scholarly journals A new complex alkali metal aluminium amide borohydride, Li2Al(ND2)4BH4: synthesis, thermal analysis and crystal structure

RSC Advances ◽  
2016 ◽  
Vol 6 (34) ◽  
pp. 28761-28766 ◽  
Author(s):  
S. Hino ◽  
T. Ichikawa ◽  
Y. Kojima ◽  
M. H. Sørby ◽  
B. C. Hauback

The first reported compound containing both [Al(ND2)4]− and BH4− anions, Li2Al(ND2)4BH4, was formed in ball-milled LiAl(ND2)4 + 2LiBH4 and NaAl(ND2)4 + 2LiBH4. Its crystal structure was solved and refined in a monoclinic unit cell.

1985 ◽  
Vol 40 (6) ◽  
pp. 726-729 ◽  
Author(s):  
Klaus Güde ◽  
Christoph Hebecker

Abstract Single crystals of KSc2F7 have been prepared from a mixture of KF and ScF3 . The samples were investigated by X-ray methods. KSc2F7 crystallizes orthorhombically with a = 10.643(2), b = 6.540(1), c = 4.030(1) Å. These data indicate a close crystallographic connection to the monoclinic unit cell of KIn2F7 [1], But in contrast to KIn2F7 , KSc2 F7 crystallizes in space group No. 65. Cmmm - D192h. The R-value for 341 observed independent reflections is 0.060.


2009 ◽  
Vol 64 (11-12) ◽  
pp. 1325-1328 ◽  
Author(s):  
Hanne Nuss ◽  
Martin Jansen

The two new ozonide compounds K([12]crown-4)2O3 ・ 1.5 NH3 (1) and Rb([12]crown-4)2O3 ・ 1.5 NH3 (2) were synthesized from the binary alkali metal ozonides and [12]crown-4 in liquid ammonia. The air- and temperature-sensitive red, needle-shaped compounds crystallize isostructurally in the non-centrosymmetric space group Fdd2 (no. 43) with 16 formula units per unit cell. The lattice parameters are a = 26.917(8), b = 43.25(1), c = 7.823(2) Å, V = 9108(5) Å3; and a = 26.730(6), b = 44.70(1), c = 7.739(2) Å, V = 9245(4) Å3 for 1 and 2, respectively. The structure comprises rod-like [([M([12]crown-4)2(NH3)]O3)2(NH3)] supramolecular units, forming a fishbone pattern parallel to (001). The ozonide anions are separated from the metal cations and interact only weakly with two ammonia molecules via N-H・ ・ ・O hydrogen bonds


2011 ◽  
Vol 67 (4) ◽  
pp. 293-301 ◽  
Author(s):  
Susanne Fritz ◽  
Horst Schmidt ◽  
Iris Paschke ◽  
Oxana V. Magdysyuk ◽  
Robert E. Dinnebier ◽  
...  

Calcium selenate subhydrate, CaSeO4·0.625H2O, was prepared by hydrothermal conversion of CaSeO4·2H2O at 463 K. From the single crystals obtained in the shape of hexagonal needles, 50–300 µm in length, the crystal structure could be solved in a trigonal unit cell with space group P3221. The cell was confirmed and refined by high-resolution synchrotron powder diffraction. The subhydrate was characterized by thermal analysis and Raman spectroscopy.


2010 ◽  
Vol 65 (9) ◽  
pp. 1066-1072 ◽  
Author(s):  
Claus Mühle ◽  
Jürgen Nuss ◽  
Robert E. Dinnebier ◽  
Martin Jansen

