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The title compound, [Pd2(C4H3OSe)4(C18H15P)2], crystallizes as a centrocymmetric furan-2-seleno­late-bridged dinuclear palladium complex. The Pd atom shows a slightly distorted square-planar coordination geometry, with bridging Pd—Se distances of 2.4568 (8) and 2.4729 (8) Å, and a terminal Pd—Se distance of 2.4623 (8) Å. Terminal seleno­late ligands are in trans positions with respect to each other.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805031247/rz6122sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805031247/rz6122Isup2.hkl
Contains datablock I

CCDC reference: 289875

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.042
  • wR factor = 0.102
  • Data-to-parameter ratio = 16.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.36 Ratio
Author Response: High Ueq(max)/Ueq(min) ratio is observed because of the positional disorder in the furyl ring.
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Pd1    -   Se2     ..       7.24 su
Author Response: This is due to the empirical multi-scan absorption correction.
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C13
Author Response: There is positional disorder in the furyl ring
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C12
Author Response: There is positional disorder in the furyl ring
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9

0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXL97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).

Di-µ-furan-2-selenolato-bis[(furan-2-selenolato)(triphenylphosphine)palladium] top
Crystal data top
[Pd2(C4H3OSe)4(C18H15P)2]F(000) = 1288
Mr = 1321.44Dx = 1.795 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3924 reflections
a = 13.045 (3) Åθ = 3.1–26.0°
b = 16.394 (3) ŵ = 3.82 mm1
c = 12.233 (2) ÅT = 120 K
β = 110.85 (3)°Plate, orange
V = 2444.8 (10) Å30.15 × 0.10 × 0.08 mm
Z = 2
Data collection top
Bruker–Nonius KappaCCD
diffractometer
4701 independent reflections
Radiation source: fine-focus sealed tube3924 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
φ scans, and ω scans with κ offsetsθmax = 26.0°, θmin = 3.1°
Absorption correction: multi-scan
(SHELXTL; Bruker, 2001)
h = 1615
Tmin = 0.638, Tmax = 0.737k = 1920
17303 measured reflectionsl = 1515
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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.102H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0378P)2 + 10.5236P]
where P = (Fo2 + 2Fc2)/3
4701 reflections(Δ/σ)max < 0.001
290 parametersΔρmax = 1.75 e Å3
0 restraintsΔρmin = 0.93 e Å3
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*/Ueq
Pd10.37476 (3)0.00294 (2)0.36834 (3)0.02079 (11)
Se20.45340 (4)0.07504 (3)0.55752 (4)0.02376 (13)
Se10.21198 (4)0.09146 (3)0.29532 (4)0.02807 (14)
P10.29905 (10)0.07365 (7)0.20388 (10)0.0217 (3)
C110.1765 (4)0.1128 (3)0.4285 (5)0.0318 (11)
