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PubMed2005

On the structure of aragonite.

High-resolution synchrotron powder diffraction measurements were carried out at the 32-ID beamline of the Advanced Photon Source of Argonne National Laboratory in order to clarify the structure of geological aragonite, a widely abundant polymorph of CaCO(3). The investigated crystals were practically free of impurity atoms, as measured by wavelength-dispersive X-ray spectroscopy in scanning electron microscopy. A superior quality of diffraction data was achieved by using the 11-channel 111 Si multi-analyzer of the diffracted beam. Applying the Rietveld refinement procedure to the high-resolution diffraction spectra, we were able to extract the aragonite lattice parameters with an accuracy of about 20 p.p.m. The data obtained unambiguously confirm that pure aragonite crystals have orthorhombic symmetry.

Journal Article↗
PubMed2005

Extremely long period-stacking structure in the Sb-Te binary system.

The crystal structure of the delta-phase in the Sb-Te binary system has been determined by synchrotron powder diffraction. It is clearly shown that many intermetallic compounds, which have different stacking periods depending on compound composition, exist in this phase. These structures are based on the cubic ABC stacking structure, and two kinds of fundamental structural units form an intergrowth along the stacking direction at the atomic level. The chemical formulae of these compounds are expressed as Sb(2n)Te3, where n is an integer and the number of stacking layers is 2n + 3. There is a relationship of inverse proportionality between the stacking period and the Te concentration.

Antimony↗
PubMed2005

Searching the Cambridge Structural Database for polymorphs.

In order to identify all pairs of polymorphs in the Cambridge Structural Database (CSD), a method was devised to automatically compare two crystal structures. The comparison is based on simulated powder diffraction patterns, but with special provisions to deal with differences in unit-cell volumes caused by temperature or pressure. Among the 325,000 crystal structures in the Cambridge Structural Database, 35,000 pairs of crystal structures of the same chemical compound were identified and compared. A total of 7300 pairs of polymorphs were identified, of which 154 previously were unknown.

Algorithms↗
PubMed2006

Structures and the oxygen deficiency of tetragonal and monoclinic zirconium oxide nanoparticles.

The crystal structure of zirconium oxide nanoparticles was refined by the Rietveld analysis of synchrotron X-ray powder diffraction data measured at 298 K. In the nanoparticles, two phases of tetragonal ZrO(2 - delta) (average particle size: 11 +/- 2 nm) and monoclinic ZrO2 (average particle size: 24 +/- 4 nm) existed, where the weight fractions were estimated to be 84.9 and 15.1 wt%, respectively. The structural refinement suggests that the tetragonal ZrO(2 - delta) has an oxygen deficiency [delta = 0.031 (7)] and that the monoclinic ZrO(2 - delta) has less oxygen deficiency (delta approximately 0), where delta is the vacancy concentration. The monoclinic ZrO2 has a larger unit-cell volume. The maximum-entropy method analysis indicated covalent bonding between Zr and O atoms.

Journal Article↗
PubMed2006

Cis/trans isomers of PtX2L2 (X = halogen, L = neutral ligand); the crystal structure of trans-dichlorobis(dimethyl sulfide)platinum(II) and the pressure dependence of its unit-cell dimensions.

trans-PtCl(2)(dms)(2) (dms is dimethyl sulfide) crystallizes in the space group P2(1)/n and adopts the molecular point group C(i), which is the most frequently occurring point group for trans-PtX(2)L(2) complexes (78%), as observed in the Cambridge Structural Database (CSD; 2005 release), followed by C(1) (16%). Density functional theory calculations show that the observed geometry for trans-PtCl(2)(dms)(2) has slightly higher energy than the most favorable geometry in the point group C(2h), but this geometry would require a space group that hampers close packing, thus showing that intermolecular forces determine the point group for the title compound. High-pressure powder diffraction studies of trans-PtCl(2)(dms)(2) show no phase transformation up to 8.0 GPa. The bulk modulus is 8.1 (6) GPa and the pressure derivative 8.1 (4). In the CSD, the number of cis- and trans-PtX(2)L(2) compounds are almost equal, viz. 156 cis and 160 trans compounds, showing no preference for either isomer in the solid state.

