The crystal and molecular structure of 14-β-N-pentylaminomorphinone,C22H28N2O3

The crystal and molecular structure of 14--N-pentylaminomorphinone (14--N-PAM), C₂₂H₂₈N₂O₃, has been determined by analysis of single crystal X-ray diffraction data. The compound crystallized at room temperature in the orthorhombic system, space group P2₁2₁2₁ witha=12.4535(8),b=13.7855(8),c=11.710(1) Å,V _c =2010.3(2) ų,Z=4,D _x =1.22 gm/cm³,(Cu K)=6.58 cm^–1, andF(000)=792. The final refinement yieldedR=0.051,R _w =0.059 for 328 variables with 1133 unique observed reflections. The absolute configuration is established via the synthesis from thebaine by the noninvolvement of certain asymmetric centers. The molecule is found to have as its central structure a T shape similar to that found in morphine and codeine. The distinctive feature of the molecule is the 14--N-pentylamino lipophilic side chain. Molecular modeling studies on the alkylamino chain result in the identification of clusters of conformations based on energy and dihedral angle criteria. Selected conformations are compared to 19-propylthevinol (etorphine), another potent analgesic which contains a lipophilic hydroxyalkyl substituent at C19. The enhanced analgesic activity of 14--N-pentylaminomorphinone is postulated to arise from an overall morphine-like contact with the receptor augmented by the interaction of the aliphatic chain with a lipophilic receptor pocket.     

The crystal structure analysis of iron nitroprusside,Fe[Fe(CN)5NO]·3H2O

The crystal structure of iron(II) pentacyanonitrosylferrate trihydrate has been determined from three dimensional, single-crystal X-ray diffraction data. Fe[Fe(CN)₅NO]·3H₂O crystallizes in the monoclinic space group P2₁/n with lattice constants,a=7.205(1),b=14.641(2),c=10.680(1) Å,=91.14(1)° andZ=4,D _m =1.89(1) g cm^–3 andD _x =1.92 g cm^–3. Final full-matrix least-squares refinement of 1691 unique reflections yieldedR=0.024 andR _w =0.028. Both iron atomic centers have distorted octahedral symmetries. The cation iron center is coordinated by five cyanide ligands and one water molecule, while the second iron center is coordinated by five cyanide ligands and one nitrosyl group. Cyanide bridging links the metal centers. Two uncoordinated water molecules, O(2) and O(3), are hydrogen bonded to the coordinated water molecule, O(1), and occupy channels in the crystal lattice. Important mean bond distances for iron nitroprusside are: Fe(cation)-N=2.159(17), Fe-C=1.936(4) and C=N=1.144(6) Å. Other notable bond lengths include: Fe-O(1)=2.152(2), Fe-NO=1.669(2) and NO=1.131(3) Å. The distances between the coordinated water molecule and two uncoordinated water molecules are 2.855(3) and 2.740(3) Å.     

Crystal and molecular structure of [Pd(η5-C5H5) (bis-1,2-diphenylphosphinoethane)] [CF3SO3]

The crystal structure of the complex [Pd( ⁵-C₅ H₅) (PPh₂) CH₂CH₂PPh₂]⁺ [CF₃SO₃]^– has been determined from single crystal X-ray data and refined by least-squares methods toR=0.046. The monoclinic crystals have unit cell dimensionsa=9.832(3),b=12.104(4),c=13.765(4)Å,=111.22(3)°, space group P2₁, andz=2. In the cationic complex the palladium atom is coordinated to the ⁵-cyclopentadienyl moiety and to the phoshorus atoms of the chelating diphosphine. The arrangement of the two phosphorus atoms and the centroid of the cyclopentadienyl ring is approximately trigonal.     

Complexation between tungsten(VI) and citrate: The crystal and molecular structure of a dinuclear complex,Na6[W2O5(cit)2]·10H2O

The crystals of the title compound are monoclinic, space groupP2₁/c witha=9.014(1),b=9.8668(5)c=17.5000(3) Å,=91.50(1)°,V=1556(1) ų. The structure was determined by Patterson methods and refined by least squares toR=0.038 for 3829 observed reflections and 224 parameters. There are two tungsten dimers in the unit cell, each formed by a bridging oxygen lying on a center of symmetry. Each tungsten has five more coordination sites; two occupied by terminal oxygens and the remaining three by citrate oxygens. Waters of crystallization are distributed throughout the cell and together with various of the anion oxygens, make the sodium cations either five-or six-coordinate.     

