C80.5539 (3)0.7766 (3)0.49112 (18)0.0499 (11)
H80.59990.77930.46530.060*
C90.5836 (4)0.7940 (3)0.5406 (2)0.0663 (15)
H90.64920.81050.54770.080*
C100.5184 (4)0.7875 (3)0.5799 (2)0.0691 (15)
H100.53990.79770.61340.083*
C110.4214 (4)0.7657 (3)0.56900 (18)0.0618 (13)
H110.37620.76210.59520.074*
C120.3901 (3)0.7490 (3)0.51913 (16)0.0464 (10)
H120.32410.73340.51240.056*
C130.4777 (3)0.8240 (3)0.37731 (16)0.0436 (10)
H13A0.51450.86230.40170.052*
H13B0.52630.79200.35690.052*
C140.4194 (2)0.8901 (2)0.34159 (14)0.0325 (9)
C150.4987 (3)0.9517 (3)0.31621 (16)0.0482 (11)
H15A0.46640.99740.29490.072*
H15B0.54070.91340.29590.072*
H15C0.53810.98240.34210.072*
C160.3684 (3)0.8362 (3)0.29736 (15)0.0440 (10)
H16A0.41600.79160.28480.053*
H16B0.35510.88030.27000.053*
C170.2630 (3)0.6659 (3)0.27227 (15)0.0376 (9)
C180.2852 (3)0.6658 (3)0.22080 (16)0.0487 (11)
H180.29760.72170.20420.058*
C190.2888 (3)0.5840 (4)0.19470 (18)0.0608 (13)
H190.30240.58470.16010.073*
C200.2729 (3)0.5008 (3)0.2185 (2)0.0582 (13)
H200.27510.44550.20010.070*
C210.2537 (3)0.4988 (3)0.2695 (2)0.0587 (13)
H210.24430.44230.28600.070*
C220.2483 (3)0.5820 (3)0.29635 (17)0.0496 (11)
H220.23470.58100.33090.060*
C230.1601 (3)0.8362 (3)0.26973 (14)0.0379 (9)
C240.0716 (3)0.7921 (3)0.25629 (15)0.0472 (11)
H240.06240.72980.26480.057*
C250.0038 (3)0.8402 (4)0.23009 (17)0.0635 (14)
H250.06390.81120.22220.076*
C260.0124 (4)0.9319 (4)0.21603 (18)0.0716 (16)
H260.03730.96430.19830.086*
C270.0991 (4)0.9750 (4)0.22772 (19)0.0705 (15)
H270.10931.03620.21740.085*
C280.1733 (3)0.9280 (3)0.25509 (16)0.0513 (11)
H280.23220.95850.26360.062*
C290.3536 (3)0.9585 (3)0.37104 (15)0.0409 (10)
H29A0.32961.00480.34680.049*
H29B0.39660.99090.39530.049*
C300.1404 (3)0.9788 (3)0.37651 (14)0.0362 (9)
C310.1473 (3)1.0711 (3)0.36160 (17)0.0522 (11)
H310.20631.10360.36720.063*
C320.0671 (4)1.1148 (3)0.33846 (19)0.0656 (14)
H320.07251.17650.32800.079*
C330.0198 (4)1.0681 (4)0.33079 (18)0.0623 (13)
H330.07341.09810.31490.075*
C340.0292 (3)0.9778 (3)0.34612 (16)0.0515 (11)
H340.08920.94660.34110.062*
C350.0507 (3)0.9329 (3)0.36909 (15)0.0424 (10)
H350.04430.87140.37970.051*
C360.2550 (3)0.9773 (2)0.46789 (15)0.0389 (9)
C370.1756 (3)1.0240 (3)0.48823 (17)0.0597 (13)
H370.11671.02970.46930.072*
C380.1828 (4)1.0628 (4)0.5367 (2)0.0768 (16)
H380.12911.09500.54970.092*
C390.2678 (5)1.0540 (4)0.56521 (19)0.0737 (16)
H390.27221.08000.59760.088*
C400.3463 (4)1.0072 (3)0.54629 (19)0.0656 (14)
H400.40421.00050.56590.079*
C410.3402 (3)0.9696 (3)0.49786 (17)0.0512 (11)
H410.39480.93830.48520.061*
C420.1589 (3)0.5405 (2)0.42803 (14)0.0347 (9)
C430.2571 (3)0.5113 (3)0.43182 (19)0.0577 (13)
