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The title compound, [Ag(AsC18H15)4]PF6, crystallizes with the cation on a threefold rotation axis and the anions on positions with site symmetry \overline3. The Ag atom is surrounded by four arsine ligands forming a distorted tetra­hedral configuration. The Ag—As distances are 2.6381 (6) and 2.6499 (9) Å, and the As—Ag—As angles are 108.91 (1) and 110.03 (1)°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806036373/hg2108sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806036373/hg2108Isup2.hkl
Contains datablock I

CCDC reference: 624722

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.032
  • wR factor = 0.072
  • Data-to-parameter ratio = 20.2

checkCIF/PLATON results

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Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.56 Ratio
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 28.25 From the CIF: _reflns_number_total 4969 From the CIF: _diffrn_reflns_limit_ max hkl 10. 17. 67. From the CIF: _diffrn_reflns_limit_ min hkl -17. -8. -67. TEST1: Expected hkl limits for theta max Calculated maximum hkl 19. 19. 68. Calculated minimum hkl -19. -19. -68.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus and XPREP (Bruker 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: SHELXL97.

Tetrakis(triphenylarsine)silver(I) hexafluorophosphate top
Crystal data top
[Ag(C18H15As)4]PF6Dx = 1.622 Mg m3
Mr = 1477.72Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3Cell parameters from 6298 reflections
Hall symbol: -R 3θ = 2.6–28.3°
a = 14.276 (5) ŵ = 2.59 mm1
c = 51.421 (5) ÅT = 100 K
V = 9076 (5) Å3Cuboid, colourless
Z = 60.43 × 0.32 × 0.22 mm
F(000) = 4440
Data collection top
Bruker X8 APEX-II 4K KappaCCD
diffractometer
4969 independent reflections
Graphite monochromator4358 reflections with I > 2σ(I)
Detector resolution: 512 pixels mm-1Rint = 0.021
ω and φ scansθmax = 28.3°, θmin = 1.2°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
h = 1710
Tmin = 0.379, Tmax = 0.565k = 817
12694 measured reflectionsl = 6767
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.032 w = 1/[σ2(Fo2) + (0.0232P)2 + 59.264P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.072(Δ/σ)max = 0.002
S = 1.05Δρmax = 2.53 e Å3
4969 reflectionsΔρmin = 1.9 e Å3
246 parameters
Special details top

Experimental. The intensity data was collected on a Bruker X8 Apex II 4 K Kappa CCD diffractometer using an exposure time of xx s/frame. A total of xxxx frames were collected with a frame width of 0.5° covering up to θ = 28.25° with 99.5% completeness accomplished.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