Crystal and molecular structure of complex compound [Fe3O(CH3COO)6(H2O)3]2[ZnCl4] ⋅ 2H2O

The X-ray crystal structure of trinuclear iron acetate [Fe₃O(CH₃COO)₆(H₂O)₃]₂ [ZnCl₄] ? 2H₂O was determined. The crystal has a ionic structure. It is monoclinic, a = 25.363(7), b = 14.533(4), c = 15.692(4) Å, β = 103.11(2)°, space group _C2/c, and R = 0.0685. The structure of the cationic complex [Fe₃O(CH₃COO)₆(H₂O)₃]⁺ is typical of trinuclear iron(III) compounds containing a μ₃-O bridge: the iron atoms are situated at the vertices of an almost equilateral triangle with the O atom at the center. Each Fe atom is coordinated by four O atoms of bridging carboxy groups, the μ₃-bridging O atom, and the water molecule in the trans position to the latter O atom. Mössbauer spectroscopy evidence indicates the high-spin state (_S = 5/2) of the iron(III) ions.     

The crystal structure of 5α,9α-peroxyergosta-7,22-dien-6-one-3β-ol acetate

Ergosterol acetate, in pyridine, reacts with hydrogen peroxide and catalytic amounts of FeCl₃ to afford the unusual product 5,9-peroxyergosta-7,22-dien-6-one-3-ol acetate. The peroxide, in the title structure, is seen to bridge the C5 and C9 positions of the sterol backbone. Crystal data: C₃₀H₄₄O₅, orthorhombic, P2₁2₁2₁, a = 6.552(2), b = 11.048(8), c = 37.60(2), V = 2772(3)ų, Z = 4.     

Synthesis and crystal structure of (CN3H6)2[UO2(OH)2(NCS)]NO3 and β-Cs3[UO2(NCS)5]

Compounds (CN₃H₆)₂[UO₂(OH)₂(NCS)]NO₃ (I) and β-Cs₃[UO₂(NCS)₅] (II) are synthesized and studied by IR spectroscopy and single-crystal X-ray diffraction. I and II crystallize in the orthorhombic system. For I, a = 12.2015(13) Å, b = 7.3295(8) Å, c = 16.310(2) Å, space group Pnma, Z = 4, and R = 0.0327; for II, a = 21.7891(6) Å, b = 13.5120(3) Å, c = 6.8522(2) Å, space group Pnma, Z = 4, and R = 0.0268. In structure I, complex groups form infinite chains [UO₂(OH)₂(NCS)] _n ^n? belonging to the AM ₂ ² M ¹ crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ , M ² = OH^?, and M ¹ = NCS^?). The main structural elements of crystals II are mononuclear [UO₂(NCS)₅]^3? groups belonging to the AM ₅ ¹ group of uranyl complexes (A = UO ₂ ²⁺ and M ¹ = NCS^?). In I and II, uranium-containing complexes are connected with outer-sphere cations by electrostatic interactions, and in I a system of hydrogen bonds also contributes to their binding. Specific features of the packing of complex [UO₂(NCS)₅]^3? groups in the structures of two modifications of Cs₃[UO₂(NCS)₅] are discussed.     

Crystal and molecular structure of [H3O·18-crown-6]2-[ReCl6] isolated from a liquid clathrate medium

The crystal and molecular structure of [H₃O·18-crown-6]₂[ReCl₆]1 is reported. Crystal data for1: trigonal, space group R ,a=13.857(2) Å,c=10.154(2) Å,D _c =2.85 g/cm³,Z=3,R _f =0.073,R _w =0.064. The oxonium ion is observed to be crystallographically disordered lying 0.37 Å on both sides of the plane defined by the crown ether oxygen atoms. The anion resides on a crystallographic position forming a slightly distorted octahedron.     

Crystal structure of 9,12-ethano-12a-methoxycarbonyl-5, 8a,9,12,12a,12b-hexahydro-6H-[1,2]dioxino[4′,5′:4,5] isoxazolo[3,2-a]isoquinoline, C17H19NO5

The title compound crystallizes in the space group P2₁/n, with a = 18.423(3), b = 9.628(3), c = 19.243(2) Å, = 116.208(8)°, with two independent molecules in the asymmetric unit, which are not enantiomers. The chiral centers C8a, C9, C12, C12a, C12b are either S,R,S,R,R or R,S,R,S,S, respectively, because of the centric space group.     

Synthesis and crystal structure of [Y(NO3)3(OH2)3]·(Me2-16-crown-5)·H2O

The complex [Y(NO₃)₃(OH₂)₃]·(Me₂-16-crown-5)·H₂O has been prepared and its crystal and molecular structure determined using single crystal X-ray diffraction. The colorless crystals belong to the monoclinic space group P2₁/n with Z = 4. Lattice parameters are a = 10.420(1), b = 17.257(3), c = 14.646(2) Å, = 96.79(1)°, V = 2615.1(6) ų. The yttrium(III) ion is nine-coordinate, bonded to three bidentate nitrate groups and three water molecules. The average Y–O(nitrate) and Y–O(water) distances are 2.42(3) and 2.33(1) Å, respectively. The average HO–H···O hydrogen bonded separation is 2.767Å.     

