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In the title compound, [Ag{P(C6H5)}4][B{P(C6H5)}4]·CH3CN, the Ag ion resides on a crystallographic twofold rotation axis and is tetrahedrally coordinated. There is a disparity between the two independent Ag-P distances. This is due, in part, to the temperature differences (all previous determinations are at room temperature) but also to the packing effects of various anions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100015079/qa0442sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100015079/qa0442Isup2.hkl
Contains datablock I

CCDC reference: 156191

Comment top

In the title compound, (I), the Ag ion resides on a crystallographic twofold rotation axis and is tetrahedrally coordinated, with P—Ag—P angles ranging from 107.98 (7) to 111.02 (4)° [average 109.5 (13)°]. There is a disparity between the two independent Ag—P distances [2.6014 (13) and 2.6435 (14) Å], these values being somewhat shorter than those found in six related [Ag{P(C6H5)}4]+ cations in the Cambridge Structural Database (Version 5.18, April 2000; Allen & Kennard, 1993). This is, in part, due to the temperature differences (all previous determinations are at room temperature) but also the packing effects of various anions. The B atom in the tetraphenylborate anion and all the non-H atoms in the acetonitrile solvent molecule are also located on twofold axes. The geometric parameters associated with the [BPh4] anion are normal. The solvent appears to be disordered across the twofold axis, resulting in a shorter than expected C—C bond. Complex (I) is isomorphous with an Au analogue also measured at 150 K (Jones, 1980), but shows none of the 7:1 tetrahedral–trigonal disorder associated with the central Au atom in the latter complex. The Ag—P distances are longer than the Au—P distances observed in studies on isostructural Ag/Au phosphine complexes (Bowmaker et al., 1997). \scheme

Experimental top

The title compound was obtained while attempting to synthesize a silicate-based nitrogen pincer ligand coordinated to a platinum centre (Kleij et al., 1999). The counter-ion in the synthesis was tetraphenylborate, whilst the triphenylphosphine was added to complete the coordination around the platinum. The complex decomposed in the presence of silver trifluoromethanesulfonate to give the final product. Colourless block-like crystals were obtained by recrystallization from a solution in acetonitrile. The colour changed to orange on irradiation in the X-ray beam.

Refinement top

The acetonitrile molecule is possibly disordered over the twofold axis resulting in large displacement parameters and a shorter than expected C—C bond. The orientation of the solvent was chosen with respect to that found in the isostructural Au complex (Jones, 1980). The Rint value is indicative of the large number of weak data. All H atoms were constrained (C—H = 0.95 and 0.98 Å) and allowed to ride on their C atoms with Uiso(H) = 1.2Ueq(C). The methyl H atoms on the acetonitrile solvent are positionally disordered across the twofold axis.

Computing details top

Data collection: locally modified CAD-4 Software (Enraf-Nonius, 1989); cell refinement: SET4 (de Boer & Duisenberg, 1984); data reduction: HELENA (Spek, 1997); program(s) used to solve structure: DIRDIF (Beurksens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: PLATON (Spek, 2000).

