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Crystallography in Poland

[Poland logo]The first description of crystalline minerals written in the Polish language was published in 1692 by Wojciech Tylkowski. Polish textbooks of mineralogy containing elements of crystallography were published in the universities of Krakow and Lwow in the second half of the 19th century. Between the World Wars, crystallography operated at the Krakow, Lwow, Poznan, Warsaw and Wilno universities. At the Jagiellonian U. in Krakow in 1933, S. Kreutz, an author of books on theoretical crystallography, supervised the Ph.D. thesis of S. Janik on the X-ray structure of ZnCl2.2NH3. At the Lwow U., L. Chrobak studied inorganic crystals by X-ray methods, T. Baranowski grew protein single crystals of muscle myogen and Z. Wayberg, studied crystal symmetry and morphology. Other early crystallographic studies included analysis of metal alloys by powder methods (W. Trzebiatowski, Technical U. of Lwow), iron hydroxides using Debye Scherrer methods (A. Krauze, Poznán U.) and geological samples (A. Rychlewski and E. Passendorfer, Wilno U.). At Warsaw U., S. Pienkowski studied polymers and single crystals by X-ray and electron diffraction and in 1935 A. Laszkiewicz, published a paper on the structure of hexamethyltetramine salicylate. J. Czochralski (Technical U. Warsaw) studied growth and properties of single crystals of metals.

[Myogen]Hexagonal crystals of myogen.
After World War II, the borders of Poland were changed and people from Lwow (Lviv) were transferred to Wroclaw, people from Wilno (Vilnius) were moved to Gdansk and Torun and intellectual refugees from a demolished Warsaw, settled in Lodz. The polish scientific infrastructure was rebuilt at new academic centers in these cities and young people began to study crystallography. W. Trzebiatowski began the first X-ray crystallographic laboratory at the Technical U. of Wroclaw, in 1946. In 1953, crystallography was introduced as an obligatory subject in university chemistry curricula producing new crystallographic laboratories, and separating crystallography from mineralogy. In 1958 powder neutron diffraction studies were initiated in Swierk.

[Czochralski]Jan Czochralski
In 1956 W. Trzebiatowski initiated annual “X-ray Crystallographic Meetings” at the Wroclaw Tech. U. which became the “Crystallographic Meetings” of the Polish Academy of Sciences (PAN). In the years 1967-1987, nine international schools on solving crystal structure were organized. Also, conferences on applied crystallography (Z. Bojarski, U. Silesia), solid crystals and liquid crystals (J. Zmija, Military U. of Tech.), defects in crystals (J. Auleytner and M. Lefeld-Sosnowska), and organic Crystal Chemistry (A. Mickiewicz, U. of Poznan). In 1966, Poland became a member of the IUCr and the 11th Int’l Congress of Crystallography was held in Warsaw in 1978 under the leadership of J. Auleytner. European Crystallographic Meetings (ECM) were held in Wroclaw (1986) organized by K. Lukaszewicz, and in Krakow (2001) organized by S. Hodorowicz. In the 1980’s, two young crystallographers in Wroclaw, D. Kucharczyk and S. Malinowski, constructed a single-crystal four-circle kappa diffractometer, known as the KUMA KM-4, which was later equipped with a CCD detector. This successful Polish firm merged with “Oxford Instruments” to became “Oxford Diffraction”.

Organizations of Polish crystallographers include The Committee of Crystallography of PAN (chair, A. Pietraszko), The Polish Society of Crystal Growth (chair, S. Krukowski), The Polish Society of Synchrotron Radiation, (chair, B. Orlowski), The Polish Society of Neutron Scattering, (chair, A. Szytula.), and the Polish Crystallographic Association (PCA), (chair, S. Hodorowicz). Universities and Institutes of PAN are the main centers of crystallographic research in Poland and there are X-ray powder diffraction laboratories in industrial institutions. In this report five areas of crystallographic study in Poland are summarized: I) chemical crystallography, II) physical crystallography, III) applied crystallography, IV) crystal growth and liquid crystals and V) protein crystallography. An additional section (VI), written by Z. Dauter (editor of Acta Cryst. Section D) discusses Polish crystallographers working outside of Poland.

Chemical crystallography

The largest groups investigating chemical crystal structures are at the Universities of Krakow, Lodz, Poznan, Warsaw and Wroclaw and the Institutes of the PAN in Warsaw and Wroclaw. Crystallographic research is also pursued in laboratories in Gdansk, Katowice, Lodz, Lublin, Opole, Torun, Czestochowa and Siedlce.

The Crystal Chemistry and Crystal Physics Dept., Jagiellonian U., Krakow (K. Stadnicka, was founded in 1963 by J. Chojnacki, who studied fibrous isopolymolybdates and published the structure of cadmium oxycyanomolybdate(IV)dihydrazine tetrahydrate, in 1969. His followers lead five independent research groups. B. Oleksyn concentrates on biologically important compounds including antimalarials, flavonoids and sweeteners, potential drugs containing Se and Te, and inhibitors of urokinase-type plasminogen activators and HIV-1 integrase. K. Stadnicka’s research interests include molybdate complexes, anti-hypertensive hydrazinephthalazines, anti-arrythmic hydantoin derivatives, optical properties of crystals, structures of molecular magnets, engineering of crystalline phases with NLO properties, and experimental electron density distribution in crystals. S. Hodorowicz’s interests include isopolymolybdates, high-temperature superconductors, the history of crystallography, the kinetics of crystallization, and phase transitions in crystalline state. W. Lasocha pursues powder diffraction analysis with ab initio and Rietveld refinement procedures. K. Lewinski’s protein studies are described in section V. Together with the staff of the Dept., S. Hodorowicz organized ECM 20 in Krakow in 2001 and promoted the Jagiellonian U. doctors honoris causa degree to Isabella and Jerome Karle in 2002. S. Hodorowicz was recently elected president of PCA.

