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The title compound, trans-[PdI2(PPh3)2]·2C4H8O, has a square-planar coordination of the Pd atom, which lies at an inversion centre. The crystal is isostructural with that of the CH2Cl2 solvate.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801007541/bt6043sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801007541/bt6043Isup2.hkl
Contains datablock I

CCDC reference: 170274

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.007 Å
  • Disorder in solvent or counterion
  • R factor = 0.036
  • wR factor = 0.073
  • Data-to-parameter ratio = 20.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 1 PLAT_302 Alert C Anion/Solvent Disorder ....................... 17.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: SHELXTL (Siemens, 1995); software used to prepare material for publication: SHELXTL.

trans-Diiodobis(triphenylphosphine)palladium(II) bis(tetrahydrofuran) solvate top
Crystal data top
[PdI2(C18H15P)2]·2C4H8OF(000) = 1016
Mr = 1028.95Dx = 1.630 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 12.011 (3) ÅCell parameters from 512 reflections
b = 20.234 (4) Åθ = 12–20°
c = 8.625 (2) ŵ = 2.03 mm1
β = 90.35 (1)°T = 150 K
V = 2096.1 (8) Å3Block, orange
Z = 20.20 × 0.15 × 0.12 mm
Data collection top
SMART 1K CCD area-detector
diffractometer
4806 independent reflections
Radiation source: fine-focus sealed tube4029 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.056
ω scansθmax = 27.5°, θmin = 1.0°
Absorption correction: integration
(XPREP SHELXTL; Siemens, 1995), Rint = 0.061 before correction
h = 1116
Tmin = 0.709, Tmax = 0.795k = 2528
15358 measured reflectionsl = 1212
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.073 w = 1/[σ2(Fo2) + 5.8022P]
where P = (Fo2 + 2Fc2)/3
S = 1.14(Δ/σ)max = 0.002
4806 reflectionsΔρmax = 0.64 e Å3
233 parametersΔρmin = 0.52 e Å3
2 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0007 (1)
Special details top

Experimental. The data collection nominally covered a hemisphere of reciprocal space, by a combination of 5 sets of ω scans; each set at different φ and/or 2θ angles and each scan (12 sec exposure) covering 0.3° in ω. Crystal to detector distance 4.51 cm. Crystal decay was monitored by repeating 50 initial frames at the end of data collection and comparing 286 duplicate reflections.