(I) top
Crystal data top
[Ag(C18H15P)4](C24H20B)·C2H3NF(000) = 6320
Mr = 1517.21Dx = 1.311 Mg m3
Orthorhombic, IbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -I 2b 2cCell parameters from 22 reflections
a = 21.763 (2) Åθ = 11.6–13.6°
b = 22.955 (2) ŵ = 0.40 mm1
c = 30.767 (2) ÅT = 150 K
V = 15370 (2) Å3Block, colourless
Z = 80.30 × 0.30 × 0.30 mm
Data collection top
Enraf-Nonius CAD-4T
diffractometer
Rint = 0.103
Radiation source: rotating anodeθmax = 25°, θmin = 1.3°
Graphite monochromatorh = 525
ω scansk = 527
11437 measured reflectionsl = 3636
6511 independent reflections3 standard reflections every 60 min
3689 reflections with I > 2σ(I) intensity decay: 0.5%
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.058Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.140H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0514P)2]
where P = (Fo2 + 2Fc2)/3
6511 reflections(Δ/σ)max < 0.001
476 parametersΔρmax = 0.72 e Å3
0 restraintsΔρmin = 0.69 e Å3
Crystal data top
[Ag(C18H15P)4](C24H20B)·C2H3NV = 15370 (2) Å3
Mr = 1517.21Z = 8
Orthorhombic, IbcaMo Kα radiation
a = 21.763 (2) ŵ = 0.40 mm1
b = 22.955 (2) ÅT = 150 K
c = 30.767 (2) Å0.30 × 0.30 × 0.30 mm
Data collection top
Enraf-Nonius CAD-4T
diffractometer
Rint = 0.103
11437 measured reflections3 standard reflections every 60 min
6511 independent reflections intensity decay: 0.5%
3689 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.0580 restraints
wR(F2) = 0.140H-atom parameters constrained
S = 1.01Δρmax = 0.72 e Å3
6511 reflectionsΔρmin = 0.69 e Å3
476 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)
Ag10.00000.25000.06285 (2)0.01927 (14)
P10.06671 (6)0.31841 (6)0.11337 (5)0.0226 (3)
P20.06968 (6)0.31386 (6)0.01336 (5)0.0194 (3)
C10.1198 (2)0.3690 (2)0.08737 (18)0.0206 (12)
C20.1059 (3)0.3932 (3)0.0480 (2)0.0369 (16)
H20.06900.38220.03360.044*
C30.1447 (3)0.4339 (2)0.0283 (2)0.0400 (17)
H30.13390.45060.00100.048*
C40.1986 (3)0.4499 (3)0.0484 (2)0.0401 (17)
H40.22500.47800.03550.048*
C50.2137 (3)0.4247 (2)0.0873 (2)0.0303 (15)
H50.25170.43440.10070.036*
C60.1752 (2)0.3858 (2)0.1072 (2)0.0307 (14)
H610.18600.37000.13480.037*
C70.0240 (2)0.3658 (2)0.1504 (2)0.0274 (13)
C80.0367 (2)0.4246 (2)0.15618 (19)0.0270 (13)
H80.06850.44240.13970.032*
C90.0036 (3)0.4575 (2)0.1856 (2)0.0349 (13)
H90.01210.49790.18860.042*
C100.0416 (3)0.4321 (3)0.2104 (2)0.0364 (16)
H100.06360.45460.23110.044*
C110.0547 (3)0.3738 (3)0.2051 (2)0.0389 (16)
H110.08610.35630.22220.047*
