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In the title compound, [PtRe4(C12H22P)2(CO)18] or [(μ-PCy2)(CO)8Re2]2Pt(CO)2 (Cy is cyclohexyl), two phosphido-bridged dirhenium groups are linked by a Pt(CO)2 unit and show different bonding patterns for stereochemical reasons. The Re—Re distances are 3.2620 (15) and 3.0739 (15) Å, and the Pt—Re distances are 2.9165 (12), 2.9025 (15) and 2.8548 (13) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101007399/jz1465sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101007399/jz1465Isup2.hkl
Contains datablock I

CCDC reference: 169930

Comment top

As a continuation of our investigations into triangular cluster complexes M2Rh(µ-PR2)(µ-CO)2(CO)8 (M = Mn, Re; R = organic residue) as hydroformylation catalysts (Beckers et al., 1998; Haupt et al., 2001), we wished for selectivity reasons to exchange the rhodium(I) atom for a more nucleophilic platinum(II) atom as reaction centre. Platinum(II) carbonyl cluster complexes of this type are very rare (Braunstein et al., 1999).

The molecule [(µ-PCy2)(CO)8Re2]2Pt(CO)2, (I) (Fig. 1), consists of two phosphido-bridged dirhenium carbonyl moieties that are linked via the central platinum atom. The Pt(CO)2 constituent extends the original (µ-P1)Re2 core to a four-membered, nearly planar µ-PRe2Pt ring. The maximum deviation of an atom from this best plane is 0.082 (6) Å for P1; the PRe2/Re2Pt dihedral angle is 8.1°. Both Re atoms have a slightly distorted octahedral coordination from four terminal CO groups, the bridging P and the Pt atom. The CO ligands at both rhenium show an ecliptic arrangement with C—Re1—Re2—C torsion angles (here and in the following text as absolute values) from 0.4 to 3.7°. The CO groups attached to Pt are also in ecliptic position relative to those at Re1 and Re2, with torsion angles from 0.5 to 6.1°. The Re1—Re2 bond measures 3.2620 (15) Å and the µ-P1 bridge is symmetric with respect to the equal P—Re bond lengths of 2.454 (6) and 2.459 (6) Å. The two Pt—Re bonds differ slightly in length with 2.9165 (12) and 2.9025 (15) Å for Re1 and Re2, respectively, but they are longer than other unsupported Pt—Re bonds known from the literature. For these, the values reported range from 2.706 (1) to 2.899 (1) Å (Casey et al., 1987, 1992; Urbancic et al., 1984; Beringhelli et al., 1990, 1993; Mague & Lin, 1994). A µ-H bridged Pt—Re edge has been reported with 2.906 (1) Å (Beringhelli et al., 1990). \sch

A third but shorter Pt—Re3 bond of 2.8548 (13) Å connects the second (µ-P2)Re2(CO)8 unit to platinum. Again, the Re3—Re4 bond of 3.0739 (15) Å is bridged by a PCy2 ligand and both rhenium atoms are attached to four terminal CO groups. These groups show also an ecliptic arrangement along the Re—Re vector, with torsion angles in the range 3.7 to 7.7°. Neglecting the Re—Re bond, Re4 is coordinated by five non-metal atoms, thus realising a distorted square pyramidal coordination, whereas Re3 reaches a strongly distorted octahedral coordination with the additional Re—Pt interaction. The CO ligands at Re3 and those attached to Pt show staggered conformation along the Re3—Pt vector with torsion angles of C9—Pt—Re3—C13 58.8 (10)° and C10—Pt—Re3—C12 57.2 (10)°, realising a sterically favourable arrangement. In contrast to the symmetric µ-P1 bridge, the µ-P2 atom shows two different P—Re bond lengths of 2.429 (6) (Re3) and 2.396 (6) Å (Re4), the longer one being trans to the Re3–Pt bond. With respect to the different Re—Pt—Re angles in the basal Re3Pt plane of 68.19 (4), 135.80 (4) and 155.33 (4)° for Re1/2, Re1/3 and Re2/3, respectively, the fivefold coordination geometry around Pt can be described as pseudo-trigonal bipyramidal with the CO groups 9 and 10 at the apices. The Re3Pt plane is almost planar with a maximum deviation of 0.082 (2) Å for Pt from the best plane. A similar Y-shaped planar coordination pattern for the central metal atom with Y-angles in the range of 64, 138 and 158° is known from the coordination of e.g. Ir or Rh in (µ-PR2)(CO)8Re2[µ-M(CO)2PPh3] (M = Ir, Rh) (Haupt et al., 1994). The uncommon coordination geometry observed here for platinum, with the different bonding patterns of one bridging and one end-on linked (µ-PCy2)(CO)8Re2 unit, must be due to stereochemical reasons. Neither an alternative planar quadratic nor spirocyclic Re4Pt arrangement, both then with two bridging Re2 units, would be possible because of the steric repulsion of the CO groups 3, 8 and 12,15 or 9, 10 and 12,15.

