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

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ISSN: 2056-9890

Tetra­kis(tri­phenyl­phosphane-κP)silver(I) tetra­fluorido­borate

aDepartment of Chemistry, Capital Normal University, Beijing 100048, People's Republic of China, and bKey Laboratory of Terahertz Optoelectronics, Ministry of Education, Department of Physics, Capital Normal University, Beijing 100048, People's Republic of China
*Correspondence e-mail: jinqh204@163.com

(Received 26 February 2012; accepted 24 April 2012; online 28 April 2012)

The title complex, [Ag(C18H15P)4]BF4, was prepared by the reaction of silver(I) tetra­fluorido­borate and triphenyl­phosphane in the presence of 1,2-bis­(pyridin-2-yl)ethyl­ene. The AgI atom is tetra­hedrally coordinated by four P atoms from triphenyl­phosphane (PPh3) ligands. Due to symmetry, the tetra­fluorido­borate anion is disordered over three positions (each with one third occupancy). The tetra­fluorido­borate anion does not coordinate to the AgI atom.

Related literature

For background to silver(I) complexes, see: Bowmaker et al. (1993[Bowmaker, G.A., Effendy, Hanna, J.V., Healy, P.C., Skelton, B.W. & White, A.H. (1993). J. Chem. Soc. Dalton Trans. pp. 1387-1397.]); Cui, Hu et al. (2010[Cui, L.-N., Hu, K.-Y., Jin, Q.-H. & Zhang, C.-L. (2010). Acta Cryst. E66, m871.]); Cui, Jin et al. (2010[Cui, L.-N., Jin, Q.-H., Hu, K.-Y. & Zhang, C.-L. (2010). Acta Cryst. E66, m969.]); Jin, Hu et al. (2010[Jin, Q. H., Hu, K. Y., Song, L. L., Wang, R., Zhang, C. L., Zuo, X. & Lu, X. M. (2010). Polyhedron, 29, 441-445.]); Jin, Song et al. (2010[Jin, Q. H., Song, L. L., Hu, K. Y., Zhou, L. L., Zhang, Y. Y. & Wang, R. (2010). Inorg. Chem. Commun. 13, 62-65.]); Meijboom et al. (2009[Meijboom, R., Bowen, R. J. & Berners-Price, S. J. (2009). Coord. Chem. Rev. 253, 325-342.]). For related structures, 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.]); Wen et al. (2011[Wen, J., Jiang, Y. H., Wu, M. H., Jin, Q. H. & Gong, H. L. (2011). Z. Kristallogr. New Cryst. Struct. 226, 269-270.]).

[Scheme 1]

Experimental

Crystal data
  • [Ag(C18H15P)4]BF4

  • Mr = 1243.76

  • Trigonal, [R \overline 3]

  • a = 14.2445 (12) Å

  • c = 51.591 (4) Å

  • V = 9065.7 (12) Å3

  • Z = 6

  • Mo Kα radiation

  • μ = 0.50 mm−1

  • T = 298 K

  • 0.30 × 0.18 × 0.15 mm

Data collection
  • Bruker SMART 1000 CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2007[Bruker (2007). SMART, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.866, Tmax = 0.930

  • 15472 measured reflections

  • 3548 independent reflections

  • 2167 reflections with I > 2σ(I)

  • Rint = 0.092

Refinement
  • R[F2 > 2σ(F2)] = 0.063

  • wR(F2) = 0.160

  • S = 1.07

  • 3548 reflections

  • 272 parameters

  • 1 restraint

  • H-atom parameters constrained

  • Δρmax = 1.34 e Å−3

  • Δρmin = −0.52 e Å−3

Data collection: SMART (Bruker, 2007[Bruker (2007). SMART, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2007[Bruker (2007). SMART, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The coordination chemistry of silver(I) is of considerable interest because of the luminescence properties and potential applications of silver(I) complexes in catalysis, cyanide, photography antimicrobial activities and electrochemical processes (Bowmaker et al., 1993; Cui, Hu et al., 2010; Cui, Jin et al., 2010; Jin, Hu et al.,2010; Jin, Song et al., 2010; Meijboom et al., 2009;). In our previous work, we obtained an AgIcomplex containing triphenylphosphane and trifluoromethanesulfonate ligands [Ag(PPh3)4(SO3CF3)](Wen et al., 2011). In this paper, we report a similar new silver(I) compound [Ag(P(C6H5)3)4][(BF4)].

The title compound is isomorphous with both [Ag(PPh3)4]ClO4 (Engelhardt et al., 1985) and [Ag(PPh3)4](SO3CF3) (Wen et al., 2011). The silver atom is coordinated by four P atoms from four triphenylphosphane ligands to form a tetrahedral geometry around the silver atom.

In [Ag(P(C6H5)3)4][(BF4)], the Ag—P bond lengths are in the range 2.633 (2)–2.6774 (13) Å, which agrees with those in the compound [Ag(PPh3)4(SO3CF3)] (Wen et al., 2011). The distorted P—Ag—P bite angles [P2—Ag1—P1 = 109.45 (3)°, P1—Ag1—P1 = 109.49 (3)°] are similar to the corresponding values for [Ag(PPh3)4(SO3CF3)] (Wen et al., 2011), too.

Related literature top

For background to silver(I) complexes, see: Bowmaker et al. (1993); Cui, Hu et al. (2010); Cui, Jin et al. (2010); Jin, Hu et al. (2010); Jin, Song et al. (2010); Meijboom et al. (2009). For related structures, see: Engelhardt et al. (1985); Wen et al. (2011).

