Polymorphism of glycine. Thermodynamic and structural aspects. E. Boldyreva, V. Drebushchak, T. Drebushchak, I. Paukov, Yu. Kovalevskaya, E.
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1 Polymorphism of glycine. Thermodynamic and structural aspects E. Boldyreva, V. Drebushchak, T. Drebushchak, I. Paukov, Yu. Kovalevskaya, E. Shutova
2 Outline Introduction Control of the crystallization of a desirable polymorph A comparative calorimetric study in a wide range of temperatures Polymorphic transitions Effects of temperature and pressure Conclusions
3 Outline Introduction Control of the crystallization of a desirable polymorph A comparative calorimetric study in a wide range of temperatures Polymorphic transitions Effects of temperature and pressure Conclusions
4 The problem of polymorphism: to find experimentally and / or to predict theoretically all the possible polymorphs of a given compound; to range the experimentally known and / or the predicted polymorphs with respect to their thermodynamic stability, their free energies of formation, etc.; to find experimentally and / or to predict, which of the polymorphs will be formed under particular experimental conditions, and to control the formation of the desired polymorph.
5 The relative stability of the polymorphs and the preferable growth of a particular polymorph in real experiments do not necessarily correlate directly. This is a reason, why much confusion and contradictory statements can be found in the literature even for seemingly simple and repeatedly studied systems. Glycine, NH 2 CH 2 COOH, can provide an example.
6 Polymorphs of glycine zwitter-ion
7 Polymorphs of glycine 1,92 1,77 a b c α β γ PowderCell 2.0 b a c PowderCell 2.0 P2 1 /n P2 1 P3 1
8 Outline Introduction Control of the crystallization of a desirable polymorph A comparative calorimetric study in a wide range of temperatures Polymorphic transitions Effects of temperature and pressure Conclusions
9 Solvent Additives of impurities to solution ph of solution Isotope substitution H 2 O D 2 O Temperature Intense nanosecond pulses of near-infrared laser light Humidity Crystallization rate were reported in the literature ( ) to influence on the crystallization of a selected polymorph The literature data were often contradictory and poorly reproducible
10 The chemicals "glycine" could be received from different chemical companies: Soyuzkhimreaktiv (Russia); ICN Biomedicals ( [ ]); Merck (104201); Riedel-de Haen (Sigma-Aldrich Laborchemikalien GmbH). Neither company indicates crystalline polymorph of glycine. Usually, the reagents contain mixture of two polymorphs (α and γ). The polymorph content in different chemicals ranges from α with admixture of γ to γ with admixture of α. Transformations on storage? Quality of tablets (caking).
11 Our results: Polymorphs of glycine = concomitant polymorphs (crystallize simultaneously from the same batch); Crystallization is very sensitive to the "age" of the solution and the presence of the even small impurities of a polymorph in the powder used for preparing the solution; In order to facilitate the crystallization of the β- or the γ-forms, it is necessary to destroy the glycine dimers present in aqueous solutions, which direct crystallization towards the α- form. Then crystallization close to equilibrium conditions (slow) gives the polar γ-form, and a non-equilibrious (rapid) crystallization gives the β-form. We have worked out special procedures of obtaining pure polymorphs in quantities of grams in one crystallization, and this enabled us to carry out a detailed calorimetric study.
12 Outline Introduction Control of the crystallization of a desirable polymorph A comparative calorimetric study in a wide range of temperatures Polymorphic transitions Effects of temperature and pressure Conclusions
13 Crystallization of the polymorphs Relative stability of the polymorphs α glycine: the easiest to crystallize, when obtained, is preserved for indefinitely long time γ - glycine: can be crystallized only under special conditions, when obtained, is preserved for indefinitely long time Which of the two is the stable form at ambient conditions?
