trans-Di­iodo­bis­(tri­phenyl­phosphine)­palladium(II) bis­(tetra­hydro­furan) solvate

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.

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


 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

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Computing details

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

Crystal data

[PdI2(C18H15P)2]·2C4H8O	F(000) = 1016
Mr = 1028.95	Dx = 1.630 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 12.011 (3) Å	Cell parameters from 512 reflections
b = 20.234 (4) Å	θ = 12–20°
c = 8.625 (2) Å	µ = 2.03 mm^−1
β = 90.35 (1)°	T = 150 K
V = 2096.1 (8) Å^3	Block, orange
Z = 2	0.20 × 0.15 × 0.12 mm

Data collection

SMART 1K CCD area-detector diffractometer	4806 independent reflections
Radiation source: fine-focus sealed tube	4029 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.056
ω scans	θmax = 27.5°, θmin = 1.0°
Absorption correction: integration (XPREP SHELXTL; Siemens, 1995), Rint = 0.061 before correction	h = −11→16
Tmin = 0.709, Tmax = 0.795	k = −25→28
15358 measured reflections	l = −12→12

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.036	H-atom parameters constrained
wR(F^2) = 0.073	w = 1/[σ^2(Fo^2) + 5.8022P] where P = (Fo^2 + 2Fc^2)/3
S = 1.14	(Δ/σ)max = 0.002
4806 reflections	Δρmax = 0.64 e Å^−3
233 parameters	Δρmin = −0.52 e Å^−3
2 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0007 (1)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
I	0.59876 (2)	0.612148 (12)	0.44335 (3)	0.02307 (8)
Pd	0.5000	0.5000	0.5000	0.01538 (10)
P	0.64544 (9)	0.43845 (5)	0.39338 (12)	0.0175 (2)
C11	0.7618 (3)	0.48191 (19)	0.3002 (5)	0.0227 (9)
C12	0.8411 (4)	0.5116 (2)	0.3946 (6)	0.0292 (10)
H12	0.8365	0.5086	0.5043	0.035*
C13	0.9297 (4)	0.5464 (2)	0.3289 (7)	0.0389 (12)
H13	0.9837	0.5671	0.3936	0.047*
C14	0.9379 (4)	0.5519 (3)	0.1699 (7)	0.0421 (13)
H14	0.9988	0.5755	0.1269	0.050*
C15	0.8594 (4)	0.5223 (3)	0.0760 (7)	0.0420 (13)
H15	0.8662	0.5264	−0.0333	0.050*
C16	0.7715 (4)	0.4873 (2)	0.1405 (6)	0.0291 (10)
H16	0.7169	0.4679	0.0747	0.035*
C21	0.7204 (3)	0.3875 (2)	0.5338 (5)	0.0200 (8)
C22	0.8110 (3)	0.3485 (2)	0.4864 (5)	0.0225 (9)
H22	0.8295	0.3464	0.3796	0.027*
C23	0.8705 (4)	0.3115 (2)	0.5953 (5)	0.0269 (10)
H23	0.9320	0.2857	0.5621	0.032*
C24	0.8424 (4)	0.3143 (2)	0.7509 (6)	0.0298 (10)
H24	0.8824	0.2882	0.8239	0.036*
C25	0.7543 (4)	0.3537 (2)	0.8003 (5)	0.0302 (10)
H25	0.7356	0.3560	0.9070	0.036*
C26	0.6932 (4)	0.3901 (2)	0.6908 (5)	0.0246 (9)
H26	0.6328	0.4169	0.7235	0.029*
C31	0.5899 (3)	0.3863 (2)	0.2394 (5)	0.0197 (8)
C32	0.6119 (4)	0.31897 (19)	0.2232 (5)	0.0222 (9)
H32	0.6589	0.2974	0.2964	0.027*
C33	0.5657 (4)	0.2831 (2)	0.1016 (5)	0.0287 (10)