Experimental top

A mixture of silver(I) tetrafluoridoborate and triphenylphosphane (PPh3) (molar ratio 1:1) and 1,2-di(2-pyridyl)ethylene (0.2 mmol) in the mixed solution of CH3OH (5 ml)/CH2Cl2 (5 ml) was stirred for 6 h at ambient temperature. The insoluble residues were removed by filtration, and the filtrate was evaporated slowly at room temperature for about three days to yield colorless crystals. Crystals suitable for single-crystal X-ray diffraction were selected directly from the sample as prepared.

Refinement top

H-atoms were positioned and refined using a riding model, with aromatic C—H = 0.93 Å, and the displacement parameters set for phenyl, H atoms at Uiso(H)=1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); 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 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular entities of the title compound, showing the atom-numbering scheme and with displacement ellipsoids drawn at the 50% probability level.
Tetrakis(triphenylphosphane-κP)silver(I) tetrafluoridoborate top
Crystal data top
[Ag(C18H15P)4]BF4Dx = 1.367 Mg m3
Mr = 1243.76Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3Cell parameters from 2109 reflections
a = 14.2445 (12) Åθ = 2.4–18.9°
c = 51.591 (4) ŵ = 0.50 mm1
V = 9065.7 (12) Å3T = 298 K
Z = 6White, block
F(000) = 38400.30 × 0.18 × 0.15 mm
Data collection top
Bruker SMART 1000 CCD
diffractometer
3548 independent reflections
Radiation source: fine-focus sealed tube2167 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.092
phi and ω scansθmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2007)
h = 1616
Tmin = 0.866, Tmax = 0.930k = 1516
15472 measured reflectionsl = 6140
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)] = 0.063Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.160H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0699P)2]
where P = (Fo2 + 2Fc2)/3
3548 reflections(Δ/σ)max = 0.001
272 parametersΔρmax = 1.34 e Å3
1 restraintΔρmin = 0.52 e Å3
Crystal data top
[Ag(C18H15P)4]BF4Z = 6
Mr = 1243.76Mo Kα radiation
Trigonal, R3µ = 0.50 mm1
a = 14.2445 (12) ÅT = 298 K
c = 51.591 (4) Å0.30 × 0.18 × 0.15 mm
V = 9065.7 (12) Å3
Data collection top
Bruker SMART 1000 CCD
diffractometer
3548 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2007)
2167 reflections with I > 2σ(I)
Tmin = 0.866, Tmax = 0.930Rint = 0.092
15472 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0631 restraint
wR(F2) = 0.160H-atom parameters constrained
S = 1.07Δρmax = 1.34 e Å3
3548 reflectionsΔρmin = 0.52 e Å3
272 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) 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*/UeqOcc. (<1)
Ag10.66670.33330.081276 (13)0.0476 (3)
P10.80962 (10)0.53162 (10)0.06400 (3)0.0464 (4)
P20.66670.33330.13231 (4)0.0475 (6)
F10.364 (3)0.600 (2)0.1780 (6)0.112 (6)0.33
F20.273 (4)0.604 (2)0.1863 (5)0.166 (11)0.33
F30.021 (3)0.921 (2)0.0089 (5)0.140 (6)0.33
F40.023 (4)1.036 (3)0.0208 (3)0.146 (9)0.33
B10.33330.66670.16670.113 (9)
B20.00001.00000.00000.130 (10)
C10.9477 (4)0.5677 (4)0.07293 (10)0.0490 (13)
C21.0219 (4)0.6654 (4)0.08427 (11)0.0575 (14)
