New Macrocyclic Ligands. XI. Synthesis, X-Ray Structure and Computational Studies of a New N2O4S2-Heteroatom Cage

2000 ◽  
Vol 53 (9) ◽  
pp. 799 ◽  
Author(s):  
Ian M. Atkinson ◽  
David C. R. Hockless ◽  
Leonard F. Lindoy ◽  
Owen A. Matthews ◽  
George V. Meehan ◽  
...  
Keyword(s):  
Single Crystals ◽  
Structure Determination ◽  
Macrocyclic Ligands ◽  
Computational Studies ◽  
Mo Calculations ◽  
X Ray ◽  
Semiempirical Mo Calculations ◽  
Cage Molecule ◽  
Helical Configuration

The synthesis and single-crystal X-ray structure determination of a new cage molecule containing four oxygen, two sulfur, and two nitrogen heteroatoms are described. The structure determination shows that a twist occurs about each (tribenzyl) nitrogen bridgehead so that an overall helical configuration within putative quasi-2 symmetry is generated; both nitrogens have their lone pairs orientatedexo. Single crystals of this compound are homochiral. Semiempirical MO calculations have been used to probe the topological rigidity of this system relative to the more symmetrical analogue incorporating six oxygen and two nitrogen heteroatoms reported previously. The introduction of the sulfur atoms appears to restrict the facile interconversion between enantiomers that was predicted for the N2O6-analogue mentioned above. The implications of the structure for the design of larger cages are discussed.

New Macrocyclic Ligands. V. Synthetic, Crystallographic and Computational Studies of a New N2O6-Heteroatom Cage

1994 ◽  
Vol 47 (6) ◽  
pp. 1155 ◽  
Author(s):  
IM Atkinson ◽  
LF Lindoy ◽  
OA Matthews ◽  
GV Meehan ◽  
AN Sobolev ◽  
...  
Keyword(s):  
Macrocyclic Ligands ◽  
Computational Studies ◽  
Mo Calculations ◽  
X Ray ◽  
Semiempirical Mo Calculations ◽  
Cage Molecule

The synthesis, characterization and X-ray structure of a new cage molecule containing six phenoxy and two nitrogen heteroatoms is reported. Semiempirical MO calculations have been used to probe the topological rigidity of the cage relative to related aliphatic systems.

Synthesis and Coordination Chemistry of Novel Binucleating Macrocyclic Ligands with Amine-thioether and Amine-thiophenolate Donor Functions

2001 ◽  
Vol 56 (9) ◽  
pp. 901-907 ◽  
Author(s):  
Marco H. Klingele ◽  
Gunther Steinfeld ◽  
Berthold Kersting
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Reductive Amination ◽  
Condensation Product ◽  
Macrocyclic Ligands ◽  
Crystal Structure Determination ◽  
Deprotonated Form ◽  
X Ray ◽  
New Compounds

Abstract The ability of the aromatic tetraaldehyde l,2-bis(4-tert-butyl-2,6-diformylphenylsulfanyl)-ethane (1) to function as a precursor in the preparation of binucleating hexaamine-dithiolate ligands has been investigated. Reductive amination of compound 1 with bis(aminoethyl)amine under medium-dilution conditions affords the macrobicyclic hexaamine-dithioether compound L1. Deprotection of the [1+2] condensation product gives the corresponding 24-membered hexa-amine-dithiophenol ligand H2L2. The formulation of L1 as a macrobicyclic amine-thioether was confirmed by an X-ray crystal structure determination of the tetranuclear nickel(II) complex of L1, [{(L1)Ni2Cl2}2(μ-Cl)3](BPh4) (2b). The formulation of the doubly deprotonated form (L2)2- of H2L2 as a 24-membered amine-thiophenolate ligand was confirmed by an X-ray crystal structure determination of the dinuclear cobalt(III) complex, [(L2)CoIII(μ-OH)](ClO4)2 · Cl (3). The preparation and the crystal structures of the new compounds are described.

Kristallstruktur von [Mo(Co)3(Ncme)(Srbu)]2 / Crystal Structure of [Mo(CO)3(NCMe)(S'Bu)]2

1998 ◽  
Vol 53 (3) ◽  
pp. 378-380
Author(s):  
Mike R. Kopp ◽  
Bernhard Neumüller
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Single Crystals ◽  
Structure Determination ◽  
Space Group ◽  
X Ray

Abstract Single crystals of [Mo(CO)3(NCMe)(S′Bu)]2 (1) and [{Mo(CO)3}2{Mo(CO)2}{S′Bu}4] (2) were obtained by the reaction of [Mo(CO)3(NCMe)3] with [(PhCH2)2GaS′Bu]2 in 1,4-dio-xane. The X-ray structure determination of 1 showed the presence of a Mo2S2 four-membe-red ring with a Mo-Mo bond length of 296,7(1) pm. Space group Pbca, Z = 4, lattice dimen­sions at -80°C: a = 1588,2(3), b = 905,8(1), c = 1676,0(1) pm, R1 = 0,0555.

Synthesis, characterization, and x-ray structure determination of chromium(I) nitrosyl complexes with macrocyclic ligands

1977 ◽  
Vol 16 (5) ◽  
pp. 1055-1060 ◽  
Author(s):  
Dennis. Wester ◽  
Robert C. Edwards ◽  
Daryle H. Busch
Keyword(s):  
Structure Determination ◽  
Macrocyclic Ligands ◽  
X Ray ◽  
Nitrosyl Complexes

Preparation and Crystal Structure Determination of [(C2Η5)4N]2Hg3Cl8

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Coordination Type ◽  
X Ray

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.

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