D. S. Sake Gowda

Structure determination of tolbutamide

N-​[(Butylamino)​carbonyl]​-​4-​methylbenzenesulfonamide, is an antidiabetic drug which crystd. in orthorhombic space group Pn21a, with a 20.16(2)​, b 9.05(1)​, c 7.85(1) A; Z = 4, d.(exptl.) = 1.24 and d.(calcd.) = 1.25 for Z = 4. The structure was solved by the Patterson search method and refined to R = 0.083 for 615 visually measured reflections. At. parameters are given. The structure is stabilized by H bonding between the polar ground and van der Waals interactions between the nonpolar groups. Of the three H bonds, two are weakly as they are bifurcated.

Crystal Structure of 4,6-dinitro-1-(5-tetrazolyl)-1H-indazole Trihydrate

The title compound, C8H4N8O4·3H2O, crystallizes in space groupP¯1 with cell constantsa=7.022(1),b=9.507(2),c=10.906(2) Å,α=84.99(1),β=71.89(1),γ=72.56(1)°,Z=2, andVc=660.2 Å3. The structure was solved by direct methods using diffractometer data and was refined by full-matrix least-squares methods to anR value of 0.060 for 2112 observed reflections. The molecule, consisting of a phenyl ring fused to a pyrazole ring with a tetrazole ring connected to it equatorially, is planar except for the N(7) nitro-group oxygen atoms. The structure is stabilized by a three-dimensional network of O-H⋯O, O-H⋯N, and N-H⋯O hydrogen bonds through the water molecules.

The crystal structure of 5-methyl-1-(octahydro-1-iodo-1H-1-inden-4-yl)-1H-tetrazole

The title compound is C11H17N4I, F.W.=330.20, monoclinic, space groupP21/a,a=11.586(2),b=10.617(1),c=10.417(1) Å, β=94.567(2)°,Z=4,F(000)=652, λ(MoKα)=0.7107 Å, μ(MoKα)=2.31 mm−1,V=1277.31 Å3,DC=1.71 gcm−3,Dm=1.70 gcm−3. The structurewassolved by Patterson and Fourier methods and refined to anR value 0.031 for 1620 observed reflections. The connectivity and conformation of the addition product ofcis-1,5-cyclononadiene and iodine azide was determined by X-ray analysis. The reaction product contains a chair-conformation cyclohexane ring that iscis fused to a cyclopentane ring. The cyclopentane ring has an envelope conformation and an equatorially oriented iodine substituent. A planar tetrazole ring is axially substituted on the cyclohexane ring. The plane of the tetrazole ring makes a dihedral angle of 69.6° with the average plane of the carbon atoms of the cyclohexane ring.

2,4‐Dinitrobenzaldehyde (1H‐tetrazol‐5‐yl)hydrazone

C s H 6 N 8 0 4 , M r = 278.2, monoclinic, P21/n, Z = 4, T = 293 K, a = 10.991 (2), b = 9.056 (2), c = 11.706(2)A, f l = 101.50(1) ° , V = 1141.8A3, D m = 1.60, D x 1.62 Mg m 3 , g 0.118 mm -~, C u K a radiation (2 -1.54051 A). Final R = 0.049 for 1228 independent reflections. The title compound, DBTYH, consists of a 2,4-dinitrobenzaldehyde moiety and a tetrazole moiety bridged by a hydrazone chain. Each molecule is hydrogen-bonded to three other molecules through four hydrogen-bond linkages (two acceptor and two donor) centered on the tetrazole ring. The entire molecule is approximately planar with the exception of one nitro group which is rotated 39 ° out of the plane of the benzene ring and has a short C H . . . O distance that could indicate a weak intramolecular hydrogen bond. The crystal was automatically recentered every 428 reflections, with four standard reflections checked after each 102 measurements. Of the resulting 1701 independent reflections, 1228 reflections with F > 3a(F) were used in the refinement. Lorentz-polarization corrections were applied; decay and absorption corrections were not necessary. The structure was solved with MULTAN (Declercq, Germain, Main & Woolfson, 1973) using 141 reflections (Emi n = 1.75) and three general phase relationships. All but one of the non-H atoms were located in Table 1. Fractional coordinates (x 104, for H x 103) and Beq or Bis o (A 2) with e.s.d.s in parentheses, and deviations (A × 10 a A) of non-hydrogen atoms from the least-squares plane (see text) Introduetlon. DBTYH, which was prepared by reacting (1H-tetrazol-5-yl)hydrazine with 2,4-dinitrobenzaldehyde (Thiele, 1898), has been used in the preparation of explosives (Jaffery, 1976) as have other tetrazole x compounds (Duke, 1971; Bryden, 1958). Its thermal o ( 1 ) -1246(6) decomposition has been studied under dynamic and o(2) 34 (7) o(3) 850 (8) isothermal conditions using a differential scanning o(4) 1770(7) calorimeter (Om Reddy, Krishna Mohan, Mohan N ( 1 ) 2158(6) N(2) 2490 (7) Murali & Chatterjee, 1981). N(3) 1856 (6) Oscillation and Weissenberg photographs of a yellow N(4) 1128 (6) N(5) 807 (6) crystal of DBTYH (grown by slow evaporation from a N(6) 1127 (6) 2:1 methanol-dioxane mixture) showed the crystal N ( 7 ) -359(6) system to be monoclinic, with systematic absences 0k0, N(8) 1249 (7) C(1) 818 (7) k = 2n + 1 and hOl, h + l = 2n + 1, indicating space c(2) 325 (7) group P21/n, with general positions x,y,z and 1⁄2 x, 1⁄2 + c(3) 450 (7) y, 1⁄2 -z. The crystal density was measured by flotation c(4) 1113 (7) C(5) 1649 (8) using iodobenzene and kerosene, c(6) 1484 (8) Accurate unit-cell parameters were obtained by c(7) 614(7) least-squares refinement of 15 carefully centered c(8) 1341(7) H(N1) 247 (8) reflections and 1952 reflections (20ma x : 120 °) were H(N5) 36(9) measured using the 0-20 scan mode on a Syntex P21H(C3) 7 (6) F diffractometer (crystal size 0.06 x 0.09 x 0.11 mm). H(C5) 214 (7) H(C6) 186 (6) H(C7) 0 (5) * Permanent address: Depar tment of Physics, Central College, Bangalore University, Bangalore 560 001, India. 0567-7408/82/092487-04501.00 Beq or