H430.30610.55390.44140.069*
C440.2832 (4)0.4211 (3)0.4217 (2)0.0725 (16)
H440.34930.40280.42450.087*
C450.2116 (4)0.3578 (3)0.40737 (19)0.0639 (13)
H450.22910.29680.39970.077*
C460.1148 (4)0.3845 (3)0.40442 (18)0.0575 (12)
H460.06620.34100.39570.069*
C470.0879 (3)0.4755 (3)0.41422 (16)0.0455 (10)
H470.02150.49290.41150.055*
C480.1349 (3)0.6788 (3)0.50546 (15)0.0387 (10)
C490.1545 (3)0.6084 (3)0.53999 (16)0.0501 (11)
H490.16450.54790.52850.060*
C500.1593 (3)0.6276 (4)0.59191 (18)0.0688 (15)
H500.17180.57950.61490.083*
C510.1462 (4)0.7142 (5)0.6093 (2)0.0836 (19)
H510.14990.72580.64420.100*
C520.1273 (4)0.7863 (4)0.5757 (2)0.0791 (17)
H520.11810.84650.58780.095*
C530.1219 (3)0.7687 (3)0.52404 (18)0.0581 (12)
H530.10960.81740.50140.070*
C540.0001 (3)0.6724 (3)0.41974 (16)0.0397 (10)
C550.0735 (3)0.6595 (3)0.45486 (18)0.0572 (12)
H550.05650.64850.48890.069*
C560.1728 (4)0.6631 (4)0.4393 (2)0.0783 (16)
H560.22200.65320.46300.094*
C570.1987 (4)0.6811 (3)0.3895 (3)0.0739 (16)
H570.26530.68360.37950.089*
C580.1262 (4)0.6953 (3)0.3544 (2)0.0700 (14)
H580.14320.70810.32060.084*
C590.0277 (3)0.6904 (3)0.36998 (18)0.0561 (12)
H590.02140.69950.34610.067*
B10.3312 (7)0.2119 (6)0.2671 (3)0.080 (2)
F10.299 (2)0.128 (2)0.2471 (10)0.143 (9)0.476 (17)
F20.3933 (14)0.2505 (10)0.2382 (7)0.152 (7)0.476 (17)
F30.2403 (7)0.2555 (7)0.2643 (6)0.120 (5)0.476 (17)
F40.3505 (12)0.1988 (13)0.3157 (5)0.160 (8)0.476 (17)
F1'0.326 (2)0.1207 (16)0.2673 (9)0.135 (9)0.524 (17)
F2'0.4334 (11)0.2230 (11)0.2776 (7)0.196 (7)0.524 (17)
F3'0.3244 (12)0.2558 (9)0.2234 (5)0.140 (6)0.524 (17)
F4'0.2890 (13)0.2538 (8)0.3048 (6)0.164 (8)0.524 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0327 (3)0.0303 (3)0.0293 (2)0.00246 (19)0.00001 (17)0.0021 (2)
P10.0303 (5)0.0334 (5)0.0378 (6)0.0010 (4)0.0031 (4)0.0056 (4)
P20.0333 (6)0.0401 (6)0.0271 (5)0.0041 (4)0.0015 (4)0.0001 (4)
P30.0351 (6)0.0281 (5)0.0342 (6)0.0019 (4)0.0021 (4)0.0008 (4)
P40.0363 (6)0.0314 (5)0.0339 (6)0.0049 (4)0.0025 (4)0.0015 (4)
C10.030 (2)0.041 (2)0.049 (3)0.0023 (17)0.0009 (18)0.000 (2)
C20.085 (4)0.065 (3)0.050 (3)0.033 (3)0.009 (3)0.002 (3)
C30.114 (5)0.087 (4)0.057 (4)0.046 (4)0.001 (3)0.015 (3)
C40.099 (4)0.065 (4)0.083 (5)0.043 (3)0.015 (3)0.003 (3)
C50.088 (4)0.059 (3)0.074 (4)0.032 (3)0.005 (3)0.021 (3)
C60.068 (3)0.044 (3)0.055 (3)0.010 (2)0.005 (2)0.008 (2)
C70.042 (2)0.030 (2)0.044 (2)0.0005 (18)0.0092 (18)0.0071 (18)
C80.043 (3)0.050 (3)0.056 (3)0.004 (2)0.010 (2)0.009 (2)
C90.071 (4)0.051 (3)0.075 (4)0.009 (2)0.041 (3)0.011 (3)
C100.106 (5)0.051 (3)0.049 (3)0.004 (3)0.029 (3)0.000 (2)
C110.085 (4)0.056 (3)0.044 (3)0.003 (3)0.000 (3)0.001 (2)
