Chlorido-(2-{(2-hy-droxy-eth-yl)[tris-(hy-droxy-meth-yl)meth-yl]amino}-ethano-lato-κ ,,','',''')copper(II).

The title complex, [Cu(CHNO)Cl] or [Cu(Hbis-tris-)Cl], was obtained starting from the previously reported [Cu(Hbis-tris-)Cl]Cl compound. The deprotonation of the amino-polyol ligand Hbis-tris {[bis-(2-hy-droxy-eth-yl)amino]-tris-(hy-droxy-meth-yl)methane, CHNO} promotes the formation of a very strong O-H⋯O inter-molecular hydrogen bond, characterized by an H⋯O separation of 1.553 (19) Å and an O-H⋯O angle of 178 (4)°.

-Di-chlorido-bis-(secnidazole-κ )copper(II).

The use of acetic acid (HOAc) in a reaction between CuCl·2HO and secnid-azole, an active pharmaceutical ingredient useful in the treatment against a variety of anaerobic Gram-positive and Gram-negative bacteria, affords the title complex, [CuCl(CHNO)]. This compound was previously synthesized using ethanol as solvent, although its crystal structure was not reported [Betanzos-Lara (2013 ▸). , , 94-100].

Methyl -{(1)-2-[(meth-oxy-carbon-yl)-oxy]-1-phenyleth-yl}carbamate.

The title mol-ecule, CHNO, is a methyl carbamate derivative obtained by reacting ()-2-phenyl-glycinol and methyl chloro-formate, with calcium hydroxide as heterogeneous catalyst. Supra-molecular chains are formed in the [100] direction, based on N-H⋯O hydrogen bonds between the amide and carboxyl-ate groups. These chains weakly inter-act in the crystal, and the phenyl rings do not display significant π-π inter-actions.

2-[3-(1-Benzimidazol-2-yl)prop-yl]-1-benzimidazol-3-ium 3,4,5-tri-hydroxy-benzoate-1,3-bis-(1-benzimidazol-2-yl)propane-ethyl acetate (2/1/2.94): co-crystallization between a salt, a neutral mol-ecule and a solvent.

The chemical formula of the title compound, 2CHN ·2CHO ·CHN·2.94CHO, was established by X-ray diffraction of a single-crystal obtained by reacting 1,3-bis-(benzimidazol-2-yl)propane () and gallic acid (HGal) in ethyl acetate. The mol-ecular structure can be described as a salt (H)(Gal) co-crystallized with a mol-ecule , with a stoichiometric relation of 2:1.

Meloxicam hydro-chloride.

The title salt, CHNOS ·Cl [systematic name: 2-(4-hy-droxy-2-methyl-1,1-dioxo-1,2-benzo-thia-zine-3-amido)-5-methyl-1,3-thia-zol-3-ium chloride] is the hydro-chloride derivative of meloxicam, a drug used to treat pain and inflammation in rheumatic disorders and osteoarthritis. Although its mol-ecular structure is similar to that previously reported for the hydro-bromide analogue, both salts are not isomorphous. Different crystal structures originate from a conformational modification, arising from a degree of rotational freedom for the thia-zolium ring in the cations.

Cyclo-hexane plastic phase I: single-crystal diffraction images and new structural model.

The plastic phase of cyclohexane (polymorph I) was studied by Kahn and co-workers, without achieving a satisfactory determination of the atomic coord-inates [Kahn (1973). . B, 131-138].

(23,23 ,25)-23,26-Ep-oxy-23-ethyl-furost-20(22)-en-3β-ol.

The title compound, CHO, is a steroid synthesized through a rearrangement of a sarsasapogenin derivative in acidic medium. The newly formed ring is a tetra-hydro-2-pyran heterocycle substituted by two methyl groups placed in equatorial positions. This ring displays a chair conformation, while di-hydro-furan ring , to which it is bonded, has an envelope conformation.

1,4-Phenyl-ene diallyl bis-(carbonate).

The title mol-ecule, CHO, is based on a benzene core di-substituted by allyl carbonate groups in the positions. The mol-ecule is placed on an inversion centre, and the substituents are twisted with respect to the central benzene ring plane. The crystal structure does not include significant inter-molecular inter-actions other than weak C-H⋯O contacts between CH groups in the benzene ring and carbonate O atoms.

Synthesis and topology analysis of chlorido-triphen-yl(triphenyl phosphate-κ)tin(IV).

The title Sn complex, [Sn(CH)Cl(CHOP)], is a formal adduct between triphenyl phosphate (PhO)P=O and the stannane derivative chlorido-tri-phenyl-tin, SnPhCl. The structure refinement reveals that this mol-ecule displays the largest Sn-O bond length for compounds including the =O→SnPhCl fragment ( = P, S, C, or V), 2.6644 (17) Å.

