The investigation of the coordination chemistry of heterometallic transition-metal complexes of palladium (Pd) and rhenium (Re) led to the isolation and crystallographic characterization of tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate, [Pd(C5H8N2)4][Re4(CO)16]·2C4H10O or [Pd(IMe)4][Re4(CO)16]·2C4H10O, (1), and dicarbonylocta-μ-carbonyl-tetrakis(triphenylphosphane)palladiumdirhenium, [Pd4Re2(C18H15P)4(CO)10] or Pd4Re2(PPh3)4(μ-CO)8(CO)2, (2), from the reaction of Pd(PPh3)4 with 1,3-dimethylimidazolium-2-carboxylate and Re2(CO)10 in a toluene–acetonitrile mixture.
Keywords: palladium, rhenium, carbonyl, NHC, triphenylphospine, crystal structure
Abstract
The investigation of the coordination chemistry of heterometallic transition-metal complexes of palladium (Pd) and rhenium (Re) led to the isolation and crystallographic characterization of tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate, [Pd(C5H8N2)4][Re4(CO)16]·2C4H10O or [Pd(IMe)4][Re4(CO)16]·2C4H10O, (1), and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium, [Pd4Re2(C18H15P)4(CO)10] or Pd4Re2(PPh3)4(μ-CO)8(CO)2, (2), from the reaction of Pd(PPh3)4 with 1,3-dimethylimidazolium-2-carboxylate and Re2(CO)10 in a toluene–acetonitrile mixture. In complex 1 the Re—Re bond lengths [2.9767 (3)–3.0133 (2) Å] are close to double the covalent Re radii (1.51 Å). The palladium–rhenium carbonyl cluster 2 has not been structurally characterized previously; the Pd—Re bond lengths [2.7582 (2)–2.7796 (2) Å] are about 0.1 Å shorter than the sum of the covalent Pd and Re radii (1.39 + 1.51 = 2.90 Å). One carbene ligand and a diethyl ether molecule are disordered over two positions with occupancy ratios of 0.5:0.5 and 0.625 (15):0.375 (15) in 1. An unidentified solvent is present in compound 2. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s). The SQUEEZE routine [Spek (2015 ▸). Acta Cryst. C71, 9–18] in PLATON was used to remove the contribution of the electron density in the solvent region from the intensity data and the solvent-free model was employed for the final refinement. The cavity with a volume of ca 311 Å3 contains approximately 98 electrons.
Chemical context
Bimetallic catalysts comprising palladium (Pd) and rhenium (Re) have important applications in alkane reforming, industrial chemical production, hydrodechlorination and biomass conversion (Thompson & Lamb, 2016 ▸; Bonarowska et al., 1999 ▸; Malinowski et al., 1998 ▸; Juszczyk & Karpiński, 2001 ▸). Heterometallic Pd–Re clusters are suitable precursors for such a catalytic system. We found that the reaction of Pd(PPh3)4 with 1,3-dimethylimidazolium-2-carboxylate and Re2(CO)10 in a toluene–acetonitrile mixture produces a mixture of two compounds: [Pd(IMe)4][Re4(CO)16]·2C4H10O (1) and Pd4Re2(PPh3)4(μ-CO)8(CO)2 (2) where IMe is 1,3-dimethylimidazolium-2-ylidene. Two other products, triphenylphosphine oxide and the known complex Re2(CO)8(PPh3)2 (Adams et al., 2013 ▸) were isolated from the reaction mixture.
Structural commentary
The displacement ellipsoid plot of 1 is depicted in Fig. 1 ▸. The molecular unit of 1 comprises a palladium(II) cation with four coordinated N-heterocyclic carbenes (NHC) lying on a twofold rotoinversion axis, and one [Re4(CO)16] anion. The geometry around the Pd atom is square-planar with one carbene unit being disordered. The C—Pd—C angles range from 86.9 (4) to 97.7 (4)°. The cluster anion lying on the inversion center has a perfectly flat rhombus geometry with the shortest Re—Re bond [2.9767 (3) Å] corresponding to the short diagonal. The other four Re—Re bond lengths [3.001 (2)–3.0132 (2) Å] are also close to double the covalent Re radii (1.51 Å; Cordero et al., 2008 ▸). The Re—Re—Re angles are 59.330 (6)–60.542 (6)°.
Figure 1.
Displacement ellipsoid plot of Pd(IMe)4Re4(CO)16·2C4H10O (1), drawn at the 30% probability level. All hydrogen atoms and solvent molecules are omitted for clarity.
The displacement ellipsoid plot of 2 is depicted in Fig. 2 ▸. The geometry of the Re2Pd4 core is found to be slightly distorted from that of a D 4h -symmetric tetragonal–bipyramidal prism. In complex 2, the Pd—Re bond lengths [2.7582 (2)–2.7796 (2) Å] are close to the sum of the covalent Pd and Re radii (1.39 + 1.51 = 2.90 Å). In comparison, the Pd—Re bond lengths in the PdRe4(CO)16(μ-SbPh2)2(μ-H)2 cluster (Adams et al., 2015 ▸) are in the range 2.9348 (18)–2.9823 (19) Å. The Pd4 fragment has an almost square geometry [the Pd—Pd—Pd angles are 89.865 (6)–90.135 (6)° and the Pd—Pd bond lengths are 2.9678 (2)–2.99 (2) Å].
Figure 2.
Displacement ellipsoid plot of Pd4Re2(PPh3)4(μ-CO)8(CO)2 (2), drawn at the 30% probability level. All hydrogen atoms are omitted for clarity.
Supramolecular features
In the ionic crystal of 1, each cation is surrounded by six anions and vice versa (Fig. 3 ▸). No classical hydrogen-bonding interactions are observed between cations and anions, but many carbonyl-O⋯H3C and carbonyl-O⋯HC intermolecular contacts (Table 1 ▸) are present. The diethyl ether molecule resides in voids between four adjacent cations and anions featuring an O⋯HC contact (2.32 Å) with one of the carbenes at the palladium atom. No π–π stacking is observed in structure 2, but several weak C—H⋯π and C—H⋯OC contacts (Fig. 4 ▸ and Table 2 ▸) are present. The axial CO groups of the Re(CO)5 fragments point towards voids filled with an unidentified solvent (Fig. 5 ▸).
Figure 3.
A view of the packing of compound 1.
Table 1. Hydrogen-bond geometry (Å, °) for 1 .
| D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A |
|---|---|---|---|---|
| C11—H11A⋯O4i | 0.98 | 2.49 | 3.436 (6) | 161 |
| C13—H13⋯O9ii | 0.95 | 2.44 | 3.36 (3) | 165 |
| C13—H13⋯O9A ii | 0.95 | 2.32 | 3.25 (5) | 163 |
| C15—H15A⋯O6iii | 0.98 | 2.44 | 3.326 (5) | 150 |
| C16—H16B⋯O9 | 0.98 | 2.57 | 3.49 (3) | 158 |
| C18—H18⋯O7iv | 0.95 | 2.43 | 3.230 (9) | 141 |
| C19—H19⋯O7iii | 0.95 | 2.56 | 3.483 (16) | 163 |
| C20—H20C⋯O5v | 0.98 | 2.35 | 3.203 (12) | 145 |
| C21—H21A⋯O2vi | 0.98 | 2.54 | 3.413 (11) | 149 |
| C21—H21C⋯O5 | 0.98 | 2.59 | 3.494 (12) | 153 |
| C24—H24B⋯O8vii | 0.99 | 2.58 | 3.473 (12) | 150 |
Symmetry codes: (i) -x, -y+1, -z; (ii) -x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1; (iii) x, -y+2, z+{\script{1\over 2}}; (iv) -x, -y+2, -z; (v) -x, y, -z+{\script{1\over 2}}; (vi) -x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}; (vii) x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}.
Figure 4.
A view of the packing of compound 2.
Table 2. Hydrogen-bond geometry (Å, °) for 2 .
Cg1 and Cg3 are the centroids of the C6–C11 and C18–C23 rings, respectively.
| D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A |
|---|---|---|---|---|
| C9—H9⋯O5i | 0.95 | 2.49 | 3.188 (3) | 130 |
| C39—H39⋯O2ii | 0.95 | 2.60 | 3.491 (4) | 157 |
| C20—H20⋯Cg1iii | 0.95 | 2.84 | 3.635 (3) | 142 |
| C34—H34⋯Cg3iv | 0.95 | 2.90 | 3.683 (3) | 140 |
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x, -y+1, -z+2; (iii) -x+1, -y+2, -z+1; (iv) x, y-1, z.
Figure 5.
The axial CO groups of the Re(CO)5 fragments in 2 point towards voids filled with an unidentified solvent.
Database survey
A search for related structures of palladium cations in the Cambridge Structural Database (CSD Version 5.42, update of November 2020; Groom et al., 2016 ▸) resulted in 27 hits. Of the structures found, the closest structures considering the connectivity of the atoms are tetrakis(N-methylimidazolin-2-ylidene)palladium(II) diiodide (JOKCIV; Fehlhammer et al., 1992 ▸) and bis[methylenebis(3-methylimidazol-2-ylidene)]palladium(II) diiodide dimethylsulfoxide solvate (REFQID; Heckenroth et al., 2006 ▸). The cation in 1 is the first structurally characterized palladium complex ion containing four NHC ligands with substituents at the 1,3 positions of the imidazole ring. There are a number of compounds containing the tetranuclear [Re4(CO)16]2− anion, which is also found in the compound reported here. A search of the CSD found two closely related cluster compounds, viz. bis(tetraethylammonium) hexadecacarbonyl-tetrarhenium (EAMCRE; Ciani et al., 1978 ▸) and bis(tetra-n-butylammonium)hexadecacarbonyltetrarhenium (BATCRE10; Churchill & Bau, 1968 ▸). The palladium–rhenium carbonyl cluster in 2 has not been structurally characterized previously.
Synthesis and crystallization
Under a nitrogen atmosphere, Pd(PPh3)4 (241 mg, 0.185 mmol) was added to a toluene–acetonitrile mixture (8 and 6 mL, respectively) and 1,3-dimethylimidazolium-2-carboxylate (104 mg, 0.704 mmol). The reaction mixture was refluxed for 1.5 h, then Re2(CO)10 (242 mg, 0.141 mmol) was added, the solution turned dark red and the solvents were removed in vacuo. The solid was washed with benzene (3 × 5 ml) and recrystallized from an acetonitrile–diethylether mixture. X-ray quality crystals of Pd(IMe)4Re4(CO)16·2C4H10O (37 mg, 13%) were grown from a dichloromethane–diethylether mixture at 277 K. 1HNMR (300.13 MHz, DMSO-d 6, ppm): 3.41 (s, 24H, 8Me), 7.37 (s, 8H, 8CH). 13C{H} NMR (75.4 MHz, DMSO-d 6, ppm): 36.9 (Me, IMe), 123.5 (CH, IMe), 168.0 (C, IMe), 197.7 (CO), 198.7 (CO), 201.1 (CO), 218.6 (CO) IR (ATR, ν, cm−1): 3152 (w, br), 1998 (vw), 1974 (vw), 1955 (m), 1927 (vw), 1912 (vw), 1881 (vs, br), 1858 (vw), 1575 (vw), 1465 (w), 1400 (vw), 1332 (vw), 1229 (m), 1131 (vw), 1083 (vw), 1013 (vw), 845 (vw), 736 (s), 701 (vw), 681 (m), 600 (w), 577 (s), 560 (vw), 508 (vw), 496 (vw), 464 (w), 436 (vw), 411 (w).
