Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270199016509/fr1241sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270199016509/fr1241Isup2.hkl |
[Pd(PhCN)2Cl2] (46 mg, 0.12 mmol), PPh3 (31 mg, 0.12 mmol) and rhodanine (27 mg, 0.24 mmol) as reducing agent were stirred in acetone (10 ml) under argon at room temperature. The suspension became clear solution during stirring. After filtration, the filtrate was transferred to glass tubes and the same amount of n-pentane was added slowly to the solution. The glass tubes were sealed and allowed to stand at room temperature. After one week, red crystals of (I) were obtained.
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation & Rigaku Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation & Rigaku Corporation, 1999); program(s) used to solve structure: DIRDIF92 (PATTY) (Beurskens et al., 1992); program(s) used to refine structure: TEXSAN and SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.
Fig. 1. The molecular structure of (I) showing 30% probability displacement ellipsoids. H atoms and (CH3)2CO solvate have been omitted for clarity. |
[Pd3Cl5(C18H15P)3]·C3H6O | Z = 2 |
Mr = 1341.42 | Dx = 1.589 Mg m−3 |
Triclinic, P1 | Mo Kα radiation, λ = 0.7107 Å |
a = 18.515 (2) Å | Cell parameters from 25 reflections |
b = 14.295 (3) Å | θ = 15.1–19.1° |
c = 10.916 (1) Å | µ = 1.31 mm−1 |
α = 84.90 (1)° | T = 296 K |
β = 87.874 (9)° | Plate, red |
γ = 77.04 (1)° | 0.20 × 0.20 × 0.10 mm |
V = 2803.9 (8) Å3 |
Rigaku AFC7R diffractometer | Rint = 0.015 |
ω–2θ scans | θmax = 27.5°, θmin = 4.0° |
Absorption correction: ψ scan (North et al., 1968) | h = −23→24 |
Tmin = 0.728, Tmax = 0.877 | k = 0→18 |
13420 measured reflections | l = −14→14 |
12899 independent reflections | 3 standard reflections every 150 reflections |
9622 reflections with I > 2σ(I) | intensity decay: 2.4% |
Refinement on F2 | w = 1/[σ2(Fo2) + (0.0451P)2 + 0.6836P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.037 | (Δ/σ)max = −0.005 |
wR(F2) = 0.101 | Δρmax = 0.44 e Å−3 |
S = 1.02 | Δρmin = −0.47 e Å−3 |
9622 reflections | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
625 parameters | Extinction coefficient: 0.0005 |
H-atom parameters not refined |
[Pd3Cl5(C18H15P)3]·C3H6O | γ = 77.04 (1)° |
Mr = 1341.42 | V = 2803.9 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 18.515 (2) Å | Mo Kα radiation |
b = 14.295 (3) Å | µ = 1.31 mm−1 |
c = 10.916 (1) Å | T = 296 K |
α = 84.90 (1)° | 0.20 × 0.20 × 0.10 mm |
β = 87.874 (9)° |
Rigaku AFC7R diffractometer | 9622 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.015 |
Tmin = 0.728, Tmax = 0.877 | 3 standard reflections every 150 reflections |
13420 measured reflections | intensity decay: 2.4% |
12899 independent reflections |
R[F2 > 2σ(F2)] = 0.037 | 625 parameters |
wR(F2) = 0.101 | H-atom parameters not refined |
S = 1.02 | Δρmax = 0.44 e Å−3 |
9622 reflections | Δρmin = −0.47 e Å−3 |
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. All hydrogen atoms connected to phenyl groups were treated with a riding model with the 1.2 fold isotropic displacement parameters of the equivalent Uiso of the corresponding carbon atom. The hydrogen atoms of CH3 groups were refined in ideal positions with C—H bond lengths of 0.96 Å. |