H21.00380.71920.08650.069*
C31.1221 (5)0.6841 (5)0.09236 (13)0.0707 (17)
H31.17080.75020.09990.085*
C41.1502 (5)0.6060 (5)0.08940 (13)0.0742 (18)
H41.21700.61790.09530.089*
C51.0794 (5)0.5100 (5)0.07767 (14)0.0774 (19)
H51.09940.45780.07490.093*
C60.9783 (5)0.4904 (5)0.06992 (12)0.0702 (17)
H60.92990.42390.06250.084*
C70.8161 (4)0.5488 (4)0.02889 (11)0.0566 (15)
C80.9121 (5)0.6150 (6)0.01588 (12)0.083 (2)
H80.97800.64620.02460.099*
C90.9082 (6)0.6344 (7)0.01077 (15)0.111 (3)
H90.97140.68240.01950.133*
C100.8122 (7)0.5829 (7)0.02380 (14)0.097 (2)
H100.81040.59510.04150.117*
C110.7195 (6)0.5142 (6)0.01119 (13)0.0782 (18)
H110.65500.47760.02040.094*
C120.7192 (5)0.4979 (5)0.01485 (11)0.0648 (16)
H120.65430.45280.02330.078*
C130.8024 (4)0.6496 (4)0.07541 (10)0.0486 (13)
C140.8377 (4)0.7441 (4)0.06072 (12)0.0626 (15)
H140.85960.74630.04360.075*
C150.8401 (5)0.8340 (5)0.07156 (14)0.0731 (18)
H150.86540.89730.06190.088*
C160.8049 (5)0.8295 (5)0.09661 (15)0.0754 (19)
H160.80750.89050.10390.090*
C170.7665 (5)0.7372 (5)0.11083 (12)0.0705 (17)
H170.74050.73450.12750.085*
C180.7660 (4)0.6478 (5)0.10054 (11)0.0612 (15)
H180.74100.58540.11050.073*
C190.6357 (4)0.4300 (4)0.14761 (10)0.0493 (13)
C200.6937 (5)0.4944 (5)0.16853 (11)0.0652 (16)
H200.75380.49230.17490.078*
C210.6615 (6)0.5616 (5)0.17986 (13)0.085 (2)
H210.69820.60210.19440.101*
C220.5770 (6)0.5693 (5)0.17011 (14)0.0799 (19)
H220.55710.61610.17770.096*
C230.5210 (5)0.5077 (5)0.14904 (13)0.0760 (18)
H230.46330.51310.14230.091*
C240.5495 (5)0.4394 (5)0.13809 (12)0.0641 (16)
H240.51060.39780.12390.077*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0492 (3)0.0492 (3)0.0444 (5)0.02459 (16)0.0000.000
P10.0451 (8)0.0450 (7)0.0468 (9)0.0208 (6)0.0015 (6)0.0032 (6)
P20.0519 (9)0.0519 (9)0.0387 (13)0.0260 (4)0.0000.000
F10.124 (15)0.082 (12)0.163 (18)0.076 (10)0.001 (18)0.001 (14)
F20.16 (3)0.12 (2)0.17 (2)0.038 (15)0.014 (19)0.048 (16)
F30.158 (18)0.134 (19)0.14 (2)0.081 (14)0.01 (2)0.020 (17)
F40.17 (3)0.15 (3)0.098 (12)0.066 (18)0.02 (2)0.027 (17)
B10.094 (15)0.094 (15)0.15 (3)0.047 (7)0.0000.000
B20.14 (2)0.14 (2)0.10 (4)0.071 (12)0.0000.000
C10.048 (3)0.045 (3)0.054 (3)0.024 (3)0.005 (3)0.006 (3)
C20.043 (3)0.054 (3)0.074 (4)0.022 (3)0.003 (3)0.005 (3)
C30.053 (4)0.060 (4)0.087 (5)0.019 (3)0.011 (3)0.011 (3)
C40.041 (3)0.085 (5)0.095 (5)0.030 (4)0.003 (3)0.008 (4)
C50.060 (4)0.071 (4)0.111 (6)0.040 (4)0.001 (4)0.001 (4)
C60.058 (4)0.062 (4)0.088 (5)0.028 (3)0.004 (3)0.004 (3)
C70.059 (4)0.059 (4)0.052 (3)0.030 (3)0.002 (3)0.006 (3)
C80.062 (4)0.109 (5)0.061 (4)0.030 (4)0.005 (3)0.019 (4)
C90.092 (6)0.147 (8)0.071 (5)0.043 (5)0.027 (5)0.035 (5)
C100.105 (6)0.138 (7)0.054 (4)0.065 (6)0.003 (5)0.015 (5)
C110.087 (5)0.096 (5)0.061 (4)0.054 (4)0.013 (4)0.004 (4)
C120.071 (4)0.070 (4)0.054 (4)0.036 (3)0.005 (3)0.001 (3)
C130.044 (3)0.044 (3)0.054 (3)0.019 (3)0.000 (3)0.004 (3)
C140.065 (4)0.059 (4)0.063 (4)0.031 (3)0.003 (3)0.006 (3)
C150.084 (5)0.052 (4)0.092 (5)0.040 (4)0.010 (4)0.007 (4)
C160.074 (4)0.058 (4)0.100 (6)0.037 (4)0.009 (4)0.012 (4)
C170.069 (4)0.078 (5)0.072 (4)0.042 (4)0.002 (3)0.014 (4)