Crystal and molecular structure of 7-hydroxyflavone monohydrate, C14H10O3·H2O

The X-ray crystal structure of 7-hydroxyflavone monohydrate, C₁₄H₁₀O₃ · H₂O, is determined. The compound crystallizes in the monoclinic space group, P2₁/n with a = 3.801(3), b = 19.665(4), c = 16. 039(6), = 93.69(3)°, and = 0.68 mm^–1 for Z = 4. The phenyl ring of the flavone moiety is rotated 18.6(1)° out of the penzopyran plane, which is a typical value for flavones. In the crystal lattice, there are wide channels which are lined mainly by C–H groups. The water molecules enclosed in these channels are severely disordered.     

Crystal and molecular structure determination, TGA, DTA, and infrared and Raman spectra of rubidium nitroprusside monohydrate, Rb2[Fe(CN)5NO]·H2O

The crystal structure of rubidium nitroprusside monohydrate, Rb₂[Fe(CN)₅NO] · H₂O, has been determined from X-ray diffraction data and refined using direct and Fourier methods to R = 0.066 and Rw = 0.075, employing 1894 independent reflections with I > 3 (I). The substance crystallizes in the monoclinic space group C2/c (C ⁶ _2h), with a = 13.987(2), b = 10.241(1), c = 18.151(1) Å, = 110.94°, and Z = 8. Anions are located at C ₁ sites, one per asymmetric unit, and are slightly distorted octahedra. TGA, DTA, FTIR, and FTIR Raman results were interpreted on the basis of the formula of the compound, its crystal structure, and the behavior of other nitroprussides.     

The synthesis and crystal structure of [La(OH2)5(phen)2]Cl3·4H2O·phen

[La(OH₂)₅(phen)₂]Cl₃·4H₂O·phen is centric, Pnna, witha=19.946(7),b=16.458(5),c=12.207(4)Å andD _calc=1.57 g cm^–3 forZ=4. The La(III) ion resides on a crystallographic twofold axis and is coordinated to four nitrogen atoms (from two phen molecules) and five water molecules resulting in a distorted tricapped trigonal prismatic geometry. An uncoordinated phen molecule, two chloride anions, and four uncoordinated water molecules are hydrogen bonded to the coordinated water molecules. The coordinated and uncoordinated phen molecules -stack diagonally through the unit cell.     

2α-Hydroxy-3α-[N-alkyl(aryl)]-pinanoamines. Part II. Synthesis and the nature of some pinanoamines and crystal and molecular structure of 2α-hydroxy-3α-(N-n-butyl)-pinanoamine hydrochloride

Several optically pure representatives of 2-hydroxy-3-[N-alkyl (aryl)] pinanoamines, potential chiral auxiliaries in organic synthesis, were obtained. In addition, a structural examination of 2-hydroxy-3-(N-n-butyl)-pinanoamine hydrochloride was conducted. Results of these studies confirm the structure of the amines obtained and the correctness of the proposed reaction pathway.Crystal data: C₁₂H₂₈NOCl,P2₁/c,a=13.196(1),b=8.562(1),c=14.276(1) Å,=110.41(3)°,R=0.034 for 2046 reflections.Part I,J. Cryst. Spec. Res. (1989)19, 535.     

Crystal structure of 17β-hydroxy-17α-methyl-5α-androstano [2,3-C] Furazan (Furazabol)

The crystal and molecular structure of 17-hydroxy-17-5-androstano [2,3-C] Furazan, Furazabol (C₂₀H₂₄N₂O₂), has been determined by direct methods and refined by full matrix least squares to a final R of 0.0528 for 1927 observed reflections and 216 parameters, CuK, = 1.54178 Å. The compound crystallizes with two molecules in the asymmetric unit, Z = 4, Dc = 1.131 Mg m^–3 space group P2₁, with unit cell parameters a = 18.747(3), b = 6.346(5), c = 15.647(4) Å, = 99.96(2)°, V = 1833.9 ų, (CuK) = 0.584 mm^–1. Whilst the two independent molecules have similar overall geometry there are small differences in bond lengths, bond angles and torsion angles in rings A and D and significant conformational differences in ring A. The A ring adopts a half-chair conformation in molecule A and an intermediate between a half-chair and a sofa in molecule B. The D ring in molecule A has a 13/14 half-chair conformation and in molecule B a conformation between an envelope and half-chair.     

