[μ-Bis(diphenyl­phosphan­yl-κP)methane]­deca­carbonyl­tri-μ-hydrido-trirhenium(I)(3 Re—Re) dichloromethane solvate

Abdel-Magied, A.F.; Singh, A.K.; Haukka, M.; Nordlander, E.

doi:10.1107/S1600536811049312

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 12| December 2011| Page m1816

https://doi.org/10.1107/S1600536811049312

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[μ-Bis(diphenylphosphanyl-κP)methane]decacarbonyltri-μ-hydrido-trirhenium(I)(3 Re—Re) dichloromethane solvate

Ahmed F. Abdel-Magied,^a Amrendra K. Singh,^a Matti Haukka ^b and Ebbe Nordlander ^a ^*

^aInorganic Chemistry Research Group, Chemical Physics, Center for Chemistry and Chemical Engineering, Lund University, Box 124, SE-221 00 Lund, Sweden, and ^bDepartment of Chemistry, University of Eastern Finland, Box 111, FIN-80 101 Joensuu, Finland
^*Correspondence e-mail: Ebbe.Nordlander@chemphys.lu.se

(Received 4 November 2011; accepted 18 November 2011; online 25 November 2011)

In the title compound, [Re₃(μ-H)₃(C₂₅H₂₂P₂)(CO)₁₀]·CH₂Cl₂, the three Re atoms form a triangle bearing ten terminal carbonyl groups and three edge-bridging hydrides. The bis(diphenylphosphanyl)methane ligand bridges two Re atoms. Neglecting the Re—Re interactions, each Re atom is in a slightly distorted octahedral coordination environment. The dichloromethane solvent molecule is disordered over two sets of sites with fixed occupancies of 0.6 and 0.4.

Related literature

For general background to the reaction between rhenium complexes and the bis(diphenylphosphanyl)methane ligand, see: Prest et al. (1982 ). For related rhenium complexes, see: Adams et al. (1993 ). For the treatment of the hydride atoms, see: Orpen (1980 ).

Experimental

Crystal data

[Re₃H₃(C₂₅H₂₂P₂)(CO)₁₀]·CH₂Cl₂
M_r = 1311.02
Monoclinic, P 2₁ /c
a = 16.7907 (6) Å
b = 14.5316 (5) Å
c = 17.1593 (6) Å
β = 106.445 (1)°
V = 4015.5 (2) Å³
Z = 4
Mo Kα radiation
μ = 9.29 mm⁻¹
T = 100 K
0.16 × 0.15 × 0.08 mm

Data collection

Bruker Kappa APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2009 ) T_min = 0.320, T_max = 0.527
35918 measured reflections
8540 independent reflections
7349 reflections with I > 2σ(I)
R_int = 0.031

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.081
S = 1.06
8540 reflections
472 parameters
42 restraints
H-atom parameters constrained
Δρ_max = 3.82 e Å⁻³
Δρ_min = −2.54 e Å⁻³

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811049312/lh5374sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811049312/lh5374Isup2.hkl

Supporting information file. DOI: https://doi.org/10.1107/S1600536811049312/lh5374Isup3.cdx

checkCIF report

Comment top

The title compound has been reported to form during the reaction between [Re₃(µ-H)₃(CO)₁₂] and bis[(diphenylphosphino)methane] (dppm) (Prest et al.1982); however, its characterization was only based on spectroscopic analysis. We have synthesized this compound during our investigation of similar clusters with diphosphine ligands and the structure of the compound has been established by single-crystal X-ray diffraction. In the title cluster (Fig. 1) the three rhenium atoms form a triangle, bearing ten terminal C≡O groups with three edge-bridging hydrides. The bis[(diphenylphosphino)methane] ligand forms a symmetric bridge over the Re1—Re2 edge. The two triangular edges, Re1—Re3 and Re2—Re3, exhibit bond lengths typical of hydrogen bridged Re—H—Re bonds, 3.2909 (4) and 3.2901 (4) Å, and the third, shorter edge, Re1—Re2 [3.2358 (4) Å], which is doubly bridged by a hydride and the bis[(diphenylphosphino)methane] ligand are comparable with the corresponding interactions in [Re₃(µ-H)₃(CO)₁₀(µ-dppa)] (dppa = C₂(PPh₂)₂), where the corresponding Re1—Re3 and Re2—Re3 distances are 3.290 (1) and 3.290 (1) Å, respectively, and the doubly bridged Re1—Re2 distance is 3.303 (1) Å (Adams et al. 1993). The two Re—P bonds, Re1—P1 and Re2—P2 are very similar, 2.4535 (17) and 2.4592 (16) Å, respectively, and also similar to the corresponding Re—P distances reported for [Re₃(µ-H)₃(CO)₁₀(µ-dppa)], Re1—P1 and Re2—P2, 2.456 (5) and 2.457 (5) Å, respectively.

