Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101009696/sk1486sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101009696/sk1486Isup2.hkl |
CCDC reference: 173353
A solution of MnRe(µ-H)(µ-PCy2)(CO)8 (0.189 mmol) in 8 ml THF was reacted at 183 K with one equivalent n-BuLi in hexane. After stirring for 15 min the solution was allowed to reach room temperature and one equivalent ClAgPPh3/PPh3 was added. After removal of the solvent the products were separated by thin-layer chromatography (eluant CH2Cl2/n-hexane 1:1). The title compound was recrystallized from CH2Cl2/n-hexane.
Hydrogen atoms were included in the refinement with the riding model approximation with isotropic displacement parameters U(H) = 1.2Ueq(C). Substantial anisotropic displacement parameters of cyclohexyl carbon atoms C11—C16 indicate some degreee of (orientational) disorder which was impossible to resolve. Therefore, the geometric parameters for this cyclohexyl group are less reliable. Additionally, it was not possible to resolve diffuse electron density residuals (enclosed solvent molecules). Treatment with the SQUEEZE facility from PLATON (Spek, 1990), with a localized void of about 215 Å3 at (0, 1/2, 0) and 24 recovered electrons, resulted in smooth refinement. Since a few low order reflections are missing from the data set, the electron count will be underestimated. Thus the values given for D(calc), F000 and Mol. Wght are only valid for the ordered part of the structure.
Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS (Bruker, 1996); data reduction: SHELXTL (Bruker, 1998); 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.
Fig. 1. Molecular structure with hydrogen atoms omitted. Displacement ellipsoids are drawn at the 50% probability level. |
[ReMnAg(C12H22P)(C18H15P)2(CO)7] | Z = 2 |
Mr = 1266.89 | F(000) = 1260 |
Triclinic, P1 | Dx = 1.531 Mg m−3 |
a = 11.583 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.842 (2) Å | Cell parameters from 31 reflections |
c = 20.728 (3) Å | θ = 7.4–17.5° |
α = 96.70 (1)° | µ = 2.91 mm−1 |
β = 98.76 (1)° | T = 293 K |
γ = 113.20 (1)° | Prism, orange |
V = 2747.4 (6) Å3 | 0.42 × 0.22 × 0.08 mm |
Bruker P4 diffractometer | 8862 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 27.5°, θmin = 2.0° |
ω scans | h = −1→15 |
Absorption correction: ψ scan (North et al., 1968) | k = −16→15 |
Tmin = 0.508, Tmax = 0.844 | l = −26→26 |
14452 measured reflections | 3 standard reflections every 397 reflections |
12576 independent reflections | intensity decay: <1% |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.038 | H-atom parameters constrained |
wR(F2) = 0.087 | w = 1/[σ2(Fo2) + (0.0436P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.89 | (Δ/σ)max = 0.001 |
12576 reflections | Δρmax = 0.74 e Å−3 |
614 parameters | Δρmin = −0.92 e Å−3 |
949 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00034 (7) |
[ReMnAg(C12H22P)(C18H15P)2(CO)7] | γ = 113.20 (1)° |
Mr = 1266.89 | V = 2747.4 (6) Å3 |
Triclinic, P1 | Z = 2 |
a = 11.583 (1) Å | Mo Kα radiation |
b = 12.842 (2) Å | µ = 2.91 mm−1 |
c = 20.728 (3) Å | T = 293 K |
α = 96.70 (1)° | 0.42 × 0.22 × 0.08 mm |
β = 98.76 (1)° |
Bruker P4 diffractometer | 8862 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.022 |
Tmin = 0.508, Tmax = 0.844 | 3 standard reflections every 397 reflections |
14452 measured reflections | intensity decay: <1% |
12576 independent reflections |
R[F2 > 2σ(F2)] = 0.038 | 949 restraints |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 0.89 | Δρmax = 0.74 e Å−3 |
12576 reflections | Δρmin = −0.92 e Å−3 |
