Synthesis of β-chlorinated macrocyclic [Au(C14H20N4Cl2)]X (X = AuCl2, ClO4, AuCl4) gold(III) complexes.: Crystal and molecular structures of [Au(C14H20N4Cl2)]ClO4

被引:4
作者
Afanas'eva, VA [1 ]
Glinskaya, LA [1 ]
Klevtsova, RF [1 ]
Mironov, IV [1 ]
Sheludyakova, LA [1 ]
Tkachev, SV [1 ]
机构
[1] Russian Acad Sci, Nikolaev Inst Inorgan Chem, Siberian Branch, Novosibirsk, Russia
关键词
gold; macrocyclic complexes; beta-chlorinated; synthesis; elemental analysis; crystal and molecular structures; IR spectra; NMR spectra;
D O I
10.1023/A:1024985031245
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
A square-planar [AuL2](+) gold (III) complex [L-2 = 6.13-dichloro-5,7,12,14-tetramethyl-1,4,8,11-tetraaza-4,6,11,13-tetraenato(2-)] containing two chlorine atoms in the beta-position of the ligand hexacyclic ring was first synthesized by the reaction of the [AuL1](+) tetraiminate complex [L-1 = 5,.7,12,14-tetramethyl-1,4,8,11-tetraaza-4,6,11,13-tetraenato(2-)] with HAuCl4 in an acetone-DMFA solution. The complex was isolated in the form of dichloroaurite (I), perchlorate (II). and tetrachloroaurate (III). Compounds I-III were studied by elemental and X-ray diffraction analyses and IR and NMR spectroscopies. Single crystals of [AuL2]ClO4 were obtained, and the crystal structure of this compound was determined from X-ray diffraction patterns. The crystals are monoclinic: a = 10.147(2) Angstrom, b = 7.260(1) Angstrom, c = 12.519(2) Angstrom, beta = 96.70(l)degrees, V = 915.9(3) Angstrom(3), Z = 2, space group P2/c, d(calc) = 2.218, d(meas) = 2.209 g/cm(3). The crystal structure is built of nearly planar [Au(C14H20N4Cl2)](+) cations and [ClO4](-) anions. Introduction of chlorine atoms into the beta-positions of the hexacyclic rings of the tetraazamacrocycle hardly changes the lengths of the delocalized C-N and C-C bonds.
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页码:68 / 73
页数:6
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