C120.051 (3)0.040 (2)0.049 (3)0.0064 (19)0.002 (2)0.004 (2)
C130.035 (2)0.050 (3)0.046 (3)0.0034 (18)0.0001 (18)0.012 (2)
C140.027 (2)0.035 (2)0.035 (2)0.0089 (16)0.0017 (16)0.0066 (17)
C150.039 (2)0.059 (3)0.047 (3)0.015 (2)0.0043 (19)0.011 (2)
C160.037 (2)0.061 (3)0.035 (2)0.011 (2)0.0022 (17)0.005 (2)
C170.031 (2)0.045 (2)0.037 (2)0.0004 (17)0.0005 (17)0.0076 (19)
C180.058 (3)0.050 (3)0.038 (3)0.013 (2)0.004 (2)0.003 (2)
C190.061 (3)0.079 (4)0.041 (3)0.023 (3)0.001 (2)0.013 (3)
C200.040 (3)0.062 (3)0.072 (4)0.013 (2)0.002 (2)0.028 (3)
C210.057 (3)0.043 (3)0.077 (4)0.007 (2)0.007 (3)0.003 (3)
C220.058 (3)0.049 (3)0.042 (3)0.004 (2)0.007 (2)0.002 (2)
C230.041 (2)0.049 (2)0.024 (2)0.0014 (19)0.0006 (16)0.0043 (18)
C240.046 (3)0.058 (3)0.037 (3)0.008 (2)0.000 (2)0.014 (2)
C250.050 (3)0.092 (4)0.048 (3)0.018 (3)0.014 (2)0.027 (3)
C260.082 (4)0.087 (4)0.044 (3)0.043 (3)0.013 (3)0.004 (3)
C270.091 (4)0.071 (4)0.050 (3)0.024 (3)0.006 (3)0.010 (3)
C280.062 (3)0.052 (3)0.041 (3)0.006 (2)0.001 (2)0.005 (2)
C290.041 (2)0.037 (2)0.045 (3)0.0085 (18)0.0060 (18)0.0058 (19)
C300.041 (2)0.034 (2)0.034 (2)0.0019 (18)0.0012 (17)0.0016 (17)
C310.054 (3)0.039 (2)0.064 (3)0.004 (2)0.004 (2)0.001 (2)
C320.077 (4)0.042 (3)0.078 (4)0.020 (3)0.003 (3)0.010 (2)
C330.056 (3)0.071 (4)0.060 (3)0.027 (3)0.002 (2)0.001 (3)
C340.037 (3)0.070 (3)0.048 (3)0.009 (2)0.003 (2)0.004 (2)
C350.046 (3)0.041 (2)0.041 (3)0.0019 (19)0.0066 (19)0.0001 (19)
C360.049 (3)0.028 (2)0.039 (2)0.0092 (18)0.0011 (19)0.0021 (17)
C370.060 (3)0.075 (3)0.044 (3)0.000 (2)0.008 (2)0.010 (2)
C380.085 (4)0.092 (4)0.054 (4)0.001 (3)0.020 (3)0.018 (3)
C390.120 (5)0.061 (3)0.041 (3)0.024 (3)0.001 (3)0.009 (3)
C400.090 (4)0.047 (3)0.058 (3)0.013 (3)0.027 (3)0.001 (2)
C410.062 (3)0.035 (2)0.056 (3)0.007 (2)0.009 (2)0.003 (2)
C420.037 (2)0.037 (2)0.031 (2)0.0050 (17)0.0021 (16)0.0057 (17)
C430.045 (3)0.039 (3)0.090 (4)0.004 (2)0.004 (2)0.011 (2)
C440.050 (3)0.053 (3)0.115 (5)0.011 (2)0.007 (3)0.012 (3)
C450.081 (4)0.040 (3)0.071 (4)0.012 (3)0.003 (3)0.002 (2)
C460.067 (3)0.038 (3)0.067 (3)0.004 (2)0.013 (2)0.008 (2)
C470.042 (3)0.040 (2)0.054 (3)0.0003 (19)0.004 (2)0.001 (2)
C480.034 (2)0.045 (2)0.038 (2)0.0110 (18)0.0053 (17)0.0031 (19)
C490.047 (3)0.065 (3)0.039 (3)0.012 (2)0.0017 (19)0.008 (2)
C500.055 (3)0.116 (5)0.035 (3)0.018 (3)0.005 (2)0.013 (3)
C510.069 (4)0.141 (6)0.041 (3)0.041 (4)0.007 (3)0.024 (4)
C520.086 (4)0.090 (4)0.063 (4)0.024 (3)0.025 (3)0.037 (3)
C530.070 (3)0.052 (3)0.053 (3)0.011 (2)0.014 (2)0.004 (2)
C540.039 (2)0.034 (2)0.046 (3)0.0029 (17)0.0001 (19)0.0031 (19)
C550.044 (3)0.070 (3)0.057 (3)0.006 (2)0.007 (2)0.006 (2)