Experimental top

The salts Pt(COD)(CF3SO3)2 and NEt4[Re2(µ-PCy2)(CO)8] were reacted in dichloromethane solution in the presence of (CO)g (removal of the COD-ligand) at 258 K. The only separable product (thin-layer chromatography, eluant dichloromethane/n-hexane 1/5) was the title compound. Crystals were grown from chloroform/n-pentane, although very few were of acceptable quality and scattering power.

Refinement top

The U values of the carbon atoms were restrained such that anisotropic components along common bonds were approximately equal (command DELU $C). The largest peak of residual electron density is close to a heavy atoms, 0.9 Å from Re3.

Computing details top

Data collection: XSCANS (Siemens, 1995a); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1995b); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. Molecular structure showing 50% probability ellipsoids. H atoms are omitted.
bis-(octacarbonyl-µ-dicyclohexylphosphido-dirhenium)- dicarbonyl-platinum top
Crystal data top
[PtRe4(CO)18(C12H22P)2]F(000) = 3392
Mr = 1838.60Dx = 2.445 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 17.561 (2) ÅCell parameters from 21 reflections
b = 16.728 (3) Åθ = 7.5–13.2°
c = 17.408 (6) ŵ = 12.58 mm1
β = 102.42 (2)°T = 203 K
V = 4994 (2) Å3Needle, red
Z = 40.40 × 0.05 × 0.04 mm
Data collection top
Bruker P4
diffractometer
4254 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.059
Graphite monochromatorθmax = 26.5°, θmin = 2.4°
ω scansh = 2221
Absorption correction: ψ scan
(North et al., 1968)
k = 021
Tmin = 0.264, Tmax = 0.532l = 021
10719 measured reflections3 standard reflections every 397 reflections
10342 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.059H-atom parameters constrained
wR(F2) = 0.170 w = 1/[σ2(Fo2) + (0.0419P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.97(Δ/σ)max = 0.001
10342 reflectionsΔρmax = 1.33 e Å3
605 parametersΔρmin = 1.09 e Å3
984 restraintsExtinction correction: SHELXL, none
Primary atom site location: structure-invariant direct methodsExtinction coefficient: none
Crystal data top
[PtRe4(CO)18(C12H22P)2]V = 4994 (2) Å3
Mr = 1838.60Z = 4
Monoclinic, P21/cMo Kα radiation
a = 17.561 (2) ŵ = 12.58 mm1
b = 16.728 (3) ÅT = 203 K
c = 17.408 (6) Å0.40 × 0.05 × 0.04 mm
β = 102.42 (2)°
Data collection top
Bruker P4
diffractometer
4254 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.059
Tmin = 0.264, Tmax = 0.5323 standard reflections every 397 reflections
10719 measured reflections intensity decay: 1%
10342 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.059984 restraints