614 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Re1 | 0.811522 (17) | 0.840472 (15) | 0.283679 (9) | 0.03726 (6) | |
Ag1 | 0.66809 (3) | 0.59741 (3) | 0.240465 (17) | 0.04515 (9) | |
Mn1 | 0.74397 (7) | 0.70008 (6) | 0.13642 (3) | 0.04315 (17) | |
P1 | 0.90972 (11) | 0.87641 (10) | 0.18973 (6) | 0.0396 (3) | |
P2 | 0.67777 (12) | 0.78113 (10) | 0.36323 (6) | 0.0429 (3) | |
P3 | 0.59006 (12) | 0.39360 (10) | 0.25281 (6) | 0.0450 (3) | |
O1 | 0.9897 (3) | 1.0594 (3) | 0.38495 (18) | 0.0694 (10) | |
C1 | 0.9217 (4) | 0.9765 (4) | 0.3462 (2) | 0.0458 (10) | |
O2 | 1.0004 (3) | 0.7312 (3) | 0.32825 (17) | 0.0591 (9) | |
C2 | 0.9272 (4) | 0.7669 (4) | 0.3115 (2) | 0.0439 (10) | |
O3 | 0.6456 (4) | 0.9674 (3) | 0.2350 (2) | 0.0751 (11) | |
C3 | 0.7035 (4) | 0.9170 (4) | 0.2514 (2) | 0.0489 (11) | |
O4 | 0.8088 (5) | 0.7159 (4) | 0.0055 (2) | 0.0941 (14) | |
C4 | 0.7847 (5) | 0.7105 (4) | 0.0572 (3) | 0.0616 (13) | |
O5 | 0.5562 (4) | 0.8015 (4) | 0.1077 (2) | 0.0940 (14) | |
C5 | 0.6314 (5) | 0.7657 (5) | 0.1211 (2) | 0.0584 (12) | |
O6 | 0.9103 (4) | 0.5787 (3) | 0.1726 (2) | 0.0776 (11) | |
C6 | 0.8473 (5) | 0.6271 (4) | 0.1602 (3) | 0.0576 (12) | |
O7 | 0.5176 (5) | 0.4791 (4) | 0.0779 (2) | 0.1052 (17) | |
C7 | 0.6048 (6) | 0.5623 (5) | 0.1046 (3) | 0.0708 (15) | |
C11 | 0.9160 (6) | 1.0062 (4) | 0.1557 (2) | 0.0628 (14) | |
H11 | 0.8289 | 0.9987 | 0.1571 | 0.075* | |
C12 | 0.9918 (6) | 1.1195 (4) | 0.2028 (3) | 0.0651 (15) | |
H12A | 1.0819 | 1.1336 | 0.2120 | 0.078* | |
H12B | 0.9634 | 1.1149 | 0.2445 | 0.078* | |
C13 | 0.9785 (9) | 1.2206 (5) | 0.1761 (3) | 0.120 (3) | |
H13A | 0.9010 | 1.2244 | 0.1862 | 0.145* | |
H13B | 1.0505 | 1.2908 | 0.2009 | 0.145* | |
C14 | 0.9730 (9) | 1.2217 (6) | 0.1091 (3) | 0.130 (3) | |
H14A | 1.0600 | 1.2489 | 0.1018 | 0.156* | |
H14B | 0.9398 | 1.2772 | 0.0974 | 0.156* | |
C15 | 0.8938 (8) | 1.1101 (5) | 0.0634 (3) | 0.096 (2) | |
H15A | 0.9157 | 1.1145 | 0.0201 | 0.115* | |
H15B | 0.8038 | 1.0958 | 0.0579 | 0.115* | |
C16 | 0.9124 (10) | 1.0096 (6) | 0.0880 (3) | 0.131 (3) | |
H16A | 0.8432 | 0.9385 | 0.0622 | 0.157* | |
H16B | 0.9922 | 1.0106 | 0.0785 | 0.157* | |
C21 | 1.0728 (4) | 0.8798 (4) | 0.2004 (2) | 0.0494 (11) | |
H21 | 1.0620 | 0.8065 | 0.2141 | 0.059* | |
C22 | 1.1764 (5) | 0.9717 (5) | 0.2575 (3) | 0.0704 (15) | |
H22A | 1.1995 | 1.0476 | 0.2464 | 0.084* | |
H22B | 1.1432 | 0.9713 | 0.2978 | 0.084* | |
C23 | 1.2937 (5) | 0.9463 (5) | 0.2691 (4) | 0.0901 (19) | |
H23A | 1.2719 | 0.8743 | 0.2850 | 0.108* | |
H23B | 1.3605 | 1.0071 | 0.3034 | 0.108* | |
C24 | 1.3456 (6) | 0.9374 (7) | 0.2060 (5) | 0.113 (3) | |
H24A | 1.3784 | 1.0125 | 0.1935 | 0.136* | |
H24B | 1.4164 | 0.9152 | 0.2150 | 0.136* | |
C25 | 1.2460 (7) | 0.8529 (7) | 0.1504 (4) | 0.103 (2) | |
H25A | 1.2233 | 0.7760 | 0.1600 | 0.124* | |
H25B | 1.2804 | 0.8557 | 0.1105 | 0.124* | |
C26 | 1.1247 (5) | 0.8750 (6) | 0.1376 (3) | 0.0780 (17) | |
H26A | 1.1447 | 0.9475 | 0.1224 | 0.094* | |
H26B | 1.0595 | 0.8138 | 0.1028 | 0.094* | |
C31 | 0.6900 (5) | 0.9056 (4) | 0.4233 (2) | 0.0522 (11) | |
C32 | 0.7660 (5) | 0.9399 (5) | 0.4867 (3) | 0.0671 (14) | |
H32 | 0.8112 | 0.8979 | 0.5007 | 0.081* | |
C33 | 0.7764 (7) | 1.0360 (6) | 0.5300 (3) | 0.092 (2) | |
H33 | 0.8262 | 1.0567 | 0.5730 | 0.110* | |
C34 | 0.7127 (8) | 1.0998 (6) | 0.5087 (4) | 0.107 (2) | |
H34 | 0.7210 | 1.1655 | 0.5369 | 0.128* | |
C35 | 0.6354 (8) | 1.0666 (6) | 0.4449 (4) | 0.105 (2) | |
H35 | 0.5902 | 1.1087 | 0.4308 | 0.126* | |
C36 | 0.6261 (7) | 0.9707 (5) | 0.4026 (3) | 0.0817 (18) | |
H36 | 0.5762 | 0.9498 | 0.3596 | 0.098* | |
