Ab initio crystal structure determination of two polymorphic modifications of a local anesthetic agent, Tetracaine Hydrochloride
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1 1 / 30 Ab initio crystal structure determination of two polymorphic modifications of a local anesthetic agent, Tetracaine Hydrochloride Robert J. Papoular Leon Brillouin Laboratory papou@llb.saclay.cea.fr PPXRD-9 23 Feb 10 - Hilton Head Island, SC, USA
2 This document was presented at PPXRD - Pharmaceutical Powder X-ray Diffraction Symposium Sponsored by The International Centre for Diffraction Data This presentation is provided by the International Centre for Diffraction Data in cooperation with the authors and presenters of the PPXRD symposia for the express purpose of educating the scientific community. All copyrights for the presentation are retained by the original authors. The ICDD has received permission from the authors to post this material on our website and make the material available for viewing. Usage is restricted for the purposes of education and scientific research. PPXRD Website ICDD Website -
3 With : APS / ANL Univ. Moscow Univ. Tours B.H. Toby N.B. Leonidov V. Agafonov J. Doebbler A.V. Dzyabchenko H. Allouchi Univ. Rouen M.-N. Petit ENSCP, Paris J.-M. Cense
4 2 / 30 What this talk is really about : Ab initio structure solution using : High-resolution XRPD [ indexing ] Molecular modeling [ starting flexible molecule ] Direct space methods [ Monte - Carlo ] Hydrogen bonds [ chemical sense ]
5 OVERVIEW 3 / 30 Motivation (a) Polymorphism : induced by freeze-drying known tetracaine HCŁ unknown leocaine Leonidov (1995) (b) Anesthetics : local (eyes) (c) Ab Initio structure solution : a textbook example? Previous work on TetraCaine HydroChloride [ TCHC ] (a) Giron et al (1997) (b) Nowell et al (2002) (c) Schmidt et al (2006) Synchrotron X-ray diffraction experiments [ APS / ANL ] OUR TALK : Leocaine = Modeling + Indexing + Direct Space Methods with a twist : Preferred Orientation included in Monte - Carlo --- Modeling ( One molecule, PMC, four molecules ) --- Indexing ( DICVOL : ok ; N-TREOR-09 : perfect ) --- Ab Initio Solving ( FOX!, EXPO 2009? ) Inter- / Intra- molecular H- bonds
6 4 / 30 I. MOTIVATION (1) : LEOCAINE, a new effective drug Paper Ł Patent Ł Industry Vestn. Oftalmol while the crystal structure remains unknown!
7 I. MOTIVATION (2) : Structure Solving Strategy 5 / 30 Preliminary modeling : (Energy minimization) (i) One molecular unit Ł Flexible model ( Hyperchem TM ) (ii) Molecular Packing (unit cell known) Ł Crystal structure prediction ( PMC, Dzyabchenko ) Ab initio solving : (i) Direct Methods ( Phase Problem ) FAILS! (ii) Direct Space Methods Monte-Carlo Parallel tempering ( FOX, Favre-Nicolin ) Post modeling : (Energy minimization) Stability check : Crystal approximated by a few molecules ( 4 for leocaine ) ( Hyperchem TM )
8 6 / 30 II. PREVIOUS WORK (1) : Tetracaine Hydrochloride C 15 H 25 N 2 O 2+ Cl - Intermolecular H - bonds Novell et al NJC (2002) Triclinic P -1 V = 822 Å 3 ab initio from XRPD [ DASH ] 2 - (dimethylamino)ethyl p - butylaminobenzoate hydrochloride
9 7 / 30 II. PREVIOUS WORK (2) : Tetracaine Hydrochloride Giron et al TCHC polymorphism ( DSC, HT XRPD ) J. Therm. Anal. (1997) 6 anhydrous crystalline forms 2 stable at T = 300 K. Schmidt et al TCHC mod.4 ( SXD ) Pharmaceutical Research (2005) Polymorphism caused by conformal flexibility of the molecules Hamaed et al TCHC ( SXD, 35 Cl NMR ) JACS (2008)
10 II. Our Experiments (1) : Sample characterization Electron microscopy ( SEM ) Raman spectroscopy ( FTR ) 8 / 30
11 9 / 30 II. Our Experiments (2) : High-resolution Synchrotron XRPD 11-BM APS / ANL ( Argonne, USA)
12 10 / 30 II. Our Experiments (3) : High-resolution Synchrotron data
13 11 / 30 III. Our Structure Solutions (1) : INDEXING with N-TREOR-09 Tetracaine (TCHC) Leocaine poly # 1 Leocaine poly # 2
14 11 / 30 III. Our Structure Solutions (1) : INDEXING with N-TREOR-09 Tetracaine (TCHC) Novell et al (2002) Leocaine poly # 1 Leocaine poly # 2
15 11 / 30 III. Our Structure Solutions (1) : INDEXING with N-TREOR-09 Tetracaine (TCHC) P Novell et al (2002) Leocaine poly # 1 P 2 1 / c Leocaine poly # 2 P 2 1 / c
