Crystal structure of the new palladium complexes tetra­kis­(1,3-di­methyl­imidazolium-2-yl­idene)palladium(II) hexa­deca­carbonyl­tetra­rhenium diethyl ether disolvate and octa-μ-carbonyl-di­carbonyl­tetra­kis­(tri­phenyl­phosphane)palladium­dirhenium (unknown solvate)

Shapovalov, S.; Tikhonova, O.; Skabitsky, I.

doi:10.1107/S2056989021009270

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ISSN: 2056-9890

Volume 77| Part 10| October 2021| Pages 1014-1018

https://doi.org/10.1107/S2056989021009270

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Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate)

Sergey Shapovalov,^a ^* Olga Tikhonova ^a and Ivan Skabitsky ^a

^aKurnakov Institute of General and Inorganic Chemistry, 119991, Leninskii pr. 31, Moscow, Russian Federation
^*Correspondence e-mail: schss@yandex.ru

Edited by B. Therrien, University of Neuchâtel, Switzerland (Received 27 August 2021; accepted 7 September 2021; online 14 September 2021)

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.

Keywords: palladium; rhenium; carbonyl; NHC; triphenylphospine; crystal structure.

CCDC references: 2108168; 2108167

1. 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.

2. 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.

3. 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).

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⋯O9Aⁱⁱ	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⋯O7^iv	0.95	2.43	3.230 (9)	141
C19—H19⋯O7ⁱⁱⁱ	0.95	2.56	3.483 (16)	163
C20—H20C⋯O5^v	0.98	2.35	3.203 (12)	145
C21—H21A⋯O2^vi	0.98	2.54	3.413 (11)	149
C21—H21C⋯O5	0.98	2.59	3.494 (12)	153
C24—H24B⋯O8^vii	0.99	2.58	3.473 (12)	150
Symmetry codes: (i) ; (ii) $[-x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1]$ ; (iii) $[x, -y+2, z+{\script{1\over 2}}]$ ; (iv) ; (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) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

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⋯Cg3^iv	0.95	2.90	3.683 (3)	140
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .

Figure 3
A view of the packing of compound 1.

Figure 4
A view of the packing of compound 2.

Figure 5
The axial CO groups of the Re(CO)₅ fragments in 2 point towards voids filled with an unidentified solvent.

4. 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.

5. 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-d₆, ppm): 3.41 (s, 24H, 8Me), 7.37 (s, 8H, 8CH). ¹³C{H} NMR (75.4 MHz, DMSO-d₆, 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.

6. 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 (sp²), 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 $[\overline{2}]$ 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)
T_min, T_max	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(F²)], wR(F²), 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
Δρ_max, Δρ_min (e Å⁻³)	1.43, −1.83	0.95, −0.70
Computer programs: APEX2 and SAINT (Bruker, 2015 ), SHELXT2014/5 (Sheldrick, 2015a ), SHELXL2014/7 (Sheldrick, 2015b ) and OLEX2 (Dolomanov et al., 2009 ).

Supporting information

CCDC references: 2108168; 2108167

Crystal structure: contains datablocks global, 1, 2. DOI: https://doi.org/10.1107/S2056989021009270/tx2041sup1.cif

Structure factors: contains datablock 1. DOI: https://doi.org/10.1107/S2056989021009270/tx20411sup2.hkl

Structure factors: contains datablock 2. DOI: https://doi.org/10.1107/S2056989021009270/tx20412sup3.hkl

checkCIF report

Computing details top

For both structures, data collection: APEX2 (Bruker, 2015); cell refinement: SAINT (Bruker, 2015); data reduction: SAINT (Bruker, 2015); program(s) used to solve structure: SHELXT2014/5 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate (1) top

Crystal data top

[Pd(C₅H₈N₂)₄][Re₄(CO)₁₆]·2C₄H₁₀O	F(000) = 3448
M_r = 1832.13	D_x = 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

Data collection top

Bruker APEXII CCD diffractometer	7392 reflections with I > 2σ(I)
φ and ω scans	R_int = 0.087
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	θ_max = 31.5°, θ_min = 1.8°
T_min = 0.285, T_max = 0.746	h = −31→31
128368 measured reflections	k = −20→20
9046 independent reflections	l = −28→28

Refinement top

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(F_o²) + (0.0239P)² + 18.7547P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.065	(Δ/σ)_max = 0.002
S = 1.06	Δρ_max = 1.43 e Å⁻³
9046 reflections	Δρ_min = −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

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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.

Hydrogen-bond geometry (Å, º) top

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···O9^iv	0.95	2.44	3.36 (3)	165
C13—H13···O9A^iv	0.95	2.32	3.25 (5)	163
C15—H15A···O6^v	0.98	2.44	3.326 (5)	150
C16—H16B···O9	0.98	2.57	3.49 (3)	158
C18—H18···O7^vi	0.95	2.43	3.230 (9)	141
C19—H19···O7^v	0.95	2.56	3.483 (16)	163
C20—H20C···O5ⁱⁱ	0.98	2.35	3.203 (12)	145
C21—H21A···O2^vii	0.98	2.54	3.413 (11)	149
C21—H21C···O5	0.98	2.59	3.494 (12)	153
C24—H24B···O8^viii	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) top

Crystal data top

[Pd₄Re₂(C₁₈H₁₅P)₄(CO)₁₀]	Z = 1
M_r = 2127.18	F(000) = 1026
Triclinic, P1	D_x = 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

Data collection top

Bruker APEXII CCD diffractometer	10906 reflections with I > 2σ(I)
φ and ω scans	R_int = 0.042
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	θ_max = 29.7°, θ_min = 2.8°
T_min = 0.515, T_max = 0.746	h = −17→17
151194 measured reflections	k = −18→18
11588 independent reflections	l = −19→19

Refinement top

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(F_o²) + (0.0148P)² + 2.1161P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.042	(Δ/σ)_max = 0.005
S = 1.10	Δρ_max = 0.95 e Å⁻³
11588 reflections	Δρ_min = −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

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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.

Hydrogen-bond geometry (Å, º) top

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···Cg1^iv	0.95	2.84	3.635 (3)	142
C34—H34···Cg3^v	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.

Acknowledgements

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).

Funding information

Funding for this research was provided by: Russian Foundation for Basic Research (grant No. 19-33-90199 to RFBR).

References

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Volume 77| Part 10| October 2021| Pages 1014-1018

https://doi.org/10.1107/S2056989021009270

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research communications\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Crystal structure of the new palladium complexes tetra­kis­(1,3-di­methyl­imidazolium-2-yl­­idene)palladium(II) hexa­deca­carbonyl­tetra­rhenium di­ethyl ether disolvate and octa-μ-carbonyl-di­carbonyl­tetra­kis­(tri­phenyl­phosphane)palladium­dirhenium (unknown solvate)

1. Chemical context

2. Structural commentary

3. Supra­molecular features

4. Database survey

5. Synthesis and crystallization

6. Refinement

Supporting information

Acknowledgements

Funding information

References

research communications

Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate)

3. Supramolecular features