scholarly journals Synthese und Strukturanalyse des gemischten Alkalimetallorthonitrats Na3K3(NO4)2 / Synthesis and X-Ray Structure Determination of the Mixed Alkali Metal Orthonitrate Na3K3(NO4)2

1991 ◽  
Vol 46 (8) ◽  
pp. 1031-1034 ◽  
Author(s):  
Thomas Bremm ◽  
Martin Jansen

The title compound has been characterized by X-ray powder and single crystal diffraction: Pbcn; a = 7.296(1), b = 15.997(4), c = 7.016(1) Å; Z = 4; 1514 diffractometer data, R = 0.04, Rw = 0.03. The vibrational spectra are compatible with a tetrahedral geometry of the anion.

1982 ◽  
Vol 60 (4) ◽  
pp. 509-513 ◽  
Author(s):  
John W. ApSimon ◽  
Rick P. Sequin ◽  
Carol P. Huber

The title compound was made following a projected synthetic route to pentacyclic triterpenes. The key step in the route is the alkylative trapping of the enolate derived from the enol trimethylsilyl ether 8. The stereochemical consequence of this reaction is confirmed by a single crystal X-ray structure determination on 4, which although of no further utility in the projected synthesis, nevertheless served as a useful template for this determination. In this way, ongoing work in a parallel series of compounds rests on a firm stereochemical footing.


1989 ◽  
Vol 42 (2) ◽  
pp. 335 ◽  
Author(s):  
LM Engelhardt ◽  
JM Patrick ◽  
AH White

The isolation and single-crystal X-ray structure determination of the title compound, [(phen)2Pb(NCS)(O2NO)] is described; crystals are triclinic, P1, a 15.554(7), b 9-670(4), c 8.429(3) α 72.53(3), β 81.90(3), γ 72.88(3)� Z = 2, yielding R 0.052 for 3405 independent 'observed' reflections. The lead atom is seven-coordinate [Pb-N 2.49(1)-2.60(1) (phen), 2.89(1) (NCS); Pb-O 2.75(1), 2.89(1) �] with a large vacancy in the coordination sphere, possibly indicative of a stereochemically active lone pair.


1993 ◽  
Vol 46 (11) ◽  
pp. 1811 ◽  
Author(s):  
CJ Adams ◽  
MI Bruce ◽  
BW Skelton ◽  
AH White

The synthesis and room-temperature single-crystal X-ray structure determination of the title compound are recorded. Crystals are monoclinic, P 21/c, a 14.43(2), b 18.39(1), c 23.64(3) Ǻ, β 123.16(7)°, Z = 4, isostructural with the recently described Fe3Ru5 analogue; R was 0.048 for 6892 'observed' data [I > 3σ(I)]. The cluster is one of the few containing separated carbide ligands within a polyhedral metal skeleton, consisting of an Ru5C square pyramid and an Ru6C octahedron sharing a triangular face, with two PPh2 groups bridging opposite Ru-Ru vectors in each polyhedron.


1993 ◽  
Vol 46 (1) ◽  
pp. 127 ◽  
Author(s):  
LM Engelhardt ◽  
JM Harrowfield ◽  
AM Sargeson ◽  
AH White

The synthesis and single-crystal X-ray structure determination of the title compound are described. Crystals are monoclinic, P 21, a 16.164(9), b 8.277(3), c 8.829(4) Ǻ, β 102.86(4)°, Z 2; 2666 independent 'observed' diffractometer data [I > 3σ(I)] were refined to a residual of 0.045. The cation is unusual amongst complexes of sarcophagine (3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane) cage amines in adopting a lel2ob conformation, seemingly in response to hydrogen bonding/crystal packing forces. In consequence, unlike the tetranitrate analogue in which Ni-N bond distances are dispersed over a narrow range (2.097(5)-2.119(5) Ǻ; mean 2.109 Ǻ], the coordination sphere is more distorted with one pair of Ni-N distances, cis to each other, being short at 2.081(5) and 2.086(5) Ǻ, while the other four are long, ranging from 2.116(5) to 2.135(5) Ǻ, the mean of this array being 2.111 Ǻ.


1990 ◽  
Vol 45 (7) ◽  
pp. 943-946 ◽  
Author(s):  
Joachim Arlt ◽  
Martin Jansen

The isostructural title compounds have been characterized by X-ray powder and single crystal diffraction: R 3̅ c; Z = 6; a = 741.81(4), c = 1639.18(9) pm; 389 diffractometer data, R = 0.04, Rw = 0.03 (K3CO3F); α = 776.1(3), c = 1741.2(9) pm; 235 diffractometer data, R = 0.07, R = 0.06 (Rb3CO3F). Both compounds are carbonate fluorides with isolated CO32- and F- anions.


2015 ◽  
Vol 70 (6) ◽  
pp. 365-372 ◽  
Author(s):  
Olaf Reckeweg ◽  
Ryo H. Wakabayashi ◽  
Francis J. DiSalvo ◽  
Armin Schulz ◽  
Christof Schneck ◽  
...  

AbstractTransparent colorless crystals of KCs[N(CN)2]2 and NaRb2[N(CN)2]3 · H2O were obtained by blending aqueous solutions of Na[N(CN)2] and RbF or KF, respectively. After evaporation of the water, the remaining solid was extracted with absolute ethanol and the solvent was allowed to evaporate at r. t.. KCs[N(CN)2]2 crystallizes in the space group C2/c (no. 15) with the cell parameters a = 1382.7(2), b = 998.1(1) and c = 1455.4(2) pm, and β = 118.085(4) °. The structure of NaRb2[N(CN)2]3 · H2O is exhibiting the space group P63/m (no. 176) with the cell parameters a = 705.98(7) and c = 1462.89(12) pm. Single-crystalline α-K[N(CN)2] was obtained while attempting to synthesize ‘NaK2[N(CN)2]3’, corroborating the results of previous X-ray powder diffraction experiments. Vibrational spectra and DSC/TGA analyses complete our results.


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


1994 ◽  
Vol 47 (9) ◽  
pp. 1799 ◽  
Author(s):  
PK Bharadwaj ◽  
AM Lee ◽  
S Mandal ◽  
BW Skelton ◽  
AH White

The synthesis and single-crystal X-ray structure determination of the title compound are recorded; crystals are monoclinic, P 21/c, a 10.309(8), b 18.817(7), c 15.542(6) Ǻ, β 121.80(5)°, Z 4; R was 0.038 for 2894 independent, 'observed' [I > 3σ(I)] reflections. The molecule has quasi-3 symmetry, with seven-coordinate bismuth [Bi-N(apical), 2.82(1); Bi-N, 2.512(8)-2.563(9); Bi-O, 2.197(8)-2.300(8)Ǻ].


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