C180.061 (4)0.053 (3)0.066 (4)0.025 (3)0.007 (3)0.005 (3)
C190.057 (3)0.057 (3)0.039 (3)0.032 (3)0.000 (3)0.003 (3)
C200.079 (4)0.074 (4)0.061 (4)0.051 (4)0.015 (3)0.023 (3)
C210.095 (5)0.087 (5)0.074 (5)0.047 (4)0.015 (4)0.026 (4)
C220.092 (5)0.075 (4)0.088 (5)0.053 (4)0.011 (4)0.008 (4)
C230.076 (4)0.081 (4)0.082 (5)0.048 (4)0.001 (4)0.001 (4)
C240.070 (4)0.075 (4)0.054 (4)0.042 (3)0.002 (3)0.004 (3)
Geometric parameters (Å, º) top
Ag1—P22.633 (2)B2—F3viii1.38 (2)
Ag1—P1i2.6772 (13)B2—F3ix1.38 (2)
Ag1—P12.6772 (13)B2—F3x1.38 (2)
Ag1—P1ii2.6772 (13)B2—F3xi1.38 (2)
P1—C71.824 (6)C1—C61.380 (7)
P1—C11.826 (5)C1—C21.388 (7)
P1—C131.831 (5)C2—C31.379 (7)
P2—C19i1.822 (5)C2—H20.9300
P2—C19ii1.822 (5)C3—C41.367 (8)
P2—C191.822 (5)C3—H30.9300
F1—F2iii0.97 (4)C4—C51.369 (8)
F1—B11.37 (2)C4—H40.9300
F1—F21.39 (5)C5—C61.382 (8)
F1—F2iv1.66 (2)C5—H50.9300
F1—F1iv1.70 (4)C6—H60.9300
F1—F1v1.70 (4)C7—C81.386 (8)
F2—F1vi0.97 (4)C7—C121.398 (8)
F2—B11.34 (3)C8—C91.409 (9)
F2—F2iii1.52 (4)C8—H80.9300
F2—F2vi1.52 (4)C9—C101.363 (10)
F2—F1v1.66 (2)C9—H90.9300
F3—F4vii1.16 (4)C10—C111.353 (9)
F3—B21.38 (2)C10—H100.9300
F3—F4viii1.42 (5)C11—C121.363 (8)
F3—F3ix1.59 (3)C11—H110.9300
F3—F3x1.59 (3)C12—H120.9300
F3—F4xi1.65 (3)C13—C181.392 (7)
F4—F3viii1.16 (4)C13—C141.401 (7)
F4—F4vii1.27 (4)C14—C151.382 (8)
F4—F4viii1.27 (4)C14—H140.9300
F4—B21.301 (18)C15—C161.376 (9)
F4—F3vii1.42 (5)C15—H150.9300
F4—F3xi1.65 (3)C16—C171.359 (8)
B1—F2iv1.34 (3)C16—H160.9300
B1—F2xii1.34 (3)C17—C181.377 (8)
B1—F2v1.34 (3)C17—H170.9300
B1—F2vi1.34 (3)C18—H180.9300
B1—F2iii1.34 (3)C19—C241.389 (7)
B1—F1iv1.37 (2)C19—C201.390 (7)
B1—F1v1.37 (2)C20—C211.381 (8)
B1—F1vi1.37 (2)C20—H200.9300
B1—F1iii1.37 (2)C21—C221.360 (9)
B1—F1xii1.37 (2)C21—H210.9300
B2—F4viii1.301 (18)C22—C231.374 (9)
B2—F4vii1.301 (18)C22—H220.9300
B2—F4xi1.301 (18)C23—C241.352 (8)
B2—F4x1.301 (18)C23—H230.9300
B2—F4ix1.301 (18)C24—H240.9300
B2—F3vii1.38 (2)
P2—Ag1—P1i109.45 (3)F1vi—B1—F1xii76.9 (13)
P2—Ag1—P1109.45 (3)F1iii—B1—F1xii76.9 (13)
P1i—Ag1—P1109.49 (3)F1—B1—F1xii179.994 (18)
P2—Ag1—P1ii109.45 (3)F4viii—B2—F4vii58.5 (15)
P1i—Ag1—P1ii109.49 (3)F4viii—B2—F458.5 (15)
P1—Ag1—P1ii109.49 (3)F4vii—B2—F458.5 (15)
C7—P1—C1103.8 (2)F4viii—B2—F4xi121.5 (15)
C7—P1—C13102.6 (2)F4vii—B2—F4xi121.5 (15)
C1—P1—C13102.0 (2)F4—B2—F4xi180.0 (8)
C7—P1—Ag1115.64 (18)F4viii—B2—F4x121.5 (15)
C1—P1—Ag1110.91 (16)F4vii—B2—F4x180 (2)
C13—P1—Ag1119.93 (17)F4—B2—F4x121.5 (15)
C19i—P2—C19ii102.6 (2)F4xi—B2—F4x58.5 (15)
C19i—P2—C19102.6 (2)F4viii—B2—F4ix180.0 (8)
C19ii—P2—C19102.6 (2)F4vii—B2—F4ix121.5 (15)
C19i—P2—Ag1115.66 (17)F4—B2—F4ix121.5 (15)
C19ii—P2—Ag1115.66 (17)F4xi—B2—F4ix58.5 (15)
C19—P2—Ag1115.66 (17)F4x—B2—F4ix58.5 (15)
F2iii—F1—B167 (3)F4viii—B2—F3vii51 (2)
F2iii—F1—F278 (3)F4vii—B2—F3vii104.3 (14)
B1—F1—F258.1 (14)F4—B2—F3vii64 (2)
F2iii—F1—F2iv111 (4)F4xi—B2—F3vii116 (2)
B1—F1—F2iv51.4 (15)F4x—B2—F3vii75.7 (14)
F2—F1—F2iv92 (2)F4ix—B2—F3vii129 (2)
F2iii—F1—F1iv71 (2)F4viii—B2—F3viii104.3 (14)
B1—F1—F1iv51.5 (7)F4vii—B2—F3viii64 (2)
F2—F1—F1iv109.3 (15)F4—B2—F3viii51 (2)
F2iv—F1—F1iv49 (2)F4xi—B2—F3viii129 (2)
F2iii—F1—F1v118 (3)F4x—B2—F3viii116 (2)
