Unidirectional crystal growth and crystalline perfection ofL-arginine phosphate monohydrate

2012 ◽  
Vol 45 (4) ◽  
pp. 679-685 ◽  
Author(s):  
B. Riscob ◽  
Mohd Shakir ◽  
N. Vijayan ◽  
K. K. Maurya ◽  
M. A. Wahab ◽  
...  

A large (∼20 mm diameter and 80 mm length) single crystal of L-arginine phosphate monohydrate (LAP) has been grown for the first time by the unidirectional Sankaranarayanan–Ramasamy method in an aqueous medium in a specially designed constant-temperature bath. The crystal structure has been confirmed by powder X-ray diffraction. The crystalline perfection was assessed by high-resolution X-ray diffractometry (HRXRD) which found that the quality of the grown single crystal is quite good. HRXRD studies along different directions show that the crystal contains a low density of edge-type dislocations formed along the growth direction. The thermal stability was assessed using thermogravimetric/differential thermal analysis. The mechanical behaviour was studied using an Omnitech micro-hardness tester. The dielectric studies were carried out over a wide frequency range of 10 Hz to 5 MHz at room temperature. The characterization studies reveal that the grown bulk single crystal of LAP is suitable for device applications.

2021 ◽  
Author(s):  
Malte Sellin ◽  
Susanne Margot Rupf ◽  
Ulrich Abram ◽  
Moritz Malischewski

Homoleptic eight-fold coordinated methylisocyanide complexes of W(IV) and W(V) have been prepared for the first time. The reaction of [NBu4]4[W(CN)8] with methyl triflate MeOTf gives [W(CNMe)8][OTf]4. The even stronger methylating mixture of methyl fluoride MeF and arsenic pentafluoride AsF5 in liquid sulfur dioxide SO2 is able to fully alkylate both [NBu4]4[W(CN)8] and [NBu4]3[W(CN)8]. The paramagnetic octakis(methylisocyanide)- tungsten(V) [W(CNMe)8][AsF6]5 is thermally highly unstable above −30 °C. All compounds have been characterized via single-crystal X-ray diffraction, IR and Raman, as well as NMR or EPR spectroscopy<br>


1996 ◽  
Vol 11 (4) ◽  
pp. 804-812 ◽  
Author(s):  
Y. Namikawa ◽  
M. Egami ◽  
S. Koyama ◽  
Y. Shiohara ◽  
H. Kutami

Large YBa2Cu3O7−x (Y123) single crystals (larger than 13 mm cubed) have been grown along the c-axis reproducibly by the modified pulling method. The crystallinity of Y123 single crystal was investigated by x-ray diffraction and x-ray topography. Crystals grown from an MgO single crystal seed had some low angle subgrain boundaries which tilted 0.1–0.8° from each other. These grain boundaries originated from the seed crystal, and the subgrains were extended along the growth direction from the seed crystal. Y123 single crystals with no marked subgrains in the whole area were obtained by using Y123 single subgrain crystal seeds. FWHM of the x-ray rocking curve for the crystal so produced was about 0.14°, which was much better than the spectrum consisting of several separated peaks obtained from the previous crystals. Tc onset of the annealed sample was about 93.6 K, and the transition width was about 0.9 K. The low angle subgrain boundaries did not seem to be effective pinning centers for the magnetic flux.


2017 ◽  
Vol 12 (11) ◽  
pp. 1934578X1701201
Author(s):  
Qiao Xu ◽  
Miao-Miao Zhang ◽  
Shu-Zhen Yana ◽  
Lu-Fen Cao ◽  
Qiang Lia ◽  
...  

Two symmetrical dibenzoquinone derivatives were isolated from solid cultures of the fungus Acremonium cavaraeanum. Compound 1 was new and identified as 2,7-dihydroxy-3,6,9-trimethyl-9 H-xanthene-1,4,5,8-tetraone. Compound 2 was 3,3’,6,6’-tetrahydroxy-4,4’-dimethyl-1,1’-bi- p-benzoquinone, i.e. oosporein, which was reported from A. cavaraeanum for the first time. The structure of the dibenzoquinone (1) was unambiguously elucidated using a combination of MS, IR, 1D- and 2D-NMR, and the dibenzoquinone (2) was further determined by single-crystal X-ray diffraction.


2019 ◽  
Vol 234 (9) ◽  
pp. 613-621
Author(s):  
Marc André Althoff ◽  
Jörn Frederik Martens ◽  
Marco Reichel ◽  
Manfred Metzulat ◽  
Thomas Matthias Klapötke ◽  
...  

Abstract The molecular and single crystal structure of O,O-diethyl O-[2-(dimethylamino)ethyl] phosphorothioate oxalate, as determined by single crystal X-ray diffraction studies, is described for the first time; although this compound is well-known by industry and research from the mid-20th century. The known decomposition product of pure O,O-diethyl O-[2-(dimethylamino)ethyl] phosphorothioate could also be structurally characterized. Additionally, the compounds are characterized by recent analytical methods e.g. NMR. The findings of our study support the thesis that the isolated decomposition product must be a by-product of the thiono-thiolo rearrangement process of the title compound.


