bluuebunny/crossref_metadata_2025 huggingface dataset:
What Counts as Effective Genetic Counselling for Presymptomatic Testing in Late‐Onset Disorders? A Study of the Consultand's Perspective
Authors: Guimarães Lídia , Sequeiros Jorge , Skirton Heather , Paneque Milena
Published: January 2013

Genetic counselling must be offered in the context of presymptomatic testing (PST) for severe late‐onset diseases; however, effective genetic counselling is not well defined, and measurement tools that allow a systematic evaluation of genetic practice are still not available. The aims of this qualitative study were to (1) recognize relevant aspects across the whole process of genetic counselling in PST for late‐onset neurodegenerative disorders that might indicate effective practice from the consultand's perspective; and (2) analyse aspects of current protocols of counselling that might be relevant for successful practice. We interviewed 22 consultands undergoing PST for late‐onset neurological disorders (Huntington disease, spinocerebellar ataxias and familial amyloid polyneuropathy ATTRV30M) in the three major counselling services for these diseases in Portugal. The main themes emerging from the content analysis were (1) the consultand's general assessment of the PST process in genetic services; (2) appropriateness and adaptation of the protocol to the consultand's personal expectations and needs; and (3) consultand's experience of the decision‐making process and the role of engagement and counselling skills of the counsellor. Participants also provided a set of recommendations and constructive criticisms relating to the length of the protocol, the time gap between consultations and the way results were delivered. These issues and the construction of the relationship between counsellor and counselee should be further investigated and used for the improvement of current protocols of counselling.
Membrane Cholesterol Affects Stimulus‐Activity Coupling in Type 1, but not Type 2, CCK Receptors: Use of Cell Lines with Elevated Cholesterol
Authors: Harikumar Kaleeckal G. , Potter Ross M. , Patil Achyut , Echeveste Valerie , Miller Laurence J.
Published: January 2013

The lipid microenvironment of membrane proteins can affect their structure, function, and regulation. We recently described differential effects of acute modification of membrane cholesterol on the function of type 1 and 2 cholecystokinin (CCK) receptors. We now explore the regulatory impact of chronic cholesterol modification on these receptors using novel receptor‐bearing cell lines with elevated membrane cholesterol. Stable CCK1R and CCK2R expression was established in clonal lines of 25RA cells having gain‐of‐function in SCAP [sterol regulatory element binding protein (SREBP) cleavage‐activating protein] and SRD15 cells having deficiencies in Insig‐1 and Insig‐2 enzymes affecting HMG CoA reductase and SREBP. Increased cholesterol in the plasma membrane of these cells was directly demonstrated, and receptor binding and signaling characteristics were shown to reflect predicted effects on receptor function. In both environments, both types of CCK receptors were internalized and recycled normally in response to agonist occupation. No differences in receptor distribution within the membrane were appreciated at the light microscopic level in these CHO‐derived cell lines. Fluorescence anisotropy was studied for these receptors occupied by fluorescent agonist and antagonist, as well as when tagged with YFP. These studies demonstrated increased anisotropy of the agonist ligand occupying the active state of the CCK1R in a cholesterol‐enriched environment, mimicking fluorescence of the uncoupled, inactive state of this receptor, while there was no effect of increasing cholesterol on fluorescence at the CCK2R. These cell lines should be quite useful for examining the functional characteristics of potential drugs that might be used in an abnormal lipid environment.
Nutrition impact symptoms in advanced cancer patients: frequency and specific interventions, a case–control study
Authors: Omlin Aurelius , Blum David , Wierecky Jan , Haile Sarah R. , Ottery Faith D. , Strasser Florian
Published: January 2013

Background

Involuntary weight loss (IWL) is frequent in advanced cancer patients causing compromised anticancer treatment outcomes and function. Cancer cachexia is influenced by nutrition impact symptoms (NIS). The aim of this study was to explore the frequency of NIS in advanced patients and to assess specific interventions guided by a 12‐item NIS checklist.

Methods

Consecutive patients from an outpatient nutrition‐fatigue clinic completed the NIS checklist. The NIS checklist was developed based on literature review and multiprofessional clinical expert consensus. Chart review was performed to detect defined NIS typical interventions. Oncology outpatients not seen in the nutrition‐fatigue clinic were matched for age, sex, and tumor to serve as controls.

Results

In 52 nutrition‐fatigue clinic patients, a mixed cancer population [IWL in 2 months 5.96 % (mean)], the five most frequent NIS were taste and smell alterations 27 %, constipation 19 %, abdominal pain 14 %, dysphagia 12 %, and epigastric pain 10 %. A statistically significant difference for NIS typical interventions in patients with taste and smell alterations (p = 0.04), constipation (p = 0.01), pain (p = 0.0001), and fatigue (p = 0.0004) were found compared to the control population [mixed cancer, 3.53 % IWL in 2 months (mean)].

Conclusion

NIS are common in advanced cancer patients. The NIS checklist can guide therapeutic nutrition‐targeted interventions. The awareness for NIS will likely evoke more research in assessment, impact, and treatment.
Occurrence and Positive Predictive Value of Additional Nonmass Findings for Risk Stratification of Breast Microcalcifications in Mammography
Authors: Rominger Marga B. , Sax Eva V. , Figiel Jens H. , Timmesfeld Nina
Published: January 2013

Purpose

To assess the occurrence and positive predictive value of additional nonmass findings to stratify the risk of breast microcalcifications.

Methods

This retrospective evaluation included 278 lesions with vacuum- or image-guided hook-wire biopsy for suspicious microcalcifications. The lesions were categorized into exclusive microcalcifications and microcalcifications with focal asymmetry, tubular density or architectural distortion (ie, nonmass findings). To evaluate the utility of additional nonmass findings for risk stratification, outcome variables were positive predictive values and odds ratios for malignancy and invasive carcinoma.