Refinement. The θ-scan width used was (1.05 + 0.30 tanθ)° at speed of 16.0 min-1 (in ω). The weak reflections were rescanned a maximum of three times and the counts accumulated to ensure good counting statistics. Stationary background counts were made on each side of the reflection with a 2:1 ratio of peak to background counting time. The structures was solved by heavy-atom Patterson and expanded using the Fourier program DIRDIF94 (Beurskens et al., 1994). Refinement using reflections with F2 > -10.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt)·The non-hydrogen atoms were refined anisotropically. Hydrogen atoms were included in the structure factor calculation but not refined. The refinements were performed by using full-matrix least-squares method. All calculations were performed using the TEXSAN crystallographic software package. |
x | y | z | Uiso*/Ueq | ||
Pd1 | 0.11145 (2) | 0.19753 (2) | −0.42754 (2) | 0.03608 (8) | |
Pd2 | 0.27008 (1) | 0.07195 (2) | −0.41085 (2) | 0.03487 (8) | |
Pd3 | 0.25061 (2) | 0.29131 (2) | −0.43973 (3) | 0.03937 (8) | |
Cl1 | 0.21258 (6) | 0.18592 (7) | −0.58230 (8) | 0.0449 (2) | |
Cl2 | 0.20608 (5) | 0.19044 (7) | −0.29496 (8) | 0.0417 (2) | |
Cl3 | 0.02258 (7) | 0.2097 (1) | −0.5771 (1) | 0.0646 (3) | |
Cl4 | 0.32521 (6) | −0.04336 (8) | −0.5437 (1) | 0.0539 (3) | |
Cl5 | 0.29512 (7) | 0.37716 (8) | −0.6052 (1) | 0.0617 (3) | |
P1 | 0.02243 (5) | 0.22919 (7) | −0.28542 (9) | 0.0379 (2) | |
P2 | 0.31220 (5) | −0.03053 (7) | −0.25035 (9) | 0.0369 (2) | |
P3 | 0.29714 (6) | 0.36933 (8) | −0.3038 (1) | 0.0456 (2) | |
O1 | 0.3529 (7) | 0.6605 (9) | 0.076 (1) | 0.323 (8) | |
C1 | −0.0076 (2) | 0.3594 (3) | −0.3053 (4) | 0.0479 (9) | |
C2 | −0.0753 (3) | 0.4026 (4) | −0.3555 (5) | 0.075 (2) | |
C3 | −0.0948 (4) | 0.5027 (5) | −0.3753 (6) | 0.096 (2) | |
C4 | −0.0479 (5) | 0.5570 (4) | −0.3480 (6) | 0.100 (2) | |
C5 | 0.0199 (4) | 0.5140 (4) | −0.3023 (7) | 0.096 (2) | |
C6 | 0.0411 (3) | 0.4147 (4) | −0.2801 (5) | 0.069 (1) | |
C7 | −0.0581 (3) | 0.1773 (4) | −0.2951 (4) | 0.055 (1) | |
C8 | −0.0556 (3) | 0.0991 (4) | −0.3629 (5) | 0.069 (1) | |
C9 | −0.1181 (5) | 0.0602 (5) | −0.3645 (6) | 0.098 (2) | |
C10 | −0.1805 (5) | 0.0987 (8) | −0.3000 (7) | 0.121 (3) | |
C11 | −0.1823 (4) | 0.1733 (7) | −0.2307 (7) | 0.114 (3) | |
C12 | −0.1211 (3) | 0.2138 (5) | −0.2285 (5) | 0.080 (2) | |
C13 | 0.0443 (2) | 0.1960 (3) | −0.1247 (3) | 0.0422 (9) | |
C14 | 0.0381 (3) | 0.2622 (4) | −0.0370 (4) | 0.065 (1) | |
C15 | 0.0473 (3) | 0.2294 (5) | 0.0863 (5) | 0.081 (2) | |
C16 | 0.0626 (3) | 0.1341 (5) | 0.1230 (5) | 0.078 (2) | |
C17 | 0.0697 (3) | 0.0671 (4) | 0.0372 (5) | 0.071 (1) | |
C18 | 0.0608 (3) | 0.0991 (4) | −0.0865 (4) | 0.057 (1) | |
C19 | 0.2500 (2) | −0.1121 (3) | −0.2216 (4) | 0.0461 (9) | |
C20 | 0.1929 (3) | −0.1069 (4) | −0.3021 (5) | 0.061 (1) | |
C21 | 0.1433 (3) | −0.1662 (4) | −0.2795 (6) | 0.078 (2) | |
C22 | 0.1504 (4) | −0.2306 (5) | −0.1792 (7) | 0.089 (2) | |
C23 | 0.2074 (4) | −0.2382 (5) | −0.0999 (6) | 0.091 (2) | |
C24 | 0.2571 (3) | −0.1787 (4) | −0.1193 (5) | 0.073 (1) | |
C25 | 0.4060 (2) | −0.0986 (3) | −0.2783 (4) | 0.0447 (9) | |
C26 | 0.4295 (3) | −0.1947 (4) | −0.2408 (6) | 0.072 (1) | |
C27 | 0.5036 (4) | −0.2391 (5) | −0.2600 (8) | 0.103 (2) | |
C28 | 0.5527 (3) | −0.1878 (6) | −0.3126 (7) | 0.099 (3) | |
C29 | 0.5293 (3) | −0.0938 (6) | −0.3495 (5) | 0.078 (2) | |
C30 | 0.4555 (2) | −0.0476 (4) | −0.3336 (4) | 0.058 (1) | |
C31 | 0.3194 (2) | 0.0172 (3) | −0.1028 (3) | 0.0399 (8) | |
C32 | 0.3850 (2) | 0.0370 (4) | −0.0676 (4) | 0.060 (1) | |
C33 | 0.3903 (3) | 0.0700 (5) | 0.0468 (5) | 0.074 (2) | |
C34 | 0.3304 (3) | 0.0825 (4) | 0.1264 (4) | 0.069 (1) | |
C35 | 0.2653 (3) | 0.0655 (4) | 0.0900 (4) | 0.067 (1) | |
C36 | 0.2588 (2) | 0.0337 (4) | −0.0235 (4) | 0.058 (1) | |
C37 | 0.3063 (3) | 0.4893 (3) | −0.3632 (4) | 0.058 (1) | |
C38 | 0.2458 (4) | 0.5534 (4) | −0.4160 (5) | 0.077 (2) | |
C39 | 0.2511 (5) | 0.6463 (5) | −0.4548 (6) | 0.104 (2) | |
C40 | 0.3151 (7) | 0.6751 (5) | −0.4457 (7) | 0.119 (3) | |
