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Instruments / Technical Area	Publication Details	Published
I19-Small Molecule Single Crystal Diffraction	Furosemide cocrystals: structures, hydrogen bonding, and implications for properties Bethany I. Harriss , Liana Vella-Zarb , Ivana Radosavljevic Evans , Claire Wilson Crystal Growth & Design 14 (2), 783 - 791 DOI: 10.1021/cg401662d Show Abstract ▼ Abstract: In this paper, we report the crystal growth of four cocrystals of furosemide (4-chloro-2-[(2-furanylmethyl)amino]-5-sulfamoylbenzoic acid), a loop diuretic drug used for the treatment of hypertension and edemas, prepared with p-aminobenzoic acid, nicotinamide, and isonicotinamide as coformers. We present four new crystal structures and elucidate the intermolecular interactions present in the cocrystals. The structures display interesting supramolecular chemistry: a number of different synthons, as well as short strong hydrogen bonds with partial proton transfer and indications of proton disorder. Using powder X-ray diffraction, solid state NMR, and thermal analysis, we provide evidence for the preparation of bulk samples of two compositions, namely, the 1:1 cocrystal of furosemide and p-aminobenzoic acid and 2:1 cocrystal of furosemide and isonicotinamide, highlighting the general necessity of such multitechnique approaches to characterize organic solids (including cocrystals and solvates) prepared by grinding methods. Finally, we correlate the structural features reported for the first time in this work with the previously published pharmacologically relevant properties (solubility and intrinsic dissolution rate) of the furosemide cocrystals.	Feb 2014
I19-Small Molecule Single Crystal Diffraction	Melaminium lanthanide oxalate coordination compounds – synthesis and structural varieties Liana Vella-Zarb , Ulrich Baisch Zeitschrift Für Anorganische Und Allgemeine Chemie 643, 1712 - 1716 DOI: 10.1002/zaac.201700299 Diamond Proposal Number(s): [6749] Show Abstract ▼ Abstract: A crystal engineering approach affords novel crystalline ionic coordination networks occurring in two different compositions. [C3H7N6]6[Ln(C2O4)4][NO3] (1) (Ln = Dy, Ho), which is isostructural to its ytterbium homologue and [C3H7N6][Ln(C2O4)2(H2O)] (2) (Ln = Ce, Gd). The crystal structure of 1 is based on the interaction between isolated monomeric building-blocks of [Ln(C2O4)4]5– and melaminium cations. The melaminium cations form parallel layers, in which the lanthanide oxalato anion is intercalated. On the other hand, 2 consists of a 2D framework of interconnected lanthanide oxalate units with isolated melaminium cations intercalated between the metal complex layers.	Nov 2017
I19-Small Molecule Single Crystal Diffraction	Small molecule, high impact: the role of water in the crystallization of paclitaxel Liana Vella-Zarb , Ulrich Baisch , Robert Dinnebier Journal Of Pharmaceutical Sciences 102 (2), 674-683 DOI: 10.1002/jps.23404 Diamond Proposal Number(s): [6749] Show Abstract ▼ Abstract: Paclitaxel is an important antineoplastic drug, which is used widely in the treatment of many forms of cancer. The crystal structures of the anhydrous form and the hemihydrate were determined from laboratory X-ray powder diffraction data, whereas the dihydrate was solved from single-crystal synchrotron diffraction data. Intermolecular spaces allow for the inclusion of loosely bound water molecules, which are then lost easily upon heating. All three forms were found to crystallize in the orthorhombic spacegroup P212121, with Z′ = 2. The unit cell parameters were found to be a = 9.6530(3) Å, b = 28.1196(8) Å, c = 33.5378(14) Å, and V = 9103.5(5) Å for the anhydrous form (363 K); a = 9.6890(2) Å, b = 28.0760(4) Å, c = 33.6166(8) Å, and V = 9144.7(3) Å3 for the hemihydrate (333 K); and a = 9.512(6) Å, b = 28.064(16) Å, c = 33.08(2) Å, and V = 8829.0(9) Å3 for the dihydrate (120 K). Water loss occurs in two steps between 120 K ≤ t ≤ 363 K. The thermal stability of the hydrates and accompanying unit cell changes were observed in situ via temperature-resolved X-ray powder diffraction and thermogravimetric analysis.	Nov 2012
