X-ray diffraction study of crystal and molecular structures of azo compounds of two beta-diketones

2019 ◽  
Vol 60 (10) ◽  
pp. 1681-1687
Author(s):  
F. N. Bahmanova ◽  
Sh. A. Tahirli ◽  
R. K. Askerov ◽  
S. R. Hajiyeva ◽  
F. M. Chyragov

1980 ◽  
Vol 33 (1) ◽  
pp. 195 ◽  
Author(s):  
MI Bruce ◽  
DA Kelly ◽  
GM Mclaughlin ◽  
GB Robertson ◽  
IB Tomkins ◽  
...  

The reaction between RuCl3,nH2O and P(OMe)3 affords RuCl2[P(OMe)3]4; one batch of RuCl3,-nH2O also gave amminetrichlorobis(trimethyl phosphite)ruthenium(III), RuCl3(NH3)[P(OMe)3]2, as a minor product. The structure of this complex has been determined from a single-crystal X-ray diffraction study (4598 data, R 0.065, Rw 0.090): the ruthenium is approximately octahedrally coordinated by the three mer chloro, two trans P(OMe)3 and one NH3 ligands. Crystals are monoclinic,P21/n, a 8.725(3), b 18.286(7), c 10.936(4)Ǻ, β 94.57(3)°, Z 4.


1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.


1990 ◽  
Vol 45 (10) ◽  
pp. 1369-1382 ◽  
Author(s):  
Heindirk tom Dieck ◽  
Lutz Stamp

Diazadienes RN = CR′-CR′ = NR (DAD) form molecular complexes with copper(I) halides of composition (DAD)CuX, the structures of which vary from [(DAD)2Cu]+(CuCl2)⁻ with a non-tetrahedral bis(chelated) cation, over [(DAD)CuCl]2 with asymmetrically bridging chloro ligands to planar three-coordinate (DAD)CuCl. The composition of the isolated complexes depends on the relative concentrations or on the solvent. The “soft” coordination geometry of copper is underlined by the structure of the coordination polymer of composition (DAD)2Cu5Cl5, in which Cu atoms of coordination number 2, 3 and 4 and very irregular geometries are encountered and where the DAD ligands are exclusively bridging. Halide ions and sp2-nitrogen donors are very competitive. Bridging DAD ligands are also encountered in (DAD)Cu-Y with the less nucleophilic anions trifluoromethane-sulphonate or perchlorate. Crystal and molecular structures are established for all these coordination geometries and the causes are discussed for the coordination flexibility of copper(I)


1986 ◽  
Vol 41 (5) ◽  
pp. 581-586 ◽  
Author(s):  
Konrad Holl ◽  
Ulf Thewalt

Among the reaction products of S4N4 with SnCl4 in chloroform, that contains acetic acid and small amounts of water, there are two salts S4N4H+[SnCl5(H2O)]- (A) and (S3N2NH2+)2[SnCl6]2- (B), both containing protonated SnNm units. The crystal and molecular structures of A and B have been determined by X-ray diffraction. A: monoclinic, P21/c, a = 9.084(2), b - 23.758(4), c = 6.587(1) Å , β = 101.86(3)°, Dc = 2.383 g·cm-3 and Z = 4. B: monoclinic, P21/n, a = 9.882(3), b = 12.873(4), c = 6.807(2) Å , β = 93.77(5)°, Dc = 2.352 g·cm-3 and Z = 2. The structures of the cations in both compounds agree well with those found of other salts containing these cations.


1975 ◽  
Vol 53 (18) ◽  
pp. 2707-2713 ◽  
Author(s):  
Debbie Allen ◽  
Colin James Lyne Lock ◽  
Graham Turner ◽  
John Powell

The crystal and molecular structures of pentane-2,4-dionato-(2,3,5,6-tetrahapto-2,3-dicarbomethoxo[2.2.1]bicycloheptadienerhodium(I), Rh(C5H7O2)(C7H6(CO2CH3)2), have been measured by single crystal X-ray diffraction. The orange crystals are monoclinic, space group P21/c, Z = 4, a = 9.245(4), b = 9.003(4), c = 21.680(15) Å, β = 113.41(5)°. The calculated and observed densities are 1.645 and 1.642(5) respectively. Intensity data were collected on a Syntex [Formula: see text] diffractometer and a full matrix least squares refinement on 3010 observed reflections leads to a conventional R = 0.0660. The structure can be considered as a roughly square planar arrangement of ligands around the rhodium atom composed of two β-ketoenolate oxygen atoms (Rh—O, 2.037(5) and 2.025(5) Å ) and the centers of the two ethylenic groups. The Rh—C distances for the olefin group attached to the two carbomethoxo groups, 2.117(8), 2.108(8) Å, appear to be slightly larger than those for the other olefinic group, 2.087(7), 2.082(6), and the corresponding C=C distances of 1.375(10) and 1.410(9) Å are different at the 95% confidence level.


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