C41 | 0.3749 (5) | 0.6127 (6) | −0.3949 (8) | 0.122 (3) | |
C42 | 0.3709 (4) | 0.5190 (4) | −0.3535 (6) | 0.090 (2) | |
C43 | 0.3901 (2) | 0.3009 (3) | −0.2694 (4) | 0.054 (1) | |
C44 | 0.4319 (3) | 0.2536 (4) | −0.3625 (5) | 0.072 (1) | |
C45 | 0.5042 (3) | 0.2017 (5) | −0.3433 (7) | 0.093 (2) | |
C46 | 0.5341 (3) | 0.1952 (5) | −0.2314 (8) | 0.098 (2) | |
C47 | 0.4943 (4) | 0.2413 (6) | −0.1377 (6) | 0.101 (2) | |
C48 | 0.4222 (3) | 0.2941 (5) | −0.1561 (5) | 0.080 (2) | |
C49 | 0.2489 (3) | 0.3881 (3) | −0.1563 (4) | 0.055 (1) | |
C50 | 0.2501 (3) | 0.3119 (4) | −0.0684 (5) | 0.066 (1) | |
C51 | 0.2144 (4) | 0.3275 (5) | 0.0440 (5) | 0.087 (2) | |
C52 | 0.1770 (5) | 0.4156 (6) | 0.0689 (7) | 0.120 (3) | |
C53 | 0.1725 (5) | 0.4914 (6) | −0.0181 (8) | 0.120 (3) | |
C54 | 0.2093 (4) | 0.4794 (4) | −0.1311 (6) | 0.084 (2) | |
C55 | 0.3997 (9) | 0.559 (1) | 0.259 (1) | 0.275 (9) | |
C56 | 0.3716 (6) | 0.5847 (9) | 0.132 (1) | 0.232 (9) | |
C57 | 0.379 (1) | 0.492 (1) | 0.079 (2) | 0.39 (2) | |
H1 | −0.1084 | 0.3642 | −0.3765 | 0.0904* | |
H2 | −0.1418 | 0.5336 | −0.4082 | 0.1155* | |
H3 | −0.0615 | 0.6251 | −0.3598 | 0.1221* | |
H4 | 0.0535 | 0.5529 | −0.2856 | 0.1142* | |
H5 | 0.0889 | 0.3852 | −0.2466 | 0.0820* | |
H6 | −0.0116 | 0.0717 | −0.4073 | 0.0838* | |
H7 | −0.1184 | 0.0075 | −0.4106 | 0.1147* | |
H8 | −0.2233 | 0.0731 | −0.3045 | 0.1455* | |
H9 | −0.2257 | 0.1964 | −0.1827 | 0.1346* | |
H10 | −0.1223 | 0.2660 | −0.1808 | 0.0977* | |
H11 | 0.0268 | 0.3292 | −0.0610 | 0.0783* | |
H12 | 0.0425 | 0.2750 | 0.1465 | 0.0983* | |
H13 | 0.0685 | 0.1128 | 0.2079 | 0.0938* | |
H14 | 0.0810 | 0.0002 | 0.0624 | 0.0852* | |
H15 | 0.0666 | 0.0531 | −0.1456 | 0.0679* | |
H16 | 0.1874 | −0.0627 | −0.3731 | 0.0740* | |
H17 | 0.1048 | −0.1625 | −0.3342 | 0.0963* | |
H18 | 0.1163 | −0.2709 | −0.1631 | 0.1084* | |
H19 | 0.2135 | −0.2851 | −0.0316 | 0.1078* | |
H20 | 0.2956 | −0.1832 | −0.0632 | 0.0887* | |
H21 | 0.3962 | −0.2307 | −0.2031 | 0.0867* | |
H22 | 0.5214 | −0.3047 | −0.2370 | 0.1242* | |
H23 | 0.6040 | −0.2186 | −0.3224 | 0.1144* | |
H24 | 0.5634 | −0.0602 | −0.3864 | 0.0989* | |
H25 | 0.4397 | 0.0184 | −0.3606 | 0.0707* | |
H26 | 0.4270 | 0.0278 | −0.1217 | 0.0720* | |
H27 | 0.4354 | 0.0830 | 0.0703 | 0.0899* | |
H28 | 0.3339 | 0.1040 | 0.2054 | 0.0828* | |
H29 | 0.2231 | 0.0756 | 0.1444 | 0.0807* | |
H30 | 0.2127 | 0.0230 | −0.0471 | 0.0707* | |
H31 | 0.2008 | 0.5336 | −0.4251 | 0.0929* | |
H32 | 0.2091 | 0.6908 | −0.4893 | 0.1230* | |
H33 | 0.3177 | 0.7388 | −0.4744 | 0.1436* | |
H34 | 0.4195 | 0.6338 | −0.3859 | 0.1437* | |
H35 | 0.4139 | 0.4754 | −0.3199 | 0.1064* | |
H36 | 0.4107 | 0.2564 | −0.4414 | 0.0873* | |
H37 | 0.5323 | 0.1713 | −0.4096 | 0.1126* | |
H38 | 0.5828 | 0.1578 | −0.2168 | 0.1177* | |
H39 | 0.5153 | 0.2366 | −0.0590 | 0.1219* | |
H40 | 0.3954 | 0.3265 | −0.0906 | 0.0954* | |
H41 | 0.2756 | 0.2489 | −0.0851 | 0.0801* | |
H42 | 0.2149 | 0.2755 | 0.1036 | 0.1049* | |
H43 | 0.1554 | 0.4266 | 0.1472 | 0.1493* | |
H44 | 0.1431 | 0.5539 | −0.0037 | 0.1403* | |
H45 | 0.2071 | 0.5331 | −0.1906 | 0.0986* | |
H46 | 0.4510 | 0.5264 | 0.2552 | 0.2812* | |
H47 | 0.3717 | 0.5169 | 0.3020 | 0.2812* | |
H48 | 0.3946 | 0.6162 | 0.3006 | 0.2812* | |
H49 | 0.3685 | 0.5032 | −0.0069 | 0.4116* | |
H50 | 0.4285 | 0.4546 | 0.0904 | 0.4116* | |
H51 | 0.3445 | 0.4579 | 0.1199 | 0.4116* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd1 | 0.0381 (2) | 0.0406 (2) | 0.0291 (1) | −0.0072 (1) | −0.0018 (1) | −0.0043 (1) |
Pd2 | 0.0327 (1) | 0.0400 (2) | 0.0320 (1) | −0.0074 (1) | −0.0006 (1) | −0.0055 (1) |
Pd3 | 0.0404 (2) | 0.0402 (2) | 0.0369 (2) | −0.0070 (1) | 0.0030 (1) | −0.0066 (1) |
