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The novel three-dimension edta-linked (edta＝ethylenediamine-N,N,N′,N′-tetraacetate) heterometallic complex [Sb 2 (edta) 2 -µ 4 -Co(H 2 O) 2 ]•5.15H 2 O has been synthesized and characterized by elemental analyses, FT-IR spectrum, X-ray diffraction analyses and thermogravimetry-differential scanning calorimetry (TG-DSC). The complex crystallizes in the monoclinic system, space group P2 1 /n, lattice parameters: a＝0.69969 (2) the Sb(III) ion is six coordinated by two nitrogen and four oxygen from edta ions, together with a lone electron pair at the equatorial position. In the complex, the coordination number of Co(II) ion is six and its coordination environment is composed of four carboxylic oxygen atoms from four different edta ions and two oxygen atoms from two H 2 O molecules. The degradation of the sample proceeds in several steps and the water molecules and ligands are successively emited.

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Abstract. CIoHIaN203, monoclinic, P2 l, a= 15.515(2), b=6.730(1), c= 12.541(2)A, fl= 113.6 (2) °, V = 1200.0/1,3, Z = 4, D x = 1.186 gcm -3, ,t(Mo Ka) = 0.71069 A, g = 0.54 cm -~, F(000) = 464, T= 295 K. The final R value for 1611 observed (3139 unique) reflections is 0.055. In both the independent molecules A and B of the asymmetric unit of the title compound, the conformation of the urethane moiety is trans. The lactam group of molecule A is non-planar, the C(9)-N(2)-C(10)-C(6) torsion angle being 12.4 (14) °. One main difference between molecules A and B is in the value of the ¢[C(5)-N(1)-C(6)-C(10)] torsion angle [52.3(11) ° for molecule A while -86.5 (10) ° for molecule B] as a consequence of a rotation of the ring relative to the tert-butyloxycarbonylamino substituent. A second major difference is the 6-1actam ring conformation which is approximate half-chair for molecule A while boat for molecule B.Introduction. Replacement or modification of the peptide backbone function can lead to enzymatically resistant biologically active analogs. Among the factors contributing to altered chemical and biochemical parameters are changes in electronic properties, differences in solubility characteristics, resistance to proteolytic processes, and, perhaps most important, conformational restrictions and changes that can modify receptor recognition (Spatola, 1983).In particular, we have recently undertaken the synthesis of a series of conformationally constrained analogs of the neuroactive tripeptide H-L-Pro-L-LeuGIy-NH 2 (Johnson, Yu, Taraporewala, Mishra & Rajakumar, 1985;Yu, Rajakumar, Srivastava, Mishra & Johnson, 1988) in which the y-and fi-lactam residues developed by Freidinger, Perlow & Veber (1982)have replaced either the leucyl or glycinamide residues. These compounds were synthesized in an attempt to determine whether the trans amide bond and the fl-bend 0108-2701/89/020215-04503.00© 1989 International Union of Crystallography 216 (3S)-3-tert-BUTYLOXYCARBONYLAMINO-2-PIPERIDONE MULTAN80 (Main, Fiske, Hull, Lessinger, Germain, Declercq & Woolfson, 1980) and refined by blockdiagonal least squares (based on /7) with anisotropic thermal parameters for all non-H atoms (w = 1). Some of the H atoms were located on the difference Fourier map but not refined and some were calculated. All calculations were performed with atomic scattering values of Sheldrick (1976). Parameters refined 271; R = 0.055; ratio of maximum least-squares shift to e.s.d, in final refinement cycle 0.8; maximum and minimum height in final difference Fourier synthesis 0.25 and -0.20 e/k-3; S = 0.66. Table 1 gives the final atomic coordinates and equivalent isotropic thermal parameters for the non-H atoms.* at the -Leu-Gly-sequence that characterize the crystal structure of H-L-Pro-L-Leu-Gly-NH2 (Reed & Johnson, 1973) are also characteristic of the biologically active conformation of the neuropeptide.Here we describe the structural characterization by X-ray diffraction of (3 S)-3-tert-butyloxycarbonylamino- Experimental.Colorless prismatic cryst...

Tolterodine is a drug substance contammg (+)-N,Ndiisopropyl-3-(2-hydroxy-5-methylphenyl)-3-phenylprolylamine hydrogen L(+)-tartrate CC26H37N07).The drug is used for the treatment of minary frequency, urgency and/or urge incontinence. The synthesis of tolterodin L(+)-tartrate is a well established procedure. The crystal structure of tolterodine L(+)-tartrate was determined from single crystal x-ray data at room temperature and 30 K. The structure is monoclinic with two formula units in.the unit cell and all the atoms in the general position of the space-group P2J. The unit cell dimensions at 30 K are a= 9.1759, b = 16.3965c =l2.9196A. = 93.427". In the final stage of the refinement the 3568 reflections recorded at 30 K were refined to an R-value of 4.0%.