A few crystals of Pd4Re2(PPh3)4(m-CO)8(CO)2 suitable for X-ray diffraction analysis were obtained from a yellow benzene solution, after several days, by slow ether diffusion into a concentrated solution of benzene at 277 K. IR (ATR, ν, cm−1): 3850 (vw), 3054 (vw, br), 2955 (vw, br), 1986 (s), 1821 (vs, br), 1585 (vw), 1571 (vw), 1515 (vw), 1477 (w), 1434 (m), 1307 (vw), 1263 (vw), 1236 (vw, br), 1182 (vw), 1159 (vw), 1119 (vw), 1092 (m), 1071 (vw), 1026 (vw), 997 (w), 907 (vw), 846 (vw), 741 (m), 690 (vs), 618 (vw), 565 (w), 541 (vw), 496 (m), 412 (vw).
Triphenylphosphine oxide (14 mg, 28%) and Re2(CO)8(PPh3)2 (29 mg, 14%) were also isolated from this crystallization.
Refinement
Crystal data, data collection and structure refinement details are summarized in Table 3 ▸. All H atoms were positioned geometrically and refined using a riding model, with C—H = 0.95 Å (sp
2), 0.98 Å (methyl) and 0.99 Å (methylene), with common isotropic temperature factors for all hydrogen atoms of the aromatic rings and methyl groups. SADI restraints on bond lengths and DELU restraints on anisotropic thermal parameters were used to model the disordered carbene ligand and diethyl ether molecule over two positions. For the refinement of 2, four reflections (100, 010, 200, 0
1) were omitted because they showed a significantly lower intensity than calculated, most probably caused by obstruction from the beam stop. The residual electron density in 2 was difficult to model and therefore, the SQUEEZE routine (Spek, 2015 ▸) in PLATON (Spek, 2020 ▸) was used to remove the contribution of the electron density in the solvent region from the intensity data and the solvent-free model was employed for the final refinement. The cavity with a volume of ca 311 Å3 contains approximately 98 electrons.
Table 3. Experimental details.
| 1 | 2 | |
|---|---|---|
| Crystal data | ||
| Chemical formula | [Pd(C5H8N2)4][Re4(CO)16]·2C4H10O | [Pd4Re2(C18H15P)4(CO)10] |
| M r | 1832.13 | 2127.18 |
| Crystal system, space group | Monoclinic, C2/c | Triclinic, P\overline{1} |
| Temperature (K) | 100 | 100 |
| a, b, c (Å) | 21.1079 (9), 14.0026 (6), 19.4346 (8) | 12.9278 (4), 13.5132 (5), 14.1184 (5) |
| α, β, γ (°) | 90, 109.342 (1), 90 | 105.983 (1), 108.510 (1), 106.129 (1) |
| V (Å3) | 5420.0 (4) | 2060.09 (12) |
| Z | 4 | 1 |
| Radiation type | Mo Kα | Mo Kα |
| μ (mm−1) | 9.30 | 3.91 |
| Crystal size (mm) | 0.17 × 0.11 × 0.03 | 0.23 × 0.18 × 0.18 |
| Data collection | ||
| Diffractometer | Bruker APEXII CCD | Bruker APEXII CCD |
| Absorption correction | Multi-scan (SADABS; Krause et al., 2015 ▸) | Multi-scan (SADABS; Krause et al., 2015 ▸) |
| Tmin, Tmax | 0.285, 0.746 | 0.515, 0.746 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 128368, 9046, 7392 | 151194, 11588, 10906 |
| R int | 0.087 | 0.042 |
| (sin θ/λ)max (Å−1) | 0.736 | 0.696 |
| Refinement | ||
| R[F2 > 2σ(F 2)], wR(F 2), S | 0.028, 0.065, 1.06 | 0.018, 0.042, 1.10 |
| No. of reflections | 9046 | 11588 |
| No. of parameters | 427 | 461 |
| No. of restraints | 45 | 0 |
| H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 1.43, −1.83 | 0.95, −0.70 |
Supplementary Material
Crystal structure: contains datablock(s) global, 1, 2. DOI: 10.1107/S2056989021009270/tx2041sup1.cif
Structure factors: contains datablock(s) 1. DOI: 10.1107/S2056989021009270/tx20411sup2.hkl
Structure factors: contains datablock(s) 2. DOI: 10.1107/S2056989021009270/tx20412sup3.hkl
Additional supporting information: crystallographic information; 3D view; checkCIF report
Acknowledgments
This work was carried out on equipment of the Center for Collective Use of the Kurnakov Institute of General and Inorganic Chemistry (Russian Academy of Sciences).
supplementary crystallographic information
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1). Crystal data
| [Pd(C5H8N2)4][Re4(CO)16]·2C4H10O | F(000) = 3448 |
| Mr = 1832.13 | Dx = 2.245 Mg m−3 |
| Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
| a = 21.1079 (9) Å | Cell parameters from 9678 reflections |
| b = 14.0026 (6) Å | θ = 2.9–31.5° |
| c = 19.4346 (8) Å | µ = 9.30 mm−1 |
| β = 109.342 (1)° | T = 100 K |
| V = 5420.0 (4) Å3 | Plate, brownish yellow |
| Z = 4 | 0.17 × 0.11 × 0.03 mm |
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1). Data collection
| Bruker APEXII CCD diffractometer | 7392 reflections with I > 2σ(I) |
| φ and ω scans | Rint = 0.087 |
| Absorption correction: multi-scan (SADABS; Krause et al., 2015) | θmax = 31.5°, θmin = 1.8° |
| Tmin = 0.285, Tmax = 0.746 | h = −31→31 |
| 128368 measured reflections | k = −20→20 |
| 9046 independent reflections | l = −28→28 |
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1). Refinement
| Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
| Least-squares matrix: full | H-atom parameters constrained |
| R[F2 > 2σ(F2)] = 0.028 | w = 1/[σ2(Fo2) + (0.0239P)2 + 18.7547P] where P = (Fo2 + 2Fc2)/3 |
| wR(F2) = 0.065 | (Δ/σ)max = 0.002 |
| S = 1.06 | Δρmax = 1.43 e Å−3 |
| 9046 reflections | Δρmin = −1.83 e Å−3 |
| 427 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 45 restraints | Extinction coefficient: 0.000167 (12) |
| Primary atom site location: dual |
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1). Special details
| Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1). Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| Re1 | 0.24123 (2) | 0.64550 (2) | 0.00757 (2) | 0.01933 (4) | |
| Re2 | 0.12119 (2) | 0.77460 (2) | −0.02794 (2) | 0.01862 (4) | |
| O1 | 0.26345 (18) | 0.6591 (2) | 0.17414 (18) | 0.0402 (8) | |
| O2 | 0.33004 (14) | 0.4665 (2) | 0.04457 (16) | 0.0282 (6) | |
| O3 | 0.21798 (18) | 0.6155 (2) | −0.15832 (16) | 0.0395 (8) | |
| O4 | 0.12446 (17) | 0.5083 (3) | −0.0062 (3) | 0.0723 (15) | |
| O5 | 0.14525 (17) | 0.7926 (3) | 0.13868 (17) | 0.0467 (9) | |
| O6 | 0.02877 (15) | 0.9489 (2) | −0.05934 (19) | 0.0360 (7) | |
| O7 | 0.09872 (16) | 0.7518 (2) | −0.19407 (16) | 0.0298 (6) | |
| O8 | 0.00308 (15) | 0.6418 (2) | −0.03953 (18) | 0.0344 (7) | |
| C1 | 0.2553 (2) | 0.6594 (3) | 0.1126 (2) | 0.0259 (8) | |
| C2 | 0.30013 (19) | 0.5380 (3) | 0.0300 (2) | 0.0222 (7) | |
| C3 | 0.2273 (2) | 0.6311 (3) | −0.0977 (2) | 0.0265 (8) | |
| C4 | 0.1656 (2) | 0.5633 (3) | −0.0026 (3) | 0.0436 (13) | |
| C5 | 0.1390 (2) | 0.7867 (3) | 0.0783 (2) | 0.0284 (8) | |
| C6 | 0.06388 (19) | 0.8834 (3) | −0.0472 (2) | 0.0265 (8) | |
| C7 | 0.10950 (19) | 0.7595 (3) | −0.1328 (2) | 0.0203 (7) | |
| C8 | 0.0477 (2) | 0.6912 (3) | −0.0359 (2) | 0.0240 (7) | |