I19-Small Molecule Single Crystal Diffraction	Systematic and controllable negative, zero, and positive thermal expansion in cubic Zr1–xSnxMo2O8 Sarah Tallentire , Felicity Child , Ian Andrew Fall , Liana Vella-Zarb , Ivana Evans , Matthew G. Tucker , David A. Keen , Claire Wilson , John S. O. Evans Journal Of The American Chemical Society 135 (34) DOI: 10.1021/ja4060564 Show Abstract ▼ Abstract: We describe the synthesis and characterization of a family of materials, Zr1–xSnxMo2O8 (0 < x < 1), whose isotropic thermal expansion coefficient can be systematically varied from negative to zero to positive values. These materials allow tunable expansion in a single phase as opposed to using a composite system. Linear thermal expansion coefficients, αl, ranging from −7.9(2) × 10–6 to +5.9(2) × 10–6 K–1 (12–500 K) can be achieved across the series; contraction and expansion limits are of the same order of magnitude as the expansion of typical ceramics. We also report the various structures and thermal expansion of “cubic” SnMo2O8, and we use time- and temperature-dependent diffraction studies to describe a series of phase transitions between different ordered and disordered states of this material.	Jul 2013
I19-Small Molecule Single Crystal Diffraction	The devil is in the detail: a rare H-bonding motif in new forms of docetaxel Liana Vella-Zarb , Robert E. Dinnebier , Ulrich Baisch Crystal Growth & Design 13 (10), 4402-4410 DOI: 10.1021/cg400814a Diamond Proposal Number(s): [6749] Show Abstract ▼ Abstract: Docetaxel is a semisynthetic analog of the taxane paclitaxel, pivotal for the treatment of various types of cancer. Minor differences in its chemical structure give docetaxel a slightly better water solubility profile when compared to paclitaxel. An understanding of the hydrogen-bonding network in docetaxel is therefore imperative if an explanation for its improved solubility over its predecessor is to be sought. New crystalline forms for solvated (ethanol), hydrated, and anhydrous docetaxel are reported. The crystal structures were determined by single crystal synchrotron and laboratory powder X-ray diffraction experiments on crystalline materials resulting from polymorph screening tests in various solvents. Variable-temperature experiments were carried out over ranges between 20 and 130 °C, with subsequent loss of crystal water at 70 and 90 °C. The resulting structures are discussed in terms of their intermolecular interactions, molecular conformations, and packing motifs. A rare hydrogen-bonding motif, observed between carbamate and tetracyclic ether groups, was found in the packing of all phases of docetaxel. Subtle but significant changes in structural hydrogen bonding motifs are discussed and their differences supported and visualized by Hirshfeld surface calculations and related two-dimensional fingerprint plots.	Sep 2013
I19-Small Molecule Single Crystal Diffraction	Towards understanding P-gp resistance: a case study of the antitumour drug cabazitaxel Ulrich Baisch , Liana Vella-Zarb Crystengcomm 16 (44), 10161-10164 DOI: 10.1039/C4CE01279H Diamond Proposal Number(s): [6749] Show Abstract ▼ Abstract: A detailed structural study and Hirshfeld surface analysis of cabazitaxel in its anhydrous, hydrated and solvated forms have revealed that the three-dimensional architecture of the drug molecule is retained regardless of the crystalline environment. This prompted comparison with its taxane predecessors, suggesting key factors contributing to cabazitaxel's poor affinity to P-gp.	Aug 2014

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