In 1954 Z. Galdecki determined the crystal structure of KAs4O6, the first structure determination at the Crystallography Lab., Lodz U. of Technology (M. Glowka, Galdecki headed the Crystallography and Crystal Chemistry Group for almost 50 years. At present the 20 member staff of professors, senior scientists, PhD students, and technicians use crystallography to explore structure - activity relationships, drug-receptor interactions, crystal engineering, weak interactions in molecular crystals, stereospecific reaction mechanisms, polymorphism, electron density and solid catalysts. Current targets for analysis include anticonvulsants and adenosine receptor ligands (J.Karolak-Wojciechowska), antibacterial quinolones (M. Glowka), herbicides and structurally constrained endomorphine analogs (R. Kruszynski), Cu(II) complexes (L. Sieron), stereoelectronic control of molecular conformation and crystal packing (W. Wolf ), nitrozyl complexes of Re (T. Bartczak), and charge density studies of biological phosphates (W. Maniukiewicz). In 1990 Lodz U. of Technology became the National Affiliated Center of the Cambridge Crystallographic Data Center in Poland. The Crystallography Group has wide international colloborations, and awarded the degrees of doctors honoris causa to H. Hauptman and W. Duax.

[Charge density model]Charge density in (1 – thyminyl) acetamide (by M. Kubicki)
After post-doctoral study with A. I. Kitaigorodskii, in the sixties, Z. Kaluski, Z. Kosturkiewicz and T. Borowiak began X-ray structural investigations in Poznan of ferrocen, and hydrogen bonding in crystals, heterocyclic compounds and natural products. Presently, five groups in the Dept. of Crystallography, A. Mickiewicz, U. Poznan (M. Gdaniec, are active in organic crystal chemistry and one group pursues protein crystallography. T. Borowiak and M. Kubicki analyze charge density distribution, phase transitions, metallo-organic compounds, supramolecular structures, heterocyclic, macrocyclic complexes and the hierarchy of intermolecular interactions (weak and strong hydrogen bonds, halogen bonds, dipole-dipole interactions, π-π stacking, etc). The main topics of interest to M. Gdaniec (a co-editor of Acta Cryst. Section E) include crystalline inclusion compounds, achiral compounds, and supramolecular synthesis of organic and metallo-organic materials with predictable architecture. The research group of A. Katrusiak studies materials science, thermodynamics and phase transitions, temperature-and pressurecontrolled crystallization, pharmaceutical polymorphs, meteorites, environmental pollution, equipment design, diffractometry and new methods of data-analysis and visualization. Z. Kosturkiewicz investigates intra- and intermolecular hydrogen bonds in crystals of organic compounds and problems of polymorphism. U. Rychlewska (co-editor of the Acta Cryst. Section B) and her group are engaged in studies of inclusion properties of supramolecular aggregates with chiral building blocs, multidentate ligands, crystal engineering and the role of weak interactions in the stabilization of crystal structures. Although the main focus of M. Jaskolski (a member of EMBO and editor of the Journal of Molecular Biology) is the structures of proteins (described in section V) he also investigates hydrogen bonds and weak interactions in small molecule systems. The researchers in the crystallography dept have also organized eleven international symposia on organic crystal chemistry.

In the 1970’s powder diffraction studies of zeolites were initiated in the Crystallography Dept., M. Curie-Sklodowska, U. Lublin (M. Koziol, under the leadership of. T. Penkala. Since 1976 the A. Koziol group has pursued single crystal studies and polymorphism of biologically active compounds and the S. Pikus group has used powder diffraction and SAXS methods to analyzse amorphous and microporous materials.

[Warsaw staff] The staff of the Crystallography Laboratory at Warsaw U.
Crystallography Lab., Warsaw U. (K. Wozniak, A. Laszkiewicz, led the crystallographic group after WWII. Next, L. Chrobak, developed powder methods to investigate minerals, and synthetic crystals (1951-1970) and A. Wiewiora applied powder methods to study phase transitions. (1970-1977). Since 1977 the crystallographic unit has focused on analysis and molecular models of aromacity, hydrogen bonding, weak interactions and long distance effects in organic crystalline compounds under the leadership of T. M. Krygowski. Today one of his former students K. Wozniak combines X-ray and neutron diffraction and NMR charge density studies to explain weak interactions in supramolecular organic, inorganic and hybrid systems.

[Glowiak]Tadeusz Glowiak
T. Glowiak initiated crystallographic research in the Chemical Crystallography Dept., Wroclaw U. (T. Lis, in 1959 with studies of oxocomplexes of metals. Amino acid cation complexes were studied by photographic methods in the 1970’s and, since 1973, with the first automatic four-circle diffractometer in Poland. The first molecular magnet (Mn12O12) was synthesized and described in this laboratory. Current fields of interest include the role of weak, directional interactions in molecular recognition, low temperature resolution of racemates, and studies of biochemical intermediates, organic sulphates and phosphonate esters. More than 1000 new compounds have been structurally characterized and described in over 700 research papers.

In the Dept. of Physical Chemistry and Crystallography, Jan Dlugosz, U. Czestochowa (M. Wieczorek, that was founded in 1990 by B. Marciniak, three professors (M. Krzesinska, M. Wieczorek and W. Pawliuk), study the growth, structure, morphology, perfection and properties of crystals formed by organic and intermetallic compounds.

In the 1970s’ Z. Dauter, A. Hempel and A. Konitz investigated crystal structures of biologically active compounds in the Crystallography Lab., Dept. of Chemistry, U. of Technology, Gdansk (J. Chojnacki, In 1995 W. Wojnowski established a laboratory for X-ray single crystal structure studies of inorganic and metallorganic compounds. Currently, X-ray crystal structures of metal complexes with ligands including low valent PP compounds and silicon-sulfur compounds are determined by J. Chojnacki and K. Baranowska and A. Konitz continues structure investigations of organic and metallorganic compounds.

In 1954, the Dept. of Solid State Chemistry was organized by W. Trzebiatowski at the Inst. of Theoretical and Physical Chemistry, Wroclaw U. Technology (I. Turowska-Tyrk, ilona and a single crystal study of BaO4TiO2 was completed by K. Lukaszewicz. Presently, T. Luty with his research group studies the dynamics of crystal lattices. I. Turowska-Tyrk studies structural changes in organic crystals during photochemical reactions and phase transitions and V. Videnova-Adrabinska (Dept. of Inorg. and Struc. Chem.) investigates inclusion compounds of molecular recognition, and organic crystal engineering.