C120.0229 (3)0.3409 (2)0.17552 (19)0.0326 (15)
H120.03280.30080.17200.039*
C130.1176 (2)0.2789 (2)0.15006 (19)0.0266 (13)
C140.1216 (3)0.2895 (2)0.19466 (19)0.0326 (14)
H140.09700.31900.20750.039*
C150.1615 (3)0.2572 (3)0.2202 (2)0.0420 (17)
H150.16380.26430.25050.050*
C160.1975 (3)0.2149 (3)0.2018 (2)0.0439 (19)
H160.22440.19260.21950.053*
C170.1950 (3)0.2045 (3)0.1581 (2)0.0404 (17)
H170.22070.17560.14550.049*
C180.1549 (2)0.2363 (2)0.1321 (2)0.0310 (16)
H180.15310.22870.10180.037*
C190.1205 (2)0.2777 (2)0.02543 (19)0.0209 (12)
C200.1535 (3)0.2288 (2)0.0117 (2)0.0303 (15)
H2010.14990.21540.01740.036*
C210.1912 (3)0.2002 (3)0.0406 (2)0.0379 (16)
H210.21320.16670.03130.045*
C220.1979 (3)0.2191 (3)0.0830 (2)0.0382 (16)
H220.22430.19930.10260.046*
C230.1655 (3)0.2674 (3)0.0961 (2)0.0435 (18)
H230.16960.28090.12520.052*
C240.1271 (2)0.2964 (2)0.06802 (19)0.0311 (13)
H240.10500.32960.07790.037*
C250.0291 (2)0.3661 (2)0.02123 (18)0.0237 (12)
C260.0191 (2)0.3454 (2)0.0467 (2)0.0280 (14)
H260.03000.30540.04530.034*
C270.0507 (3)0.3819 (3)0.0734 (2)0.0433 (17)
H270.08370.36710.09040.052*
C280.0353 (3)0.4398 (3)0.0762 (2)0.0477 (19)
H280.05760.46510.09480.057*
C290.0132 (3)0.4609 (3)0.0515 (2)0.047 (2)
H290.02460.50080.05360.056*
C300.0448 (3)0.4242 (2)0.0240 (2)0.0347 (15)
H300.07760.43900.00690.042*
C310.1218 (2)0.3606 (2)0.04394 (18)0.0232 (12)
C320.1839 (2)0.3644 (2)0.0365 (2)0.0352 (15)
H320.20180.34250.01360.042*
C330.2207 (3)0.3994 (3)0.0618 (2)0.0503 (19)
H330.26370.40110.05640.060*
C340.1954 (3)0.4320 (3)0.0949 (2)0.0437 (18)
H340.22080.45650.11200.052*
C350.1332 (3)0.4290 (2)0.1032 (2)0.0342 (15)
H350.11570.45150.12590.041*
C360.0967 (3)0.3931 (2)0.07824 (18)0.0241 (13)
H360.05400.39040.08430.029*
B10.2161 (4)0.00000.25000.0234 (19)
C370.1712 (2)0.0363 (2)0.21717 (18)0.0234 (13)
C380.1227 (2)0.0703 (2)0.23330 (19)0.0279 (13)
H380.11650.07200.26380.033*
C390.0830 (3)0.1019 (3)0.2061 (2)0.0353 (15)
H390.05110.12470.21850.042*
C400.0897 (3)0.1004 (3)0.1622 (2)0.0361 (16)
H400.06390.12300.14390.043*
C410.1348 (3)0.0652 (3)0.1447 (2)0.0429 (17)
H410.13860.06150.11410.051*
C420.1748 (3)0.0352 (3)0.17210 (18)0.0309 (14)
H420.20640.01260.15920.037*
C430.2614 (2)0.0445 (2)0.22240 (17)0.0221 (12)
C440.3144 (3)0.0240 (2)0.20171 (16)0.0247 (13)
H440.32290.01650.20290.030*
C450.3549 (2)0.0594 (3)0.17965 (19)0.0328 (14)
H450.39080.04320.16690.039*
C460.3434 (3)0.1188 (2)0.17599 (19)0.0336 (15)
H460.37100.14360.16070.040*
C470.2914 (3)0.1406 (2)0.19496 (18)0.0313 (14)