16 12 / 30 III. Our Structure Solutions (2): Flexible molecular model for Tetracaine ( Novell, NJC, 2002 ) Quantum-Mechanical Semi-Empirical Methods : AM1 PM3 ZNDO (best)
17 13 / 30 III. Our Structure Solutions (3): Flexible molecular model for Leocaine 2 more experimental models Tetracaine (TCHC) XRPD (Novell,2002) Tetracaine (TCHC) SXD (2010) _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength _diffrn_reflns_av_r_equivalents _diffrn_reflns_av_sigmai/neti _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5899 _diffrn_reflns_theta_full _diffrn_reflns_theta_max _diffrn_reflns_theta_min 3.39 [ IL MILIONE ]
18 13 / 30 III. Our Structure Solutions (3): Flexible molecular model for Leocaine 2 more experimental models Tetracaine (TCHC) XRPD (Novell,2002) Tetracaine (TCHC) SXD (2010) _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength _diffrn_reflns_av_r_equivalents _diffrn_reflns_av_sigmai/neti _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5899 _diffrn_reflns_theta_full _diffrn_reflns_theta_max _diffrn_reflns_theta_min 3.39 [ IL MILIONE ]
19 III. Our Structure Solutions (4) : 14 / 30 Theoretical Crystal Model PMC : Packing of Molecules in Crystals ( Dzyabchenko, 2008 ) Russ. J. Phys. Chem. Ł minimizes the energy of the lattice Ł requires : the unit cell a rigid molecular model
20 15 / 30 III. Our Structure Solutions (5) : SOLVING THE STRUCTURE! OUR STRATEGY : (i) Fine-tune the solving procedure on a known case : ( Tetracaine Hydrochloride ) (ii) Transpose it to cases of similar complexity : The two new polymorphs ( Leocaine )
21 16 / 30 III. Our Structure Solutions (6) : SOLVING THE STRUCTURE! EXPO-2009? (i) DIRECT METHODS [ Phase problem ] FAIL WHY : Not enough triplets / quartets in the Lebail- extracted F(hkl) s (ii) SIMULATED ANNEALING FAILS ( for now ) WHY : Preferred Orientation not yet included in the Monte-Carlo search
22 17 / 30 III. Our Structure Solutions (7) : SOLVING THE STRUCTURE! WHAT : DIRECT SPACE METHODS FOX! ( Favre-Nicolin, Cerny ) J. Appl. Cryst HOW : Monte-Carlo Parallel Tempering + Relaxed Flexible Molecular Model WHY : Preferred Orientation IS included in the Monte-Carlo search WORKS WITH TETRACAINEŁ WE TRY IT ON LEOCAINE
23 18 / 30 III. Our Structure Solutions (8) : A TYPICAL FOX SCREEN Key part : Preferred Orientation
24 19 / 30 III. Our Structure Solutions (9) : FOX solutions for LEO Polymorph # 1 Polymorph # 2
25 after GSAS refinement 20 / 30 III. Our Structure Solutions (10) : FOX solutions for LEO Polymorph # 1 Polymorph # 2
26 21 / 30 III. Our Structure Solutions (11) : FOX solutions for LEO Polymorph # 1 : GSAS-fit diffraction data R wp = R p = variables
27 22 / 30 III. Our Structure Solutions (12) : FOX solutions for LEO Polymorph # 2 : GSAS-fit diffraction data R wp = R p = variables
28 23 / 30 III. Our Structure Solutions (13) : FOX solutions for LEO Polymorph # 1 versus Polymorph # 2
29 24 / 30 III. Our Structure Solutions (14) : Do they make sense? Polymorph # 1 PMC / THEORY
30 25 / 30 III. Our Structure Solutions (15) : Do they make sense? TETRACAINE MOGUL [ CCDC ] LEO Polymorph # 1
31 26 / 30 III. Our Structure Solutions (16) : Are they stable? LEOCAINE polymorph # 1 Hyperchem / PM3
32 27 / 30 III. Our Structure Solutions (17) : Are they stable? LEOCAINE polymorph # 2 Hyperchem / PM3
33 28 / 30 III. Our Structure Solutions (18): Intramolecular H-bonds? ( 2000 ) Leocaine : poly # 1
34 CONCLUSION Freeze-drying TCHC generates a new unknow polymorph: Leocaine #1 29 / 30 Leocaine #1 exposure to intense X-ray beams [ synchrotron, 27 kev ] produces a second new polymorph: Leocaine #2 Structure solution with : Index [ N-TREOR-09 / EXPO-2009 ] ; Solve [ FOX ] ; Refine [ GSAS ] FOX requires a flexible molecular model: (i) Molecular Modeling (ii) XRPD [ TCHC, 2002 ] (iii) SXD [ TCHC ] Why FOX works better than EXPO-2009 on Leocaine Preferred Orientation is included in the Monte-Carlo search Next : observe Leocaine #1 Ł Leocaine #2 transition in situ
35 THANK YOU : 30 / 30 Prof. Carmelo GIACOVAZZO : IC-CNR, U. Bari, Italy N-TREOR-09 EXPO-2009 IL MILIONE Free Web resources : GSAS [ R. Von Dreele ] FOX [ V. Favre-Nicolin ] MERCURY [ CCDC ] Last but not least : ICDD staff : Newton Square, PA, USA my participation
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