The Lab. of X-ray Structural Analysis, Inst. of Physical Chemistry (PAN), Warsaw (J. Lipkowski, was founded by W. Wolfram in 1964 and has been led by J. Lipkowski since 1978. Research is focused on the study of heteromolecular complexes in which one of the components (the host) binds a variety of molecular species (the guests) in a selective and reversible manner. The ultimate goals of the research are the design of systems that selectively separate mixtures, activate chemical reactions, self assemble and transport specific molecules. Host systems with internal cavities of molecular dimensions (organic, zeolites, cyclodextrins, and calixarenes) involving H-bonds and other non-covalent bonding are under analysis. The physicochemistry and phase transitions structure dynamics of supramolecular complexes are studied over a temperature range of 80 to 400 K. The Laboratory head, J. Lipkowski, is presently the Vice President of the PAN and a member of Editorial Advisory Board of Central European J. of Chem. K. Suwinska manages the distribution of the IUCr Newsletter in Poland.

In1969, after post-doctoral study with J.D. Dunitz, T. Krajewski produced the first Polish integrated computer system for structure solution and refinement in the Crystallography Lab., Inst. of Organic Chemistry, PAN, Warsaw (Z. Urbanczyk-Lipkowska, The research team (P. Gluzinski, J. Krajewski, Z. Urbanczyk-Lipkowska) was engaged in conformational studies of mono- and disaccharides, structure - activity relationships of small biomolecules and application of molecular recognition in chemistry.

Chemical crystallography has also been studied in other Polish universities. In the early years crystallographic research in this area centered on organic compounds including acridine derivatives (Lab. of Crystallography, U. of Gdansk, A. Sikorski, art@chem., metal complexes and small organic molecules (Dept. of Crystallography, Copernicus U.,Torun, A. Wojtczak,, crystal structures and quantum chemistry studies of organic compounds (U. of Lodz, S. Grabowski, since 1987, organometallic compounds and neutron spectroscopic studies of hydrogen bonds in amino acids (Inst. of Nuclear Chemistry and Technology, Warsaw, J. Leciejewicz,

Since 1997 projects have focused on organic crystals, high-pressure studies, phase transitions, electron charge density, chemical reactivity, ferroelectrical, piezoelectrical and ferroelastic materials (U. of Opole, J. Zaleski,, magnetic properties of metal alloys (U. of Silesia, Katowice, I. Okonska,,pl), organic compounds with pharmaceutical activity including Cinchona alkaloids, and glucocorticosteroids, and polymorphism of new liquid crystal materials including cholesterol-containing dimers in collaboration with Wageningen U. in Holland (U. of Podlasie, Siedlce, Z. Karczmarzyk,

Physical crystallography and crystal defects

[Structural research dept.]The staff of the Dept. of Structural Research, Warsaw U.
The main centers of physical crystallography in Poland are at the Universities in Warsaw, Krakow and Katowice as well as the Institutes of the PAN in Warsaw and Wroclaw. X-ray research was initiated in the 1920’s in the Dept. of Structural Research, Warsaw U. (M. Lefeld-Sosnowska, by S. Pienkowski. In the 1960s, X-ray diffraction topography was developed by J Auleytner and next by M. Lefeld-Sosnowska to study defects in single crystals. Since the 1990s high-resolution X-ray diffractometry has been used to study diffuse scattering from point defects in gallium arsenide (GaAs) crystals, semi-insulating low-temperature GaAs containing defects, low temperature GaAs doped with beryllium and mismatched layers of nitrides grown on sapphire. Recently, synchrotron topography has been used to analyze defects in gadolinium-calcium oxyborates and, to detect, for the first time, dislocations in nonlinear optical crystals used to generate second and higher harmonics of light, using neutron diffraction and inelastic scattering. Investigations of semimagnetic semiconductors (Cd1-xMnxTe) have revealed antiferromagnetic ordering of manganese spins. In an EuS and superlattice strong antiferromagnetic coupling of the EuS layers across the nonmagnetic PbS layers was revealed, whereas much weaker coupling was observed across the YbSe layers in a EuS/YbSe supelattice. Reflectometric measurements using polarized neutrons proved that magnetic ordering detected in GaMnAs had a long-range character. The exchange interactions between pairs of Mn-Mn atoms in diluted magnetic semiconductors have been studied using neutron inelastic scattering.

[Buras]Bronislaw Buras
Structure and lattice dynamics studies of condensed matter by neutron scattering and Mossbauer spectroscopy are the main activities of the Div. of Structural and Lattice Dynamics, Warsaw U. (I. Sosnowska, The Time-of-Flight (TOF) neutron diffraction technique was developed by B. Buras in the 1960s. The pulsed neutron source in Dubna (USSR) was used for the first time for crystal structure determination and phonon dispersion determinations by Sosnowska. Due to the extremely high resolution of the TOF method, a long period magnetic cycloid (620 Å) was detectable in BiFeO3. Since the 1970’s members of the division staff have studied the anisotropy of hydrogen diffusion in crystals (R. Kutner, I. Sosnowska, K. Kehr), hydrogen behavior in ferroelectrics, the mobility of water in opal (with a Research Center in Julich), magnetic moments in spin glass systems (with ETH, Zurich), neutron diffraction studies of phase transition in polycrystalline materials, and inelastic neutron scattering studies of rare earth metals in hard magnetic materials (with M. Loewen, Julich). Recently it was found (with Bonn U.) that the modulation of the cycloid in BiFeO3 changed drastically when iron ions are replaced by manganese ions. High resolution synchrotron radiation studies have shown phase separation and charge modulation in CaMn7O12. Neutron diffraction studies have shown that the Yoshimori model cannot be used to describe long range magnetic ordering of Mn4+ ions in β-MnO2 (M. Regulski ) and that nanocrystalline Cr has spin density-wave modulated magnetic ordering characteristic of Cr single crystals. Small angle neutron scattering studies of the microstructures of electrodeposited nano-Ni, Co and Cr revealed a fractal-like density autocorrelation function (R. Przenioslo with R. Hempelmann, Saarbrucken, and A. Hewat, Grenoble).
[Magnetic satellites graph]Magnetic satellites in BiFeO3
Research in the Dept. of Phase Transition Kinetics, Jagiellonian U. (R. Kozubski, rafal concerns Monte-Carlo and molecular dynamics simulations of structural transformations in intermetallics, elementary atomic-migration processes, and structural relaxation in superalloys. Recent discoveries include detection of different ordering and diffusion mechanisms in FePt intermetallics, self diffusion of iron in ordered FePt films and stability of superstructure variants in FePt nanolayers. The research is performed in cooperation with scientists from U. of Wien, the CNRS Inst. in Strasbourg, the Inst. of Theor. and Gen. Phys. in Stuttgart, and Network of Excellence of E. U.
[The Shiojiris]M. Shiojiri and his wife visiting I. Sosnowska’s Laboratory.
In the Solid State Physics Dept., Jagiellonian U. Krakow (A. Szytula, crystal and magnetic structures of ernary intermetallic rare earth compounds with varying stoichiometries are investigated by powder and neutron diffraction methods. Neutron diffraction data are used to analyze and correlate atomic and molecular structure with classical magnetic measurements. The majority of these compounds show a change in the magnetic structure from the collinear form commesurate with the crystal structure at low temperature to a modulated incommensurate form near the Neel temperature. The structures of over 200 intermetallic compounds have been determined and published in The Handbook of Crystal Structures and Magnetic Properties of Rare Earth Intermetallics, (1994), and Crystal Structures and Magnetic Properties of RTX Rare Earth Intermetallics, (1998) by A. Szytula and J. Leciejewicz. Neutron diffraction experiments are carried out in collaboration with the Berlin Neutron Scattering Center, the Hahn-Meitner Inst., Germany, and the Paul Scherrer Institute, Villingen, Switzerland.