Results

Forty-five of 278 microcalcification lesions (16%) were associated with nonmass findings: 28 focal asymmetries, 2 tubular densities, and 15 focal asymmetries in conjunction with tubular densities. Architectural distortion was observed in 28 of these cases. The odds ratio for additional nonmass findings relative to exclusive microcalcifications was 5.9 and was statistically significant ( P < .00001). Architectural distortion was the most specific indicator for malignancy and invasiveness, with odds ratios of 6.5 ( P = .0072) and 5.6 ( P = .0214), respectively.

Conclusions

Microcalcifications with nonmass findings were less frequent than exclusive microcalcifications but were more predictive for malignancy. Architectural distortion demonstrated the highest risk of malignancy and invasiveness. Assessment of additional nonmass findings might be useful for further risk stratification of microcalcifications, indications for additional imaging, and pretreatment considerations.
Lipid droplet synthesis is limited by acetate availability in starchless mutant of Chlamydomonas reinhardtii
Authors: Ramanan Rishiram , Kim Byung-Hyuk , Cho Dae-Hyun , Ko So-Ra , Oh Hee-Mock , Kim Hee-Sik
Published: January 2013

Phenotypic and genotypic changes in Chlamydomonas reinhardtii BafJ5, a starchless mutant, with respect to lipid metabolism was studied in different trophic states under nitrogen (N) sufficient and limited conditions. Interestingly, cellular lipid content increased linearly with input acetate concentration with highest lipid content (∼42%) under nitrogen limitation and mixotrophic state. RT‐qPCR studies indicate that key fatty acid biosynthesis genes are down‐regulated under N limitation but not under mixotrophic state, whereas, ACS2, encoding Acetyl‐CoA synthetase, and DGTT4, encoding Diacylglycerol O‐acyltransferase, are up‐regulated under all conditions. These results collectively indicate that acetate is the limiting factor and central molecule in lipid droplet synthesis. The study also provides further evidence of the presence of a chloroplast pathway for triacylglycerol synthesis in microalgae.
Preventive Health Care Among Community‐Dwelling Persons with Spinal Cord Injury
Authors: Roach Mary Joan , Nagy Jennifer A. , Mejia Melvin , Nemunaitis Gregory
Published: January 2013

Objective

To describe preventive health examinations/tests and behaviors of persons with traumatic spinal cord injury (SCI).

Design

Survey.

Setting

SCI clinic and telephone contact.

Participants

A total of 59 persons ≥18 years of age with traumatic SCI.

Intervention

None.

Main Outcome Measures

Preventive health examinations/tests and reason for not receiving an examination or test.

Results

Preventive health tests/examinations received within the past year: flu vaccination (40.7%); eye examination (50.8%); dental check‐up (64.4%); physical examination (61.0%); vitamin D level (56.0%); cholesterol level (25.4%); and blood glucose level (39.0%). For men, 20.0% had a prostate examination and 20.0% had a colonoscopy. For women, 25.0% had a pelvic examination and 62.5% had a mammogram in the past 2 years. The most endorsed reasons for not getting an examination/test was “It was my choice” followed by “No one told me to have [examination/test].” The number of years injured had an inverse relationship with having vitamin D level checked (r = −334) and had a positive association with having serum cholesterol level checked (r = .474).

Conclusion

Preventive health tests and examinations in the SCI population are being obtained at about the same rate as in the U.S. population with some exceptions (ie, cholesterol level check, colonoscopy, and pelvic examination); however, the rates are far from the goals of Healthy People 2020. Primary care and SCI clinicians should be proactive in educating their patients about the importance of preventive health, especially those who have been injured for a long time.
Tolerability and Effectiveness of a Neuroprosthesis for the Treatment of Footdrop in Pediatric Patients With Hemiparetic Cerebral Palsy
Authors: Meilahn Jill R.
Published: January 2013

Objective

To assess the tolerability and efficacy of a commercially available footdrop neuroprosthesis for treatment of footdrop in children with hemiparetic cerebral palsy.

Design

A prospective, observational pilot study.

Setting

Marshfield Clinic, Department of Physical Medicine.

Participants

Ten children, ages 7‐12 years, with hemiparetic cerebral palsy, who use an ankle foot orthosis (AFO) for correction of footdrop.

Methods

Children replaced their AFO with a transcutaneous peroneal (fibular) nerve stimulation neuroprosthesis for 3 months.

Main Outcome Measurements

The ability to tolerate fitting and programming of the device, device‐recorded wear time, a daily‐use diary, satisfaction survey, and secondary measures, including passive range of motion and gait laboratory measurement of gait velocity and ankle kinematics.

Results

All 10 participants (100%) tolerated fitting and programming of the neuroprosthesis and wore the device for 6 weeks. Seven of 10 (70%) wore the device for the entire 3‐month study period; 6 of 10 (60%) continued to use the device after study completion. Wear time varied from 2 to 11 hours per day. Tolerability and satisfaction were high; although 6 participants complained of “size” and “bulkiness” of the device, and 2 reported skin irritation. Gait velocity increased in 5 subjects (50%). Seven participants (70%) preferred the neuroprosthesis to their AFO.

Conclusion

Analysis of the preliminary evidence suggests that electrical stimulation by a footdrop neuroprosthesis is tolerated well by children and is effective for the treatment of footdrop in children with hemiparetic cerebral palsy. Commercially available neuroprostheses may offer a promising alternative treatment option for children with footdrop.
The nitric oxide synthase inhibitor and serotonin-receptor agonist NXN-188 during the aura phase of migraine with aura: A randomized, double-blind, placebo-controlled cross-over study
Authors: Hougaard Anders , Hauge Anne Werner , Guo Song , Tfelt-Hansen Peer
Published: January 2013

Background and aims

NXN-188 is a combined neuronal nitric oxide synthase (nNOS) inhibitor and 5HT-1B/1D receptor agonist which has previously shown efficacy in the acute treatment of migraine. Nitric oxide (NO) is involved in the pathogenesis of migraine pain and is formed after cortical spreading depression. Therefore NXN-188 could perhaps prevent the development of the headache phase in migraine with aura if taken during the aura. The aims of the present study were to evaluate the efficacy and safety of 600mg NXN-188 in the acute treatment of migraine when dosed during the aura.