Journal Article↗
PubMed2006

Compressibility of the nitridosilicate SrYb[Si4N7] and the oxonitridoaluminosilicates MYb[Si4-xAlxOxN7-x] (x = 2; M = Sr, Ba).

The compressibilities of the nitridosilicate SrYb[Si(4)N(7)] and the oxonitridoaluminosilicates MYb[Si(4-x)Al(x)O(x)N(7-x)] (x = 2; M = Sr, Ba) were investigated by in situ high-pressure X-ray powder diffraction. Pressures up to 42 GPa were generated using the diamond-anvil cell technique. The title compounds are structurally stable to the highest pressure obtained. A fit of a third-order Birch-Murnaghan equation-of-state to the p-V data results in V(0) = 302.91 (6) A(3), B(0) = 176 (2) GPa and B' = 4.4 (2) for SrYb[Si(4)N(7)]; V(0) = 310.4 (1) A(3), B(0) = 161 (2) GPa and B' = 4.6 (2) for SrYb[Si(4-x)Al(x)O(x)N(7-x)]; and V(0) = 317.3 (5) A(3), B(0) = 168 (2) GPa and B' = 4.7 (2) for BaYb[Si(4-x)Al(x)O(x)N(7-x)]. While the linear compressibilities of the a and c axes of BaYb[Si(4-x)Al(x)O(x)N(7-x)] are very similar up to 30 GPa, distinct differences were observed for SrYb[Si(4)N(7)] and SrYb[Si(4-x)Al(x)O(x)N(7-x)], with the c axis being the most compressible axis. In all of the investigated compounds the bulk compressibility is dominated by the compression behaviour of the tetrahedral network, while the size of the substituted cation plays a minor role.

Journal Article↗
PubMed2006

Classification of stacking faults and their stepwise elimination during the disorder --> order transformation of nickel hydroxide.

Nickel hydroxide samples obtained by strong alkali precipitation are replete with stacking faults. The local structures of the stacking faults resemble the stacking patterns of different polytypic modifications that are theoretically possible among the layered hydroxides. This resemblance becomes a basis for the classification of stacking faults into different types. Each type of stacking fault produces a characteristic non-uniform broadening of peaks in the X-ray powder diffraction pattern of nickel hydroxide. DIFFaX simulations aid the classification and quantification of stacking faults. Hydrothermal treatment of a poorly ordered nickel hydroxide slurry at different temperatures (338-473 K) and different durations (5-48 h) shows that the stacking faults are removed in a stepwise manner. The as-precipitated sample has 17-20% stacking faults of the 3R(2) variety, which evolve into the 2H(2) type at 413 K. The 2H(2) stacking faults persist up to 443 K. The stacking faults are completely removed only at 473 K. At this temperature an ordered beta-Ni(OH)(2) phase is observed.

Journal Article↗
PubMed2006

The low-temperature phase III structure and phase transition behaviour of cyclohexanone.

The crystal structure of phase III of perdeuterocyclohexanone, C(6)D(10)O, has been determined at 5 K using high-resolution neutron powder diffraction. Below its melting point of 245 K cyclohexanone forms a plastic crystal in the space group Fm3m. On cooling below 225 K the crystal transforms to the monoclinic phase III structure in the space group P2(1)/n. The orthorhombic phase II structure exists under high pressure, but the triple point for all three phases is close to atmospheric pressure. Details of the phase II structure are also reported at 4.8 kbar (273 K) and ambient pressure. The phase behaviour of the compound and isotope effects are discussed.

Journal Article↗
PubMed2006

Structural phase transition and hydrogen ordering of TlH2PO4 at low temperature.