C120.1147 (4)0.0644 (4)0.4719 (5)0.0349 (12)
H120.08460.01270.44270.042*
C130.1045 (7)0.1051 (7)0.5662 (7)0.073 (3)
H130.06560.08630.61390.087*
C140.1582 (7)0.1746 (7)0.5785 (6)0.079 (3)
H140.16400.21390.63740.095*
O10.2066 (4)0.1824 (3)0.4911 (5)0.0640 (14)
C1110.2031 (4)0.1458 (3)0.2282 (4)0.0237 (10)
C1120.1771 (4)0.1401 (3)0.3291 (4)0.0274 (11)
H1120.20700.09710.38320.033*
C1130.1081 (4)0.1967 (3)0.3507 (5)0.0354 (12)
H1130.09150.19250.42010.043*
C1140.0629 (4)0.2593 (3)0.2727 (5)0.0368 (13)
H1140.01570.29800.28840.044*
C1150.0868 (5)0.2650 (4)0.1716 (5)0.0414 (14)
H1150.05480.30730.11700.050*
C1160.1569 (4)0.2096 (3)0.1494 (5)0.0329 (12)
H1160.17390.21470.08040.040*
C1210.3893 (4)0.1391 (3)0.1582 (4)0.0269 (10)
C1220.4389 (4)0.2060 (3)0.2272 (5)0.0338 (12)
H1220.42170.21900.29450.041*
C1230.5133 (5)0.2537 (3)0.1982 (6)0.0418 (14)
H1230.54710.29880.24620.050*
C1240.5388 (5)0.2367 (4)0.1010 (6)0.0477 (16)
H1240.58950.27000.08170.057*
C1250.4900 (5)0.1705 (4)0.0308 (5)0.0431 (14)
H1250.50730.15840.03660.052*
C1260.4153 (4)0.1216 (3)0.0596 (5)0.0332 (12)
H1260.38220.07620.01180.040*
C1310.2271 (4)0.0136 (3)0.0740 (4)0.0269 (10)
C1320.1266 (4)0.0355 (4)0.0086 (5)0.0345 (12)
H1320.09210.08500.00060.041*
C1330.0769 (5)0.0159 (4)0.1033 (5)0.0483 (16)
H1330.00770.00140.15940.058*
C1340.1261 (6)0.0868 (4)0.1168 (6)0.0506 (17)
H1340.09050.12160.18130.061*
C1350.2271 (6)0.1078 (4)0.0371 (6)0.0494 (16)
H1350.26250.15630.04740.059*
C1360.2773 (5)0.0576 (3)0.0590 (5)0.0391 (13)
H1360.34660.07230.11460.047*
C210.3819 (4)0.0153 (3)0.6427 (5)0.0311 (11)
C220.3483 (5)0.0328 (4)0.7298 (5)0.0455 (15)
H220.35670.08370.76910.055*
C230.2966 (6)0.0392 (5)0.7546 (6)0.0547 (17)
H230.26350.04460.81200.066*
C240.3044 (6)0.0958 (4)0.6819 (7)0.061 (2)
H240.27780.15000.67930.073*
O20.3563 (4)0.0660 (2)0.6098 (4)0.0459 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.01984 (19)0.02059 (19)0.01961 (19)0.00004 (13)0.00418 (15)0.00194 (13)
Se20.0230 (2)0.0220 (2)0.0226 (3)0.00181 (18)0.0036 (2)0.00239 (18)
Se10.0258 (3)0.0282 (3)0.0277 (3)0.00639 (19)0.0065 (2)0.0014 (2)
P10.0198 (6)0.0231 (6)0.0195 (6)0.0013 (5)0.0038 (5)0.0020 (5)
C110.027 (3)0.029 (3)0.038 (3)0.009 (2)0.011 (2)0.001 (2)
C120.031 (3)0.041 (3)0.038 (3)0.008 (2)0.019 (2)0.009 (2)
C130.055 (5)0.117 (8)0.055 (5)0.040 (5)0.030 (4)0.028 (5)
C140.068 (5)0.116 (8)0.042 (4)0.058 (5)0.003 (4)0.026 (5)
O10.054 (3)0.056 (3)0.075 (4)0.010 (2)0.015 (3)0.021 (3)
C1110.022 (2)0.025 (2)0.020 (2)0.0014 (19)0.0022 (19)0.0016 (19)
C1120.028 (3)0.026 (3)0.025 (3)0.003 (2)0.006 (2)0.000 (2)
C1130.033 (3)0.039 (3)0.036 (3)0.008 (2)0.014 (2)0.011 (2)
C1140.029 (3)0.031 (3)0.053 (4)0.001 (2)0.017 (3)0.009 (3)
C1150.038 (3)0.035 (3)0.048 (4)0.016 (2)0.010 (3)0.010 (3)
C1160.035 (3)0.034 (3)0.029 (3)0.008 (2)0.010 (2)0.008 (2)
C1210.023 (2)0.025 (2)0.026 (3)0.0018 (19)0.001 (2)0.010 (2)
C1220.037 (3)0.025 (3)0.038 (3)0.003 (2)0.011 (2)0.007 (2)