H470.28250.18100.19260.038*
C480.2511 (3)0.1044 (2)0.21769 (18)0.0268 (12)
H480.21540.12100.23040.032*
N2000.00000.25000.3637 (5)0.172 (8)
C1000.00000.25000.3285 (5)0.079 (4)
C3000.00000.25000.2850 (6)0.264 (16)
H3010.00760.28960.27440.396*0.50
H3020.04000.23650.27440.396*0.50
H3030.03240.22390.27440.396*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0199 (2)0.0211 (2)0.0168 (3)0.0021 (4)0.0000.000
P10.0234 (7)0.0224 (7)0.0221 (8)0.0009 (6)0.0045 (6)0.0016 (6)
P20.0178 (7)0.0194 (7)0.0212 (8)0.0016 (6)0.0019 (6)0.0015 (6)
C10.021 (3)0.017 (3)0.024 (3)0.000 (2)0.003 (2)0.007 (2)
C20.034 (4)0.039 (4)0.037 (4)0.006 (3)0.002 (3)0.001 (3)
C30.064 (5)0.030 (3)0.026 (4)0.005 (3)0.006 (3)0.004 (3)
C40.037 (4)0.035 (4)0.048 (4)0.010 (3)0.015 (3)0.005 (3)
C50.021 (3)0.029 (3)0.041 (4)0.004 (3)0.006 (3)0.010 (3)
C60.025 (3)0.034 (3)0.034 (4)0.005 (3)0.003 (3)0.005 (3)
C70.025 (3)0.028 (3)0.030 (4)0.000 (2)0.007 (3)0.008 (3)
C80.024 (3)0.030 (3)0.027 (3)0.000 (3)0.003 (3)0.000 (3)
C90.036 (3)0.025 (2)0.044 (3)0.002 (3)0.006 (4)0.010 (3)
C100.025 (3)0.048 (4)0.036 (4)0.002 (3)0.002 (3)0.010 (3)
C110.029 (3)0.046 (4)0.041 (4)0.008 (3)0.006 (3)0.003 (3)
C120.038 (3)0.029 (3)0.031 (4)0.007 (3)0.007 (3)0.007 (3)
C130.023 (3)0.031 (3)0.026 (3)0.008 (3)0.003 (3)0.007 (3)
C140.036 (3)0.028 (3)0.033 (4)0.003 (2)0.007 (3)0.002 (3)
C150.049 (4)0.048 (5)0.029 (3)0.020 (4)0.018 (3)0.010 (3)
C160.044 (4)0.035 (4)0.053 (5)0.006 (3)0.019 (3)0.023 (3)
C170.025 (3)0.029 (3)0.068 (5)0.005 (3)0.002 (3)0.001 (3)
C180.031 (3)0.035 (4)0.027 (4)0.000 (3)0.004 (3)0.004 (3)
C190.011 (3)0.015 (2)0.037 (4)0.003 (2)0.004 (2)0.001 (2)
C200.028 (3)0.025 (3)0.038 (4)0.004 (2)0.007 (3)0.007 (3)
C210.033 (3)0.035 (3)0.047 (4)0.010 (3)0.001 (3)0.010 (3)
C220.032 (4)0.043 (4)0.040 (4)0.001 (3)0.011 (3)0.011 (3)
C230.044 (4)0.055 (5)0.033 (4)0.007 (3)0.013 (3)0.003 (3)
C240.032 (3)0.031 (3)0.030 (4)0.005 (3)0.005 (3)0.002 (3)
C250.019 (3)0.028 (3)0.024 (3)0.004 (2)0.002 (2)0.003 (3)
C260.021 (3)0.029 (3)0.034 (4)0.006 (2)0.001 (2)0.003 (3)
C270.039 (4)0.060 (4)0.031 (4)0.001 (3)0.007 (3)0.006 (3)
C280.066 (5)0.040 (4)0.037 (4)0.020 (4)0.010 (4)0.012 (3)
C290.077 (7)0.024 (3)0.039 (4)0.006 (3)0.009 (3)0.005 (3)
C300.044 (4)0.030 (3)0.030 (4)0.002 (3)0.006 (3)0.001 (3)
C310.023 (3)0.023 (3)0.024 (3)0.000 (2)0.002 (2)0.001 (2)
C320.022 (3)0.038 (3)0.046 (4)0.005 (3)0.007 (3)0.015 (3)
C330.024 (3)0.055 (4)0.072 (6)0.008 (3)0.008 (4)0.024 (4)