Cl1 | 0.0510 (5) | 0.0519 (6) | 0.0310 (4) | −0.0092 (4) | 0.0015 (4) | −0.0059 (4) |
Cl2 | 0.0422 (5) | 0.0493 (5) | 0.0329 (4) | −0.0073 (4) | −0.0007 (4) | −0.0068 (4) |
Cl3 | 0.0617 (7) | 0.0969 (9) | 0.0400 (5) | −0.0282 (7) | −0.0152 (5) | 0.0016 (6) |
Cl4 | 0.0498 (6) | 0.0606 (7) | 0.0506 (6) | −0.0038 (5) | −0.0017 (4) | −0.0229 (5) |
Cl5 | 0.0735 (8) | 0.0545 (6) | 0.0554 (6) | −0.0144 (6) | 0.0175 (5) | −0.0019 (5) |
P1 | 0.0346 (5) | 0.0440 (5) | 0.0354 (5) | −0.0097 (4) | −0.0005 (4) | −0.0028 (4) |
P2 | 0.0309 (5) | 0.0432 (5) | 0.0376 (5) | −0.0105 (4) | −0.0029 (4) | −0.0025 (4) |
P3 | 0.0466 (6) | 0.0457 (6) | 0.0465 (6) | −0.0120 (5) | 0.0027 (5) | −0.0118 (5) |
O1 | 0.33 (2) | 0.24 (1) | 0.39 (2) | −0.06 (1) | −0.20 (1) | 0.07 (1) |
C1 | 0.052 (2) | 0.044 (2) | 0.044 (2) | −0.003 (2) | 0.010 (2) | −0.005 (2) |
C2 | 0.075 (3) | 0.074 (4) | 0.061 (3) | 0.019 (3) | −0.009 (3) | −0.002 (3) |
C3 | 0.119 (6) | 0.071 (4) | 0.068 (4) | 0.037 (4) | −0.005 (4) | −0.002 (3) |
C4 | 0.146 (7) | 0.050 (3) | 0.078 (4) | 0.021 (4) | 0.033 (4) | 0.011 (3) |
C5 | 0.121 (6) | 0.051 (3) | 0.117 (5) | −0.023 (4) | 0.048 (4) | −0.013 (3) |
C6 | 0.058 (3) | 0.051 (3) | 0.096 (4) | −0.011 (2) | 0.018 (3) | −0.010 (3) |
C7 | 0.054 (3) | 0.074 (3) | 0.040 (2) | −0.027 (2) | −0.010 (2) | 0.007 (2) |
C8 | 0.087 (4) | 0.074 (3) | 0.055 (3) | −0.039 (3) | −0.013 (3) | 0.010 (2) |
C9 | 0.142 (6) | 0.109 (5) | 0.067 (4) | −0.088 (5) | −0.043 (4) | 0.023 (3) |
C10 | 0.105 (6) | 0.202 (9) | 0.083 (5) | −0.107 (6) | −0.041 (4) | 0.052 (5) |
C11 | 0.066 (4) | 0.193 (9) | 0.093 (5) | −0.063 (5) | −0.006 (3) | 0.018 (5) |
C12 | 0.049 (3) | 0.130 (5) | 0.070 (3) | −0.039 (3) | 0.005 (2) | −0.005 (3) |
C13 | 0.033 (2) | 0.058 (2) | 0.034 (2) | −0.009 (2) | 0.001 (1) | 0.000 (2) |
C14 | 0.074 (3) | 0.073 (3) | 0.050 (3) | −0.016 (3) | −0.001 (2) | −0.012 (2) |
C15 | 0.087 (4) | 0.113 (5) | 0.040 (3) | −0.013 (4) | 0.002 (2) | −0.021 (3) |
C16 | 0.061 (3) | 0.125 (5) | 0.044 (3) | −0.018 (3) | 0.003 (2) | 0.008 (3) |
C17 | 0.063 (3) | 0.083 (4) | 0.061 (3) | −0.013 (3) | −0.002 (2) | 0.020 (3) |
C18 | 0.055 (3) | 0.065 (3) | 0.049 (2) | −0.014 (2) | −0.005 (2) | 0.003 (2) |
C19 | 0.042 (2) | 0.054 (2) | 0.047 (2) | −0.019 (2) | 0.002 (2) | −0.004 (2) |
C20 | 0.047 (2) | 0.064 (3) | 0.077 (3) | −0.024 (2) | −0.013 (2) | −0.001 (2) |
C21 | 0.054 (3) | 0.086 (4) | 0.104 (4) | −0.038 (3) | −0.012 (3) | −0.011 (3) |
C22 | 0.081 (4) | 0.089 (4) | 0.112 (5) | −0.053 (4) | 0.024 (4) | −0.015 (4) |
C23 | 0.116 (5) | 0.088 (4) | 0.083 (4) | −0.060 (4) | 0.007 (4) | 0.011 (3) |
C24 | 0.085 (4) | 0.081 (4) | 0.064 (3) | −0.046 (3) | −0.009 (3) | 0.012 (3) |
C25 | 0.037 (2) | 0.054 (2) | 0.042 (2) | −0.003 (2) | −0.005 (2) | −0.009 (2) |
C26 | 0.061 (3) | 0.053 (3) | 0.099 (4) | 0.000 (2) | −0.018 (3) | −0.014 (3) |
C27 | 0.075 (4) | 0.070 (4) | 0.153 (7) | 0.024 (3) | −0.034 (4) | −0.044 (4) |
C28 | 0.046 (3) | 0.142 (7) | 0.103 (5) | 0.021 (4) | −0.023 (3) | −0.072 (5) |
C29 | 0.037 (2) | 0.143 (6) | 0.057 (3) | −0.018 (3) | 0.001 (2) | −0.028 (3) |
C30 | 0.035 (2) | 0.090 (4) | 0.049 (2) | −0.013 (2) | 0.000 (2) | −0.004 (2) |
C31 | 0.034 (2) | 0.048 (2) | 0.036 (2) | −0.007 (2) | −0.003 (1) | −0.003 (2) |
C32 | 0.044 (2) | 0.087 (4) | 0.054 (3) | −0.020 (2) | −0.002 (2) | −0.022 (2) |
C33 | 0.050 (3) | 0.116 (5) | 0.064 (3) | −0.022 (3) | −0.011 (2) | −0.030 (3) |
C34 | 0.077 (3) | 0.093 (4) | 0.039 (2) | −0.014 (3) | −0.013 (2) | −0.016 (2) |
C35 | 0.067 (3) | 0.095 (4) | 0.044 (3) | −0.032 (3) | 0.012 (2) | −0.010 (3) |
C36 | 0.045 (2) | 0.084 (3) | 0.048 (2) | −0.022 (2) | 0.005 (2) | −0.010 (2) |
C37 | 0.068 (3) | 0.051 (3) | 0.058 (3) | −0.017 (2) | 0.002 (2) | −0.013 (2) |