Related literature top

For general background to the reaction between rhenium complexes and the bis[(diphenylphosphino)methane] ligand, see: Prest et al. (1982). For related rhenium complexes, see: Adams et al. (1993). For the treatment of the hydride atoms, see: Orpen (1980).

Experimental top

The cluster [Re₃(µ-H)₃(CO)₁₁(NCMe)] (50 mg, 0.055 mmol) and bis[(diphenylphosphino)methane] (42 mg, 0.11 mmol) were stirred for 120 min in dichloromethane (20 ml). A solution of trimethylamine N-oxide (8.2 mg, 0.11 mmol) in dichloromethane (5 ml) was added dropwise during 30 minutes and the reaction was stirred at room temperature until complete conversion had occurred, as judged by spot TLC. The solvent was removed under vacuum and the residue dissolved in a minimum quantity of dichloromethane. The products were then separated by thin layer chromatography on silica using dichloromethane:petroleum ether (1:1) mixture as eluent. The order of elution (decreasing R_f values) was [Re₂(CO)₈(dppm)] (1) and [Re₃(µ-H)₃(CO)₁₀(dppm)] (2). Final purification was achieved by recrystallization of compound (2) from dichloromethane-hexane.

Structure description top

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

Fig. 1. The molecular structure of the title compound, showing 50% probability displacement ellipsoids.

[µ-Bis(diphenylphosphanyl-κP)methane]decacarbonyltri-µ-hydrido- trirhenium(I)(3 Re—Re) dichloromethane solvate top

Crystal data top

[Re₃H₃(C₂₅H₂₂P₂)(CO)₁₀]·CH₂Cl₂	F(000) = 2448
M_r = 1311.02	D_x = 2.169 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9836 reflections
a = 16.7907 (6) Å	θ = 2.5–28.3°
b = 14.5316 (5) Å	µ = 9.29 mm⁻¹
c = 17.1593 (6) Å	T = 100 K
β = 106.445 (1)°	Block, colourless
V = 4015.5 (2) Å³	0.16 × 0.15 × 0.08 mm
Z = 4

Data collection top

Bruker Kappa APEXII CCD diffractometer	8540 independent reflections
Radiation source: fine-focus sealed tube	7349 reflections with I > 2σ(I)
Horizontally mounted graphite crystal monochromator	R_int = 0.031
Detector resolution: 16 pixels mm^-1	θ_max = 27.0°, θ_min = 1.9°
φ scans and ω scans with κ offset	h = −19→21
Absorption correction: multi-scan (SADABS; Bruker, 2009)	k = −18→18
T_min = 0.320, T_max = 0.527	l = −21→21
35918 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.081	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0308P)² + 45.3016P] where P = (F_o² + 2F_c²)/3
8540 reflections	(Δ/σ)_max = 0.001
472 parameters	Δρ_max = 3.82 e Å⁻³
42 restraints	Δρ_min = −2.54 e Å⁻³

Crystal data top

[Re₃H₃(C₂₅H₂₂P₂)(CO)₁₀]·CH₂Cl₂	V = 4015.5 (2) Å³
M_r = 1311.02	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 16.7907 (6) Å	µ = 9.29 mm⁻¹
b = 14.5316 (5) Å	T = 100 K
c = 17.1593 (6) Å	0.16 × 0.15 × 0.08 mm
β = 106.445 (1)°

Data collection top

Bruker Kappa APEXII CCD diffractometer	8540 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2009)	7349 reflections with I > 2σ(I)
T_min = 0.320, T_max = 0.527	R_int = 0.031
35918 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	42 restraints
wR(F²) = 0.081	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0308P)² + 45.3016P] where P = (F_o² + 2F_c²)/3
8540 reflections	Δρ_max = 3.82 e Å⁻³
472 parameters	Δρ_min = −2.54 e Å⁻³