The crystal structure of 5α-cyano-3-keto-10-methyl-octahydronaphthalene

Abstract5α-cyano-3-keto-10-methyl-octahydronaphthalene, C12H17NO, crystallizes in monoclinic space group P21·c witha = 7.28(2),b = 7.48(2),c = 19.29(5)Å, β= 88.0(2)∘ and has four molecules per unit cell. The structure was solved by direct methods and refined to anR-value of 11.4% by block diagonal least-squares method for 565 observed reflections recorded by film method. The cyano group iscis to methyl group at C(10) and the fused rings have a chair conformation. The carbonitrile fragment is almost linear, the angle C-C= N being 175.6(3.0)∘.

Ethyl α-phenylhydrazono-2-furanpropionate

The title compd. is orthorhombic, space group Pca21, with a 11.115(1)​, b 8.170(1)​, and c 15.341(1) A; Z = 4 for dm = 1.290 and dc = 1.293. The structure was solved by direct methods and refined to an R of 0.041 for 1033 reflections. At. coordinates are given. The structure conforms to the non-​H-​bonded α form. The hydrazine moiety is planar with sp2 hybridization at the N and neighboring atoms. Intermol. N-​H...O hydrogen bonds link the mols. into chains along a.

The structure of 2-piperidinotricyclo[5.2.2.02,6]undecan-9-one

The title compd. is monoclinic, space group Cc, with a 24.28(4)​, b 8.76(6)​, c 14.03(2) A, and β 108.00(9)​°; d.(exptl.) = 1.18 and d.(calcd.) = 1.16 for Z = 4 (2 mols.​/Z)​. The structure was detd. to obtain accurate information about the geometry of the mol. as there was ambiguity in the chem. structure. The structure was refined to R = 6.3​% for 1165 visually measured reflections. At parameters, bond angles and distances are given. The established structure proposed on the basis of chem. and phys. data. The new structure explains some reactions which could not be understood from the previously proposed structure.

Crystal structure of ethyl pyruvate-2-methyl-4-chloro-phenyl hydrazone

Ethyl pyruvate-2-methyl-4-chloro-phenylhydrazone, C12H15N2O2Cl, is an important intermediate for the synthesis of ethyl-5-chloro-7-methyl indole-2-carboxy-late. Crystals are orthorhombic witha=6.99(4),b=23.75(6),c=17.05(6) A and eight molecules per cell in the space group Cmca. The structure was solved by direct methods using film data and refined by block diagonal least squares method to anR-index of 0.052. The molecule occupies the space group mirror(m) special position. The stacking of the molecules is stabilized by van der Waal’s contacts.

5(S)-Cyano-9-oxotricyclo[4.2.1.14,7]dec-2-en-8-yl methanesulfonate

The title compd. is orthorhombic, space group Pca21, with a 10.159(5)​, b 8.656(3)​, and c 13.950(5) A; d.(exptl.) = 1.43 and d.(calcd.) = 1.45 for Z = 4. The structure was solved by the Patterson search method and refined to R = 0.054 for 960 reflections. At. parameters, bond lengths, and bond angles are given. No H bonding is obsd. and the structure is held together by van der Waals interactions.