wR(F2) = 0.170H-atom parameters constrained
S = 0.97Δρmax = 1.33 e Å3
10342 reflectionsΔρmin = 1.09 e Å3
605 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Max./min. residual electron density in the very close vicinity of heavy atoms.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pt10.13666 (5)0.77198 (6)0.61435 (6)0.0344 (2)
Re10.02254 (5)0.73598 (6)0.60120 (5)0.0306 (2)
Re20.02303 (5)0.82922 (6)0.74965 (6)0.0302 (2)
Re30.28918 (5)0.73284 (6)0.52740 (6)0.0304 (2)
Re40.38559 (5)0.61900 (6)0.40553 (6)0.0322 (2)
P10.1020 (3)0.7773 (4)0.7288 (3)0.0301 (12)
P20.4254 (3)0.7394 (4)0.4603 (4)0.0331 (13)
O10.0310 (9)0.8999 (10)0.5165 (10)0.046 (4)
C10.0275 (12)0.8417 (13)0.5502 (13)0.031 (4)
O20.0119 (12)0.5667 (11)0.6715 (12)0.072 (6)
C20.0148 (15)0.6298 (14)0.6479 (15)0.042 (5)
O30.0892 (8)0.6832 (10)0.4455 (10)0.049 (5)
C30.0494 (13)0.7047 (14)0.5034 (15)0.042 (5)
O40.1674 (9)0.6786 (11)0.5457 (11)0.056 (5)
C40.1154 (13)0.6997 (13)0.5659 (14)0.037 (5)
O50.0407 (9)0.6729 (10)0.8449 (10)0.050 (5)
C50.0331 (13)0.7258 (13)0.8079 (11)0.028 (4)
O60.0033 (10)0.9914 (10)0.6649 (10)0.050 (5)
C60.0099 (11)0.9306 (14)0.6953 (13)0.030 (4)
O70.0502 (9)0.9086 (10)0.9083 (9)0.046 (4)
C70.0239 (12)0.8794 (12)0.8495 (13)0.028 (4)
O80.1857 (8)0.8813 (11)0.7792 (11)0.050 (5)
C80.1267 (12)0.8617 (13)0.7653 (13)0.032 (4)
O90.1457 (10)0.9309 (11)0.5287 (11)0.058 (5)
C90.1396 (12)0.8708 (14)0.5585 (14)0.035 (4)
O100.1499 (10)0.6152 (12)0.7002 (11)0.063 (6)
C100.1473 (14)0.6742 (16)0.6695 (13)0.041 (5)
O110.2405 (9)0.8193 (10)0.3846 (10)0.049 (5)
C110.2576 (12)0.7886 (16)0.4388 (14)0.041 (5)
O120.1938 (10)0.5779 (11)0.5093 (12)0.062 (5)
C120.2325 (11)0.6343 (14)0.5079 (16)0.042 (5)
O130.3084 (9)0.8931 (10)0.6154 (11)0.049 (5)
C130.2979 (13)0.8360 (13)0.5828 (14)0.035 (4)
O140.3374 (9)0.6491 (9)0.6697 (9)0.039 (4)
C140.3197 (12)0.6777 (12)0.6159 (13)0.030 (4)
O150.2839 (10)0.4811 (11)0.3645 (11)0.057 (5)
C150.3215 (13)0.5306 (13)0.3795 (15)0.037 (5)
O160.3517 (11)0.7080 (10)0.2587 (11)0.058 (5)
C160.3632 (12)0.6754 (13)0.3126 (13)0.030 (4)
O170.4220 (9)0.5205 (10)0.5451 (10)0.044 (4)
C170.4093 (12)0.5591 (14)0.4939 (13)0.033 (4)
O180.5402 (9)0.5650 (12)0.3008 (11)0.056 (5)
C180.4804 (14)0.5857 (15)0.3400 (14)0.042 (5)
C210.1876 (12)0.8453 (12)0.7341 (10)0.039 (5)
H210.23440.81120.75020.047*
C220.1948 (12)0.8842 (13)0.6568 (11)0.045 (5)
H22A0.19310.84290.61650.054*
H22B0.15070.92050.63890.054*
C230.2709 (12)0.9307 (13)0.6670 (13)0.053 (6)
H23A0.27430.95560.61690.064*
H23B0.31490.89380.68210.064*
C240.2760 (13)0.9953 (11)0.7300 (11)0.044 (5)