2007 ◽  
Vol 63 (11) ◽  
pp. i186-i186 ◽  
Author(s):  
Stanislav Ferdov ◽  
Uwe Kolitsch ◽  
Christian Lengauer ◽  
Ekkehart Tillmanns ◽  
Zhi Lin ◽  
...  

The structure of the layered noncentrosymmetric titanosilicate AM-1 (also known as JDF-L1, disodium titanium tetrasilicate dihydrate), Na4Ti2Si8O22·4H2O, grown as small single crystals without the use of organics, has been refined from single-crystal X-ray diffraction data. The H atom has been located for the first time, and the hydrogen-bonding scheme is also characterized by IR and Raman spectroscopy. All atoms are in general positions except for the Na, the Ti, one Ti-bound O, one Si-bound O and the water O atoms (site symmetries 2, 4, 4, 2 and 2, respectively).


2007 ◽  
Vol 63 (6) ◽  
pp. 836-842 ◽  
Author(s):  
Sebastian Prinz ◽  
Karine M. Sparta ◽  
Georg Roth

The V4+ (spin ½) oxovanadates AV3O7 (A = Ca, Sr) were synthesized and studied by means of single-crystal X-ray diffraction. The room-temperature structures of both compounds are orthorhombic and their respective space groups are Pnma and Pmmn. The previously assumed structure of SrV3O7 has been revised and the temperature dependence of both crystal structures in the temperature ranges 297–100 K and 315–100 K, respectively, is discussed for the first time.


Author(s):  
Alexander M. Antipin ◽  
Natalia I. Sorokina ◽  
Olga A. Alekseeva ◽  
Alexandra N. Kuskova ◽  
Elena P. Kharitonova ◽  
...  

A single crystal of Nd5Mo3O16with lead partly substituting for neodymium, which has a fluorite-like structure, was studied by precision X-ray diffraction, high-resolution transmission microscopy and EDX microanalysis. The crystal structure is determined in the space group Pn\bar 3n. It was found that the Pb atoms substitute in part for Nd atoms in the structure and are located in the vicinity of Nd2 positions. Partial substitutions of Mo cations for Nd positions and of Nd for Mo positions in crystals of theLn5Mo3O16oxide family are corroborated by X-ray diffraction for the first time. The first experimental verification of the location of an additional oxygen ion in the voids abutting MoO4tetrahedra was obtained.


2011 ◽  
Vol 170 ◽  
pp. 198-202 ◽  
Author(s):  
Junji Akimoto ◽  
Hiroshi Hayakawa ◽  
Norihito Kijima ◽  
Junji Awaka ◽  
Fuji Funabiki

Single crystals of Na0.44MnO2 (=Na4Mn9O18) have been synthesized by a flux method at 1173 K for the first time. The crystal structure of Na0.44MnO2 has been refined by single-crystal X-ray diffraction method. The framework structure consists of double and triple rutile-type chains of edge-sharing MnO6 octahedra and a single chain of edge-sharing MnO5. The Mn-O bond distance and bond valence analyses revealed the manganese valence Mn3+/Mn4+ ordering in the Na0.44MnO2 structure.


2021 ◽  
Author(s):  
Malte Sellin ◽  
Susanne Margot Rupf ◽  
Ulrich Abram ◽  
Moritz Malischewski

Homoleptic eight-fold coordinated methylisocyanide complexes of W(IV) and W(V) have been prepared for the first time. The reaction of [NBu4]4[W(CN)8] with methyl triflate MeOTf gives [W(CNMe)8][OTf]4. The even stronger methylating mixture of methyl fluoride MeF and arsenic pentafluoride AsF5 in liquid sulfur dioxide SO2 is able to fully alkylate both [NBu4]4[W(CN)8] and [NBu4]3[W(CN)8]. The paramagnetic octakis(methylisocyanide)- tungsten(V) [W(CNMe)8][AsF6]5 is thermally highly unstable above −30 °C. All compounds have been characterized via single-crystal X-ray diffraction, IR and Raman, as well as NMR or EPR spectroscopy<br>


2019 ◽  
Vol 5 (11) ◽  
pp. eaax7863 ◽  
Author(s):  
Xi Kang ◽  
Fengqing Xu ◽  
Xiao Wei ◽  
Shuxin Wang ◽  
Manzhou Zhu

The valence self-regulation of sulfur from the “−2” valence state in thiols to the “−1” valence state in hydroxylated thiolates has been accomplished using the Pt1Ag28 nanocluster as a platform—the first time that the “−1” valent sulfur has been detected as S−1. Two previously unknown nanoclusters, Pt1Ag28(SR)20 and Pt1Ag28(SR)18(HO-SR)2 (where SR represents 2-adamantanethiol), have been synthesized and characterized—in the latter nanocluster, the presence of hydroxyl induces the valence regulation of two special S atoms from “−2” (in SR) to “−1” valence state in the HO-S(Ag)R. Because of the contrasting nature of the capping ligands in these two nanoclusters [i.e., only SR in Pt1Ag28(SR)20 or both SR- and HO-SR- in Pt1Ag28(SR)18(HO-SR)2], they exhibit differing shell architectures, even though their cores (Pt1Ag12) are in the same icosahedral configuration. Single-crystal x-ray diffraction analysis revealed their 1:1 cocrystallization, and mass spectrometry verified the presence of hydroxyls on Pt1Ag28(SR)18(HO-SR)2.


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