Synthesis and antifungal properties of benzylamines containing boronate esters

2001 ◽  
Vol 79 (7) ◽  
pp. 1115-1123 ◽  
Author(s):  
Christopher M Vogels ◽  
Liliya G Nikolcheva ◽  
David W Norman ◽  
Heather A Spinney ◽  
Andreas Decken ◽  
...  
Keyword(s):  
Aspergillus Niger ◽  
Diffraction Study ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Boronate Esters ◽  
Space Group ◽  
X Ray ◽  
Antifungal Properties ◽  
High Yields

Addition of 3-H2NC6H4Bpin (pin = 1,2-O2C2Me4) to a series of aldehydes and 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)acetophenone afforded the corresponding benzylideneamines in moderate to high yields. Hydroboration of these imines with catecholborane (HBcat, cat = 1,2-O2C6H4) at room temperature gives, upon aqueous workup, the corresponding borylamines. An X-ray diffraction study was carried out on imine 1h derived from 9-anthraldehyde and 3-H2NC6H4Bpin. Crystals of1h were triclinic, a = 9.6793(4) Å, b = 10.7397(4) Å, c = 11.5353(4) Å, α = 105.1890(10)o, β = 97.3030(10)o, γ = 102.1480(10)o, Z = 2 with space group P[Formula: see text] and crystals of N-[3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]-4-methoxybenzylamine 2c were orthorhombic, a = 8.6612(4) Å, b = 10.3794(4) Å, c = 20.6033(9) Å, Z = 4 with space group P212121. Amines have been tested for their antifungal properties against Aspergillus niger and Aspergillus flavus.Key words: benzylamines, boronate esters, aminoboron, hydroboration, antifungal.

X-ray powder diffraction study on ErNi2Ge2

1999 ◽  
Vol 14 (2) ◽  
pp. 145-146
Author(s):  
Liangqin Nong ◽  
Lingmin Zeng
Keyword(s):  
Least Squares ◽  
Diffraction Study ◽  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Analysis ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

An X-ray diffraction pattern for ErNi2Ge2 at room temperature is reported. ErNi2Ge2 is tetragonal with lattice parameters a=4.0191(2) Å, c=9.7643(2) Å, space group I4/mmm, and Z=2. The lattice parameters derived from Rietveld analysis agree well with the results of a least-squares refinement.

Synthesis and reactivity of novel Schiff bases containing boronate esters

2002 ◽  
Vol 80 (1) ◽  
pp. 31-40 ◽  
Author(s):  
David W Norman ◽  
Janet P Edwards ◽  
Christopher M Vogels ◽  
Andreas Decken ◽  
Stephen A Westcott
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Schiff Bases ◽  
Oxidative Cyclization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Boronate Esters ◽  
Space Group ◽  
X Ray ◽  
Manganese Triacetate

Condensation of 2-aminophenol with boronate ester derivatives of benzaldehyde afforded the corresponding boron-containing Schiff bases, 2-HOC6H4N=C(H)C6H4R (1a: R = 2-Bpin; 1b: R = 3-Bpin; 1c: R = 4-Bpin; pin = 1,2-O2C2Me4). Crystals of 1b were triclinic, space group P[Formula: see text], a = 11.9420(6), b = 13.0871(7), and c = 13.2720(7) Å, α = 70.983(1), β = 67.793(1), and γ = 78.380(1)°, Z = 2. Reaction of 2-aminophenol with 2-HC(O)C6H4B(OH)2 in EtOH, however, gave a macrocyclic dimer 2 with a OBOBO structural unit. The molecular structure of this dimer has been confirmed by an X-ray diffraction study. Crystals of 2 were monoclinic, space group P21/c, a = 10.0447(8), b = 21.0894(15), and c = 12.6214(9) Å, β = 105.301(2)°, Z = 4. Further reaction of these Schiff bases with manganese triacetate in toluene afforded 2-arylbenzoxazoles 3a–c via an oxidative cyclization pathway. The molecular structure of the 4-Bpin derivative (3c) was characterized by an X-ray diffraction study. Crystals of 3c were monoclinic, space group P21/n, a = 6.5392(3), b = 16.3330(8), and c = 16.1942(8) Å, β = 97.9620(10)°, Z = 4.Key words: boron heterocycles, Schiff bases, arylbenzoxazoles.

CRYSTAL STRUCTURE OF ZIRCONIUM TRICHLORIDE

1964 ◽  
Vol 42 (10) ◽  
pp. 1886-1889 ◽  
Author(s):  
B. Swaroop ◽  
S. N. Flengas
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Main Cell ◽  
Diffraction Patterns

The crystal structure of zirconium trichloride was determined from X-ray diffraction patterns. Zirconium trichloride belongs to the [Formula: see text]space group. The dimensions of the main cell at room temperature are: a = 5.961 ± 0.005 Å and c = 9.669 ± 0.005 Å.The density of zirconium trichloride was measured and gave the value of 2.281 ± 0.075 g/cm3 while, from the X-ray calculations, the value was found to be 2.205 g/cm3.