| Pd1 | 0.0000 | 0.73266 (3) | 0.2500 | 0.01708 (8) | |
| N1 | 0.01104 (15) | 0.5294 (2) | 0.20006 (16) | 0.0208 (6) | |
| N2 | 0.08671 (16) | 0.7599 (2) | 0.40944 (16) | 0.0207 (6) | |
| N3 | 0.14126 (16) | 0.6837 (3) | 0.35200 (18) | 0.0264 (7) | |
| C9 | 0.0000 | 0.5885 (3) | 0.2500 | 0.0163 (9) | |
| C10 | 0.0072 (2) | 0.4355 (3) | 0.2188 (2) | 0.0291 (8) | |
| H10 | 0.0135 | 0.3810 | 0.1927 | 0.035* | |
| C11 | 0.0244 (2) | 0.5602 (3) | 0.1342 (2) | 0.0280 (8) | |
| H11A | −0.0169 | 0.5553 | 0.0921 | 0.042* | |
| H11B | 0.0591 | 0.5194 | 0.1264 | 0.042* | |
| H11C | 0.0399 | 0.6266 | 0.1400 | 0.042* | |
| C12 | 0.08194 (18) | 0.7269 (3) | 0.34247 (19) | 0.0197 (7) | |
| C13 | 0.1480 (2) | 0.7374 (3) | 0.4598 (2) | 0.0272 (8) | |
| H13 | 0.1630 | 0.7529 | 0.5102 | 0.033* | |
| C14 | 0.1825 (2) | 0.6895 (3) | 0.4242 (2) | 0.0306 (9) | |
| H14 | 0.2265 | 0.6643 | 0.4445 | 0.037* | |
| C15 | 0.0357 (2) | 0.8150 (3) | 0.4261 (2) | 0.0263 (8) | |
| H15A | 0.0515 | 0.8807 | 0.4381 | 0.040* | |
| H15B | 0.0265 | 0.7864 | 0.4678 | 0.040* | |
| H15C | −0.0055 | 0.8154 | 0.3837 | 0.040* | |
| C16 | 0.1617 (2) | 0.6371 (4) | 0.2951 (3) | 0.0372 (11) | |
| H16A | 0.1578 | 0.5677 | 0.2988 | 0.056* | |
| H16B | 0.2084 | 0.6538 | 0.3015 | 0.056* | |
| H16C | 0.1327 | 0.6587 | 0.2471 | 0.056* | |
| N4 | −0.0689 (5) | 0.9322 (6) | 0.2333 (5) | 0.0253 (17) | 0.5 |
| N5 | 0.0364 (4) | 0.9444 (6) | 0.2548 (5) | 0.0250 (16) | 0.5 |
| C17 | −0.0127 (4) | 0.8789 (5) | 0.2461 (10) | 0.0184 (18) | 0.5 |
| C18 | −0.0558 (5) | 1.0282 (6) | 0.2331 (5) | 0.038 (2) | 0.5 |
| H18 | −0.0875 | 1.0788 | 0.2239 | 0.045* | 0.5 |
| C19 | 0.0112 (8) | 1.0359 (6) | 0.2485 (19) | 0.037 (4) | 0.5 |
| H19 | 0.0361 | 1.0935 | 0.2541 | 0.044* | 0.5 |
| C20 | −0.1373 (5) | 0.8957 (8) | 0.2173 (6) | 0.034 (2) | 0.5 |
| H20A | −0.1550 | 0.8755 | 0.1662 | 0.051* | 0.5 |
| H20B | −0.1659 | 0.9462 | 0.2261 | 0.051* | 0.5 |
| H20C | −0.1367 | 0.8411 | 0.2491 | 0.051* | 0.5 |
| C21 | 0.1067 (6) | 0.9243 (7) | 0.2723 (6) | 0.030 (2) | 0.5 |
| H21A | 0.1261 | 0.9091 | 0.3243 | 0.045* | 0.5 |
| H21B | 0.1295 | 0.9803 | 0.2612 | 0.045* | 0.5 |
| H21C | 0.1126 | 0.8698 | 0.2433 | 0.045* | 0.5 |
| O9 | 0.3252 (14) | 0.7269 (9) | 0.3616 (17) | 0.034 (3) | 0.625 (15) |
| C23 | 0.3548 (9) | 0.5629 (10) | 0.3719 (8) | 0.038 (3) | 0.625 (15) |
| H23A | 0.3132 | 0.5457 | 0.3330 | 0.057* | 0.625 (15) |
| H23B | 0.3473 | 0.5604 | 0.4191 | 0.057* | 0.625 (15) |
| H23C | 0.3903 | 0.5177 | 0.3721 | 0.057* | 0.625 (15) |
| C22 | 0.3752 (7) | 0.6610 (9) | 0.3592 (8) | 0.027 (3) | 0.625 (15) |
| H22A | 0.4184 | 0.6774 | 0.3970 | 0.033* | 0.625 (15) |
| H22B | 0.3815 | 0.6642 | 0.3110 | 0.033* | 0.625 (15) |
| C24 | 0.3390 (5) | 0.8233 (8) | 0.3464 (6) | 0.032 (2) | 0.625 (15) |
| H24A | 0.3523 | 0.8250 | 0.3021 | 0.038* | 0.625 (15) |
| H24B | 0.3766 | 0.8490 | 0.3877 | 0.038* | 0.625 (15) |
| C25 | 0.2780 (5) | 0.8827 (7) | 0.3352 (5) | 0.045 (2) | 0.625 (15) |
| H25A | 0.2418 | 0.8594 | 0.2924 | 0.068* | 0.625 (15) |
| H25B | 0.2881 | 0.9493 | 0.3274 | 0.068* | 0.625 (15) |
| H25C | 0.2639 | 0.8784 | 0.3783 | 0.068* | 0.625 (15) |
| O9A | 0.333 (3) | 0.7156 (16) | 0.371 (3) | 0.033 (6) | 0.375 (15) |
| C22A | 0.3655 (13) | 0.6404 (13) | 0.3477 (13) | 0.029 (5) | 0.375 (15) |
| H22C | 0.4123 | 0.6592 | 0.3540 | 0.035* | 0.375 (15) |
| H22D | 0.3422 | 0.6280 | 0.2952 | 0.035* | 0.375 (15) |
| C24A | 0.3289 (11) | 0.8017 (10) | 0.3296 (9) | 0.027 (4) | 0.375 (15) |
| H24C | 0.2916 | 0.7966 | 0.2827 | 0.032* | 0.375 (15) |
| H24D | 0.3712 | 0.8108 | 0.3188 | 0.032* | 0.375 (15) |
| C23A | 0.3655 (13) | 0.5520 (12) | 0.3901 (11) | 0.020 (3) | 0.375 (15) |
| H23D | 0.3939 | 0.5037 | 0.3783 | 0.030* | 0.375 (15) |
| H23E | 0.3195 | 0.5277 | 0.3776 | 0.030* | 0.375 (15) |
| H23F | 0.3831 | 0.5665 | 0.4424 | 0.030* | 0.375 (15) |
| C25A | 0.3175 (8) | 0.8841 (9) | 0.3715 (8) | 0.037 (4) | 0.375 (15) |
| H25D | 0.3118 | 0.9421 | 0.3419 | 0.056* | 0.375 (15) |
| H25E | 0.3562 | 0.8918 | 0.4161 | 0.056* | 0.375 (15) |
| H25F | 0.2770 | 0.8731 | 0.3844 | 0.056* | 0.375 (15) |
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1). Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Re1 | 0.01832 (7) | 0.01206 (7) | 0.02740 (8) | 0.00109 (5) | 0.00727 (5) | −0.00045 (5) |
| Re2 | 0.01763 (7) | 0.01595 (7) | 0.02291 (7) | 0.00130 (5) | 0.00757 (5) | −0.00270 (5) |
| O1 | 0.053 (2) | 0.039 (2) | 0.0373 (17) | 0.0041 (16) | 0.0264 (16) | 0.0060 (14) |
| O2 | 0.0337 (15) | 0.0177 (14) | 0.0362 (15) | 0.0062 (12) | 0.0156 (12) | 0.0079 (12) |
| O3 | 0.052 (2) | 0.0295 (17) | 0.0295 (16) | 0.0116 (15) | 0.0032 (14) | −0.0019 (13) |
| O4 | 0.0295 (17) | 0.0229 (19) | 0.163 (5) | −0.0023 (14) | 0.029 (2) | −0.004 (2) |
| O5 | 0.0373 (18) | 0.075 (3) | 0.0284 (16) | 0.0133 (18) | 0.0116 (14) | −0.0083 (17) |
| O6 | 0.0276 (14) | 0.0205 (15) | 0.059 (2) | 0.0059 (12) | 0.0128 (14) | −0.0041 (14) |
| O7 | 0.0361 (16) | 0.0266 (16) | 0.0279 (15) | 0.0001 (12) | 0.0122 (12) | 0.0020 (12) |
| O8 | 0.0324 (15) | 0.0296 (17) | 0.0465 (18) | −0.0084 (13) | 0.0202 (14) | −0.0073 (14) |
| C1 | 0.0295 (19) | 0.0196 (19) | 0.035 (2) | 0.0015 (15) | 0.0191 (17) | 0.0027 (16) |
| C2 | 0.0258 (17) | 0.0211 (19) | 0.0217 (16) | −0.0004 (14) | 0.0107 (14) | 0.0010 (14) |
| C3 | 0.0299 (19) | 0.0134 (18) | 0.032 (2) | 0.0042 (15) | 0.0052 (16) | −0.0015 (15) |
| C4 | 0.026 (2) | 0.016 (2) | 0.088 (4) | 0.0035 (17) | 0.018 (2) | 0.001 (2) |
| C5 | 0.0239 (18) | 0.030 (2) | 0.032 (2) | 0.0046 (16) | 0.0101 (16) | −0.0061 (17) |
| C6 | 0.0214 (17) | 0.023 (2) | 0.036 (2) | −0.0010 (15) | 0.0117 (16) | −0.0049 (17) |
| C7 | 0.0233 (17) | 0.0119 (16) | 0.0270 (18) | 0.0007 (13) | 0.0099 (14) | 0.0018 (13) |
| C8 | 0.0289 (18) | 0.0175 (18) | 0.0281 (19) | 0.0023 (15) | 0.0127 (15) | −0.0021 (15) |
| Pd1 | 0.02756 (18) | 0.00932 (17) | 0.01613 (16) | 0.000 | 0.00962 (14) | 0.000 |
| N1 | 0.0257 (15) | 0.0122 (14) | 0.0230 (14) | −0.0005 (12) | 0.0062 (12) | −0.0024 (12) |
| N2 | 0.0265 (15) | 0.0175 (16) | 0.0190 (14) | −0.0068 (12) | 0.0085 (12) | −0.0013 (11) |
| N3 | 0.0223 (15) | 0.0286 (19) | 0.0294 (17) | −0.0082 (13) | 0.0101 (13) | −0.0123 (14) |
| C9 | 0.015 (2) | 0.012 (2) | 0.020 (2) | 0.000 | 0.0026 (17) | 0.000 |
| C10 | 0.042 (2) | 0.0100 (17) | 0.033 (2) | 0.0016 (16) | 0.0093 (18) | −0.0034 (15) |
| C11 | 0.036 (2) | 0.022 (2) | 0.0274 (19) | 0.0000 (17) | 0.0123 (17) | −0.0041 (16) |
| C12 | 0.0253 (17) | 0.0152 (17) | 0.0201 (16) | −0.0068 (14) | 0.0096 (14) | −0.0023 (13) |