C41 | 0.5009 (4) | 0.7103 (4) | 0.3354 (2) | 0.0489 (11) | |
C42 | 0.4427 (5) | 0.6770 (4) | 0.2689 (3) | 0.0553 (12) | |
H42 | 0.4931 | 0.6875 | 0.2372 | 0.066* | |
C43 | 0.3088 (5) | 0.6277 (5) | 0.2482 (3) | 0.0699 (15) | |
H43 | 0.2704 | 0.6051 | 0.2031 | 0.084* | |
C44 | 0.2350 (5) | 0.6129 (5) | 0.2944 (4) | 0.0787 (17) | |
H44 | 0.1458 | 0.5799 | 0.2808 | 0.094* | |
C45 | 0.2909 (6) | 0.6462 (5) | 0.3606 (4) | 0.0802 (17) | |
H45 | 0.2393 | 0.6358 | 0.3917 | 0.096* | |
C46 | 0.4228 (5) | 0.6950 (5) | 0.3820 (3) | 0.0673 (14) | |
H46 | 0.4599 | 0.7178 | 0.4273 | 0.081* | |
C51 | 0.7194 (5) | 0.6917 (4) | 0.4173 (2) | 0.0477 (11) | |
C52 | 0.6295 (6) | 0.5878 (4) | 0.4277 (2) | 0.0593 (13) | |
H52 | 0.5426 | 0.5621 | 0.4085 | 0.071* | |
C53 | 0.6712 (7) | 0.5228 (5) | 0.4670 (3) | 0.0749 (16) | |
H53 | 0.6117 | 0.4537 | 0.4741 | 0.090* | |
C54 | 0.7980 (7) | 0.5598 (6) | 0.4949 (3) | 0.0835 (18) | |
H54 | 0.8246 | 0.5154 | 0.5206 | 0.100* | |
C55 | 0.8869 (6) | 0.6620 (5) | 0.4855 (3) | 0.0713 (15) | |
H55 | 0.9733 | 0.6869 | 0.5053 | 0.086* | |
C56 | 0.8490 (5) | 0.7281 (5) | 0.4469 (2) | 0.0578 (12) | |
H56 | 0.9099 | 0.7971 | 0.4405 | 0.069* | |
C61 | 0.7215 (4) | 0.3638 (4) | 0.2930 (2) | 0.0458 (10) | |
C62 | 0.8288 (5) | 0.4536 (4) | 0.3321 (3) | 0.0619 (13) | |
H62 | 0.8323 | 0.5278 | 0.3374 | 0.074* | |
C63 | 0.9312 (5) | 0.4366 (6) | 0.3636 (3) | 0.0774 (17) | |
H63 | 1.0036 | 0.4990 | 0.3894 | 0.093* | |
C64 | 0.9267 (6) | 0.3274 (6) | 0.3571 (3) | 0.0740 (16) | |
H64 | 0.9962 | 0.3156 | 0.3780 | 0.089* | |
C65 | 0.8192 (6) | 0.2361 (5) | 0.3197 (3) | 0.0735 (16) | |
H65 | 0.8151 | 0.1618 | 0.3164 | 0.088* | |
C66 | 0.7168 (5) | 0.2527 (4) | 0.2869 (3) | 0.0647 (14) | |
H66 | 0.6449 | 0.1902 | 0.2609 | 0.078* | |
C71 | 0.5289 (5) | 0.2922 (4) | 0.1738 (2) | 0.0492 (11) | |
C72 | 0.6139 (6) | 0.2828 (5) | 0.1365 (3) | 0.0769 (17) | |
H72 | 0.7017 | 0.3257 | 0.1532 | 0.092* | |
C73 | 0.5717 (8) | 0.2108 (6) | 0.0747 (3) | 0.098 (2) | |
H73 | 0.6305 | 0.2051 | 0.0501 | 0.118* | |
C74 | 0.4420 (8) | 0.1479 (6) | 0.0500 (3) | 0.096 (2) | |
H74 | 0.4126 | 0.0981 | 0.0089 | 0.116* | |
C75 | 0.3569 (7) | 0.1581 (6) | 0.0854 (3) | 0.090 (2) | |
H75 | 0.2691 | 0.1165 | 0.0681 | 0.108* | |
C76 | 0.3996 (6) | 0.2300 (5) | 0.1472 (3) | 0.0692 (15) | |
H76 | 0.3401 | 0.2363 | 0.1710 | 0.083* | |
C81 | 0.4651 (5) | 0.3408 (4) | 0.2999 (2) | 0.0502 (11) | |
C82 | 0.4682 (5) | 0.2709 (4) | 0.3452 (3) | 0.0635 (14) | |
H82 | 0.5340 | 0.2463 | 0.3513 | 0.076* | |
C83 | 0.3733 (6) | 0.2372 (5) | 0.3817 (3) | 0.0835 (18) | |
H83 | 0.3762 | 0.1901 | 0.4122 | 0.100* | |
C84 | 0.2766 (6) | 0.2717 (5) | 0.3738 (3) | 0.0850 (18) | |
H84 | 0.2133 | 0.2483 | 0.3984 | 0.102* | |
C85 | 0.2726 (6) | 0.3415 (5) | 0.3290 (4) | 0.0825 (18) | |
H85 | 0.2064 | 0.3655 | 0.3232 | 0.099* | |
C86 | 0.3673 (5) | 0.3766 (4) | 0.2921 (3) | 0.0659 (14) | |
H86 | 0.3645 | 0.4244 | 0.2620 | 0.079* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.03497 (10) | 0.03659 (10) | 0.03719 (10) | 0.01198 (7) | 0.00682 (7) | 0.00824 (7) |
Ag1 | 0.0454 (2) | 0.03743 (18) | 0.0479 (2) | 0.01132 (16) | 0.01097 (17) | 0.01150 (15) |
Mn1 | 0.0453 (4) | 0.0408 (4) | 0.0354 (4) | 0.0102 (3) | 0.0069 (3) | 0.0089 (3) |
P1 | 0.0383 (6) | 0.0402 (6) | 0.0396 (6) | 0.0139 (5) | 0.0094 (5) | 0.0130 (5) |
P2 | 0.0437 (7) | 0.0421 (6) | 0.0391 (6) | 0.0135 (5) | 0.0111 (5) | 0.0070 (5) |
P3 | 0.0435 (7) | 0.0371 (6) | 0.0501 (7) | 0.0123 (5) | 0.0087 (6) | 0.0111 (5) |
O1 | 0.060 (2) | 0.058 (2) | 0.063 (2) | 0.0055 (19) | 0.0041 (19) | −0.0081 (18) |
