scholarly journals Reaction of Pentaphenylphosphorus with Hexachloroplatinic Acid

2021 ◽  
Vol 13 (1) ◽  
pp. 31-38
Author(s):  
A.R. Zykova ◽  
Keyword(s):  
Ir Spectroscopy ◽  
Structural Data ◽  
Unit Cell Parameters ◽  
Absorption Bands ◽  
X Ray ◽  
Cell Parameters ◽  
Hexachloroplatinic Acid ◽  
Tetrahedral Environment ◽  
Stretching Vibrations ◽  
Group 1

Tetraphenylphosphonium hexachloroplatinate (1) was synthesized by the interaction of pentaphenylphosphorus with hexachloroplatinic acid in acetone. The recrystallization of complex 1 from dimethylsulfoxide gave tetraphenylphosphonium dimethylsulfoxidopentachloroplatinate (2). The compounds have been characterized by IR-spectroscopy and X-ray analysis. The absorption bands characterizing stretching vibrations of the phenyl groups are present in the IR spectra, recorded on a Shimadzu IRAffinity-1S Fourier spectrometer in the 4000–400 cm–1 area in KBr pellets. According to the X-ray analysis, the compound unit cell parameters are: triclinic syngony, space group (1, 2), а = 10.205(10), b = 10.970(15), c = 12.160(11) Å (1), а = 7.7667(4), b = 13.3069(7), c = 14.2562(7) Å (2), a = 73,65(4)°, β = 80.64(3)°, g = 77.48° (1), a = 80.972(4)°, β = 88.205(4)°, g = 89.199(4)° (2), V = 1272(2) Å3 (1), 1454.38(13) Å3 (2). The crystals of complexes 1 and 2 consist of the tetrahedral tetraphenylphosphonium cations and octahedral anions. In cations the phosphorus atoms have a slightly distorted tetrahedral environment (the CPC angles are 107.8(3)-113.2(3)° (1), 105.9(3)–112.9(3)° (2), the P-C distance is 1.785(6)-1.805(6) Å (1), 1.783(7)–1.791(6) Å (2). Platinum atoms in the anions of complexes 1 and 2 are hexacoordinated. In complex 2 the dimethyl sulfoxide ligand is coordinated with the Pt atom via the sulfur atom 2.290(2) Å. Complete tables of coordinates of atoms, bond lengths and valence angles are deposited at the Cambridge Structural Data (CCDC 1865783, 829586 http://www.ccdc.cam.ac.uk).

Compressibility of β-As4S4: an in situ high-pressure single-crystal X-ray study

2012 ◽  
Vol 76 (4) ◽  
pp. 963-973 ◽  
Author(s):  
G. O. Lepore ◽  
T. Boffa Ballaran ◽  
F. Nestola ◽  
L. Bindi ◽  
D. Pasqual ◽  
...  
Keyword(s):  
Pressure Range ◽  
Substantial Reduction ◽  
Structural Data ◽  
Unit Cell ◽  
Van Der Waals Interactions ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Intermolecular Distances

AbstractAmbient temperature X-ray diffraction data were collected at different pressures from two crystals of β-As4S4, which were made by heating realgar under vacuum at 295ºC for 24 h. These data were used to calculate the unit-cell parameters at pressures up to 6.86 GPa. Above 2.86 GPa, it was only possible to make an approximate measurement of the unit-cell parameters. As expected for a crystal structure that contains molecular units held together by weak van der Waals interactions, β-As4S4 has an exceptionally high compressibility. The compressibility data were fitted to a third-order Birch–Murnaghan equation of state with a resulting volume V0 = 808.2(2) Å3, bulk modulus K0 = 10.9(2) GPa and K' = 8.9(3). These values are extremely close to those reported for the low-temperature polymorph of As4S4, realgar, which contains the same As4S4 cage-molecule. Structural analysis showed that the unit-cell contraction is due mainly to the reduction in intermolecular distances, which causes a substantial reduction in the unit-cell volume (∼21% at 6.86 GPa). The cage-like As4S4 molecules are only slightly affected. No phase transitions occur in the pressure range investigated.Micro-Raman spectra, collected across the entire pressure range, show that the peaks associated with As–As stretching have the greatest pressure dependence; the S–As–S bending frequency and the As–S stretching have a much weaker dependence or no variation at all as the pressure increases; this is in excellent agreement with the structural data.