| C13 | 0.031 (2) | 0.026 (2) | 0.0219 (17) | −0.0112 (16) | 0.0042 (15) | −0.0039 (15) |
| C14 | 0.0220 (18) | 0.031 (2) | 0.034 (2) | −0.0065 (16) | 0.0023 (16) | −0.0061 (18) |
| C15 | 0.033 (2) | 0.026 (2) | 0.0236 (18) | −0.0035 (17) | 0.0148 (16) | −0.0063 (16) |
| C16 | 0.025 (2) | 0.047 (3) | 0.041 (2) | −0.0039 (19) | 0.0137 (18) | −0.019 (2) |
| N4 | 0.035 (4) | 0.023 (4) | 0.021 (4) | 0.014 (4) | 0.012 (5) | 0.004 (3) |
| N5 | 0.041 (4) | 0.020 (4) | 0.019 (4) | −0.005 (3) | 0.017 (4) | −0.004 (3) |
| C17 | 0.030 (6) | 0.015 (3) | 0.013 (4) | 0.004 (3) | 0.011 (7) | 0.000 (3) |
| C18 | 0.074 (6) | 0.019 (4) | 0.026 (5) | 0.018 (4) | 0.024 (5) | 0.010 (3) |
| C19 | 0.068 (9) | 0.016 (3) | 0.029 (4) | −0.001 (5) | 0.020 (12) | −0.001 (5) |
| C20 | 0.039 (5) | 0.041 (7) | 0.027 (5) | 0.018 (4) | 0.017 (5) | 0.009 (5) |
| C21 | 0.043 (5) | 0.020 (5) | 0.032 (5) | −0.017 (5) | 0.018 (6) | −0.003 (4) |
| O9 | 0.038 (5) | 0.033 (5) | 0.037 (9) | −0.011 (5) | 0.021 (6) | −0.010 (5) |
| C23 | 0.043 (8) | 0.046 (5) | 0.022 (7) | 0.000 (5) | 0.008 (6) | 0.001 (4) |
| C22 | 0.021 (4) | 0.036 (5) | 0.026 (5) | −0.005 (4) | 0.010 (4) | −0.005 (4) |
| C24 | 0.035 (4) | 0.036 (5) | 0.023 (5) | −0.008 (4) | 0.006 (4) | −0.006 (4) |
| C25 | 0.050 (6) | 0.043 (5) | 0.038 (5) | 0.002 (4) | 0.008 (4) | −0.006 (4) |
| O9A | 0.055 (15) | 0.022 (5) | 0.028 (9) | 0.000 (6) | 0.022 (10) | 0.002 (5) |
| C22A | 0.037 (11) | 0.028 (8) | 0.019 (8) | 0.001 (7) | 0.005 (7) | 0.003 (7) |
| C24A | 0.044 (9) | 0.016 (6) | 0.015 (7) | −0.005 (6) | 0.002 (6) | −0.006 (4) |
| C23A | 0.023 (7) | 0.023 (6) | 0.009 (8) | −0.007 (5) | −0.001 (6) | −0.005 (5) |
| C25A | 0.044 (8) | 0.024 (6) | 0.046 (8) | 0.005 (5) | 0.016 (7) | −0.006 (5) |
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1). Geometric parameters (Å, º)
| Re1—Re1i | 2.9767 (3) | C16—H16B | 0.9800 |
| Re1—Re2i | 3.0133 (2) | C16—H16C | 0.9800 |
| Re1—Re2 | 3.0011 (2) | N4—C17 | 1.353 (9) |
| Re1—C1 | 1.973 (4) | N4—C18 | 1.373 (11) |
| Re1—C2 | 1.909 (4) | N4—C20 | 1.464 (11) |
| Re1—C3 | 1.978 (4) | N5—C17 | 1.352 (9) |
| Re1—C4 | 1.925 (5) | N5—C19 | 1.378 (11) |
| Re2—Re1i | 3.0134 (2) | N5—C21 | 1.436 (11) |
| Re2—C5 | 1.980 (4) | C18—H18 | 0.9500 |
| Re2—C6 | 1.904 (4) | C18—C19 | 1.349 (15) |
| Re2—C7 | 1.982 (4) | C19—H19 | 0.9500 |
| Re2—C8 | 1.908 (4) | C20—H20A | 0.9800 |
| O1—C1 | 1.150 (5) | C20—H20B | 0.9800 |
| O2—C2 | 1.167 (5) | C20—H20C | 0.9800 |
| O3—C3 | 1.150 (5) | C21—H21A | 0.9800 |
| O4—C4 | 1.145 (6) | C21—H21B | 0.9800 |
| O5—C5 | 1.139 (5) | C21—H21C | 0.9800 |
| O6—C6 | 1.153 (5) | O9—C22 | 1.415 (12) |
| O7—C7 | 1.140 (5) | O9—C24 | 1.431 (12) |
| O8—C8 | 1.151 (5) | C23—H23A | 0.9800 |
| Pd1—C9 | 2.019 (5) | C23—H23B | 0.9800 |
| Pd1—C12ii | 2.042 (4) | C23—H23C | 0.9800 |
| Pd1—C12 | 2.042 (4) | C23—C22 | 1.486 (12) |
| Pd1—C17 | 2.064 (6) | C22—H22A | 0.9900 |
| N1—C9 | 1.353 (4) | C22—H22B | 0.9900 |
| N1—C10 | 1.375 (5) | C24—H24A | 0.9900 |
| N1—C11 | 1.464 (5) | C24—H24B | 0.9900 |
| N2—C12 | 1.353 (4) | C24—C25 | 1.488 (12) |
| N2—C13 | 1.375 (5) | C25—H25A | 0.9800 |
| N2—C15 | 1.446 (5) | C25—H25B | 0.9800 |
| N3—C12 | 1.347 (5) | C25—H25C | 0.9800 |
| N3—C14 | 1.387 (5) | O9A—C22A | 1.413 (16) |
| N3—C16 | 1.467 (5) | O9A—C24A | 1.439 (16) |
| C9—N1ii | 1.353 (4) | C22A—H22C | 0.9900 |
| C10—C10ii | 1.343 (8) | C22A—H22D | 0.9900 |
| C10—H10 | 0.9500 | C22A—C23A | 1.487 (15) |
| C11—H11A | 0.9800 | C24A—H24C | 0.9900 |
| C11—H11B | 0.9800 | C24A—H24D | 0.9900 |
| C11—H11C | 0.9800 | C24A—C25A | 1.479 (14) |
| C13—H13 | 0.9500 | C23A—H23D | 0.9800 |
| C13—C14 | 1.338 (6) | C23A—H23E | 0.9800 |
| C14—H14 | 0.9500 | C23A—H23F | 0.9800 |
| C15—H15A | 0.9800 | C25A—H25D | 0.9800 |
| C15—H15B | 0.9800 | C25A—H25E | 0.9800 |
| C15—H15C | 0.9800 | C25A—H25F | 0.9800 |
| C16—H16A | 0.9800 | ||
| Re1i—Re1—Re2 | 60.542 (6) | H15B—C15—H15C | 109.5 |
| Re1i—Re1—Re2i | 60.127 (5) | N3—C16—H16A | 109.5 |
| Re2—Re1—Re2i | 120.669 (6) | N3—C16—H16B | 109.5 |
| C1—Re1—Re1i | 91.41 (12) | N3—C16—H16C | 109.5 |
| C1—Re1—Re2i | 91.11 (12) | H16A—C16—H16B | 109.5 |
| C1—Re1—Re2 | 90.28 (12) | H16A—C16—H16C | 109.5 |
| C1—Re1—C3 | 179.77 (18) | H16B—C16—H16C | 109.5 |
| C2—Re1—Re1i | 134.85 (11) | C17—N4—C18 | 112.1 (9) |
| C2—Re1—Re2 | 164.59 (11) | C17—N4—C20 | 126.2 (8) |
| C2—Re1—Re2i | 74.73 (11) | C18—N4—C20 | 121.7 (9) |
| C2—Re1—C1 | 88.73 (16) | C17—N5—C19 | 111.2 (8) |
| C2—Re1—C3 | 91.05 (15) | C17—N5—C21 | 125.8 (8) |
| C2—Re1—C4 | 90.39 (17) | C19—N5—C21 | 122.9 (9) |
| C3—Re1—Re1i | 88.79 (11) | N4—C17—Pd1 | 130.5 (6) |
| C3—Re1—Re2 | 89.91 (11) | N5—C17—Pd1 | 125.7 (6) |
| C3—Re1—Re2i | 88.89 (12) | N5—C17—N4 | 103.8 (8) |
| C4—Re1—Re1i | 134.75 (13) | N4—C18—H18 | 127.0 |
| C4—Re1—Re2i | 165.04 (13) | C19—C18—N4 | 105.9 (9) |
| C4—Re1—Re2 | 74.23 (13) | C19—C18—H18 | 127.0 |
| C4—Re1—C1 | 90.0 (2) | N5—C19—H19 | 126.5 |
| C4—Re1—C3 | 89.9 (2) | C18—C19—N5 | 107.0 (9) |
| Re1—Re2—Re1i | 59.330 (6) | C18—C19—H19 | 126.5 |
| C5—Re2—Re1i | 89.40 (12) | N4—C20—H20A | 109.5 |
| C5—Re2—Re1 | 87.57 (12) | N4—C20—H20B | 109.5 |
| C5—Re2—C7 | 176.24 (15) | N4—C20—H20C | 109.5 |
| C6—Re2—Re1 | 163.81 (12) | H20A—C20—H20B | 109.5 |
| C6—Re2—Re1i | 104.51 (12) | H20A—C20—H20C | 109.5 |
| C6—Re2—C5 | 91.43 (17) | H20B—C20—H20C | 109.5 |
| C6—Re2—C7 | 91.67 (16) | N5—C21—H21A | 109.5 |
| C6—Re2—C8 | 91.55 (16) | N5—C21—H21B | 109.5 |
| C7—Re2—Re1 | 88.86 (10) | N5—C21—H21C | 109.5 |
| C7—Re2—Re1i | 87.76 (11) | H21A—C21—H21B | 109.5 |
| C8—Re2—Re1i | 163.93 (12) | H21A—C21—H21C | 109.5 |
| C8—Re2—Re1 | 104.61 (12) | H21B—C21—H21C | 109.5 |
| C8—Re2—C5 | 90.28 (17) | C22—O9—C24 | 113.7 (13) |
| C8—Re2—C7 | 91.76 (15) | H23A—C23—H23B | 109.5 |
| O1—C1—Re1 | 174.2 (4) | H23A—C23—H23C | 109.5 |
| O2—C2—Re1 | 172.3 (3) | H23B—C23—H23C | 109.5 |
| O3—C3—Re1 | 174.7 (4) | C22—C23—H23A | 109.5 |
| O4—C4—Re1 | 174.2 (4) | C22—C23—H23B | 109.5 |
| O5—C5—Re2 | 175.9 (4) | C22—C23—H23C | 109.5 |
| O6—C6—Re2 | 179.4 (4) | O9—C22—C23 | 109.7 (11) |
| O7—C7—Re2 | 175.8 (3) | O9—C22—H22A | 109.7 |
| O8—C8—Re2 | 178.7 (4) | O9—C22—H22B | 109.7 |
| C9—Pd1—C12 | 87.72 (10) | C23—C22—H22A | 109.7 |
| C9—Pd1—C12ii | 87.72 (10) | C23—C22—H22B | 109.7 |
| C9—Pd1—C17 | 173.0 (2) | H22A—C22—H22B | 108.2 |
| C12ii—Pd1—C12 | 175.4 (2) | O9—C24—H24A | 109.8 |
| C12ii—Pd1—C17 | 86.9 (4) | O9—C24—H24B | 109.8 |
| C12—Pd1—C17 | 97.7 (4) | O9—C24—C25 | 109.4 (11) |
| C9—N1—C10 | 110.8 (3) | H24A—C24—H24B | 108.2 |
| C9—N1—C11 | 125.2 (3) | C25—C24—H24A | 109.8 |
