scholarly journals Crystal structure of [Th3(Cp*)3(O)(OH)3]2Cl2(N3)6: a discrete molecular capsule built from multinuclear organothorium cluster cations

Author(s):  
Steven P. Kelley ◽  
Pokpong Rungthanaphatsophon ◽  
Justin R. Walensky

An unusually large and structurally complex charge-neutral polynuclear cluster, hexa-μ2-azido-di-μ3-chlorido-hexa-μ2-hydroxido-di-μ3-oxido-hexakis(pentamethylcyclopentadienyl)hexathorium–diethyl ether–tetrahydrofuran (1/0.56/1.44), [Th3(C10H15)6Cl3(N3)6(OH)6O2]·0.56C4H10O·1.44C4H8O or [Th3(Cp*)3(O)(OH)3]2Cl2(N3)6·0.56C4H10O·1.44C4H8O (Cp* = [pentamethylcyclopentadienyl])−, has been crystallized as a mixed tetrahydrofuran/diethyl ether solvate and structurally characterized. The molecule contains a number of unusual features, the most notable being a finite yet exceptionally long cyclic metal-azido chain. These rare features are the consequence of both sterically protecting Cp* ligands and highly bridging oxide and hydroxide ligands in the same system and illustrate the interesting new possibilities that can arise from combining organometallic and solvothermal f-block element chemistry.

Author(s):  
Thomas E. Shaw ◽  
Alfred P. Sattelberger ◽  
Titel Jurca

The true identity of the diethyl ether adduct of tungsten(IV) chloride, WCl4(Et2O) x , has been in doubt since 1985. Initially postulated as the bis-adduct, WCl4(Et2O)2, questions arose when elemental analyses were more in line with a mono-ether adduct, viz. WCl4(Et2O). It was proposed that this was due to the thermal instability of the bis-adduct. Here, we report the room-temperature X-ray crystal structure and Hirshfeld surface characteristics of trans-tetrachloridobis(diethyl ether)tungsten(IV), trans-WCl4(Et2O)2 or trans-[WCl4(C4H10O)2]. The compound crystallizes, with half of the molecule in the asymmetric unit, in the centrosymmetric space group P21/n. The W—O distance is 2.070 (2) Å, while the W—Cl distances are 2.3586 (10) and 2.3554 (10) Å.


1992 ◽  
Vol 11 (11) ◽  
pp. 3907-3910 ◽  
Author(s):  
Gregory S. Girolami ◽  
Matthew E. Riehl ◽  
Kenneth S. Suslick ◽  
Scott R. Wilson

2001 ◽  
Vol 56 (4-5) ◽  
pp. 443-445 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Christian Lustig

The thermally highly unstable diethyl ether solvate of lithium chloride was crystallised and its crystal structure determined. It consists of a cubic cluster of the composition Li4Cl4 with each of the four Li atoms coordinated to a molecule of diethyl ether.


1986 ◽  
Vol 17 (18) ◽  
Author(s):  
G. BOCHE ◽  
H. ETZRODT ◽  
M. MARSCH ◽  
W. MASSA ◽  
G. BAUM ◽  
...  

2018 ◽  
Vol 74 (11) ◽  
pp. 1609-1612 ◽  
Author(s):  
Lisa Leben ◽  
Eike Schaub ◽  
Christian Näther ◽  
Rainer Herges

The crystal structure of the title compound, [Zn(C48H24N8S4)(C4H10O)]·C4H10O, consists of discrete porphyrin complexes that are located on a twofold rotation axis. The ZnII cation is fivefold coordinated by four N atoms of the porphyrin moiety and one O atom of a diethyl ether molecule in a slightly distorted square-pyramidal environment with the diethyl ether molecule in the apical position. The porphyrin backbone is nearly planar with the metal cation slightly shifted out of the plane towards the coordinating diethyl ether molecule. All four isothiocyanato groups of the phenyl substituents at the meso-positions face the same side of the porphyrin, as is characteristic for picket fence porphyrins. In the crystal structure, the discrete porphyrin complexes are arranged in such a way that cavities are formed in which additional diethyl ether solvate molecules are located around a twofold rotation axis. The O atom of the solvent molecule is not positioned exactly on the twofold rotation axis, thus making the whole molecule equally disordered over two symmetry-related positions.


2020 ◽  
Vol 76 (10) ◽  
pp. 947-951
Author(s):  
Thomas E. Shaw ◽  
Pierre LeMagueres ◽  
Alfred P. Sattelberger ◽  
Titel Jurca

First reported in 1930, MoCl3O(Et2O)2 is a by-product of the reductive synthesis of MoCl4(OEt2)2 from MoCl5. We report herein the X-ray crystal structure and Hirshfeld surface characteristics of mer-MoCl3O(Et2O)2, or [MoCl3O(C4H10O)2]. The compound crystallizes in the orthorhombic space group P212121. The molybdenyl (Mo=O) bond length is 1.694 (3) Å and the cis- and trans-Mo—O distances are 2.157 (3) and 2.304 (3) Å, respectively. Intermolecular Mo=O...H bonding is present in the lattice, with the shortest distance being 2.572 Å.


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