Synthesis, structure, and reactivity of transition metal/main group metal bridging carboxylate complexes of the formula (.eta.5-C5H5)Re(NO)(PPh3)(CO2MLn) (M = Li, K, Ge, Sn, Pb)

Senn, Dwayne R.; Gladysz, J.A.; Emerson, K.; Larsen, R. D.

doi:10.1021/ic00264a001

Cited by 45 publications

(30 citation statements)

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“…The Sn---O bond lengths in this molecule differ by 0.219 A [2.123 (4) and 2.342(4) A]. The difference is considerably greater than observed (Senn et al, 1987) for the related compound CpRe(NO)(PPha)CO2SnPh3 (0.082 A) but smaller than that observed for monomeric triaryltin organocarboxylates (Holmes, Day, Chandrasekhar, Vollano & Holmes, 1986) (Johnson, 1965) plot of compound showing the atomic numbering system. The thermal ellipsoids are drawn at the 50% probability level.…”

Section: Discussionmentioning

confidence: 70%

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1-Carbonyl-1-η5-cyclopentadienyl-2,2,2-triphenyl-1-triphenylphosphine-μ-carboxylato-1κC:2κO:2κO'-irontin

Gibson¹,

Richardson²,

Ong³

1991

Acta Crystallogr C

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GAYLANI, KILNER, FRENCH, PICK AND WALLWORK 259After preliminary X-ray photography, lattice parameters were refined from 16 reflections with 11 ° < 0 < 14 ° and about 3300 X-ray intensities were measured on a Hilger & Watts computer-controlled, four-circle diffractometer up to 0 = 25 ° using a 0/20 scan technique in the range -11 ___ h ___ 9, -12 ___ k ___ 12, 0 < 1 <_ 12. Of these, 3067 were regarded as significant [I> 3tr(/)]. No corrections were made for absorption, in view of the low absorption coefficient and small crystal size (maximum dimension ca 0.5 mm). The structure was solved by the heavyatom Patterson method, and refined by least-squares calculations (on F), using anisotropic thermal parameters, to a final R value of 0.032, wR = 0.044. H atoms were included in calculated positions with fixed isotropic thermal parameters, and not refined. A weighting scheme of the form of a four-term Chebyshev polynomial was applied in the last few cycles of refinement (235 parameters refined). A/trmax = 0"14. The CRYSTALS system of programs was employed.Discussion. A drawing of the molecular structure showing the atomic numbering scheme is given in Fig. 1. Table 1 gives the atomic coordinates and Ueq values for the non-H atoms and Fig. 2 shows the crystal structure projected along the b axis.*The bond distances and angles found for the present complex (Table 2) centres, and the substituent at the skeletal C atom. The skeletal NCN angle is generally lower (108.0 °) when the latter substituent is methyl, than when it is phenyl (usually 110-112°), except for the case where each N atom substituent is CH(CH3)C6Hs. Also for this acetamidinato complex the Mo atom is positioned, within experimental error, in the skeletal NCN plane whereas for the chiral complexes dihedral angles up to 5.7 ° occur. The planes of the phenyl rings of the present complex are twisted so that two ortho-H atoms lie below the plane containing the metal and skeletal NCN atoms, whereas the methyl C atom lies above this plane, thus minimizing repulsion. The packing of the molecules in the crystal is in layers parallel to (10T), with adjacent molecules within the layers in opposite orientations.We thank the Science and Engineering Research Council for supplying the X-ray diffractometer. Abstract.[FeSn(CsHs)(C6Hs)3(CO)(CO2){P(C6-H5)3}], Mr = 805.27, orthorhombic, Pbca, a =

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Section: Discussionmentioning

confidence: 70%

“…Selected bond lengths (A) and angles (°) are given in Table 2. The structure is isomorphous with the related compound CpRe(NO)(PPha)CO2SnPh3 (Senn, Gladysz, Emerson & Larsen, 1987) (space group Pcab) with some minor differences. The Sn---O bond lengths in this molecule differ by 0.219 A [2.123 (4) and 2.342(4) A].…”