C560.042 (3)0.094 (4)0.099 (5)0.004 (3)0.012 (3)0.008 (4)
C570.044 (3)0.070 (4)0.107 (5)0.009 (2)0.019 (3)0.004 (3)
C580.063 (4)0.079 (4)0.067 (4)0.001 (3)0.028 (3)0.000 (3)
C590.052 (3)0.067 (3)0.049 (3)0.009 (2)0.005 (2)0.001 (2)
B10.099 (7)0.076 (5)0.066 (5)0.006 (5)0.007 (5)0.004 (4)
F10.178 (14)0.120 (17)0.131 (17)0.055 (12)0.007 (11)0.015 (12)
F20.137 (14)0.164 (11)0.157 (19)0.049 (12)0.063 (12)0.030 (12)
F30.092 (7)0.122 (7)0.146 (13)0.041 (5)0.023 (7)0.006 (7)
F40.152 (13)0.211 (17)0.114 (11)0.023 (10)0.060 (9)0.032 (10)
F1'0.192 (19)0.076 (9)0.141 (19)0.017 (11)0.048 (14)0.028 (11)
F2'0.151 (12)0.254 (15)0.182 (15)0.042 (9)0.029 (11)0.041 (12)
F3'0.164 (15)0.127 (7)0.127 (9)0.027 (9)0.035 (11)0.040 (6)
F4'0.208 (18)0.145 (10)0.141 (14)0.025 (9)0.063 (14)0.041 (10)
Geometric parameters (Å, º) top
Cu1—P42.2852 (11)C27—C281.391 (6)
Cu1—P32.2983 (12)C27—H270.9300
Cu1—P22.3177 (12)C28—H280.9300
Cu1—P12.3314 (12)C29—H29A0.9700
P1—C71.826 (4)C29—H29B0.9700
P1—C11.843 (4)C30—C311.386 (5)
P1—C131.855 (4)C30—C351.386 (5)
P2—C171.818 (4)C31—C321.378 (6)
P2—C231.831 (4)C31—H310.9300
P2—C161.843 (4)C32—C331.360 (6)
P3—C301.821 (4)C32—H320.9300
P3—C361.833 (4)C33—C341.364 (6)
P3—C291.859 (3)C33—H330.9300
P4—C421.817 (4)C34—C351.381 (5)
P4—C481.822 (4)C34—H340.9300
P4—C541.828 (4)C35—H350.9300
C1—C21.367 (6)C36—C411.380 (5)
C1—C61.387 (6)C36—C371.381 (5)
C2—C31.374 (6)C37—C381.389 (6)
C2—H20.9300C37—H370.9300
C3—C41.363 (7)C38—C391.359 (7)
C3—H30.9300C38—H380.9300
C4—C51.356 (7)C39—C401.356 (7)
C4—H40.9300C39—H390.9300
C5—C61.367 (6)C40—C411.382 (6)
C5—H50.9300C40—H400.9300
C6—H60.9300C41—H410.9300
C7—C121.376 (5)C42—C471.379 (5)
C7—C81.399 (5)C42—C431.388 (5)
C8—C91.373 (6)C43—C441.371 (6)
C8—H80.9300C43—H430.9300
C9—C101.372 (7)C44—C451.371 (6)
C9—H90.9300C44—H440.9300
C10—C111.368 (7)C45—C461.358 (6)
C10—H100.9300C45—H450.9300
C11—C121.386 (6)C46—C471.381 (5)
C11—H110.9300C46—H460.9300
C12—H120.9300C47—H470.9300
C13—C141.537 (5)C48—C491.378 (5)
C13—H13A0.9700C48—C531.393 (5)
C13—H13B0.9700C49—C501.390 (6)
C14—C291.542 (5)C49—H490.9300
C14—C161.543 (5)C50—C511.337 (7)
C14—C151.549 (5)C50—H500.9300
C15—H15A0.9600C51—C521.380 (8)
C15—H15B0.9600C51—H510.9300
C15—H15C0.9600C52—C531.378 (7)
C16—H16A0.9700C52—H520.9300
C16—H16B0.9700C53—H530.9300
C17—C221.376 (5)C54—C591.373 (6)
C17—C181.390 (5)C54—C551.380 (5)
C18—C191.362 (6)C55—C561.390 (6)
C18—H180.9300C55—H550.9300
C19—C201.368 (6)C56—C571.370 (7)
C19—H190.9300C56—H560.9300
C20—C211.367 (6)C57—C581.374 (7)
C20—H200.9300C57—H570.9300
C21—C221.390 (6)C58—C591.381 (6)
C21—H210.9300C58—H580.9300
C22—H220.9300C59—H590.9300
C23—C281.385 (5)B1—F11.38 (3)