Crystal structures of the cyanoplatinates A2[Pt(CN)4X2] (A = Rb, Cs; X = Cl, Br, I) have been determined by single-crystal analysis and X-ray powder diffraction. The compounds were synthesized by metathesis from Ba[Pt(CN)4] ·4 H2O and alkali metal sulfates, and by subsequent oxidation with the respective halogens. The crystals were grown by slowly concentrating respective aqueous solutions. The PtIV cations are octahedrally coordinated by four cyanide ligands and two halogen atoms, the latter being located in trans positions. Rb2[Pt(CN)4Cl2]: triclinic, P¯1 (Z = 2), a = 6.7779(2), b = 9.3149(3), c = 9.6707(3) Å , α = 89.37(0), β = 76.05(0), γ = 72.98(0)◦, V = 565.42(2) Å3, N` hkl= 5616, R(F)N` = 0.0273; Rb2[Pt(CN)4I2]: monoclinic, P21/c (Z = 2), a = 7.4239(2), b = 9.2486(2), c = 9.1189(2) Å , β = 107.22(3)◦, V = 598.04(6) Å3, N` hkl = 2917, R(F)N` = 0.0295; Cs2[Pt(CN)4I2]: monoclinic, P21/c (Z = 2), a = 7.6740(4), b = 9.5397(5), c = 9.3474(5) Å , β = 106.46(0)◦, V = 656.3(2) Å3, Z = 2, N` hkl = 2738, R(F)N` = 0.0283; Cs2[Pt(CN)4Cl2]: monoclinic, C2/c (Z = 4), a = 17.947(4), b = 7.395(2), c = 12.031(3) Å , β = 131.904(1)◦, V = 1188.4(5) Å3, R-wp = 2.77; Cs2[Pt(CN)4Br2]: monoclinic, C2/c (Z = 4), a = 18.404(1), b = 7.2819(5), c = 12.4156(8) Å , β = 132.156(1)◦, V = 1233.5(1) Å3, N` hkl = 2566, R(F)N` = 0.0268. All compounds were characterized by differential thermal analysis, thermogravimetry, and infrared and Raman spectroscopy.


1981 ◽  
Vol 36 (5) ◽  
pp. 644-645 ◽  
Author(s):  
M. C. Apella ◽  
E. J. Baran

It is shown that the apatite phases of composition Ca10-xNax(PO4)6-x(SO4)xF2 crystallize in a monoclinic unit cell, which is related to those of pure fluoroapatite by doubling the b-parameter. Some comparisons with related systems are made and a possible explanation for the origin of the small monoclinic distortion is advanced


1980 ◽  
Vol 35 (5) ◽  
pp. 614-619 ◽  
Author(s):  
Hans-Friedrich Klein ◽  
Joachim Groß ◽  
Jean-Marie Bassett ◽  
Ulrich Schubert

Abstract Semicobaltates (Co-1/2) containing olefin and trimethylphosphane ligands are synthe-sized from Co(olefin)(PMe3)3 and potassium metal. The X-ray crystal structure determination of the title compound shows that the unit cell contains two K atoms in equal ionic contact with the ethylene ligands of four Co(C2H4)(PMe3)3 complex units, two of which are interacting with both K atoms. In solution the semicobaltates exist in hydrocarbon solvents under argon only, while in contrast under ethylene or nitrogen atmospheres or in donor solvents disproportionation occurs to give Co(O) and Co(-I) species. Allgemeines


1984 ◽  
Vol 39 (4) ◽  
pp. 416-420 ◽  
Author(s):  
P. Böttcher ◽  
H. Buchkremer-Hermanns ◽  
J. Baron

Ethylenediammonium hexasulfide has been synthesized from ethylenediamine, sulfur, and gaseous H2S in aqueous solution. X-ray investigations on single crystals revealed its structure. The monoclinic unit cell contains eight formula units, the space group is Cc. The sulfur atoms form unbranched zig-zag chains S62- in all-trans-conformation.


Author(s):  
H. Brigitte Krause ◽  
Yonglin Qian

A polycrystalline specimen of nominal formula EuGaAl with unknown crystal structure was investigated by various electron microscope techniques; EDS-, SED-, and CBED data were taken on a Philips 400 electron microscope operated at 100kV, HREM data on a Hitachi 9000 microscope operated at 300kV. The EDS data confirmed the composition for the bulk of the material but, in addition, revealed particles with other fractions of the elements. Only the EuGaAl particles were further investigated. The unit cell was determined to be orthorhombic with a ratio: a/b=0.969(2) , a/c=0.234(2) and b/c=0.234(2). The lattice constants are a=4.54(5)Ȧ, b=4.68Ȧ and c=19.97(20)Ȧ. Based on systematic extinctions for hkl reflections with h+l=2n+l, the unit cell was found to be b-centered. CBED patterns of the [001], [100], and [010] zone axes are shown in Fig. 1. The zone axis patterns are in agreement with the above stated data except for diffused (2m+l,2n+l,0)- reflections, not compatible with the above stated systematic absences. But these occurred only occasionally in conjunction with a complicated noncommensurate superlattice pattern.


2021 ◽  
Vol 23 (15) ◽  
pp. 9325-9336
Author(s):  
Akio Yoshinaka ◽  
Serge Desgreniers ◽  
Anguang Hu

Raman and IR vibrational spectra confirm two molecular units associated with the monoclinic unit cell of nitroethane under high pressure. Raman spectra are extremely sensitive to predicted effects of unit cell distortion due to changes in H-bonding.


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