Methods

A single-centre, randomized, double-blind, placebo-controlled, two-way crossover trial. The study medication was taken during the aura and the patients kept a study diary for 48h post-dose.

Results

Of 615 patients screened, 50 patients were included in the study and randomized. Only 18 patients completed both treatments in compliance with the study procedures. 22% of patients reported freedom of headache at 2h after intake of NXN-188 compared with only 11% of patients after placebo.

Conclusions

The dual-action drug NXN-188 with 5HT-1B/1D agonism and nNOS inhibition, taken orally during the aura phase did not have a statistically substantial effect on migraine headache in this study. This study was limited by a high drop-out rate and small sample of included patients who were able to complete the cross-over protocol. Therefore, efficacy of the treatment cannot be refuted with certainty.

Implications

This study illustrates the difficulties of doing well controlled studies in migraine patients with aura. nNOS inhibition is expected to be effective mostly in the aura phase, i.e. the oral administration may have had too slow pharmacokinetics to have effect. Parenteral administration may overcome this obstacle. 5HT-1B/1D agonism is not effective when dosed during migraine aura. Repeated dosing of the NXN-188 during and immediately following the aura may have exploited more the dualaction. The high drop-out rate may be reduced in future studies by having the patients familiarize themselves with the study procedure by filling out the attack report form while treating one attack with their own medication before entering the trial. A parallel group comparison may be a more effective trial design for treatment during an aura.
X-ray powder diffraction data for Ba3MnSi2O8—A new phase in the system BaO–MnO–SiO2
Authors: Georgieva Irena , Ivanov Ivan , Petrov Ognyan
Published: January 2013

A new compound—Ba3MnSi2O8 in the system BaO–MnO–SiO2 was synthesized and studied by powder X-ray diffraction. The compound is hexagonal, space group—P6/mmm, a=5.67077 Å, c=7.30529 Å, Z=1, Dx=5.353. The obtained powder X-ray diffractometry (XRD) data were interpreted by the Powder Data Interpretation Package.
Powder diffraction of La1−xAxCo0.8Fe0.2O3(A=Sr,Ba)
Authors: ten Elshof Johan E. , Boeijsma Jaap
Published: January 2013

Powder X-ray diffraction data are reported for La1−xSrxCo0.8Fe0.2O3 (x=0.2, 0.4) and La0.8Ba0.2Co0.8Fe0.2O3. The powders were prepared by thermal decomposition of metal-containing complex solutions. All compositions have rhombohedral unit cells. In hexagonal setting, the cell parameters are a=5.4451(2) Å, c=13.2553(2) Å for La0.6Sr0.4Co0.8Fe0.2O3; a=5.4556(3) Å, c=13.1999(2) Å for La0.8Sr0.2Co0.8Fe0.2O3 and a=5.4795(1) Å, c=13.2983(5) Å for La0.8Ba0.2Co0.8Fe0.2O3. The space group is probably R3c (167) for all three compositions.
About the crystal structure of La1−xSrxCoO3−δ (0≤x≤0.6)
Authors: Closset Nicole M. L. N. P. , van Doorn René H. E. , Kruidhof Henk , Boeijsma Jaap
Published: January 2013

The crystal structure of La1−xSrxCoO3−δ (0≤x≤0.6) has been studied, using powder X-Ray diffraction. The crystal structure shows a transition from rhombohedral distorted perovskite for LaCoO3−δ into cubic perovskite for La0.4Sr0.6CoO3−δ. The cubic unit cell parameter is ac=3.8342(1) Å for La0.4Sr0.6CoO3−δ, the space group probably being Pm3m. Using a hexagonal setting, the cell parameters for La0.5Sr0.5CoO3−δ, are a=5.4300(3) Å, c=13.2516(10) Å; a=5.4375(1) Å, c=13.2313(4) Å for La0.6Sr0.4CoO3−δ; a=5.4437(1) Å, c=13.2085(5) Å for La0.7Sr0.3CoO3−δ; a=5.4497(2) Å, c=13.1781(6) Å for La0.8Sr0.2CoO3−δ and a=5.4445(2) Å, c=13.0936(6) Å for LaCoO3−δ with the space group probably being R3c.
Lattice parameters determination from powder diffraction data: Results from a round robin project
Authors: Masciocchi Norberto , Artioli Gilberto
Published: January 2013

A well-crystallized sample of powdered KCl has been distributed among several laboratories in order to test the reproducibility of the lattice parameter measurement on different X-ray powder diffraction instruments. The precision of the determined unit-cell dimension is in the 10−5 Å range, while the discrepancies among the results from different laboratories using the same numerical analysis are at least one order of magnitude higher. It is shown that if different numerical analyses, including full pattern refinement, are used, values differing in the third decimal digit are obtained for the same data set.
X-ray powder diffraction characterization of Bi14(Sr,Ca)12O33 solid solutions
Authors: Wong-Ng Winnie , Jiang F. , Jarabek Bryan R. , McCarthy Gregory J.
Published: January 2013

Powder X-ray diffraction was used to investigate the solid solution range of the Bi14SrxCa12−xO33 series in the Bi–Sr–Ca–O system. Solid solution forms over the range 1≤x≤7 in Bi14SrxCa12−xO33. Experimental X-ray reference patterns of selected members with x=1, 3, 5, and 7 have been prepared for the powder diffraction file (PDF). These phases are monoclinic, C2/m, with cell parameter a ranging from 21.473(4) to 21.868(4) Å, b from 4.3564(9) to 4.3898(9) Å, c from 12.753(2) to 12.962(2) Å, β from 102.91(2)° to 102.79(1)°, and V from 1162.9(3) to 1213.5(3) Å3, respectively. These parameters increase monotonically as Ca is continuously replaced by the larger Sr.
The ICDD/PDF Superconductor SubFile
Authors: Wong-Ng W. , Snyder R. L. , Park C. , Antipov E. , McClune W. F.
Published: January 2013

