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58 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3, 4, 5, 6 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I11-High Resolution Powder Diffraction	Influence of crystal packing on the mechanism of decomposition of the acetonitrile-solvated co-crystal of piroxicam and succinic acid Xiaojiao Liu , Chiu C. Tang , Elena V. Boldyreva , Colin R. Pulham Crystal Growth & Design DOI: 10.1021/acs.cgd.9b01189 Diamond Proposal Number(s): [20626] Show Abstract ▼ Abstract: Variable-temperature single-crystal and powder X-ray diffraction techniques have been used to study the thermal and mechanical decomposition of the acetonitrile solvate of the co-crystal formed between piroxicam and succinic acid (PRXSA-ACN). The results show that the thermal expansion behavior of PRXSA-ACN is highly anisotropic and can be correlated with structural features of the crystal lattice. Thermally-induced desolvation of PRXSA-ACN led initially to the formation of the α-form of piroxicam and the 1:1 piroxicam:succinic acid co-crystal (PRXSA), and this can be rationalized on the basis of the crystal structure of PRXSA-ACN and its thermal expansion behavior. Subsequent decomposition of PRXSA produced amorphous succinic acid and the thermodynamically more stable β-form of piroxicam. The α- and β-forms co-existed up until the melting point of the α-form, at which point the sample recrystallized to give the β-form of piroxicam. Mechanical treatment (light grinding) of PRXSA-ACN resulted in mild structural damage to the crystal structure and this led to subsequent desolvation.	Nov 2019
I11-High Resolution Powder Diffraction I19-Small Molecule Single Crystal Diffraction	The anisotropic responses of a flexible metal-organic framework constructed from asymmetric flexible linkers and heptanuclear zinc carboxylate secondary building units Elliot J. Carrington , Rémi Pétuya , Rebecca K. Hylton , Yong Yan , Dmytro Antypov , George R. Darling , Matthew S. Dyer , Neil G. Berry , Alexandros P. Katsoulidis , Matthew Rosseinsky Crystal Growth & Design DOI: 10.1021/acs.cgd.9b00558 Show Abstract ▼ Abstract: A new porous and flexible metal-organic framework (MOF) has been synthesised from the flexible asymmetric linker N-(4-Carboxyphenyl)succinamate (CSA) and heptanuclear zinc oxo-clusters of formula [Zn7O2(Carboxylate)10DMF2] involving two coordinated terminal DMF ligands. The structural response of this MOF to the removal or exchange of its guest molecules has been probed using a combination of experimental and computational approaches. The topology of the material, involving double linker connections in the a and b directions and single linker connections along the c axis, is shown to be key in the materials anisotropic response. The a and b directions remain locked during guest removal, while the c axis linker undergoes large changes significantly reducing the material’s void space. The changes to the c axis linker involve a combination of a hinge motion on the linker’s rigid side and conformational rearrangements on its flexible end, which were probed in detail during this process despite the presence of crystallographic disorder along this axis which prevented accurate characterisation by experimental methods alone. While inactive during guest removal, the flexible ends of the a and b axis linkers are observed to play a prominent role during DMF to DMSO solvent exchange, facilitating the exchange reaction arising in the cluster.	Aug 2019
I12-JEEP: Joint Engineering, Environmental and Processing	New pharmaceutical cocrystal forms of flurbiprofen: structural, physicochemical and thermodynamic characterization Artem O. Surov , Alex N. Manin , Alexander P. Voronin , Denis Boycov , Oxana V. Magdysyuk , German L. Perlovich Crystal Growth & Design DOI: 10.1021/acs.cgd.9b00781 Show Abstract ▼ Abstract: In this work, three new cocrystals of the nonsteroidal anti-inflammatory drug flurbiprofen with salicylamide, benzamide and picolinamide have been discovered using thermodynamic analysis of solid-liquid binary phase diagrams, and their crystal structures have been determined from the high-resolution synchrotron powder diffraction data. Solid state DFT calculations have been carried out to gain additional insight into energy differences between the cocrystal structures. The pH-solubility behavior and solubility advantage of the cocrystals have been examined via eutectic concentrations of the components, and the thermodynamic stability relationships between different solid phases have been rationalized in terms of Gibbs energies of the formation reactions. In addition, a new model has been proposed for estimating the solubility product (Ksp) of a cocrystal, based on the experimental intrinsic solubility of the drug and coformer complemented by calculated physicochemical HYBOT descriptors. The applicability of the molecular volume of cocrystal formation as a reliable parameter for clarifying the relationship between the driving force of the cocrystallization process and the structural features of participating solids has been also discussed.	Aug 2019