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 on F2 for ALL reflections except for 50 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_gt etc. and is not relevant to the choice of reflections for refinement.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
I0.59876 (2)0.612148 (12)0.44335 (3)0.02307 (8)
Pd0.50000.50000.50000.01538 (10)
P0.64544 (9)0.43845 (5)0.39338 (12)0.0175 (2)
C110.7618 (3)0.48191 (19)0.3002 (5)0.0227 (9)
C120.8411 (4)0.5116 (2)0.3946 (6)0.0292 (10)
H120.83650.50860.50430.035*
C130.9297 (4)0.5464 (2)0.3289 (7)0.0389 (12)
H130.98370.56710.39360.047*
C140.9379 (4)0.5519 (3)0.1699 (7)0.0421 (13)
H140.99880.57550.12690.050*
C150.8594 (4)0.5223 (3)0.0760 (7)0.0420 (13)
H150.86620.52640.03330.050*
C160.7715 (4)0.4873 (2)0.1405 (6)0.0291 (10)
H160.71690.46790.07470.035*
C210.7204 (3)0.3875 (2)0.5338 (5)0.0200 (8)
C220.8110 (3)0.3485 (2)0.4864 (5)0.0225 (9)
H220.82950.34640.37960.027*
C230.8705 (4)0.3115 (2)0.5953 (5)0.0269 (10)
H230.93200.28570.56210.032*
C240.8424 (4)0.3143 (2)0.7509 (6)0.0298 (10)
H240.88240.28820.82390.036*
C250.7543 (4)0.3537 (2)0.8003 (5)0.0302 (10)
H250.73560.35600.90700.036*
C260.6932 (4)0.3901 (2)0.6908 (5)0.0246 (9)
H260.63280.41690.72350.029*
C310.5899 (3)0.3863 (2)0.2394 (5)0.0197 (8)
C320.6119 (4)0.31897 (19)0.2232 (5)0.0222 (9)
H320.65890.29740.29640.027*
C330.5657 (4)0.2831 (2)0.1016 (5)0.0287 (10)
H330.58030.23710.09150.034*
C340.4968 (4)0.3137 (2)0.0057 (5)0.0309 (10)
H340.46550.28890.08870.037*
C350.4727 (4)0.3808 (2)0.0095 (5)0.0290 (10)
H350.42700.40200.06580.035*
C360.5175 (4)0.4165 (2)0.1319 (5)0.0248 (9)
H360.49800.46170.14490.030*
O10.0569 (4)0.2825 (3)0.2968 (6)0.0811 (16)
C2A0.1011 (8)0.3458 (5)0.2895 (13)0.050 (3)*0.60
H20A0.11880.36310.39420.065*0.60
H21A0.04550.37550.24060.065*0.60
C2B0.0792 (11)0.3437 (7)0.220 (2)0.060 (5)*0.40
H20B0.05580.38220.28310.078*0.40
H21B0.03880.34460.11990.078*0.40
C30.2035 (5)0.3432 (3)0.1912 (8)0.0529 (15)
H300.25020.37720.24260.069*
H310.20290.35150.07800.069*
C40.2456 (5)0.2751 (3)0.2353 (9)0.0641 (19)
H400.29500.27540.32760.083*
H410.28680.25650.14630.083*
C50.1434 (6)0.2357 (4)0.2579 (10)0.075 (2)
H500.12120.21050.16420.097*
H510.15560.20410.34400.097*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I0.02519 (15)0.01400 (12)0.03006 (16)0.00184 (11)0.00310 (11)0.00015 (11)
Pd0.0174 (2)0.01099 (18)0.0177 (2)0.00050 (16)0.00067 (16)0.00094 (15)
P0.0200 (5)0.0133 (5)0.0192 (5)0.0010 (4)0.0007 (4)0.0003 (4)
C110.021 (2)0.0108 (17)0.036 (3)0.0037 (15)0.0084 (18)0.0017 (16)
C120.026 (2)0.022 (2)0.040 (3)0.0021 (18)0.001 (2)0.0013 (19)
C130.024 (3)0.026 (2)0.067 (4)0.0044 (19)0.001 (2)0.004 (2)
C140.035 (3)0.033 (3)0.059 (4)0.005 (2)0.020 (3)0.006 (3)
C150.046 (3)0.035 (3)0.046 (3)0.000 (2)0.021 (3)0.006 (2)
C160.032 (3)0.024 (2)0.031 (2)0.0005 (18)0.007 (2)0.0005 (19)
C210.0159 (19)0.0176 (18)0.027 (2)0.0051 (16)0.0037 (16)0.0012 (17)
C220.023 (2)0.023 (2)0.021 (2)0.0014 (17)0.0014 (17)0.0019 (17)
C230.026 (2)0.020 (2)0.035 (3)0.0041 (17)0.0024 (19)0.0040 (18)
C240.028 (2)0.024 (2)0.037 (3)0.0025 (19)0.010 (2)0.0074 (19)
C250.037 (3)0.031 (2)0.023 (2)0.005 (2)0.000 (2)0.0055 (19)
C260.024 (2)0.025 (2)0.025 (2)0.0002 (18)0.0017 (18)0.0032 (18)
C310.020 (2)0.0174 (18)0.022 (2)0.0018 (16)0.0057 (16)0.0030 (16)
C320.027 (2)0.0167 (19)0.023 (2)0.0002 (17)0.0034 (18)0.0016 (16)
C330.034 (3)0.020 (2)0.032 (2)0.0043 (18)0.006 (2)0.0063 (18)
C340.030 (2)0.035 (2)0.027 (2)0.009 (2)0.0020 (19)0.013 (2)
C350.025 (2)0.041 (3)0.020 (2)0.0057 (19)0.0017 (18)0.003 (2)
C360.029 (2)0.021 (2)0.024 (2)0.0047 (17)0.0023 (18)0.0025 (17)
O10.069 (3)0.069 (3)0.105 (4)0.035 (3)0.038 (3)0.024 (3)
C30.054 (4)0.045 (3)0.059 (4)0.007 (3)0.003 (3)0.004 (3)
C40.051 (4)0.045 (4)0.096 (5)0.004 (3)0.012 (4)0.001 (4)
C50.079 (5)0.058 (5)0.088 (6)0.019 (4)0.015 (4)0.006 (4)
Geometric parameters (Å, º) top
I—Pd2.6081 (5)C23—C241.387 (6)
Pd—Pi2.3384 (11)C24—C251.394 (7)
Pd—P2.3384 (11)C25—C261.401 (6)
Pd—Ii2.6081 (5)C31—C321.394 (5)
P—C311.820 (4)C31—C361.408 (6)
P—C211.824 (4)C32—C331.389 (6)
P—C111.840 (4)C33—C341.385 (7)
C11—C121.387 (6)C34—C351.393 (6)
C11—C161.387 (6)C35—C361.386 (6)
C12—C131.399 (6)O1—C2A1.389 (10)
C13—C141.380 (8)O1—C2B1.429 (13)
C14—C151.376 (8)O1—C51.446 (9)
C15—C161.391 (7)C2A—C31.499 (10)
C21—C261.396 (6)C2B—C31.516 (14)
C21—C221.408 (6)C3—C41.516 (8)
C22—C231.395 (6)C4—C51.478 (9)
Pi—Pd—P180.0C23—C22—C21119.9 (4)
Pi—Pd—I87.25 (3)C24—C23—C22120.2 (4)
P—Pd—I92.75 (3)C23—C24—C25120.6 (4)
Pi—Pd—Ii92.75 (3)C24—C25—C26119.4 (4)
P—Pd—Ii87.25 (3)C21—C26—C25120.6 (4)
I—Pd—Ii180.0C32—C31—C36118.4 (4)
C31—P—C21109.51 (18)C32—C31—P124.8 (3)
C31—P—C11103.56 (19)C36—C31—P116.8 (3)
C21—P—C11100.76 (19)C33—C32—C31120.8 (4)
C31—P—Pd108.96 (14)C34—C33—C32120.3 (4)
C21—P—Pd114.00 (14)C33—C34—C35119.8 (4)
C11—P—Pd119.24 (13)C36—C35—C34120.0 (4)
C12—C11—C16119.2 (4)C35—C36—C31120.7 (4)
C12—C11—P118.1 (3)C2A—O1—C2B26.7 (8)
C16—C11—P122.7 (3)C2A—O1—C5108.6 (6)
C11—C12—C13120.1 (5)C2B—O1—C5108.9 (7)
C14—C13—C12120.2 (5)O1—C2A—C3108.0 (7)
C15—C14—C13119.8 (5)O1—C2B—C3105.0 (9)
C14—C15—C16120.3 (5)C2A—C3—C499.4 (6)
C11—C16—C15120.4 (5)C2A—C3—C2B25.0 (7)
C26—C21—C22119.2 (4)C4—C3—C2B106.9 (7)
C26—C21—P120.4 (3)C5—C4—C3104.3 (5)
C22—C21—P120.2 (3)O1—C5—C4106.0 (6)
Symmetry code: (i) x+1, y+1, z+1.
 

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