Structural Study of Optical Resolution. XII. The Crystal and Molecular Structure of (−)589-trans-SS-Bis(isothiocyanato)(triethylenetetramine)cobalt(III) μ-(+)-Tartrato(4−)-μ-(+)-hydrogentartrato(3−)diantimonate(III) Tetrahydrate

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Abstract
The crystal and molecular structure of the diastereoisomeric salt, (−)589-trans-[Co(NCS)2(trien)][Sb2((+)-tart)((+)-tartH)]·4H2O, has been determined by the X-ray diffraction method. The red crystals were monoclinic, with the space group P21, a=8.987(1), b=15.949(2), c=10.726(1) Å, β=102.57(2)°, and Z=2. The structure was solved by the heavy-atom method and refined by the block-diagonal least-squares method, using 2976 independent reflections, to the final R-value of 0.033. In the complex cation, the conformations of the three five-membered chelate rings are (δλδ), while the absolute configurations of the two asymmetric nitrogen atoms are both S. The mononegative anion has a dimeric structure of [Sb2((+)-C4H2O6)((+)-C4H3O6)]−, in which (+)-C4H2O64− and (+)-C4H3O63− coordinate to two SbIII atoms. The extra hydrogen atom in (+)-C4H3O63− bonds to the free oxygen atom(OTB5) of the carboxylato group, and a short contact is formed between this oxygen atom and a water molecule(OW2); OTB5···OW2 2.43(1) Å. Though six N–H hydrogen atoms are present in the complex cation, three of them form N–H···O hydrogen bonds to the oxygen atoms of the dimeric anion; NTR3···OTA1 2.86(1), NTR4···OTA6 2.86(1), and NTR1···OTB4 3.19(1) Å.

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