scholarly journals Crystallochemical aspects of two microlite-group new mineral species

2014 ◽  
Vol 70 (a1) ◽  
pp. C1095-C1095
Author(s):  
Marcelo Andrade ◽  
Javier Ellena ◽  
Daniel Atencio
Keyword(s):  
Microprobe Analysis ◽  
Electron Microprobe Analysis ◽  
New Mineral ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
New Mineral Species ◽  
Group 1

Fluorcalciomicrolite, Ca1.5Ta2O6F, and hydroxycalciomicrolite, Ca1.5Ta2O6(OH), are new microlite-group [1] minerals found in the Volta Grande pegmatite, Nazareno, Minas Gerais, Brazil. Both occur as octahedral and rhombododecahedral crystals. The crystals are colourless, yellow and translucent, with vitreous to resinous luster. The densities calculated for fluorcalciomicrolite [2] and hydroxycalciomicrolite are 6.160 and 6.176 g/cm3, respectively. The empirical formulae obtained from electron microprobe analysis are (Ca1.07Na0.81□0.12)Σ2(Ta1.84Nb0.14Sn0.02)Σ2[O5.93(OH)0.07]Σ6.00[F0.79(OH)0.21] for fluorcalciomicrolite and (Ca1.48Na0.06Mn0.01)Σ1.55(Ta1.88Nb0.11Sn0.01)Σ2O6[(OH)0.76F0.20O0.04] for hydroxycalmicrolite. Fluorcalciomicrolite is cubic, space group Fd-3m, a = 10.4191(6) Å, V = 1131.07(11) Å3, and Z = 8. Hydroxycalciomicrolite is also cubic; however, the presence of P-lattice is confirmed by the large number of weak reflections observed by X-ray diffraction. As a result, the space group is P4332 and unit-cell parameters are a = 10.4211(8) Å, and V = 1131.72(15) Å3.

scholarly journals Brattforsite, Mn19(AsO3)12Cl2, a new arsenite mineral related to magnussonite, from Brattforsgruvan, Nordmark, Värmland, Sweden

2021 ◽  
Author(s):  
Dan Holtstam ◽  
Cristian Biagioni ◽  
Ulf Hålenius
Keyword(s):  
Three Dimensional ◽  
Structural Data ◽  
Type Specimen ◽  
Structural Topology ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Calculated Density ◽  
X Ray ◽  
Cell Parameters ◽  
Density Values

AbstractBrattforsite is an approved mineral (IMA2019-127), with ideal formula Mn19(AsO3)12Cl2. Associated minerals in the type specimen from the Brattfors mine, Nordmark (Värmland, Sweden) include jacobsite, alleghanyite, phlogopite, calcite and dolomite. Brattforsite, forming subhedral, mostly equant crystals up to 0.5 mm across, is orange to reddish-brown with a white streak, and translucent with a resinous to vitreous lustre. The fracture is uneven to subconchoidal, and no cleavage is observed. It is very weakly pleochroic in yellow, optically biaxial (–) with 2V = 44(5)° and has calculated mean refractive index of 1.981. Measured and calculated density values are 4.49(1) and 4.54(1) g·cm− 3, respectively. Chemical analyses yields (in wt%): MgO 0.62, CaO 1.26, MnO 48.66, FeO 0.13, As2O3 46.72, Cl 2.61, H2Ocalc 0.07, O ≡ Cl –0.59, sum 99.49, corresponding to the empirical formula (Mn17.67Ca0.58Mg0.40Fe0.05)∑18.70As12.17O35.90Cl1.90(OH)0.20, based on 38 (O + Cl + OH) atoms per formula unit. The five strongest Bragg peaks in the powder X-ray diffraction pattern are [d (Å), I (%), (hkl)]: 2.843,100, ($$ \overline{4} $$ 4 - 44); 2.828, 99, (444); 1.731, 32, (880); 2.448, 28, (800); 1.739, 25, (088). Brattforsite is monoclinic and pseudotetragonal, space group I2/a, with unit-cell parameters a = 19.5806(7), b = 19.5763(7), c = 19.7595(7) Å, β = 90.393(3)°, V = 7573.9(5) Å3 and Z = 8. The crystal structure was solved and refined to an R1 index of 3.4 % for 7445 reflections [Fo > 4σ(Fo)]. Brattforsite has the same overall structural topology as magnussonite (i.e., the species can be considered as homeotypic), but with 12 independent tetrahedrally coordinated As sites and 21 Mn sites with varying (4–8) coordination. The Mn-centered polyhedra, bonded through edge- and face-sharing, give rise to a three-dimensional framework. The (AsO3)3− groups are bonded to this framework through corner- and edge-sharing. Spectroscopic measurements (optical absorption, Raman, FTIR) carried out support the interpretation of the compositional and structural data.

