scholarly journals Synthesis, Crystal Structures and Characterization of Two Nonmetal Cation Tetrafluoroborates

Crystals ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 812
Author(s):  
Noura Othman Alzamil ◽  
Ghareeba Mussad Al-Enzi ◽  
Aishah Hassan Alamri ◽  
Insaf Abdi ◽  
Amor BenAli

Two new nonmetal cation tetrafluoroborate phases [H3tren](BF4)3 (I) and [H3tren](BF4)3 HF (II) were synthesized by microwave-assisted solvothermal and characterized by single crystal X-ray diffraction, IR spectroscopy and thermal analysis DTA-TGA. [H3tren](BF4)3 is cubic (P213) with unit cell parameter a = 11.688(1) Å. [H3tren](BF4)3•HF is trigonal (R3c) with unit cell parameters a = 15.297(6) Å and c = 12.007(2) Å. Both (I) and (II) structures can be described from isolated tetrafluoroborate BF4- anions, triprotonated tris-(2-aminoethyl)amine (tren) [H3tren]3+. Phase (II) contains disordered BF4- tetrahedron and hydrofluoric acid.

1987 ◽  
Vol 2 (4) ◽  
pp. 225-226
Author(s):  
Peter Bayliss ◽  
Slade St. J. Warne

AbstractMagnesium-chlorophoenicite may be differentiated from the Mn-analogue chlorophoenicite, because for magnesium-chlorophoenicite at 7Å, whereas for chlorophoenicite.In a review of the literature for the Mineral Powder Diffraction File by Bayliss et al. (1980), powder X-ray diffraction data could not be found of the mineral species magnesium-chlorophoenicite, (Mg,Mn)3Zn2(AsO4)(OH,O)6. Dunn (1981) states that the powder X-ray diffraction data of magnesium-chlorophoenicite is essentially identical to that of chlorophoenicite (Mn analogue) and confirms that the minerals are isostructural.With the crystal structure parameters determined by Moore (1968) for a Harvard University specimen from New Jersey of chlorophoenicite, a powder X-ray diffraction pattern was calculated with the programme of Langhof, Physikalische Chemie Institute, Darmstadt. The calculated pattern was used to correct and complete the indexing of the powder X-ray diffraction data of chlorophoenicite specimen ROM M15667 from Franklin, Sussex County, New Jersey, U.S.A. by the Royal Ontario Museum (PDF 25-1159). With the correctly indexed data of ROM M15667, the unitcell parameters were refined by least-squares analysis and are listed in Table 1.The most magnesium-rich magnesium-chlorophoenicite found in the literature is a description of Harvard University specimen 92803 from Franklin, Sussex County, New Jersey, U.S.A. by Dunn (1981), where Mg is slightly greater than Mn. A 114.6 mm Debye-Schemer film taken of HU92803 with Cu radiation and a Ni filter (CuKα = 1.5418Å) was obtained from Dr. P. Dunn and measured visually. The unit-cell parameters, which were refined by least-squares analysis starting from the unit-cell parameters of PDF 25-1159 in space group C2/m(#12), are listed in Table 1, and give F28 = 4.1(0.050,136) by the method of Smith & Snyder (1979).The hkl, dcalulated, dobserved and relative intensities (I/I1) of HU92803 are presented in Table 2. With the atomic positions and temperature factors of chlorophoenicite determined by Moore (1968), the Mn atomic positions occupied by 50% Mg and 50% Mn, and the unit-cell parameters of HU92803, a powder X-ray diffraction pattern was calculated and Icalculated is recorded in Table 2. A third powder X-ray diffraction pattern was calculated with the Mn atomic positions fully occupied by Mg. Because the atomic scattering factor of Mn is more than twice greater than Mg, chlorophoenicite may be differentiated from magnesium-chlorophoenicite based upon the calculated intensities of the first three reflections given in Table 3.Although the a, c and β unit-cell parameters of chlorphoenicite are similar to those of magnesium-chlorphoenicite, the b unit-cell parameter of chlorophoenicite is significantly greater than that of magnesium-chlorophoenicite (Table 1). The b unit-cell parameter represents the 0–0 distance of the Mn octahedra (Moore, 1968). Since the size of Mn is greater than that of Mg, chlorophoenicite may be differentiated from magnesium-chlorophoenicite based upon the b unit-cell parameter given in Table 1.American Museum of Natural History (New York, N.Y., U.S.A.) specimen 28942 from Sterling Hill, Ogdensburg, New Jersey is composed of willemite, haidingerite and magnesian chlorophoenicite. A spectrographic analysis of the magnesian chlorophoenicite shows As, Mg, Mn and Zn. Powder X-ray diffraction data (PDF 34-190) of the magnesian chlorophoenicite was collected by diffractometer with Cu radiation and a graphite 0002 monochromator (Kα1 = 1.5405) at a scanning speed of 0.125° 2θ per minute. The unit-cell parameters, which were refined by leastsquares analysis starting from the unit-cell parameters of PDF 25-1159, are given in Table 1. Specimen AM 28942 is called chlorophoenicite, because of its large b unit-cell parameter (Table 1), and the I/I1 of 25 for reflection 001 and of 50 for reflection 201 compared to the Icalculated in Table 3.