The activity of the high Tc task group of the ICDD Ceramic Subcommittee is described. This activity includes the compilation of X-ray powder diffraction patterns of the high Tc superconductors and related phases identified from the International Centre for Diffraction Data/Powder Diffraction File (ICDD/PDF). The coverage of this ICDD/PDF Superconductor SubFile (SC) includes high Tc phases and their structurally related phases, products of elemental substitution in the high Tc phases, phases found in the phase diagrams containing the high Tc phases, as well as potential reaction products with commonly used sample containers, and potential conventional low-temperature (metallic and nonmetallic) superconductors.
Crystal structure of KCaF3 determined by the Rietveld profile method
Authors: Ratuszna Alicja , Rousseau Michel , Daniel Philippe
Published: January 2013

Using the Rietveld profile method, the atomic coordinates and anisotropic temperature factors of KCaF3 were refined. At room temperature, KCaF3 crystallizes in monoclinic B21/m symmetry, with the lattice parameters: a=8.754(2) Å, b=8.765(4) Å, c=8.760(5) Å, β=90.48(3)°, V=672.1(3) Å3, Z=8. The refinement procedure was stopped when RB=0.05 and the Durbin–Watson statistic factor=0.85 had been reached. The structure determined is related to the tilting of CaF6 octahedra of the a−b+c− type, which are responsible for the monoclinic distortion in perovskite crystals.
X-ray diffraction study of HgBa2CuO4+δ at high pressures
Authors: Gonzalez Eduardo J. , Wong-Ng Winnie , Piermarini Gasper J. , Wolters Christian , Schwartz Justin
Published: January 2013

An in situ high pressure study using energy dispersive X-ray diffraction has been carried out on the polycrystalline high-Tc superconductor, HgBa2CuO4+δ (Hg-1201), to study its phase stability under pressure and also to measure its compressibility and bulk modulus. No evidence of pressure-induced polymorphism was found in the pressure range investigated, i.e., from 0.1 MPa (1 atm) to 5 GPa. The compound exhibited anisotropic elastic properties. The axial compressibility along the c axis was measured to be (3.96±0.35)×10−3GPa−1 and along the a axis (3.42±0.13)×10−3GPa−1, corresponding to an anisotropy ratio of 1.16±0.11. The bulk modulus was determined to be (94.7±4.2) GPa and, assuming a Poisson's ratio of 0.2, Young's modulus was estimated to be (170±8) GPa.
X-ray powder diffraction data for compound DyNiSn
Authors: Nong Liangqin , Zeng Lingmin , Hao Jianmin
Published: January 2013

The compound DyNiSn has been studied by X-ray powder diffraction. The X-ray diffraction patterns for this compound at room temperature are reported. DyNiSn is orthorhombic with lattice parameters a=7.1018(1) Å, b=7.6599(2) Å, c=4.4461(2) Å, space group Pna21 and 4 formula units of DyNiSn in unit cell. The Smith and Snyder Figure-of-Merit F30 for this powder pattern is 26.7(0.0178,63).
Crystallographic data about hydrated and anhydrous lithium monoborates
Authors: Bétourné E. , Touboul M.
Published: January 2013

The anhydrous and hydrated lithium monoborates have been studied. The most hydrated phase is LiBO2·8H2O; its structural formula in the P3 space group is Li(H2O)4B(OH)4·2H2O. Refinement of the cell parameters yielded the following results: a=6.5483(5) Å, c=6.1692(7) Å with F(30)=64(0.015, 32), Z=1, and Dx=1.402 g/cm3. This phase gives LiB(OH)4 by spontaneous dehydration. An X-ray powder diffraction study of LiB(OH)4 as a function of temperature indicated three poorly crystallized hydrates. Two of these hydrates have the formula LiBO2·0.3H2O; the other, LiBO2·xH2O, has an undetermined water content. Crystal data for α-LiBO2 have been obtained: a=5.8473(10) Å, b=4.3513(6) Å, c=6.4557(10) Å, β=115.08(1)°, F(27)=58.5(0.001, 41); space group P21/c, Z=4, and Dx=2.18 g/cm3. β-LiBO2 does not exist but corresponds to the α-LiBO2 form observed at 600 °C. Numerous other LiBO2 forms reported recently have not been found.
Powder diffraction data for the intermetallic compoundsRhAl2.63,IrAl2.75andAuZn3
Authors: Gotzmann K. , Burkhardt U. , Ellner M. , Grin Yu.
Published: January 2013

A significant feature of the atomic structure of the intermetallic compoundsRhAl2.63(Pearson-Parthé symbolcP(34-5) [notation according to Parthéet al.(1993)], space groupP23),IrAl2.75(cP(34-4),P23) andAuZn3(cP32,Pm3¯n) is the occurrence of icosahedral clusters. Least squares refined lattice parameters and powder diffraction data are reported for these homeotypic phases.
The quantification of lateritic bauxite minerals using X-ray powder diffraction by the Rietveld method
Authors: Aylmore Mark G. , Walker Graham S.
Published: January 2013