P10000.0155 (3)
F10.04155 (14)0.10501 (13)0.01799 (3)0.0279 (4)
P20.33330.66670.16670.0193 (3)
F20.32187 (16)0.56998 (15)0.14871 (3)0.0347 (4)
Ag0.66670.33330.086232 (6)0.01314 (6)
As10.52854 (2)0.39282 (2)0.102934 (4)0.01314 (6)
As20.66670.33330.034928 (8)0.01314 (6)
C110.5317 (2)0.5225 (2)0.08997 (5)0.0159 (5)
C120.4911 (2)0.5775 (2)0.10415 (5)0.0202 (5)
H120.46420.55440.12120.024*
C130.4899 (2)0.6660 (2)0.09339 (5)0.0236 (6)
H130.46230.70340.10320.028*
C140.5288 (2)0.6999 (2)0.06844 (5)0.0231 (6)
H140.52630.75940.0610.028*
C150.5712 (2)0.6469 (2)0.05441 (5)0.0239 (6)
H150.59970.67120.03750.029*
C160.5722 (2)0.5584 (2)0.06511 (5)0.0204 (5)
H160.60080.52190.05540.024*
C210.5203 (2)0.4091 (2)0.14013 (5)0.0181 (5)
C220.4239 (2)0.3861 (2)0.15219 (5)0.0274 (6)
H220.35870.35650.14240.033*
C230.4236 (3)0.4068 (3)0.17855 (6)0.0402 (8)
H230.35820.39250.18680.048*
C240.5179 (3)0.4480 (3)0.19283 (6)0.0398 (9)
H240.51710.46250.21080.048*
C250.6132 (3)0.4683 (3)0.18118 (6)0.0331 (7)
H250.67750.4950.19120.04*
C260.6147 (2)0.4495 (2)0.15466 (5)0.0243 (6)
H260.68040.46440.14650.029*
C310.3813 (2)0.2836 (2)0.09391 (5)0.0162 (5)
C320.3502 (2)0.1758 (2)0.09796 (5)0.0223 (5)
H320.39720.15780.10690.027*
C330.2510 (2)0.0941 (2)0.08906 (6)0.0268 (6)
H330.23050.02060.09190.032*
C340.1819 (2)0.1200 (2)0.07606 (6)0.0256 (6)
H340.11470.0640.06960.031*
C350.2107 (2)0.2271 (2)0.07246 (5)0.0243 (6)
H350.16260.24470.06390.029*
C360.3104 (2)0.3091 (2)0.08140 (5)0.0204 (5)
H360.330.38270.0790.025*
C410.5338 (2)0.2294 (2)0.01776 (5)0.0156 (5)
C420.4363 (2)0.2159 (2)0.02718 (5)0.0189 (5)
H420.43630.25780.04150.023*
C430.3394 (2)0.1415 (2)0.01568 (5)0.0229 (6)
H430.27290.13180.02230.027*
C440.3398 (2)0.0814 (2)0.00543 (6)0.0253 (6)
H440.27360.03150.01360.03*
C450.4361 (2)0.0937 (2)0.01469 (6)0.0269 (6)
H450.43580.05140.0290.032*
C460.5335 (2)0.1676 (2)0.00318 (5)0.0215 (5)
H460.59970.1760.00960.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P10.0137 (5)0.0137 (5)0.0191 (7)0.0068 (2)00
F10.0300 (9)0.0197 (8)0.0320 (9)0.0108 (7)0.0035 (7)0.0084 (7)
P20.0224 (5)0.0224 (5)0.0131 (7)0.0112 (3)00
F20.0430 (11)0.0333 (10)0.0293 (9)0.0202 (9)0.0011 (8)0.0105 (7)
Ag0.01311 (7)0.01311 (7)0.01319 (9)0.00656 (3)00
As10.01311 (7)0.01311 (7)0.01319 (9)0.00656 (3)00
As20.01311 (7)0.01311 (7)0.01319 (9)0.00656 (3)00
C110.0129 (11)0.0169 (12)0.0178 (11)0.0074 (10)0.0014 (9)0.0025 (9)