C23—C241.389 (5)B1—F21.271 (14)
C24—C251.396 (6)B1—F31.375 (12)
C24—H240.9300B1—F41.309 (14)
C25—C261.386 (7)B1—F1'1.31 (2)
C25—H250.9300B1—F2'1.407 (14)
C26—C271.351 (7)B1—F3'1.312 (14)
C26—H260.9300B1—F4'1.299 (12)
P4—Cu1—P3122.79 (4)C27—C26—C25121.0 (5)
P4—Cu1—P2124.27 (4)C27—C26—H26119.5
P3—Cu1—P291.17 (4)C25—C26—H26119.5
P4—Cu1—P1117.67 (4)C26—C27—C28120.1 (5)
P3—Cu1—P196.58 (4)C26—C27—H27119.9
P2—Cu1—P197.65 (4)C28—C27—H27119.9
C7—P1—C1101.56 (18)C23—C28—C27120.6 (5)
C7—P1—C13103.00 (18)C23—C28—H28119.7
C1—P1—C13101.86 (18)C27—C28—H28119.7
C7—P1—Cu1116.88 (13)C14—C29—P3121.1 (2)
C1—P1—Cu1124.63 (13)C14—C29—H29A107.0
C13—P1—Cu1106.09 (12)P3—C29—H29A107.0
C17—P2—C23100.77 (17)C14—C29—H29B107.0
C17—P2—C16104.58 (18)P3—C29—H29B107.0
C23—P2—C16103.28 (18)H29A—C29—H29B106.8
C17—P2—Cu1116.87 (13)C31—C30—C35118.6 (4)
C23—P2—Cu1123.33 (12)C31—C30—P3122.2 (3)
C16—P2—Cu1105.93 (13)C35—C30—P3119.2 (3)
C30—P3—C36101.10 (18)C32—C31—C30120.2 (4)
C30—P3—C29103.67 (18)C32—C31—H31119.9
C36—P3—C29103.94 (18)C30—C31—H31119.9
C30—P3—Cu1115.43 (13)C33—C32—C31120.3 (4)
C36—P3—Cu1124.83 (12)C33—C32—H32119.9
C29—P3—Cu1105.61 (12)C31—C32—H32119.9
C42—P4—C48103.82 (17)C32—C33—C34120.6 (4)
C42—P4—C54103.55 (17)C32—C33—H33119.7
C48—P4—C54103.19 (18)C34—C33—H33119.7
C42—P4—Cu1112.70 (12)C33—C34—C35119.7 (4)
C48—P4—Cu1112.73 (12)C33—C34—H34120.1
C54—P4—Cu1119.24 (13)C35—C34—H34120.1
C2—C1—C6117.8 (4)C34—C35—C30120.5 (4)
C2—C1—P1120.1 (3)C34—C35—H35119.7
C6—C1—P1122.1 (3)C30—C35—H35119.7
C1—C2—C3121.2 (5)C41—C36—C37117.4 (4)
C1—C2—H2119.4C41—C36—P3120.7 (3)
C3—C2—H2119.4C37—C36—P3121.6 (3)
C4—C3—C2120.1 (5)C36—C37—C38120.7 (5)
C4—C3—H3119.9C36—C37—H37119.7
C2—C3—H3119.9C38—C37—H37119.7
C5—C4—C3119.4 (5)C39—C38—C37120.5 (5)
C5—C4—H4120.3C39—C38—H38119.8
C3—C4—H4120.3C37—C38—H38119.8
C4—C5—C6120.9 (5)C40—C39—C38119.9 (5)
C4—C5—H5119.5C40—C39—H39120.1
C6—C5—H5119.5C38—C39—H39120.1
C5—C6—C1120.5 (5)C39—C40—C41120.0 (5)
C5—C6—H6119.7C39—C40—H40120.0
C1—C6—H6119.7C41—C40—H40120.0
C12—C7—C8117.7 (4)C36—C41—C40121.6 (4)
C12—C7—P1120.4 (3)C36—C41—H41119.2
C8—C7—P1121.8 (3)C40—C41—H41119.2
C9—C8—C7120.2 (4)C47—C42—C43117.9 (4)
C9—C8—H8119.9C47—C42—P4123.5 (3)
C7—C8—H8119.9C43—C42—P4118.5 (3)
C10—C9—C8121.4 (5)C44—C43—C42121.3 (4)
C10—C9—H9119.3C44—C43—H43119.3
C8—C9—H9119.3C42—C43—H43119.3
C11—C10—C9118.9 (5)C43—C44—C45119.8 (4)
C11—C10—H10120.5C43—C44—H44120.1
C9—C10—H10120.5C45—C44—H44120.1
C10—C11—C12120.3 (5)C46—C45—C44119.8 (4)
C10—C11—H11119.8C46—C45—H45120.1
C12—C11—H11119.8C44—C45—H45120.1
C7—C12—C11121.4 (4)C45—C46—C47120.8 (4)
C7—C12—H12119.3C45—C46—H46119.6
C11—C12—H12119.3C47—C46—H46119.6
C14—C13—P1120.0 (3)C42—C47—C46120.4 (4)