The application of the Rietveld method to quantify mineral components of bauxite and lateritic samples was carried out in order to determine the ability of the method to obtain accurate mineralogical abundances for these materials. The method was initially applied to synthetic mixtures using both Cu and Co Kα radiations, and it was shown that Rietveld-derived data compared favourably with the weighed compositions. Application to two types of natural bauxite resulted in a high correlation between Rietveld predicted values and those calculated by proportioning peak intensities with chemical assays. The use of the whole pattern rather than selected peak intensities gives greater accuracy, confirmed by a strong correlation between derived oxide concentrations from XRF assays. Accuracy and precision were improved by the determination of isomorphous substitution of aluminum in goethite and hematite by refinement of unit cell dimensions. Importantly, the ability of the Rietveld program to successfully model several goethites with different levels of isomorphous substitution improved the correlation between predicted and calculated values. In addition, crystallinity and crystallite size that influence the reactivity of the mineral components can be derived from refined peak profiles.
Characterization of standard reference materials for obtaining instrumental line profiles
Authors: Leoni Matteo , Scardi Paolo , Langford J. Ian
Published: January 2013

Standard Reference Materials (SRMs) for determining instrumental line profiles should not exhibit measurable broadening from structural imperfections, but owing the effects of sample transparency and other geometrical effects, the quality of possible SRMs cannot necessarily be assessed satisfactorily with data from a conventional divergent-beam diffractometer. The problem of transparency can be avoided if parallel beam optics is used, as for instance on a synchrotron radiation powder diffraction station employing Parrish (Soller-type receiving slit assembly) geometry. Data from such a configuration are used to compare three SRMs commonly used in line-profile analysis.
Ab initio determination and Rietveld refinement of the crystal structure of Ni0.50TiO(PO4)
Authors: Gravereau P. , Chaminade J. P. , Manoun B. , Krimi S. , El Jazouli A.
Published: January 2013

The structure of the oxyphosphate Ni0.50TiO(PO4) has been determined ab initio from conventional X-ray powder diffraction data by the “heavy atom” method. The cell is monoclinic (space group P21/c, Z=4) with a=7.3830(5) Å, b=7.3226(5) Å, c=7.3444(5) Å, and β=120.233(6)°. Refinement of 46 parameters by the Rietveld method, using 645 reflexions, leads to cRwp=0.152, cRp=0.120, and RB=0.043. The structure of Ni0.50TiO(PO4) can be described as a TiOPO4 framework constituted by chains of tilted corner-sharing TiO6 octahedra running parallel to the c axis, crosslinked by phosphate tetrahedra and in which one-half of octahedral cavities created are occupied by Ni atoms. Ti atoms are displaced from the center of octahedra units in alternating long (2.231) and short (1.703 Å) Ti–O bonds along chains.
farhan—a qualitative and quantitative PC program for X-ray powder diffraction
Authors: AL-Farhan Khalid A.
Published: January 2013

FARHAN is a PC interactive, graphically oriented search–match–identification–quantification computer program for X-ray powder diffraction, which uses a variable intensity-error window (IEW). Both the intensity scale factor and the IEW for each standard phase are estimated by a simple iterative procedure. A new tunable combined figure-of-merit (agreement function) is suggested for estimating the goodness-of-fit of matches. The concentrations of the identified phases may be determined by normalized or generalized RIR quantification methods, if the RIRs of the identified phases are known.
Use of an ellipsoid model for the determination of average crystallite shape and size in polycrystalline samples
Authors: Balić Žunić Tonči , Dohrup Jesper
Published: January 2013

A mathematical model for interpreting the anisotropical broadening of the powder diffraction lines by an average crystallite in the form of a triaxial ellipsoid is developed. The model covers satisfactorily a broad range of averaged crystallite shapes in polycrystalline samples of all crystal symmetries and provides simple formulas for use in powder pattern fitting routines. When ra, rb, rc are the principal ellipsoid radii, and ca, cb, cc direction cosines of diffraction vector related to the principal axes of ellipsoid, the average dimension of crystallites along the diffraction vector (Dhkl) is: Dhkl=K/ca2/ra2+cb2/rb2+cc2/rc2. The coefficient K has the value 3/2 if Dhkl is the volume average dimension of crystallites along the diffraction vector, or 4/3 in the case of the surface average dimension. The appropriate expression for use in whole pattern fitting routines is: b11h2+b22k2+b33l2+2b12hk+2b13hl+2b23kl=K2/Lhkl2dhkl2, where bij are the elements of a second-rank symmetric tensor. Finding eigenvalues and vectors of tensor b gives dimensions and orientations of the principal ellipsoid radii in reciprocal lattice values.
X-ray powder diffraction data ofAII(ZnXVO4)2compounds (A=Sr, Ba;X=P, As)
Authors: Lucas F. , Elfakir A. , Quarton M.
Published: January 2013

Two new arsenates with general formulaAII(ZnAsO4)2(A=Sr, Ba) were synthetized by solid state reaction. Furthermore, a high pressure form ofBa(ZnPO4)2was obtained under hydrothermal conditions. Indexing of their X-ray diffractograms was carried out with a monoclinic unit-cell and space groupP21/c. These compounds are isostructural withSr(ZnPO4)2and the paracelsian form ofBa(AlSiO4)2.
XLENS, a direct methods program based on the modulus sum function: Its application to powder data
Authors: Rius Jordi
Published: January 2013

XLENS is a traditional direct methods program working exclusively in reciprocal space. The distinctive feature of XLENS is the use of the modulus sum function as target function for the phase refinement. Due to its efficiency, robustness, and no need of weighting schemes, this function is specially well suited for treating powder diffraction data. The mathematical basis as well as the significance of the most important control parameters of the program will be described here. To illustrate how XLENS works, three different examples will be shown. Due to its simplicity, the modulus sum function can be easily combined with real-space filtering procedures to produce even more efficient crystal structure solving strategies.
Heating device for high temperature X-ray powder diffraction studies under controlled water vapour pressure (0–1000 mbar) and gas temperature (20–200 °C)
Authors: Oetzel Martin , Scherberich Franz-Dieter , Heger Gernot
Published: January 2013