C340.045 (4)0.034 (4)0.052 (5)0.014 (3)0.015 (4)0.016 (3)
C350.039 (4)0.034 (3)0.030 (4)0.004 (3)0.000 (3)0.010 (3)
C360.026 (3)0.021 (3)0.025 (3)0.001 (3)0.002 (2)0.001 (2)
B10.029 (5)0.019 (4)0.022 (5)0.0000.0000.004 (4)
C370.027 (3)0.022 (3)0.021 (3)0.006 (2)0.001 (2)0.002 (2)
C380.033 (3)0.030 (3)0.020 (3)0.004 (3)0.000 (3)0.002 (2)
C390.028 (3)0.038 (4)0.041 (4)0.004 (3)0.001 (3)0.001 (3)
C400.035 (4)0.038 (4)0.035 (4)0.006 (3)0.002 (3)0.011 (3)
C410.046 (4)0.060 (5)0.023 (4)0.005 (4)0.003 (3)0.010 (3)
C420.027 (3)0.038 (3)0.028 (3)0.006 (3)0.007 (3)0.007 (3)
C430.023 (3)0.025 (3)0.018 (3)0.002 (2)0.005 (2)0.006 (2)
C440.033 (3)0.023 (3)0.018 (3)0.000 (2)0.003 (2)0.004 (2)
C450.028 (3)0.044 (3)0.027 (4)0.001 (3)0.008 (3)0.005 (3)
C460.034 (3)0.037 (3)0.030 (4)0.014 (3)0.011 (3)0.003 (3)
C470.047 (3)0.026 (3)0.020 (3)0.002 (3)0.001 (3)0.005 (2)
C480.025 (3)0.032 (3)0.024 (3)0.001 (2)0.002 (3)0.005 (3)
N2000.28 (2)0.175 (14)0.065 (11)0.120 (16)0.0000.000
C1000.118 (10)0.060 (7)0.060 (9)0.039 (9)0.0000.000
C3000.59 (5)0.119 (14)0.088 (17)0.17 (2)0.0000.000
Geometric parameters (Å, º) top
Ag1—P2i2.6013 (13)C25—C301.378 (7)
Ag1—P22.6014 (13)C25—C261.393 (7)
Ag1—P1i2.6435 (14)C26—C271.360 (8)
Ag1—P12.6436 (14)C26—H260.9500
P1—C11.822 (5)C27—C281.373 (9)
P1—C131.823 (6)C27—H270.9500
P1—C71.829 (6)C28—C291.387 (9)
P2—C311.822 (5)C28—H280.9500
P2—C191.827 (5)C29—C301.380 (8)
P2—C251.830 (6)C29—H290.9500
C1—C21.368 (8)C30—H300.9500
C1—C61.405 (7)C31—C321.374 (7)
C2—C31.398 (8)C31—C361.403 (8)
C2—H20.9500C32—C331.374 (8)
C3—C41.376 (9)C32—H320.9500
C3—H30.9500C33—C341.378 (9)
C4—C51.367 (9)C33—H330.9500
C4—H40.9500C34—C351.378 (9)
C5—C61.372 (8)C34—H340.9500
C5—H50.9500C35—C361.377 (8)
C6—H610.9500C35—H350.9500
C7—C81.388 (7)C36—H360.9500
C7—C121.404 (7)B1—C371.633 (7)
C8—C91.380 (8)B1—C37ii1.633 (7)
C8—H80.9500B1—C43ii1.656 (7)
C9—C101.376 (9)B1—C431.656 (7)
C9—H90.9500C37—C421.389 (8)
C10—C111.377 (8)C37—C381.404 (7)
C10—H100.9500C38—C391.405 (8)
C11—C121.372 (8)C38—H380.9500
C11—H110.9500C39—C401.359 (8)
C12—H120.9500C39—H390.9500
C13—C181.385 (7)C40—C411.380 (8)
C13—C141.397 (8)C40—H400.9500
C14—C151.385 (8)C41—C421.393 (8)
C14—H140.9500C41—H410.9500
C15—C161.370 (9)C42—H420.9500
C15—H150.9500C43—C441.398 (7)
C16—C171.367 (9)C43—C481.400 (7)
C16—H160.9500C44—C451.378 (7)
C17—C181.390 (8)C44—H440.9500
C17—H170.9500C45—C461.390 (8)
C18—H180.9500C45—H450.9500
C19—C241.387 (8)C46—C471.369 (8)
C19—C201.397 (7)C46—H460.9500
C20—C211.379 (8)C47—C481.396 (7)