scholarly journals Synthesis, Structural and Electrical Studies of Li-Ni-Cu Nano Ferrites

2018 ◽  
Vol 26 (1) ◽  
pp. 1-12 ◽  
Author(s):  
Shashidhar N. Adarakatti ◽  
Veeresh S. Pattar ◽  
Prashant K. Korishettar ◽  
Bhagyashri V. Grampurohit ◽  
Ravindra G. Kharabe ◽  
...  
Keyword(s):  
Spinel Ferrite ◽  
Unit Cell ◽  
Ir Absorption ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Absorption Bands ◽  
X Ray ◽  
Cell Parameters ◽  
Ir Absorption Spectra ◽  
Vegard’S Law

Abstract Li-Ni ferrite has gained great scientific elicit owing to of its unparalleled properties and applications. The copper doped Li-Ni ferrite has been synthesized by sucrose method. The structure was characterized by X-ray diffraction, which has confirmed the formation of single-phase spinel structure. X-ray diffraction and FTIR data reveals the formation of cubic structure phase. Unit cell parameters vary with copper content; overall variation of the unit cell parameters obeys Vegard’s law. The main absorption bands of spinel ferrite have appeared through IR absorption spectra recorded in the range of 300–700 cm−1. The copper concentration dependence of lattice parameters obeys Vegard’s law. DC electrical resistivity of the prepared samples decreases with increasing in the temperature which shows the semiconducting behaviour of all nano ferrites. The most prominent influence copper doping on the electrical properties of Li-Ni ferrites has been reported.

scholarly journals Na3MP3O10·12H2O (M = Co, Ni): Crystal Structure and IR Spectroscopy

2012 ◽  
Vol 2012 ◽  
pp. 1-6
Author(s):  
Khalil Azzaoui ◽  
Rachid Essehli ◽  
El Miloud Mejdoubi ◽  
Brahim El Bali ◽  
Michal Dusek ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Ir Spectrum ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Wet Chemistry ◽  
X Ray ◽  
Cell Parameters ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Two new dodecahydrate trisodium triphosphates Na3MP3O10·12H2O (M = Co (1), Ni (2)) were synthesized using a wet chemistry route and characterized by X-ray diffraction and FT-IR spectroscopy. They are isotypic, monoclinic (P21/n, Z=2), with pseudoorthorhombic unit cell parameters (Ǻ,°): (a=14,9906 (4), b=9,1628 (2), c=14,6660 (4), β=90,098 (2), for (1) and a=15,0236 (3), b=9,1972 (2), c=14,6654 (3), β=90,0492 (16) for (2)). Values of R/Rw are 0.0267/0.0738 and 0.0284/0.0907, respectively, for (1) and (2). Both compounds were found to be systematically twinned by 180° rotation around a. Their frameworks are made by slabs parallel to ab plane, resulting from the cohesion of two kinds of metallic chains. IR spectrum confirms the presence of characteristic bands from P3O10 phosphate group.