| C10—N1—C11 | 124.0 (3) | C25—C24—H24B | 109.8 |
| C12—N2—C13 | 111.0 (3) | C24—C25—H25A | 109.5 |
| C12—N2—C15 | 125.0 (3) | C24—C25—H25B | 109.5 |
| C13—N2—C15 | 123.9 (3) | C24—C25—H25C | 109.5 |
| C12—N3—C14 | 110.9 (3) | H25A—C25—H25B | 109.5 |
| C12—N3—C16 | 126.1 (3) | H25A—C25—H25C | 109.5 |
| C14—N3—C16 | 123.1 (4) | H25B—C25—H25C | 109.5 |
| N1ii—C9—Pd1 | 127.7 (2) | C22A—O9A—C24A | 113 (2) |
| N1—C9—Pd1 | 127.7 (2) | O9A—C22A—H22C | 109.5 |
| N1—C9—N1ii | 104.6 (4) | O9A—C22A—H22D | 109.5 |
| N1—C10—H10 | 126.6 | O9A—C22A—C23A | 110.6 (16) |
| C10ii—C10—N1 | 106.9 (2) | H22C—C22A—H22D | 108.1 |
| C10ii—C10—H10 | 126.6 | C23A—C22A—H22C | 109.5 |
| N1—C11—H11A | 109.5 | C23A—C22A—H22D | 109.5 |
| N1—C11—H11B | 109.5 | O9A—C24A—H24C | 109.8 |
| N1—C11—H11C | 109.5 | O9A—C24A—H24D | 109.8 |
| H11A—C11—H11B | 109.5 | O9A—C24A—C25A | 109.5 (18) |
| H11A—C11—H11C | 109.5 | H24C—C24A—H24D | 108.2 |
| H11B—C11—H11C | 109.5 | C25A—C24A—H24C | 109.8 |
| N2—C12—Pd1 | 127.2 (3) | C25A—C24A—H24D | 109.8 |
| N3—C12—Pd1 | 128.1 (3) | C22A—C23A—H23D | 109.5 |
| N3—C12—N2 | 104.6 (3) | C22A—C23A—H23E | 109.5 |
| N2—C13—H13 | 126.5 | C22A—C23A—H23F | 109.5 |
| C14—C13—N2 | 107.0 (3) | H23D—C23A—H23E | 109.5 |
| C14—C13—H13 | 126.5 | H23D—C23A—H23F | 109.5 |
| N3—C14—H14 | 126.7 | H23E—C23A—H23F | 109.5 |
| C13—C14—N3 | 106.6 (4) | C24A—C25A—H25D | 109.5 |
| C13—C14—H14 | 126.7 | C24A—C25A—H25E | 109.5 |
| N2—C15—H15A | 109.5 | C24A—C25A—H25F | 109.5 |
| N2—C15—H15B | 109.5 | H25D—C25A—H25E | 109.5 |
| N2—C15—H15C | 109.5 | H25D—C25A—H25F | 109.5 |
| H15A—C15—H15B | 109.5 | H25E—C25A—H25F | 109.5 |
| H15A—C15—H15C | 109.5 | ||
| N2—C13—C14—N3 | 0.1 (5) | C16—N3—C14—C13 | 179.1 (4) |
| C9—N1—C10—C10ii | 0.6 (6) | N4—C18—C19—N5 | 2 (3) |
| C10—N1—C9—Pd1 | 179.8 (2) | C17—N4—C18—C19 | −2 (2) |
| C10—N1—C9—N1ii | −0.2 (2) | C17—N5—C19—C18 | −2 (3) |
| C11—N1—C9—Pd1 | −1.0 (4) | C18—N4—C17—Pd1 | −178.0 (11) |
| C11—N1—C9—N1ii | 179.0 (4) | C18—N4—C17—N5 | 0.7 (17) |
| C11—N1—C10—C10ii | −178.6 (4) | C19—N5—C17—Pd1 | 179.6 (18) |
| C12—N2—C13—C14 | 0.0 (5) | C19—N5—C17—N4 | 1 (2) |
| C12—N3—C14—C13 | −0.3 (5) | C20—N4—C17—Pd1 | −1 (2) |
| C13—N2—C12—Pd1 | 175.6 (3) | C20—N4—C17—N5 | 177.6 (9) |
| C13—N2—C12—N3 | −0.2 (4) | C20—N4—C18—C19 | −179.0 (17) |
| C14—N3—C12—Pd1 | −175.4 (3) | C21—N5—C17—Pd1 | −4 (2) |
| C14—N3—C12—N2 | 0.3 (4) | C21—N5—C17—N4 | 177.6 (9) |
| C15—N2—C12—Pd1 | −6.8 (5) | C21—N5—C19—C18 | −179.0 (14) |
| C15—N2—C12—N3 | 177.5 (3) | C22—O9—C24—C25 | 168.3 (18) |
| C15—N2—C13—C14 | −177.7 (4) | C24—O9—C22—C23 | −177.2 (18) |
| C16—N3—C12—Pd1 | 5.2 (6) | C22A—O9A—C24A—C25A | −160 (3) |
| C16—N3—C12—N2 | −179.1 (4) | C24A—O9A—C22A—C23A | −177 (3) |
Symmetry codes: (i) −x+1/2, −y+3/2, −z; (ii) −x, y, −z+1/2.
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1). Hydrogen-bond geometry (Å, º)
| D—H···A | D—H | H···A | D···A | D—H···A |
| C11—H11A···O4iii | 0.98 | 2.49 | 3.436 (6) | 161 |
| C13—H13···O9iv | 0.95 | 2.44 | 3.36 (3) | 165 |
| C13—H13···O9Aiv | 0.95 | 2.32 | 3.25 (5) | 163 |
| C15—H15A···O6v | 0.98 | 2.44 | 3.326 (5) | 150 |
| C16—H16B···O9 | 0.98 | 2.57 | 3.49 (3) | 158 |
| C18—H18···O7vi | 0.95 | 2.43 | 3.230 (9) | 141 |
| C19—H19···O7v | 0.95 | 2.56 | 3.483 (16) | 163 |
| C20—H20C···O5ii | 0.98 | 2.35 | 3.203 (12) | 145 |
| C21—H21A···O2vii | 0.98 | 2.54 | 3.413 (11) | 149 |
| C21—H21C···O5 | 0.98 | 2.59 | 3.494 (12) | 153 |
| C24—H24B···O8viii | 0.99 | 2.58 | 3.473 (12) | 150 |
Symmetry codes: (ii) −x, y, −z+1/2; (iii) −x, −y+1, −z; (iv) −x+1/2, −y+3/2, −z+1; (v) x, −y+2, z+1/2; (vi) −x, −y+2, −z; (vii) −x+1/2, y+1/2, −z+1/2; (viii) x+1/2, −y+3/2, z+1/2.
Octa-µ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (2). Crystal data
| [Pd4Re2(C18H15P)4(CO)10] | Z = 1 |
| Mr = 2127.18 | F(000) = 1026 |
| Triclinic, P1 | Dx = 1.715 Mg m−3 |
| a = 12.9278 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
| b = 13.5132 (5) Å | Cell parameters from 9325 reflections |
| c = 14.1184 (5) Å | θ = 2.8–29.6° |
| α = 105.983 (1)° | µ = 3.91 mm−1 |
| β = 108.510 (1)° | T = 100 K |
| γ = 106.129 (1)° | Block, red |
| V = 2060.09 (12) Å3 | 0.23 × 0.18 × 0.18 mm |
Octa-µ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (2). Data collection
| Bruker APEXII CCD diffractometer | 10906 reflections with I > 2σ(I) |
| φ and ω scans | Rint = 0.042 |
| Absorption correction: multi-scan (SADABS; Krause et al., 2015) | θmax = 29.7°, θmin = 2.8° |
| Tmin = 0.515, Tmax = 0.746 | h = −17→17 |
| 151194 measured reflections | k = −18→18 |
| 11588 independent reflections | l = −19→19 |
Octa-µ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (2). Refinement
| Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
| Least-squares matrix: full | H-atom parameters constrained |
| R[F2 > 2σ(F2)] = 0.018 | w = 1/[σ2(Fo2) + (0.0148P)2 + 2.1161P] where P = (Fo2 + 2Fc2)/3 |
| wR(F2) = 0.042 | (Δ/σ)max = 0.005 |
| S = 1.10 | Δρmax = 0.95 e Å−3 |
| 11588 reflections | Δρmin = −0.70 e Å−3 |
| 461 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 0 restraints | Extinction coefficient: 0.00119 (9) |
| Primary atom site location: dual |
Octa-µ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (2). Special details
| Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Octa-µ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (2). Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | ||
| Re1 | −0.03789 (2) | 0.58284 (2) | 0.59592 (2) | 0.01288 (3) | |
| Pd1 | 0.11939 (2) | 0.64837 (2) | 0.50923 (2) | 0.01377 (3) | |
| Pd2 | 0.13798 (2) | 0.50124 (2) | 0.63029 (2) | 0.01360 (3) | |
| P1 | 0.27753 (4) | 0.79978 (4) | 0.52970 (4) | 0.01537 (9) | |
| P2 | 0.27280 (5) | 0.48255 (4) | 0.77255 (4) | 0.01634 (10) | |
| O1 | −0.11990 (18) | 0.71938 (18) | 0.74578 (16) | 0.0433 (5) | |
| O2 | −0.12746 (15) | 0.42760 (14) | 0.70708 (13) | 0.0266 (3) | |
| O3 | 0.18975 (14) | 0.70585 (13) | 0.81880 (12) | 0.0236 (3) | |
| O4 | 0.03880 (14) | 0.82425 (13) | 0.59258 (13) | 0.0240 (3) | |
| O5 | 0.30356 (13) | 0.45945 (14) | 0.53745 (13) | 0.0236 (3) | |
| C1 | −0.0874 (2) | 0.66930 (19) | 0.69145 (18) | 0.0246 (4) | |
| C2 | −0.10429 (18) | 0.45891 (18) | 0.64488 (17) | 0.0198 (4) | |
| C3 | 0.12010 (18) | 0.64157 (17) | 0.73175 (16) | 0.0178 (4) | |
| C4 | 0.03254 (17) | 0.73328 (17) | 0.57964 (16) | 0.0175 (4) | |
| C5 | 0.20750 (18) | 0.45438 (17) | 0.51815 (16) | 0.0174 (4) | |
| C6 | 0.37893 (17) | 0.75557 (17) | 0.48099 (17) | 0.0188 (4) | |
| C7 | 0.4316 (2) | 0.69504 (19) | 0.53169 (19) | 0.0242 (4) | |