C1230.040 (3)0.027 (3)0.053 (4)0.007 (2)0.010 (3)0.003 (3)
C1240.037 (3)0.041 (3)0.064 (4)0.004 (3)0.017 (3)0.023 (3)
C1250.039 (3)0.056 (4)0.039 (3)0.001 (3)0.020 (3)0.011 (3)
C1260.030 (3)0.039 (3)0.029 (3)0.000 (2)0.008 (2)0.005 (2)
C1310.028 (3)0.032 (3)0.022 (2)0.002 (2)0.011 (2)0.000 (2)
C1320.029 (3)0.046 (3)0.030 (3)0.002 (2)0.012 (2)0.001 (2)
C1330.031 (3)0.076 (5)0.031 (3)0.015 (3)0.001 (3)0.012 (3)
C1340.053 (4)0.063 (4)0.037 (3)0.027 (3)0.018 (3)0.024 (3)
C1350.062 (4)0.043 (4)0.043 (4)0.001 (3)0.019 (3)0.016 (3)
C1360.041 (3)0.037 (3)0.037 (3)0.004 (3)0.011 (3)0.006 (2)
C210.024 (2)0.041 (3)0.025 (3)0.001 (2)0.005 (2)0.004 (2)
C220.044 (3)0.050 (4)0.042 (4)0.009 (3)0.015 (3)0.008 (3)
C230.056 (4)0.072 (5)0.037 (3)0.008 (4)0.020 (3)0.014 (3)
C240.066 (5)0.043 (4)0.092 (6)0.002 (3)0.049 (4)0.017 (4)
O20.057 (3)0.032 (2)0.061 (3)0.0012 (19)0.035 (2)0.0005 (19)
Geometric parameters (Å, º) top
Pd1—P12.2771 (13)C121—C1221.395 (7)
Pd1—Se2i2.4568 (8)C122—C1231.387 (8)
Pd1—Se12.4623 (8)C122—H1220.9500
Pd1—Se22.4729 (8)C123—C1241.372 (9)
Se2—C211.900 (5)C123—H1230.9500
Se2—Pd1i2.4568 (8)C124—C1251.389 (9)
Se1—C111.877 (5)C124—H1240.9500
P1—C1311.820 (5)C125—C1261.400 (8)
P1—C1111.822 (5)C125—H1250.9500
P1—C1211.822 (5)C126—H1260.9500
C11—O11.352 (7)C131—C1361.381 (7)
C11—C121.366 (7)C131—C1321.388 (7)
C12—C131.380 (10)C132—C1331.392 (8)
C12—H120.9500C132—H1320.9500
C13—C141.318 (13)C133—C1341.366 (9)
C13—H130.9500C133—H1330.9500
C14—O11.428 (10)C134—C1351.376 (10)
C14—H140.9500C134—H1340.9500
C111—C1121.395 (7)C135—C1361.393 (8)
C111—C1161.404 (7)C135—H1350.9500
C112—C1131.383 (7)C136—H1360.9500
C112—H1120.9500C21—C221.319 (8)
C113—C1141.382 (8)C21—O21.397 (7)
C113—H1130.9500C22—C231.445 (10)
C114—C1151.382 (8)C22—H220.9500
C114—H1140.9500C23—C241.315 (10)
C115—C1161.383 (7)C23—H230.9500
C115—H1150.9500C24—O21.379 (8)
C116—H1160.9500C24—H240.9500
C121—C1261.394 (7)
P1—Pd1—Se2i95.23 (4)C126—C121—P1121.8 (4)
P1—Pd1—Se187.57 (4)C122—C121—P1119.2 (4)
Se2i—Pd1—Se1175.18 (2)C123—C122—C121120.3 (5)
P1—Pd1—Se2174.50 (4)C123—C122—H122119.9
Se2i—Pd1—Se283.28 (3)C121—C122—H122119.9
Se1—Pd1—Se294.29 (3)C124—C123—C122121.0 (5)
C21—Se2—Pd1i95.21 (16)C124—C123—H123119.5
C21—Se2—Pd198.37 (16)C122—C123—H123119.5
Pd1i—Se2—Pd196.72 (3)C123—C124—C125119.7 (5)
C11—Se1—Pd1104.01 (16)C123—C124—H124120.2
C131—P1—C111108.8 (2)C125—C124—H124120.2
C131—P1—C121103.9 (2)C124—C125—C126119.9 (6)
C111—P1—C121102.9 (2)C124—C125—H125120.0
C131—P1—Pd1113.55 (17)C126—C125—H125120.0
C111—P1—Pd1108.73 (16)C121—C126—C125120.3 (5)
C121—P1—Pd1118.14 (16)C121—C126—H126119.8
O1—C11—C12111.2 (5)C125—C126—H126119.8
O1—C11—Se1122.5 (4)C136—C131—C132119.4 (5)
C12—C11—Se1126.2 (4)C136—C131—P1116.8 (4)
C11—C12—C13106.9 (6)C132—C131—P1123.8 (4)
C11—C12—H12126.5C131—C132—C133119.3 (6)
C13—C12—H12126.5C131—C132—H132120.4
C14—C13—C12107.9 (7)C133—C132—H132120.4
C14—C13—H13126.1C134—C133—C132121.1 (6)