Special details top

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

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

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Re1	0.351643 (16)	0.492337 (18)	0.253498 (15)	0.01644 (7)
H1H	0.3064	0.3969	0.1844	0.025*
Re2	0.347215 (15)	0.278309 (18)	0.200401 (15)	0.01512 (7)
H2H	0.4030	0.4350	0.3503	0.023*
Re3	0.485711 (16)	0.347203 (18)	0.367087 (15)	0.01646 (7)
H3H	0.4244	0.2583	0.2995	0.025*
P1	0.23187 (10)	0.45699 (12)	0.30346 (10)	0.0171 (3)
P2	0.24865 (10)	0.24363 (12)	0.27854 (10)	0.0156 (3)
O1	0.2401 (4)	0.6139 (5)	0.1200 (4)	0.0461 (17)
O2	0.4131 (4)	0.6613 (4)	0.3622 (4)	0.0428 (15)
O3	0.4858 (3)	0.5337 (4)	0.1674 (3)	0.0276 (11)
O4	0.2093 (4)	0.2497 (4)	0.0421 (3)	0.0341 (13)
O5	0.3835 (3)	0.0763 (4)	0.1708 (3)	0.0317 (12)
O6	0.4694 (3)	0.3388 (4)	0.1046 (3)	0.0304 (12)
O7	0.6062 (4)	0.1901 (4)	0.4430 (4)	0.0381 (14)
O8	0.5898 (3)	0.4864 (4)	0.4905 (3)	0.0275 (12)
O9	0.6049 (3)	0.3830 (4)	0.2584 (3)	0.0346 (13)
O10	0.3944 (3)	0.3069 (4)	0.4985 (3)	0.0282 (12)
C1	0.2817 (5)	0.5669 (6)	0.1700 (5)	0.0308 (18)
C2	0.3884 (5)	0.5988 (5)	0.3212 (5)	0.0277 (16)
C3	0.4386 (4)	0.5154 (5)	0.2015 (4)	0.0206 (14)
C4	0.2602 (4)	0.2650 (5)	0.1007 (4)	0.0229 (15)
C5	0.3719 (4)	0.1514 (5)	0.1863 (4)	0.0223 (15)
C6	0.4252 (4)	0.3156 (5)	0.1403 (4)	0.0197 (14)
C7	0.5611 (5)	0.2486 (5)	0.4131 (4)	0.0270 (16)
C8	0.5520 (4)	0.4352 (5)	0.4442 (4)	0.0211 (14)
C9	0.5576 (4)	0.3729 (5)	0.2943 (4)	0.0240 (15)
C10	0.4252 (4)	0.3192 (5)	0.4483 (4)	0.0209 (14)
C11	0.2221 (4)	0.5281 (5)	0.3884 (4)	0.0201 (14)
C12	0.2253 (4)	0.6224 (5)	0.3785 (4)	0.0253 (15)
H12	0.2265	0.6469	0.3275	0.030*
C13	0.2270 (5)	0.6815 (6)	0.4424 (5)	0.0304 (17)
H13	0.2293	0.7461	0.4348	0.036*
C14	0.2253 (4)	0.6475 (6)	0.5162 (5)	0.0304 (18)
H14	0.2276	0.6882	0.5602	0.036*
C15	0.2203 (4)	0.5532 (6)	0.5264 (4)	0.0281 (17)
H15	0.2182	0.5293	0.5773	0.034*
C16	0.2182 (4)	0.4935 (5)	0.4629 (4)	0.0227 (15)
H16	0.2142	0.4291	0.4703	0.027*
C17	0.1310 (4)	0.4679 (5)	0.2275 (4)	0.0234 (15)
C18	0.0606 (5)	0.4920 (5)	0.2507 (5)	0.0285 (16)
H18	0.0658	0.5097	0.3052	0.034*
C19	−0.0172 (5)	0.4901 (7)	0.1940 (5)	0.041 (2)
H19	−0.0651	0.5062	0.2099	0.049*
C20	−0.0250 (5)	0.4648 (8)	0.1147 (5)	0.049 (3)
H20	−0.0784	0.4633	0.0764	0.058*
C21	0.0444 (5)	0.4415 (7)	0.0906 (5)	0.043 (2)
H21	0.0390	0.4243	0.0359	0.051*
C22	0.1219 (5)	0.4436 (6)	0.1471 (4)	0.0302 (17)
H22	0.1697	0.4281	0.1306	0.036*
C23	0.2261 (4)	0.3387 (4)	0.3400 (4)	0.0161 (13)
H23A	0.2651	0.3339	0.3952	0.019*
H23B	0.1695	0.3291	0.3453	0.019*
C24	0.1478 (4)	0.2025 (5)	0.2166 (4)	0.0202 (14)
C25	0.0718 (4)	0.2421 (6)	0.2124 (5)	0.0289 (17)
H25	0.0693	0.2940	0.2453	0.035*
C26	−0.0006 (5)	0.2072 (6)	0.1609 (5)	0.0354 (19)
H26	−0.0521	0.2358	0.1585	0.042*
C27	0.0007 (5)	0.1314 (7)	0.1127 (5)	0.037 (2)
H27	−0.0494	0.1082	0.0771	0.045*
C28	0.0762 (5)	0.0894 (7)	0.1170 (5)	0.041 (2)
H28	0.0781	0.0369	0.0846	0.049*
C29	0.1488 (5)	0.1247 (6)	0.1689 (5)	0.0316 (18)
H29	0.2002	0.0954	0.1720	0.038*
C30	0.2760 (4)	0.1528 (5)	0.3552 (4)	0.0183 (13)
C31	0.2201 (4)	0.1287 (5)	0.3989 (4)	0.0217 (14)
H31	0.1677	0.1583	0.3874	0.026*
C32	0.2409 (5)	0.0618 (5)	0.4586 (4)	0.0253 (15)
H32	0.2030	0.0461	0.4884	0.030*
C33	0.3170 (5)	0.0177 (6)	0.4750 (5)	0.036 (2)
H33	0.3316	−0.0277	0.5165	0.043*
C34	0.3718 (5)	0.0397 (7)	0.4312 (5)	0.041 (2)
H34	0.4232	0.0081	0.4414	0.049*
C35	0.3521 (5)	0.1075 (6)	0.3726 (5)	0.0299 (17)
H35	0.3909	0.1234	0.3438	0.036*
C1S	−0.0818 (8)	0.2204 (10)	0.3584 (7)	0.199 (3)	0.60
H1S1	−0.1101	0.1945	0.3969	0.238*	0.60
H1S2	−0.0693	0.1696	0.3253	0.238*	0.60
Cl1	0.0123 (9)	0.2785 (10)	0.4128 (11)	0.199 (3)	0.60
Cl2	−0.1495 (9)	0.3089 (10)	0.2913 (7)	0.199 (3)	0.60
C1SB	0.020 (3)	0.244 (3)	0.421 (5)	0.199 (3)	0.40
H1S3	0.0627	0.2072	0.4057	0.238*	0.40
H1S4	0.0250	0.2341	0.4796	0.238*	0.40
Cl1B	0.0272 (15)	0.3638 (16)	0.3988 (11)	0.199 (3)	0.40
Cl2B	−0.0818 (8)	0.2204 (10)	0.3584 (7)	0.199 (3)	0.40