C38 | 0.100 (4) | 0.051 (3) | 0.077 (4) | −0.011 (3) | 0.003 (3) | −0.008 (3) |
C39 | 0.168 (7) | 0.052 (3) | 0.088 (5) | −0.014 (4) | −0.015 (5) | −0.009 (3) |
C40 | 0.21 (1) | 0.058 (4) | 0.102 (6) | −0.055 (5) | −0.001 (6) | −0.003 (4) |
C41 | 0.157 (8) | 0.093 (5) | 0.143 (7) | −0.082 (6) | −0.001 (6) | −0.013 (5) |
C42 | 0.102 (5) | 0.072 (4) | 0.106 (5) | −0.041 (4) | −0.007 (4) | −0.010 (3) |
C43 | 0.048 (2) | 0.058 (3) | 0.059 (3) | −0.014 (2) | −0.005 (2) | −0.010 (2) |
C44 | 0.048 (3) | 0.081 (4) | 0.086 (4) | −0.003 (3) | −0.004 (2) | −0.026 (3) |
C45 | 0.055 (3) | 0.099 (5) | 0.123 (6) | −0.002 (3) | −0.005 (3) | −0.034 (4) |
C46 | 0.056 (3) | 0.096 (5) | 0.138 (7) | −0.006 (3) | −0.016 (4) | 0.000 (5) |
C47 | 0.066 (4) | 0.154 (7) | 0.086 (4) | −0.029 (4) | −0.023 (3) | 0.001 (5) |
C48 | 0.060 (3) | 0.111 (5) | 0.070 (3) | −0.018 (3) | −0.008 (3) | −0.014 (3) |
C49 | 0.062 (3) | 0.056 (3) | 0.050 (2) | −0.018 (2) | 0.008 (2) | −0.021 (2) |
C50 | 0.074 (3) | 0.072 (3) | 0.056 (3) | −0.022 (3) | 0.005 (2) | −0.018 (3) |
C51 | 0.112 (5) | 0.098 (5) | 0.057 (3) | −0.036 (4) | 0.021 (3) | −0.020 (3) |
C52 | 0.176 (8) | 0.121 (6) | 0.084 (5) | −0.070 (6) | 0.070 (5) | −0.051 (5) |
C53 | 0.155 (7) | 0.092 (5) | 0.110 (6) | −0.018 (5) | 0.055 (5) | −0.046 (5) |
C54 | 0.109 (5) | 0.066 (3) | 0.076 (4) | −0.017 (3) | 0.030 (3) | −0.025 (3) |
C55 | 0.37 (2) | 0.25 (2) | 0.26 (2) | −0.19 (2) | −0.02 (2) | 0.07 (1) |
C56 | 0.31 (2) | 0.13 (1) | 0.27 (2) | −0.08 (1) | −0.18 (2) | 0.06 (1) |
C57 | 0.69 (5) | 0.19 (2) | 0.30 (2) | −0.10 (2) | −0.03 (3) | −0.04 (2) |
Pd1—Pd2 | 3.0818 (5) | C23—C24 | 1.39 (1) |
Pd1—Pd3 | 3.1537 (6) | C23—H19 | 0.950 |
Pd2—Pd3 | 3.0639 (4) | C24—H20 | 0.946 |
Pd1—Cl1 | 2.462 (1) | C25—C26 | 1.375 (6) |
Pd1—Cl2 | 2.293 (1) | C25—C30 | 1.384 (7) |
Pd1—Cl3 | 2.329 (1) | C26—C27 | 1.393 (8) |
Pd1—P1 | 2.220 (1) | C26—H21 | 0.949 |
Pd2—Pd3 | 3.0639 (4) | C27—C28 | 1.37 (1) |
Pd2—Cl1 | 2.4735 (9) | C27—H22 | 0.937 |
Pd2—Cl2 | 2.2896 (9) | C28—C29 | 1.35 (1) |
Pd2—Cl4 | 2.328 (1) | C28—H23 | 0.959 |
Pd2—P2 | 2.2264 (9) | C29—C30 | 1.389 (6) |
Pd3—Cl1 | 2.482 (1) | C29—H24 | 0.936 |
Pd3—Cl2 | 2.300 (1) | C30—H25 | 0.947 |
Pd3—Cl5 | 2.323 (1) | C31—C32 | 1.382 (6) |
Pd3—P3 | 2.238 (1) | C31—C36 | 1.383 (6) |
P1—C1 | 1.814 (4) | C32—C33 | 1.388 (8) |
P1—C7 | 1.817 (5) | C32—H26 | 0.951 |
P1—C13 | 1.813 (4) | C33—C34 | 1.371 (7) |
P2—C19 | 1.815 (5) | C33—H27 | 0.945 |
P2—C25 | 1.820 (4) | C34—C35 | 1.362 (8) |
P2—C31 | 1.826 (4) | C34—H28 | 0.950 |
P3—C37 | 1.820 (5) | C35—C36 | 1.376 (7) |
P3—C43 | 1.813 (4) | C35—H29 | 0.955 |
P3—C49 | 1.823 (5) | C36—H30 | 0.948 |
O1—C56 | 1.18 (2) | C37—C38 | 1.387 (7) |
C1—C2 | 1.377 (7) | C37—C42 | 1.367 (9) |
C1—C6 | 1.376 (8) | C38—C39 | 1.381 (9) |
C2—C3 | 1.395 (9) | C38—H31 | 0.948 |
C2—H1 | 0.956 | C39—C40 | 1.35 (2) |
C3—C4 | 1.34 (1) | C39—H32 | 0.953 |
C3—H2 | 0.951 | C40—C41 | 1.36 (1) |
C4—C5 | 1.36 (1) | C40—H33 | 0.947 |
C4—H3 | 0.947 | C41—C42 | 1.39 (1) |
C5—C6 | 1.387 (8) | C41—H34 | 0.952 |
C5—H4 | 0.955 | C42—H35 | 0.957 |
C6—H5 | 0.961 | C43—C44 | 1.385 (7) |
C7—C8 | 1.387 (8) | C43—C48 | 1.378 (7) |
C7—C12 | 1.376 (7) | C44—C45 | 1.390 (7) |
C8—C9 | 1.39 (1) | C44—H36 | 0.954 |
C8—H6 | 0.955 | C45—C46 | 1.35 (1) |
C9—C10 | 1.36 (1) | C45—H37 | 0.953 |
C9—H7 | 0.944 | C46—C47 | 1.37 (1) |
C10—C11 | 1.35 (1) | C46—H38 | 0.951 |
C10—H8 | 0.948 | C47—C48 | 1.390 (8) |
C11—C12 | 1.39 (1) | C47—H39 | 0.947 |
C11—H9 | 0.954 | C48—H40 | 0.950 |
C12—H10 | 0.943 | C49—C50 | 1.383 (7) |
C13—C14 | 1.389 (7) | C49—C54 | 1.390 (7) |
C13—C18 | 1.379 (6) | C50—C51 | 1.384 (8) |
C14—C15 | 1.390 (7) | C50—H41 | 0.948 |