| H7 | 0.4156 | 0.6822 | 0.5894 | 0.029* | |
| C8 | 0.5067 (2) | 0.65387 (19) | 0.4984 (2) | 0.0270 (5) | |
| H8 | 0.5409 | 0.6118 | 0.5322 | 0.032* | |
| C9 | 0.5315 (2) | 0.6744 (2) | 0.41544 (19) | 0.0283 (5) | |
| H9 | 0.5830 | 0.6464 | 0.3924 | 0.034* | |
| C10 | 0.4819 (2) | 0.7353 (2) | 0.36630 (19) | 0.0278 (5) | |
| H10 | 0.5008 | 0.7504 | 0.3106 | 0.033* | |
| C11 | 0.40389 (18) | 0.77520 (18) | 0.39750 (17) | 0.0215 (4) | |
| H11 | 0.3683 | 0.8154 | 0.3619 | 0.026* | |
| C12 | 0.38172 (18) | 0.90224 (17) | 0.66794 (16) | 0.0180 (4) | |
| C13 | 0.34659 (19) | 0.91169 (18) | 0.75257 (17) | 0.0216 (4) | |
| H13 | 0.2686 | 0.8649 | 0.7381 | 0.026* | |
| C14 | 0.4253 (2) | 0.9896 (2) | 0.85853 (18) | 0.0264 (5) | |
| H14 | 0.4004 | 0.9956 | 0.9156 | 0.032* | |
| C15 | 0.5392 (2) | 1.0578 (2) | 0.88081 (19) | 0.0299 (5) | |
| H15 | 0.5922 | 1.1113 | 0.9527 | 0.036* | |
| C16 | 0.5758 (2) | 1.0476 (2) | 0.7971 (2) | 0.0292 (5) | |
| H16 | 0.6544 | 1.0935 | 0.8122 | 0.035* | |
| C17 | 0.49795 (19) | 0.97081 (18) | 0.69209 (18) | 0.0230 (4) | |
| H17 | 0.5237 | 0.9645 | 0.6356 | 0.028* | |
| C18 | 0.22924 (18) | 0.88071 (17) | 0.45395 (16) | 0.0184 (4) | |
| C19 | 0.3060 (2) | 0.98359 (18) | 0.46489 (18) | 0.0229 (4) | |
| H19 | 0.3875 | 1.0152 | 0.5148 | 0.027* | |
| C20 | 0.2634 (2) | 1.0399 (2) | 0.4029 (2) | 0.0281 (5) | |
| H20 | 0.3162 | 1.1093 | 0.4102 | 0.034* | |
| C21 | 0.1449 (2) | 0.9955 (2) | 0.3312 (2) | 0.0347 (6) | |
| H21 | 0.1161 | 1.0346 | 0.2897 | 0.042* | |
| C22 | 0.0676 (2) | 0.8933 (3) | 0.3198 (2) | 0.0387 (6) | |
| H22 | −0.0139 | 0.8622 | 0.2699 | 0.046* | |
| C23 | 0.1098 (2) | 0.8368 (2) | 0.3815 (2) | 0.0282 (5) | |
| H23 | 0.0566 | 0.7676 | 0.3742 | 0.034* | |
| C24 | 0.42622 (18) | 0.57138 (19) | 0.80973 (17) | 0.0208 (4) | |
| C25 | 0.5207 (2) | 0.5376 (2) | 0.8357 (2) | 0.0294 (5) | |
| H25 | 0.5070 | 0.4651 | 0.8366 | 0.035* | |
| C26 | 0.6346 (2) | 0.6093 (2) | 0.8602 (2) | 0.0401 (6) | |
| H26 | 0.6982 | 0.5855 | 0.8774 | 0.048* | |
| C27 | 0.6561 (2) | 0.7155 (3) | 0.8598 (2) | 0.0409 (6) | |
| H27 | 0.7342 | 0.7642 | 0.8765 | 0.049* | |
| C28 | 0.5630 (2) | 0.7502 (3) | 0.8347 (3) | 0.0415 (7) | |
| H28 | 0.5776 | 0.8233 | 0.8353 | 0.050* | |
| C29 | 0.4486 (2) | 0.6779 (2) | 0.8087 (2) | 0.0326 (5) | |
| H29 | 0.3850 | 0.7015 | 0.7901 | 0.039* | |
| C30 | 0.26705 (19) | 0.34177 (18) | 0.75156 (17) | 0.0199 (4) | |
| C31 | 0.3181 (2) | 0.3138 (2) | 0.83814 (19) | 0.0296 (5) | |
| H31 | 0.3604 | 0.3699 | 0.9103 | 0.036* | |
| C32 | 0.3073 (3) | 0.2043 (2) | 0.8192 (2) | 0.0365 (6) | |
| H32 | 0.3425 | 0.1860 | 0.8784 | 0.044* | |
| C33 | 0.2453 (2) | 0.1214 (2) | 0.7143 (2) | 0.0335 (5) | |
| H33 | 0.2382 | 0.0465 | 0.7018 | 0.040* | |
| C34 | 0.1937 (2) | 0.1477 (2) | 0.6279 (2) | 0.0280 (5) | |
| H34 | 0.1506 | 0.0909 | 0.5561 | 0.034* | |
| C35 | 0.20507 (19) | 0.25749 (18) | 0.64649 (17) | 0.0213 (4) | |
| H35 | 0.1702 | 0.2754 | 0.5869 | 0.026* | |
| C36 | 0.25498 (19) | 0.52324 (18) | 0.89861 (16) | 0.0201 (4) | |
| C37 | 0.1507 (2) | 0.4569 (2) | 0.8988 (2) | 0.0303 (5) | |
| H37 | 0.0943 | 0.3913 | 0.8359 | 0.036* | |
| C38 | 0.1295 (3) | 0.4865 (3) | 0.9907 (2) | 0.0414 (7) | |
| H38 | 0.0592 | 0.4403 | 0.9910 | 0.050* | |
| C39 | 0.2099 (3) | 0.5825 (3) | 1.0819 (2) | 0.0443 (7) | |
| H39 | 0.1948 | 0.6030 | 1.1446 | 0.053* | |
| C40 | 0.3120 (3) | 0.6484 (2) | 1.0815 (2) | 0.0407 (7) | |
| H40 | 0.3671 | 0.7148 | 1.1441 | 0.049* | |
| C41 | 0.3356 (2) | 0.6192 (2) | 0.99088 (18) | 0.0277 (5) | |
| H41 | 0.4070 | 0.6649 | 0.9920 | 0.033* |
Octa-µ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (2). Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Re1 | 0.01245 (4) | 0.01357 (4) | 0.01647 (4) | 0.00659 (3) | 0.00863 (3) | 0.00710 (3) |
| Pd1 | 0.01249 (7) | 0.01311 (7) | 0.01861 (7) | 0.00468 (5) | 0.00858 (5) | 0.00854 (5) |
| Pd2 | 0.01236 (7) | 0.01464 (7) | 0.01648 (7) | 0.00662 (5) | 0.00670 (5) | 0.00807 (5) |
| P1 | 0.0134 (2) | 0.0141 (2) | 0.0215 (2) | 0.00506 (18) | 0.00935 (18) | 0.00943 (19) |
| P2 | 0.0163 (2) | 0.0175 (2) | 0.0174 (2) | 0.00879 (19) | 0.00679 (18) | 0.00836 (19) |
| O1 | 0.0443 (11) | 0.0454 (11) | 0.0439 (11) | 0.0246 (9) | 0.0282 (9) | 0.0054 (9) |
| O2 | 0.0308 (8) | 0.0263 (8) | 0.0236 (7) | 0.0053 (7) | 0.0156 (7) | 0.0124 (6) |
| O3 | 0.0248 (8) | 0.0196 (7) | 0.0221 (7) | 0.0100 (6) | 0.0058 (6) | 0.0062 (6) |
| O4 | 0.0241 (8) | 0.0162 (7) | 0.0341 (8) | 0.0097 (6) | 0.0128 (7) | 0.0111 (6) |
| O5 | 0.0180 (7) | 0.0314 (8) | 0.0300 (8) | 0.0145 (6) | 0.0135 (6) | 0.0156 (7) |
| C1 | 0.0216 (10) | 0.0260 (11) | 0.0263 (10) | 0.0104 (9) | 0.0120 (9) | 0.0075 (9) |
| C2 | 0.0168 (9) | 0.0221 (10) | 0.0220 (9) | 0.0069 (8) | 0.0104 (8) | 0.0090 (8) |
| C3 | 0.0190 (9) | 0.0182 (9) | 0.0213 (9) | 0.0089 (8) | 0.0109 (8) | 0.0109 (8) |
| C4 | 0.0138 (8) | 0.0190 (9) | 0.0199 (9) | 0.0070 (7) | 0.0074 (7) | 0.0073 (7) |
| C5 | 0.0190 (9) | 0.0161 (9) | 0.0218 (9) | 0.0082 (7) | 0.0109 (8) | 0.0101 (7) |
| C6 | 0.0142 (9) | 0.0151 (9) | 0.0270 (10) | 0.0041 (7) | 0.0108 (8) | 0.0079 (8) |
| C7 | 0.0234 (10) | 0.0231 (10) | 0.0361 (12) | 0.0112 (9) | 0.0180 (9) | 0.0177 (9) |
| C8 | 0.0252 (11) | 0.0224 (11) | 0.0411 (13) | 0.0132 (9) | 0.0172 (10) | 0.0163 (10) |
| C9 | 0.0222 (11) | 0.0284 (12) | 0.0331 (12) | 0.0127 (9) | 0.0131 (9) | 0.0063 (9) |
| C10 | 0.0257 (11) | 0.0367 (13) | 0.0256 (10) | 0.0144 (10) | 0.0157 (9) | 0.0113 (9) |
| C11 | 0.0174 (9) | 0.0242 (10) | 0.0233 (10) | 0.0077 (8) | 0.0092 (8) | 0.0104 (8) |
| C12 | 0.0175 (9) | 0.0154 (9) | 0.0226 (9) | 0.0069 (7) | 0.0079 (8) | 0.0100 (7) |
| C13 | 0.0216 (10) | 0.0218 (10) | 0.0255 (10) | 0.0108 (8) | 0.0098 (8) | 0.0132 (8) |
| C14 | 0.0305 (12) | 0.0291 (11) | 0.0236 (10) | 0.0146 (10) | 0.0112 (9) | 0.0139 (9) |
| C15 | 0.0316 (12) | 0.0213 (11) | 0.0251 (11) | 0.0071 (9) | 0.0031 (9) | 0.0071 (9) |
| C16 | 0.0219 (11) | 0.0220 (11) | 0.0326 (12) | 0.0024 (9) | 0.0058 (9) | 0.0089 (9) |
| C17 | 0.0201 (10) | 0.0196 (10) | 0.0287 (10) | 0.0060 (8) | 0.0104 (8) | 0.0110 (8) |
| C18 | 0.0200 (9) | 0.0191 (9) | 0.0228 (9) | 0.0097 (8) | 0.0122 (8) | 0.0120 (8) |
| C19 | 0.0243 (10) | 0.0201 (10) | 0.0284 (10) | 0.0082 (8) | 0.0143 (9) | 0.0126 (8) |
| C20 | 0.0370 (13) | 0.0227 (11) | 0.0358 (12) | 0.0133 (10) | 0.0215 (10) | 0.0190 (10) |
| C21 | 0.0403 (14) | 0.0394 (14) | 0.0441 (14) | 0.0236 (12) | 0.0217 (12) | 0.0318 (12) |
| C22 | 0.0243 (12) | 0.0525 (17) | 0.0478 (15) | 0.0158 (12) | 0.0116 (11) | 0.0357 (14) |