C20—H2010.9500C47—H470.9500
C21—C221.381 (9)C48—H480.9500
C21—H210.9500N200—C1001.083 (17)
C22—C231.374 (8)C100—C3001.34 (2)
C22—H220.9500C300—H3010.9800
C23—C241.374 (8)C300—H3020.9800
C23—H230.9500C300—H3030.9800
C24—H240.9500
P2i—Ag1—P2108.34 (6)C23—C24—H24119.7
P2i—Ag1—P1i109.24 (4)C19—C24—H24119.7
P2—Ag1—P1i111.02 (4)C30—C25—C26118.8 (5)
P2i—Ag1—P1111.02 (4)C30—C25—P2123.4 (4)
P2—Ag1—P1109.24 (4)C26—C25—P2117.8 (4)
P1i—Ag1—P1107.98 (7)C27—C26—C25120.7 (5)
C1—P1—C13101.7 (2)C27—C26—H26119.6
C1—P1—C7102.5 (2)C25—C26—H26119.6
C13—P1—C7102.6 (3)C26—C27—C28120.6 (6)
C1—P1—Ag1117.93 (18)C26—C27—H27119.7
C13—P1—Ag1113.70 (18)C28—C27—H27119.7
C7—P1—Ag1116.17 (18)C27—C28—C29119.4 (6)
C31—P2—C19103.2 (2)C27—C28—H28120.3
C31—P2—C25102.4 (2)C29—C28—H28120.3
C19—P2—C25102.1 (3)C30—C29—C28120.1 (6)
C31—P2—Ag1113.09 (18)C30—C29—H29120.0
C19—P2—Ag1118.64 (16)C28—C29—H29120.0
C25—P2—Ag1115.38 (18)C25—C30—C29120.4 (6)
C2—C1—C6117.6 (5)C25—C30—H30119.8
C2—C1—P1120.6 (4)C29—C30—H30119.8
C6—C1—P1121.8 (4)C32—C31—C36118.2 (5)
C1—C2—C3121.5 (6)C32—C31—P2124.4 (4)
C1—C2—H2119.2C36—C31—P2117.3 (4)
C3—C2—H2119.2C31—C32—C33121.1 (6)
C4—C3—C2119.8 (6)C31—C32—H32119.4
C4—C3—H3120.1C33—C32—H32119.4
C2—C3—H3120.1C32—C33—C34120.1 (6)
C5—C4—C3119.1 (6)C32—C33—H33119.9
C5—C4—H4120.4C34—C33—H33119.9
C3—C4—H4120.4C33—C34—C35120.1 (6)
C4—C5—C6121.3 (6)C33—C34—H34119.9
C4—C5—H5119.3C35—C34—H34119.9
C6—C5—H5119.3C36—C35—C34119.6 (6)
C5—C6—C1120.6 (6)C36—C35—H35120.2
C5—C6—H61119.7C34—C35—H35120.2
C1—C6—H61119.7C35—C36—C31120.8 (6)
C8—C7—C12118.1 (5)C35—C36—H36119.6
C8—C7—P1123.9 (5)C31—C36—H36119.6
C12—C7—P1118.0 (4)C37—B1—C37ii106.6 (6)
C9—C8—C7120.8 (5)C37—B1—C43ii111.0 (2)
C9—C8—H8119.6C37ii—B1—C43ii110.7 (3)
C7—C8—H8119.6C37—B1—C43110.7 (3)
C10—C9—C8120.3 (5)C37ii—B1—C43111.0 (2)
C10—C9—H9119.8C43ii—B1—C43106.8 (6)
C8—C9—H9119.8C42—C37—C38113.9 (5)
C9—C10—C11119.7 (6)C42—C37—B1125.1 (5)
C9—C10—H10120.2C38—C37—B1121.0 (5)
C11—C10—H10120.2C37—C38—C39122.6 (6)
C12—C11—C10120.6 (6)C37—C38—H38118.7
C12—C11—H11119.7C39—C38—H38118.7
C10—C11—H11119.7C40—C39—C38120.8 (6)
C11—C12—C7120.5 (5)C40—C39—H39119.6
C11—C12—H12119.7C38—C39—H39119.6
C7—C12—H12119.7C39—C40—C41118.7 (6)
C18—C13—C14118.5 (5)C39—C40—H40120.7
C18—C13—P1117.5 (5)C41—C40—H40120.7
C14—C13—P1124.0 (4)C40—C41—C42119.9 (6)
C15—C14—C13120.1 (6)C40—C41—H41120.1
C15—C14—H14119.9C42—C41—H41120.1
C13—C14—H14119.9C37—C42—C41124.0 (6)
C16—C15—C14120.3 (6)C37—C42—H42118.0
C16—C15—H15119.9C41—C42—H42118.0
