f-Element–crown ether complexes. Part 9. The role of solvent hydrogen bonding: synthesis and crystal structure of aquatetrachlorotris(ethanol)thorium(IV)–1,4,7,10,13,16-hexaoxacyclo-octadecane–water (1/1/1)

1988 ◽  
pp. 13-16 ◽  
Author(s):  
Robin D. Rogers ◽  
Lynn K. Kurihara ◽  
Matthew M. Benning
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Crown Ether ◽  
Synthesis And Crystal Structure ◽  
Crown Ether Complexes ◽  
Role Of Solvent

Synthesis and Crystal Structure of a Caesium Hydrogen Benzoylcyanoximate Complex with 18-Crown-6: Cs(18-Crown-6){H(L)2}

1997 ◽  
Vol 52 (8) ◽  
pp. 901-905 ◽  
Author(s):  
Vera V Ponomareva ◽  
Victor V Skopenko ◽  
Konstantin V Domasevitch ◽  
Joachim Sieler ◽  
Thomas Gelbrich
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Crown Ether ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
The Mean ◽  
Cyano Groups ◽  
Oxygen Atoms

Abstract The caesium hydrogen benzoylcyanoximate (L-) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [monoclinic, space group P21/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Å, β = 90.13(1)°, V = 3434.3(9) Å, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of Cs(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}-, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O - - - O ca. 2.456(5)Å]. The caesium atom deviates by 1.492(3) Å from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical “sunrise coordination” [Cs-O (ether) 3.040(9)-3.312(7) Å]. The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (Cs-O ca. 3.040(9), 3.312(7) Å; Cs-N ca. 3.469(5), 3.679(6) Å). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism.

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