In 1963, A. Oles began neutron diffraction investigations of crystal and magnetic structures, and phase transitions in crystals at the Stanislaw Staszic U. of Science and Technology, Krakow (J. Wolny,

A neutron diffractometer was constructed and mounted at the reactor in Swierk. The method of texture determination by neutron diffraction was worked out, and in 1976 A. Oles published the book Magnetic Structures Determined by Neutron Diffraction. Recent research areas include: solid state electronic structures (St. Kasprzyk), group theory analysis of crystal symmetry (W. Sikora), aperiodic systems (J. Wolny), and investigations of the mechanisms of plastic deformation (K. Wierzbanowski).

Research in the Dept. of Crystal Physics, U. of Silesia, Katowice (J. Warczewski, concerns crystalline and magnetic periodic and aperiodic structures, modulated and electronic structures, quasicrystals, and the magnetic properties, transport phenomena, mathematical analysis and theory of the condensed phase including chromium containing magnetic crystals having commensurate and incommensurate modulation.

Since 1968, magnetic, electric and transport properties of ionic perowskite, spinel crystals, metals and alloys have been investigated at low and high temperatures in the Dept. of Solid State Physics, U. of Silesia, Katowice (A. Ratuszna,

[Central lab staff]Staff of the Central Lab. of X-ray and Electron Microscopy of the Inst. of Physics, PAN, Warsaw.
The Central Lab. of X-ray and Electron Microscopy of the Inst. of Physics, PAN, Warsaw (K. Ludwiczak-Jablonska, led by J. Auleytner since 1967 focuses on interdisciplinary characterization of matter using microanalysis spectroscopy, X-ray optics, applied crystallography and electron microscopy. Studies include investigations of the mechanisms of the solid surface damage induced by ultra short VUV pulses from free electron lasers and simulations of the propagation of strong EM pulsed beams within the XUV and SXR wavelength.Chemical bonds, ionic strength, phase and dipole analysis are studied with X-ray absorption and emission spectroscopy, using conventional and synchrotron radiation. The shape of the spectra is a fingerprint of the chemical compound, useful for solving a variety of scientific problems including determination of the composition of disordered composites. Electron microscopists are engaged in the characterization of semiconductors, metal oxides, superconductors and fullerene nano-objects. Computational analysis, simulation of diffraction patterns and transmission electron microscopy images are used to determine the structure of new materials. EXAFS oscillations provide information on short-range order in low-dimensional structures and dopants in semiconductors.

[X-ray diffuse scattering diagram]X-ray diffuse scattering in (CH3)4NCdCl3 a: hk0, b: hk 0.5, c: hk 1.5, d: hk 2 reciprocal layer. (A. Pietraszko)
Crystallographic studies initiated at the Dept. of Crystallography, Inst. of Low Temperature and Structural Research, PAN, Wroclaw (A. Pietraszko, by W. Trzebiatowski in 1966 and expanded by K. Lukaszewicz and A. Pietraszko currently focus on temperature and pressure dependent phase transitions in ferroelectic, ferroelastic and magnetic crystals, superconductors, superionic conductors, intermetallic and organometallic compounds. Modulated phases of a number of crystals have been determined using computer programs developed by K. Lukaszewicz, A. Pietraszko and W. Paciorek. Precise measurement of lattice parameters of single crystals in a broad range of temperatures are obtained using the Bond-type diffractometers constructed for this purpose. X-ray diffuse scattering is studied using 2-dimensional detectors. Other studies in the department include electron crystallography of mono- and multi-component oxides (M. Wolcyrz) and analysis of lattice defects, impurities and dielectric relaxation in silica glasses after ionic exchange processes (M. Suszynska). The Department collaborates with institutes in Stockholm, Copenhagen, Darmstadt, Padova, Bello Horizonte, Lviv, Lutsk, Vilnius and Moscow. Two crystallographers from the Department, (D. Kucharczyk and M. Malinowski), designed and produced an automatic four-circle X-ray diffractometer KM-4. Now, the Oxford Diffraction Company, through a joint venture of KUMA Diffraction and Oxford Instruments produces Xcalibur and Gemini systems in its production facility located in Wroclaw. The Inst. of Low Temperature and Structural Research houses the Committee of Crystallography, PAN, chaired successively by W. Trzebiatowski, K. Lukaszewicz and A. Pietraszko. The Committee, which represents Poland in the IUCr, organizes the annual Polish Crystallographic Meetings (48th in 2006).
[Bialowieza 2000]Participants of the conference in Bialowieza in 2000.
In 1958, a group of scientists and engineers at the Inst. of Nuclear Research, Swierk (J. Leciejewicz) headed by B. Buras constructed a neutron spectrometer, at the EWA reactor and large single monochromators of copper, zinc, lead and aluminium were grown by A. Modrzejewski. Early studies included powder neutron diffraction of lead oxides and tungsten carbides (J. Leciejewicz) and magnetic studies of intermetallic uranium compounds (A. Murasik and J. Leciejewicz). Some neutron diffractometers built in Swierk from 1960 to 1970 under the supervision of K. Blinowski, were sold abroad. In 1963 B. Buras adopted time-of-flight techniques for neutron powder diffraction and experiments using a Fermi chopper and silicon powder samples were performed with J. Leciejewicz. In 1983 The Inst. of Nuclear Research was subdivided into three Institutes. Activities at the. Inst. of Nuclear Chemistry are described, in section I and the others are described below.