B1—F1—F1v51.5 (7)F4ix—B2—F3viii75.7 (14)
F2—F1—F1v64.0 (10)F3vii—B2—F3viii109.5 (10)
F2iv—F1—F1v33.5 (15)F4viii—B2—F3ix75.7 (14)
F1iv—F1—F1v78 (2)F4vii—B2—F3ix116 (2)
F1vi—F2—B171 (3)F4—B2—F3ix129 (2)
F1vi—F2—F1130 (5)F4xi—B2—F3ix51 (2)
B1—F2—F160 (2)F4x—B2—F3ix64 (2)
F1vi—F2—F2iii117 (3)F4ix—B2—F3ix104.3 (14)
B1—F2—F2iii55.4 (9)F3vii—B2—F3ix70.5 (10)
F1—F2—F2iii39 (2)F3viii—B2—F3ix180 (2)
F1vi—F2—F2vi63 (3)F4viii—B2—F3x129 (2)
B1—F2—F2vi55.4 (9)F4vii—B2—F3x75.7 (14)
F1—F2—F2vi95 (2)F4—B2—F3x116 (2)
F2iii—F2—F2vi60.000 (9)F4xi—B2—F3x64 (2)
F1vi—F2—F1v76 (3)F4x—B2—F3x104.3 (14)
B1—F2—F1v53.0 (11)F4ix—B2—F3x51 (2)
F1—F2—F1v67 (3)F3vii—B2—F3x180 (2)
F2iii—F2—F1v93.8 (19)F3viii—B2—F3x70.5 (10)
F2vi—F2—F1v105.2 (11)F3ix—B2—F3x109.5 (10)
F4vii—F3—B261.0 (17)F4viii—B2—F364 (2)
F4vii—F3—F4viii58 (2)F4vii—B2—F351 (2)
B2—F3—F4viii55.5 (14)F4—B2—F3104.3 (14)
F4vii—F3—F3ix110.8 (16)F4xi—B2—F375.7 (14)
B2—F3—F3ix54.7 (5)F4x—B2—F3129 (2)
F4viii—F3—F3ix66.1 (12)F4ix—B2—F3116 (2)
F4vii—F3—F3x71.6 (15)F3vii—B2—F3109.5 (10)
B2—F3—F3x54.7 (5)F3viii—B2—F3109.5 (10)
F4viii—F3—F3x106.9 (14)F3ix—B2—F370.5 (10)
F3ix—F3—F3x90 (2)F3x—B2—F370.5 (10)
F4vii—F3—F4xi107 (3)F4viii—B2—F3xi116 (2)
B2—F3—F4xi50.0 (13)F4vii—B2—F3xi129 (2)
F4viii—F3—F4xi95 (3)F4—B2—F3xi75.7 (14)
F3ix—F3—F4xi41.9 (19)F4xi—B2—F3xi104.3 (14)
F3x—F3—F4xi52 (2)F4x—B2—F3xi51 (2)
F3viii—F4—F4vii71 (4)F4ix—B2—F3xi64 (2)
F3viii—F4—F4viii121 (3)F3vii—B2—F3xi70.5 (10)
F4vii—F4—F4viii60.000 (6)F3viii—B2—F3xi70.5 (10)
F3viii—F4—B267.9 (19)F3ix—B2—F3xi109.5 (10)
F4vii—F4—B260.7 (7)F3x—B2—F3xi109.5 (10)
F4viii—F4—B260.7 (7)F3—B2—F3xi180 (2)
F3viii—F4—F3vii122 (3)C6—C1—C2117.4 (5)
F4vii—F4—F3vii104 (3)C6—C1—P1118.2 (4)
F4viii—F4—F3vii51 (3)C2—C1—P1124.2 (4)
B2—F4—F3vii60.8 (19)C3—C2—C1121.2 (5)
F3viii—F4—F3xi66.5 (14)C3—C2—H2119.4
F4vii—F4—F3xi111.3 (13)C1—C2—H2119.4
F4viii—F4—F3xi102 (2)C4—C3—C2120.3 (6)
B2—F4—F3xi54.3 (9)C4—C3—H3119.8
F3vii—F4—F3xi62.1 (16)C2—C3—H3119.8
F2iv—B1—F2xii69.2 (18)C3—C4—C5119.5 (6)
F2iv—B1—F2v69.2 (18)C3—C4—H4120.2
F2xii—B1—F2v69.2 (18)C5—C4—H4120.2
F2iv—B1—F2vi180.0 (15)C4—C5—C6120.2 (6)
F2xii—B1—F2vi110.8 (18)C4—C5—H5119.9
F2v—B1—F2vi110.8 (18)C6—C5—H5119.9
F2iv—B1—F2110.8 (18)C1—C6—C5121.3 (6)
F2xii—B1—F2179.995 (13)C1—C6—H6119.3
F2v—B1—F2110.8 (18)C5—C6—H6119.3
F2vi—B1—F269.2 (18)C8—C7—C12118.9 (5)
F2iv—B1—F2iii110.8 (18)C8—C7—P1122.6 (5)
F2xii—B1—F2iii110.8 (18)C12—C7—P1118.3 (4)
F2v—B1—F2iii179.994 (19)C7—C8—C9119.0 (6)
F2vi—B1—F2iii69.2 (18)C7—C8—H8120.5
F2—B1—F2iii69.2 (18)C9—C8—H8120.5
F2iv—B1—F1iv62 (2)C10—C9—C8120.2 (7)
F2xii—B1—F1iv42.0 (17)C10—C9—H9119.9
F2v—B1—F1iv104.4 (11)C8—C9—H9119.9
F2vi—B1—F1iv118 (2)C11—C10—C9120.3 (7)
F2—B1—F1iv138.0 (17)C11—C10—H10119.8
F2iii—B1—F1iv75.6 (11)C9—C10—H10119.8
F2iv—B1—F1v42.0 (18)C10—C11—C12121.1 (7)
F2xii—B1—F1v104.4 (11)C10—C11—H11119.5
F2v—B1—F1v62 (2)C12—C11—H11119.5
F2vi—B1—F1v138.0 (17)C11—C12—C7120.3 (6)
F2—B1—F1v75.6 (11)C11—C12—H12119.9
F2iii—B1—F1v118 (2)C7—C12—H12119.9
F1iv—B1—F1v103.1 (13)C18—C13—C14118.2 (5)
F2iv—B1—F1vi118 (2)C18—C13—P1118.3 (4)
F2xii—B1—F1vi138.0 (17)C14—C13—P1123.4 (4)
F2v—B1—F1vi75.6 (11)C15—C14—C13120.1 (6)
F2vi—B1—F1vi62 (2)C15—C14—H14119.9
