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The Pd atom in the title compound, [Pd(C6H5S)2(C22H36FeP2)], possesses a distorted square-planar geometry. The phenyl rings attached to the S atoms are located on opposite sides of the plane defined by the Pd and two S atoms. The Pd-S bonds are statistically significantly different, with values of 2.3703 (7) and 2.3887 (7) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100000172/fr1253sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100000172/fr1253Isup2.hkl
Contains datablock I

CCDC reference: 145532

Comment top

Since the first synthesis of 1,1'-bis(diphenylphosphino)ferrocene (dppf) in 1971 (Bishop et al., 1971), bimetallic complexes of dppf and its alkyl derivatives have been used as catalysts in organic cross-coupling reactions (Hayashi et al., 1984) and in olefin hydrogenation reactions (Cullen et al., 1985). We recently started using group ten metals dppf and dippf [dippf = bis(diisopropylphoshino)ferrocene] dihalides as starting materials in the synthesis of dithiolato metal complexes. During the course of this study, we attempted to prepare Pd(dippf)(SC6H4Te), by first generating LiSC6H4TeLi and reacting the dilithio salt with Pd(dippf)Cl2. The lithium salt was prepared by following the procedure reported by Giolando et al. (1987). Unexpectedly, the product isolated from our reaction was Pd(dippf)(SC6H5)2 (I), whose structure is reported here. \sch

The molecular structure of (I) is shown in Fig.1. Selected bond distances and angles are presented in Table 1. The Pd atom in (I) exhibits a square planar geometry with the cis angles ranging between 85.78 (2)–101.09 (2)° and trans angles spanning 168.45 (2) and 170.55 (2)°. The presence of two alkyl substituents on the phosphorous atoms results in the expansion of the P—Pd—P angle to 101.09 (2)° with concomitant reduction of the S—Pd—S angle to 87.69 (2)°. The corresponding angles in PdCl2(dppf) [dppf = 1,1'-bis(diphenylphosphino)ferrocene; Hayashi et al., 1984] (II) measured 99.07 (5) and 87.8 (1)°, while in Pd(SC6H4S)(dppf) (III) (Maisela & Darkwa, 1999) they were 97.24 (3) and 88.34 (3)°, respectively. In (I), atoms Pd, S1, S2, and P2 are planar within 0.07 Å while phosphorous P1 is displaced 0.570 (1) Å out of that plane. The Pd—P distances are slightly different [2.3303 (6) and 2.3463 (7) Å], with the Pd—P1 distance being 0.0160 (3) Å shorter. This difference is statistically significant. Similar deviation from planarity in the coordination sphere of the Pd center was observed in (II) with one phosphorous atom lying 0.21 Å out of the Pd—S—S—P plane. However, the Pd—P bond length to the P atom located out of the plane [2.301 (1) Å] was 0.018 (1) Å longer than the other Pd—P bond. In contrast, the Pd, two S and two P atoms in (III) are planar within 0.02 Å. The Pd—P bond lengths in (I) are somewhat longer than the `normal' Pd—P bond of 2.29 (5) Å. The latter value was obtained by averaging of 2422 Pd—P distances in complexes reported in the Cambridge Structural Database (CSD) (Allen & Kennard, 1993). The Pd—S distances in (I) [2.3887 (7) and 2.3703 (7) Å] are also statistically different with the Pd—S bond trans to atom P2 being 0.0184 (7) Å longer. Both Pd—S distances in (I) appreciably exceed the length of the `typical' Pd—S distance [2.30 (3) Å] obtained by averaging 340 Pd—S distances found in relevant complexes reported in the CSD. The S···S separation in (I) is rather short [3.297 (1) Å] as compared to the sum of van der Waals radii of S atoms (3.6 Å, Porterfield, 1984). The phenyl groups on the sulfur atoms point to the opposite sides of the plane defined by the Pd and two S atoms. The Pd—S—C angles are close to the ideal tetrahredal value of 109.4°. The ferrocene moiety is quite typical. The cyclopentadienyl rings are almost perfectly parallel with the dihedral angle between the Cp planes being 1.39 (19)° and the Cp—Cp interplanar distance measuring 3.28 (2) Å. The Cp rings are staggered and the Fe atom is closer to the C1—C5 plane [1.637 (1) Å] than to the C6—C10 plane [1.639 (1) Å]. In contrast, the Fe-Centroid distances are very similar and average 1.639 (3) Å with the Centroid-Fe-Centroid angle spanning 178.3 (1)°.