In this paper we present a high temperature heating device, working under defined environmental conditions, for a Siemens D500 Bragg–Brentano powder diffractometer. The powder sample is prepared in a flat mould on a metal block consisting either of copper or of platinum depending on the temperature range selected for investigations. Although the heating cell can be used separately under ambient conditions up to sample temperatures of 1000 °C, it is possible to work under defined environmental conditions in the temperature range between 20 and 200 °C and up to a water vapour pressure of 1000 mbar. For that purpose a special cover for the in situ control of temperature and water vapour pressure has been constructed. It is important to note that the three sample conditions (sample temperature, gas temperature, and gas humidity) can be adjusted separately by the user. Current studies have shown that the described X-ray heating device is a powerful tool to study dehydration reactions in the frame of fundamental research as well as to understand industrially relevant processes concerning dehydration reactions and their mechanisms.
Improved powder X-ray data for the cement phaseCa12Al14O32F2(C11A7f)
Authors: Costa Umberto , Ballirano Paolo
Published: January 2013

New powder X-ray diffraction data ofCa12Al14O32F2(C11A7f), a cementitious compound, were collected on a conventional X-ray powder diffractometer; the cubic cell parameter isa=11.96269(6) Å, volume 1711.93(2) Å3(space groupI-43d(No. 220)). The strongest lines are 4.887(100), 2.676(95), 2.992(46), 2.443(46), 2.185(37), 3.198(32), 1.599(26), and 1.941(25). Reported intensities are validated by Rietveld analysis. The new data consist of measured intensities and cover a wider 2θ angular range with respect to the calculated PDF 25-394 and the indexed PDF 36-678: experimental, calculated, and difference patterns are reported together with crystal-chemical considerations.
Powder X-ray data for adenosineC10H13N5O4
Authors: Caminiti Ruggero , Ortaggi Giancarlo , Mazzei Raffaele Antonio , Ballirano Paolo , Rizzi Rita
Published: January 2013

New powder X-ray diffraction data of adenosineC10H13N5O4were reported: cell parameters area=4.8386(4) Å,b=10.2919(4) Å,c=11.8555(4) Å,β=99.298(5)°, volume 582.63(4)Å for the monoclinic space groupP21. The strongest lines are: 7.723 (100), 5.085 (50), 5.851 (45), 4.710 (11), 3.881 (10), 3.899 (9), 3.292 (9), and 3.261 (9). Reported intensities are validated by Rietveld analysis. The data consist of measured positions and intensities and cover an angular range up to 75° 2θ and are significantly better than PDF 35-1977. Experimental, calculated, and difference patterns are also reported.
Crystal structure and X-ray powder diffraction pattern of Ti2ZrAl
Authors: Sornadurai D. , Panigrahi B. , Sastry V. S. , Ramani
Published: January 2013

We report precision X-ray powder-diffraction (XRD) data of single phase pure Ti2ZrAl. Ti2ZrAl samples were prepared by an arc melting method and annealed at 1000 °C for 30 days. XRD analysis was carried out on these samples and it was found that Ti2ZrAl has a DO19 structure (space group P63/mmc, No. 194). The lattice parameters are found to be a=5.961±0.001 Å and c=4.793±0.001 Å.
X-ray powder diffraction data and Rietveld refinement for Ln6WO12 (Ln=Y, Ho)
Authors: Diot N. , Bénard-Rocherullé P. , Marchand R.
Published: January 2013

The crystal structure of the two isostructural rare earth tungstates Ln6WO12 (Ln=Y, Ho) has been refined by the Rietveld method from X-ray powder diffraction data. They crystallize with a three-dimensional rhombohedral structure (S.G. R3¯ and Z=3 for the R-centered setting) closely related to that of the binary oxides Ln7O12 and deriving from the ideal fluorite structure. Final refinements, with isotropic thermal motion for each atom, resulted in profile and structure factors Rwp=0.166, RF=0.037 with Ln=Y and Rwp=0.121, RF=0.040 with Ln=Ho. The rare earth element is sevenfold coordinated with Ln–O bond lengths ranging from 2.19 to 2.70 Å for Y6WO12 and from 2.18 to 2.68 Å for Ho6WO12; the coordination polyhedron may be described as a monocapped trigonal prism. The tungsten atom is located at the center of a WO6 octahedron with a unique W–O distance of 1.98 and 1.92 Å for Y6WO12 and Ho6WO12, respectively.
Données Cristallographiques Sur Le Trioxalato-Chromate(III) De Potassium Trihydrate: K3(Cr(C2O4)3).3H2O
Authors: Merrachi E. H. , Chassagneux F. , Mentzen B. F.
Published: January 2013

The trihydrated potassium trioxalato-chromate(III), K3(Cr(C2O4)3).3H2O, crystallizes in the monoclinic system with:

the space group is P21/c.
“PC-PDF”: A Search/Display System Utilizing the CD-ROM and the Complete Powder Diffraction File
Authors: Jenkins R. , Holomany M.
Published: January 2013

The Powder Diffraction File (PDF) is a collection of single phase X-ray powder patterns, maintained and distributed by the JCPDS-International Centre for Diffraction Data. Over the past 10 years there has been increasing use of the PDF in computer readable form, but the limited amount of disk space available on most commercial powder diffractometer systems has limited use to a small subset of the total PDF. The recent availability of low-cost Compact Disk Read Only Memory (CD-ROM) systems offers an attractive alternative to conventional disk media. This paper describes a low-cost Personal Computer/CD-ROM system, “PC-PDF”, having a total available storage of 550 Mbytes. While seek times are relatively slow – typically, 0.5 seconds are required to traverse the complete PDF – by use of optimum packing and access algorithms, search strategies based on PDF numbers, chemistry, strongest d-spacing, etc., operate at a speed causing no great inconvenience to the user.
Characterization of CoCrTa Alloy Thin Films by X-Ray Powder Diffraction
Authors: Huang T. C.
Published: January 2013

