Specific features of the structure of monomeric octahedral d 0-rhenium(VII) oxo complexes

Сергиенко, В. С.; Churakov, Andrei V.

doi:10.1134/s1063774514030171

Cited by 15 publications

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“…As in the previous publications [9][10][11][12][13][14][15][16][17][18], the struc tural manifestation of the trans effect of the multiply bonded oxo ligand, namely, the elongation of the The present study considers the structural details of monomeric octahedral mono oxo complexes with monodentate anionic (in the vast majority of cases, singly charged) ОR -ligands, except for the hydroxo and aliphatic alkoxo ligands (R = Me, Et, Pr), which were described previously [13][14][15][16]. Note that in all but one compounds considered here, the Re-O(OR) dis tances (R = Ph, Cy, C 6 H 4 R' (R' = OH, OMe), C 10 H 6 OH, P(O)(OMe) 2 In two complexes of the general formula [ReO(OR)(Hal) 2 (L 1 ) [19], where Hal = Br, R = Ph (I); Hal = Cl, R = Cy (cyclohexyl, С 6 Н 11 ) (II) (Fig.…”

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“…Five publica tions of this series cover the structural details of MOC with monodentate aqua [12], hydroxo [13], and alkoxo (methoxo [14], ethoxo [15], and propoxo [16]) ligands in trans positions to the oxo ligands. We also pub lished survey papers dealing with the crystal structures of the MOC of d 0 Re(VII) in the higher oxidation state [17] and d 0 and d 2 technetium [18].…”

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confidence: 99%

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Structural details of monomeric octahedral d 2-rhenium(V) oxo complexes with oxygen atoms in the trans-positions to oxo ligands. Complexes with the anionic ligands OR n− (n = 1, 2) in trans-positions to O(oxo)

Сергиенко

2015

Russ. J. Inorg. Chem.

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The paper considers details of the structures of mononuclear octahedral rhenium(V) oxo com plexes with oxygen atoms of aromatic (phenolic) and other similar cyclic ligands OR -(R = Ph, Cy, C 6 H 4 R' (R' = OH, OMe), C 10 H 6 OH) and with other structurally studied anionic ligands OR n-(n = 1, 2) (R = P(O)(OMe) 2 , C(O)(CF 3 ), OC(Me(CF 3 ) 2 , BF 3 ) located in the trans position to the multiply bonded oxo ligands. The complexes contain halide ligands and organic mono , bi , and tetradentate ligands in the equa torial plane. The Re-O(OR) trans bonds as well as the bonds with aliphatic alkoxo ligands (OR alk ) trans (R = Me, Et, Pr) are not elongated due to the trans effect of doubly bonded oxo groups but are substantially shortened (with one exception). This is attributable to the fact that these Re-O(OR) bonds, like Re-O(oxo) bonds, have a higher order, i.e., d 2 rhenium(V) complexes of this type should be treated as pseudo dioxo compounds [Re(=O)(=OR)] 3 -n (n = 1, 2).

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Structural details of monomeric octahedral d 2-rhenium(V) oxo complexes with oxygen atoms in the trans-positions to oxo ligands. Complexes with the anionic ligands OR n− (n = 1, 2) in trans-positions to O(oxo)

Сергиенко

2015

Russ. J. Inorg. Chem.

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“…This leads us to conclude that the samples were contaminated with + crystallized as an iodide salt instead of a chloride. The distance between the Re and I atoms is 3.72 Å, much longer than a typical Re-I bond length 46. ions were observed in both cases.…”

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“…) 46. Thermal ellipsoids are shown at the 50% probability level.ReO(hpp)2Cl was also predicted by Gaussian calculations, for both hppand hpp* -.…”

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Early transition metal and actinide coordination chemistry of a bicyclic guanidinate ligand