Experimental top

A Schlenk tube was charged with Pd(dippf)Cl2 (0.73 g, 1.23 mmol) and flushed with nitrogen for about 15 min. Degassed toluene (30 ml) was added to give an orange solution to which thiophenol (0.25 ml, 2.46 mmol) and Et3N (0.5 ml) were added. The orange solution immediately turned maroon with some precipitation. The mixture was filtered to remove Et3NH+Cl- as by-product. The filtrate was evaporated to dryness and the residue recrystallized from a CH2Cl2/hexane (1:2) mixture. Single crystals of (I) were grown by layering its CH2Cl2 solution with hexane, followed by a slow diffusion of the hexane at 258 K. Yield = 0.62 g, 68%. Analysis calculated for C34H46P2S2FePd·CH2Cl2: C, 50.77; H, 5.84%. Found: C, 50.80; H, 5.99%. 1H NMR (CDCl3): δ 7.30 (m, 4H, C6H5); 6.92 (m, 6H, C6H5); 4.47 (s, 8H, C5H4); 3.01 (sept, 4H, HC(CH3)2); 1.49 (q, 12H, JHH = 7.0 Hz, HC(CH3)2); 1.19 (q, 12H, JHH = 7.0 Hz, HC(CH3)2). 31P{H} NMR (CDCl3): δ 25.94.

