Synthesis and X-ray crystal structures of heavy-metal complexes of 1,5,9,13-tetrathiacyclohexadecane

Journal Article · Wed Sep 18 00:00:00 EDT 1991 · Inorganic Chemistry; (United States)

DOI:https://doi.org/10.1021/ic00019a016· OSTI ID:6837270

Setzer, W N; Tang, Yaping ^[1]; Grant, G J ^[2]; VanDerveer, D G ^[3]

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1. Univ. of Alabama, Huntsville (United States)
2. Univ. of Tennessee, Chattanooga (United States)
3. Georgia Inst. of Tech., Atlanta (United States)

Heavy-metal complexes of the macrocyclic tetrathioether 1,5,9,13-tetrathiacyclohexadecane (16S4) have been prepared by reaction of the ligand with the appropriate heavy-metal salts. The complexes [Hg(16S4)](ClO[sub 4])[sub 2], [Cd(16S4)](ClO[sub 4])[sub 2], and (16S4)(HgCl[sub 2])[sub 2] have been synthesized and characterized. Single-crystal X-ray structural studies have been carried out on [Hg(16S4)](ClO[sub 4])[sub 2] and [Cd(16S4)](ClO[sub 4])[sub 2]. Crystal data for [Hg(16S4)](ClO[sub 4])[sub 2]: C[sub 12]H[sub 24]S[sub 4]HgCl[sub 2]O[sub 8]; monoclinic space group C2/c; a = 10.033 (3), b = 13.421 (4), c = 15.960 (4) [angstrom]; [beta] = 96.48 (2)[degree]; Z = 4; R = 0.051. Crystal data for [Cd(16S4)](ClO[sub 4])[sub 2]: C[sub 12]H[sub 24]S[sub 4]CdCl[sub 2]O[sub 8]; triclinic space group P[bar I]; a = 8.346 (2), b = 8.349 (3), c = 8.688 (2) [angstrom]; [alpha] = 69.87 (2), [beta] = 68.97 (2), [gamma] = 82.33 (2)[degree]; Z = 1; R = 0.043. Molecular mechanics calculations have been carried out on the 16S4 ligand, and the lowest energy conformation is a quadrangular [4444] conformation with the sulfur atoms occupying the corners (exodentate) of the quadrangle.

• OSTI ID: 6837270
• Journal Information: Inorganic Chemistry; (United States), Vol. 30:19; ISSN 0020-1669
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
CADMIUM COMPLEXES
CHEMICAL PREPARATION
MERCURY COMPLEXES
THIOLS
MOLECULAR MODELS
EXPERIMENTAL DATA
LATTICE PARAMETERS
MOLECULAR STRUCTURE
MONOCLINIC LATTICES
TRICLINIC LATTICES
X-RAY DIFFRACTION
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
DATA
DIFFRACTION
INFORMATION
MATHEMATICAL MODELS
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC SULFUR COMPOUNDS
SCATTERING
SYNTHESIS
400201* - Chemical & Physicochemical Properties