14 Heat capacity of the glycine polymorphs (5 K 500 K) DSC-111 (SETARAM) DSC-204 (NETZSCH) DSC-30 (Mettler) 140 K 500 K A low-temperature adiabatic calorimeter 4 K 320 K Sublimation was studied using TG-209 (NETZSCH) X-ray diffraction was studied using Bruker GADDS system (powders) and STOE STADI-4 (single crystals)
15 Heat capacity of the glycine polymorphs (5 K 500 K) The values of heat capacity are close for all the three polymorphs; in the range K the differences do not exceed 3%. C, J p mol K β α γ T, K
16 Relative stability of the glycine polymorphs Ambient temperature: γ > α > β Increased temperature: α > γ > β The difference in the free energy between the three polymorphs is very small (ΔG about J mol -1 for β-α transition, J mol -1 for γ α transition on heating, -325 J mol -1 as estimated for a hypothetical α γ transition at ambient temperature). This explains, why, once formed, the less stable polymorphs can exist at normal conditions for a long time, sometimes for an indefinitely long time. Crystallization of a polymorph is determined by kinetics rather than by thermodynamics.
17 Low-temperature phase transitions in the glycine polymorphs Reversible low-temperature phase transitions were detected for the β- and the γ-polymorphs. C p (α) C p (γ) C p (β)
18 Cell volume & cell parameters changes in the temperature range of the lowtemperature phase transition No kinks at the curves of the changes of cell volume / cell parameters versus temperature could be noticed in the temperature range of the phase transition V, A a, A T, K T, K
19 Outline Introduction Control of the crystallization of a desirable polymorph A comparative calorimetric study in a wide range of temperatures Polymorphic transitions Effects of temperature and pressure Conclusions
20 Polymorphic transformations of the glycine polymorphs on heating Polymorphic transformation β α (exothermic, irreversible) C p ( α) - C p( β), mj/g K β α Δ tr H = 200 J/mol T, K X-ray diffraction has confirmed a complete transformation into the α-form. The transformation was shown to involve the recrystallization of the sample. Optical microscopy has shown the transformation to be heterogeneous; after an induction period an interface propagated rapidly from one face of the crystal to the opposite one.
21 Polymorphic transformations of the glycine polymorphs on heating Polymorphic transformation γ α (endothermic, irreversible) X-ray diffraction has confirmed a transformation into the α-form. The transition temperatures were different for powder (1) and single crystals (2); numerous peaks at different temperatures were observed for a large single crystal (3). X-ray diffraction has proved that the 'jumps' corresponded to a partial transformation of some blocks of the crystal into the α- form.
22 Temperature induced transitions between the polymorphs T α-glycine β-glycine T T γ-glycine
23 Effect of gases on the polymorphic transformations of the glycine polymorphs α-glycine H 2 O β-glycine NH 3 NH 3 γ-glycine
24 Effect of gases on the polymorphic transformations of the glycine polymorphs EtOH CH 3 COOH NH 3 H 2 O NH 3 + H 2 O NH 4 Cl HCl α-gly α-gly α-gly α-gly α-gly α-gly α-gly gly x HCl α-gly (+γ-gly) α-gly (+γ-gly) α-gly (+γ-gly) α-gly (+γ-gly) α-gly (+γ-gly) γ-gly α-gly (+γ-gly) gly x HCl γ-gly γ-gly γ-gly γ-gly γ-gly γ-gly γ-gly gly x HCl β-gly β-gly β-gly β-gly α-gly γ-gly (+α-gly) (α+β+γ)- gly gly x HCl
25 Effect of gases on the polymorphic transformations of the glycine polymorphs β-form, H 2 O ( α-form) β-form, NH 3 ( γ-form) α-form, NH 3 ( γ-form) β-form, NH 4 Cl ( (α+β+γ)-forms)
26 Transitions between the polymorphs induced by grinding (important for sample preparation for instrumental analysis and for processing glycine as a drug) wet grinding α-glycine dry grinding β-glycine heavy treatment in an activator; or wet grinding dry grinding γ-glycine
27 Transformations between the polymorphs of glycine are related to the reconstruction of the extended hydrogen bond network in the crystal, are kinetically controlled, related to recrystallization, and are extremely sensitive to the interaction with the molecules of gases, that can be involved in the hydrogen bond formation with the molecules at the surface.