Computing details top

Data collection: SMART (Bruker, 1996); cell refinement: SMART; data reduction: SHELXTL (Sheldrick, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. Molecular structure of (I). The displacement ellipsoids are shown at 30% probability level.
(I) top
Crystal data top
[Pd(C6H5S)2(C22H36FeP2)]F(000) = 1536
Mr = 743.02Dx = 1.471 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.5873 (4) ÅCell parameters from 7356 reflections
b = 17.5830 (7) Åθ = 2–25°
c = 18.0564 (7) ŵ = 1.21 mm1
β = 93.303 (1)°T = 173 K
V = 3355.7 (2) Å3Block, yellow
Z = 40.40 × 0.30 × 0.20 mm
Data collection top
CCD area detector
diffractometer
6858 independent reflections
Radiation source: fine-focus sealed tube5180 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ϕ and ω scansθmax = 26.4°, θmin = 1.6°
Absorption correction: empirical
(SADABS; Blessing, 1995)
h = 1313
Tmin = 0.643, Tmax = 0.794k = 021
27957 measured reflectionsl = 022
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)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.052H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.010P)2]
where P = (Fo2 + 2Fc2)/3
6858 reflections(Δ/σ)max = 0.001
369 parametersΔρmax = 0.41 e Å3
0 restraintsΔρmin = 0.33 e Å3
Crystal data top
[Pd(C6H5S)2(C22H36FeP2)]V = 3355.7 (2) Å3
Mr = 743.02Z = 4
Monoclinic, P21/nMo Kα radiation
a = 10.5873 (4) ŵ = 1.21 mm1
b = 17.5830 (7) ÅT = 173 K
c = 18.0564 (7) Å0.40 × 0.30 × 0.20 mm
β = 93.303 (1)°
Data collection top
CCD area detector
diffractometer
6858 independent reflections
Absorption correction: empirical
(SADABS; Blessing, 1995)
5180 reflections with I > 2σ(I)
Tmin = 0.643, Tmax = 0.794Rint = 0.040
27957 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.052H-atom parameters constrained
S = 1.04Δρmax = 0.41 e Å3
6858 reflectionsΔρmin = 0.33 e Å3
369 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*/Ueq
Pd0.559703 (18)0.237404 (10)0.230833 (10)0.02160 (6)
Fe0.79737 (3)0.216777 (19)0.036277 (18)0.02152 (9)
S10.34697 (6)0.20597 (4)0.25616 (4)0.03489 (18)
S20.58363 (7)0.28745 (4)0.35273 (3)0.03362 (17)
P10.50194 (6)0.20509 (4)0.10838 (3)0.02004 (14)
P20.77786 (6)0.25736 (3)0.22406 (3)0.01976 (14)
C10.6150 (2)0.18462 (13)0.03969 (12)0.0204 (5)
C20.6333 (2)0.22562 (14)0.02766 (12)0.0251 (6)
H20.59030.27420.04310.030*
C30.7246 (2)0.18673 (15)0.06783 (13)0.0303 (6)
H30.75770.20340.11600.036*
C40.7623 (2)0.12110 (15)0.02738 (13)0.0303 (6)
H40.82710.08340.04190.036*
C50.6962 (2)0.11918 (13)0.03898 (13)0.0237 (6)
H50.70470.07920.07830.028*
C60.8536 (2)0.26149 (13)0.13642 (12)0.0199 (5)
C70.8382 (2)0.32027 (13)0.08096 (13)0.0248 (6)
H70.77870.36440.08230.030*
C80.9213 (2)0.30460 (15)0.02388 (14)0.0319 (7)
H80.92940.33540.02220.038*
C90.9877 (2)0.23696 (15)0.04219 (13)0.0315 (6)
H91.05100.21170.01140.038*
C100.9487 (2)0.21077 (14)0.11142 (12)0.0232 (6)
H100.97990.16370.13770.028*
C110.3938 (2)0.12292 (14)0.09411 (13)0.0280 (6)
H110.31410.13620.11840.034*
C120.3564 (3)0.10785 (16)0.01210 (14)0.0421 (8)
H12A0.43250.09700.01450.063*
H12B0.31390.15280.00960.063*
H12C0.29900.06410.00800.063*
C130.4461 (2)0.05095 (13)0.13261 (14)0.0333 (7)
H13A0.38080.01140.13050.050*
H13B0.47090.06250.18450.050*
H13C0.52000.03300.10740.050*
C140.4137 (2)0.28669 (13)0.06608 (13)0.0246 (6)
H140.40080.27570.01180.030*
C150.2820 (2)0.29828 (15)0.09565 (14)0.0348 (7)
H15A0.29080.31530.14740.052*
H15B0.23520.25020.09280.052*
H15C0.23580.33680.06560.052*
C160.4886 (2)0.36073 (14)0.07355 (14)0.0337 (7)
H16A0.44230.40120.04630.051*
H16B0.57150.35380.05310.051*
H16C0.49990.37470.12610.051*
C170.8604 (2)0.17587 (13)0.27107 (12)0.0227 (6)
H170.95180.17920.26020.027*
C180.8104 (2)0.09982 (13)0.24072 (13)0.0290 (6)
H18A0.86080.05830.26340.044*
H18B0.81660.09860.18680.044*