H24A0.32641.02260.73750.053*
H24B0.23481.03500.71310.053*
C250.2670 (12)0.9573 (13)0.8074 (11)0.047 (5)
H25A0.31200.92280.82730.056*
H25B0.26650.99950.84630.056*
C260.1931 (11)0.9083 (12)0.7981 (11)0.040 (5)
H26A0.14780.94390.78500.049*
H26B0.19180.88210.84810.049*
C310.1413 (12)0.6920 (12)0.7931 (10)0.041 (5)
H310.09670.65580.79280.050*
C320.1717 (12)0.7169 (10)0.8798 (10)0.035 (4)
H32A0.13140.74760.89790.042*
H32B0.21760.75120.88390.042*
C330.1935 (12)0.6424 (12)0.9329 (11)0.049 (6)
H33A0.21440.65940.98720.059*
H33B0.14680.61020.93220.059*
C340.2550 (11)0.5912 (12)0.9037 (11)0.044 (5)
H34A0.30350.62180.90880.053*
H34B0.26650.54310.93630.053*
C350.2250 (14)0.5669 (11)0.8170 (11)0.048 (6)
H35A0.17890.53280.81270.058*
H35B0.26530.53600.79910.058*
C360.2037 (14)0.6411 (12)0.7639 (12)0.049 (6)
H36A0.18330.62410.70950.059*
H36B0.25050.67340.76510.059*
C410.4939 (9)0.7258 (12)0.5247 (11)0.033 (4)
H410.46980.68540.56400.040*
C420.5750 (10)0.6907 (13)0.4839 (11)0.038 (5)
H42A0.60560.73150.45040.045*
H42B0.56770.64540.45050.045*
C430.6194 (12)0.6627 (13)0.5473 (13)0.050 (6)
H43A0.67010.64060.52160.060*
H43B0.58960.62040.57940.060*
C440.6316 (11)0.7336 (14)0.6009 (13)0.056 (6)
H44A0.65720.71440.64220.068*
H44B0.66540.77370.56970.068*
C450.5520 (11)0.7721 (15)0.6390 (12)0.053 (6)
H45A0.51940.73320.67330.063*
H45B0.56030.81820.67100.063*
C460.5104 (12)0.7994 (12)0.5730 (12)0.044 (5)
H46A0.54340.83760.53820.053*
H46B0.46120.82610.59640.053*
C510.4505 (9)0.8276 (10)0.3938 (13)0.036 (4)
H510.41800.82480.35390.043*
C520.4345 (12)0.9088 (9)0.4360 (12)0.043 (5)
H52A0.46350.91160.47820.051*
H52B0.37880.91290.46020.051*
C530.4582 (12)0.9797 (11)0.3796 (13)0.050 (6)
H53A0.45091.02970.40960.060*
H53B0.42430.98130.34160.060*
C540.5435 (11)0.9733 (11)0.3352 (14)0.050 (6)
H54A0.55591.01730.29740.060*
H54B0.57800.97730.37240.060*
C550.5565 (14)0.8926 (11)0.2914 (12)0.056 (6)
H55A0.61100.88840.26320.067*
H55B0.52350.88970.25280.067*
C560.5368 (10)0.8230 (11)0.3498 (13)0.046 (6)
H56A0.54630.77210.32150.055*
H56B0.57060.82530.38790.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.0285 (4)0.0394 (5)0.0349 (5)0.0035 (4)0.0060 (4)0.0022 (5)
Re10.0304 (4)0.0338 (5)0.0276 (5)0.0027 (4)0.0067 (4)0.0015 (4)
Re20.0311 (5)0.0312 (5)0.0292 (5)0.0004 (4)0.0084 (4)0.0009 (4)
Re30.0281 (4)0.0322 (5)0.0305 (5)0.0018 (4)0.0054 (4)0.0001 (4)
Re40.0313 (5)0.0335 (5)0.0323 (5)0.0007 (4)0.0078 (4)0.0024 (4)
P10.033 (3)0.030 (3)0.029 (3)0.002 (2)0.011 (2)0.002 (3)
P20.031 (3)0.037 (3)0.032 (3)0.001 (2)0.008 (2)0.001 (3)
O10.054 (10)0.037 (8)0.049 (12)0.000 (8)0.015 (9)0.002 (7)