C1 | 0.044 (3) | 0.045 (2) | 0.047 (3) | 0.015 (2) | 0.013 (2) | 0.011 (2) |
O2 | 0.056 (2) | 0.065 (2) | 0.064 (2) | 0.0316 (19) | 0.0095 (18) | 0.0229 (18) |
C2 | 0.043 (2) | 0.044 (2) | 0.044 (3) | 0.013 (2) | 0.012 (2) | 0.018 (2) |
O3 | 0.068 (3) | 0.082 (3) | 0.093 (3) | 0.050 (2) | 0.013 (2) | 0.024 (2) |
C3 | 0.042 (3) | 0.052 (3) | 0.054 (3) | 0.019 (2) | 0.016 (2) | 0.014 (2) |
O4 | 0.140 (4) | 0.105 (3) | 0.057 (2) | 0.061 (3) | 0.045 (3) | 0.024 (2) |
C4 | 0.074 (4) | 0.058 (3) | 0.048 (3) | 0.023 (3) | 0.017 (3) | 0.008 (2) |
O5 | 0.083 (3) | 0.129 (4) | 0.080 (3) | 0.065 (3) | −0.007 (2) | 0.013 (3) |
C5 | 0.052 (3) | 0.071 (3) | 0.041 (3) | 0.017 (3) | 0.004 (2) | 0.008 (2) |
O6 | 0.082 (3) | 0.071 (3) | 0.093 (3) | 0.044 (2) | 0.024 (2) | 0.014 (2) |
C6 | 0.064 (3) | 0.046 (3) | 0.057 (3) | 0.016 (2) | 0.015 (3) | 0.008 (2) |
O7 | 0.101 (3) | 0.065 (3) | 0.087 (3) | −0.009 (2) | −0.035 (3) | 0.014 (2) |
C7 | 0.071 (4) | 0.060 (3) | 0.059 (3) | 0.010 (3) | −0.004 (3) | 0.015 (3) |
C11 | 0.084 (4) | 0.048 (3) | 0.050 (3) | 0.024 (3) | 0.004 (3) | 0.017 (2) |
C12 | 0.086 (4) | 0.048 (3) | 0.058 (3) | 0.024 (3) | 0.011 (3) | 0.019 (2) |
C13 | 0.218 (9) | 0.050 (3) | 0.087 (4) | 0.053 (5) | 0.017 (6) | 0.023 (3) |
C14 | 0.220 (9) | 0.064 (4) | 0.089 (5) | 0.042 (5) | 0.018 (6) | 0.042 (4) |
C15 | 0.152 (7) | 0.078 (4) | 0.059 (4) | 0.048 (4) | 0.012 (4) | 0.036 (3) |
C16 | 0.248 (10) | 0.072 (4) | 0.058 (4) | 0.058 (6) | 0.004 (5) | 0.026 (3) |
C21 | 0.044 (2) | 0.050 (3) | 0.057 (3) | 0.018 (2) | 0.016 (2) | 0.018 (2) |
C22 | 0.045 (3) | 0.060 (3) | 0.097 (4) | 0.019 (3) | −0.002 (3) | 0.012 (3) |
C23 | 0.050 (3) | 0.073 (4) | 0.130 (5) | 0.023 (3) | −0.016 (3) | 0.011 (4) |
C24 | 0.053 (4) | 0.121 (6) | 0.186 (7) | 0.047 (4) | 0.034 (4) | 0.062 (5) |
C25 | 0.081 (4) | 0.143 (7) | 0.121 (6) | 0.067 (5) | 0.053 (4) | 0.045 (5) |
C26 | 0.058 (3) | 0.113 (5) | 0.079 (4) | 0.040 (3) | 0.039 (3) | 0.031 (3) |
C31 | 0.056 (3) | 0.045 (3) | 0.049 (3) | 0.013 (2) | 0.020 (2) | 0.004 (2) |
C32 | 0.075 (4) | 0.061 (3) | 0.057 (3) | 0.023 (3) | 0.013 (3) | −0.002 (3) |
C33 | 0.112 (6) | 0.080 (4) | 0.065 (4) | 0.027 (4) | 0.021 (4) | −0.009 (3) |
C34 | 0.158 (7) | 0.070 (4) | 0.091 (5) | 0.043 (4) | 0.051 (5) | −0.007 (4) |
C35 | 0.150 (7) | 0.094 (5) | 0.096 (5) | 0.079 (5) | 0.035 (5) | 0.004 (4) |
C36 | 0.116 (5) | 0.079 (4) | 0.066 (4) | 0.059 (4) | 0.020 (4) | 0.007 (3) |
C41 | 0.043 (2) | 0.044 (3) | 0.058 (3) | 0.015 (2) | 0.015 (2) | 0.010 (2) |
C42 | 0.050 (3) | 0.055 (3) | 0.061 (3) | 0.022 (2) | 0.012 (2) | 0.014 (2) |
C43 | 0.051 (3) | 0.071 (4) | 0.085 (4) | 0.027 (3) | −0.002 (3) | 0.021 (3) |
C44 | 0.043 (3) | 0.065 (4) | 0.126 (5) | 0.017 (3) | 0.022 (3) | 0.022 (4) |
C45 | 0.056 (3) | 0.075 (4) | 0.113 (5) | 0.024 (3) | 0.041 (3) | 0.013 (4) |
C46 | 0.060 (3) | 0.070 (4) | 0.070 (3) | 0.021 (3) | 0.027 (3) | 0.014 (3) |
C51 | 0.058 (3) | 0.054 (3) | 0.035 (2) | 0.025 (2) | 0.013 (2) | 0.010 (2) |
C52 | 0.074 (3) | 0.050 (3) | 0.044 (3) | 0.018 (3) | 0.008 (3) | 0.007 (2) |
C53 | 0.103 (4) | 0.053 (3) | 0.058 (4) | 0.022 (3) | 0.015 (3) | 0.017 (3) |
C54 | 0.118 (5) | 0.083 (4) | 0.055 (4) | 0.050 (4) | 0.006 (4) | 0.026 (3) |
C55 | 0.075 (4) | 0.098 (4) | 0.044 (3) | 0.041 (3) | 0.006 (3) | 0.019 (3) |
C56 | 0.062 (3) | 0.072 (3) | 0.038 (3) | 0.026 (3) | 0.012 (2) | 0.014 (2) |
C61 | 0.046 (2) | 0.045 (2) | 0.044 (3) | 0.014 (2) | 0.010 (2) | 0.012 (2) |
C62 | 0.058 (3) | 0.053 (3) | 0.064 (3) | 0.015 (2) | 0.005 (3) | 0.014 (2) |
C63 | 0.050 (3) | 0.084 (4) | 0.074 (4) | 0.011 (3) | −0.004 (3) | 0.010 (3) |