X-ray powder diffraction study of La2LiTaO6

2014 ◽  
Vol 30 (1) ◽  
pp. 57-62
Author(s):  
Mark A. Rodriguez ◽  
James J. M. Griego ◽  
Harlan J. Brown-Shaklee ◽  
Mia A. Blea-Kirby ◽  
John F. Ihlefeld ◽  
...  
Keyword(s):  
Powder Diffraction ◽  
Structural Data ◽  
Impurity Phase ◽  
Unit Cell Parameters ◽  
Powder Diffraction File ◽  
Ion Conductor ◽  
X Ray ◽  
Cell Parameters ◽  
Fast Ion Conductor ◽  
Fast Ion

The structure of La2LiTaO6 has been derived from the powder X-ray powder diffraction (XRD) data. La2LiTaO6 is monoclinic with unit-cell parameters a = 5.621(1) Å, b = 5.776(1) Å, c = 7.954(2) Å, β = 90.34(2)°, space group P21/n (14), and Z = 2. The structure of La2LiTaO6 is an ordered perovskite with alternating Li and Ta octahedra. A new set of powder XRD data (d-spacing and intensity listing) has been generated to replace entry 00-039-0897 within the Powder Diffraction File. The newly elucidated structural data for La2LiTaO6 shall facilitate quantitative analysis of this impurity phase which is often observed during synthesis of the fast-ion conductor phase Li5La3Ta2O12.

Structural Study of a new Compound Based on Acid 1,4-Cyclohexanedicarboxylic (1,4-CDC)

2010 ◽  
Vol 6 (1) ◽  
pp. 891-896
Author(s):  
Manel Halouani ◽  
M. Dammak ◽  
N. Audebrand ◽  
L. Ktari
Keyword(s):  
Aqueous Solution ◽  
Water Molecules ◽  
Carboxyl Group ◽  
X Ray Diffraction ◽  
Compound I ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Parameters ◽  
Cyclohexanedicarboxylic Acid

One nickel 1,4-cyclohexanedicarboxylate coordination polymers, Ni2 [(O10C6H4)(COO)2].2H2O  (I), was hydrothermally synthesized from an aqueous solution of Ni (NO3)2.6H2O, (1,4-CDC) (1,4-CDC = 1,4-cyclohexanedicarboxylic acid) and tetramethylammonium nitrate. Compound (I) crystallizes in the monoclinic system with the C2/m space group. The unit cell parameters are a = 20.1160 (16) Å, b = 9.9387 (10) Å, c = 6.3672 (6) Å, β = 97.007 (3) (°), V= 1263.5 (2) (Å3) and Dx= 1.751g/cm3. The refinement converged into R= 0.036 and RW = 0.092. The structure, determined by single crystal X-ray diffraction, consists of two nickel atoms Ni (1) and Ni (2). Lots of ways of which is surrounded by six oxygen atoms, a carboxyl group and two water molecules.

scholarly journals Crystallization and preliminary X-ray diffraction analysis of the Csu pili CsuC–CsuA/B chaperone–major subunit pre-assembly complex fromAcinetobacter baumannii

2015 ◽  
Vol 71 (6) ◽  
pp. 770-774 ◽  
Author(s):  
Natalia Pakharukova ◽  
Minna Tuittila ◽  
Sari Paavilainen ◽  
Anton Zavialov
Keyword(s):  
Diffusion Method ◽  
X Ray Diffraction ◽  
Hanging Drop ◽  
Unit Cell Parameters ◽  
Gram Negative ◽  
X Ray ◽  
Cell Parameters ◽  
Abiotic Surfaces ◽  
Vapour Diffusion ◽  
Fimbrial Adhesins