Crystalline structures of one single- and two multi-layer magnetic CoCrTa films were characterized by X-ray powder diffraction technique. Structural parameters such as crystalline phase, preferred orientation, crystallite size and microstrain (which control the magnetic properties) have been determined. Polycrystalline diffractions from lattice planes parallel and perpendicular to the surface of a film were obtained with the specimen in reflection and in transmission, respectively. Phase identification of the ternary alloy (Co85Cr15)90Ta10 magnetic layers of the specimens indicated a disordered solid solution of Cr and Ta in Co, and the alloy has a hexagonal close-packed (h.c.p.) (A3) structure. Line broadening analysis showed crystallite size anisotropy and columnar CoCrTa grains. The crystal growth was disrupted by the nonmagnetic “amorphous” spacing layers in the multi-layer specimens. The disruption increased with the decreasing magnetic layer thickness. Compared to those of the single-layer film, a lesser (00l) basal plane preferred orientation with a larger perpendicular c-axis dispersion, smaller crystallite sizes and higher microstrains at L≥50Å were obtained in the multi-layer specimen consisting of eight 500Å thick magnetic layers. The magnetic particles were found to be poorly crystallized in the multi-layer specimen where the thicknesses of the 33 magnetic layers were limited to 150Å each.
X-Ray Powder Data for the Isomers of Nitroaniline (NO2C6H4NH2)
Authors: Schmierer Jeffrey G. , McCarthy Gregory J.
Published: January 2013

X-ray powder data and crystal data for the ortho (2 –), meta (3 – ) and para (4 – ) isomers of nitroaniline, NO2C6H4NH2, are reported. The results are compared to existing PDF patterns.
Refinement of Structural Parameters for Polycrystalline CdSb2O6: A Comparison of Two Methods
Authors: Castro A. , Rasines I. , Sánchez-Martos M.C. , García-Casado P.
Published: January 2013

Trigonal CdSb2O6, prepared as a very crystalline powder by solid state reaction of CdO and Sb2O3, is isostructural with PbSb2O6 Space Group (S.G.) P31m (162), with a = 5.2399(2), c = 4.8045(4) Å, Z = 1 and Dc = 6.57 Mg.m−3. For the refinement of structural parameters from X-ray powder diffraction data two different methods have been employed and compared, both leading to very similar results. The refinements converged to RI = 0.025 using 35 intensities in the incremental optimization technique and to RF = 0.038, RW = 0.033 from 161 reflections in the least-squares refinement.
Standardless Quantitative X-Ray Phase Analysis – Estimation of Precision
Authors: Zevin L.S. , Zevin Sh.L.
Published: January 2013

Quantitative phase analysis of n-phase mixtures can be performed if at least n samples composed of no more than n identical phases are available. The fact that there is no need for pure phases (analytical standards) constitutes the main advantage of the method presented here. However, substitution for the pure phases by an unknown mixture of these phases decreases the diversity of the sample set and also the precision of the analysis. The crucial step in a standardless method is the creation of an initial sample set. A simple test is developed to estimate the suitability of the sample set for analysis and to evaluate the analysis error. Application of this test to 13 four-phase mixtures has confirmed its high quality.
X-Ray Diffraction and EXAFS Study of Palladium Tetrammine Dichromate, [Pd(NH3)4]Cr2O7
Authors: Borgna A. , Moraweck B. , Fessler P.
Published: January 2013

Palladium tetrammine dichromate, [Pd(NH3)4]Cr2O7, was obtained by precipitation from [Pd(NH3)4]Cl2·H2O and (NH4)2Cr2O7. The X-ray diffraction pattern of this compound corresponds to a new phase, which was indexed in the triclinic system, but on a cell that should be considered as preliminary. From the chemical analysis and the X-ray absorption experiments at both K-edges of Pd and Cr, we conclude that the surrounding of these atoms is kept during formation.
Improved powder X-ray data for cancrinites II: Liottite and sacrofanite
Authors: Ballirano Paolo , Maras Adriana , Buseck Peter R. , Wang Su , Yates Ann M.
Published: January 2013

Improved powder X-ray diffraction (XRD) data for liottite and sacrofanite, two members of the cancrinite group of minerals, were obtained using a rotating anode diffractometer. The cell parameters of liottite are a = 12.8575(3), c = 16.0905(6) Å, and the space group is ; the strongest reflections are at 4.834(38), 3.783(12), 3.714(100), 3.312(91), 2.784(13), 2.682(26), 2.470(17), and 2.143(27) Å. The cell parameters of sacrofanite are a = 12.8945(4) and c =74.2128(37) Å, and the possible space groups are P63/mmc, P63mc, and ; the strongest reflections are at 11.18(23), 3.757(25), 3.723(100), 3.488(27), 3.302(62), 2.651(31), 2.645(30), and 2.149(18) Å. The new data include an increased number of indexed peaks and empirical formulae that differ from the reference data (PDF 29-1187 and PDF 35-653, respectively).
New phases and solid solutions in the systems PbO–Bi2O3–P2O5/As2O5/V2O5
Authors: Jie Y. C. , Eysel W.
Published: January 2013

The systems PbO–Bi2O3–P2O5/As2O5/V2O5 have been studied with respect to their compounds and solid solutions. A number of new compounds, particularly with high-Bi contents were found. Most of them are structurally closely related to the CaF2 and δ-Bi2O3 structures. Several binary and ternary solid solutions with P/As/V substitutions were investigated.
My life at the National Bureau of Standards and the National Institute for Standards and Technology
Authors: McMurdie Howard F.
Published: January 2013

I had just completed my BS in chemistry at Northwestern University in 1928 and had passed the Civil Service Chemistry Examination, and my fiance had passed an examination for the Civil Service Commission and had been offered a job at that agency in Washington. So we got on a train and came to DC, arriving 15 March 1928. I went to the Civil Service Commission (now called the Office of Personnel Management) and was directed to NBS where there were a number of openings for a P1 chemist. There I talked to Dr. Wichers in Chemistry and to J. Murray in the Lime and Gypsum Section. I took a job in the latter. On 31 March, we got married and on Monday, 2 April 1928, I started work in the Lime and Gypsum Section of the Clay and Mineral Products Division.
Indexing Powder Patterns from Relative Axial Dimensions
Authors: Post Ben , McClune W. Frank
Published: January 2013

The usefulness of an X-ray powder diffraction data base, such as the one published by the International Centre for Diffraction Data, is largely dependent on continued additions of indexed powder patterns of single-phase materials of interest to data-base users. The single-phase character of a specimen is generally established by using known values of the unit cell constants to index all its powder pattern lines.