C10.031 (9)0.034 (7)0.027 (9)0.007 (7)0.006 (8)0.003 (7)
O20.101 (15)0.039 (9)0.067 (15)0.018 (11)0.007 (12)0.010 (9)
C20.060 (13)0.025 (7)0.043 (13)0.003 (7)0.014 (10)0.011 (7)
O30.032 (9)0.055 (11)0.056 (10)0.011 (8)0.001 (7)0.017 (10)
C30.041 (10)0.041 (12)0.042 (9)0.005 (9)0.007 (6)0.011 (9)
O40.038 (9)0.059 (12)0.078 (14)0.009 (8)0.026 (9)0.013 (11)
C40.041 (8)0.031 (11)0.036 (11)0.013 (8)0.002 (8)0.003 (9)
O50.054 (10)0.041 (9)0.058 (12)0.017 (8)0.017 (9)0.027 (8)
C50.050 (11)0.031 (7)0.019 (8)0.001 (8)0.019 (7)0.007 (6)
O60.063 (11)0.047 (9)0.047 (12)0.015 (9)0.028 (10)0.003 (8)
C60.023 (9)0.038 (8)0.028 (10)0.003 (6)0.001 (8)0.005 (7)
O70.059 (11)0.053 (11)0.025 (8)0.008 (9)0.005 (8)0.009 (8)
C70.039 (10)0.016 (9)0.031 (8)0.008 (8)0.008 (7)0.002 (7)
O80.023 (7)0.070 (12)0.060 (12)0.004 (8)0.012 (8)0.010 (10)
C80.030 (7)0.037 (12)0.028 (10)0.000 (7)0.008 (7)0.005 (8)
O90.056 (11)0.054 (10)0.065 (14)0.002 (9)0.014 (10)0.025 (9)
C90.031 (9)0.044 (10)0.033 (10)0.001 (6)0.012 (8)0.005 (9)
O100.053 (11)0.074 (12)0.063 (13)0.016 (10)0.012 (10)0.034 (10)
C100.050 (10)0.058 (11)0.015 (11)0.020 (10)0.008 (7)0.007 (8)
O110.043 (9)0.059 (12)0.054 (11)0.015 (9)0.030 (9)0.002 (9)
C110.029 (9)0.066 (12)0.030 (8)0.009 (9)0.007 (6)0.003 (8)
O120.052 (11)0.049 (10)0.087 (15)0.012 (8)0.020 (11)0.001 (11)
C120.016 (7)0.038 (8)0.076 (16)0.009 (6)0.021 (7)0.017 (9)
O130.031 (8)0.043 (9)0.072 (13)0.001 (8)0.010 (9)0.014 (8)
C130.040 (8)0.026 (7)0.040 (12)0.006 (7)0.012 (9)0.001 (7)
O140.052 (10)0.047 (10)0.022 (8)0.015 (8)0.014 (7)0.012 (7)
C140.036 (9)0.023 (9)0.033 (7)0.005 (8)0.009 (6)0.003 (7)
O150.055 (11)0.054 (11)0.069 (13)0.005 (8)0.026 (10)0.025 (10)
C150.041 (10)0.022 (8)0.054 (14)0.006 (7)0.020 (10)0.001 (7)
O160.088 (13)0.039 (10)0.046 (11)0.005 (10)0.014 (10)0.015 (8)
C160.030 (10)0.027 (10)0.030 (7)0.002 (8)0.001 (7)0.003 (6)
O170.046 (9)0.050 (11)0.039 (10)0.008 (8)0.015 (8)0.007 (8)
C170.030 (11)0.040 (8)0.027 (9)0.011 (8)0.003 (8)0.006 (8)
O180.032 (8)0.083 (14)0.052 (12)0.009 (9)0.005 (7)0.001 (11)
C180.045 (8)0.050 (13)0.026 (11)0.007 (8)0.001 (8)0.004 (9)
C210.029 (8)0.060 (12)0.031 (10)0.015 (8)0.013 (8)0.016 (8)
C220.044 (12)0.052 (13)0.047 (11)0.018 (9)0.028 (10)0.012 (9)
C230.049 (12)0.050 (13)0.076 (14)0.020 (10)0.045 (12)0.020 (11)
C240.039 (11)0.035 (12)0.060 (13)0.014 (9)0.013 (11)0.010 (9)
C250.044 (12)0.044 (13)0.042 (11)0.004 (9)0.012 (11)0.003 (10)
C260.042 (11)0.038 (11)0.040 (11)0.000 (8)0.006 (10)0.004 (9)
C310.051 (12)0.037 (10)0.034 (8)0.013 (7)0.005 (8)0.001 (8)
C320.042 (11)0.022 (10)0.038 (8)0.004 (8)0.004 (9)0.002 (7)