C14—C15—H15119.9C44—C43—C48114.6 (5)
C17—C16—C15120.5 (6)C44—C43—B1121.2 (5)
C17—C16—H16119.7C48—C43—B1124.3 (4)
C15—C16—H16119.7C45—C44—C43123.6 (5)
C16—C17—C18119.8 (6)C45—C44—H44118.2
C16—C17—H17120.1C43—C44—H44118.2
C18—C17—H17120.1C44—C45—C46120.2 (5)
C13—C18—C17120.7 (6)C44—C45—H45119.9
C13—C18—H18119.6C46—C45—H45119.9
C17—C18—H18119.6C47—C46—C45118.2 (5)
C24—C19—C20118.8 (5)C47—C46—H46120.9
C24—C19—P2122.7 (4)C45—C46—H46120.9
C20—C19—P2118.6 (4)C46—C47—C48121.1 (5)
C21—C20—C19119.5 (6)C46—C47—H47119.5
C21—C20—H201120.2C48—C47—H47119.5
C19—C20—H201120.2C47—C48—C43122.4 (5)
C20—C21—C22121.5 (6)C47—C48—H48118.8
C20—C21—H21119.2C43—C48—H48118.8
C22—C21—H21119.2N200—C100—C300180.0
C23—C22—C21118.5 (6)C100—C300—H301109.5
C23—C22—H22120.7C100—C300—H302109.5
C21—C22—H22120.7H301—C300—H302109.5
C22—C23—C24121.2 (6)C100—C300—H303109.5
C22—C23—H23119.4H301—C300—H303109.5
C24—C23—H23119.4H302—C300—H303109.5
C23—C24—C19120.5 (5)
P2i—Ag1—P1—C158.1 (2)Ag1—P2—C19—C2043.5 (4)
P2—Ag1—P1—C161.3 (2)C24—C19—C20—C210.5 (8)
P1i—Ag1—P1—C1177.8 (2)P2—C19—C20—C21178.8 (5)
P2i—Ag1—P1—C1360.8 (2)C19—C20—C21—C220.8 (9)
P2—Ag1—P1—C13179.7 (2)C20—C21—C22—C230.5 (9)
P1i—Ag1—P1—C1358.9 (2)C21—C22—C23—C240.1 (9)
P2i—Ag1—P1—C7179.7 (2)C22—C23—C24—C190.3 (9)
P2—Ag1—P1—C760.9 (2)C20—C19—C24—C230.0 (8)
P1i—Ag1—P1—C759.9 (2)P2—C19—C24—C23179.3 (5)
P2i—Ag1—P2—C31179.4 (2)C31—P2—C25—C307.2 (6)
P1i—Ag1—P2—C3159.4 (2)C19—P2—C25—C3099.4 (5)
P1—Ag1—P2—C3159.5 (2)Ag1—P2—C25—C30130.5 (5)
P2i—Ag1—P2—C1958.4 (2)C31—P2—C25—C26174.3 (4)
P1i—Ag1—P2—C1961.6 (2)C19—P2—C25—C2679.0 (5)
P1—Ag1—P2—C19179.5 (2)Ag1—P2—C25—C2651.1 (5)
P2i—Ag1—P2—C2563.18 (19)C30—C25—C26—C270.8 (9)
P1i—Ag1—P2—C25176.86 (19)P2—C25—C26—C27179.3 (5)
P1—Ag1—P2—C2557.9 (2)C25—C26—C27—C280.6 (10)
C13—P1—C1—C2158.1 (5)C26—C27—C28—C290.3 (11)
C7—P1—C1—C296.0 (5)C27—C28—C29—C301.0 (11)
Ag1—P1—C1—C233.0 (6)C26—C25—C30—C290.1 (9)
C13—P1—C1—C623.8 (5)P2—C25—C30—C29178.5 (5)
C7—P1—C1—C682.1 (5)C28—C29—C30—C250.8 (11)
Ag1—P1—C1—C6148.9 (4)C19—P2—C31—C320.4 (6)
C6—C1—C2—C30.9 (9)C25—P2—C31—C32105.4 (5)
P1—C1—C2—C3177.3 (5)Ag1—P2—C31—C32129.8 (5)
C1—C2—C3—C40.7 (10)C19—P2—C31—C36177.4 (4)
C2—C3—C4—C51.0 (9)C25—P2—C31—C3676.8 (5)
C3—C4—C5—C62.6 (9)Ag1—P2—C31—C3648.0 (5)
C4—C5—C6—C12.4 (9)C36—C31—C32—C330.3 (9)
C2—C1—C6—C50.6 (8)P2—C31—C32—C33178.0 (5)
P1—C1—C6—C5178.8 (4)C31—C32—C33—C340.9 (11)
C1—P1—C7—C83.7 (6)C32—C33—C34—C351.0 (11)
C13—P1—C7—C8101.6 (5)C33—C34—C35—C360.2 (10)
Ag1—P1—C7—C8133.8 (4)C34—C35—C36—C311.4 (9)