| C23 | 0.0199 (10) | 0.0316 (12) | 0.0356 (12) | 0.0069 (9) | 0.0106 (9) | 0.0219 (10) |
| C24 | 0.0159 (9) | 0.0252 (10) | 0.0209 (9) | 0.0081 (8) | 0.0070 (8) | 0.0097 (8) |
| C25 | 0.0229 (11) | 0.0282 (12) | 0.0347 (12) | 0.0144 (9) | 0.0076 (9) | 0.0103 (10) |
| C26 | 0.0217 (12) | 0.0435 (15) | 0.0497 (16) | 0.0166 (11) | 0.0105 (11) | 0.0130 (13) |
| C27 | 0.0200 (11) | 0.0465 (16) | 0.0527 (16) | 0.0072 (11) | 0.0150 (11) | 0.0218 (14) |
| C28 | 0.0262 (13) | 0.0395 (15) | 0.0630 (18) | 0.0097 (11) | 0.0167 (12) | 0.0322 (14) |
| C29 | 0.0216 (11) | 0.0350 (13) | 0.0496 (15) | 0.0127 (10) | 0.0150 (11) | 0.0278 (12) |
| C30 | 0.0208 (10) | 0.0204 (10) | 0.0236 (10) | 0.0118 (8) | 0.0100 (8) | 0.0115 (8) |
| C31 | 0.0352 (13) | 0.0260 (11) | 0.0273 (11) | 0.0163 (10) | 0.0071 (10) | 0.0134 (9) |
| C32 | 0.0438 (15) | 0.0329 (13) | 0.0403 (14) | 0.0248 (12) | 0.0120 (12) | 0.0223 (11) |
| C33 | 0.0376 (13) | 0.0249 (12) | 0.0465 (14) | 0.0204 (11) | 0.0179 (12) | 0.0183 (11) |
| C34 | 0.0304 (12) | 0.0219 (11) | 0.0335 (12) | 0.0132 (9) | 0.0152 (10) | 0.0087 (9) |
| C35 | 0.0213 (10) | 0.0202 (10) | 0.0238 (10) | 0.0097 (8) | 0.0098 (8) | 0.0093 (8) |
| C36 | 0.0226 (10) | 0.0250 (10) | 0.0195 (9) | 0.0154 (8) | 0.0091 (8) | 0.0120 (8) |
| C37 | 0.0246 (11) | 0.0393 (14) | 0.0319 (12) | 0.0155 (10) | 0.0143 (10) | 0.0157 (10) |
| C38 | 0.0430 (16) | 0.0624 (19) | 0.0491 (16) | 0.0326 (15) | 0.0350 (14) | 0.0348 (15) |
| C39 | 0.076 (2) | 0.0585 (19) | 0.0360 (14) | 0.0490 (18) | 0.0393 (15) | 0.0307 (14) |
| C40 | 0.068 (2) | 0.0340 (14) | 0.0219 (11) | 0.0274 (14) | 0.0168 (12) | 0.0101 (10) |
| C41 | 0.0364 (13) | 0.0240 (11) | 0.0215 (10) | 0.0124 (10) | 0.0105 (9) | 0.0094 (9) |
Octa-µ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (2). Geometric parameters (Å, º)
| Re1—Pd1i | 2.7748 (2) | C15—H15 | 0.9500 |
| Re1—Pd1 | 2.7555 (2) | C15—C16 | 1.394 (4) |
| Re1—Pd2i | 2.7796 (2) | C16—H16 | 0.9500 |
| Re1—Pd2 | 2.7582 (2) | C16—C17 | 1.383 (3) |
| Re1—C1 | 1.921 (2) | C17—H17 | 0.9500 |
| Re1—C2 | 2.058 (2) | C18—C19 | 1.400 (3) |
| Re1—C3 | 2.062 (2) | C18—C23 | 1.391 (3) |
| Re1—C4 | 2.092 (2) | C19—H19 | 0.9500 |
| Re1—C5i | 2.087 (2) | C19—C20 | 1.393 (3) |
| Pd1—Re1i | 2.7747 (2) | C20—H20 | 0.9500 |
| Pd1—Pd2 | 2.9678 (2) | C20—C21 | 1.379 (4) |
| Pd1—Pd2i | 2.9909 (2) | C21—H21 | 0.9500 |
| Pd1—P1 | 2.3291 (5) | C21—C22 | 1.393 (4) |
| Pd1—C2i | 2.170 (2) | C22—H22 | 0.9500 |
| Pd1—C4 | 2.088 (2) | C22—C23 | 1.392 (3) |
| Pd2—Re1i | 2.7796 (2) | C23—H23 | 0.9500 |
| Pd2—Pd1i | 2.9910 (2) | C24—C25 | 1.398 (3) |
| Pd2—P2 | 2.3317 (5) | C24—C29 | 1.393 (3) |
| Pd2—C3 | 2.158 (2) | C25—H25 | 0.9500 |
| Pd2—C5 | 2.094 (2) | C25—C26 | 1.387 (4) |
| P1—C6 | 1.825 (2) | C26—H26 | 0.9500 |
| P1—C12 | 1.830 (2) | C26—C27 | 1.385 (4) |
| P1—C18 | 1.825 (2) | C27—H27 | 0.9500 |
| P2—C24 | 1.822 (2) | C27—C28 | 1.389 (4) |
| P2—C30 | 1.819 (2) | C28—H28 | 0.9500 |
| P2—C36 | 1.821 (2) | C28—C29 | 1.390 (3) |
| O1—C1 | 1.140 (3) | C29—H29 | 0.9500 |
| O2—C2 | 1.158 (3) | C30—C31 | 1.398 (3) |
| O3—C3 | 1.162 (2) | C30—C35 | 1.396 (3) |
| O4—C4 | 1.167 (3) | C31—H31 | 0.9500 |
| O5—C5 | 1.161 (2) | C31—C32 | 1.386 (3) |
| C2—Pd1i | 2.170 (2) | C32—H32 | 0.9500 |
| C5—Re1i | 2.087 (2) | C32—C33 | 1.387 (4) |
| C6—C7 | 1.403 (3) | C33—H33 | 0.9500 |
| C6—C11 | 1.389 (3) | C33—C34 | 1.383 (4) |
| C7—H7 | 0.9500 | C34—H34 | 0.9500 |
| C7—C8 | 1.385 (3) | C34—C35 | 1.390 (3) |
| C8—H8 | 0.9500 | C35—H35 | 0.9500 |
| C8—C9 | 1.385 (3) | C36—C37 | 1.398 (3) |
| C9—H9 | 0.9500 | C36—C41 | 1.386 (3) |
| C9—C10 | 1.376 (3) | C37—H37 | 0.9500 |
| C10—H10 | 0.9500 | C37—C38 | 1.386 (4) |
| C10—C11 | 1.398 (3) | C38—H38 | 0.9500 |
| C11—H11 | 0.9500 | C38—C39 | 1.379 (5) |
| C12—C13 | 1.394 (3) | C39—H39 | 0.9500 |
| C12—C17 | 1.400 (3) | C39—C40 | 1.374 (5) |
| C13—H13 | 0.9500 | C40—H40 | 0.9500 |
| C13—C14 | 1.397 (3) | C40—C41 | 1.386 (3) |
| C14—H14 | 0.9500 | C41—H41 | 0.9500 |
| C14—C15 | 1.381 (3) | ||
| Pd1—Re1—Pd1i | 99.105 (5) | C6—C7—H7 | 119.7 |
| Pd1—Re1—Pd2i | 65.413 (5) | C8—C7—C6 | 120.6 (2) |
| Pd1i—Re1—Pd2i | 64.596 (5) | C8—C7—H7 | 119.7 |
| Pd1—Re1—Pd2 | 65.131 (5) | C7—C8—H8 | 120.2 |
| Pd2—Re1—Pd1i | 65.445 (5) | C7—C8—C9 | 119.6 (2) |
| Pd2—Re1—Pd2i | 99.238 (5) | C9—C8—H8 | 120.2 |
| C1—Re1—Pd1 | 131.04 (7) | C8—C9—H9 | 119.9 |
| C1—Re1—Pd1i | 129.69 (7) | C10—C9—C8 | 120.3 (2) |
| C1—Re1—Pd2 | 133.48 (7) | C10—C9—H9 | 119.9 |
| C1—Re1—Pd2i | 127.28 (7) | C9—C10—H10 | 119.7 |
| C1—Re1—C2 | 83.99 (9) | C9—C10—C11 | 120.7 (2) |
| C1—Re1—C3 | 85.84 (9) | C11—C10—H10 | 119.7 |
| C1—Re1—C4 | 83.85 (9) | C6—C11—C10 | 119.5 (2) |
| C1—Re1—C5i | 81.63 (9) | C6—C11—H11 | 120.3 |
| C2—Re1—Pd1 | 141.37 (6) | C10—C11—H11 | 120.3 |
| C2—Re1—Pd1i | 50.76 (6) | C13—C12—P1 | 119.88 (16) |
| C2—Re1—Pd2 | 78.91 (6) | C13—C12—C17 | 118.49 (19) |
| C2—Re1—Pd2i | 109.51 (6) | C17—C12—P1 | 121.62 (16) |
| C2—Re1—C3 | 87.43 (8) | C12—C13—H13 | 119.8 |
| C2—Re1—C4 | 166.84 (8) | C12—C13—C14 | 120.4 (2) |
| C2—Re1—C5i | 91.78 (8) | C14—C13—H13 | 119.8 |
| C3—Re1—Pd1i | 109.34 (6) | C13—C14—H14 | 119.8 |
| C3—Re1—Pd1 | 80.75 (6) | C15—C14—C13 | 120.4 (2) |
| C3—Re1—Pd2 | 50.73 (6) | C15—C14—H14 | 119.8 |
| C3—Re1—Pd2i | 143.08 (6) | C14—C15—H15 | 120.2 |
| C3—Re1—C4 | 86.69 (8) | C14—C15—C16 | 119.6 (2) |
| C3—Re1—C5i | 167.46 (8) | C16—C15—H15 | 120.2 |
| C4—Re1—Pd1 | 48.71 (5) | C15—C16—H16 | 119.9 |
| C4—Re1—Pd1i | 142.40 (5) | C17—C16—C15 | 120.2 (2) |
| C4—Re1—Pd2i | 82.00 (5) | C17—C16—H16 | 119.9 |
| C4—Re1—Pd2 | 106.14 (5) | C12—C17—H17 | 119.5 |
| C5i—Re1—Pd1 | 107.18 (6) | C16—C17—C12 | 120.9 (2) |
| C5i—Re1—Pd1i | 79.46 (5) | C16—C17—H17 | 119.5 |
| C5i—Re1—Pd2 | 141.24 (5) | C19—C18—P1 | 123.40 (16) |
| C5i—Re1—Pd2i | 48.43 (5) | C23—C18—P1 | 117.73 (16) |
| C5i—Re1—C4 | 91.42 (8) | C23—C18—C19 | 118.9 (2) |
| Re1—Pd1—Re1i | 80.894 (5) | C18—C19—H19 | 119.8 |
| Re1i—Pd1—Pd2 | 57.781 (5) | C20—C19—C18 | 120.3 (2) |
| Re1i—Pd1—Pd2i | 57.011 (4) | C20—C19—H19 | 119.8 |
| Re1—Pd1—Pd2 | 57.477 (4) | C19—C20—H20 | 119.8 |
| Re1—Pd1—Pd2i | 57.681 (5) | C21—C20—C19 | 120.3 (2) |
| Pd2—Pd1—Pd2i | 90.135 (6) | C21—C20—H20 | 119.8 |
| P1—Pd1—Re1i | 133.608 (14) | C20—C21—H21 | 120.0 |
| P1—Pd1—Re1 | 143.861 (14) | C20—C21—C22 | 119.9 (2) |
| P1—Pd1—Pd2i | 143.699 (14) | C22—C21—H21 | 120.0 |
| P1—Pd1—Pd2 | 125.624 (14) | C21—C22—H22 | 120.0 |
| C2i—Pd1—Re1i | 47.26 (6) | C23—C22—C21 | 119.9 (2) |
| C2i—Pd1—Re1 | 122.58 (6) | C23—C22—H22 | 120.0 |
| C2i—Pd1—Pd2i | 72.07 (5) | C18—C23—C22 | 120.6 (2) |
| C2i—Pd1—Pd2 | 100.12 (6) | C18—C23—H23 | 119.7 |
