Abstract
The separation of compounds by inorganic/organic boundary is of less importance for the structure determination by diffraction methods. More important for the diffraction is how the atoms build up larger building units and the crystal itself. A molecular/non-molecular boundary is therefore relevant for the choice of a structure determination method. Non-molecular compounds – also called extended solids – are constructed by bonds that extend “infinitely” in three dimensions through a crystal. These non-molecular crystals usually crystallize with higher symmetries, and atoms often occupy special Wyckoff positions. A review of actual methodology is given first, and then highlights and pitfalls of structure determination from powder diffraction, its problems and their solutions are shown and discussed using selected examples.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
David WIF, Shankland K, McCusker LB, Baerlocher C (eds) (2002) Structure determination from powder diffraction data. Oxford University Press, Oxford
Deem MW, Newsam JM (1989) Determination of 4-connected framework crystal structures by simulated annealing. Nature 342:260–262
Favre-Nicolin V, Černý R (2002) FOX, “Free objects for crystallography”: a modular approach to ab initio structure determination from powder diffraction. J Appl Crystallogr 35:734–743
Favre-Nicolin V, Černý R (2004) A better FOX: using flexible modeling and maximum likelihood to improve direct-space ab initio structure determination from powder diffraction. Z Kristallogr 219:847–856
Edgar M, Carter VJ, Tunstall DP, Grewal P, Favre-Nicolin V, Cox PA, Lightfoot P, Wright PA (2002) Al2(CH3PO3)3: Structure solution of a novel aluminium methylphosphonate using a new simulated annealing program and powder X-ray diffraction data. Chem Commun 8:808–809
Černý R, Filinchuk Y, Hagemann H, Yvon K (2007) Magnesium borohydride: synthesis and crystal structure. Angew Chem Int Ed 46:5765–5767
Her J-H, Stephens PW, Gao Y, Soloveichik GL, Rijssenbeek J, Andrus M, Zhao J-C (2007) Structure of unsolvated magnesium borohydride Mg(BH4)2. Acta Crystallogr B63:561–568
Černý R, Favre-Nicolin V (2007) Direct space methods of structure determination from powder diffraction: principles, guidelines and perspectives. Z Kristallogr 222:105–113
Altomare A, Caliandro R, Camalli M, Cuocci C, Giacovazzo C, Moliternia AGG, Rizzi R (2004) Automatic structure determination from powder data with EXPO2004. J Appl Crystallogr 37:1025–1028
Ravnsbæk D, Filinchuk Y, Cerenius Y, Jakobsen HJ, Besenbacher F, Skibsted J, Jensen TRM (2009) A series of mixed-metal borohydrides. Angew Chem Int Ed 48:6659–6663
Černý R, Kim KC, Penin N, D’Anna V, Hagemann H, Sholl DS (2010) AZn2(BH4)5 (A = Li, Na) and NaZn(BH4)3: structural studies. J Phys Chem C 114:19127–19133
Filinchuk Y, Chernyshov D, Nevidomskyy A, Dmitriev V (2008) High-pressure polymorphism as a step towards destabilization of LiBH4. Angew Chem Int Ed 47:529–532
Dai B, Sholl DS, Johnson JKJ (2008) First-principles study of experimental and hypothetical Mg(BH4)2 crystal structures. Phys Chem C 112:4391–4395
Filinchuk Y, Černý R, Hagemann H (2009) Insight into Mg(BH4)2 with synchrotron X-ray diffraction: structure revision, crystal chemistry, and anomalous thermal expansion. Chem Mater 21:925–933
Lindemann I, Ferrer RD, Dunsch L, Filinchuk Y, Cerný R, Hagemann H, D’Anna V, Lawson Daku LM, Latevi M, Schultz L, Gutfleisch O (2010) Al3Li4(BH4)13: a complex double-cation borohydride with a new structure. Chem Eur J 16:8707–8712