28 Outline Introduction Control of the crystallization of a desirable polymorph A comparative calorimetric study in a wide range of temperatures Polymorphic transitions Effects of temperature and pressure Conclusions
29 Effects of temperature and pressure Low temperature: single crystal X-ray diffraction, STOE STADI-4, Oxford Cryosystems cooling device, down to K; High pressure: powder high resolution X-ray diffraction, synchrotron radiation at ESRF (λ = 0,7 Å, MAR345 detector), up to 4 GPa. Effects of temperature and pressure manifestations of the differences in hydrogen bond networks in the polymorphs
30 Bulk compressibility Pressure increase Cooling V/мол, A V / мол, Å P, GPa T, K α, β, γ
31 α-glycine (P2 1 /n) Р = 1 GPа 2 Р = 2 GPа b c a 1 Т = 150 К 1.79 c a 1 expansion (close to the direction of the shortest NH O bonds) 2 medium compression (close to the direction of the longer NH O bonds) Axis 3 (maximum compression) is normal to the molecular layers (along b)
32 Lattice strain α glycine β glycine a a 2 2 short NH O 1 c long NH O 1 c at Р = 1 GPа at Р = 2 GPа Axis 3 is normal to the plot plane (along b) at Т = 150 К
33 γ-glycine (P3 1 ) c a b c a b minimum compression along c (along the shortest hydrogen bonds) E. Boldyreva et al.,
34 Hydrogen bonds A comparison of compression on cooling from 294 К to 150 К Δl, Å 0.06 l Å Å l3.1 0, Е α, β, γ
35 Lattice strain Pressure increase Cooling Δl / l, % Δl ΠlΠΦlΠΦ / l, % T, K P, GPa Rhombs along axis 1, squares along axis 2, triangles along axis 3 Red α-form, green β-form, blue γ-form For γ-glycine: rhombs along с, triangles along а
36 Outline Introduction Control of the crystallization of a desirable polymorph A comparative calorimetric study in a wide range of temperatures Polymorphic transitions Effects of temperature and pressure Conclusions
37 Conclusions Glycine provides an example of how complicated the relationships between the polymorphs can be, even if the structure is built from small simple molecules. The differences in the free energies between the polymorphs of glycine and the heats of transitions between the polymorphs are related to the differences in the weak intermolecular interactions and are therefore rather small. At the same time, the kinetic barriers for the transformations seem to be rather large. This is why, once obtained, the metastable polymorphs can be preserved for indefinitely long time, also at the conditions at which they are not thermodynamically stable. Gas molecules (water, NH 3 ) catalyze the phase transitions between the polymorphs, (β α, β γ, α γ). Different gases direct transformation into different forms. Initiation of a phase transition plays a very important role. Therefore the transitions are so sensitive to the presence of even traces of another polymorph, as well as to the impurities or structural defects in the glycine crystal. The mechanisms of the transitions, which must involve some cooperative reorganization of the whole hydrogen bonded network in the crystal, require further detailed studies, and so do the mechanisms of the effect of gases and of the mechanical treatment on the polymorphs. Model computer simulations can be helpful for this purpose. The experimental thermodynamic and structural variable-temperature and variable-pressure data can be used to work out better potentials describing the interatomic interactions in the glycine polymorphs and to test the predictive power of the simulations.
38 Acknowledgements The study was supported by RFBR (grant ), by BRHE (a joint grant REC-008 of CRDF and Russian Ministry of Education), by the Russian Ministry of Education (grant Ч0069 Integration, grant ), and by the programs of the Presidium of Russian Academy of Sciences. The authors thank Dr. G. Perlovich for providing them a sample of γ-glycine and A. Achkasov for the assistance with the experiments with gaseous NH 3
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