I19-Small Molecule Single Crystal Diffraction	Synthesis of a large, shape-flexible, solvatomorphic porous organic cage Baiyang Teng , Marc A. Little , Tom Hasell , Samantha Y. Chong , Kim E. Jelfs , Michael E. Briggs , Andrew I. Cooper Crystal Growth & Design DOI: 10.1021/acs.cgd.8b01761 Diamond Proposal Number(s): [15777] Show Abstract ▼ Abstract: Porous organic cages have emerged over the last 10 years as a subclass of functional microporous materials. However, among all of the organic cages published, large multicomponent organic cages with 20 components or more are still rare. Here, we present an [8+12] porous organic imine cage, CC20, which has an apparent surface area up to 1752 m2 g-1, depending on the crystallization and activation conditions. The cage is solvatomorphic and displays distinct geometrical cage structures, caused by crystal packing ef-fects, in its crystal structures. This indicates that larger cages can display a certain range of shape flexibility in the solid state, while remaining shape persistent and porous.	May 2019
	Temperature-dependent structural properties, phase transition behaviour and dynamic properties of a benzene derivative in the solid state Yating Zhou , Rhian Patterson , P. Andrew Williams , Benson M. Kariuki , Colan E. Hughes , Ranita Samanta , Ramesh Devarapalli , C. Malla Reddy , David C. Apperley , Kenneth D. M. Harris Crystal Growth & Design DOI: 10.1021/acs.cgd.8b01775 Show Abstract ▼ Abstract: We report the solid-state structural properties and phase transition behaviour of 1,4-dibromo-2,3,5,6-tetramethylbenzene, demonstrating that this material undergoes an order-disorder phase transition below ambient temperature (at ca. 156 K on cooling and ca. 159 K on heating). In both the high-temperature and low-temperature phases, the crystal structure is based on π-stacking of the molecules. In the high-temperature phase, the bromine and methyl groups are located with essentially equal probability in each of the six substituent positions, and it is shown by natural-abundance solid-state 2H NMR spectroscopy that, at ambient temperature, this disorder is dynamic via rapid molecular reorientation about an axis perpendicular to the aromatic ring. In the low-temperature phase, the bromine and methyl substituents occupy preferred sites within the crystal structure, with the distribution of site occupancies becoming progressively more ordered on decreasing temperature.	Mar 2019
I12-JEEP: Joint Engineering, Environmental and Processing	Olanzapine form IV: discovery of a new polymorphic form enabled by computed crystal energy landscapes Sean Askin , Jeremy K. Cockcroft , Louise S. Price , Andrea Goncalves , Min Zhao , Derek A. Tocher , Gareth R. Williams , Simon Gaisford , Duncan Q. M. Craig Crystal Growth & Design DOI: 10.1021/acs.cgd.8b01881 Diamond Proposal Number(s): [17450] Show Abstract ▼ Abstract: Olanzapine is a polymorphic drug molecule that has been extensively studied, with over 60 structures reported in the Cambridge Structural Database. All anhydrous and solvated forms of olanzapine known to date contain the SC0 dimer packing motif. In this study, a new screening approach was adopted involving heat-induced forced crystallization from a polymer-based molecular dispersion of olanzapine. Simultaneous differential scanning calorimetry-powder X-ray diffraction (DSC-PXRD) was used to heat the amorphous dispersion and to identify a novel physical form from diffraction and heat flow data. Comparison of the diffraction data with those from a computed crystal energy landscape allowed the crystal structure to be determined. The result was the discovery of a new polymorph, form IV, which does not use the SC0 motif. Hence, while dimer formation is the dominant process that defines crystal packing for olanzapine formed from solution, it seems that molecularly dispersing the drug in a polymeric ma-trix permits crystallization of alternative motifs. Having identified form IV, it proved possible to scale up the synthesis and demonstrate its enhanced dissolution properties over form I.	Mar 2019
I19-Small Molecule Single Crystal Diffraction	Metal–organic frameworks constructed from Group 1 metals (Li, Na) and silicon-centered linkers David Pugh , Emma Ashworth , Karen Robertson , Luke C. Delmas , Andrew J. P. White , Peter N. Horton , Graham J. Tizzard , Simon J. Coles , Paul D. Lickiss , Robert P. Davies Crystal Growth & Design 19, 487 - 497 DOI: 10.1021/acs.cgd.8b01567 Diamond Proposal Number(s): [2871] Show Abstract ▼ Abstract: A series of “light metal” metal–organic frameworks containing secondary building units (SBUs) based on Li+ and Na+ cations have been prepared using the silicon-centered linkers MexSi(p-C6H4CO2H)4-x (x = 2, 1, 0). The unipositive charge, small size, and oxophilic nature of the metal cations give rise to some unusual and unique SBUs, including a three-dimensional nodal structure built from sodium and oxygen ions when using the triacid linker (x = 1). The same linker with Li+ cations generated a chiral, helical SBU, formed from achiral starting materials. One-dimensional rod SBUs are observed for the diacid (x = 2) and tetra-acid (x = 0) linkers with both Li+ and Na+ cations, where the larger size of Na+ compared to Li+ leads to subtle differences in the constitution of the metal nodes.	Nov 2018