Bis{[amino-(iminium-yl)meth-yl]urea} tetra-kis-{2-[(di-methyl-amino)(iminium-yl)meth-yl]guanidine} di-μ-oxido-tetra-μ-oxido-tetra-deca-μ-oxido-octa-oxidodeca-vanadium(V) tetra-hydrate.

The title compound, (CHN)(CHNO)[VO]·4HO, is a by-product obtained by reacting ammonium metavanadate(V), metformin hydro-chloride and acetic acid in the presence of sodium hypochlorite, at pH = 5. The crystal structure comprises a deca-vanadate(V) anion (VO) lying on an inversion centre in space group , while cations and solvent water mol-ecules are placed in general positions, surrounding the anion, and forming numerous N-H⋯O and O-H⋯O hydrogen bonds. Metforminium (CHN) and guanylurea (CHNO) cations display the expected shape.

Bis(4-hy-droxy-phen-yl) 1,4-phenyl-enebiscarbamate.

The title compound, CHNO (systematic name: 4-hy-droxy-phenyl -{4-[(4-hy-droxy-phen-oxy-carbon-yl)amino]-phen-yl}carbamate), contains two urethane groups substituting the central benzene ring in positions. The mol-ecule is centrosymmetric, and displays a twisted conformation for the three aromatic rings [the dihedral angle between central benzene ring and the urethane group is 33.4 (6)°, and that between the latter and the terminal ring is 65.

Concomitant dimorphism in poly[di-μ-azido-(5,5'-dimethyl-2,2'-bipyridine)iron(II)].

The title metal-organic polymer, catena-poly[[(5,5'-dimethyl-2,2'-bipyridine-κN,N')iron(II)]-di-μ-azido-κN:N-[(5,5'-dimethyl-2,2'-bipyridine-κN,N')iron(II)]-di-μ-azido-κN:N], [Fe(N)(CHN)], features alternating μ-1,1 (end-on mode of coordination) and μ-1,3 (end-to-end mode of coordination) double azide bridges, forming chains running in the [100] direction. The octahedral coordination geometry around the Fe centre is completed by a bidentate 5,5'-dimethyl-2,2'-bipyridine ligand. Two polymorphs for this compound were obtained from the crude reaction product, the first in the space group P-1 and the other in P2/c.

Diastereoselective synthesis of new zwitterionic bicyclic lactams, scaffolds for construction of 2-substituted-4-hydroxy piperidine and its pipecolic acid derivatives.

The synthesis of new chiral highly functionalized zwitterionic bicyclic lactams starting from acyclic β-enaminoesters derived from ()-(-)-2-phenylglycinol is described. The key step involved an intramolecular non-classical Corey-Chaykovsky ring-closing reaction of the corresponding sulfonium salts derived from β-enaminoesters. This methodology permits the generation of two or three new stereogenic centers with high diastereoselectivity.

Refinement of K[HgI]·HO using non-spherical atomic form factors.

The crystal structure model for potassium tri-iodido-mercurate(II) monohydrate, K[HgI]·HO, based on single-crystal data, was reported 50 years ago [Nyqvist & Johansson (1971 ▸). . , 1615-1629].

Stereoselective synthesis of (26R)-26-hydroxydiosgenin and its effect on the regulation of rat ovarian function.

The stereoselective cyclization of a C-16 acetylated 22,26-dioxocholestene derivative to give the spirostane E and F rings, under alkaline conditions, yields exclusively the (26R)-26-hydroxydiosgenin. Both experimental and computational data support the formation of a single diastereoisomer. The effect of diosgenin and (26R)-26-hydroxydiosgenin on rat ovary is also investigated.

,'-Di-cyclo-hexyl--(phthaloylglyc-yl)urea.

The mol-ecular structure of the title compound {systematic name: 1,3-di-cyclo-hexyl-1-[2-(1,3-dioxo-2,3-di-hydro-1-isoindol-2-yl)acet-yl]urea}, CHNO, derived from ,'-di-cyclo-hexyl-urea, shows that the tertiary N atom substituted by a cyclo-hexyl and phthaloylglycyl groups adopts a perfectly planar geometry (bond-angle sum = 360.0°). In the same way as for ,'-di-cyclo-hexyl-urea, the extended structure of the title compound features N-H⋯O hydrogen bonds, which generate chains of mol-ecules running in the [001] direction.

Tetra-ammonium bis-(metforminium) di-μ-oxido-tetra-μ-oxido-tetra-deca-μ-oxido-octa-oxidodeca-vanadium(V) hexa-hydrate.

The title compound, (NH)(CHN)[VO]·6HO, crystallizes with the deca-vanadate anion placed on an inversion centre in space group . This anion is surrounded by a first shell of ammonium cations and water mol-ecules, forming efficient N-H⋯O and O-H⋯O hydrogen bonds. A second shell includes metforminium monocations with a twisted geometry, also forming numerous inter-molecular hydrogen bonds.

