Can. J. Chem. 62, 2657 (1984. Three types of complexes, trans-[Pt(LH),Cl,], [Pt(L),I, and [Pt(LH),(SR),I where LH = NH2-C(CH3)2(CH20H) and NH2--C(CH20H)3 and L are the deprotonated ligands, have been synthesized.The crystal structure of ~~~~S-[P~(NH,-C(CH~)~CH~OH)~C~~] has been determined by X-ray diffraction methods. The crystals are monoclinic, space group P2!/c, with a = 6,282(3), b = 20,901(13), c = 10,769(10) A, f3 = 92,64(6)", and Z = 4. The structure was refined by full-matrix least-squares analysis to a conventional R factor of 0.049 and R,, = 0.042. The coordination around the platinum atom is square planar. The Pt-C1 distances are 2.306(2) and 2.309(3) A and the Pt-N bonds are 2.060(8) and 2.07 l(7) A. The hydroxyl oxygen atoms are disordered; the disorder is different for each organic ligand.The structure is stabilized by an extensive hydrogen bonding system. We have modified these methods to prepare trans-[Pt(LH),-
C12] add [Pt(L),] . Compounds of NH2-C(CH3),CH20H (identified below as L'H) were also synthesized. Organic sulphur compounds R-SH (thiophenol and thiouracil) can react with [Pt(L),] or [Pt(L1),] to form [Pt(LH),(SR),] (or L'H). The three types of complexes [Pt(LH),Cl,], [Pt(L),], and [Pt(LH),(SR),] (or L'H) are believed to be trans-isomers.In order to confirm these hypotheses, we wanted to determine the crystal structures of one compound of each type. Unfortunately, up to now, only [Pt(L1H),Cl2] gave suitable crystals for X-ray diffraction. Its crystal structure is reported below.
Experimental[Pt(L2)l and lPt(L1),l K,PtC14 and LH or L'H were dissolved in water in a ratio of LH : Pt > 5. The mixture was heated to 50-70°C for about 1 h and then cooled to room temperature. The light yellow precipitate was filtered, washed with water, and dried with a vacuum pump overnight. The compounds crystallized with one (L) and two (L') molecules of water (Table 1). Yield: 80%.crystals slowly formed and they were washed with water and dried under vacuum overnight. Yield: 90%.[Pt(LH), ( A set of precession photographs showed that the crystals belong to the P 2 , l c space group. The cell parameters were calculated by least-squares refinement from the setting angles of 15 centered reflections on a Syntex P1 diffractometer using graphite-monochromatized MoKa radiation. A total of 4140 independent reflections were measured with 28 < 60" by the 8-28 scan technique using MoKa radiation. The scan rate was l o (28) min-' for most reflections, but rates as high as 24" min-I were selected for strong reflections by the autocollection program. A 28 scan range of lo below Ka, and lo above Ka, was chosen. The background time to scan time ratio was 0.50. Reflections with I,,, <
Crystal data