2014 ◽  
Vol 70 (10) ◽  
pp. 1372-1375 ◽  
Author(s):  
Shanghua Fan ◽  
Defeng Li ◽  
Joy Fleming ◽  
Yuan Hong ◽  
Tao Chen ◽  
...  

7-Keto-8-aminopelargonic acid synthase (KAPA synthase; BioF) is an essential enzyme for mycobacterial growth that catalyses the first committed step in the biotin-synthesis pathway. It is a pyridoxal 5′-phosphate (PLP)-dependent enzyme and is a potential drug target. Here, the cloning, expression, purification and crystallization of KAPA synthase fromMycobacterium smegmatis(MsBioF) and the characterization of MsBioF crystals using X-ray diffraction are described. The crystals diffracted to 2.3 Å resolution and belonged to the monoclinic space groupP21, with unit-cell parametersa= 70.88,b= 91.68,c= 109.84 Å, β = 97.8°. According to the molecular weight of MsBioF, the unit-cell parameters and the self-rotation function map, four molecules are present in each asymmetric unit with aVMvalue of 2.06 Å3 Da−1and a solvent content of 40.20%.


2014 ◽  
Vol 29 (4) ◽  
pp. 379-382 ◽  
Author(s):  
Sandra Amaya ◽  
Johana Arboleda ◽  
Adriana Echavarría

A new trimetallic compound with formula (NH4)Ni2.4Co0.6O(OH)(MoO4)2•1.5H2O was obtained by hydrothermal synthesis. The solid was characterized by X-ray diffraction, thermal analysis (thermogravimetric analysis and differential thermal analysis), Fourier-transformed infrared spectroscopy, Laser Raman spectroscopy, and chemical analysis by atomic absorption, confirming the formation of the layered phase ϕy. Crystallographic studies showed that the compound obtained is trigonal with hexagonal unit-cell parameters, a = 6.0468 ± 0.0016 Å and c = 21.8433 ± 0.0001 Å, and space group R-3m.


1998 ◽  
Vol 12 (11) ◽  
pp. 427-431
Author(s):  
K. Jeyabalan ◽  
L. K. Kaliyaperumal ◽  
A. Sekar ◽  
J. Srinivas

Synthesis and characterization of A 2 CaCuO 5( A=Nd, Sm ) system is reported. Powder X-ray diffraction analysis shows that the compounds crystallizes in an orthorhombic crystal systems and the unit cell parameters are found to be a=6.399(9)Å, b=7.218(8) Å and c=12.167(17) Å for Nd 2 CaCuO 5 and a=5.872(8) Å, b=7.457(3) Å and c=12.682(18) Å for Sm 2 CaCuO 5.


