Abstract :
The structures of five of the seven possible isomeric forms in the [Co(dien)(ampy)Cl]2þ system (three mer- and two fac-) have been
determined by single crystal X-ray diffraction: (1) m1·Cl2·H2O, triclinic P1¯, a ¼ 7:3757ð12Þ; b ¼ 9:9250ð16Þ; c ¼ 11:5002ð19Þ A ° , a ¼
100:242ð3Þ8; b ¼ 100:832ð3Þ8; g ¼ 94:615ð3Þ8; Z ¼ 2; (2) m3·ZnCl4, monoclinic P21/c, a ¼ 11:057ð3Þ; b ¼ 9:581ð2Þ; c ¼ 17:568ð4Þ A ° ,
b ¼ 95:560ð5Þ8; Z ¼ 4; (3) m4·ZnCl4 monoclinic P21/n, a ¼ 8:4464ð14Þ; b ¼ 24:398ð4Þ; c ¼ 10:0645ð17Þ A ° , b ¼ 112:510ð3Þ8; Z ¼ 4; (4)
f1·ZnCl4, triclinic P1¯ , a ¼ 10:318ð1Þ; b ¼ 12:706ð3Þ; c ¼ 7:578ð1Þ A ° , a ¼ 107:01ð2Þ8; b ¼ 94:90ð1Þ8; g ¼ 99:07ð1Þ8; Z ¼ 2; (5)
f2·(ZnCl4)0.5·Cl·H2O, triclinic P1, a¼7:7225ð18Þ; b¼8:359ð2Þ; c¼15:898ð4Þ A ° , a¼96:025ð4Þ8; b¼93:298ð5Þ8; g ¼ 116:191ð4Þ8; Z ¼ 1:
The last structure provides an example of spontaneous resolution. Two additional and independently determined structures are reported, in
excellent agreement with these results. The structural work confirms the results of the detailed 2D NMR study. The agreement between the
single crystal data and the calculated ab initio molecular parameters is excellent (within ^3%). The calculated total energies have been
computed for the gas phase and aqueous solution, and are been used to explain the relative abundances of the seven isomers observed
experimentally. The modes of isomer rearrangement are discussed.
q 2004 Elsevier B.V. All rights reserved.
Keywords :
Conglomerates , Co(III) complexes , 2-Aminomethylpyridine , diethylenetriamine , ab initio calculations , X-ray structures , Rearrangement