C64 | 0.060 (3) | 0.107 (4) | 0.063 (4) | 0.048 (3) | 0.004 (3) | 0.015 (3) |
C65 | 0.081 (4) | 0.076 (4) | 0.075 (4) | 0.051 (3) | 0.003 (3) | 0.007 (3) |
C66 | 0.060 (3) | 0.053 (3) | 0.075 (4) | 0.025 (3) | 0.001 (3) | 0.006 (3) |
C71 | 0.054 (3) | 0.041 (2) | 0.046 (3) | 0.014 (2) | 0.007 (2) | 0.010 (2) |
C72 | 0.074 (4) | 0.097 (4) | 0.054 (3) | 0.038 (3) | 0.005 (3) | −0.004 (3) |
C73 | 0.114 (5) | 0.115 (6) | 0.061 (4) | 0.052 (5) | 0.019 (4) | −0.010 (4) |
C74 | 0.127 (6) | 0.081 (4) | 0.052 (4) | 0.024 (4) | 0.001 (4) | 0.002 (3) |
C75 | 0.090 (4) | 0.084 (4) | 0.053 (4) | 0.001 (4) | −0.007 (3) | 0.011 (3) |
C76 | 0.069 (3) | 0.063 (3) | 0.051 (3) | 0.005 (3) | 0.008 (3) | 0.012 (2) |
C81 | 0.049 (3) | 0.036 (2) | 0.056 (3) | 0.010 (2) | 0.010 (2) | 0.005 (2) |
C82 | 0.058 (3) | 0.061 (3) | 0.071 (4) | 0.018 (3) | 0.025 (3) | 0.022 (3) |
C83 | 0.087 (4) | 0.077 (4) | 0.082 (4) | 0.019 (3) | 0.036 (4) | 0.031 (3) |
C84 | 0.076 (4) | 0.067 (4) | 0.092 (5) | 0.006 (3) | 0.040 (4) | −0.003 (3) |
C85 | 0.066 (4) | 0.062 (4) | 0.119 (5) | 0.023 (3) | 0.035 (4) | 0.006 (3) |
C86 | 0.051 (3) | 0.053 (3) | 0.088 (4) | 0.015 (3) | 0.017 (3) | 0.012 (3) |
Re1—C1 | 1.890 (5) | C32—C33 | 1.391 (8) |
Re1—C3 | 1.961 (5) | C32—H32 | 0.9300 |
Re1—C2 | 1.978 (5) | C33—C34 | 1.369 (9) |
Re1—P1 | 2.4020 (12) | C33—H33 | 0.9300 |
Re1—P2 | 2.4168 (12) | C34—C35 | 1.393 (10) |
Re1—Ag1 | 2.8485 (6) | C34—H34 | 0.9300 |
Re1—Mn1 | 3.1712 (8) | C35—C36 | 1.383 (8) |
Ag1—P3 | 2.4688 (12) | C35—H35 | 0.9300 |
Ag1—Mn1 | 2.7367 (8) | C36—H36 | 0.9300 |
Mn1—C4 | 1.781 (5) | C41—C42 | 1.375 (7) |
Mn1—C5 | 1.820 (6) | C41—C46 | 1.401 (7) |
Mn1—C7 | 1.822 (6) | C42—C43 | 1.396 (7) |
Mn1—C6 | 1.835 (6) | C42—H42 | 0.9300 |
Mn1—P1 | 2.3193 (14) | C43—C44 | 1.360 (8) |
P1—C21 | 1.851 (5) | C43—H43 | 0.9300 |
P1—C11 | 1.864 (5) | C44—C45 | 1.364 (8) |
P2—C51 | 1.838 (5) | C44—H44 | 0.9300 |
P2—C41 | 1.845 (5) | C45—C46 | 1.378 (7) |
P2—C31 | 1.852 (5) | C45—H45 | 0.9300 |
P3—C71 | 1.817 (5) | C46—H46 | 0.9300 |
P3—C61 | 1.817 (5) | C51—C56 | 1.395 (7) |
P3—C81 | 1.821 (5) | C51—C52 | 1.397 (6) |
O1—C1 | 1.160 (5) | C52—C53 | 1.397 (7) |
O2—C2 | 1.142 (5) | C52—H52 | 0.9300 |
O3—C3 | 1.144 (5) | C53—C54 | 1.358 (8) |
O4—C4 | 1.152 (6) | C53—H53 | 0.9300 |
O5—C5 | 1.148 (6) | C54—C55 | 1.370 (8) |
O6—C6 | 1.150 (6) | C54—H54 | 0.9300 |
O7—C7 | 1.144 (6) | C55—C56 | 1.378 (7) |
C11—C16 | 1.405 (7) | C55—H55 | 0.9300 |
C11—C12 | 1.497 (7) | C56—H56 | 0.9300 |
C11—H11 | 0.9800 | C61—C62 | 1.371 (6) |
C12—C13 | 1.523 (7) | C61—C66 | 1.397 (6) |
C12—H12A | 0.9700 | C62—C63 | 1.373 (7) |
C12—H12B | 0.9700 | C62—H62 | 0.9300 |
C13—C14 | 1.384 (8) | C63—C64 | 1.372 (8) |
C13—H13A | 0.9700 | C63—H63 | 0.9300 |
C13—H13B | 0.9700 | C64—C65 | 1.367 (8) |
C14—C15 | 1.475 (9) | C64—H64 | 0.9300 |
C14—H14A | 0.9700 | C65—C66 | 1.379 (7) |
C14—H14B | 0.9700 | C65—H65 | 0.9300 |
C15—C16 | 1.519 (8) | C66—H66 | 0.9300 |
C15—H15A | 0.9700 | C71—C72 | 1.373 (7) |
C15—H15B | 0.9700 | C71—C76 | 1.374 (7) |
C16—H16A | 0.9700 | C72—C73 | 1.383 (8) |
C16—H16B | 0.9700 | C72—H72 | 0.9300 |
C21—C26 | 1.521 (7) | C73—C74 | 1.373 (9) |
C21—C22 | 1.536 (7) | C73—H73 | 0.9300 |
C21—H21 | 0.9800 | C74—C75 | 1.352 (9) |
C22—C23 | 1.509 (7) | C74—H74 | 0.9300 |
C22—H22A | 0.9700 | C75—C76 | 1.381 (8) |
C22—H22B | 0.9700 | C75—H75 | 0.9300 |
C23—C24 | 1.531 (9) | C76—H76 | 0.9300 |
C23—H23A | 0.9700 | C81—C86 | 1.376 (7) |
C23—H23B | 0.9700 | C81—C82 | 1.380 (7) |
C24—C25 | 1.468 (10) | C82—C83 | 1.387 (7) |
C24—H24A | 0.9700 | C82—H82 | 0.9300 |
C24—H24B | 0.9700 | C83—C84 | 1.353 (9) |