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Re1	0.01569 (13)	0.02024 (14)	0.01461 (13)	0.00154 (10)	0.00627 (10)	0.00231 (10)
Re2	0.01404 (12)	0.02085 (14)	0.01086 (12)	−0.00069 (10)	0.00418 (9)	−0.00074 (9)
Re3	0.01399 (13)	0.02069 (14)	0.01367 (13)	0.00099 (10)	0.00226 (10)	−0.00083 (10)
P1	0.0156 (8)	0.0220 (9)	0.0142 (8)	0.0041 (7)	0.0053 (6)	0.0028 (6)
P2	0.0126 (8)	0.0214 (9)	0.0127 (8)	0.0003 (6)	0.0034 (6)	0.0007 (6)
O1	0.036 (3)	0.062 (4)	0.047 (4)	0.023 (3)	0.023 (3)	0.036 (3)
O2	0.052 (4)	0.033 (3)	0.052 (4)	−0.013 (3)	0.027 (3)	−0.017 (3)
O3	0.026 (3)	0.034 (3)	0.026 (3)	−0.003 (2)	0.012 (2)	0.000 (2)
O4	0.038 (3)	0.042 (3)	0.018 (3)	−0.013 (3)	−0.001 (2)	0.003 (2)
O5	0.040 (3)	0.030 (3)	0.024 (3)	0.004 (2)	0.006 (2)	−0.004 (2)
O6	0.032 (3)	0.040 (3)	0.026 (3)	−0.011 (2)	0.020 (2)	−0.011 (2)
O7	0.033 (3)	0.030 (3)	0.043 (3)	0.012 (3)	−0.003 (3)	−0.001 (3)
O8	0.019 (3)	0.037 (3)	0.025 (3)	−0.003 (2)	0.004 (2)	−0.012 (2)
O9	0.024 (3)	0.048 (4)	0.036 (3)	−0.004 (3)	0.016 (2)	−0.003 (3)
O10	0.028 (3)	0.039 (3)	0.018 (3)	0.000 (2)	0.006 (2)	0.006 (2)
C1	0.028 (4)	0.038 (5)	0.034 (4)	0.008 (3)	0.021 (3)	0.011 (4)
C2	0.027 (4)	0.031 (4)	0.030 (4)	0.000 (3)	0.016 (3)	0.004 (3)
C3	0.016 (3)	0.029 (4)	0.017 (3)	0.001 (3)	0.004 (3)	−0.001 (3)
C4	0.024 (4)	0.029 (4)	0.015 (3)	−0.006 (3)	0.005 (3)	0.006 (3)
C5	0.021 (3)	0.032 (4)	0.013 (3)	0.000 (3)	0.003 (3)	−0.001 (3)
C6	0.023 (3)	0.020 (3)	0.016 (3)	−0.006 (3)	0.006 (3)	−0.006 (3)
C7	0.026 (4)	0.032 (4)	0.020 (4)	−0.003 (3)	0.002 (3)	−0.006 (3)
C8	0.016 (3)	0.025 (4)	0.022 (3)	0.005 (3)	0.005 (3)	0.002 (3)
C9	0.018 (3)	0.029 (4)	0.021 (3)	0.001 (3)	0.001 (3)	−0.004 (3)
C10	0.016 (3)	0.024 (4)	0.019 (3)	0.000 (3)	−0.001 (3)	0.002 (3)
C11	0.011 (3)	0.031 (4)	0.018 (3)	0.005 (3)	0.004 (3)	0.001 (3)
C12	0.020 (3)	0.035 (4)	0.021 (3)	0.007 (3)	0.006 (3)	0.001 (3)
C13	0.027 (4)	0.034 (4)	0.030 (4)	0.003 (3)	0.008 (3)	−0.006 (3)
C14	0.020 (4)	0.046 (5)	0.023 (4)	0.002 (3)	0.003 (3)	−0.015 (3)
C15	0.021 (4)	0.046 (5)	0.017 (3)	0.000 (3)	0.005 (3)	−0.003 (3)
C16	0.019 (3)	0.032 (4)	0.019 (3)	0.003 (3)	0.008 (3)	0.000 (3)
C17	0.019 (3)	0.030 (4)	0.021 (3)	0.008 (3)	0.004 (3)	0.008 (3)
C18	0.023 (4)	0.032 (4)	0.031 (4)	0.008 (3)	0.007 (3)	0.003 (3)
C19	0.020 (4)	0.063 (6)	0.037 (5)	0.014 (4)	0.004 (3)	0.006 (4)
C20	0.023 (4)	0.085 (8)	0.027 (5)	0.012 (4)	−0.009 (3)	0.012 (5)
C21	0.032 (4)	0.072 (7)	0.019 (4)	0.010 (4)	−0.003 (3)	0.006 (4)
C22	0.024 (4)	0.048 (5)	0.018 (4)	0.003 (3)	0.006 (3)	0.004 (3)
C23	0.013 (3)	0.020 (3)	0.013 (3)	0.000 (2)	0.000 (2)	0.003 (2)
C24	0.020 (3)	0.025 (4)	0.015 (3)	−0.005 (3)	0.003 (3)	0.004 (3)
C25	0.018 (4)	0.033 (4)	0.035 (4)	0.002 (3)	0.006 (3)	0.008 (3)
C26	0.018 (4)	0.042 (5)	0.044 (5)	0.001 (3)	0.005 (3)	0.012 (4)
C27	0.020 (4)	0.064 (6)	0.027 (4)	−0.020 (4)	0.003 (3)	0.003 (4)
C28	0.033 (5)	0.061 (6)	0.031 (4)	−0.018 (4)	0.013 (4)	−0.014 (4)
C29	0.020 (4)	0.044 (5)	0.031 (4)	−0.007 (3)	0.008 (3)	−0.013 (4)
C30	0.018 (3)	0.022 (3)	0.012 (3)	−0.001 (3)	0.000 (3)	0.000 (2)
C31	0.020 (3)	0.027 (4)	0.017 (3)	0.001 (3)	0.003 (3)	−0.002 (3)
C32	0.027 (4)	0.031 (4)	0.021 (3)	−0.001 (3)	0.011 (3)	0.004 (3)
C33	0.042 (5)	0.042 (5)	0.028 (4)	0.020 (4)	0.016 (4)	0.020 (4)
C34	0.032 (4)	0.054 (6)	0.041 (5)	0.023 (4)	0.016 (4)	0.029 (4)
C35	0.022 (4)	0.043 (5)	0.027 (4)	0.008 (3)	0.011 (3)	0.010 (3)
C1S	0.246 (8)	0.210 (8)	0.128 (5)	0.019 (7)	0.033 (5)	−0.037 (5)
Cl1	0.246 (8)	0.210 (8)	0.128 (5)	0.019 (7)	0.033 (5)	−0.037 (5)
Cl2	0.246 (8)	0.210 (8)	0.128 (5)	0.019 (7)	0.033 (5)	−0.037 (5)
C1SB	0.246 (8)	0.210 (8)	0.128 (5)	0.019 (7)	0.033 (5)	−0.037 (5)
Cl1B	0.246 (8)	0.210 (8)	0.128 (5)	0.019 (7)	0.033 (5)	−0.037 (5)
Cl2B	0.246 (8)	0.210 (8)	0.128 (5)	0.019 (7)	0.033 (5)	−0.037 (5)