C14—H11 | 0.948 | C51—C52 | 1.34 (1) |
C15—C16 | 1.354 (10) | C51—H42 | 0.942 |
C15—H12 | 0.954 | C52—C53 | 1.37 (1) |
C16—C17 | 1.380 (9) | C52—H43 | 0.941 |
C16—H13 | 0.952 | C53—C54 | 1.39 (1) |
C17—C18 | 1.389 (7) | C53—H44 | 0.959 |
C17—H14 | 0.950 | C54—H45 | 0.956 |
C18—H15 | 0.948 | C55—C56 | 1.48 (2) |
C19—C20 | 1.385 (7) | C55—H46 | 0.960 |
C19—C24 | 1.392 (7) | C55—H47 | 0.960 |
C20—C21 | 1.385 (8) | C55—H48 | 0.960 |
C20—H16 | 0.949 | C56—C57 | 1.47 (2) |
C21—C22 | 1.357 (9) | C57—H49 | 0.960 |
C21—H17 | 0.935 | C57—H50 | 0.960 |
C22—C23 | 1.37 (1) | C57—H51 | 0.960 |
C22—H18 | 0.947 | ||
Cl3···C4i | 3.492 (7) | O1···C24v | 3.25 (1) |
Cl3···C16ii | 3.539 (6) | O1···C23v | 3.35 (1) |
Cl4···C10iii | 3.499 (10) | O1···C47vi | 3.54 (2) |
Cl5···C28iv | 3.590 (7) | ||
Cl1—Pd1—Cl2 | 82.58 (4) | C21—C22—H18 | 120.8 |
Cl1—Pd1—Cl3 | 92.30 (4) | C23—C22—H18 | 119.2 |
Cl1—Pd1—P1 | 171.78 (4) | C22—C23—C24 | 120.5 (6) |
Cl2—Pd1—Cl3 | 174.50 (4) | C22—C23—H19 | 120.0 |
Cl2—Pd1—P1 | 94.69 (4) | C24—C23—H19 | 119.4 |
Cl3—Pd1—P1 | 90.11 (4) | C19—C24—C23 | 119.8 (5) |
Pd3—Pd2—Cl1 | 51.94 (3) | C19—C24—H20 | 120.0 |
Pd3—Pd2—Cl2 | 48.26 (3) | C23—C24—H20 | 120.2 |
Pd3—Pd2—Cl4 | 129.93 (3) | P2—C25—C26 | 123.0 (4) |
Pd3—Pd2—P2 | 128.68 (3) | P2—C25—C30 | 116.8 (3) |
Cl1—Pd2—Cl2 | 82.40 (3) | C26—C25—C30 | 120.1 (4) |
Cl1—Pd2—Cl4 | 92.40 (3) | C25—C26—C27 | 118.7 (5) |
Cl1—Pd2—P2 | 175.16 (4) | C25—C26—H21 | 121.1 |
Cl2—Pd2—Cl4 | 173.96 (4) | C27—C26—H21 | 120.2 |
Cl2—Pd2—P2 | 95.00 (3) | C26—C27—C28 | 120.9 (6) |
Cl4—Pd2—P2 | 89.97 (4) | C26—C27—H22 | 121.0 |
Pd2—Pd3—Cl1 | 51.68 (2) | C28—C27—H22 | 118.0 |
Pd2—Pd3—Cl2 | 47.98 (2) | C27—C28—C29 | 120.1 (5) |
Pd2—Pd3—Cl5 | 124.95 (3) | C27—C28—H23 | 120.1 |
Pd2—Pd3—P3 | 121.54 (3) | C29—C28—H23 | 119.8 |
Cl1—Pd3—Cl2 | 82.01 (4) | C28—C29—C30 | 120.5 (6) |
Cl1—Pd3—Cl5 | 90.18 (4) | C28—C29—H24 | 118.9 |
Cl1—Pd3—P3 | 172.31 (4) | C30—C29—H24 | 120.5 |
Cl2—Pd3—Cl5 | 171.95 (4) | C25—C30—C29 | 119.6 (5) |
Cl2—Pd3—P3 | 95.42 (4) | C25—C30—H25 | 120.7 |
Cl5—Pd3—P3 | 92.08 (5) | C29—C30—H25 | 119.7 |
Pd1—Cl1—Pd2 | 77.27 (3) | P2—C31—C32 | 121.2 (3) |
Pd1—Cl1—Pd3 | 79.26 (3) | P2—C31—C36 | 120.0 (3) |
Pd2—Cl1—Pd3 | 76.38 (3) | C32—C31—C36 | 118.8 (4) |
Pd1—Cl2—Pd2 | 84.53 (3) | C31—C32—C33 | 120.4 (4) |
Pd1—Cl2—Pd3 | 86.74 (3) | C31—C32—H26 | 120.1 |
Pd2—Cl2—Pd3 | 83.77 (3) | C33—C32—H26 | 119.5 |
Pd1—P1—C1 | 103.0 (1) | C32—C33—C34 | 120.2 (5) |
Pd1—P1—C7 | 118.0 (1) | C32—C33—H27 | 119.8 |
Pd1—P1—C13 | 119.4 (1) | C34—C33—H27 | 120.0 |
C1—P1—C7 | 108.5 (2) | C33—C34—C35 | 119.2 (5) |
C1—P1—C13 | 107.7 (2) | C33—C34—H28 | 120.6 |
C7—P1—C13 | 99.7 (2) | C35—C34—H28 | 120.2 |
Pd2—P2—C19 | 108.0 (1) | C34—C35—C36 | 121.4 (4) |
Pd2—P2—C25 | 111.7 (1) | C34—C35—H29 | 119.5 |
Pd2—P2—C31 | 118.7 (1) | C36—C35—H29 | 119.1 |
C19—P2—C25 | 109.9 (2) | C31—C36—C35 | 119.9 (4) |
C19—P2—C31 | 105.3 (2) | C31—C36—H30 | 120.2 |
C25—P2—C31 | 102.9 (2) | C35—C36—H30 | 119.9 |
Pd3—P3—C37 | 113.4 (2) | P3—C37—C38 | 119.5 (4) |
Pd3—P3—C43 | 107.3 (2) | P3—C37—C42 | 121.6 (4) |
Pd3—P3—C49 | 118.4 (2) | C38—C37—C42 | 118.9 (5) |
C37—P3—C43 | 106.4 (2) | C37—C38—C39 | 119.8 (7) |
C37—P3—C49 | 104.1 (2) | C37—C38—H31 | 120.0 |
C43—P3—C49 | 106.5 (2) | C39—C38—H31 | 120.2 |
P1—C1—C2 | 120.9 (4) | C38—C39—C40 | 121.0 (7) |
P1—C1—C6 | 118.9 (3) | C38—C39—H32 | 119.8 |
C2—C1—C6 | 119.9 (4) | C40—C39—H32 | 119.2 |
C1—C2—C3 | 119.3 (6) | C39—C40—C41 | 119.7 (8) |
C1—C2—H1 | 120.1 | C39—C40—H33 | 119.5 |
C3—C2—H1 | 120.6 | C41—C40—H33 | 120.8 |
C2—C3—C4 | 120.8 (6) | C40—C41—C42 | 120.5 (9) |
C2—C3—H2 | 120.1 | C40—C41—H34 | 119.6 |
C4—C3—H2 | 119.0 | C42—C41—H34 | 119.9 |