C14—C13—H13A107.3C42—C47—H47119.8
P1—C13—H13A107.3C46—C47—H47119.8
C14—C13—H13B107.3C49—C48—C53118.2 (4)
P1—C13—H13B107.3C49—C48—P4124.3 (3)
H13A—C13—H13B106.9C53—C48—P4117.3 (3)
C13—C14—C29112.3 (3)C48—C49—C50120.2 (5)
C13—C14—C16111.2 (3)C48—C49—H49119.9
C29—C14—C16116.4 (3)C50—C49—H49119.9
C13—C14—C15105.5 (3)C51—C50—C49121.1 (5)
C29—C14—C15105.2 (3)C51—C50—H50119.5
C16—C14—C15105.2 (3)C49—C50—H50119.5
C14—C15—H15A109.5C50—C51—C52120.1 (5)
C14—C15—H15B109.5C50—C51—H51119.9
H15A—C15—H15B109.5C52—C51—H51119.9
C14—C15—H15C109.5C53—C52—C51119.8 (5)
H15A—C15—H15C109.5C53—C52—H52120.1
H15B—C15—H15C109.5C51—C52—H52120.1
C14—C16—P2119.4 (3)C52—C53—C48120.6 (5)
C14—C16—H16A107.5C52—C53—H53119.7
P2—C16—H16A107.5C48—C53—H53119.7
C14—C16—H16B107.5C59—C54—C55118.6 (4)
P2—C16—H16B107.5C59—C54—P4118.8 (3)
H16A—C16—H16B107.0C55—C54—P4122.6 (3)
C22—C17—C18118.8 (4)C54—C55—C56119.9 (5)
C22—C17—P2118.9 (3)C54—C55—H55120.0
C18—C17—P2122.3 (3)C56—C55—H55120.0
C19—C18—C17120.0 (4)C57—C56—C55120.6 (5)
C19—C18—H18120.0C57—C56—H56119.7
C17—C18—H18120.0C55—C56—H56119.7
C18—C19—C20121.0 (4)C56—C57—C58119.9 (5)
C18—C19—H19119.5C56—C57—H57120.0
C20—C19—H19119.5C58—C57—H57120.0
C21—C20—C19120.0 (4)C57—C58—C59119.2 (5)
C21—C20—H20120.0C57—C58—H58120.4
C19—C20—H20120.0C59—C58—H58120.4
C20—C21—C22119.5 (4)C54—C59—C58121.8 (4)
C20—C21—H21120.3C54—C59—H59119.1
C22—C21—H21120.3C58—C59—H59119.1
C17—C22—C21120.6 (4)F2—B1—F4121.8 (14)
C17—C22—H22119.7F2—B1—F3111.5 (12)
C21—C22—H22119.7F4—B1—F3105.9 (12)
C28—C23—C24118.6 (4)F2—B1—F1110.9 (17)
C28—C23—P2122.6 (3)F4—B1—F1107.4 (13)
C24—C23—P2118.7 (3)F3—B1—F196.3 (15)
C23—C24—C25120.6 (4)F4'—B1—F1'115.8 (14)
C23—C24—H24119.7F4'—B1—F3'114.9 (12)
C25—C24—H24119.7F1'—B1—F3'118.7 (13)
C26—C25—C24119.0 (5)F4'—B1—F2'104.0 (12)
C26—C25—H25120.5F1'—B1—F2'99.5 (15)
C24—C25—H25120.5F3'—B1—F2'99.5 (11)
P4—Cu1—P1—C764.02 (14)C17—P2—C23—C28131.1 (3)
P3—Cu1—P1—C768.51 (13)C16—P2—C23—C2823.2 (4)
P2—Cu1—P1—C7160.59 (13)Cu1—P2—C23—C2896.4 (3)
P4—Cu1—P1—C164.53 (17)C17—P2—C23—C2452.1 (3)
P3—Cu1—P1—C1162.94 (17)C16—P2—C23—C24160.0 (3)
P2—Cu1—P1—C170.87 (17)Cu1—P2—C23—C2480.4 (3)
P4—Cu1—P1—C13178.14 (15)C28—C23—C24—C252.1 (6)
P3—Cu1—P1—C1345.61 (15)P2—C23—C24—C25174.8 (3)
P2—Cu1—P1—C1346.47 (15)C23—C24—C25—C262.3 (6)
P4—Cu1—P2—C1752.27 (14)C24—C25—C26—C270.6 (7)
P3—Cu1—P2—C17175.71 (13)C25—C26—C27—C281.2 (8)
P1—Cu1—P2—C1778.91 (13)C24—C23—C28—C270.3 (6)
P4—Cu1—P2—C2373.46 (16)P2—C23—C28—C27176.5 (3)
P3—Cu1—P2—C2358.56 (16)C26—C27—C28—C231.4 (7)
P1—Cu1—P2—C23155.35 (16)C13—C14—C29—P367.7 (4)
P4—Cu1—P2—C16168.27 (14)C16—C14—C29—P362.1 (4)
P3—Cu1—P2—C1659.71 (15)C15—C14—C29—P3178.1 (3)