C25—C26 | 1.530 (8) | C83—H83 | 0.9300 |
C25—H25A | 0.9700 | C84—C85 | 1.372 (9) |
C25—H25B | 0.9700 | C84—H84 | 0.9300 |
C26—H26A | 0.9700 | C85—C86 | 1.391 (8) |
C26—H26B | 0.9700 | C85—H85 | 0.9300 |
C31—C32 | 1.379 (7) | C86—H86 | 0.9300 |
C31—C36 | 1.380 (7) | ||
C1—Re1—C3 | 90.2 (2) | C25—C24—H24A | 109.2 |
C1—Re1—C2 | 89.88 (19) | C23—C24—H24A | 109.2 |
C3—Re1—C2 | 176.10 (18) | C25—C24—H24B | 109.2 |
C1—Re1—P1 | 100.12 (14) | C23—C24—H24B | 109.2 |
C3—Re1—P1 | 88.51 (14) | H24A—C24—H24B | 107.9 |
C2—Re1—P1 | 87.63 (13) | C24—C25—C26 | 112.4 (6) |
C1—Re1—P2 | 89.50 (14) | C24—C25—H25A | 109.1 |
C3—Re1—P2 | 87.33 (14) | C26—C25—H25A | 109.1 |
C2—Re1—P2 | 96.57 (13) | C24—C25—H25B | 109.1 |
P1—Re1—P2 | 169.54 (4) | C26—C25—H25B | 109.1 |
C1—Re1—Ag1 | 154.68 (14) | H25A—C25—H25B | 107.8 |
C3—Re1—Ag1 | 108.42 (14) | C21—C26—C25 | 110.9 (5) |
C2—Re1—Ag1 | 72.69 (13) | C21—C26—H26A | 109.5 |
P1—Re1—Ag1 | 97.42 (3) | C25—C26—H26A | 109.5 |
P2—Re1—Ag1 | 74.86 (3) | C21—C26—H26B | 109.5 |
C1—Re1—Mn1 | 146.81 (14) | C25—C26—H26B | 109.5 |
C3—Re1—Mn1 | 88.07 (14) | H26A—C26—H26B | 108.0 |
C2—Re1—Mn1 | 89.72 (13) | C32—C31—C36 | 118.6 (5) |
P1—Re1—Mn1 | 46.71 (3) | C32—C31—P2 | 122.7 (4) |
P2—Re1—Mn1 | 123.50 (3) | C36—C31—P2 | 118.6 (4) |
Ag1—Re1—Mn1 | 53.757 (17) | C31—C32—C33 | 121.5 (6) |
P3—Ag1—Mn1 | 131.20 (4) | C31—C32—H32 | 119.3 |
P3—Ag1—Re1 | 155.10 (3) | C33—C32—H32 | 119.3 |
Mn1—Ag1—Re1 | 69.16 (2) | C34—C33—C32 | 119.3 (7) |
C4—Mn1—C5 | 93.6 (2) | C34—C33—H33 | 120.4 |
C4—Mn1—C7 | 93.2 (2) | C32—C33—H33 | 120.4 |
C5—Mn1—C7 | 85.9 (2) | C33—C34—C35 | 120.1 (6) |
C4—Mn1—C6 | 93.2 (2) | C33—C34—H34 | 120.0 |
C5—Mn1—C6 | 172.8 (2) | C35—C34—H34 | 120.0 |
C7—Mn1—C6 | 91.5 (2) | C36—C35—C34 | 119.7 (7) |
C4—Mn1—P1 | 94.31 (17) | C36—C35—H35 | 120.1 |
C5—Mn1—P1 | 91.81 (17) | C34—C35—H35 | 120.1 |
C7—Mn1—P1 | 172.2 (2) | C31—C36—C35 | 120.8 (6) |
C6—Mn1—P1 | 89.93 (16) | C31—C36—H36 | 119.6 |
C4—Mn1—Ag1 | 157.40 (17) | C35—C36—H36 | 119.6 |
C5—Mn1—Ag1 | 100.55 (16) | C42—C41—C46 | 118.4 (5) |
C7—Mn1—Ag1 | 70.56 (17) | C42—C41—P2 | 121.2 (4) |
C6—Mn1—Ag1 | 72.29 (16) | C46—C41—P2 | 120.3 (4) |
P1—Mn1—Ag1 | 102.66 (4) | C41—C42—C43 | 120.9 (5) |
C4—Mn1—Re1 | 142.87 (17) | C41—C42—H42 | 119.6 |
C5—Mn1—Re1 | 83.99 (16) | C43—C42—H42 | 119.6 |
C7—Mn1—Re1 | 123.39 (19) | C44—C43—C42 | 119.6 (6) |
C6—Mn1—Re1 | 91.94 (16) | C44—C43—H43 | 120.2 |
P1—Mn1—Re1 | 48.92 (3) | C42—C43—H43 | 120.2 |
Ag1—Mn1—Re1 | 57.086 (18) | C43—C44—C45 | 120.4 (6) |
C21—P1—C11 | 107.3 (2) | C43—C44—H44 | 119.8 |
C21—P1—Mn1 | 114.87 (16) | C45—C44—H44 | 119.8 |
C11—P1—Mn1 | 117.16 (17) | C44—C45—C46 | 120.9 (6) |
C21—P1—Re1 | 115.21 (16) | C44—C45—H45 | 119.6 |
C11—P1—Re1 | 116.90 (19) | C46—C45—H45 | 119.6 |
Mn1—P1—Re1 | 84.37 (4) | C45—C46—C41 | 119.8 (6) |
C51—P2—C41 | 105.5 (2) | C45—C46—H46 | 120.1 |
C51—P2—C31 | 103.1 (2) | C41—C46—H46 | 120.1 |
C41—P2—C31 | 98.1 (2) | C56—C51—C52 | 118.9 (5) |
C51—P2—Re1 | 115.10 (16) | C56—C51—P2 | 117.5 (4) |
C41—P2—Re1 | 120.26 (16) | C52—C51—P2 | 123.5 (4) |
C31—P2—Re1 | 112.26 (15) | C51—C52—C53 | 119.4 (5) |
C71—P3—C61 | 103.1 (2) | C51—C52—H52 | 120.3 |
C71—P3—C81 | 105.0 (2) | C53—C52—H52 | 120.3 |
C61—P3—C81 | 105.3 (2) | C54—C53—C52 | 120.5 (6) |
C71—P3—Ag1 | 113.35 (15) | C54—C53—H53 | 119.7 |
C61—P3—Ag1 | 110.78 (15) | C52—C53—H53 | 119.7 |
C81—P3—Ag1 | 117.96 (15) | C53—C54—C55 | 120.6 (6) |
O1—C1—Re1 | 179.3 (5) | C53—C54—H54 | 119.7 |
O2—C2—Re1 | 175.6 (4) | C55—C54—H54 | 119.7 |
O3—C3—Re1 | 176.0 (5) | C54—C55—C56 | 120.3 (6) |
O4—C4—Mn1 | 178.8 (6) | C54—C55—H55 | 119.8 |