Geometric parameters (Å, º) top

Re1—C1	1.911 (8)	C15—C16	1.385 (10)
Re1—C2	1.928 (8)	C15—H15	0.9500
Re1—C3	1.945 (7)	C16—H16	0.9500
Re1—P1	2.4535 (17)	C17—C22	1.390 (10)
Re1—Re2	3.2358 (4)	C17—C18	1.393 (10)
Re1—Re3	3.2909 (4)	C18—C19	1.391 (11)
Re1—H1H	1.8430	C18—H18	0.9500
Re1—H2H	1.8410	C19—C20	1.379 (13)
Re2—C4	1.919 (7)	C19—H19	0.9500
Re2—C5	1.920 (8)	C20—C21	1.385 (12)
Re2—C6	1.959 (7)	C20—H20	0.9500
Re2—P2	2.4592 (16)	C21—C22	1.385 (11)
Re2—Re3	3.2901 (4)	C21—H21	0.9500
Re2—H1H	1.8465	C22—H22	0.9500
Re2—H3H	1.8461	C23—H23A	0.9900
Re3—C7	1.927 (8)	C23—H23B	0.9900
Re3—C8	1.947 (7)	C24—C25	1.383 (10)
Re3—C10	1.985 (7)	C24—C29	1.400 (10)
Re3—C9	2.002 (7)	C25—C26	1.381 (11)
Re3—H2H	1.8464	C25—H25	0.9500
Re3—H3H	1.8431	C26—C27	1.382 (13)
P1—C17	1.829 (7)	C26—H26	0.9500
P1—C11	1.831 (7)	C27—C28	1.390 (13)
P1—C23	1.842 (7)	C27—H27	0.9500
P2—C24	1.826 (7)	C28—C29	1.387 (11)
P2—C30	1.827 (7)	C28—H28	0.9500
P2—C23	1.841 (7)	C29—H29	0.9500
O1—C1	1.162 (9)	C30—C35	1.392 (10)
O2—C2	1.153 (9)	C30—C31	1.402 (9)
O3—C3	1.141 (8)	C31—C32	1.384 (10)
O4—C4	1.142 (9)	C31—H31	0.9500
O5—C5	1.153 (9)	C32—C33	1.386 (11)
O6—C6	1.138 (8)	C32—H32	0.9500
O7—C7	1.157 (9)	C33—C34	1.380 (11)
O8—C8	1.142 (8)	C33—H33	0.9500
O9—C9	1.145 (9)	C34—C35	1.378 (11)
O10—C10	1.137 (8)	C34—H34	0.9500
C11—C12	1.384 (11)	C35—H35	0.9500
C11—C16	1.393 (9)	C1S—Cl1	1.801 (13)
C12—C13	1.386 (10)	C1S—Cl2	1.879 (12)
C12—H12	0.9500	C1S—H1S1	0.9900
C13—C14	1.368 (11)	C1S—H1S2	0.9900
C13—H13	0.9500	C1SB—Cl1B	1.790 (16)
C14—C15	1.388 (12)	C1SB—H1S3	0.9900
C14—H14	0.9500	C1SB—H1S4	0.9900