P1—Cu1—P2—C1637.08 (15)C30—P3—C29—C14120.1 (3)
P4—Cu1—P3—C3071.03 (14)C36—P3—C29—C14134.6 (3)
P2—Cu1—P3—C3062.05 (14)Cu1—P3—C29—C141.7 (3)
P1—Cu1—P3—C30159.89 (14)C36—P3—C30—C3168.0 (4)
P4—Cu1—P3—C3655.16 (17)C29—P3—C30—C3139.5 (4)
P2—Cu1—P3—C36171.75 (16)Cu1—P3—C30—C31154.5 (3)
P1—Cu1—P3—C3673.91 (16)C36—P3—C30—C35110.8 (3)
P4—Cu1—P3—C29175.10 (14)C29—P3—C30—C35141.7 (3)
P2—Cu1—P3—C2951.81 (14)Cu1—P3—C30—C3526.7 (3)
P1—Cu1—P3—C2946.02 (14)C35—C30—C31—C322.0 (6)
P3—Cu1—P4—C42172.36 (14)P3—C30—C31—C32179.2 (3)
P2—Cu1—P4—C4269.71 (14)C30—C31—C32—C331.0 (7)
P1—Cu1—P4—C4252.92 (14)C31—C32—C33—C340.4 (7)
P3—Cu1—P4—C4855.23 (15)C32—C33—C34—C350.8 (7)
P2—Cu1—P4—C48173.16 (14)C33—C34—C35—C300.2 (6)
P1—Cu1—P4—C4864.21 (15)C31—C30—C35—C341.6 (6)
P3—Cu1—P4—C5465.96 (15)P3—C30—C35—C34179.5 (3)
P2—Cu1—P4—C5451.97 (15)C30—P3—C36—C41163.0 (3)
P1—Cu1—P4—C54174.60 (14)C29—P3—C36—C4155.8 (4)
C7—P1—C1—C2160.4 (4)Cu1—P3—C36—C4164.9 (4)
C13—P1—C1—C254.3 (4)C30—P3—C36—C3723.6 (4)
Cu1—P1—C1—C265.0 (4)C29—P3—C36—C37130.9 (3)
C7—P1—C1—C620.1 (4)Cu1—P3—C36—C37108.5 (3)
C13—P1—C1—C6126.2 (3)C41—C36—C37—C381.0 (6)
Cu1—P1—C1—C6114.5 (3)P3—C36—C37—C38174.6 (4)
C6—C1—C2—C30.5 (7)C36—C37—C38—C391.0 (8)
P1—C1—C2—C3179.0 (4)C37—C38—C39—C400.1 (8)
C1—C2—C3—C40.3 (9)C38—C39—C40—C410.8 (7)
C2—C3—C4—C51.0 (10)C37—C36—C41—C400.1 (6)
C3—C4—C5—C60.8 (9)P3—C36—C41—C40173.8 (3)
C4—C5—C6—C10.0 (8)C39—C40—C41—C360.8 (7)
C2—C1—C6—C50.7 (7)C48—P4—C42—C47105.0 (3)
P1—C1—C6—C5178.9 (4)C54—P4—C42—C472.6 (4)
C1—P1—C7—C12114.6 (3)Cu1—P4—C42—C47132.8 (3)
C13—P1—C7—C12140.2 (3)C48—P4—C42—C4380.1 (3)
Cu1—P1—C7—C1224.3 (3)C54—P4—C42—C43172.3 (3)
C1—P1—C7—C864.9 (3)Cu1—P4—C42—C4342.2 (4)
C13—P1—C7—C840.4 (3)C47—C42—C43—C440.7 (7)
Cu1—P1—C7—C8156.2 (3)P4—C42—C43—C44174.5 (4)
C12—C7—C8—C92.0 (6)C42—C43—C44—C450.1 (8)
P1—C7—C8—C9178.5 (3)C43—C44—C45—C461.4 (8)
C7—C8—C9—C102.3 (7)C44—C45—C46—C471.9 (8)
C8—C9—C10—C111.8 (7)C43—C42—C47—C460.2 (6)
C9—C10—C11—C121.1 (7)P4—C42—C47—C46174.7 (3)
C8—C7—C12—C111.3 (6)C45—C46—C47—C421.1 (7)
P1—C7—C12—C11179.2 (3)C42—P4—C48—C490.4 (4)
C10—C11—C12—C70.9 (6)C54—P4—C48—C49108.2 (3)
C7—P1—C13—C14127.0 (3)Cu1—P4—C48—C49121.8 (3)
C1—P1—C13—C14128.0 (3)C42—P4—C48—C53176.6 (3)
Cu1—P1—C13—C143.7 (3)C54—P4—C48—C5375.6 (3)
P1—C13—C14—C2968.2 (4)Cu1—P4—C48—C5354.3 (3)
P1—C13—C14—C1664.2 (4)C53—C48—C49—C501.1 (6)
P1—C13—C14—C15177.7 (3)P4—C48—C49—C50177.2 (3)
C13—C14—C16—P278.9 (4)C48—C49—C50—C510.7 (7)
C29—C14—C16—P251.5 (4)C49—C50—C51—C520.2 (8)
C15—C14—C16—P2167.5 (3)C50—C51—C52—C530.1 (8)
C17—P2—C16—C14141.1 (3)C51—C52—C53—C480.4 (7)
C23—P2—C16—C14113.8 (3)C49—C48—C53—C520.9 (6)
Cu1—P2—C16—C1417.1 (3)P4—C48—C53—C52177.3 (4)