C330.040 (12)0.062 (14)0.045 (10)0.017 (11)0.009 (10)0.022 (10)
C340.034 (11)0.035 (11)0.060 (11)0.001 (8)0.002 (10)0.010 (10)
C350.053 (13)0.037 (12)0.052 (12)0.010 (9)0.006 (11)0.014 (9)
C360.069 (14)0.035 (12)0.046 (11)0.018 (9)0.021 (11)0.003 (9)
C410.032 (7)0.035 (10)0.034 (11)0.008 (8)0.010 (7)0.007 (8)
C420.041 (9)0.038 (12)0.036 (12)0.009 (9)0.015 (8)0.004 (9)
C430.041 (11)0.056 (14)0.063 (15)0.003 (10)0.032 (10)0.005 (10)
C440.044 (11)0.080 (16)0.057 (14)0.000 (11)0.038 (10)0.001 (12)
C450.046 (11)0.066 (15)0.055 (14)0.005 (11)0.030 (10)0.005 (11)
C460.036 (11)0.046 (12)0.054 (14)0.007 (9)0.017 (9)0.013 (9)
C510.020 (8)0.031 (6)0.052 (12)0.017 (7)0.002 (8)0.005 (7)
C520.050 (12)0.028 (7)0.052 (14)0.021 (9)0.017 (9)0.010 (8)
C530.064 (12)0.033 (9)0.050 (15)0.000 (11)0.004 (11)0.006 (10)
C540.049 (11)0.044 (10)0.059 (15)0.009 (11)0.014 (10)0.007 (10)
C550.061 (14)0.057 (13)0.044 (14)0.006 (11)0.005 (10)0.004 (9)
C560.046 (10)0.047 (10)0.033 (12)0.007 (9)0.015 (9)0.013 (9)
Geometric parameters (Å, º) top
Pt1—C91.91 (2)O7—C71.14 (2)
Pt1—C101.93 (2)O8—C81.16 (2)
Pt1—Re32.8548 (13)O9—C91.12 (3)
Pt1—Re22.9025 (15)O10—C101.13 (3)
Pt1—Re12.9165 (12)O11—C111.17 (3)
Re1—Re23.2620 (15)O12—C121.16 (3)
Re1—C41.96 (2)O13—C131.15 (3)
Re1—C31.96 (2)O14—C141.15 (2)
Re1—C21.97 (2)O15—C151.12 (2)
Re1—C11.99 (2)O16—C161.14 (3)
Re1—P12.454 (6)O17—C171.16 (3)
Re2—C71.95 (2)O18—C181.18 (3)
Re2—C81.97 (2)C21—C261.523 (15)
Re2—C61.98 (2)C21—C221.525 (15)
Re2—C52.03 (2)C22—C231.523 (15)
Re2—P12.459 (6)C23—C241.528 (15)
Re3—C141.97 (2)C24—C251.528 (15)
Re3—C111.98 (2)C25—C261.514 (15)
Re3—C121.99 (2)C31—C321.546 (15)
Re3—C132.00 (2)C31—C361.557 (15)
Re3—P22.429 (6)C32—C331.550 (15)
Re3—Re43.0739 (15)C33—C341.547 (15)
Re4—C181.89 (2)C34—C351.542 (15)
Re4—C171.95 (2)C35—C361.545 (15)
Re4—C151.97 (2)C41—C461.553 (15)
Re4—C161.98 (2)C41—C421.563 (15)
Re4—P22.396 (6)C42—C431.555 (15)
P1—C311.853 (19)C43—C441.552 (15)
P1—C211.872 (18)C44—C451.552 (15)
P2—C411.825 (18)C45—C461.558 (16)
P2—C511.870 (19)C51—C521.542 (15)
O1—C11.14 (2)C51—C561.546 (15)
O2—C21.14 (3)C52—C531.539 (15)
O3—C31.15 (3)C53—C541.534 (15)
O4—C41.10 (2)C54—C551.543 (16)
O5—C51.12 (2)C55—C561.535 (16)
O6—C61.16 (2)
C9—Pt1—C10172.9 (10)C17—Re4—C1591.4 (10)
C9—Pt1—Re390.5 (7)C18—Re4—C1687.2 (9)
C10—Pt1—Re383.6 (7)C17—Re4—C16177.3 (9)
C9—Pt1—Re293.8 (7)C15—Re4—C1686.9 (9)
C10—Pt1—Re289.9 (7)C18—Re4—P2101.1 (8)
Re3—Pt1—Re2155.33 (4)C17—Re4—P289.3 (7)
C9—Pt1—Re193.4 (6)C15—Re4—P2162.3 (7)
C10—Pt1—Re193.5 (7)C16—Re4—P292.9 (6)
Re3—Pt1—Re1135.80 (4)C18—Re4—Re3152.0 (8)