C1—Re1—C2	91.2 (4)	O2—C2—Re1	177.7 (7)
C1—Re1—C3	86.6 (3)	O3—C3—Re1	174.9 (6)
C2—Re1—C3	89.1 (3)	O4—C4—Re2	174.5 (7)
C1—Re1—P1	89.4 (2)	O5—C5—Re2	174.1 (6)
C2—Re1—P1	96.4 (2)	O6—C6—Re2	178.6 (7)
C3—Re1—P1	173.3 (2)	O7—C7—Re3	177.9 (7)
C1—Re1—Re2	111.9 (3)	O8—C8—Re3	178.5 (6)
C2—Re1—Re2	156.8 (2)	O9—C9—Re3	173.1 (6)
C3—Re1—Re2	89.8 (2)	O10—C10—Re3	175.3 (6)
P1—Re1—Re2	86.64 (4)	C12—C11—C16	118.8 (7)
C1—Re1—Re3	168.3 (2)	C12—C11—P1	116.5 (5)
C2—Re1—Re3	96.3 (2)	C16—C11—P1	124.4 (6)
C3—Re1—Re3	84.6 (2)	C11—C12—C13	120.7 (7)
P1—Re1—Re3	98.61 (4)	C11—C12—H12	119.6
Re2—Re1—Re3	60.536 (8)	C13—C12—H12	119.6
C1—Re1—H1H	83.7	C14—C13—C12	120.5 (8)
C2—Re1—H1H	174.1	C14—C13—H13	119.8
C3—Re1—H1H	93.5	C12—C13—H13	119.8
P1—Re1—H1H	80.7	C13—C14—C15	119.4 (7)
Re2—Re1—H1H	28.7	C13—C14—H14	120.3
Re3—Re1—H1H	89.3	C15—C14—H14	120.3
C1—Re1—H2H	164.8	C16—C15—C14	120.6 (7)
C2—Re1—H2H	80.3	C16—C15—H15	119.7
C3—Re1—H2H	105.7	C14—C15—H15	119.7
P1—Re1—H2H	79.1	C15—C16—C11	119.9 (7)
Re2—Re1—H2H	77.7	C15—C16—H16	120.0
Re3—Re1—H2H	26.9	C11—C16—H16	120.0
H1H—Re1—H2H	104.0	C22—C17—C18	118.9 (7)
C4—Re2—C5	85.9 (3)	C22—C17—P1	120.3 (5)
C4—Re2—C6	90.7 (3)	C18—C17—P1	120.5 (6)
C5—Re2—C6	89.9 (3)	C19—C18—C17	119.9 (7)
C4—Re2—P2	90.3 (2)	C19—C18—H18	120.0
C5—Re2—P2	94.3 (2)	C17—C18—H18	120.0
C6—Re2—P2	175.7 (2)	C20—C19—C18	120.3 (8)
C4—Re2—Re1	107.4 (2)	C20—C19—H19	119.8
C5—Re2—Re1	165.9 (2)	C18—C19—H19	119.8
C6—Re2—Re1	85.2 (2)	C19—C20—C21	120.4 (8)
P2—Re2—Re1	90.51 (4)	C19—C20—H20	119.8
C4—Re2—Re3	167.9 (2)	C21—C20—H20	119.8
C5—Re2—Re3	106.1 (2)	C20—C21—C22	119.3 (8)
C6—Re2—Re3	87.73 (19)	C20—C21—H21	120.4
P2—Re2—Re3	90.43 (4)	C22—C21—H21	120.4
Re1—Re2—Re3	60.561 (8)	C21—C22—C17	121.1 (7)
C4—Re2—H1H	78.7	C21—C22—H22	119.4
C5—Re2—H1H	164.1	C17—C22—H22	119.4
C6—Re2—H1H	86.5	P2—C23—P1	117.8 (3)
P2—Re2—H1H	89.6	P2—C23—H23A	107.9
Re1—Re2—H1H	28.7	P1—C23—H23A	107.9