In this manuscript we describe indexing procedures based on crystal data which provide only relative values of the cell dimensions, rather than the absolute values usually considered to be essential to the indexing process. To the best of our knowledge, the use of such data for indexing powder diffraction patterns has generally been overlooked or ignored by X-ray crystallographers. We refer to the large numbers of goniometric measurements of crystals which have been published both before, and since, the discovery of X-ray diffraction. These provide useful descriptions of chemical and physical properties of crystals as well as measurements of relative dimensions of unit cell axes. The latter are presented in the form of a/b, b/b and c/b, together with the interaxial angle or angles, if the cell is nonorthogonal.
XPAS: An Interactive Computer Program for Analysis of X-Ray Powder Diffraction Patterns
Authors: Singh Balbir , Gilkes R.J.
Published: January 2013

An interactive computer program to display, process and analyze raw powder X-ray diffraction data is described. The program extensively employs graphic means of input and output with the help of “pop-up” windows and menus. In addition to those tasks that are common to most primary raw data analyzing programs, it performs many functions which are generally assigned to separate secondary programs. These functions include on-screen correction of d-spacing with reference to a standard compound, calculation of peak width and crystallite size, subtraction of patterns for differential X-ray diffraction and unrestricted overlay of patterns. The advantages of an integrated single program to process X-ray diffraction data in mineral research are illustrated and discussed.
X-Ray Powder Data for Ca4Al6O12SO4
Authors: Krstanović I. , Radaković A. , Karanović Lj.
Published: January 2013

An indexed X-ray powder diffraction pattern is reported for Ca4A6O12SO4, prepared by solid state reaction. The compound crystallizes in the tetragonal system with a = 13.031(3) and c = 9.164(2) Å, V = 1556.1 (8) Å3, Z = 4.
Intensity Round Robin Report
Authors: Jenkins Ron , Schreiner Walter N.
Published: January 2013

The intensity round-robin is one of a series of round-robins sponsored by the International Centre for Diffraction Data. The purpose of these round-robins is to attempt to quantify problems encountered in the acquisition, analysis and interpretation of powder diffraction data. Previous International Centre sponsored round-robins have addressed topics including: manual and automated search match methods; sample preparation methods; d-spacing accuracy; cell parameter refinement and peak profile calibration.

The primary focus of the intensity round-robin was to study measured intensities obtained from modern computer controlled powder diffractometers. However, the tests were designed in such a way as to also yield information on the performance of data treatment software packages. To this end, participants were asked to submit both raw and treated data, thus allowing evaluation of, for example, the efficiency of peak hunting algorithms in finding peaks.
Crystal and X-Ray Powder Data for Three Orthovanadates M Th2 (VO4)3 (M = K, Rb, Cs)
Authors: Elfakir A. , Souron J.P. , Quartern M.
Published: January 2013

Three isotopic orthovanadates MTh2 (VO4)3 with M = K, Rb, Cs have been syndiesized by solid state reaction. Single crystals of K Th2 (VO4)3 and Rb Th2 (VO4)3 were obtained. These compounds are isotypic with the corresponding orthophosphates: monoclinic, space group C2/c, Z = 4. Unit-cell parameters for die diree compounds were determined. Powder diffraction data for each phase are reported.
Crystallographic and X-Ray Powder Data for Ca8ZnSi4O16Cl2, a New Compound in The System CaO-ZnO-SiO2-CaCl2
Authors: Bolin Wu , Wei Shang
Published: January 2013

The synthesis, thermal behavior, crystallographic and X-ray powder diffraction data, and infrared spectral data for Ca8ZnSi4O16Cl2 have been determined. This compound is cubic with isolated silicate tetrahedra.
X-ray diffraction peak-broadening analysis of (La-M)2CuO4 high-Tc superconductors
Authors: Balzar Davor , Ledbetter Hassel , Roshko Alexana
Published: January 2013

An X-ray diffraction peak-broadening analysis of four oxides is described: La2CuO4 and La1.85M0.15CuO4 (M = Ca,Ba,Sr) high-Tc superconductors. The diffraction line profiles were fitted with a convolution of specimen and instrumental functions, and the specimen peakbroadening angular dependence was analyzed with the Warren-Averbach method. It was found that microstrains and incoherently diffracting domains are highly anisotropic. In the superconductors, stacking-fault probability increases with increasing Tc; microstrain decreases. In La2CuO4, different broadening of (h00) and (0k0) reflections is not caused by stacking faults; it might arise from lower crystallographic symmetry.
Development of an improved XRD sample holder
Authors: Li Chi-Tang , Albe William R.
Published: January 2013

A new and improved sample holder suited for small samples has been developed for X-ray diffractometry. This holder is made from a commercial semiconductor grade of silicon wafer grown and cut along the [100]-axis, i.e., Si(100). This new holder not only meets almost all basic requirements of an ideal holder, namely, flat and damage free surface, low background noise, few interference peaks, and desired shape with different cavity sizes, but also provides additional advantages for measuring crystallite sizes and mass absorption coefficients. Furthermore, this holder is easy to clean and has good appearance because of its polished surface. A U.S. patent has been issued and a commercialization effort is underway.