H33	0.5803	0.2371	0.0915	0.034*
C34	0.4968 (4)	0.3137 (2)	−0.0057 (5)	0.0309 (10)
H34	0.4655	0.2889	−0.0887	0.037*
C35	0.4727 (4)	0.3808 (2)	0.0095 (5)	0.0290 (10)
H35	0.4270	0.4020	−0.0658	0.035*
C36	0.5175 (4)	0.4165 (2)	0.1319 (5)	0.0248 (9)
H36	0.4980	0.4617	0.1449	0.030*
O1	0.0569 (4)	0.2825 (3)	0.2968 (6)	0.0811 (16)
C2A	0.1011 (8)	0.3458 (5)	0.2895 (13)	0.050 (3)*	0.60
H20A	0.1188	0.3631	0.3942	0.065*	0.60
H21A	0.0455	0.3755	0.2406	0.065*	0.60
C2B	0.0792 (11)	0.3437 (7)	0.220 (2)	0.060 (5)*	0.40
H20B	0.0558	0.3822	0.2831	0.078*	0.40
H21B	0.0388	0.3446	0.1199	0.078*	0.40
C3	0.2035 (5)	0.3432 (3)	0.1912 (8)	0.0529 (15)
H30	0.2502	0.3772	0.2426	0.069*
H31	0.2029	0.3515	0.0780	0.069*
C4	0.2456 (5)	0.2751 (3)	0.2353 (9)	0.0641 (19)
H40	0.2950	0.2754	0.3276	0.083*
H41	0.2868	0.2565	0.1463	0.083*
C5	0.1434 (6)	0.2357 (4)	0.2579 (10)	0.075 (2)
H50	0.1212	0.2105	0.1642	0.097*
H51	0.1556	0.2041	0.3440	0.097*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
I	0.02519 (15)	0.01400 (12)	0.03006 (16)	−0.00184 (11)	0.00310 (11)	0.00015 (11)
Pd	0.0174 (2)	0.01099 (18)	0.0177 (2)	0.00050 (16)	0.00067 (16)	−0.00094 (15)
P	0.0200 (5)	0.0133 (5)	0.0192 (5)	0.0010 (4)	0.0007 (4)	−0.0003 (4)
C11	0.021 (2)	0.0108 (17)	0.036 (3)	0.0037 (15)	0.0084 (18)	−0.0017 (16)
C12	0.026 (2)	0.022 (2)	0.040 (3)	−0.0021 (18)	−0.001 (2)	0.0013 (19)
C13	0.024 (3)	0.026 (2)	0.067 (4)	−0.0044 (19)	0.001 (2)	0.004 (2)
C14	0.035 (3)	0.033 (3)	0.059 (4)	−0.005 (2)	0.020 (3)	0.006 (3)
C15	0.046 (3)	0.035 (3)	0.046 (3)	0.000 (2)	0.021 (3)	0.006 (2)
C16	0.032 (3)	0.024 (2)	0.031 (2)	−0.0005 (18)	0.007 (2)	−0.0005 (19)
C21	0.0159 (19)	0.0176 (18)	0.027 (2)	−0.0051 (16)	−0.0037 (16)	−0.0012 (17)
C22	0.023 (2)	0.023 (2)	0.021 (2)	0.0014 (17)	−0.0014 (17)	−0.0019 (17)
C23	0.026 (2)	0.020 (2)	0.035 (3)	0.0041 (17)	−0.0024 (19)	−0.0040 (18)
C24	0.028 (2)	0.024 (2)	0.037 (3)	−0.0025 (19)	−0.010 (2)	0.0074 (19)
C25	0.037 (3)	0.031 (2)	0.023 (2)	−0.005 (2)	0.000 (2)	0.0055 (19)
C26	0.024 (2)	0.025 (2)	0.025 (2)	0.0002 (18)	−0.0017 (18)	−0.0032 (18)
C31	0.020 (2)	0.0174 (18)	0.022 (2)	−0.0018 (16)	0.0057 (16)	0.0030 (16)
C32	0.027 (2)	0.0167 (19)	0.023 (2)	0.0002 (17)	0.0034 (18)	−0.0016 (16)
C33	0.034 (3)	0.020 (2)	0.032 (2)	−0.0043 (18)	0.006 (2)	−0.0063 (18)
C34	0.030 (2)	0.035 (2)	0.027 (2)	−0.009 (2)	0.0020 (19)	−0.013 (2)
C35	0.025 (2)	0.041 (3)	0.020 (2)	0.0057 (19)	0.0017 (18)	−0.003 (2)
C36	0.029 (2)	0.021 (2)	0.024 (2)	0.0047 (17)	−0.0023 (18)	−0.0025 (17)
O1	0.069 (3)	0.069 (3)	0.105 (4)	−0.035 (3)	0.038 (3)	−0.024 (3)
C3	0.054 (4)	0.045 (3)	0.059 (4)	−0.007 (3)	0.003 (3)	0.004 (3)
C4	0.051 (4)	0.045 (4)	0.096 (5)	−0.004 (3)	−0.012 (4)	−0.001 (4)
C5	0.079 (5)	0.058 (5)	0.088 (6)	−0.019 (4)	−0.015 (4)	0.006 (4)