C120.0222 (13)0.0236 (14)0.0174 (11)0.0134 (12)0.0007 (10)0.0021 (10)
C130.0285 (15)0.0215 (14)0.0263 (13)0.0165 (12)0.0021 (11)0.0046 (11)
C140.0239 (14)0.0170 (13)0.0277 (13)0.0097 (11)0.0060 (11)0.0002 (10)
C150.0224 (14)0.0246 (14)0.0215 (12)0.0093 (12)0.0023 (10)0.0030 (10)
C160.0204 (13)0.0230 (14)0.0204 (12)0.0128 (11)0.0024 (10)0.0015 (10)
C210.0232 (13)0.0150 (12)0.0170 (11)0.0102 (11)0.0013 (10)0.0001 (9)
C220.0255 (15)0.0300 (16)0.0219 (13)0.0104 (13)0.0036 (11)0.0019 (11)
C230.045 (2)0.042 (2)0.0239 (15)0.0150 (17)0.0137 (14)0.0015 (13)
C240.061 (2)0.0285 (17)0.0162 (13)0.0117 (17)0.0014 (14)0.0016 (11)
C250.0431 (19)0.0239 (15)0.0240 (14)0.0105 (14)0.0133 (13)0.0027 (11)
C260.0271 (15)0.0216 (14)0.0244 (13)0.0123 (12)0.0060 (11)0.0013 (10)
C310.0146 (12)0.0187 (12)0.0142 (10)0.0075 (10)0.0009 (9)0.0032 (9)
C320.0191 (13)0.0208 (14)0.0277 (13)0.0105 (11)0.0003 (10)0.0017 (10)
C330.0239 (15)0.0169 (13)0.0353 (15)0.0070 (12)0.0006 (12)0.0016 (11)
C340.0150 (13)0.0238 (15)0.0291 (14)0.0031 (11)0.0017 (10)0.0054 (11)
C350.0162 (13)0.0288 (15)0.0267 (13)0.0104 (12)0.0038 (10)0.0007 (11)
C360.0175 (13)0.0182 (13)0.0249 (13)0.0084 (11)0.0015 (10)0.0010 (10)
C410.0162 (12)0.0149 (12)0.0154 (11)0.0076 (10)0.0005 (9)0.0028 (9)
C420.0201 (13)0.0200 (13)0.0186 (11)0.0116 (11)0.0012 (10)0.0016 (9)
C430.0178 (13)0.0232 (14)0.0294 (14)0.0116 (12)0.0019 (10)0.0045 (11)
C440.0191 (14)0.0191 (14)0.0328 (15)0.0058 (11)0.0076 (11)0.0024 (11)
C450.0265 (15)0.0262 (15)0.0275 (14)0.0127 (13)0.0059 (11)0.0103 (11)
C460.0185 (13)0.0236 (14)0.0210 (12)0.0095 (11)0.0005 (10)0.0045 (10)
Geometric parameters (Å, º) top
P1—F1i1.6018 (16)C21—C261.389 (4)
P1—F1ii1.6018 (16)C21—C221.391 (4)
P1—F11.6018 (16)C22—C231.388 (4)
P1—F1iii1.6018 (16)C22—H220.95
P1—F1iv1.6018 (16)C23—C241.381 (5)
P1—F1v1.6018 (16)C23—H230.95
P2—F2vi1.5995 (17)C24—C251.379 (5)
P2—F2vii1.5995 (18)C24—H240.95
P2—F21.5995 (17)C25—C261.392 (4)
P2—F2viii1.5995 (17)C25—H250.95
P2—F2ix1.5996 (18)C26—H260.95
P2—F2x1.5996 (17)C31—C321.387 (4)
Ag—As22.6381 (6)C31—C361.394 (4)
Ag—As1xi2.6499 (9)C32—C331.386 (4)
Ag—As1xii2.6499 (9)C32—H320.95
Ag—As12.6499 (9)C33—C341.386 (4)
As1—C211.937 (2)C33—H330.95
As1—C311.946 (3)C34—C351.383 (4)
As1—C111.947 (3)C34—H340.95
As2—C41xi1.941 (3)C35—C361.393 (4)
As2—C411.941 (3)C35—H350.95
As2—C41xii1.941 (3)C36—H360.95
C11—C161.391 (3)C41—C461.390 (3)
C11—C121.393 (4)C41—C421.393 (4)
C12—C131.387 (4)C42—C431.387 (4)
C12—H120.95C42—H420.95
C13—C141.386 (4)C43—C441.386 (4)
C13—H130.95C43—H430.95
C14—C151.385 (4)C44—C451.381 (4)
C14—H140.95C44—H440.95
