Cocoa butter equivalent from Kpangnan butter and Pequi oil

Novel cocoa butter equivalents were designed using dry fractionated Pequi oil and solvent fractionated Kpangnan butter. Static crystallization of binary mixtures of these two fractions into the triclinic form (β2) was achieved after 12 days for all mixtures and after 4 days for the 80:20 w/w and 90:10 w/w fractionated Kpangnan:Pequi oil mixtures. Moreover, after 60 days of storage at 22oC, all binary blends (except 100% fractionated pequi oil and 100% fractionated Kpangnan butter) were crystallized in the most stable triclinic crystal form (β1). Here we also discovered an unusual melting behavior for the fractionaled 30:70 w/w and 20:80 w/w fractionated Kpangnan:Pequi oil mixtures, where after 4 days of static crystallization at room 22oC, these mixtures displayed higher than predicted melting points, 41.89 oC and 33.32 oC, respectively. This suggested a faster kinetics of transformation to the triclinic β2 form for those mixtures. Our results suggest that the 30:70 w/w fractionated Kpangnan:Pequi oil mixture with a melting point of 34oC after 60 days storage at 22oC, a stable triclinic β2 form, and a triglyceride composition of 28% POP, 4.6% POS and 33% SOS displayed solid state characteristics, melting point and crystal structure, of a commercial cocoa butter equivalent.

Analysis of slip systems in protein crystals with triclinic form using the phenomenological macro-bond method

Slip systems in triclinic hen egg-white lysozyme (Tri-HEWL) crystals, which is one of typical protein crystals, were identified by the indentation method. Eleven kinds of the slip systems are clearly...

Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κS)(triphenylphosphane-κP)osmium(IV): a monoclinic polymorph

The structure of the title compound, [Os(C6HF4S)4{P(C6H5)3}], has been previously reported [Arroyo et al. (1994). J. Chem. Soc. Dalton Trans. pp. 1819–1824], in the space group P\overline{1}. We have now obtained a monoclinic polymorph for this compound, crystallized from ethanol, while the previous form was obtained from a hexane/chloroform mixture. The molecular structure is based on a trigonal–bipyramidal OsIV coordination geometry, close to that observed previously in the triclinic form.

A new crystalline form of αβ-D-lactose prepared by oven drying a concentrated aqueous solution of D-lactose

A new crystalline form of αβ-D-lactose (C12H22O11) has been prepared by the rapid drying of an approximately 40% w/v syrup of D-lactose. Initially identified from its novel powder X-ray diffraction pattern, the monoclinic crystal structure was solved from a microcrystal recovered from the generally polycrystalline mixed-phase residue obtained at the end of the drying step. This is the second crystalline form of αβ-D-lactose to be identified and it has a high degree of structural three-dimensional similarity to the previously identified triclinic form.

Polymorphic modifications of a 1H-pyrrolo[3,2,1-ij]quinoline-5-carboxamide possessing strong diuretic properties

6-Hydroxy-N-(4-methoxyphenyl)-4-oxo-2,4-dihydro-1H-pyrrolo[3,2,1-ij]quinoline-5-carboxamide, C19H16N2O4, possesses strong diuretic properties and can be used as a new hypertension remedy. Two polymorphic modifications of this compound have been found, namely the triclinic polymorph (space group P\overline{1}), with one molecule in the asymmetric unit, and the monoclinic polymorph (space group P21/n), with two molecules in asymmetric unit. An analysis of the pairwise interaction energies between the molecules in the crystal phase revealed differences in the crystal packing. The triclinic form has only one level of organization, namely a chain/column, while the monoclinic form has two levels of organization, with a chain/column as the primary basic structural motif and a layer as the secondary basic structural motif.

Design, synthesis and crystallographic study of novel indole-based cyano derivatives as key building blocks for heteropolycyclic compounds of major complexity