The crystal structure of TlH(2)PO(4) (TDP) has been studied at low temperature. The lattice parameters were derived from high-resolution X-ray powder diffraction in the temperature range between 8 and 300 K. A detailed crystal structure analysis of the antiferroelectric low-temperature phase TDP-III has been performed based on neutron diffraction data measured at 210 K on a twinned crystal consisting of two domain states. The structure model in the triclinic space group P\bar 1 is characterized by a complete ordering of all the H atoms in the asymmetric O-H...O hydrogen bonds. The phase transition from the ferroelastic TDP-II to the antiferroelectric TDP-III phase at 229.5 +/- 0.5 K is only slightly of first order and shows no detectable hysteresis effects. Its mechanism is driven by the hydrogen ordering between the partially ordered TDP-II state and the completely ordered TDP-III state. The polymorphism of TDP and the fully deuterated TlD(2)PO(4) (DTDP) is presented in the form of group-subgroup relations between the different space groups.

Journal Article↗
PubMed2006

Structures and phase transitions in the ordered double perovskites Ba2BiIIIBiVO6 and Ba2BiIIISbVO6.

High-resolution neutron powder diffraction has been used to investigate the structures and phase transitions in the double perovskites Ba(2)Bi(3+)Bi(5+)O(6) (dibarium dibismuth hexaoxide) and Ba(2)BiSbO(6) (dibarium bismuth antimony hexaoxide) in the temperature ranges 4.2-973 and 4.2-625 K, respectively. The charge-ordered bismuthate adopts four structures in the temperature range - monoclinic in P2(1)/n, monoclinic in I2/m, rhombohedral in R3, and finally cubic in Fm3m. The low-temperature monoclinic structure has been determined for the first time. The transitions from P2(1)/n to I2/m, at 132 K, and R3 to Fm3m, at 820 K, are tricritical in nature; the transition from I2/m to R3 at ca 430 K is discontinuous. The behaviour of Ba(2)BiSbO(6) is very similar, except that the transition temperatures are lower - 250 K for I2/m to R3 and 515 K for R3 to Fm3m - and the low-temperature structure is not formed at all. The R3 to Fm3m transition in this compound is closer to second order in nature, although there is evidence for some contribution from higher-order terms.

Journal Article↗
PubMed2006

On the compression mechanism of FeF3.

The structure of FeF3, iron trifluoride, has been studied in the pressure range from ambient to 8.28 GPa by time-of-flight neutron powder diffraction. No structural phase transitions were found within the investigated pressure range, and least-squares refinements of the crystal structures were performed in the space group R3c for all recorded data sets. It was found that volume reduction is achieved through rotation of the FeF6 octahedra, and the Fe-F-Fe bond angle decreases from 152.5 (2) to 134.8 (3) degrees within the investigated pressure range. A small octahedral strain was found to develop during compression, which reflects an elongation of the FeF6 octahedra along the c axis. The zero-pressure bulk modulus Bo and its pressure derivative B'o were determined to be 14 (1) GPa and 12 (1), respectively.

Journal Article↗
PubMed1999

Structures of 2,6-disubstituted naphthalenes.

The crystal structures of 2,6-naphthalenedicarboxylic acid (NDA) and dimethyl 2,6-naphthalenedicarboxylate (NDC) have been solved ab initio using a combination of X-ray powder diffraction and computational chemistry techniques. These two crystal structures, and that of 2,6-dimethylnaphthalene (DMN), have been refined by the Rietveld technique. DMN crystallizes in the orthorhombic space group Pbca, with a = 7.4544 (4), b = 6.0826 (6), c = 20.0946 (12) Å, V = 911.1 (1) Å(3) and Z = 4. The structure consists of a herringbone stacking parallel to a, resulting in loosely bound layers perpendicular to c. NDA crystallizes in the triclinic space group P1;, with a = 3.7061 (8), b = 7.4688 (14), c = 8.5352 (22) Å, alpha = 86.62 (2), beta = 85.49 (2), gamma = 87.99 (2) degrees, V = 235.00 (6) Å(3) and Z = 1. The structure consists of loosely packed hydrogen-bonded chains along [11;1]. NDC crystallizes in the monoclinic space group P2(1)/c, with a = 13.41931 (14), b = 6.14869 (5), c = 7.15257 (5) Å, beta = 100.400 (1) degrees, V = 580.47 (1) Å(3) at 300 K and Z = 2. The structure consists of layers of NDC molecules perpendicular to a. The ester group is twisted 20 degrees out of the mean ring plane in NDC. The conformations of the carboxyl groups in NDA and NDC differ. MP2 calculations suggest that the observed twist in NDC corresponds to an increase in conformational energy of 9 kJ mol(-1).