-Hydroboration-oxidation products in Δ-steroids a hydroboration--hydroboration mechanism.

Herein, we report for the first time a "-hydroboration-oxidation product" isolated and characterized under traditional hydroboration-oxidation conditions using cholesterol and diosgenin as substrates. These substrates are excellent starting materials because of the rigidity and different structural environments around the double bond. Further investigations based on experimental evidence, in conjunction with theoretical studies, indicate that the formation of this -species occurs a -hydroboration of the major product to generate the corresponding Δ-structure and the subsequent hydroboration by the β-face.

Structure and NMR properties of the dinuclear complex di-μ-azido-κ : -bis-[(azido-κ)(pyridine-2-carboxamide-κ ,)zinc(II)].

The new diamagnetic complex, [Zn(N)(CHNO)] or [Zn(pca)(μ-N)(N)] was synthesized using pyridine-2-carboxamide (pca) and azido ligands, and characterized using various techniques: IR spectroscopy and single-crystal X-ray diffraction in the solid state, and nuclear magnetic resonance (NMR) in solution. The mol-ecule is placed on an inversion centre in space group . The pca ligand chelates the metal centre the pyridine N atom and the carbonyl O atom.

Crystal structure of a new hydrate form of the NSAID sodium diclofenac.

The crystal structure is reported of sodium 2-[2-(2,6-di-chloro-anilino)phen-yl]acetate 3.5-hydrate or tetra-μ-aqua-κ :-deca-aqua-bis-{μ-2-[2-(2,6-di-chloro-anilino)phen-yl]acetato-κ ::}tetra-sodium(I) bis-{2-[2-(2,6-di-chloro-anil-ino)phen-yl]acetate}, {[Na(CHClNO)(HO)](CHClNO)} , which re-presents a new hydrate form of the NSAID sodium diclofenac (SD). The triclinic unit cell contains one ionic compound with formula Na(CHClNO)(HO), in which two symmetry-related carboxyl-ate anions CHClNO are bonded to a centrosymmetric [Na] core cationic cluster, while the others are only hydrogen bonded to the cationic cluster.

Azasteroids from diosgenin: Synthesis and evaluation of their antiproliferative activity.

In this work, we report the synthesis of two new azasteroids through the modification of the A and B rings of diosgenin 1. The 4-azasteroid derivative 12 was prepared in three steps using the α,β-insaturated-3-keto compound 11 as a precursor, which was first oxidized with KMnO/KIO followed by an oxidative cleavage of ring A, and subsequently cyclized with an ammonium salt, under focused microwave irradiation for a short time of 3 min. A second azasteroid was synthesized, for which the key step was the Beckmann rearrangement of ring B of the oxime 16, affording the lactam-type enamide 17 in good yield.

Diosgenin-3,6-dione: second polymorph in space group 222.

The title steroid, [(25)-spirost-4-en-3,6-dione, CHO], is obtained by oxidation of diosgenin, using the Jones reagent (CrO/HSO). The crystal structure was previously reported in space group 222, but nonetheless with the wrong absolute configuration and omitting positions for H atoms [Rajnikant (2000 ▸). , , 101-110].

One mol-ecule, three crystal structures: conformational trimorphism of -[(1)-1-phenyl-eth-yl]benzamide.

The title compound, CHNO, is an enanti-opure small mol-ecule, which has been synthesized many times, although its crystal structure was never determined. By recrystallization from a variety of solvent mixtures (pure aceto-nitrile, ethanol-water, toluene-ethanol, THF-methanol), we obtained three unsolvated polymorphs, in space groups 2 and 222. Form is obtained from aceto-nitrile, without admixture of other forms, whereas forms and are obtained simultaneously by concomitant crystallizations from alcohol-based solvent mixtures.

Ethyl (3)-3-[(3a,5,6,6a)-6-hy-droxy-2,2-di-methyl-tetra-hydro-furo[4,5-][1,3]dioxol-5-yl]-3-{(3)-3-[(3a,5,6,6a)-6-hy-droxy-2,2-di-methyl-tetra-hydro-furo[4,5-][1,3]dioxol-5-yl]-5-oxoisoxazolidin-2-yl}propano-ate chloro-form monosolvate.

The title compound, CHNO·CHCl, was obtained as a product of a double aza-Michael addition of hydroxyl-amine on a Chiron with a known absolute configuration. The enanti-opure compound crystallized as a chloro-form solvate, in space group 1, and diffraction data were collected at room temperature with Ag α radiation. The Flack parameter refined to = -0.

Redetermination of di-ammonium trivanadate, (NH)VO.

The crystal structure of (NH)VO has been reported twice using single-crystal X-ray data [Theobald (1984 ▸). , , 581-587; Range (1988 ▸). , , 309-317].