A four-stage reaction sequence has been designed and developed for the synthesis of highly functionalized enolate esters as key building blocks for the synthesis of novel heteropolycyclic compounds of potential pharmaceutical value. The sequence starts with simple commercially available indoles and proceeds via 3-(indol-3-yl)-3-oxopropanenitriles, which react with 2-bromobenzaldehyde to form the corresponding chalcones; these are readily reduced to dihydrochalcones, which are in turn acylated to form the enolate esters. The compounds in this sequence have been characterized by IR and 1H and 13C NMR spectroscopy, by mass spectrometry and by elemental analysis. The molecular and supramolecular structures are reported for representative examples, namely (E)-3-(2-bromophenyl)-2-(1-methyl-1H-indole-3-carbonyl)acrylonitrile, C19H13BrN2O, (Ib), (2RS)-2-(2-bromobenzyl)-3-(1-methyl-1H-indol-3-yl)-3-oxopropanenitrile, C19H15BrN2O, (IIb), and (2RS)-3-(1-benzyl-1H-indol-3-yl)-2-(2-bromobenzyl)-3-oxopropanenitrile, C25H19BrN2O, (IIc), the latter two of which crystallize with Z′ = 2, and (E)-1-(1-acetyl-1H-indol-3-yl)-3-(2-bromophenyl)-2-cyanoprop-1-en-1-yl acetate, C22H17BrN2O, (III), and (E)-1-(1-benzyl-1H-indol-3-yl)-3-(2-bromophenyl)-2-cyanoprop-1-en-1-yl benzoate, C32H23BrN2O, (IV). The structure of the related chalcone (E)-2-benzoyl-3-(2-bromophenyl)prop-2-enenitrile, (V), has been redetermined at 100 K, where it is monoclinic, as opposed to the triclinic form reported at ambient temperature.

A metastable polymorphic form of the antifungal anilinopyrimidine active pyrimethanil

A second metastable form of the title compound, C12H13N3(systematic name: 4,6-dimethyl-N-phenylpyrimidin-2-amine), was isolated from an attempted co-crystallization experiment withmeso-erythriol in dimethyl sulfoxide (DMSO). The crystals of form 2 at 120 K are monoclinic, space groupP21/nwithZ′ = 4 compared to the previously reported triclinic form withZ′ = 2 [Sunet al.(2011).Acta Chim. Sin.69, 1909–1914]. The four independent molecules in the asymmetric unit form two discrete dimeric units through a concerted pair of N—H...N hydrogen bonds with a graph-set notation ofR22(8). The origin of the polymorphic behaviour is revealed in that the conformation of each dimer present in the asymmetric unit of the structure is unique and determined by the rotation of the second molecule in the dimer with respect to the first.

A monoclinic polymorph of [(Z)-N-(3-chlorophenyl)-O-methylthiocarbamato-κS](triphenylphosphane-κP)gold(I): crystal structure and Hirshfeld surface analysis

The title compound, [Au(C8H7ClNOS)(C18H15P)], is a monoclinic (P21/n,Z′ = 1; form β) polymorph of the previously reported triclinic form (P-1,Z′ = 1; form α) [Tadbuppa & Tiekink (2010).Acta Cryst. E66, m664]. The molecular structures of both forms feature an almost linear gold(I) coordination geometry [P—Au—S = 175.62 (5)° in the title polymorph], being coordinated by thiolate S and phosphane P atoms, aZconformation about the C=N bond and an intramolecular Au...O contact. The major conformational difference relates to the relative orientations of the residues about the Au—S bond: the P—Au—S—C torsion angles are −8.4 (7) and 106.2 (7)° in forms α and β, respectively. The molecular packing of form β features centrosymmetric aggregates sustained by aryl-C—H...O interactions, which are connected into a three-dimensional network by aryl-C—H...π contacts. The Hirshfeld analysis of forms α and β shows many similarities with the notable exception of the influence of C—H...O interactions in form β.

A phase transition from monoclinicC2 withZ′ = 1 to triclinicP1 withZ′ = 4 for the quasiracemateL-2-aminobutyric acid–D-methionine (1/1)

Racemates of hydrophobic amino acids with linear side chains are known to undergo a unique series of solid-state phase transitions that involve sliding of molecular bilayers upon heating or cooling. Recently, this behaviour was shown to extend also to quasiracemates of two different amino acids with opposite handedness [Görbitz & Karen (2015).J. Phys. Chem. B,119, 4975–4984]. Previous investigations are here extended to an L-2-aminobutyric acid–D-methionine (1/1) co-crystal, C4H9NO2·C5H11NO2S. The significant difference in size between the –CH2CH3and –CH2CH2SCH3side chains leads to extensive disorder at room temperature, which is essentially resolved after a phase transition at 229 K to an unprecedented triclinic form where all four D-methionine molecules in the asymmetric unit have different side-chain conformations and all three side-chain rotamers are used for the four partner L-2-aminobutyric acid molecules.