H18C0.72180.09380.25250.044*
C190.8531 (3)0.17729 (15)0.35558 (12)0.0352 (7)
H19A0.76460.17270.36820.053*
H19B0.88810.22530.37510.053*
H19C0.90200.13470.37750.053*
C200.8502 (2)0.34148 (13)0.27182 (13)0.0289 (6)
H200.83230.33690.32540.035*
C210.7889 (3)0.41557 (13)0.24375 (14)0.0383 (7)
H21A0.81760.45760.27620.058*
H21B0.69670.41100.24390.058*
H21C0.81330.42560.19310.058*
C220.9933 (3)0.34460 (15)0.26817 (16)0.0451 (8)
H22A1.01490.35070.21650.068*
H22B1.03050.29730.28820.068*
H22C1.02670.38780.29750.068*
C230.3542 (3)0.13274 (14)0.32250 (13)0.0308 (6)
C240.2422 (3)0.11399 (16)0.35534 (14)0.0387 (7)
H240.16750.14210.34280.046*
C250.2385 (3)0.05527 (19)0.40566 (17)0.0577 (10)
H250.16150.04380.42780.069*
C260.3451 (4)0.01304 (18)0.42419 (17)0.0615 (10)
H260.34180.02790.45830.074*
C270.4563 (3)0.03092 (17)0.39266 (16)0.0535 (9)
H270.53040.00230.40540.064*
C280.4614 (3)0.09061 (15)0.34214 (14)0.0396 (7)
H280.53920.10250.32100.048*
C290.5124 (2)0.37831 (14)0.34391 (13)0.0254 (6)
C300.4201 (3)0.39787 (15)0.28971 (14)0.0358 (7)
H300.39380.36130.25330.043*
C310.3650 (3)0.46961 (15)0.28727 (14)0.0356 (7)
H310.30190.48140.24950.043*
C320.4015 (2)0.52362 (14)0.33936 (14)0.0325 (7)
H320.36360.57260.33800.039*
C330.4938 (2)0.50566 (14)0.39367 (14)0.0314 (6)
H330.51970.54250.42990.038*
C340.5488 (2)0.43424 (14)0.39554 (13)0.0296 (6)
H340.61300.42310.43290.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd0.02317 (11)0.02562 (11)0.01635 (10)0.00499 (9)0.00396 (7)0.00056 (8)
Fe0.0180 (2)0.0300 (2)0.01661 (18)0.00243 (16)0.00083 (14)0.00127 (15)
S10.0268 (4)0.0468 (4)0.0321 (4)0.0065 (3)0.0107 (3)0.0080 (3)
S20.0430 (4)0.0406 (4)0.0174 (3)0.0173 (3)0.0024 (3)0.0016 (3)
P10.0170 (3)0.0239 (4)0.0193 (3)0.0001 (3)0.0015 (3)0.0007 (3)
P20.0233 (4)0.0198 (3)0.0158 (3)0.0012 (3)0.0018 (3)0.0010 (3)
C10.0178 (14)0.0274 (14)0.0157 (12)0.0027 (11)0.0015 (10)0.0048 (10)
C20.0187 (14)0.0378 (16)0.0182 (13)0.0003 (12)0.0035 (10)0.0002 (11)
C30.0251 (15)0.0490 (18)0.0169 (13)0.0041 (13)0.0009 (11)0.0066 (12)
C40.0218 (15)0.0377 (17)0.0315 (15)0.0009 (12)0.0015 (12)0.0169 (13)
C50.0211 (14)0.0254 (14)0.0243 (14)0.0027 (11)0.0009 (11)0.0061 (11)
C60.0176 (13)0.0217 (13)0.0197 (12)0.0041 (11)0.0039 (10)0.0003 (10)
C70.0258 (15)0.0218 (14)0.0261 (14)0.0058 (11)0.0037 (11)0.0034 (11)
C80.0286 (16)0.0413 (17)0.0255 (15)0.0145 (13)0.0009 (12)0.0059 (12)
C90.0163 (14)0.0512 (18)0.0270 (14)0.0072 (13)0.0007 (11)0.0047 (13)
C100.0172 (13)0.0302 (15)0.0216 (13)0.0001 (11)0.0037 (11)0.0011 (11)
C110.0182 (14)0.0323 (16)0.0338 (15)0.0025 (12)0.0027 (12)0.0007 (12)
C120.0357 (18)0.0427 (18)0.0459 (18)0.0121 (14)0.0138 (14)0.0050 (14)
C130.0299 (16)0.0242 (15)0.0461 (17)0.0037 (12)0.0037 (13)0.0036 (13)
C140.0211 (14)0.0302 (15)0.0222 (13)0.0039 (11)0.0020 (11)0.0031 (11)
C150.0257 (16)0.0378 (17)0.0406 (17)0.0107 (13)0.0021 (13)0.0043 (13)
C160.0309 (17)0.0295 (16)0.0407 (17)0.0061 (13)0.0016 (13)0.0045 (13)
C170.0229 (14)0.0240 (14)0.0212 (13)0.0012 (11)0.0005 (11)0.0031 (11)
C180.0317 (16)0.0231 (14)0.0324 (15)0.0027 (12)0.0027 (12)0.0016 (12)
C190.0455 (19)0.0361 (17)0.0230 (14)0.0088 (14)0.0066 (13)0.0026 (12)
C200.0424 (18)0.0214 (14)0.0224 (14)0.0030 (13)0.0036 (12)0.0063 (11)
C210.054 (2)0.0200 (15)0.0415 (17)0.0035 (14)0.0034 (15)0.0061 (13)
C220.0416 (19)0.0355 (18)0.056 (2)0.0084 (15)0.0148 (15)0.0144 (15)
C230.0398 (18)0.0306 (16)0.0221 (14)0.0020 (13)0.0037 (13)0.0080 (12)
C240.0412 (19)0.0446 (19)0.0311 (16)0.0136 (15)0.0083 (14)0.0059 (14)
C250.074 (3)0.056 (2)0.043 (2)0.033 (2)0.0093 (19)0.0006 (17)
C260.108 (3)0.034 (2)0.042 (2)0.022 (2)0.004 (2)0.0058 (16)
C270.086 (3)0.0370 (19)0.0370 (19)0.0124 (18)0.0026 (18)0.0031 (15)
C280.051 (2)0.0387 (18)0.0297 (16)0.0084 (15)0.0101 (14)0.0023 (13)