C12—C13—H13126.1C134—C133—H133119.5
C13—C14—O1110.6 (6)C132—C133—H133119.5
C13—C14—H14124.7C133—C134—C135120.0 (6)
O1—C14—H14124.7C133—C134—H134120.0
C11—O1—C14103.4 (6)C135—C134—H134120.0
C112—C111—C116118.5 (4)C134—C135—C136119.6 (6)
C112—C111—P1119.9 (4)C134—C135—H135120.2
C116—C111—P1121.6 (4)C136—C135—H135120.2
C113—C112—C111120.3 (5)C131—C136—C135120.6 (6)
C113—C112—H112119.9C131—C136—H136119.7
C111—C112—H112119.9C135—C136—H136119.7
C114—C113—C112120.8 (5)C22—C21—O2109.1 (5)
C114—C113—H113119.6C22—C21—Se2134.3 (5)
C112—C113—H113119.6O2—C21—Se2116.5 (4)
C115—C114—C113119.5 (5)C21—C22—C23107.8 (6)
C115—C114—H114120.3C21—C22—H22126.1
C113—C114—H114120.3C23—C22—H22126.1
C114—C115—C116120.4 (5)C24—C23—C22106.3 (6)
C114—C115—H115119.8C24—C23—H23126.8
C116—C115—H115119.8C22—C23—H23126.8
C115—C116—C111120.5 (5)C23—C24—O2110.9 (6)
C115—C116—H116119.8C23—C24—H24124.6
C111—C116—H116119.8O2—C24—H24124.6
C126—C121—C122118.9 (5)C24—O2—C21106.0 (5)
Se2i—Pd1—Se2—C2196.30 (16)Pd1—P1—C121—C126108.6 (4)
Se1—Pd1—Se2—C2187.88 (16)C131—P1—C121—C122165.7 (4)
Se2i—Pd1—Se2—Pd1i0.0C111—P1—C121—C12252.2 (4)
Se1—Pd1—Se2—Pd1i175.82 (2)Pd1—P1—C121—C12267.5 (4)
P1—Pd1—Se1—C11137.63 (17)C126—C121—C122—C1230.3 (8)
Se2—Pd1—Se1—C1137.19 (17)P1—C121—C122—C123175.9 (4)
Se2i—Pd1—P1—C131138.78 (17)C121—C122—C123—C1240.6 (8)
Se1—Pd1—P1—C13137.28 (17)C122—C123—C124—C1250.4 (9)
Se2i—Pd1—P1—C11199.89 (16)C123—C124—C125—C1260.0 (9)
Se1—Pd1—P1—C11184.05 (16)C122—C121—C126—C1250.1 (8)
Se2i—Pd1—P1—C12116.8 (2)P1—C121—C126—C125176.2 (4)
Se1—Pd1—P1—C121159.3 (2)C124—C125—C126—C1210.2 (9)
Pd1—Se1—C11—O198.6 (4)C111—P1—C131—C136163.5 (4)
Pd1—Se1—C11—C1284.6 (5)C121—P1—C131—C13687.3 (4)
O1—C11—C12—C130.2 (7)Pd1—P1—C131—C13642.3 (4)
Se1—C11—C12—C13176.9 (4)C111—P1—C131—C13216.5 (5)
C11—C12—C13—C140.2 (8)C121—P1—C131—C13292.6 (5)
C12—C13—C14—O10.1 (8)Pd1—P1—C131—C132137.7 (4)
C12—C11—O1—C140.2 (6)C136—C131—C132—C1331.8 (8)
Se1—C11—O1—C14177.0 (4)P1—C131—C132—C133178.2 (4)
C13—C14—O1—C110.1 (7)C131—C132—C133—C1340.8 (9)
C131—P1—C111—C112116.2 (4)C132—C133—C134—C1351.0 (10)
C121—P1—C111—C112134.0 (4)C133—C134—C135—C1361.8 (10)
Pd1—P1—C111—C1127.9 (4)C132—C131—C136—C1351.0 (8)
C131—P1—C111—C11666.0 (5)P1—C131—C136—C135179.0 (5)
C121—P1—C111—C11643.7 (5)C134—C135—C136—C1310.8 (10)
Pd1—P1—C111—C116169.8 (4)Pd1i—Se2—C21—C22112.6 (6)
C116—C111—C112—C1130.6 (7)Pd1—Se2—C21—C22149.8 (6)
P1—C111—C112—C113177.2 (4)Pd1i—Se2—C21—O267.7 (4)
C111—C112—C113—C1140.6 (8)Pd1—Se2—C21—O229.9 (4)
C112—C113—C114—C1150.3 (8)O2—C21—C22—C231.0 (7)
C113—C114—C115—C1161.2 (9)Se2—C21—C22—C23178.7 (5)
C114—C115—C116—C1111.2 (9)C21—C22—C23—C241.1 (8)
C112—C111—C116—C1150.3 (8)C22—C23—C24—O20.8 (8)
P1—C111—C116—C115178.1 (4)C23—C24—O2—C210.2 (8)
C131—P1—C121—C12618.2 (5)C22—C21—O2—C240.6 (7)
C111—P1—C121—C126131.6 (4)Se2—C21—O2—C24179.2 (4)
Symmetry code: (i) x+1, y, z+1.
 

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