Synthesis and crystal structure of 3-ammoniumphenyl sulfone selenate, 3-aminophenyl sulfone [C12H14N2O2S]SeO4 · [C12H12N2O2S]

The crystal structure of [C₁₂H₁₄N₂O₂S]SeO₄ · [C₁₂H₁₂N₂O₂S] was determined by X-ray diffraction on single crystal. Crystals are orthorhombic, space group Pbca, with cell parameters a = 11.545 (1), b = 8.143 (1), c = 55.783(1)Å, V = 5244.2 (8)ų and Z = 8. The structure can be described as organic layers built by [C₁₂H₁₄N₂O₂S]²⁺ cations and [C₁₂H₁₂N₂O₂S] molecules, parallel to ab plane, between which the inorganic groups SeO ₄ ^2? are inserted. In this atomic arrangement, H-bonds between the different species play an important role in the three-dimensional network cohesion.     

Crystal and molecular structure of [Cu2(3,5-dihydroxybenzoate)4 (acetonitrile)2] ⋅ 8H2O

The crystal and molecular structure of the title compound, [Cu₂(3,5-dihydroxybenzoate)₄ (acetonitrile)₂] 8H₂O 1, is reported. Crystal data for 1: tetragonal, space group I 4/m, a = 11.720(2) Å, c = 15.304(3) Å, V = 2102.4(6), and D _c = 1.53 g/cm³, for Z = 2. The metal and organic components crystallize to form a Cu paddle-wheel complex, of idealized D_4h symmetry, that assembles in the solid-state, along with eight equivalents of water, to form a 3D hydrogen-bonded network held together by O–H O hydrogens bonds. The metal complexes pack to form a 2D layered structure.     

The crystal structure and supramolecular chain of [La(NO3)3(OH2)2(phen)] ⊙ 15-crown-5

[La(NO₃)₃(OH₂)₂(phen)] · 15-crown-5 is hexagonal,P6₅, witha=10.955(2),c=43.769(9), andD _calc =1.668 g cm^–3 for Z=6. In the complex, two nitrogen atoms (from phen) and eight oxygen atoms (six from three bidentate nitrate anions and two from water molecules) are coordinated to the central La(III) ion, forming a coordination polyhedron which is approximately a bicapped square antiprism. The coordinated water molecules donate hydrogen bonds to the oxygen atoms of the crown ether, forming polymeric hydrogen bonded chains which wrap helically along the unit cell directionc.     

Synthesis and crystal structure of (+)-(2R,3R)-N, N′-bis-trityl-2,3-bis-aziridine

A new C₂ symmetric bis-aziridine derivative was synthesized starting from L-(+)-tartaric acid. The molecular structure of (+)-(2R, 3R)-N, N-bis-trityl-2,3-bis-aziridine 4, was determined by ¹H, ¹³C NMR and elemental analysis and was confirmed by single-crystal X-ray diffraction. Crystal data for 4: C₄₂H₃₆N₂, orthorhombic, space group: P2₁2₁2₁, a = 12.7633(14), b = 14.5661(6), c = 17.4184(14) Å, and Z = 4.     

Crystal and molecular structure of 1-chloro-1,2-benziodoxolin-3(1H)-one·tetra-n-butylammonium chloride

The title compound,6, a novel 11 complex of 1-chloro-1,2-benziodoxolin-3(1H)-one (5) andtetra-n-butylammonium chloride, was prepared from tetra-n-butylammoniumo-iodoxybenzoate (7) and acetyl chloride. A single crystal of6 was subjected to X-ray analysis: triclinic, space group a=10.239(2),b=11.518(2),c=11.523(3)Å; =73.20(2); =87.85(2), =87.72(2)°; R1=0.0326. The most notable structural feature of crystalline6 is the existence of a secondary bond [I· ·Cl(2), 2.943(1)Å] between the chloride ion and the iodine atom of the chlorobenziodoxolinone moiety. Further coordination at iodine includes three primary bonds: I–C [2.115(4) Å], I–O [2.145(3) Å], I–Cl(1) [2.454(1) Å]. The entire 1-chlorobenziodoxolinone-chloride sub-structure is planar and exhibits iodine-centered bond angles of 78.8(1)° [C–I–O], 92.0(1)° [C–I–Cl(1)], 97.6(1)° [Cl(2)–I–O] and 91.6(1)° [Cl(2)–I–Cl(1)]. The unit cell of6 contains two loosely packed formula units. The chlorobenziodoxolinone-chloride sub-structures occupy a common plane and exhibit a centrosymmetric relationship, while the tetra-n-butylammonium ions are situated one above and one below the plane. Bonding at the iodine atom in6 is more consistent with a 10-I-3 species electrostatically associated with the chloride ion than a 12-I-4 species such as the tetrachloroiodate ion.