F2—B1—F1vi42.0 (17)C13—C14—H14119.9
F2iii—B1—F1vi104.4 (11)C16—C15—C14119.8 (6)
F1iv—B1—F1vi179.996 (10)C16—C15—H15120.1
F1v—B1—F1vi76.9 (13)C14—C15—H15120.1
F2iv—B1—F1iii138.0 (17)C17—C16—C15120.8 (6)
F2xii—B1—F1iii75.6 (11)C17—C16—H16119.6
F2v—B1—F1iii118 (2)C15—C16—H16119.6
F2vi—B1—F1iii42.0 (18)C16—C17—C18120.0 (6)
F2—B1—F1iii104.4 (11)C16—C17—H17120.0
F2iii—B1—F1iii62 (2)C18—C17—H17120.0
F1iv—B1—F1iii76.9 (13)C17—C18—C13120.8 (6)
F1v—B1—F1iii180.0 (11)C17—C18—H18119.6
F1vi—B1—F1iii103.1 (13)C13—C18—H18119.6
F2iv—B1—F175.6 (11)C24—C19—C20118.3 (5)
F2xii—B1—F1118 (2)C24—C19—P2118.6 (4)
F2v—B1—F1138.1 (17)C20—C19—P2123.1 (4)
F2vi—B1—F1104.4 (11)C21—C20—C19119.5 (6)
F2—B1—F162 (2)C21—C20—H20120.3
F2iii—B1—F142.0 (17)C19—C20—H20120.3
F1iv—B1—F176.9 (13)C22—C21—C20120.9 (6)
F1v—B1—F176.9 (13)C22—C21—H21119.5
F1vi—B1—F1103.1 (13)C20—C21—H21119.5
F1iii—B1—F1103.1 (13)C21—C22—C23119.8 (6)
F2iv—B1—F1xii104.4 (11)C21—C22—H22120.1
F2xii—B1—F1xii62 (2)C23—C22—H22120.1
F2v—B1—F1xii42.0 (17)C24—C23—C22120.2 (6)
F2vi—B1—F1xii75.6 (11)C24—C23—H23119.9
F2—B1—F1xii118 (2)C22—C23—H23119.9
F2iii—B1—F1xii138.0 (17)C23—C24—C19121.3 (6)
F1iv—B1—F1xii103.1 (13)C23—C24—H24119.3
F1v—B1—F1xii103.1 (13)C19—C24—H24119.3
P2—Ag1—P1—C7177.16 (19)F3viii—F4—B2—F4xi65 (100)
P1i—Ag1—P1—C762.9 (2)F4vii—F4—B2—F4xi145 (100)
P1ii—Ag1—P1—C757.2 (2)F4viii—F4—B2—F4xi145 (100)
P2—Ag1—P1—C165.07 (18)F3vii—F4—B2—F4xi86 (100)
P1i—Ag1—P1—C154.9 (2)F3xi—F4—B2—F4xi11 (100)
P1ii—Ag1—P1—C1174.96 (18)F3viii—F4—B2—F4x100 (4)
P2—Ag1—P1—C1353.4 (2)F4vii—F4—B2—F4x180.000 (11)
P1i—Ag1—P1—C13173.35 (19)F4viii—F4—B2—F4x110.1 (6)
P1ii—Ag1—P1—C1366.6 (2)F3vii—F4—B2—F4x51 (3)
P1i—Ag1—P2—C19i57.77 (18)F3xi—F4—B2—F4x24 (4)
P1—Ag1—P2—C19i62.23 (18)F3viii—F4—B2—F4ix30 (4)
P1ii—Ag1—P2—C19i177.77 (18)F4vii—F4—B2—F4ix110.1 (6)
P1i—Ag1—P2—C19ii62.23 (18)F4viii—F4—B2—F4ix180.000 (14)
P1—Ag1—P2—C19ii177.77 (18)F3vii—F4—B2—F4ix121 (3)
P1ii—Ag1—P2—C19ii57.77 (18)F3xi—F4—B2—F4ix46 (4)
P1i—Ag1—P2—C19177.77 (18)F3viii—F4—B2—F3vii151.3 (19)
P1—Ag1—P2—C1957.77 (18)F4vii—F4—B2—F3vii129 (3)
P1ii—Ag1—P2—C1962.23 (18)F4viii—F4—B2—F3vii59 (3)
F2iii—F1—F2—F1vi84 (6)F3xi—F4—B2—F3vii75.0 (10)
B1—F1—F2—F1vi13 (4)F4vii—F4—B2—F3viii80 (4)
F2iv—F1—F2—F1vi27 (4)F4viii—F4—B2—F3viii150 (4)
F1iv—F1—F2—F1vi20 (6)F3vii—F4—B2—F3viii151.3 (19)
F1v—F1—F2—F1vi46 (3)F3xi—F4—B2—F3viii76.3 (9)
F2iii—F1—F2—B171 (3)F3viii—F4—B2—F3ix180.000 (2)
F2iv—F1—F2—B140.6 (18)F4vii—F4—B2—F3ix100 (4)
F1iv—F1—F2—B16 (2)F4viii—F4—B2—F3ix30 (4)
F1v—F1—F2—B159.2 (9)F3vii—F4—B2—F3ix28.7 (19)
B1—F1—F2—F2iii71 (3)F3xi—F4—B2—F3ix103.7 (9)
F2iv—F1—F2—F2iii111 (4)F3viii—F4—B2—F3x28.7 (19)
F1iv—F1—F2—F2iii65 (2)F4vii—F4—B2—F3x51 (3)
F1v—F1—F2—F2iii130 (4)F4viii—F4—B2—F3x121 (3)
F2iii—F1—F2—F2vi25 (3)F3vii—F4—B2—F3x180.000 (8)
B1—F1—F2—F2vi45.4 (10)F3xi—F4—B2—F3x105.0 (10)
F2iv—F1—F2—F2vi86 (2)F3viii—F4—B2—F3103.7 (9)
F1iv—F1—F2—F2vi39 (2)F4vii—F4—B2—F324 (4)
F1v—F1—F2—F2vi104.6 (15)F4viii—F4—B2—F346 (4)
F2iii—F1—F2—F1v130 (4)F3vii—F4—B2—F3105.0 (10)
B1—F1—F2—F1v59.2 (9)F3xi—F4—B2—F3180.00 (2)
F2iv—F1—F2—F1v18.6 (17)F3viii—F4—B2—F3xi76.3 (9)
F1iv—F1—F2—F1v65 (3)F4vii—F4—B2—F3xi156 (4)