The attachment of many Gram-negative pathogens to biotic and abiotic surfaces is mediated by fimbrial adhesins, which are assembledviathe classical, alternative and archaic chaperone–usher (CU) pathways. The archaic CU fimbrial adhesins have the widest phylogenetic distribution, yet very little is known about their structure and mechanism of assembly. To elucidate the biogenesis of archaic CU systems, structural analysis of the Csu fimbriae, which are used byAcinetobacter baumanniito form stable biofilms and cause nosocomial infection, was focused on. The major fimbriae subunit CsuA/B complexed with the CsuC chaperone was purified from the periplasm ofEscherichia colicells co-expressing CsuA/B and CsuC, and the complex was crystallized in PEG 3350 solution using the hanging-drop vapour-diffusion method. Selenomethionine-labelled CsuC–CsuA/B complex was purified and crystallized under the same conditions. The crystals diffracted to 2.40 Å resolution and belonged to the hexagonal space groupP6422, with unit-cell parametersa=b= 94.71,c = 187.05 Å, α = β = 90, γ = 120°. Initial phases were derived from a single anomalous diffraction (SAD) experiment using the selenomethionine derivative.

Silicate-germanate K2Y[(Si3Ge)O10(OH)] with unusual complex corrugated layer and its correlation to ring silicate gerenite and chain silicate chkalovite

2020 ◽  
Vol 235 (4-5) ◽  
pp. 167-172
Author(s):  
Anastasiia P. Topnikova ◽  
Elena L. Belokoneva ◽  
Olga V. Dimitrova ◽  
Anatoly S. Volkov ◽  
Leokadiya V. Zorina
Keyword(s):  
Low Temperature ◽  
Cross Section ◽  
Complex Anion ◽  
Diffraction Experiment ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Chain Silicate ◽  
Novel Complex

AbstractA new silicate-germanate K2Y[(Si3Ge)O10(OH)] was synthesized hydrothermally in a system Y2O3:GeO2:SiO2 = 1:1:2 (T = 280 °C; P = 90–100 atm.); K2CO3 was added to the solution as a mineralizer. Single-crystal X-ray diffraction experiment was carried out at low temperature (150 K). The unit cell parameters are a = 10.4975(4), b = 6.9567(2), c = 15.4001(6) Å, β = 104.894(4)°; V = 1086.86(7) Å3; space group is P 21/c. A novel complex anion is presented by corrugated (Si,Ge) tetrahedral layers connected by couples of YO6 octahedra into the mixed microporous framework with the channels along b and a axes, the maximal size of cross-section is ~5.6 Å. This structure has similarity with the two minerals: ring silicate gerenite (Ca,Na)2(Y,REE)3Si6O18 · 2H2O and chain silicate chkalovite Na2BeSi2O6. Six-member rings with 1̅ symmetry as in gerenite are distinguished in the new layer. They are mutually perpendicular to each other and connected by additional tetrahedra. Straight crossing chains in chkalovite change to zigzag four-link chains in the new silicate-germanate layer.

X-ray powder diffraction data of LaNi0.5Ti0.45Co0.05O3, LaNi0.45Co0.05Ti0.5O3, and LaNi0.5Ti0.5O3 perovskites

2021 ◽  
pp. 1-6
Author(s):  
Mariana M. V. M. Souza ◽  
Alex Maza ◽  
Pablo V. Tuza
Keyword(s):  
Crystal Structure ◽  
Rietveld Method ◽  
Pechini Method ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Modified Pechini Method ◽  
Scanning Electron

In the present work, LaNi0.5Ti0.45Co0.05O3, LaNi0.45Co0.05Ti0.5O3, and LaNi0.5Ti0.5O3 perovskites were synthesized by the modified Pechini method. These materials were characterized using X-ray fluorescence, scanning electron microscopy, and powder X-ray diffraction coupled to the Rietveld method. The crystal structure of these materials is orthorhombic, with space group Pbnm (No 62). The unit-cell parameters are a = 5.535(5) Å, b = 5.527(3) Å, c = 7.819(7) Å, V = 239.2(3) Å3, for the LaNi0.5Ti0.45Co0.05O3, a = 5.538(6) Å, b = 5.528(4) Å, c = 7.825(10) Å, V = 239.5(4) Å3, for the LaNi0.45Co0.05Ti0.5O3, and a = 5.540(2) Å, b = 5.5334(15) Å, c = 7.834(3) Å, V = 240.2(1) Å3, for the LaNi0.5Ti0.5O3.

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