O5—C5—Mn1 | 175.5 (5) | C56—C55—H55 | 119.8 |
O6—C6—Mn1 | 177.4 (5) | C55—C56—C51 | 120.2 (5) |
O7—C7—Mn1 | 172.6 (5) | C55—C56—H56 | 119.9 |
C16—C11—C12 | 115.6 (5) | C51—C56—H56 | 119.9 |
C16—C11—P1 | 121.7 (4) | C62—C61—C66 | 118.3 (5) |
C12—C11—P1 | 115.3 (3) | C62—C61—P3 | 118.8 (4) |
C16—C11—H11 | 99.1 | C66—C61—P3 | 122.8 (4) |
C12—C11—H11 | 99.1 | C61—C62—C63 | 121.5 (5) |
P1—C11—H11 | 99.1 | C61—C62—H62 | 119.2 |
C11—C12—C13 | 113.2 (5) | C63—C62—H62 | 119.2 |
C11—C12—H12A | 108.9 | C64—C63—C62 | 119.9 (5) |
C13—C12—H12A | 108.9 | C64—C63—H63 | 120.0 |
C11—C12—H12B | 108.9 | C62—C63—H63 | 120.0 |
C13—C12—H12B | 108.9 | C65—C64—C63 | 119.6 (5) |
H12A—C12—H12B | 107.8 | C65—C64—H64 | 120.2 |
C14—C13—C12 | 118.4 (6) | C63—C64—H64 | 120.2 |
C14—C13—H13A | 107.7 | C64—C65—C66 | 120.9 (6) |
C12—C13—H13A | 107.7 | C64—C65—H65 | 119.6 |
C14—C13—H13B | 107.7 | C66—C65—H65 | 119.6 |
C12—C13—H13B | 107.7 | C65—C66—C61 | 119.8 (5) |
H13A—C13—H13B | 107.1 | C65—C66—H66 | 120.1 |
C13—C14—C15 | 115.8 (6) | C61—C66—H66 | 120.1 |
C13—C14—H14A | 108.3 | C72—C71—C76 | 118.0 (5) |
C15—C14—H14A | 108.3 | C72—C71—P3 | 119.2 (4) |
C13—C14—H14B | 108.3 | C76—C71—P3 | 122.6 (4) |
C15—C14—H14B | 108.3 | C71—C72—C73 | 121.4 (6) |
H14A—C14—H14B | 107.4 | C71—C72—H72 | 119.3 |
C14—C15—C16 | 112.8 (6) | C73—C72—H72 | 119.3 |
C14—C15—H15A | 109.0 | C74—C73—C72 | 119.1 (7) |
C16—C15—H15A | 109.0 | C74—C73—H73 | 120.4 |
C14—C15—H15B | 109.0 | C72—C73—H73 | 120.4 |
C16—C15—H15B | 109.0 | C75—C74—C73 | 120.2 (6) |
H15A—C15—H15B | 107.8 | C75—C74—H74 | 119.9 |
C11—C16—C15 | 117.1 (6) | C73—C74—H74 | 119.9 |
C11—C16—H16A | 108.0 | C74—C75—C76 | 120.4 (6) |
C15—C16—H16A | 108.0 | C74—C75—H75 | 119.8 |
C11—C16—H16B | 108.0 | C76—C75—H75 | 119.8 |
C15—C16—H16B | 108.0 | C71—C76—C75 | 120.8 (6) |
H16A—C16—H16B | 107.3 | C71—C76—H76 | 119.6 |
C26—C21—C22 | 110.7 (4) | C75—C76—H76 | 119.6 |
C26—C21—P1 | 116.2 (4) | C86—C81—C82 | 118.9 (5) |
C22—C21—P1 | 116.4 (3) | C86—C81—P3 | 118.5 (4) |
C26—C21—H21 | 103.9 | C82—C81—P3 | 122.5 (4) |
C22—C21—H21 | 103.9 | C81—C82—C83 | 120.0 (6) |
P1—C21—H21 | 103.9 | C81—C82—H82 | 120.0 |
C23—C22—C21 | 109.6 (5) | C83—C82—H82 | 120.0 |
C23—C22—H22A | 109.8 | C84—C83—C82 | 121.1 (6) |
C21—C22—H22A | 109.8 | C84—C83—H83 | 119.4 |
C23—C22—H22B | 109.8 | C82—C83—H83 | 119.4 |
C21—C22—H22B | 109.8 | C83—C84—C85 | 119.4 (6) |
H22A—C22—H22B | 108.2 | C83—C84—H84 | 120.3 |
C22—C23—C24 | 112.4 (6) | C85—C84—H84 | 120.3 |
C22—C23—H23A | 109.1 | C84—C85—C86 | 120.3 (6) |
C24—C23—H23A | 109.1 | C84—C85—H85 | 119.8 |
C22—C23—H23B | 109.1 | C86—C85—H85 | 119.9 |
C24—C23—H23B | 109.1 | C81—C86—C85 | 120.3 (6) |
H23A—C23—H23B | 107.9 | C81—C86—H86 | 119.9 |
C25—C24—C23 | 111.9 (6) | C85—C86—H86 | 119.9 |
Experimental details
Crystal data | |
Chemical formula | [ReMnAg(C12H22P)(C18H15P)2(CO)7] |
Mr | 1266.89 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 11.583 (1), 12.842 (2), 20.728 (3) |
α, β, γ (°) | 96.70 (1), 98.76 (1), 113.20 (1) |
V (Å3) | 2747.4 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.91 |
Crystal size (mm) | 0.42 × 0.22 × 0.08 |
Data collection | |
Diffractometer | Bruker P4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.508, 0.844 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14452, 12576, 8862 |
Rint | 0.022 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.087, 0.89 |
No. of reflections | 12576 |
No. of parameters | 614 |
No. of restraints | 949 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.74, −0.92 |
Computer programs: XSCANS (Bruker, 1996), SHELXTL (Bruker, 1998), SHELXTL.