Geometric parameters (Å, º)

I—Pd	2.6081 (5)	C23—C24	1.387 (6)
Pd—P^i	2.3384 (11)	C24—C25	1.394 (7)
Pd—P	2.3384 (11)	C25—C26	1.401 (6)
Pd—I^i	2.6081 (5)	C31—C32	1.394 (5)
P—C31	1.820 (4)	C31—C36	1.408 (6)
P—C21	1.824 (4)	C32—C33	1.389 (6)
P—C11	1.840 (4)	C33—C34	1.385 (7)
C11—C12	1.387 (6)	C34—C35	1.393 (6)
C11—C16	1.387 (6)	C35—C36	1.386 (6)
C12—C13	1.399 (6)	O1—C2A	1.389 (10)
C13—C14	1.380 (8)	O1—C2B	1.429 (13)
C14—C15	1.376 (8)	O1—C5	1.446 (9)
C15—C16	1.391 (7)	C2A—C3	1.499 (10)
C21—C26	1.396 (6)	C2B—C3	1.516 (14)
C21—C22	1.408 (6)	C3—C4	1.516 (8)
C22—C23	1.395 (6)	C4—C5	1.478 (9)
P^i—Pd—P	180.0	C23—C22—C21	119.9 (4)
P^i—Pd—I	87.25 (3)	C24—C23—C22	120.2 (4)
P—Pd—I	92.75 (3)	C23—C24—C25	120.6 (4)
P^i—Pd—I^i	92.75 (3)	C24—C25—C26	119.4 (4)
P—Pd—I^i	87.25 (3)	C21—C26—C25	120.6 (4)
I—Pd—I^i	180.0	C32—C31—C36	118.4 (4)
C31—P—C21	109.51 (18)	C32—C31—P	124.8 (3)
C31—P—C11	103.56 (19)	C36—C31—P	116.8 (3)
C21—P—C11	100.76 (19)	C33—C32—C31	120.8 (4)
C31—P—Pd	108.96 (14)	C34—C33—C32	120.3 (4)
C21—P—Pd	114.00 (14)	C33—C34—C35	119.8 (4)
C11—P—Pd	119.24 (13)	C36—C35—C34	120.0 (4)
C12—C11—C16	119.2 (4)	C35—C36—C31	120.7 (4)
C12—C11—P	118.1 (3)	C2A—O1—C2B	26.7 (8)
C16—C11—P	122.7 (3)	C2A—O1—C5	108.6 (6)
C11—C12—C13	120.1 (5)	C2B—O1—C5	108.9 (7)
C14—C13—C12	120.2 (5)	O1—C2A—C3	108.0 (7)
C15—C14—C13	119.8 (5)	O1—C2B—C3	105.0 (9)
C14—C15—C16	120.3 (5)	C2A—C3—C4	99.4 (6)
C11—C16—C15	120.4 (5)	C2A—C3—C2B	25.0 (7)
C26—C21—C22	119.2 (4)	C4—C3—C2B	106.9 (7)
C26—C21—P	120.4 (3)	C5—C4—C3	104.3 (5)
C22—C21—P	120.2 (3)	O1—C5—C4	106.0 (6)

Symmetry code: (i) −x+1, −y+1, −z+1.