Journal Article↗
PubMed1999

Arrangement of C atoms in the SiC-C solid solution.

The microstructure of a silicon carbide-carbon solid-solution powder (SiC-C), obtained from a fine powder of silicon and thermal expansive graphite, is investigated by X-ray powder diffraction methods. The microstructure is characterized by Williamson-Hall analysis and the strain-field model suggested by van Berkum et al. [Acta Cryst. (1996), A52, 730-747]. SiC-C adopts a layered structure like the solid solutions formed by compounds possessing a diamond-like structure, e.g. SiC-AlN. Superstoichiometric C atoms are located as planar defects. The SiC-C solid solution is destroyed on heating in a vacuum in the temperature range of graphitization of diamond but is maintained after sintering at high pressure (4-8 GPa) and high temperature (1673 and 2073 K). However, at the higher temperature (2073 K), it is observed that planar defects formed by C atoms decompose to non-correlated point defects accompanied simultaneously by a decrease in the lattice parameter from 4.3540 (2) to 4.35234 (5) Å.

Journal Article↗
PubMed1999

Structural investigation of the negative-thermal-expansion material ZrW2O8.

High-resolution powder diffraction data have been recorded on cubic ZrW(2)O(8) [a = 9.18000 (3) Å at 2 K] at 260 temperatures from 2 to 520 K in 2 K steps. These data have confirmed that alpha-ZrW(2)O(8) has a negative coefficient of thermal expansion, alpha = -9.07 x 10(-6) K(-1) (2-350 K). A 'parametric' approach to Rietveld refinement is adopted and it is demonstrated that a full anisotropic refinement can be performed at each temperature, despite using a data collection time of only 5 min. Examination of the resulting structural parameters suggests that the origin of the contraction with increasing temperature can be traced straightforwardly to the rigid-body transverse librations of bridging O atoms. alpha-ZrW(2)O(8) undergoes a phase transition from P2(1)3 to Pa3; at 448 K that is associated with the onset of considerable oxygen mobility. The phase transition can be described in terms of a simple cubic three-dimensional Ising model. Unusual kinetics are associated with this phase transition. Hysteresis in the cell parameter through the phase transition is the opposite of that normally observed.

Journal Article↗
PubMed1999

Structures des phases paraélectrique et ferroélectrique de Pb2KNb5O15.

The paraelectric and the ferroelectric/ferroelastic structures of Pb(2)KNb(5)O(15) have been refined by the Rietveld method from neutron and X-ray powder diffraction data. The paraelectric phase is tetragonal (space group P4/mbm) with lattice parameters a(t) = 12.646 (1) and c(t) = 3.9551 (2) Å at 790 K. The Pb- and K-atom distribution has been determined. It was established that the Pb atoms situated on the 15-coordinate sites are not on the special position (2mm) but are distributed over two disordered positions as in the tetragonal phase of Pb(2)KTa(5)O(15). The ferroelectric/ferroelastic phase is orthorhombic. The space group of the average structure is Cm2m and the lattice parameters are a(o) = 17.779 (2), b(o) = 18.015 (2), c(o) = 3.9209 (4) Å at 294 K and a(o) = 17.756 (1), b(o) = 18.019 (1), c(o) = 3.9141 (2) Å at 81 K. It is isostructural with the average ferroelectric/ferroelastic structure of PbNb(2)O(6). The orthorhombic distortion is of the same order but the Curie temperature is lowered by the substitution 2K(+)-Pb(2+). The structures of PbNb(2)O(6), PbTa(2)O(6), Pb(2)KNb(5)O(15) and Pb(2)KTa(5)O(15) are compared. The ferroelectric polarization of the niobates is due to both the Pb off-site position and the Nb displacements, which induce a distortion of the oxygen lattice. In PbTa(2)O(6), the oxygen-lattice distortion is very weak. The polarization seems to be due only to the Pb atom. In the tantalates the substitution 2K(+)-Pb(2+) should weaken the correlations between the Pb atoms and consequently suppress the ferroelectric transition. Only a local polarization should take place; this might be the origin of the dielectric relaxation observed in this compound.