Section: Discussionmentioning

confidence: 99%

1-Carbonyl-1-η5-cyclopentadienyl-2,2,2-triphenyl-1-triphenylphosphine-μ-carboxylato-1κC:2κO:2κO'-irontin

Gibson¹,

Richardson²,

Ong³

1991

Acta Crystallogr C

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“…Each tin atom has pseudotetrahedral geometry (SnCbRe, SnCkCRe or SnC2ClRe) and the rhenium atoms are sandwiched by cyclopentadienyl groups. The Sn-O bond distances are not equal, differing by 8.2 pm in the case shown [109] and much larger at 30.7 pm in the other [110]. Here the bridge is seen to be CO2 molecule bridging in a μ-η -CO2 fashion by both Ο atoms to Sn an the C atom to Re.…”

Section: Figure 2 Structure Of [Chbusn^-v-s2cpcy 3 )([I-cimo(co)2(pcmentioning

confidence: 83%

“…There are six examples with tin and rhenium [107][108][109][110], with a direct Sn-Re bond in four of them [107,108] with distances ranging from 260.9(1) to 279.3(1) pm (ave. 267 pm). Each tin atom has pseudotetrahedral geometry (SnCbRe, SnCkCRe or SnC2ClRe) and the rhenium atoms are sandwiched by cyclopentadienyl groups.…”

Section: Figure 2 Structure Of [Chbusn^-v-s2cpcy 3 )([I-cimo(co)2(pcmentioning

confidence: 99%

Heterometallic Tin Compounds: Classification and Analysis of Crystallographic and Structural Data: Part 1. Dimeric Derivatives

Holloway¹,

Melnı́k²

2001

Main Group Metal Chemistry

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This review covers the crystallographic data for dimeric tin compounds with one other metal atom centre, following the pattern of the previous reviews on tin coordination and organometallic compounds. Over two hundred and forty such derivatives have been characterised, twenty three with a non-transition heterometal atom, one with an actinide metal and the rest with a transition metal atom. The predominant geometries of the tin and the heteroatom are discussed along with the relationships between atom size, bond distances and bond angles. The occurrences of direct metal-metal bonds, and examples of isomerism are illustrated CONTENTS 0. ABBREVIATIONS 1. DIMERIC COMPOUNDS 2.1 Α-Group (Non-Transition) MetalsCrystallographic and structural data for some twenty three tin heterometallic compounds with sub-group A. or non-transition metals, are summarised in Table 1. These are listed in their Periodic Group order, with the typical metals of each group first, and then the Sn-M distance. The first eight derivatives contain tin with lithium [6][7][8][9][10][11][12][13], with the tin in the +2 oxidation state and lithium in its usual +1 oxidation state. The shortest Sn-Li bond 136 Brought to you by | Purdue University Libraries Authenticated Download Date | 6/11/15 11:28 PM Main Group Metal Chemistry Vol. 24, Nr. 3, 2001 distance is found in a yellow derivative [6] at 277.6(4) pm. Here, three Ph(Bu')CN ligands bridge the lithium and tin atoms via their Ν atoms, with Sn-N-Li bridge angles of 81,5( 1A slightly longer Sn-Li distance of 278.4(4) pm is found in a cyclometalated dimer [7] leid together by bridging Ο atoms of three 2,6diphenylphenoxide ligands, with mean Sn-O-Li bridge angles of 84.5(2)°.Two crystallographically independent molecules within the asymmetric units of Ph3SnLi(pmdeta) [8] differ essentially by degree of distortion. While the Sn(II) atom is coordinated by three phenyl groups, the Li(I) atom utilises the tridentate pmdeta moiety. Four coordination is accomplished by each metal via a direct Sn-Li bond of 286.1(7) and 288.2(7) pm in the respective distortion isomers. Another colourless derivative [9] also contains two crystallographically independent molecules. A direct Sn-Li bond of 289(4) and 297(5) pm, respectively, hold together the N3Sn and LiCb moieties.A lithium atom in the next derivative [ 10] ties two amido groups together to generate an N-donor arrangement which forms part of the N3Sn pyramid, one corner of which is the Sn(II) atom. The structure of a red derivative [11] involves a {(Me3Si)3}2Sn unit coordinated to a LiCl(thf)3 moiety via a chlorine bridge. The tricoordinated Sn(II) atom is also at one corner of a pyramid. A tricoordinated tin atom is also found in a metallocyclic arrangement [12] of a four membered (Sn-P-Li-P) ring with average Sn-P-Li angles of 89.5(7)°.The Sn centre in a sandwich style complex [13] is attached to two distorted η-cp ligands and the planar Ν atom of a (Me3Si)2N group, as seen in Figure 1. The tin atom has a distorted pyramidal geometry, and the cp(Y) ligand h...