F1vi—F2—B1—F2iv110 (4)F4viii—F4—B2—F3xi134 (4)
F1—F2—B1—F2iv59.5 (19)F3vii—F4—B2—F3xi75.0 (10)
F2iii—F2—B1—F2iv105.2 (9)F4vii—F3—B2—F4viii70 (2)
F2vi—F2—B1—F2iv180.000 (12)F3ix—F3—B2—F4viii83.3 (15)
F1v—F2—B1—F2iv23 (3)F3x—F3—B2—F4viii156.6 (18)
F1vi—F2—B1—F2xii72 (6)F4xi—F3—B2—F4viii137 (3)
F1—F2—B1—F2xii119 (6)F4viii—F3—B2—F4vii70 (2)
F2iii—F2—B1—F2xii74 (8)F3ix—F3—B2—F4vii153 (2)
F2vi—F2—B1—F2xii1 (8)F3x—F3—B2—F4vii87.1 (16)
F1v—F2—B1—F2xii158 (5)F4xi—F3—B2—F4vii154 (3)
F1vi—F2—B1—F2v35 (4)F4vii—F3—B2—F426 (3)
F1—F2—B1—F2v134 (2)F4viii—F3—B2—F443 (3)
F2iii—F2—B1—F2v180.005 (4)F3ix—F3—B2—F4127 (2)
F2vi—F2—B1—F2v105.2 (9)F3x—F3—B2—F4113 (3)
F1v—F2—B1—F2v52 (3)F4xi—F3—B2—F4180.00 (2)
F1vi—F2—B1—F2vi70 (4)F4vii—F3—B2—F4xi154 (3)
F1—F2—B1—F2vi120.5 (19)F4viii—F3—B2—F4xi137 (3)
F2iii—F2—B1—F2vi74.8 (9)F3ix—F3—B2—F4xi53 (2)
F1v—F2—B1—F2vi157 (3)F3x—F3—B2—F4xi67 (3)
F1vi—F2—B1—F2iii145 (4)F4vii—F3—B2—F4x180.000 (15)
F1—F2—B1—F2iii46 (2)F4viii—F3—B2—F4x110 (2)
F2vi—F2—B1—F2iii74.8 (9)F3ix—F3—B2—F4x27 (2)
F1v—F2—B1—F2iii128 (3)F3x—F3—B2—F4x92.9 (16)
F1vi—F2—B1—F1iv179.994 (11)F4xi—F3—B2—F4x26 (3)
F1—F2—B1—F1iv11 (3)F4vii—F3—B2—F4ix110 (2)
F2iii—F2—B1—F1iv35 (4)F4viii—F3—B2—F4ix180.000 (12)
F2vi—F2—B1—F1iv110 (4)F3ix—F3—B2—F4ix96.7 (15)
F1v—F2—B1—F1iv93.6 (19)F3x—F3—B2—F4ix23.4 (18)
F1vi—F2—B1—F1v86.4 (19)F4xi—F3—B2—F4ix43 (3)
F1—F2—B1—F1v82.7 (17)F4vii—F3—B2—F3vii92.9 (16)
F2iii—F2—B1—F1v128 (3)F4viii—F3—B2—F3vii23.4 (18)
F2vi—F2—B1—F1v157 (3)F3ix—F3—B2—F3vii60 (3)
F1—F2—B1—F1vi169 (3)F3x—F3—B2—F3vii180.000 (2)
F2iii—F2—B1—F1vi145 (4)F4xi—F3—B2—F3vii113 (3)
F2vi—F2—B1—F1vi70 (4)F4vii—F3—B2—F3viii27 (2)
F1v—F2—B1—F1vi86.4 (19)F4viii—F3—B2—F3viii96.7 (15)
F1vi—F2—B1—F1iii93.6 (19)F3ix—F3—B2—F3viii180.000 (9)
F1—F2—B1—F1iii97.3 (17)F3x—F3—B2—F3viii60 (3)
F2iii—F2—B1—F1iii52 (3)F4xi—F3—B2—F3viii127 (2)
F2vi—F2—B1—F1iii23 (3)F4vii—F3—B2—F3ix153 (2)
F1v—F2—B1—F1iii179.998 (10)F4viii—F3—B2—F3ix83.3 (15)
F1vi—F2—B1—F1169 (3)F3x—F3—B2—F3ix120 (3)
F2iii—F2—B1—F146 (2)F4xi—F3—B2—F3ix53 (2)
F2vi—F2—B1—F1120.5 (19)F4vii—F3—B2—F3x87.1 (16)
F1v—F2—B1—F182.7 (17)F4viii—F3—B2—F3x156.6 (18)
F1vi—F2—B1—F1xii11 (3)F3ix—F3—B2—F3x120 (3)
F1—F2—B1—F1xii180.00 (2)F4xi—F3—B2—F3x67 (3)
F2iii—F2—B1—F1xii134 (2)F4vii—F3—B2—F3xi131 (3)
F2vi—F2—B1—F1xii59.5 (19)F4viii—F3—B2—F3xi159 (4)
F1v—F2—B1—F1xii97.3 (17)F3ix—F3—B2—F3xi76 (4)
F2iii—F1—B1—F2iv147 (4)F3x—F3—B2—F3xi44 (4)
F2—F1—B1—F2iv124 (2)F4xi—F3—B2—F3xi22 (4)
F1iv—F1—B1—F2iv64 (3)C7—P1—C1—C681.1 (5)
F1v—F1—B1—F2iv43.2 (18)C13—P1—C1—C6172.5 (5)
F2iii—F1—B1—F2xii90 (4)Ag1—P1—C1—C643.7 (5)
F2—F1—B1—F2xii180.00 (2)C7—P1—C1—C2103.6 (5)
F2iv—F1—B1—F2xii56 (2)C13—P1—C1—C22.8 (5)
F1iv—F1—B1—F2xii7 (2)Ag1—P1—C1—C2131.6 (4)
F1v—F1—B1—F2xii99.5 (11)C6—C1—C2—C30.4 (8)
F2iii—F1—B1—F2v179.993 (15)P1—C1—C2—C3174.9 (5)
F2—F1—B1—F2v90 (4)C1—C2—C3—C40.2 (9)
F2iv—F1—B1—F2v33 (4)C2—C3—C4—C51.8 (10)
F1iv—F1—B1—F2v97.2 (17)C3—C4—C5—C62.8 (10)
F1v—F1—B1—F2v10 (3)C2—C1—C6—C50.6 (9)
F2iii—F1—B1—F2vi33 (4)P1—C1—C6—C5176.3 (5)
F2—F1—B1—F2vi56 (2)C4—C5—C6—C12.3 (10)
F2iv—F1—B1—F2vi180.00 (5)C1—P1—C7—C822.7 (6)
F1iv—F1—B1—F2vi116 (3)C13—P1—C7—C883.2 (6)
F1v—F1—B1—F2vi136.8 (19)Ag1—P1—C7—C8144.4 (5)