Re1—P1 | 2.4020 (12) | Ag1—P3 | 2.4688 (12) |
Re1—P2 | 2.4168 (12) | Ag1—Mn1 | 2.7367 (8) |
Re1—Ag1 | 2.8485 (6) | Mn1—P1 | 2.3193 (14) |
Re1—Mn1 | 3.1712 (8) | ||
P1—Re1—P2 | 169.54 (4) | P3—Ag1—Re1 | 155.10 (3) |
P1—Re1—Ag1 | 97.42 (3) | Mn1—Ag1—Re1 | 69.16 (2) |
P2—Re1—Ag1 | 74.86 (3) | P1—Mn1—Ag1 | 102.66 (4) |
P1—Re1—Mn1 | 46.71 (3) | P1—Mn1—Re1 | 48.92 (3) |
P2—Re1—Mn1 | 123.50 (3) | Ag1—Mn1—Re1 | 57.086 (18) |
Ag1—Re1—Mn1 | 53.757 (17) | Mn1—P1—Re1 | 84.37 (4) |
P3—Ag1—Mn1 | 131.20 (4) |
Compounds of the type M2(M'PR3)(µ-PR'2)(CO)8 (M2 = Mn2, Re2, MnRe; R, R' = organic residue) serve as precursor complexes for the synthesis of metallatetrahedrane structures (Haupt et al., 1999; Petters, 1999). In this context the title compound, (I), is the first crystallographically characterized heteronuclear coin metal-manganese-rhenium cluster. \sch
The basic structural element is the AgMnRe triangle with a µ-PCy2 group which bridges the Mn–Re bond to form a AgMnReP ring. Similar ring patterns are known from related compounds, e.g. Re2(CuPPh3)(µ-PCy2)(CO)8 (Flörke & Haupt, 1992) Mn2(AuPMe2Ph)(µ-PPh2)(CO)8 (Iggo et al., 1984) or Re2(AuPPh3)(µ-PPh2)(CO)7(PHPh2) (Haupt et al., 1999). The manganese atom has four terminal carbonyl groups and the phosphorous atom as non-metal ligands. Its distorted octahedral coordination sphere is completed with the silver atom. The same coordination geometry is valid for the Re atom, but one equatorial CO group is substituted by a PPh3 ligand. These ligands at both metal atoms show ecliptic arrangements with C—Mn—Re—C and C—Mn—Re—P torsion angles from 1.2 (2)° to 7.9 (4)° (absolute values). The central AgMnReP ring is not planar but folded along the Mn—Re bond with a PMnRe/ReMnAg dihedral angle of 24.4 (1)°. This corresponds to a position of the silver atom 0.949 (1) Å above the MnReP1 plane and is in contrast to related but nearly planar ring structures M2(M'PR3)(µ-PR'2)(CO)7L where the coin metal deviations are only 0.011 (1) to 0.260 (2) Å from the M2P-planes (M = Re, M' = Ag, L = CO (Flörke & Haupt, 1999); M' = Cu (Flörke & Haupt, 1992); M' = Au, L = ax-PHPh2 (Haupt et al., 1999); M = Mn, M' = Au, L = CO (Iggo et al., 1984; Haupt et al., 1992, 1995)). This strong folding of the AgMnReP ring is obviously due to endeavours to minimize intramolecular steric repulsions between the PPh3 ligand of the silver atom and the one attached to rhenium which is in equatorial position trans to the µ-P bridge. The P2 atom of this PPh3 ligand lies 0.165 (1) Å below the plane in consideration. Comparison with the related monosubstituted but almost planar compound Re2(AuPPh3)(µ-PPh2)(CO)7(PHPh2) with an axially attached PHPh2 ligand shows the Au atom only 0.011 (1) Å above the Re2P plane. The Mn—Re single bond of (I) measures 3.1712 (8) Å, this is nearly the same as 3.164 (1) Å in MnRe(RhPPh3)(µ-PCy2)(CO)8 (Beckers et al., 1995) but clearly longer than 3.0397 (7) Å in MnRe(µ-H)(µ-PCy2)(CO)8 (Flörke et al., 1995) which represent the only other known µ-P bridged Mn—Re complexes. The M—P1 bond lengths of 2.3193 (14) Å (Mn) and 2.4020 (12) Å (Re) reflect the different metal radii, the enclosed Mn—P—Re angle is 84.37 (4)°. The Ag—Mn and Ag—Re single bond lengths are 2.7367 (8) and 2.8485 (6) Å, respectively. This is the first characterized unsupported Ag—Mn bond as the only other kown Ag—Mn structure units are bridged by µ-CO, µ-H or µ3-H ligands and exhibit metal-metal distances from 2.902 to 3.044 Å (Horton et al., 1988; Carreño et al., 1992; Carreño et al., 1994). Few more Ag—Re interactions have been reported of which the related Re2Ag(µ-P)-type structures show Ag—Re bond lengths of 2.7957 (7) and 2.8235 (7) Å in Re2(AgPPh3)(µ-PCy2)(CO)8 (Flörke & Haupt, 1999) or 2.8199 (9) and 2.8476 (6) Å in Re2(AgPPh3)(µ-S(2-naphthyl))(CO)8 (Egold et al., 1999). The distorted Y-shaped coordination at the silver atom with angles Re—Ag—P3 155.10 (3)°, Mn—Ag—P3 131.20 (4)°, and Re—Ag—Mn 69.16 (2)° is a common structural pattern known from various other M2(M'PR3) units, e.g. Re2(M'(CO)2PPh3)(µ-PR2)(CO)8 with M' = Rh, Ir (Haupt et al., 1994) or the above mentioned coin metal complexes M2(M'PR3)(µ-PR'2)(CO)7L.