C15—C161.384 (4)C45—C461.389 (4)
C15—H150.95C45—H450.95
C16—H160.95C46—H460.95
F1i—P1—F1ii89.99 (9)C16—C15—C14119.9 (3)
F1i—P1—F1180.00 (16)C16—C15—H15120.1
F1ii—P1—F190.01 (9)C14—C15—H15120.1
F1i—P1—F1iii89.99 (9)C15—C16—C11120.7 (2)
F1ii—P1—F1iii89.99 (9)C15—C16—H16119.7
F1—P1—F1iii90.01 (9)C11—C16—H16119.7
F1i—P1—F1iv90.01 (9)C26—C21—C22119.9 (2)
F1ii—P1—F1iv180.00 (14)C26—C21—As1118.4 (2)
F1—P1—F1iv89.99 (9)C22—C21—As1121.6 (2)
F1iii—P1—F1iv90.01 (9)C23—C22—C21119.6 (3)
F1i—P1—F1v90.01 (9)C23—C22—H22120.2
F1ii—P1—F1v90.01 (9)C21—C22—H22120.2
F1—P1—F1v89.99 (9)C24—C23—C22120.3 (3)
F1iii—P1—F1v180.0 (2)C24—C23—H23119.9
F1iv—P1—F1v89.99 (9)C22—C23—H23119.9
F2vi—P2—F2vii90.02 (10)C25—C24—C23120.5 (3)
F2vi—P2—F290.02 (10)C25—C24—H24119.7
F2vii—P2—F290.02 (10)C23—C24—H24119.7
F2vi—P2—F2viii179.9950 (10)C24—C25—C26119.6 (3)
F2vii—P2—F2viii89.99 (10)C24—C25—H25120.2
F2—P2—F2viii89.99 (10)C26—C25—H25120.2
F2vi—P2—F2ix89.99 (10)C21—C26—C25120.1 (3)
F2vii—P2—F2ix180.00 (13)C21—C26—H26119.9
F2—P2—F2ix89.99 (10)C25—C26—H26119.9
F2viii—P2—F2ix90.01 (10)C32—C31—C36119.2 (2)
F2vi—P2—F2x89.99 (10)C32—C31—As1118.2 (2)
F2vii—P2—F2x89.99 (10)C36—C31—As1122.4 (2)
F2—P2—F2x180.00 (15)C33—C32—C31120.6 (3)
F2viii—P2—F2x90.01 (10)C33—C32—H32119.7
F2ix—P2—F2x90.01 (10)C31—C32—H32119.7
As2—Ag—As1xi108.911 (10)C34—C33—C32119.9 (3)
As2—Ag—As1xii108.911 (10)C34—C33—H33120
As1xi—Ag—As1xii110.026 (10)C32—C33—H33120
As2—Ag—As1108.911 (10)C35—C34—C33120.1 (3)
As1xi—Ag—As1110.026 (10)C35—C34—H34120
As1xii—Ag—As1110.026 (10)C33—C34—H34120
C21—As1—C31103.03 (11)C34—C35—C36120.0 (3)
C21—As1—C11101.42 (10)C34—C35—H35120
C31—As1—C11100.55 (11)C36—C35—H35120
C21—As1—Ag117.25 (8)C35—C36—C31120.2 (3)
C31—As1—Ag110.14 (7)C35—C36—H36119.9
C11—As1—Ag121.77 (7)C31—C36—H36119.9
C41xi—As2—C41100.93 (9)C46—C41—C42119.7 (2)
C41xi—As2—C41xii100.93 (9)C46—C41—As2121.94 (19)
C41—As2—C41xii100.93 (9)C42—C41—As2118.33 (19)
C41xi—As2—Ag117.06 (7)C43—C42—C41120.2 (2)
C41—As2—Ag117.06 (7)C43—C42—H42119.9
C41xii—As2—Ag117.06 (7)C41—C42—H42119.9
C16—C11—C12119.1 (2)C44—C43—C42119.8 (3)
C16—C11—As1118.24 (19)C44—C43—H43120.1
C12—C11—As1122.59 (19)C42—C43—H43120.1
C13—C12—C11120.2 (2)C45—C44—C43120.3 (3)
C13—C12—H12119.9C45—C44—H44119.9
C11—C12—H12119.9C43—C44—H44119.9
C14—C13—C12120.1 (3)C44—C45—C46120.3 (3)
C14—C13—H13119.9C44—C45—H45119.9
C12—C13—H13119.9C46—C45—H45119.9
C15—C14—C13120.0 (3)C45—C46—C41119.8 (3)
C15—C14—H14120C45—C46—H46120.1
C13—C14—H14120C41—C46—H46120.1
As2—Ag—As1—C21175.89 (9)Ag—As1—C21—C22147.1 (2)
As1xi—Ag—As1—C2164.80 (9)C26—C21—C22—C231.8 (4)