C3—C4—C5 | 119.8 (6) | C37—C42—C41 | 120.0 (6) |
C3—C4—H3 | 120.8 | C37—C42—H35 | 120.4 |
C5—C4—H3 | 119.4 | C41—C42—H35 | 119.5 |
C4—C5—C6 | 121.1 (7) | P3—C43—C44 | 118.4 (4) |
C4—C5—H4 | 119.3 | P3—C43—C48 | 123.8 (4) |
C6—C5—H4 | 119.5 | C44—C43—C48 | 117.8 (4) |
C1—C6—C5 | 119.0 (5) | C43—C44—C45 | 121.4 (6) |
C1—C6—H5 | 120.6 | C43—C44—H36 | 119.4 |
C5—C6—H5 | 120.4 | C45—C44—H36 | 119.2 |
P1—C7—C8 | 121.2 (4) | C44—C45—C46 | 119.7 (6) |
P1—C7—C12 | 118.8 (4) | C44—C45—H37 | 119.7 |
C8—C7—C12 | 119.9 (5) | C46—C45—H37 | 120.5 |
C7—C8—C9 | 119.0 (5) | C45—C46—C47 | 120.2 (6) |
C7—C8—H6 | 120.7 | C45—C46—H38 | 120.2 |
C9—C8—H6 | 120.3 | C47—C46—H38 | 119.6 |
C8—C9—C10 | 120.3 (7) | C46—C47—C48 | 120.6 (6) |
C8—C9—H7 | 121.1 | C46—C47—H39 | 120.2 |
C10—C9—H7 | 118.7 | C48—C47—H39 | 119.2 |
C9—C10—C11 | 120.8 (9) | C43—C48—C47 | 120.3 (5) |
C9—C10—H8 | 119.3 | C43—C48—H40 | 120.0 |
C11—C10—H8 | 119.9 | C47—C48—H40 | 119.7 |
C10—C11—C12 | 120.0 (7) | P3—C49—C50 | 120.7 (3) |
C10—C11—H9 | 119.1 | P3—C49—C54 | 120.4 (4) |
C12—C11—H9 | 120.9 | C50—C49—C54 | 118.9 (5) |
C7—C12—C11 | 120.0 (6) | C49—C50—C51 | 120.1 (5) |
C7—C12—H10 | 119.8 | C49—C50—H41 | 120.0 |
C11—C12—H10 | 120.1 | C51—C50—H41 | 120.0 |
P1—C13—C14 | 123.7 (3) | C50—C51—C52 | 121.0 (6) |
P1—C13—C18 | 117.3 (3) | C50—C51—H42 | 120.1 |
C14—C13—C18 | 118.7 (4) | C52—C51—H42 | 118.9 |
C13—C14—C15 | 119.3 (5) | C51—C52—C53 | 120.0 (7) |
C13—C14—H11 | 120.3 | C51—C52—H43 | 120.7 |
C15—C14—H11 | 120.4 | C53—C52—H43 | 119.2 |
C14—C15—C16 | 121.5 (6) | C52—C53—C54 | 120.8 (7) |
C14—C15—H12 | 119.2 | C52—C53—H44 | 120.9 |
C16—C15—H12 | 119.3 | C54—C53—H44 | 118.2 |
C15—C16—C17 | 120.0 (5) | C49—C54—C53 | 119.1 (5) |
C15—C16—H13 | 120.4 | C49—C54—H45 | 120.5 |
C17—C16—H13 | 119.5 | C53—C54—H45 | 120.3 |
C16—C17—C18 | 119.0 (5) | C56—C55—H46 | 109.5 |
C16—C17—H14 | 120.3 | C56—C55—H47 | 109.5 |
C18—C17—H14 | 120.7 | C56—C55—H48 | 109.5 |
C13—C18—C17 | 121.4 (5) | H46—C55—H47 | 109.5 |
C13—C18—H15 | 119.5 | H46—C55—H48 | 109.5 |
C17—C18—H15 | 119.0 | H47—C55—H48 | 109.5 |
P2—C19—C20 | 119.4 (3) | O1—C56—C55 | 130 (1) |
P2—C19—C24 | 121.9 (4) | O1—C56—C57 | 124 (1) |
C20—C19—C24 | 118.7 (5) | C55—C56—C57 | 104 (1) |
C19—C20—C21 | 120.3 (5) | C56—C57—H49 | 109.5 |
C19—C20—H16 | 120.3 | C56—C57—H50 | 109.5 |
C21—C20—H16 | 119.4 | C56—C57—H51 | 109.5 |
C20—C21—C22 | 120.5 (6) | H49—C57—H50 | 109.5 |
C20—C21—H17 | 119.9 | H49—C57—H51 | 109.5 |
C22—C21—H17 | 119.5 | H50—C57—H51 | 109.5 |
C21—C22—C23 | 120.1 (7) |
Symmetry codes: (i) −x, −y+1, −z−1; (ii) x, y, z−1; (iii) −x, −y, −z−1; (iv) −x+1, −y, −z−1; (v) x, y+1, z; (vi) −x+1, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Pd3Cl5(C18H15P)3]·C3H6O |
Mr | 1341.42 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 296 |
a, b, c (Å) | 18.515 (2), 14.295 (3), 10.916 (1) |
α, β, γ (°) | 84.90 (1), 87.874 (9), 77.04 (1) |
V (Å3) | 2803.9 (8) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.31 |
Crystal size (mm) | 0.20 × 0.20 × 0.10 |
Data collection | |
Diffractometer | Rigaku AFC7R diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.728, 0.877 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13420, 12899, 9622 |
Rint | 0.015 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.101, 1.02 |
No. of reflections | 9622 |
No. of parameters | 625 |
No. of restraints | ? |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.44, −0.47 |
Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation & Rigaku Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation & Rigaku Corporation, 1999), DIRDIF92 (PATTY) (Beurskens et al., 1992), TEXSAN and SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), TEXSAN.