Re3—Re2—H1H	89.2	P2—C23—H23B	107.9
C4—Re2—H3H	164.6	P1—C23—H23B	107.9
C5—Re2—H3H	81.1	H23A—C23—H23B	107.2
C6—Re2—H3H	97.4	C25—C24—C29	118.0 (7)
P2—Re2—H3H	82.6	C25—C24—P2	125.8 (6)
Re1—Re2—H3H	86.4	C29—C24—P2	116.2 (5)
Re3—Re2—H3H	26.9	C26—C25—C24	120.8 (8)
H1H—Re2—H3H	114.7	C26—C25—H25	119.6
C7—Re3—C8	91.6 (3)	C24—C25—H25	119.6
C7—Re3—C10	88.2 (3)	C25—C26—C27	121.1 (8)
C8—Re3—C10	88.0 (3)	C25—C26—H26	119.5
C7—Re3—C9	87.2 (3)	C27—C26—H26	119.5
C8—Re3—C9	88.4 (3)	C26—C27—C28	119.1 (7)
C10—Re3—C9	174.1 (3)	C26—C27—H27	120.5
C7—Re3—Re2	110.5 (2)	C28—C27—H27	120.5
C8—Re3—Re2	156.6 (2)	C29—C28—C27	119.7 (8)
C10—Re3—Re2	99.9 (2)	C29—C28—H28	120.2
C9—Re3—Re2	85.2 (2)	C27—C28—H28	120.2
C7—Re3—Re1	168.3 (2)	C28—C29—C24	121.3 (8)
C8—Re3—Re1	98.3 (2)	C28—C29—H29	119.3
C10—Re3—Re1	98.4 (2)	C24—C29—H29	119.3
C9—Re3—Re1	86.7 (2)	C35—C30—C31	118.6 (6)
Re2—Re3—Re1	58.903 (8)	C35—C30—P2	121.7 (5)
C7—Re3—H2H	162.8	C31—C30—P2	119.7 (5)
C8—Re3—H2H	85.0	C32—C31—C30	120.4 (6)
C10—Re3—H2H	74.9	C32—C31—H31	119.8
C9—Re3—H2H	109.5	C30—C31—H31	119.8
Re2—Re3—H2H	76.1	C31—C32—C33	120.0 (7)
Re1—Re3—H2H	26.8	C31—C32—H32	120.0
C7—Re3—H3H	85.5	C33—C32—H32	120.0
C8—Re3—H3H	176.3	C34—C33—C32	120.0 (7)
C10—Re3—H3H	89.6	C34—C33—H33	120.0
C9—Re3—H3H	93.8	C32—C33—H33	120.0
Re2—Re3—H3H	26.9	C35—C34—C33	120.3 (7)
Re1—Re3—H3H	84.8	C35—C34—H34	119.9
H2H—Re3—H3H	97.2	C33—C34—H34	119.9
C17—P1—C11	104.1 (3)	C34—C35—C30	120.7 (7)
C17—P1—C23	101.3 (3)	C34—C35—H35	119.6
C11—P1—C23	103.3 (3)	C30—C35—H35	119.6
C17—P1—Re1	114.7 (2)	Cl1—C1S—Cl2	106.6 (10)
C11—P1—Re1	115.3 (2)	Cl1—C1S—H1S1	110.4
C23—P1—Re1	116.2 (2)	Cl2—C1S—H1S1	110.4
C24—P2—C30	100.7 (3)	Cl1—C1S—H1S2	110.4
C24—P2—C23	105.7 (3)	Cl2—C1S—H1S2	110.4
C30—P2—C23	100.4 (3)	H1S1—C1S—H1S2	108.6
C24—P2—Re2	114.0 (2)	Cl1B—C1SB—H1S3	111.8
C30—P2—Re2	118.0 (2)	Cl1B—C1SB—H1S4	111.8
C23—P2—Re2	116.0 (2)	H1S3—C1SB—H1S4	109.6
O1—C1—Re1	178.6 (9)