C1—P1—C7—C12178.4 (5)C32—C31—C36—C351.5 (9)
C13—P1—C7—C1276.3 (5)P2—C31—C36—C35179.3 (4)
Ag1—P1—C7—C1248.4 (5)C37ii—B1—C37—C42127.5 (6)
C12—C7—C8—C90.5 (9)C43ii—B1—C37—C42111.8 (5)
P1—C7—C8—C9178.3 (5)C43—B1—C37—C426.6 (8)
C7—C8—C9—C101.6 (10)C37ii—B1—C37—C3849.7 (4)
C8—C9—C10—C111.6 (10)C43ii—B1—C37—C3871.0 (7)
C9—C10—C11—C120.4 (10)C43—B1—C37—C38170.6 (5)
C10—C11—C12—C70.7 (10)C42—C37—C38—C392.2 (8)
C8—C7—C12—C110.7 (9)B1—C37—C38—C39179.7 (5)
P1—C7—C12—C11177.3 (5)C37—C38—C39—C400.7 (9)
C1—P1—C13—C1877.3 (4)C38—C39—C40—C412.5 (10)
C7—P1—C13—C18176.8 (4)C39—C40—C41—C424.0 (10)
Ag1—P1—C13—C1850.5 (5)C38—C37—C42—C410.7 (9)
C1—P1—C13—C14101.8 (5)B1—C37—C42—C41178.0 (5)
C7—P1—C13—C144.0 (5)C40—C41—C42—C372.5 (10)
Ag1—P1—C13—C14130.3 (4)C37—B1—C43—C4479.6 (6)
C18—C13—C14—C151.1 (8)C37ii—B1—C43—C44162.1 (5)
P1—C13—C14—C15179.7 (4)C43ii—B1—C43—C4441.3 (4)
C13—C14—C15—C160.5 (9)C37—B1—C43—C48100.5 (5)
C14—C15—C16—C170.7 (10)C37ii—B1—C43—C4817.7 (7)
C15—C16—C17—C181.2 (10)C43ii—B1—C43—C48138.5 (6)
C14—C13—C18—C170.6 (8)C48—C43—C44—C452.3 (8)
P1—C13—C18—C17179.8 (4)B1—C43—C44—C45177.6 (5)
C16—C17—C18—C130.5 (9)C43—C44—C45—C461.8 (9)
C31—P2—C19—C2498.3 (5)C44—C45—C46—C470.3 (9)
C25—P2—C19—C247.7 (5)C45—C46—C47—C480.5 (9)
Ag1—P2—C19—C24135.8 (4)C46—C47—C48—C430.0 (9)
C31—P2—C19—C2082.4 (4)C44—C43—C48—C471.4 (8)
C25—P2—C19—C20171.6 (4)B1—C43—C48—C47178.5 (5)
Symmetry codes: (i) x, y+1/2, z; (ii) x, y, z+1/2.

Experimental details

Crystal data
Chemical formula[Ag(C18H15P)4](C24H20B)·C2H3N
Mr1517.21
Crystal system, space groupOrthorhombic, Ibca
Temperature (K)150
a, b, c (Å)21.763 (2), 22.955 (2), 30.767 (2)
V3)15370 (2)
Z8
Radiation typeMo Kα
µ (mm1)0.40
Crystal size (mm)0.30 × 0.30 × 0.30
Data collection
DiffractometerEnraf-Nonius CAD-4T
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
11437, 6511, 3689
Rint0.103
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.058, 0.140, 1.01
No. of reflections6511
No. of parameters476
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.72, 0.69

Computer programs: locally modified CAD-4 Software (Enraf-Nonius, 1989), SET4 (de Boer & Duisenberg, 1984), HELENA (Spek, 1997), DIRDIF (Beurksens et al., 1999), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2000).

Selected geometric parameters (Å, º) top
Ag1—P22.6014 (13)Ag1—P12.6436 (14)
P2i—Ag1—P2108.34 (6)P2—Ag1—P1109.24 (4)
P2i—Ag1—P1111.02 (4)P1i—Ag1—P1107.98 (7)
Symmetry code: (i) x, y+1/2, z.
 

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