| C2i—Pd1—P1 | 93.27 (6) | C22—C23—H23 | 119.7 |
| C4—Pd1—Re1 | 48.82 (6) | C25—C24—P2 | 123.95 (18) |
| C4—Pd1—Re1i | 125.79 (6) | C29—C24—P2 | 117.27 (17) |
| C4—Pd1—Pd2 | 99.39 (6) | C29—C24—C25 | 118.8 (2) |
| C4—Pd1—Pd2i | 76.94 (5) | C24—C25—H25 | 119.8 |
| C4—Pd1—P1 | 100.27 (6) | C26—C25—C24 | 120.3 (2) |
| C4—Pd1—C2i | 143.15 (8) | C26—C25—H25 | 119.8 |
| Re1—Pd2—Re1i | 80.762 (5) | C25—C26—H26 | 119.8 |
| Re1—Pd2—Pd1i | 57.545 (5) | C27—C26—C25 | 120.5 (2) |
| Re1i—Pd2—Pd1 | 57.623 (5) | C27—C26—H26 | 119.8 |
| Re1—Pd2—Pd1 | 57.392 (5) | C26—C27—H27 | 120.2 |
| Re1i—Pd2—Pd1i | 56.904 (4) | C26—C27—C28 | 119.7 (2) |
| Pd1—Pd2—Pd1i | 89.865 (6) | C28—C27—H27 | 120.2 |
| P2—Pd2—Re1i | 139.454 (14) | C27—C28—H28 | 120.0 |
| P2—Pd2—Re1 | 138.742 (14) | C27—C28—C29 | 119.9 (3) |
| P2—Pd2—Pd1i | 128.138 (15) | C29—C28—H28 | 120.0 |
| P2—Pd2—Pd1 | 141.995 (15) | C24—C29—H29 | 119.6 |
| C3—Pd2—Re1 | 47.70 (5) | C28—C29—C24 | 120.8 (2) |
| C3—Pd2—Re1i | 123.96 (5) | C28—C29—H29 | 119.6 |
| C3—Pd2—Pd1i | 99.53 (5) | C31—C30—P2 | 122.07 (17) |
| C3—Pd2—Pd1 | 74.39 (5) | C35—C30—P2 | 119.19 (16) |
| C3—Pd2—P2 | 96.08 (6) | C35—C30—C31 | 118.7 (2) |
| C5—Pd2—Re1 | 124.34 (6) | C30—C31—H31 | 119.9 |
| C5—Pd2—Re1i | 48.21 (6) | C32—C31—C30 | 120.3 (2) |
| C5—Pd2—Pd1i | 99.26 (6) | C32—C31—H31 | 119.9 |
| C5—Pd2—Pd1 | 74.81 (6) | C31—C32—H32 | 119.8 |
| C5—Pd2—P2 | 96.36 (6) | C31—C32—C33 | 120.5 (2) |
| C5—Pd2—C3 | 143.64 (8) | C33—C32—H32 | 119.8 |
| C6—P1—Pd1 | 112.32 (7) | C32—C33—H33 | 120.0 |
| C6—P1—C12 | 100.69 (9) | C34—C33—C32 | 119.9 (2) |
| C12—P1—Pd1 | 117.97 (7) | C34—C33—H33 | 120.0 |
| C18—P1—Pd1 | 112.89 (7) | C33—C34—H34 | 120.1 |
| C18—P1—C6 | 105.65 (10) | C33—C34—C35 | 119.8 (2) |
| C18—P1—C12 | 105.98 (9) | C35—C34—H34 | 120.1 |
| C24—P2—Pd2 | 111.89 (7) | C30—C35—H35 | 119.6 |
| C30—P2—Pd2 | 116.83 (7) | C34—C35—C30 | 120.9 (2) |
| C30—P2—C24 | 106.51 (10) | C34—C35—H35 | 119.6 |
| C30—P2—C36 | 101.65 (10) | C37—C36—P2 | 117.43 (17) |
| C36—P2—Pd2 | 114.10 (7) | C41—C36—P2 | 123.41 (18) |
| C36—P2—C24 | 104.65 (10) | C41—C36—C37 | 119.1 (2) |
| O1—C1—Re1 | 178.1 (2) | C36—C37—H37 | 119.9 |
| Re1—C2—Pd1i | 81.98 (7) | C38—C37—C36 | 120.1 (2) |
| O2—C2—Re1 | 152.98 (18) | C38—C37—H37 | 119.9 |
| O2—C2—Pd1i | 124.90 (17) | C37—C38—H38 | 119.8 |
| Re1—C3—Pd2 | 81.57 (7) | C39—C38—C37 | 120.4 (3) |
| O3—C3—Re1 | 152.27 (17) | C39—C38—H38 | 119.8 |
| O3—C3—Pd2 | 126.08 (16) | C38—C39—H39 | 120.2 |
| Pd1—C4—Re1 | 82.47 (7) | C40—C39—C38 | 119.6 (2) |
| O4—C4—Re1 | 149.43 (17) | C40—C39—H39 | 120.2 |
| O4—C4—Pd1 | 128.10 (16) | C39—C40—H40 | 119.6 |
| Re1i—C5—Pd2 | 83.36 (7) | C39—C40—C41 | 120.8 (3) |
| O5—C5—Re1i | 149.52 (17) | C41—C40—H40 | 119.6 |
| O5—C5—Pd2 | 127.10 (16) | C36—C41—C40 | 120.0 (3) |
| C7—C6—P1 | 115.78 (16) | C36—C41—H41 | 120.0 |
| C11—C6—P1 | 124.87 (17) | C40—C41—H41 | 120.0 |
| C11—C6—C7 | 119.32 (19) | ||
| Pd1—P1—C6—C7 | −58.98 (17) | C15—C16—C17—C12 | 0.0 (4) |
| Pd1—P1—C6—C11 | 119.34 (17) | C17—C12—C13—C14 | 1.2 (3) |
| Pd1—P1—C12—C13 | −21.58 (19) | C18—P1—C6—C7 | 177.54 (16) |
| Pd1—P1—C12—C17 | 157.12 (15) | C18—P1—C6—C11 | −4.1 (2) |
| Pd1—P1—C18—C19 | 171.11 (16) | C18—P1—C12—C13 | 106.03 (18) |
| Pd1—P1—C18—C23 | −9.1 (2) | C18—P1—C12—C17 | −75.28 (19) |
| Pd2—P2—C24—C25 | −139.46 (18) | C18—C19—C20—C21 | 0.8 (4) |
| Pd2—P2—C24—C29 | 38.6 (2) | C19—C18—C23—C22 | 0.9 (4) |
| Pd2—P2—C30—C31 | −162.18 (17) | C19—C20—C21—C22 | −0.6 (4) |
| Pd2—P2—C30—C35 | 14.8 (2) | C20—C21—C22—C23 | 0.6 (4) |
| Pd2—P2—C36—C37 | 66.91 (19) | C21—C22—C23—C18 | −0.8 (4) |
| Pd2—P2—C36—C41 | −109.26 (18) | C23—C18—C19—C20 | −0.9 (3) |
| P1—C6—C7—C8 | 177.66 (18) | C24—P2—C30—C31 | 72.0 (2) |
| P1—C6—C11—C10 | −178.91 (17) | C24—P2—C30—C35 | −111.09 (18) |
| P1—C12—C13—C14 | 179.96 (17) | C24—P2—C36—C37 | −170.48 (18) |
| P1—C12—C17—C16 | −179.77 (18) | C24—P2—C36—C41 | 13.4 (2) |
| P1—C18—C19—C20 | 178.85 (17) | C24—C25—C26—C27 | 0.3 (4) |
| P1—C18—C23—C22 | −178.9 (2) | C25—C24—C29—C28 | −1.0 (4) |
| P2—C24—C25—C26 | 178.2 (2) | C25—C26—C27—C28 | 0.1 (5) |
| P2—C24—C29—C28 | −179.2 (2) | C26—C27—C28—C29 | −0.9 (5) |
| P2—C30—C31—C32 | 177.2 (2) | C27—C28—C29—C24 | 1.4 (5) |
| P2—C30—C35—C34 | −176.80 (17) | C29—C24—C25—C26 | 0.1 (4) |
| P2—C36—C37—C38 | −177.0 (2) | C30—P2—C24—C25 | −10.7 (2) |
| P2—C36—C41—C40 | 175.83 (19) | C30—P2—C24—C29 | 167.39 (19) |
| C6—P1—C12—C13 | −144.12 (17) | C30—P2—C36—C37 | −59.76 (19) |
| C6—P1—C12—C17 | 34.58 (19) | C30—P2—C36—C41 | 124.07 (19) |
| C6—P1—C18—C19 | −65.8 (2) | C30—C31—C32—C33 | −0.3 (4) |
| C6—P1—C18—C23 | 114.00 (18) | C31—C30—C35—C34 | 0.2 (3) |
| C6—C7—C8—C9 | 1.1 (4) | C31—C32—C33—C34 | −0.1 (4) |
| C7—C6—C11—C10 | −0.6 (3) | C32—C33—C34—C35 | 0.5 (4) |
| C7—C8—C9—C10 | 0.0 (4) | C33—C34—C35—C30 | −0.6 (4) |
| C8—C9—C10—C11 | −1.4 (4) | C35—C30—C31—C32 | 0.2 (4) |
| C9—C10—C11—C6 | 1.7 (3) | C36—P2—C24—C25 | 96.5 (2) |
| C11—C6—C7—C8 | −0.8 (3) | C36—P2—C24—C29 | −85.4 (2) |
| C12—P1—C6—C7 | 67.42 (18) | C36—P2—C30—C31 | −37.3 (2) |
| C12—P1—C6—C11 | −114.25 (19) | C36—P2—C30—C35 | 139.62 (18) |
| C12—P1—C18—C19 | 40.5 (2) | C36—C37—C38—C39 | 1.1 (4) |
| C12—P1—C18—C23 | −139.70 (18) | C37—C36—C41—C40 | −0.3 (3) |
| C12—C13—C14—C15 | −0.3 (3) | C37—C38—C39—C40 | −0.6 (4) |
| C13—C12—C17—C16 | −1.1 (3) | C38—C39—C40—C41 | −0.4 (4) |
| C13—C14—C15—C16 | −0.8 (4) | C39—C40—C41—C36 | 0.8 (4) |
| C14—C15—C16—C17 | 1.0 (4) | C41—C36—C37—C38 | −0.7 (4) |
Symmetry code: (i) −x, −y+1, −z+1.
Octa-µ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (2). Hydrogen-bond geometry (Å, º)
Cg1 and Cg3 are the centroids of the C6–C11 and C18–C23 rings, respectively.
| D—H···A | D—H | H···A | D···A | D—H···A |
| C9—H9···O5ii | 0.95 | 2.49 | 3.188 (3) | 130 |
| C39—H39···O2iii | 0.95 | 2.60 | 3.491 (4) | 157 |
| C20—H20···Cg1iv | 0.95 | 2.84 | 3.635 (3) | 142 |
| C34—H34···Cg3v | 0.95 | 2.90 | 3.683 (3) | 140 |
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) −x, −y+1, −z+2; (iv) −x+1, −y+2, −z+1; (v) x, y−1, z.
Funding Statement
This work was funded by Russian Foundation for Basic Research grant 19-33-90199 to RFBR.
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablock(s) global, 1, 2. DOI: 10.1107/S2056989021009270/tx2041sup1.cif
Structure factors: contains datablock(s) 1. DOI: 10.1107/S2056989021009270/tx20411sup2.hkl
Structure factors: contains datablock(s) 2. DOI: 10.1107/S2056989021009270/tx20412sup3.hkl
Additional supporting information: crystallographic information; 3D view; checkCIF report