Pd1—Pd2 | 3.0818 (5) | Pd2—Cl1 | 2.4735 (9) |
Pd1—Pd3 | 3.1537 (6) | Pd2—Cl2 | 2.2896 (9) |
Pd2—Pd3 | 3.0639 (4) | Pd2—Cl4 | 2.328 (1) |
Pd1—Cl1 | 2.462 (1) | Pd2—P2 | 2.2264 (9) |
Pd1—Cl2 | 2.293 (1) | Pd3—Cl1 | 2.482 (1) |
Pd1—Cl3 | 2.329 (1) | Pd3—Cl2 | 2.300 (1) |
Pd1—P1 | 2.220 (1) | Pd3—Cl5 | 2.323 (1) |
Pd2—Pd3 | 3.0639 (4) | Pd3—P3 | 2.238 (1) |
Cl1—Pd1—Cl2 | 82.58 (4) | Cl2—Pd2—Cl4 | 173.96 (4) |
Cl1—Pd1—Cl3 | 92.30 (4) | Cl2—Pd2—P2 | 95.00 (3) |
Cl1—Pd1—P1 | 171.78 (4) | Cl4—Pd2—P2 | 89.97 (4) |
Cl2—Pd1—Cl3 | 174.50 (4) | Pd2—Pd3—Cl1 | 51.68 (2) |
Cl2—Pd1—P1 | 94.69 (4) | Pd2—Pd3—Cl2 | 47.98 (2) |
Cl3—Pd1—P1 | 90.11 (4) | Pd2—Pd3—Cl5 | 124.95 (3) |
Pd3—Pd2—Cl1 | 51.94 (3) | Pd2—Pd3—P3 | 121.54 (3) |
Pd3—Pd2—Cl2 | 48.26 (3) | Cl1—Pd3—Cl2 | 82.01 (4) |
Pd3—Pd2—Cl4 | 129.93 (3) | Cl1—Pd3—Cl5 | 90.18 (4) |
Pd3—Pd2—P2 | 128.68 (3) | Cl1—Pd3—P3 | 172.31 (4) |
Cl1—Pd2—Cl2 | 82.40 (3) | Cl2—Pd3—Cl5 | 171.95 (4) |
Cl1—Pd2—Cl4 | 92.40 (3) | Cl2—Pd3—P3 | 95.42 (4) |
Cl1—Pd2—P2 | 175.16 (4) | Cl5—Pd3—P3 | 92.08 (5) |
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As far as we know (Allen et al., 1983, 1987), only chalcogen atoms have been reported for µ3-bridging ligands in compounds [M3(µ3-E)2(L)6]2+ (M = Ni, Pd; E = O, S, or Se(SiMe3)2; L = P– or S-centered ligands or halogen anions) (Ghilardi et al., 1978, 1984, 1985; Carmona et al., 1985; Cecconi et al., 1990; Werner et al., 1980; Cowan et al., 1987; Fenske et al., 1990) with a three-fliers-waterwheel structure. As a chalcogen-bridged system has 48 valence electrons, replacing two bridging ligands from chalcogen to halogen causes an addition of two electrons to the trimetal compound, forming a compound with 50-valence electrons. Trimetal compounds with more than 49 valence electrons are rare. To our knowledge, only those containing electronegative cyclopentadienyl (Cp) ligands in cobalt and nickel systems are known to exist (Michael et al., 1990). During the course of our study in trimetal cluster chemistry (Maekawa et al., 1995a,b), we have found a new tripalladium compound with two bridging chlorine atoms, [Pd3(µ3-Cl)2(PPh3)3Cl3].(CH3)2CO, (I). The valence electron count of (I) is 49. We report here the crystal structure and electron spin resonance (ESR) study of (I). \sch
An ORTEPII view of the molecular structure of (I) together with the atom-numbering scheme is shown in Fig. 1. The core framework of Pd3(µ3– Cl)2P3Cl3 is just similar to those of chalcogen-bridged tripalladium compounds, which can be described as three square planar PdPCl3 moieties having two chloride anions in common. One of two bridging chlorine atoms, (Cl1), is located at trans to all phosphorus atoms while the other, (Cl2), is located at cis, which corresponds to a pseudo C3v symmetry for the core framework. The average distance of Pd—Cl1 is 2.473 (8) Å, which is significantly longer than 2.294 (4) Å for that of Pd—Cl2, due to the strong trans effect of a phosphorus atom compared to a chlorine atom. The average Pd—Cl distance of 2.327 (3) Å for terminal chloride anions falls within two Pd—Cl distances for bridging chloride anions. The average Pd—P distance of 2.22 (1) Å is fairly shorter than those reported for chalcogen-bridged tripalladium compounds [2.248 (7)–2.339 (3) Å]. Pd···Pd distances are 3.0817 (5), 3.0638 (4), and 3.1536 (5) Å for Pd1···Pd2, Pd2···Pd3, and Pd1···Pd3, respectively. These values are similar to those reported for chalcogen-bridged tripalladium compounds [3.011 (2)–3.1814 (4) Å], indicating weak Pd···Pd interaction.
In contrast to the chalcogen-bridged trimetal compounds, (I), shows paramagnetic behaviour. The solid state powder ESR spectrum of (I) measured at room temperature shows a rhombic pattern with g1 = 2.144, g2 = 2.044, and g3 = 1.996. The observation of the ESR signal is consistent with the valence electron count of 49 and S = 1/2.