Olson¹

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The bicyclic guanidinate 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidinate (hpp-) has been recognized as an excellent stabilizing ligand for low oxidation state metals for about a decade. It has been used as a dinucleating anionic ligand in the synthesis of complexes containing the 'paddlewheel' structure motif (which often contain metal-metal multiple bonds) and is resistant to reductive cleavage by low-valent metal centers. One drawback to the ligand is that its metal complexes often have reduced solubility. This can be problematic in isolation and characterization. One solution to this problem is alkylation of the rings. Two derivatives of hpp-, tetramethyl-hppH (hpp*H) and tetraethyl-hppH (hpp"H) have published syntheses that were irreproducible by our research group. New and easily reproducible syntheses for hpp*H and hpp"H are presented. The syntheses of (hpp*)SiMe3 and (hpp")SiMe3, which are liquid silanes that can be isolated and purified for better stoichiometric control when transferring hpp-, hpp*-, and hpp"onto metal centers, are also described. Chapter 3 details the synthesis of several highvalent mononuclear tantalum and zirconium complexes containing hppand hpp*using these silanes. The solid-state structures of the Ta(hpp*) compounds are compared to those of the previously reported Ta(hpp) compounds. In the course of this research, it was discovered that the M(hpp)/M(hpp*) [M = Zr, Ta] complexes were highly fluorescent, exhibiting intense Ligand-to-Metal Charge Transfer (LMCT). A series of Zr(hpp)(bpy) [bpy = 2,2'-bipyridine] complexes containing different bpy derivatives were synthesized to explore the possibility of Ligand-to-Ligand Charge Transfer, a very rare phenomenon for zirconium, and are also detailed in chapter v 3. Chapter 4 describes the spectrofluorimetry of the synthesized Ta(hpp), Ta(hpp*), Zr(hpp), and Zr(hpp)(bpy) complexes. Since hpp*is known to change electronics at the metal center compared to hpp-, we wanted to investigate if its effects could be examined by spectroscopy. Chapter 5 describes the synthesis of several metal-oxo hpp complexes that were characterized via the M=O IR stretch. The comparison was made between MO(hpp)2L and MO(hpp*)2L [M = W, Re]. The M=O IR stretches were verified by 18 O isotopic labeling. Attempts at synthesizing TaOCl3 and TaO(hpp)2L are also detailed. In the last chapter (chapter 6), a few U(hpp) complexes were generated during our development of non-cyclopentadienyl hppcoordination chemistry of uranium, and are discussed. Two of the complexes characterized via X-ray crystallography are diuranium

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ChemInform Abstract: Specific Features of the Structure of Monomeric Octahedral D⁰‐Rhenium(VII) Oxo Complexes

Сергиенко

Чураков

2015

ChemInform

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Specific features of the structure of monomeric octahedral d 0-rhenium(VII) oxo complexes

Cited by 15 publications

References 60 publications

Structural details of monomeric octahedral d 2-rhenium(V) oxo complexes with oxygen atoms in the trans-positions to oxo ligands. Complexes with the anionic ligands OR n− (n = 1, 2) in trans-positions to O(oxo)

Structural details of monomeric octahedral d 2-rhenium(V) oxo complexes with oxygen atoms in the trans-positions to oxo ligands. Complexes with the anionic ligands OR n− (n = 1, 2) in trans-positions to O(oxo)

Early transition metal and actinide coordination chemistry of a bicyclic guanidinate ligand

ChemInform Abstract: Specific Features of the Structure of Monomeric Octahedral D⁰‐Rhenium(VII) Oxo Complexes

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Specific features of the structure of monomeric octahedral d 0-rhenium(VII) oxo complexes

Cited by 15 publications

References 60 publications

Structural details of monomeric octahedral d 2-rhenium(V) oxo complexes with oxygen atoms in the trans-positions to oxo ligands. Complexes with the anionic ligands OR n− (n = 1, 2) in trans-positions to O(oxo)

Structural details of monomeric octahedral d 2-rhenium(V) oxo complexes with oxygen atoms in the trans-positions to oxo ligands. Complexes with the anionic ligands OR n− (n = 1, 2) in trans-positions to O(oxo)

Early transition metal and actinide coordination chemistry of a bicyclic guanidinate ligand

ChemInform Abstract: Specific Features of the Structure of Monomeric Octahedral D0‐Rhenium(VII) Oxo Complexes

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ChemInform Abstract: Specific Features of the Structure of Monomeric Octahedral D⁰‐Rhenium(VII) Oxo Complexes