2021 ◽  
Vol 12 (2) ◽  
pp. 2586-2602

The triphosphate dodecahydrate of cobalt and sodium CoNa3P3O10.12H2O was prepared by the ion exchange resin process. Its structure was studied by X-ray diffraction and determined in the monoclinic space group P121/c1with the unit-cell parameters a = 14.6650(5) Å, b=9.1916(3) Å, c = 15.0239(5) Å, =90.2210(10) °, Z = 4 and V = 2025.13(12) Å3. The thermal dehydration of this compound was performed, leading to an anhydrous new form, CoNa3P3O10, which was characterized by X-ray diffraction. The obtained CoNa3P3O10 crystallized in monoclinic space group P21/n with the unit-cell parameters a=15,3774 Å, b=7,6988 A°, c=14,2832A°, β=92,9115°.The characteristic IR wavenumbers of the P3O105− ions observed in the vibrational spectra were calculated using isotopic substitutions, which confirms the existence of these groups in the studied compound. A comparison between the IR and Raman wavenumbers of CoNa3P3O10.12H2O, CoNa3P3O10 and Na5P3O10.12H2O was performed. A kinetic study was also made for CoNa3P3O10·12H2O.


2018 ◽  
Vol 33 (1) ◽  
pp. 55-61 ◽  
Author(s):  
José A. Fernandes ◽  
Olufunso Abosede ◽  
Simona Galli

The reduction of cis-[CoIII(κ2N,N′-1,10-phenanthroline-5,6-dione)2Cl2]Cl into the neutral compound cis-[CoII(κ2N,N′-1,10-phenanthroline-5,6-dione)2Cl2] was observed during developmental studies of new antimalarial drugs. The crystal structure of cis-[CoII(κ2N,N′-1,10-phenanthroline-5,6-dione)2Cl2] was unveiled by powder X-ray diffraction studies (PXRD). PXRD details, unit cell parameters, and space group for cis-[CoII(κ2N,N′-1,10-phenanthroline-5,6-dione)2Cl2], C24H12Cl2CoN4O4, are reported [a = 41.4951 (13) Å, b = 8.2768 (2) Å, c = 12.4994 (3) Å, unit cell volume V = 4292.9 (2) Å3, Z = 8, and space group Fdd2]. Infrared spectroscopy features are also discussed.


Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1028 ◽  
Author(s):  
M. Mashrur Zaman ◽  
Sytle M. Antao

This study investigates the crystal chemistry of monazite (APO4, where A = Lanthanides = Ln, as well as Y, Th, U, Ca, and Pb) based on four samples from different localities using single-crystal X-ray diffraction and electron-probe microanalysis. The crystal structure of all four samples are well refined, as indicated by their refinement statistics. Relatively large unit-cell parameters (a = 6.7640(5), b = 6.9850(4), c = 6.4500(3) Å, β = 103.584(2)°, and V = 296.22(3) Å3) are obtained for a detrital monazite-Ce from Cox’s Bazar, Bangladesh. Sm-rich monazite from Gunnison County, Colorado, USA, has smaller unit-cell parameters (a = 6.7010(4), b = 6.9080(4), c = 6.4300(4) Å, β = 103.817(3)°, and V = 289.04(3) Å3). The a, b, and c unit-cell parameters vary linearly with the unit-cell volume, V. The change in the a parameter is large (0.2 Å) and is related to the type of cations occupying the A site. The average <A-O> distances vary linearly with V, whereas the average <P-O> distances are nearly constant because the PO4 group is a rigid tetrahedron.


2012 ◽  
Vol 76 (4) ◽  
pp. 963-973 ◽  
Author(s):  
G. O. Lepore ◽  
T. Boffa Ballaran ◽  
F. Nestola ◽  
L. Bindi ◽  
D. Pasqual ◽  
...  

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.