C290.0222 (15)0.0355 (16)0.0193 (13)0.0037 (12)0.0069 (11)0.0014 (11)
C300.0470 (19)0.0344 (17)0.0250 (15)0.0087 (14)0.0061 (13)0.0090 (12)
C310.0339 (17)0.0366 (17)0.0356 (16)0.0062 (14)0.0045 (13)0.0010 (13)
C320.0307 (17)0.0230 (15)0.0449 (17)0.0001 (12)0.0117 (13)0.0008 (13)
C330.0332 (17)0.0296 (16)0.0319 (16)0.0091 (13)0.0067 (13)0.0053 (12)
C340.0233 (15)0.0386 (17)0.0267 (15)0.0049 (13)0.0004 (12)0.0023 (12)
Geometric parameters (Å, º) top
Pd—P12.3303 (6)C4—C51.423 (3)
Pd—P22.3463 (7)C6—C101.437 (3)
Pd—S22.3703 (7)C6—C71.442 (3)
Pd—S12.3887 (7)C7—C81.420 (3)
Fe—C12.016 (2)C8—C91.411 (3)
Fe—C52.025 (2)C9—C101.416 (3)
Fe—C72.027 (2)C11—C131.532 (3)
Fe—C62.029 (2)C11—C121.534 (3)
Fe—C22.036 (2)C14—C161.526 (3)
Fe—C102.042 (2)C14—C151.535 (3)
Fe—C92.042 (2)C17—C181.528 (3)
Fe—C82.047 (2)C17—C191.532 (3)
Fe—C32.059 (2)C20—C221.522 (3)
Fe—C42.059 (2)C20—C211.528 (3)
S1—C231.757 (3)C23—C281.385 (3)
S2—C291.770 (2)C23—C241.395 (3)
P1—C11.809 (2)C24—C251.377 (4)
P1—C111.853 (2)C25—C261.376 (4)
P1—C141.853 (2)C26—C271.373 (4)
P2—C61.816 (2)C27—C281.394 (4)
P2—C201.855 (2)C29—C301.386 (3)
P2—C171.858 (2)C29—C341.394 (3)
C1—C21.436 (3)C30—C311.389 (3)
C1—C51.436 (3)C31—C321.376 (3)
C2—C31.417 (3)C32—C331.381 (3)
C3—C41.411 (3)C33—C341.384 (3)
P1—Pd—P2101.09 (2)C2—C1—C5106.54 (19)
P1—Pd—S2168.45 (2)C2—C1—P1127.40 (18)
P2—Pd—S286.56 (2)C5—C1—P1125.82 (18)
P1—Pd—S185.78 (2)C2—C1—Fe69.97 (13)
P2—Pd—S1170.55 (2)C5—C1—Fe69.52 (13)
S2—Pd—S187.69 (3)P1—C1—Fe129.64 (12)
C1—Fe—C541.64 (9)C3—C2—C1108.7 (2)
C1—Fe—C7114.97 (10)C3—C2—Fe70.64 (14)
C5—Fe—C7148.44 (9)C1—C2—Fe68.51 (13)
C1—Fe—C6108.27 (9)C4—C3—C2108.1 (2)
C5—Fe—C6115.79 (9)C4—C3—Fe69.97 (14)
C7—Fe—C641.64 (8)C2—C3—Fe68.87 (13)
C1—Fe—C241.52 (9)C3—C4—C5108.5 (2)
C5—Fe—C269.08 (10)C3—C4—Fe69.95 (14)
C7—Fe—C2108.22 (10)C5—C4—Fe68.34 (13)
C6—Fe—C2132.27 (9)C4—C5—C1108.2 (2)
C1—Fe—C10132.95 (9)C4—C5—Fe70.90 (14)
C5—Fe—C10109.65 (10)C1—C5—Fe68.84 (13)
C7—Fe—C1068.95 (10)C10—C6—C7106.2 (2)
C6—Fe—C1041.35 (8)C10—C6—P2126.97 (17)
C2—Fe—C10172.85 (9)C7—C6—P2126.58 (18)
C1—Fe—C9172.14 (10)C10—C6—Fe69.80 (12)
C5—Fe—C9131.89 (10)C7—C6—Fe69.10 (13)
C7—Fe—C968.66 (10)P2—C6—Fe129.75 (12)
C6—Fe—C969.41 (9)C8—C7—C6108.4 (2)
C2—Fe—C9145.43 (10)C8—C7—Fe70.35 (14)
C10—Fe—C940.56 (9)C6—C7—Fe69.26 (13)
C1—Fe—C8146.70 (10)C9—C8—C7108.3 (2)
C5—Fe—C8170.15 (10)C9—C8—Fe69.65 (14)
C7—Fe—C840.80 (9)C7—C8—Fe68.86 (14)
C6—Fe—C869.41 (9)C8—C9—C10108.3 (2)
C2—Fe—C8114.31 (10)C8—C9—Fe69.98 (14)
C10—Fe—C868.18 (10)C10—C9—Fe69.71 (13)
C9—Fe—C840.37 (10)C9—C10—C6108.7 (2)
C1—Fe—C369.35 (9)C9—C10—Fe69.74 (13)
C5—Fe—C368.53 (10)C6—C10—Fe68.85 (13)
C7—Fe—C3130.82 (10)C13—C11—C12111.2 (2)
C6—Fe—C3171.12 (10)C13—C11—P1112.13 (17)
C2—Fe—C340.50 (9)C12—C11—P1113.07 (17)
C10—Fe—C3146.25 (10)C16—C14—C15109.5 (2)
C9—Fe—C3114.11 (10)C16—C14—P1112.14 (17)
C8—Fe—C3107.59 (10)C15—C14—P1113.96 (16)
C1—Fe—C469.26 (9)C18—C17—C19109.6 (2)
C5—Fe—C440.76 (9)C18—C17—P2111.52 (16)
C7—Fe—C4169.44 (10)C19—C17—P2113.14 (16)
C6—Fe—C4148.00 (10)C22—C20—C21111.1 (2)
C2—Fe—C467.99 (10)C22—C20—P2113.19 (17)
C10—Fe—C4115.97 (10)C21—C20—P2111.69 (17)
C9—Fe—C4108.46 (10)C28—C23—C24118.0 (3)
C8—Fe—C4130.64 (10)C28—C23—S1124.7 (2)
C3—Fe—C440.08 (10)C24—C23—S1117.3 (2)
C23—S1—Pd107.19 (9)C25—C24—C23121.0 (3)
C29—S2—Pd103.26 (8)C26—C25—C24120.7 (3)
C1—P1—C11100.25 (11)C27—C26—C25119.1 (3)
C1—P1—C14102.09 (11)C26—C27—C28120.7 (3)
C11—P1—C14104.68 (11)C23—C28—C27120.5 (3)
C1—P1—Pd123.45 (8)C30—C29—C34117.0 (2)
C11—P1—Pd116.64 (8)C30—C29—S2124.5 (2)
C14—P1—Pd107.51 (8)C34—C29—S2118.45 (19)
C6—P2—C20100.50 (11)C29—C30—C31121.7 (2)
C6—P2—C17102.08 (11)C32—C31—C30120.3 (3)
C20—P2—C17103.40 (11)C31—C32—C33119.1 (2)
C6—P2—Pd122.46 (7)C32—C33—C34120.3 (2)
C20—P2—Pd118.43 (8)C33—C34—C29121.6 (2)
C17—P2—Pd107.42 (8)