The main topics of study at X-ray Lab. of the Inst. of Atomic Energy, Swierk (K. Wieteska,, a successor of the Inst. of Nuclear Research, are crystal lattice defects using X-ray topography, phase transitions in ceramics using powder diffraction, phase transitions in polycrystalline materials using electron microscopy and organic X-ray crystal structures.

Magnetic and spectroscopic properties of crystals and electronic charge density in crystals are studied in the Inst. of Experimental Phyics, U. of Bialystok, (L. Dobrzynski, ). International conferences on polarized neutron scattering, high resolution Compton scattering as a probe of Fermiology and charge, spin and momentum density were organized by L. Dobrzynski.

Lattice defects in the single crystals applied in optoelectronics are investigated by J. Pajaczkowska and colleagues at the Inst. of Technology of Electronic Material (J. Pajaczkowska,

Applied crystallography

[18th conference attendees]Participants of the 18th Conference on Applied Crystallography
Since 1974 the Inst. of Material Science, U. of Silesia, Katowice (E. Lagiewka, has been led by Z. Bojarski. X-ray and electron diffraction, topography, small angle scattering and spectroscopic methods are used to study metallic, ceramic and polymeric materials and alloys having crystalline, amorphous, nanocrystalline and quasicrystalline structures. Targets of study include phase transitions, mosaicity, textures, chemisorption, whiskers growth and electrochemical processes. Techniques applied include the Bond method for lattice parameter analysis, Rietveld and ab initio methods of refinement and structure solution and Auger spectroscopy for the investigation of alloy surfaces. Instruments have been designed and constructed at the Inst. and crystallographic textbooks have been edited by Z. Bojarski and co-authors. Research groups are headed by Z. Bojarski, J. Barcik, J. Frackowiak, H. Morawiec, L. Pajak, J. Rasek, M. Surowiec, K. Wokulska and Z. Wokulski. The 20th Conference of Applied Crystallography and a School on ab initio methods of analysis of polycrystalline materials was held in September 2006.
[Whiskers of TiN] Whiskers of TiN. (K. Wokulska)
At the St. Staszic Inst. of Iron Metalurgy, Gliwice (T. Bold, studies of the structures of minerals and phase transitions of steel products began in 1957 using instruments constructed in the institute. The textures of thin sheets of iron and phase transitions in the range -180oC to +1200oC were investigated. The techniques of replication in electron microscopy and X-ray microanalysis were perfected and inter-laboratory tests of quantitative phase analysis were organized.

[Quasicrystal diffraction] Electron diffraction of decagonal quasicrystal (by W. Bogdanowicz)
At the Inst. of Textile Engineering and Polymer Materials, U. of Bielsko – Biala (A. Wlochowicz,, A.Wlochowicz and colleagues investigate the degree of crystallinity of polymers and fibrousness of materials using small-angle scattering methods. Nanostructures, thermal proprieties of homogenous copolymers and phase transitions in fibrous materials are also studied by using synchrotron radiation. The Sixth International Conference on X-ray Investigation of Polymer Structures organized by the Bielsko-Biala U. and the Catholic U. of Leuven (Belgium) was held in 2004. At the Inst. of Technology and Chemical Engineering, Poznan (J. Garbarczyk, jozef, J. Garbarczyk and coworkers determine X-ray crystal structures of organic crystals and are currently analyzing conditions of crystallization and polymorphism of isotactic polypropylene.

At the Dept. of Macromolecular Physics, Adam Mickiewicz U., Poznan (M. Kozak,, M. Kozak investigates structures of fibrous materials using the small-angle X-ray scattering and is currently studying the effect of cationic surfactants on the structure of phospholipidic systems.

The staff of the Lab. of X-ray Powder Diffraction and Spectrometry, Inst. of Physical Chemistry, PAN, Warsaw (Z. Kaszkur, is engaged in phase determination and Rietveld refinement of high resolution powder diffraction data as well as dynamical and kinetic powder diffraction studies at variable temperature (up to 600ºC) and pressure. Quasi-amorphous materials are analyzed using X-ray powder diffraction and radial distribution function methods. Numerical methods for studying highly dispersed solids (transition metals) deposited on supports (SiO2, Al2O3) are developed including reliable background estimation data, smoothing procedures, and quantitative analysis for in situ studies. Recently, analytic tools allowing an insight into the structure and dynamics of nanocrystalline metallic particles in a chemical reaction have been developed. Violations of Bragg’s law and subtle changes in the peak intensity and width can be traced to nanocrystalline variations during chemical reactions. A similar approach has been used successfully for the analysis of concentration profiles for bimetallic nanoalloys modified by chemisorption of gasses.

In the Dept. of Powder Diffraction, Inst. of Low Temperature and Structure Research, PAN, Wroclaw (R. Kubiak, phthalocyaninato complexes with rare earth metals and their salts are synthesized and investigated by X-ray and electron diffraction methods. The synthesis of new cyanic derivatives including new sandwich–type metallodiphthalocyaninato complexes, investigation of their transformations and crystal structure determination are the specialty of the research group.

A semiconductor strip detector with a significantly increased rate of acquisition of powder diffraction data was constructed in Dept. of Physics and Applied Informatics, St. Staszic U. of Science and Technology, Krakow (A. Zieba) by a group led by A. Dabrowski. The detector was commercialized by Bruker – AXS under the name Lynx Eye.