Re2—Pt1—Re168.19 (4)C17—Re4—Re387.4 (6)
C4—Re1—Re2139.4 (7)C15—Re4—Re3111.5 (7)
C3—Re1—Re2126.4 (7)C16—Re4—Re395.3 (6)
C2—Re1—Re293.1 (7)P2—Re4—Re350.89 (14)
C1—Re1—Re288.3 (6)C31—P1—C21104.3 (10)
P1—Re1—Re248.47 (13)C31—P1—Re1113.3 (7)
Pt1—Re1—Re255.70 (3)C21—P1—Re1120.7 (6)
C4—Re1—C394.0 (10)C31—P1—Re2114.3 (7)
C4—Re1—C289.2 (10)C21—P1—Re2120.8 (7)
C3—Re1—C291.7 (10)Re1—P1—Re283.19 (18)
C4—Re1—C190.9 (9)C41—P2—C51112.3 (10)
C3—Re1—C186.0 (10)C41—P2—Re4115.3 (7)
C2—Re1—C1177.7 (10)C51—P2—Re4117.8 (7)
C4—Re1—P191.2 (7)C41—P2—Re3114.2 (7)
C3—Re1—P1174.7 (7)C51—P2—Re3114.2 (5)
C2—Re1—P187.5 (7)Re4—P2—Re379.15 (18)
C1—Re1—P194.8 (6)O1—C1—Re1176 (2)
C4—Re1—Pt1164.9 (7)O2—C2—Re1176 (2)
C3—Re1—Pt170.9 (7)O3—C3—Re1177 (2)
C2—Re1—Pt190.1 (7)O4—C4—Re1179 (2)
C1—Re1—Pt189.2 (6)O5—C5—Re2173.9 (18)
P1—Re1—Pt1103.81 (14)O6—C6—Re2178 (2)
C7—Re2—Re1141.7 (6)O7—C7—Re2179 (2)
C8—Re2—Re1129.2 (7)O8—C8—Re2176 (2)
C6—Re2—Re187.5 (7)O9—C9—Pt1175 (2)
C5—Re2—Re192.9 (5)O10—C10—Pt1176 (2)
P1—Re2—Re148.34 (14)O11—C11—Re3177 (2)
Pt1—Re2—Re156.11 (3)O12—C12—Re3169 (2)
C7—Re2—C889.1 (9)O13—C13—Re3175 (2)
C7—Re2—C689.3 (9)O14—C14—Re3176.5 (19)
C8—Re2—C692.1 (9)O15—C15—Re4179 (2)
C7—Re2—C589.2 (8)O16—C16—Re4179 (2)
C8—Re2—C589.0 (9)O17—C17—Re4177 (2)
C6—Re2—C5178.1 (9)O18—C18—Re4178 (2)
C7—Re2—P193.7 (6)C26—C21—C22110.2 (14)
C8—Re2—P1175.2 (7)C26—C21—P1112.4 (12)
C6—Re2—P191.8 (6)C22—C21—P1115.7 (12)
C5—Re2—P187.1 (6)C23—C22—C21110.6 (14)
C7—Re2—Pt1162.2 (6)C22—C23—C24111.1 (14)
C8—Re2—Pt173.1 (7)C25—C24—C23109.7 (14)
C6—Re2—Pt191.4 (6)C26—C25—C24112.3 (13)
C5—Re2—Pt190.3 (6)C25—C26—C21111.7 (13)
P1—Re2—Pt1104.08 (15)C32—C31—C36110.3 (14)
C14—Re3—C11179.5 (9)C32—C31—P1112.9 (12)
C14—Re3—C1288.6 (10)C36—C31—P1114.9 (13)
C11—Re3—C1291.3 (11)C31—C32—C33110.8 (13)
C14—Re3—C1388.0 (9)C34—C33—C32110.5 (13)
C11—Re3—C1391.8 (10)C35—C34—C33110.6 (13)
C12—Re3—C13152.9 (9)C34—C35—C36111.2 (14)
C14—Re3—P289.5 (6)C35—C36—C31109.9 (14)
C11—Re3—P291.0 (6)C46—C41—C42106.6 (13)
C12—Re3—P2115.6 (7)C46—C41—P2117.2 (12)
C13—Re3—P291.3 (7)C42—C41—P2115.1 (12)
C14—Re3—Pt194.3 (6)C43—C42—C41109.7 (13)
C11—Re3—Pt185.2 (6)C44—C43—C42110.6 (14)
C12—Re3—Pt180.5 (6)C43—C44—C45110.3 (14)
C13—Re3—Pt173.0 (6)C44—C45—C46109.2 (14)
P2—Re3—Pt1163.66 (16)C41—C46—C45109.8 (14)
C14—Re3—Re492.7 (6)C52—C51—C56109.8 (13)
C11—Re3—Re487.7 (7)C52—C51—P2113.9 (13)
C12—Re3—Re465.8 (7)C56—C51—P2110.0 (12)
C13—Re3—Re4141.2 (6)C53—C52—C51112.2 (14)
P2—Re3—Re449.95 (15)C54—C53—C52111.6 (14)
Pt1—Re3—Re4145.35 (4)C53—C54—C55109.6 (14)
C18—Re4—C1790.8 (10)C56—C55—C54110.4 (14)
C18—Re4—C1596.5 (10)C55—C56—C51110.3 (14)