As1xii—Ag—As1—C2156.58 (9)As1—C21—C22—C23175.1 (2)
As2—Ag—As1—C3166.79 (8)C21—C22—C23—C241.2 (5)
As1xi—Ag—As1—C3152.52 (8)C22—C23—C24—C250.5 (5)
As1xii—Ag—As1—C31173.90 (8)C23—C24—C25—C261.5 (5)
As2—Ag—As1—C1150.37 (9)C22—C21—C26—C250.8 (4)
As1xi—Ag—As1—C11169.68 (8)As1—C21—C26—C25176.2 (2)
As1xii—Ag—As1—C1168.94 (9)C24—C25—C26—C210.9 (5)
As1xi—Ag—As2—C41xi65.12 (8)C21—As1—C31—C3281.5 (2)
As1xii—Ag—As2—C41xi54.88 (8)C11—As1—C31—C32174.0 (2)
As1—Ag—As2—C41xi174.88 (8)Ag—As1—C31—C3244.3 (2)
As1xi—Ag—As2—C4154.88 (8)C21—As1—C31—C36104.6 (2)
As1xii—Ag—As2—C41174.88 (8)C11—As1—C31—C360.2 (2)
As1—Ag—As2—C4165.12 (8)Ag—As1—C31—C36129.51 (19)
As1xi—Ag—As2—C41xii174.88 (8)C36—C31—C32—C331.8 (4)
As1xii—Ag—As2—C41xii65.12 (8)As1—C31—C32—C33172.2 (2)
As1—Ag—As2—C41xii54.88 (8)C31—C32—C33—C340.2 (4)
C21—As1—C11—C16159.4 (2)C32—C33—C34—C351.4 (4)
C31—As1—C11—C1694.8 (2)C33—C34—C35—C361.5 (4)
Ag—As1—C11—C1627.0 (2)C34—C35—C36—C310.2 (4)
C21—As1—C11—C1223.3 (2)C32—C31—C36—C351.8 (4)
C31—As1—C11—C1282.4 (2)As1—C31—C36—C35172.0 (2)
Ag—As1—C11—C12155.75 (18)C41xi—As2—C41—C466.7 (2)
C16—C11—C12—C130.8 (4)C41xii—As2—C41—C4696.81 (17)
As1—C11—C12—C13176.4 (2)Ag—As2—C41—C46134.95 (19)
C11—C12—C13—C140.2 (4)C41xi—As2—C41—C42172.3 (2)
C12—C13—C14—C151.5 (4)C41xii—As2—C41—C4284.2 (3)
C13—C14—C15—C161.7 (4)Ag—As2—C41—C4244.0 (2)
C14—C15—C16—C110.6 (4)C46—C41—C42—C430.2 (4)
C12—C11—C16—C150.7 (4)As2—C41—C42—C43179.2 (2)
As1—C11—C16—C15176.7 (2)C41—C42—C43—C440.7 (4)
C31—As1—C21—C26157.0 (2)C42—C43—C44—C451.4 (4)
C11—As1—C21—C2699.2 (2)C43—C44—C45—C461.0 (5)
Ag—As1—C21—C2635.9 (2)C44—C45—C46—C410.1 (4)
C31—As1—C21—C2226.0 (3)C42—C41—C46—C450.5 (4)
C11—As1—C21—C2277.8 (2)As2—C41—C46—C45179.5 (2)
Symmetry codes: (i) x, y, z; (ii) xy, x, z; (iii) y, x+y, z; (iv) x+y, x, z; (v) y, xy, z; (vi) x+y, x+1, z; (vii) y+1, xy+1, z; (viii) xy+2/3, x+1/3, z+1/3; (ix) y1/3, x+y+1/3, z+1/3; (x) x+2/3, y+4/3, z+1/3; (xi) y+1, xy, z; (xii) x+y+1, x+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C13—H13···F2vii0.952.553.373 (3)145
Symmetry code: (vii) y+1, xy+1, z.
Comparative geometrical parameters for selected [Ag(AsPh3)4]X complexes. top
XAg—As (Å)Ag—As (Å)Ag—As (Å)Ag—As (Å)Notes
NO32.6502.649--(i)
ClO42.6802.652--(i)
PF62.6381 (6)2.6499 (9)--TW
BF42.6451 (10)2.6578 (5)--(ii)
BrO32.655 (1)2.637 (1)2.659 (1)2.644 (1)(iii)
Notes: TW is this work; (i) Bowmaker et al. (1997), extracted from CSD; (ii) Tripathi et al. (1997); (iii) Cingolani et al. (2003).
 

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