Experimental details

Crystal data
Chemical formula[Pd(C6H5S)2(C22H36FeP2)]
Mr743.02
Crystal system, space groupMonoclinic, P21/n
Temperature (K)173
a, b, c (Å)10.5873 (4), 17.5830 (7), 18.0564 (7)
β (°) 93.303 (1)
V3)3355.7 (2)
Z4
Radiation typeMo Kα
µ (mm1)1.21
Crystal size (mm)0.40 × 0.30 × 0.20
Data collection
DiffractometerCCD area detector
diffractometer
Absorption correctionEmpirical
(SADABS; Blessing, 1995)
Tmin, Tmax0.643, 0.794
No. of measured, independent and
observed [I > 2σ(I)] reflections
27957, 6858, 5180
Rint0.040
(sin θ/λ)max1)0.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.052, 1.04
No. of reflections6858
No. of parameters369
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.41, 0.33

Computer programs: SMART (Bruker, 1996), SMART, SHELXTL (Sheldrick, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL.

Selected geometric parameters (Å, º) top
Pd—P12.3303 (6)Pd—S22.3703 (7)
Pd—P22.3463 (7)Pd—S12.3887 (7)
P1—Pd—P2101.09 (2)P1—Pd—S185.78 (2)
P1—Pd—S2168.45 (2)P2—Pd—S1170.55 (2)
P2—Pd—S286.56 (2)S2—Pd—S187.69 (3)
 

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