Djerdj I, Cao M, Rocquefelte X, Černý R, Jagličič Z, Arcon D, Potocnik A, Gozzo F, Niederberger M (2009) Structural characterization of a nanocrystalline inorganic–organic hybrid with fiberlike morphology and one-dimensional antiferromagnetic properties. Chem Mater 21:3356–3369
Evans IR, Howard JAK, Evans JSO (2003) α-Bi2Sn2O7 – a 176 atom crystal structure from powder diffraction data. J Mater Chem 13:2098–2103
Stinton GW, Evans JSO (2007) Parametric Rietveld refinement. J Appl Crystallogr 40:87–95
Müller M, Dinnebier RE, Ali Naveed Z, Campbell BJ, Jansen M (2010) Direct access to the order parameter: parameterized symmetry modes and rigid body movements as a function of temperature. Mater Sci Forum 651:79–95
Černý R, Ravnsbæk DB, Severa G, Filinchuk Y, D’Anna V, Hagemann H, Haase D, Jensen CM, Jensen TR (2010) Structure and characterization of KSc(BH4)4. J Phys Chem C 114:19540–19549
Černý R, Bonhomme F, Yvon K, Fischer P, Zolliker P, Cox DE, Hewat A (1992) Hexamagnesium dicobalt undecadeuteride Mg6Co2D11: containing CoD4 and CoD5 complex anions conforming to the 18-electron rule. J Alloy Compd 187:233–241
Ravnsbæk DB, Filinchuk Y, Černý R, Ley MB, Haase D, Jakobsen HJ, Skibsted J, Jensen TR (2010) Thermal polymorphism and decomposition of Y(BH4)3. Inorg Chem 49:3801–3809
Frommen C, Aliouane N, Daledda S, Fonneløp JE, Grove H, Lieutenant K, Llamas-Jansa I, Sartori S, Sørby MH, Hauback BCJ (2010) Crystal structure, polymorphism, and thermal properties of yttrium borohydride Y(BH4)3. Alloy Compd 496:710–716
Joubert J-M, Černý R, Latroche M, Percheron-Guégan A, Yvon K (1998) Site occupancies in the battery electrode material LaNi3.55Mn0.4Al0.3Co0.75 as determined by multiwavelength synchrotron powder diffraction. J Appl Crystallogr 31:327–332
Egami T, Billinge SJL (2003) Underneath the Bragg-peaks: structural analysis of complex materials. Pergamon Press, Oxford
Ropka J, Cerný R, Paul-Boncour VJ (2011) Local deuterium order in apparently disordered Laves phase deuteride YFe2D4.2. J Solid State Chem 184(9):2516–2524
Černý R, Renaudin G, Favre-Nicolin V, Hlukhyy V, Pöttgen R (2004) Mg1 + xIr1–x (x = 0, 0.037 and 0.054), a binary intermetallic compound with a new orthorhombic structure type determined from powder and single-crystal X-ray diffraction. Acta Crystallogr B 60:272–281
Filinchuk YE, Yvon K, Meisner GP, Pinkerton FE, Balogh MP (2006) On the composition and crystal structure of the new quaternary hydride phase Li4BN3H10. Inorg Chem 45:1433–1435
Filinchuk YE, Chernyshov D, Černý R (2008) The lightest borohydride probed by synchrotron diffraction: experiment calls for a new theoretical revision. J Phys Chem C 112:10579–10584
Acknowledgments
The author wants to thank to all users of Fox, and especially to them who have kindly provided the details of their work when solving the crystal structures.
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2012 Springer Science+Business Media Dordrecht
About this paper
Cite this paper
Černý, R. (2012). Inorganic Materials. In: Kolb, U., Shankland, K., Meshi, L., Avilov, A., David, W. (eds) Uniting Electron Crystallography and Powder Diffraction. NATO Science for Peace and Security Series B: Physics and Biophysics. Springer, Dordrecht. https://doi.org/10.1007/978-94-007-5580-2_4
Download citation
DOI: https://doi.org/10.1007/978-94-007-5580-2_4
Published:
Publisher Name: Springer, Dordrecht
Print ISBN: 978-94-007-5579-6
Online ISBN: 978-94-007-5580-2
eBook Packages: Physics and AstronomyPhysics and Astronomy (R0)