X-ray powder methods are used by A. Mazurek and coworkers at the Central Forensic Lab. of Polish Police, Warsaw (A. Mazurek, for the identification of drugs, explosives, and unknown substances. The most effort is focused on analysis of trace samples found in clandestine amphetamine laboratories and amphetamine samples from the illegal drug market.

Powder X-ray diffraction methods are also used in the investigation of inorganic and organic materials in five other laboratories in Poland (Inst. of Material Engineering, Poznan U. of Technology; Dept. of Engineering & Polymer Technology, Wroclaw U.; Inst. of Material Engineering, Technical U. of Czestochowa; Dept. of Magnetochemistry, Fac. of Chemistry, A. Mickiewicz U.; Inst. of Electronics, Wroclaw; Condensed Phase Physics Group, AGH U. of Science & Technology).

Crystal growth and liquid crystals

[MUT lab crystals] Single crystals grown in the MUT Lab
The main center of crystal growth and research on liquid crystals in Poland is at the Div. of Physics and Crystal Growth, Military U. of Technology, Warsaw (J. Zmija, In 1958, J. Zmija began investigating the growth of intermetallic compounds, metallic single crystals, and diffusion effects in crystals. In 1965 studies were begun on new materials for lasers and microwave acoustics. The self-diffusion of dopants in crystals of semiconducting compounds (ie AIIIBV, AIIBVI) were studied using radioisotopic methods and small-angle scattering. Structures of single crystals doped with Al, Cd, Se, In, and Mn were investigated and a theory of diffraction from polytype crystals was developed. Studies of epitaxy on GaAs led to the production of a semiconductor laser. In 1974, under the direction of J. Zmija chemists, physicists and materials engineers began work on liquid crystals. They created new mixtures and phases for displays and other electro and thermo-optical elements including smectic- and thermo-ferroelectrics. New methods for liquid crystal study were developed. Research using single crystal technology of boron, bismuth, lead and other oxide materials was begun. Due to their acoustic properties single crystals of BGeO and BeSO, were used in construction of transducers of surface waves and a filter model for medium frequencies of color television were designed. The photochromic effect was detected in the BGeO single crystals.

[Zakopane] The participants of the International Conference on Single Crystals and Liquid Crystals in Zakopane.
Presently, the group prepares single crystals of KGd(WO4)2 (KGW), pure and doped by rare earth ions to enable construction of diode pumped lasers, doubled frequency lasers and Raman shifters. Single crystals of LiB4O7, CsLiB6O10, and BiB3O6 having large nonlinear optical properties are used in the generation of higher harmonics of laser radiation with the ultimate goal of obtaining lasers with doubled frequencies. Acousto-optical single crystals of TeO2 are used as light modulators and tuning filters and to steer laser beams. Other studies include structures of semiconductors in the group of E. Igras and small-angle X-ray scattering by J. Frydrychowicz and R. Swilla. The 16 scientists engaged in liquid crystal research make this the largest group in Poland and one of the largest in Europe working in the liquid crystal field. 43 scientists from the Division received PhDs and ScDs degrees. The Military U. of Tech. has been organizing international conferences on single crystals and liquid crystals since 1972.

Other institutions engaged in studies of single crystal growth and epitaxial film technology include groups investigating the dependence of liquid crystalline properties on molecular mass at the Inst. of Physics, Lodz U. of Technology, Lodz (G. Derfel,, defects in single crystals of pseudoperovskite at the Inst. of Electronic Materials Technology, Warsaw (A. Pajaczkowska,, the influence of impurities on the kinetics of crystal growth and structural and electrical properties of amorphous alloys at the Inst. of Chemistry & Environmental Protection, Jan Dlugosz U., Czestochowa (M. Wieczorek), cubic nanocrystalline La2O3 in transmission electron microscopy at the Inst. of Low Temperature and Structural Research, PAN, Wroclaw (M. Malecka,, crystal growth from water solutions in a magnetic field at the Technical U. of Rzeszow (W. Proszak, low-temperature synthesis of garnet – powder luminofors of submicron dimensions at the Faculty of Chemistry, Wroclaw U. (E. Zych,, crystal seeding, the kinetics of crystal growth, and influence of dopants on inorganic crystal growth at the Inst. of Physics, Lublin U. of Technology (K. Sangwal,, and the modeling of the process of single crystal growth from solutions at the Dept. of Physics, Lodz U. of Technology (G. Derfel, Other research on liquid crystals, is being conducted at Lodz U. of Technology (P. Adamski, G. Derfel), Poznan U. of Technology (D. Bauman), Inst. of Molecular Physics, PAN (J. Jazdzyn, W. Kuczynski), U. of Podlasie (Z. Karczmarzyk), Warsaw U. (J. Przedmojski), and Jagiellonian U. (S. Urban).

Protein crystallography

[CBB] People working at the CBB, left to right, H. Fernandes, M. Sikorski, G. Bujacz, O. Pasternak, M. Gilski, O. Cakici, A. Hernandez-Santoyo, E. Bartoszak-Adamska, E. Tykarska,K. Michalska, K. Brzezinski, A. Wojtkowiak, Sz. Krzywda, M. Jaskolski, K. Banaszak, W. Rypniewski, J. Raczynska.
The Center for Biocrystallographic Research, Inst. of Bioorganic Chemistry, PAN, Poznan (CBB) (M. Jaskolski, was created in 1994 with financial support from the Foundation for Polish Science as a joint initiative of the Dept. of Crystallography, A. Mickiewicz U. and the Inst. of Bioorganic Chemistry, PAN. It was the first macromolecular crystallography laboratory in Poland, and the second in Central and Eastern Europe. From its inception, the Center had three main goals: to conduct competitive biostructural research, to breed a new generation of protein crystallographers, and to become a site for integration and collaboration around structural biological problems on a national and regional scale. The CBB has always been an open laboratory, making its infrastructure, in particular the protein crystallization and data collection facilities, freely available to colleagues who had interesting projects but no equipment to study them.