Author(s):  
Fang Lu ◽  
Bei Zhang ◽  
Yong Liu ◽  
Ying Song ◽  
Gangxing Guo ◽  
...  

Phytases are phosphatases that hydrolyze phytates to less phosphorylatedmyo-inositol derivatives and inorganic phosphate. β-Propeller phytases, which are very diverse phytases with improved thermostability that are active at neutral and alkaline pH and have absolute substrate specificity, are ideal substitutes for other commercial phytases. PhyH-DI, a β-propeller phytase fromBacillussp. HJB17, was found to act synergistically with other single-domain phytases and can increase their efficiency in the hydrolysis of phytate. Crystals of native and selenomethionine-substituted PhyH-DI were obtained using the vapour-diffusion method in a condition consisting of 0.2 Msodium chloride, 0.1 MTris pH 8.5, 25%(w/v) PEG 3350 at 289 K. X-ray diffraction data were collected to 3.00 and 2.70 Å resolution, respectively, at 100 K. Native PhyH-DI crystals belonged to space groupC121, with unit-cell parametersa = 156.84,b = 45.54,c = 97.64 Å, α = 90.00, β = 125.86, γ = 90.00°. The asymmetric unit contained two molecules of PhyH-DI, with a corresponding Matthews coefficient of 2.17 Å3 Da−1and a solvent content of 43.26%. Crystals of selenomethionine-substituted PhyH-DI belonged to space groupC2221, with unit-cell parametersa = 94.71,b= 97.03,c= 69.16 Å, α = β = γ = 90.00°. The asymmetric unit contained one molecule of the protein, with a corresponding Matthews coefficient of 2.44 Å3 Da−1and a solvent content of 49.64%. Initial phases for PhyH-DI were obtained from SeMet SAD data sets. These data will be useful for further studies of the structure–function relationship of PhyH-DI.


2011 ◽  
Vol 26 (2) ◽  
pp. 119-125 ◽  
Author(s):  
Sytle M. Antao ◽  
Ishmael Hassan

The crystal structures of marialite (Me6) from Badakhshan, Afghanistan and meionite (Me93) from Mt. Vesuvius, Italy were obtained using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and Rietveld structure refinements. Their structures were refined in space groups I4/m and P42/n, and similar results were obtained. The Me6 sample has a formula Ca0.24Na3.37K0.24[Al3.16Si8.84O24]Cl0.84(CO3)0.15, and its unit-cell parameters are a=12.047555(7), c=7.563210(6) Å, and V=1097.751(1) Å3. The average ⟨T1-O⟩ distances are 1.599(1) Å in I4/m and 1.600(2) Å in P42/n, indicating that the T1 site contains only Si atoms. In P42/n, the average distances of ⟨T2-O⟩=1.655(2) and ⟨T3-O⟩=1.664(2) Å are distinct and are not equal to each other. However, the mean ⟨T2,3-O⟩=1.659(2) Å in P42/n and is identical to the ⟨T2′-O⟩=1.659(1) Å in I4/m. The ⟨M-O⟩ [7]=2.754(1) Å (M site is coordinated to seven framework O atoms) and M-A=2.914(1) Å; these distances are identical in both space groups. The Me93 sample has a formula of Na0.29Ca3.76[Al5.54Si6.46O24]Cl0.05(SO4)0.02(CO3)0.93, and its unit-cell parameters are a=12.19882(1), c=7.576954(8) Å, and V=1127.535(2) Å3. A similar examination of the Me93 sample also shows that both space groups give similar results; however, the C–O distance is more reasonable in P42/n than in I4/m. Refining the scapolite structure near Me0 or Me100 in I4/m forces the T2 and T3 sites (both with multiplicity 8 in P42/n) to be equivalent and form the T2′ site (with multiplicity 16 in I4/m), but ⟨T2-O⟩ is not equal to ⟨T3-O⟩ in P42/n. Using different space groups for different regions across the series implies phase transitions, which do not occur in the scapolite series.


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