Journal Article↗
PubMed1999

Molecular co-crystals of 2-aminothiazole derivatives.

A series of molecular adducts of 2-aminothiazole derivatives - 2-aminothiazole, 2-amino-2-thiazoline and 2-aminobenzothiazole with the carboxylic-acid-substituted heterocyclics indole-2-carboxylic acid, N-methylpyrrole-2-carboxylic acid and thiophene-2-carboxylic acid - have been prepared and characterized using X-ray powder diffraction and in five cases by single-crystal X-ray diffraction methods. These five compounds are the adducts of 2-amino-2-thiazolium with indole-2-carboxylate [(C(3)H(7)N(2)S)(+)(C(9)H(6)NO(2))(-)], and N-methylpyrrole-2-carboxylate [(C(3)H(7)N(2)S)(+)-(C(6)H(6)NO(2))(-)], 2-aminobenzothiazolium with indole-2-carboxylate [(C(7)H(7)N(2)S)(+)(C(9)H(6)NO(2))(-)], N-methylpyrrole-2-carboxylate [(C(7)H(7)N(2)S)(+)(C(6)H(6)NO(2))(-)] and thiophene-2-carboxylate [(C(7)H(7)N(2)S)(+)(C(5)H(3)O(2)S)(-)]. All complexes involve proton transfer, as indicated by IR spectroscopy, while the five crystal structures display similar hydrogen-bonding patterns with the dominant interaction being an R(2)(2)(8) graph set dimer association between carboxylate groups and the amine/heterocyclic nitrogen sites. Futhermore, in each case a subsiduary interaction between an amino proton and a carboxylate oxygen completes a linear hydrogen-bonded chain. In addition to this, the indole-2-carboxylate molecules in the adduct structure with 2-amino-2-thiazolium form associated dimers which add to the hydrogen-bonding network.

Journal Article↗
PubMed1999

Crystal structure of moganite-type phosphorus oxynitride: relationship to other twinned-quartz-based structures.

The structure of moganite-type phosphorus oxynitride quenched from high-pressure high-temperature conditions has been refined using neutron powder diffraction data. This moganite-type structure, space group I2/a, Z = 12, is slightly less distorted with respect to the Imab aristotype than is moganite (a monoclinic form of silica). A close topological relationship has been identified between the moganite-type and orthorhombic BeH(2) structures indicating that SiO(2), PON and BeH(2) all adopt structures belonging to the twinned-quartz-based group. This group represents another possible structure type for systems composed of corner-sharing AX(4) tetrahedra. Structures of this group are obvious candidates for intermediate phases between the cristobalite and quartz types.

Journal Article↗
PubMed2000

High-pressure transformations of NbO2F

The ReO3-type structure NbO2F, niobium dioxyfluoride, has been studied at high pressures using diamond anvil cells and synchrotron X-ray radiation. High-pressure powder diffraction measurements have been performed up to 40.1 GPa. A phase transition from the cubic (Pm3m) ambient pressure structure to a rhombohedral (R3c) structure at 0.47 GPa has been observed. Rietveld refinements at 1.38, 1.96, 3.20, 6.23, 9.00 and 10.5 GPa showed that the transition involves an a-a-a- tilting of the cation-anion coordination octahedra and a change of the anion-anion arrangement to approach hexagonal close packing. Compression and distortion of the Nb(O/F)6 octahedra is also revealed by the Rietveld refinements. At 17-18 GPa, the diffraction pattern disappears and the structure becomes X-ray amorphous.

Journal Article↗