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“…To the best of our knowledge, in 1987, Gladysz et al reported the first X-ray characterization of a transition metal/tin bridging CO 2 complex by isolating (η-C 5 H 5 )Re(NO)(PPh 3 ) (CO 2 SnPh 3 ) (16) [72]. Compound 16 was obtained in high yield (86%) by reacting (η-C 5 H 5 )Re(NO)(PPh 3 )(CO 2 K) with 1.1 equivalent of Ph 3 SnCl at −78 • C in THF (Scheme 23).…”

Section: X-ray Crystal Structuresmentioning

confidence: 99%

CO2 Derivatives of Molecular Tin Compounds. Part 2: Carbamato, Formato, Phosphinoformato and Metallocarboxylato Complexes

Plasseraud

2021

Inorganics

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Single-crystal X-ray diffraction structures of organotin compounds bearing hemicarbonate and carbonate ligands were recently reviewed by us—“CO2 Derivatives of Molecular Tin Compounds. Part 1: Hemicarbonato and Carbonato Complexes”, Inorganics2020, 8, 31—based on crystallographic data available from the Cambridge Structural Database. Interestingly, this first collection revealed that most of the compounds listed were isolated in the context of studies devoted to the reactivity of tin precursors towards carbon dioxide, at atmospheric pressure or under pressure, thus highlighting the suitable disposition of Sn to fix CO2. In the frame of a second part, the present review carries on to explore CO2 derivatives of molecular tin compounds by describing successively the complexes with carbamato, formato, and phosphinoformato ligands, and obtained from insertion reactions of carbon dioxide into Sn–X bonds (X = N, H, P, respectively). The last chapter is devoted to X-ray structures of transition metal/tin CO2 complexes exhibiting metallocarboxylato ligands. As in Part 1, for each tin compound reported and when described in the original study, the structural descriptions are supplemented by synthetic conditions and spectroscopic data.

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Synthesis, structure, and reactivity of transition metal/main group metal bridging carboxylate complexes of the formula (.eta.5-C5H5)Re(NO)(PPh3)(CO2MLn) (M = Li, K, Ge, Sn, Pb)

Cited by 45 publications

References 4 publications

1-Carbonyl-1-η5-cyclopentadienyl-2,2,2-triphenyl-1-triphenylphosphine-μ-carboxylato-1κC:2κO:2κO'-irontin

1-Carbonyl-1-η5-cyclopentadienyl-2,2,2-triphenyl-1-triphenylphosphine-μ-carboxylato-1κC:2κO:2κO'-irontin

Heterometallic Tin Compounds: Classification and Analysis of Crystallographic and Structural Data: Part 1. Dimeric Derivatives

CO2 Derivatives of Molecular Tin Compounds. Part 2: Carbamato, Formato, Phosphinoformato and Metallocarboxylato Complexes

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