Experimental details

Crystal data
Chemical formula	[Re₃H₃(C₂₅H₂₂P₂)(CO)₁₀]·CH₂Cl₂
M_r	1311.02
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	100
a, b, c (Å)	16.7907 (6), 14.5316 (5), 17.1593 (6)
β (°)	106.445 (1)
V (Å³)	4015.5 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	9.29
Crystal size (mm)	0.16 × 0.15 × 0.08

Data collection
Diffractometer	Bruker Kappa APEXII CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2009)
T_min, T_max	0.320, 0.527
No. of measured, independent and observed [I > 2σ(I)] reflections	35918, 8540, 7349
R_int	0.031
(sin θ/λ)_max (Å⁻¹)	0.639

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.081, 1.06
No. of reflections	8540
No. of parameters	472
No. of restraints	42
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0308P)² + 45.3016P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	3.82, −2.54

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), publCIF (Westrip, 2010).

Acknowledgements

The authors gratefully acknowledge the financial support of the Swedish Research Council (VR). AFA thanks the EU Erasmus Mundus program, FFEEBB1 office, for a scholarship. AKS thanks the Carl Trygger Foundation for a postdoctoral fellowship.

References

Adams, J., Bruce, I., Skelton, W. & White, H. (1993). J. Organomet. Chem. 447, 91–101. CSD CrossRef CAS Web of Science Google Scholar
Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
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Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar

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