Experimental details

Crystal data
Chemical formula[PtRe4(CO)18(C12H22P)2]
Mr1838.60
Crystal system, space groupMonoclinic, P21/c
Temperature (K)203
a, b, c (Å)17.561 (2), 16.728 (3), 17.408 (6)
β (°) 102.42 (2)
V3)4994 (2)
Z4
Radiation typeMo Kα
µ (mm1)12.58
Crystal size (mm)0.40 × 0.05 × 0.04
Data collection
DiffractometerBruker P4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.264, 0.532
No. of measured, independent and
observed [I > 2σ(I)] reflections
10719, 10342, 4254
Rint0.059
(sin θ/λ)max1)0.628
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.059, 0.170, 0.97
No. of reflections10342
No. of parameters605
No. of restraints984
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.33, 1.09

Computer programs: XSCANS (Siemens, 1995a), XSCANS, SHELXTL (Siemens, 1995b), SHELXTL.

Selected geometric parameters (Å, º) top
Pt1—Re32.8548 (13)Re2—P12.459 (6)
Pt1—Re22.9025 (15)Re3—P22.429 (6)
Pt1—Re12.9165 (12)Re3—Re43.0739 (15)
Re1—Re23.2620 (15)Re4—P22.396 (6)
Re1—P12.454 (6)
C9—Pt1—C10172.9 (10)Pt1—Re2—Re156.11 (3)
Re3—Pt1—Re2155.33 (4)P1—Re2—Pt1104.08 (15)
Re3—Pt1—Re1135.80 (4)P2—Re3—Pt1163.66 (16)
Re2—Pt1—Re168.19 (4)C12—Re3—Re465.8 (7)
C3—Re1—Re2126.4 (7)P2—Re3—Re449.95 (15)
P1—Re1—Re248.47 (13)Pt1—Re3—Re4145.35 (4)
Pt1—Re1—Re255.70 (3)C15—Re4—Re3111.5 (7)
P1—Re1—Pt1103.81 (14)P2—Re4—Re350.89 (14)
C8—Re2—Re1129.2 (7)Re1—P1—Re283.19 (18)
P1—Re2—Re148.34 (14)Re4—P2—Re379.15 (18)
 

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