I22-Small angle scattering & Diffraction	Nanoparticle assembly leads to mackinawite formation Adriana Matamoros-veloza , Tomasz M. Stawski , Liane G. Benning Crystal Growth & Design DOI: 10.1021/acs.cgd.8b01025 Diamond Proposal Number(s): [8973] Show Abstract ▼ Abstract: Iron sufides are important mineral phases in natural environments where they control global elemental cycles. Fe-S phases have been suggested to form through transformation of several possible precursors to finally reach stable crystalline structures. Mackinawite is a metastable intermediate, of which a full chemical and structural characteristisation of various possible intermediate stages in its formation pathways, or the chemical conditions that affect the transformations to the metastable mackinawite are well understood. Here we report, the various steps of mackinawite formation via oriented aggregation (OA) from a nanoparticulate precursor. During OA, the formation of aggregates is a crucial stage for self-assembly of primary particles to reach stable structures. The formation occurs in five steps: (1) homogeneous nucleation of primary FeSnano particles, (2 and 3) formation of mass fractal-like aggregates from the FeSnano as precursor towards the transformation to mackinawite; (4) oriented alignment and self-assembly of these mackinawite-like aggregates, and (5) transformation to a still metastable but typical layered mackinawite structure.	Sep 2018
I04-Macromolecular Crystallography	Hydrogel Composite Membranes Incorporating Iron Oxide Nanoparticles as Topographical Designers for Controlled Heteronucleation of Proteins Shabnam Majidi Salehi , Ana C. Manjua , Benny D. Belviso , Carla A. M. Portugal , Isabel M. Coelhoso , Valentina Mirabelli , Enrica Fontananova , Rocco Caliandro , João G. Crespo , Efrem Curcio , Gianluca Di Profio Crystal Growth & Design DOI: 10.1021/acs.cgd.7b01760 Diamond Proposal Number(s): [15832] Show Abstract ▼ Abstract: In this study, we exploited the possibility of tuning physical–chemical properties of hydrogel composite membranes (HCMs) surfaces, by using iron oxide nanoparticles (NPs) as topographical designers, with the aim of examining the effect of surface topography and wettability on the heterogeneous nucleation of protein crystals. On the basis of roughness and contact angle measurements, it was found that surface structural characteristics, in addition to chemical interactions between the surface and protein molecules, have influence on the heterogeneous nucleation of lysozyme and thermolysin crystals to different extents. We demonstrated that increasing the amount of NPs incorporated in the hydrogel matrix promotes protein nucleation to a higher extent, potentially due to the increase of local solute concentration, arising from the enhanced wetting tendency in the Wenzel regime, and physical confinement at rougher hydrophilic surfaces. An extensive crystallographic analysis suggested the tendency of the growing crystals to incorporate hydrogel materials, which allows inducement of protein conformational states slightly different from those covered by standard crystallization methods. Protein flexibility can be thus sampled by changing the amount of NPs in the HCMs, with negligible influence on the quantity and quality of X-ray diffraction data.	May 2018
I18-Microfocus Spectroscopy	Characterization of the structural environment of dithionate ions associated with their role in the crystal habit modification of sodium chlorate Zhipeng Lan , Guilherme A. Calligaris , Alan S. De Menezes , Adenilson O. Dos Santos , Xiaojun Lai , Lisandro P. Cardoso , Kevin J. Roberts Crystal Growth & Design DOI: 10.1021/acs.cgd.7b01770 Show Abstract ▼ Abstract: Sodium chlorate (NaClO3) crystals change from a cuboid to a tetrahedron of {1 ̅1 ̅1 ̅} morphology when crystallized in the presence of sodium dithionate (Na2S2O6) impurity. Polarized Extended X-Ray Absorption Fine Structure at the S K-edge, used to probe the local structure around this impurity with respect to its orientation within the bulk crystal lattice, reveals that the S-S bond of the S2O62- ions is closely aligned along the <111>/<1 ̅1 ̅1 ̅> lattice direction. High resolution diffraction studies using X-ray Multiple Diffraction reveal growth-induced anisotropy in the doped crystals associated with subtle lattice distortions in the symmetry-independent {1 ̅1 ̅1 ̅} and {111} growth sectors. The data is consistent with a mechanistic model involving creation of lattice vacancies and the substitution of one of the SO3 anionic groups of the dopant ion for a host ClO3 ion when incorporated at the {1 ̅1 ̅1 ̅} growth interface with the other SO3 group substituting for one or more anionic sites in the succeeding growth layer depending on the degree of impurity concentration within the crystallization solution. This mechanism is also fully consistent with the formation of twinning at higher impurity concentrations previously reported by Lan et.al.	May 2018

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