Throughout the years, we’ve had visitors from Warsaw, Cracow, Gdansk, Torun, Wroclaw and Lodz in Poland, and from Prague, Halle, Lund, Vilnius, and Lviv. Several of those visits have resulted in lasting and fruitful collaborations. A regular visitor, C. Sansom (Birkbeck College, London) worked on our asparaginase project and was instrumental in the development of our teaching program. Specifically, there were very close connections between our institutions when Birkbeck was introducing their innovative internet courses on protein structure and crystallography. A number of our students graduated with Advanced Certificates, some with MSc from the U. of London. Two of our Indian postdoctoral fellows (A. Addlagatta and R. Thaimattam) were transmuted from smallmolecule-to macromolecular crystallographers while conducting high-caliber research on protein structure at atomic resolution. Currently, we have two candidates in a European Ph.D. program, H. Fernandes (Portugal) and O. Cakici (Turkey), a postdoctoral associate from Mexico (A. Hernandez-Santoyo) and a host of native students. A number of masters and doctoral degrees have been conferred in CBB. Sz. Krzywda brought a study of myoglobin variants from G. Dodson and A. Wilkinson in York. M. Kozak, now using SAXS for macromolecular studies at the Physics Dept. of the university wrote a thesis about antileukemic bacterial asparaginases. D. Borek, who discovered a new plant enzyme and its cousin in E. coli, and initiated a fascinating series of structural studies as a student is now in the Otwinowski Lab in Dallas, TX. R. Janowski who’s Ph.D. thesis concerned domain-swapped dimers in amyloidogenic cystatin C. is now working in the MTB structural genomics project at EMBL in Hamburg. J. Biesiadka determined the structure of proteins responding to pathogens in symbiotic plants. The project is now evolving towards hormone-binding plant proteins, while J. Biesiadka is busy with the structure of a photosystem in W. Saenger’s lab. at FU, Berlin.

We also have projects based on collaborations with Polish partners (Universities of Wroclaw, Gdansk) and foreign labs (U. of Lund). A. Wlodawer (another Polish compatriot) at the National Cancer Inst. (USA) has been the initial seed for our scientific growth and an inexhaustible source of support, and scientific inspiration. Our protein crystallographic work started in collaboration with Wlodawer, included studies of retroviral protease, retroviral integrase and an antileukemic amidohydrolase. After nearly 20 years this collaboration is very much alive. The Wlodawer lab has provided training in protein crystallography to a number of postdocs and associates from Poland including G. Bujacz, a Professor at the Tech. U. of Lodz, who also holds a part-time position at the CBB. He is Poland’s foremost asset in protein crystallization. During his visits to Poznan he supervises nearly all students’ crystallization projects.

[Proteins] Selected macromolecular structures determined at the CBB (with PDB codes). 1G6X, water molecules (with H atoms) in a BPTI map at 0.86 Å; 1JJA, antileukemic asparaginasefrom E. coli. 1G96, 3D domain-swapped dimer of human cystatin C; 1IFV, pathogenesis-related protein from yellow lupine; 2FLH, plant hormone-binding protein in complex with a ligand (1.2 Å); 1R3O, left-handed RNA duplex; 1SEO, bacterial isoaspartyl aminopeptidase.
In 1998, during ECM-18 in Prague, with encouragement from E. and G. Dodson and A. Lewit-Bentley, we organized a Consortium of Central and Eastern European Struc. Biology Groups (CCEESBG) and we were among the initiating groups, who under the leadership of R. Hilgenfeld and M. Weiss began annual meetings of young biocrystallographers in the Heart of Europe (HEC). The 3rd HEC meeting in 2000 took place in Poznan. In 2001, the CBB was one of the sites of a practical workshop “Determination of High-Resolution Structures for the Post-Genomic Age” sponsored by the National Science Foundation (USA), for young researchers from Central and Eastern Europe. The organization of the workshop was coordinated by A. Wlodawer with financial support from the Howard Hughes Medical Inst. The CBB established an EU-supported Training, Implementation and Dissemination (TID) Centre of the European BioXHIT project in 2005. The TID Centre organizes practical training workshops for the future users of synchrotron beamlines.

Our research has been supported by grants from the State Committee for Scientific Research, Howard Hughes Medical Inst., and the International Centre for Genetic Engineering and Biotechnology. Smaller grants have supported bilateral collaborations, like that with G. Desiraju in India. This collaboration is worth emphasizing because it reflects our efforts to treat macro- and small-molecule crystallography as one discipline. Initiated many years ago by the late M. Wiewiorowski - the founder of our Institute and a great advocate of biocrystallographic research in Poland, our studies into the unifying role of hydrogen bonding and other weak intermolecular interactions continue to be an exciting and evolving story.

Recently, the CBB has been reorganized to incorporate two new groups led by highly skilled specialists. In 2002, W. Rypniewski returned to Poland after receiving training in western laboratories at a time when he was entering the most creative period of his scientific career. Few scientists have the courage he has shown in resisting the brain drain to take on the challenge of working in “less privileged” regions. He has started a vigorous research program that includes determination of large macromolecular complexes and atomic resolution structures of proteins and nucleic acids. M. Sikorski heads the other new group doing protein expression and purification.

Other protein crystallography laboratories in Poland

After a post-doc in A. Wlodawer’s Lab, G. Bujacz started research in the field of protein crystallography at the Inst. of Technical Biochemistry, Lodz U. of Technology (M. Bujacz, and at CBB in Poznan. His achievements include crystal structure and mutational analysis of the cofactor-binding domain of the Cb1 trancriptional regulator, and an HIV protease complexes with inhibitors. He was an initiator of the Lodz U. of Technology award of doctors honoris causa to Alex Wlodawer (USA).

K. Lewinski and his research group investigate enzymatic mechanisms and inhibition of proteins in the Dept. of Crystal Chemistry and Crystal Physics, Jagiellonian U., Krakow (K. Lewinski, In collaboration with L. Lebioda (U. of South Carolina, USA) they determined the crystal structures of human prostatic acid phosphatase, enolase, glutaminase-asparginase, arylsulphatase A and formyltetrahydrofolate synthetase. Their field of research also includes crystallographic studies of ribonuclease A and its variants under ambient and high pressure conditions. K. Lewinski is the editor of the Bioorganic Crystal Chemistry section in the Central European Journal of Chemistry,

A. Wojtczak with his research group at the Dept. of Crystallography, Nicolaus Copernicus U., Torun (A. Wojtczak, has solved protein crystal structures of human and rat transthyretin.