C23—P2—C17—C22125.5 (3)C42—P4—C54—C5990.2 (3)
C16—P2—C17—C22127.6 (3)C48—P4—C54—C59161.8 (3)
Cu1—P2—C17—C2210.9 (4)Cu1—P4—C54—C5935.9 (4)
C23—P2—C17—C1854.2 (3)C42—P4—C54—C5588.1 (4)
C16—P2—C17—C1852.7 (4)C48—P4—C54—C5519.9 (4)
Cu1—P2—C17—C18169.4 (3)Cu1—P4—C54—C55145.7 (3)
C22—C17—C18—C192.2 (6)C59—C54—C55—C561.2 (6)
P2—C17—C18—C19177.5 (3)P4—C54—C55—C56177.1 (4)
C17—C18—C19—C201.3 (7)C54—C55—C56—C571.2 (7)
C18—C19—C20—C210.5 (7)C55—C56—C57—C580.3 (8)
C19—C20—C21—C221.5 (6)C56—C57—C58—C590.6 (8)
C18—C17—C22—C211.3 (6)C55—C54—C59—C580.4 (7)
P2—C17—C22—C21178.4 (3)P4—C54—C59—C58178.1 (4)
C20—C21—C22—C170.6 (6)C57—C58—C59—C540.6 (7)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C10—H10···F4i0.932.353.229 (12)158
Symmetry code: (i) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Cu(C18H15P)(C41H39P3)]BF4
Mr1037.25
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)13.470 (4), 14.356 (4), 26.240 (7)
β (°) 91.338 (5)
V3)5073 (2)
Z4
Radiation typeMo Kα
µ (mm1)0.61
Crystal size (mm)0.20 × 0.16 × 0.14
Data collection
DiffractometerBruker SMART
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.696, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
29232, 10469, 5826
Rint0.072
(sin θ/λ)max1)0.628
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.057, 0.138, 0.98
No. of reflections10469
No. of parameters660
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.49, 0.31

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Cu1—P42.2852 (11)Cu1—P22.3177 (12)
Cu1—P32.2983 (12)Cu1—P12.3314 (12)
P4—Cu1—P3122.79 (4)P4—Cu1—P1117.67 (4)
P4—Cu1—P2124.27 (4)P3—Cu1—P196.58 (4)
P3—Cu1—P291.17 (4)P2—Cu1—P197.65 (4)
 

Acknowledgements

We acknowledge the National Natural Science Foundation of China (20761006).

References

First citationFarrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  CrossRef IUCr Journals Google Scholar
First citationKourkine, I. V., Maslennikov, S. V., Ditchfield, R., Glueck, D. S., Yap, G. P. A., Liable-Sands, L. M. & Rheingold, A. L. (1996). Inorg. Chem. 35, 6708–6716.  CSD CrossRef PubMed CAS Web of Science Google Scholar
First citationMautz, J., Heinze, K., Wadepohl, H. & Huttner, G. (2008). Eur. J. Inorg. Chem. pp. 1413–1422.  Web of Science CSD CrossRef Google Scholar
First citationPawlowski, V., Knor, G., Lennartz, C. & Vogler, A. (2005). Eur. J. Inorg. Chem. pp. 3167–3171.  Web of Science CrossRef Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Ctyst. A63, 112-122.  Web of Science CrossRef Google Scholar
First citationSiemens (1996). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.  Google Scholar

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