F2iii—F1—B1—F290 (4)C1—P1—C7—C12161.1 (4)
F2iv—F1—B1—F2124 (2)C13—P1—C7—C1293.0 (5)
F1iv—F1—B1—F2173 (2)Ag1—P1—C7—C1239.5 (5)
F1v—F1—B1—F280.5 (11)C12—C7—C8—C93.9 (10)
F2—F1—B1—F2iii90 (4)P1—C7—C8—C9172.2 (6)
F2iv—F1—B1—F2iii147 (4)C7—C8—C9—C104.2 (12)
F1iv—F1—B1—F2iii82.9 (17)C8—C9—C10—C111.1 (13)
F1v—F1—B1—F2iii170 (3)C9—C10—C11—C122.4 (12)
F2iii—F1—B1—F1iv82.9 (17)C10—C11—C12—C72.7 (10)
F2—F1—B1—F1iv173 (2)C8—C7—C12—C110.5 (9)
F2iv—F1—B1—F1iv64 (3)P1—C7—C12—C11175.7 (5)
F1v—F1—B1—F1iv107 (2)C7—P1—C13—C18162.0 (4)
F2iii—F1—B1—F1v170 (3)C1—P1—C13—C1890.7 (5)
F2—F1—B1—F1v80.5 (11)Ag1—P1—C13—C1832.2 (5)
F2iv—F1—B1—F1v43.2 (18)C7—P1—C13—C1422.0 (5)
F1iv—F1—B1—F1v107 (2)C1—P1—C13—C1485.3 (5)
F2iii—F1—B1—F1vi97.1 (17)Ag1—P1—C13—C14151.8 (4)
F2—F1—B1—F1vi7 (2)C18—C13—C14—C152.6 (8)
F2iv—F1—B1—F1vi116 (3)P1—C13—C14—C15173.4 (4)
F1iv—F1—B1—F1vi180.00 (2)C13—C14—C15—C161.7 (9)
F1v—F1—B1—F1vi73 (2)C14—C15—C16—C170.8 (10)
F2iii—F1—B1—F1iii10 (3)C15—C16—C17—C182.3 (9)
F2—F1—B1—F1iii99.5 (11)C16—C17—C18—C131.4 (9)
F2iv—F1—B1—F1iii136.8 (18)C14—C13—C18—C171.1 (8)
F1iv—F1—B1—F1iii73 (2)P1—C13—C18—C17175.1 (4)
F1v—F1—B1—F1iii179.995 (15)C19i—P2—C19—C24171.7 (4)
F2iii—F1—B1—F1xii50 (5)C19ii—P2—C19—C2482.0 (6)
F2—F1—B1—F1xii40 (4)Ag1—P2—C19—C2444.9 (5)
F2iv—F1—B1—F1xii164 (3)C19i—P2—C19—C208.8 (5)
F1iv—F1—B1—F1xii133 (4)C19ii—P2—C19—C2097.5 (4)
F1v—F1—B1—F1xii120 (4)Ag1—P2—C19—C20135.7 (4)
F3viii—F4—B2—F4viii150 (4)C24—C19—C20—C212.8 (9)
F4vii—F4—B2—F4viii69.9 (6)P2—C19—C20—C21176.7 (5)
F3vii—F4—B2—F4viii59 (3)C19—C20—C21—C223.0 (10)
F3xi—F4—B2—F4viii134 (4)C20—C21—C22—C231.5 (11)
F3viii—F4—B2—F4vii80 (4)C21—C22—C23—C240.3 (10)
F4viii—F4—B2—F4vii69.9 (6)C22—C23—C24—C190.4 (10)
F3vii—F4—B2—F4vii129 (3)C20—C19—C24—C231.1 (9)
F3xi—F4—B2—F4vii156 (4)P2—C19—C24—C23178.4 (5)
Symmetry codes: (i) x+y+1, x+1, z; (ii) y+1, xy, z; (iii) y+1, xy+1, z; (iv) xy+2/3, x+1/3, z+1/3; (v) y1/3, x+y+1/3, z+1/3; (vi) x+y, x+1, z; (vii) y+1, xy+2, z; (viii) x+y1, x+1, z; (ix) xy+1, x+1, z; (x) y1, x+y, z; (xi) x, y+2, z; (xii) x+2/3, y+4/3, z+1/3.

Experimental details

Crystal data
Chemical formula[Ag(C18H15P)4]BF4
Mr1243.76
Crystal system, space groupTrigonal, R3
Temperature (K)298
a, c (Å)14.2445 (12), 51.591 (4)
V3)9065.7 (12)
Z6
Radiation typeMo Kα
µ (mm1)0.50
Crystal size (mm)0.30 × 0.18 × 0.15
Data collection
DiffractometerBruker SMART 1000 CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2007)
Tmin, Tmax0.866, 0.930
No. of measured, independent and
observed [I > 2σ(I)] reflections
15472, 3548, 2167
Rint0.092
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.063, 0.160, 1.07
No. of reflections3548
No. of parameters272
No. of restraints1
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.34, 0.52

Computer programs: SMART (Bruker, 2007), SAINT-Plus (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. 21171119), the National Keystone Basic Research Program (973 Program) under grant Nos. 2007CB310408 and 2006CB302901 and the Committee of Education of the Beijing Foundation of China (grant No. KM201210028020).

References

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