The Int’l Inst. of Molecular and Cell Biology, Max-Planck – PAN Joint Junior Research Group, Warsaw (M. Bochtler, was established in 2001 as a collaborative venture between the Polish Academy of Sciences and the German Max-Planck- Society. Its head, Matthias Bochtler (a former student of Robert Huber) is officially a Junior Group Leader in the Max-Planck-Inst. of Molecular and Cell Biology and Genetics (MPI-CBG) in Dresden, but in practice he is on “loan” to IIMCB in Poland. With funding from the MPI in Dresden, the European Union, and Polish sources, M. Bochtler, has quickly established a dynamic and competitive group, which is almost exclusively Polish. Its short but impressive record of achievement includes discoveries in the area of new peptidases, endonuclease, nucleoside phosphorylases and their inhibitors. The Bochtler lab is advancing protein crystallography in Poland at the international level.

Polish crystallographers outside of Poland or anomalous scattering of multi-poles

(Z. Dauter,

It is quite remarkable how many Polish scientists scattered abroad are crystallographers, or especially protein crystallographers. “Scattered” is not a good word as many of us preserve close links, often involving the “old land”.

Already in the 1960’s and 70’s, several senior crystallographers had a vision to organize excellent schools and workshops where young disciples were taught by such authorities as Nikolay V. Belov, Yuri T. Struchkov, Mikhail A. Porai-Koshits, from Russia, Dorothy Hodgkin, Tom Blundell, Eleanor and Guy Dodson from the UK, Herbert Hauptman, Jerome and Isabella Karle, and Bill Duax from the USA, John Stezowski and Wolfram Saenger from Germany, Ivar Olovsson from Sweden, and Lodovico Riva di Sanseverino from Italy. We were in Poland a very happy crystallographic family with strong links to our “cousins” all over the world. We could learn good crystallography, but unfortunately in those days in Poland access to advanced computing was almost impossible and good X-ray facilities were scarce. It was virtually impossible to pursue protein crystallography.

The political difficulties of the 1980’s created additional problems. As a result, a number of Polish scientists decided to stay abroad and today we find many of them at senior positions in various institutions (Aleksander Roszak, U. of Glasgow, UK; Andrzej Joachimiak, Argonne Natl. Lab., USA; Andrzej M. Brzozowski, U. of York, UK; Boguslaw Stec, USA; Ewa Ciszak, NASA, USA; Ewa Skrzypczak-Jankun, Toledo, USA; Jacek Lubkowski, Zbigniew Dauter, Alex Wlodawer, NCI, USA; Krzysztof Appelt, pharmaceuticals, USA; Lukasz Lebioda, U. of S. Carolina, USA; Mirek Cygler, NRC, Canada; Pawel Dokurno, Ribotargets Ltd., UK; Pawel Grochulski, U. of Saskatchewan, Canada; Tadeusz Skarzynski, Glaxo-Wellcome, UK; Zbyszek Otwinowski, U. of Texas, USA; Zdzislaw Wawrzak, APS, USA; Zygmunt Derewenda, Wladek Minor, Michal Sabat, U. of Virginia, USA). In addition, there is a host of younger postdocs in virtually all places where crystallography is being done.

It is interesting that several of us have direct or indirect links to various synchrotron facilities. Alex Wlodawer participated (with Jim Phillips and Keith Hodgson) in the first ever synchrotron diffraction experiment on protein crystals at Stanford in 1975. Andrzej Joachimiak, who earlier worked at the Universities of Chicago and Yale, is now directing the Structural Biology Center and its synchrotron facility at Sector 19 of APS (Advanced Photon Source) at Argonne and heads the Midwest Center for Structural Genomics. Zbigniew Dauter served for ten years at the EMBL synchrotron outstation at DESY in Hamburg and now for the last eight years heads the Synchrotron Research Section of the National Cancer Inst., located first in Brookhaven and now at the Argonne synchrotron site. Zdzislaw Wawrzak after several years at the Hauptman-Woodward Inst. in Buffalo, since 1998 has been taking care of crystallographic activity at the DND (DuPont, Northwestern, Dow) Sector 5 of the APS synchrotron at Argonne. Pawel Grochulski, after a post at the NRC lab in Montreal, since 2000 is responsible for the construction and activity of the protein crystallography beamlines of the Canadian Light Source at Saskatoon. Last but not least, Zbyszek Otwinowski and Wladek Minor are the authors of the HKL2000 data processing suite, widely used at almost every synchrotron beamline.

As I said before, our younger years bring back very fond memories. But when I really think about it, we are still a very happy and closely knit community. This is why this note belongs in “Crystallography in Poland”.

Article Edited by Zofi a Kosturkiewicz

Editors Note: As we did not have access to a full set of diacritical marks, they were omitted from proper names in the article.

Thank you to the many contributors of Crystallography in Poland:

Grzegorz Bujacz, Jaroslaw Chojnacki, Zbigniew Dauter, Jozef Garbarczyk, Mariusz Jaskolski, Zbigniew Karczmarzyk, Anna Koziol, Tadeusz Marek Krygowski, Janusz Leciejewicz, Maria Lefeld-Sosnowska, Krzysztof Lewinski, Eugeniusz Lagiewka, Barbara Oleksyn, Andrzej Oles, Jerzy Pielaszek, Izabela Sosnowska, Katarzyna Stadnicka, Kinga Suwinska, Katarzyna Slepokura, Ilona Turowska-Tyrk, Zofi a Urbanczyk-Lipkowska, Jerzy Warczewski, Michal Wieczorek, Andrzej Wlochowicz, Janusz Wolny, Marek Wolcyrz, Krzysztof Wozniak, Jacek Zaleski, Andrzej Zieba, Jozef Zmija, 

Rare crystallographic phenomenon recorded in Poznan

An extremely rare natural phenomenon has been observed early in the morning on April 1, 2007, from the windows of the Department of Crystallography, Faculty of Chemistry, A. Mickiewicz University in Poznan, Poland. A series of crystallographic two-fold screw axes (21) appeared in this unusual sighting on an opposite building wall. The scientific background of this phenomenon is still a mystery but it is widely believed that it heralds good fortune for those who have sighted it.
Mariusz Jaskolski, photographed by. M. Gilski