Ein tricyclisches Tetraboradisiladodecan aus Dimethyl-di-1-propinylsilan und Ethyldiboranen(6) / A Tricyclic Tetraboradisiladodecane from Dimethyl-di-1-propynylsilane and Ethyldiboranes(6)

1995 ◽  
Vol 50 (3) ◽  
pp. 439-447 ◽  
Author(s):  
Roland Köster ◽  
Günter Seidel ◽  
Roland Boese ◽  
Bernd Wrackmeyer
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Structure Space ◽  
Thermal Elimination

The exhaustive hydroboration of the (C ≡ C )-groups in Me2Si(C ≡ CMe)2 (A ) by adding ethyldiboranes(6) at room temperature is presumed to lead initially to the formation of a mixture of the threo- and erythro-3,3,5,6-tetrakis(diethylboryl)-4,4-dimethyl-4-silaheptanes (1a , b). The threo-1a reacts further by borane catalysed intermolecular condensation to the substituted disilatetraboratricyclo[6.2.1.16.9]dodecane 2 with the formula , whose crystal structure [space group C2/c, a = 19.696(2), b = 10.371(1), c = 16.580(2) Å; β = 125.90(1)°; at 122 K] has been established by X -ray diffraction. In contrast, the erythro-1b undergoes intramolecular, thermal elimination of Et3B to give the 1,2-diethyl-2,4-bis(diethylboryl)- 3,3,5-trim ethyl-3-silaborolane (4). If A is added to an excess of undiluted B (“hydridebath”), then the two substituted diastereomers of the 1-carba-arachno-pentaboranes(10) (endo/exo-Et,SiH Me2) (3a, b), are formed preferentially as the result of an initial Si-C ≡-c le a v e d hydroboration.

The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2]

2019 ◽  
Vol 75 (6) ◽  
pp. 1144-1151
Author(s):  
Tamara J. Bednarchuk ◽  
Wolfgang Hornfeck ◽  
Vasyl Kinzhybalo ◽  
Zhengyang Zhou ◽  
Michal Dušek ◽  
...  
Keyword(s):  
Phase Transitions ◽  
Single Crystal ◽  
Room Temperature ◽  
Variable Temperature ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Hybrid Compound ◽  
Space Group ◽  
X Ray

The organic–inorganic hybrid compound 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2] (4apFeS), was obtained by slow evaporation of the solvent at room temperature and characterized by single-crystal X-ray diffraction in the temperature range from 290 to 80 K. Differential scanning calorimetry revealed that the title compound undergoes a sequence of three reversible phase transitions, which has been verified by variable-temperature X-ray diffraction analysis during cooling–heating cycles over the temperature ranges 290–100–290 K. In the room-temperature phase (I), space group C2/c, oxygen atoms from the closest Fe-atom environment (octahedral) were disordered over two equivalent positions around a twofold axis. Two intermediate phases (II), (III) were solved and refined as incommensurately modulated structures, employing the superspace formalism applied to single-crystal X-ray diffraction data. Both structures can be described in the (3+1)-dimensional monoclinic X2/c(α,0,γ)0s superspace group (where X is ½, ½, 0, ½) with modulation wavevectors q = (0.2943, 0, 0.5640) and q = (0.3366, 0, 0.5544) for phases (II) and (III), respectively. The completely ordered low-temperature phase (IV) was refined with the twinning model in the triclinic P{\overline 1} space group, revealing the existence of two domains. The dynamics of the disordered anionic substructure in the 4apFeS crystal seems to play an essential role in the phase transition mechanisms. The discrete organic moieties were found to be fully ordered even at room temperature.

NEUTRON DIFFRACTION STUDY ON (Bi−Pb)2Sr2Ca2Cu3O10

1990 ◽  
Vol 04 (12) ◽  
pp. 791-794 ◽  
Author(s):  
YANG JI-LIAN ◽  
YE CHUN-TANG ◽  
ZHANG BAI-SHENG ◽  
LI JI-ZHOU ◽  
KANG JIAN ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Neutron Diffraction ◽  
Diffraction Study ◽  
Single Phase ◽  
Polycrystalline Sample ◽  
Neutron Diffraction Study ◽  
Structure Study ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The polycrystalline sample of (Bi–Pb)2Sr2Ca2Cu3O10 with Tc=107 K was prepared. The X-ray diffraction proved that the sample is single phase. The crystal structure study on the sample has been carried out by neutron diffraction. The result shows that its structure is tetragonal body-centre structure with space group of I4/mmm, containing a few oxygen atoms at 4e site in Bi–Pb layers.

scholarly journals Synthesis and Characterization of New Diiron and Diruthenium μ-Aminocarbyne Complexes Containing Terminal S-, P- and C-Ligands

2007 ◽  
Vol 62 (3) ◽  
pp. 427-438 ◽  
Author(s):  
Vincenzo G. Albano ◽  
Luigi Busetto ◽  
Fabio Marchetti ◽  
Magda Monari ◽  
Stefano Zacchini ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Coordination Mode ◽  
Bond Cleavage ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dithiocarbamate Ligand ◽  
High Yields

The diiron aminocarbyne complexes [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (R = Xy1, 1a; R = Me, 1b; R = CH2Ph, 1c; Xy1 = 2,6-Me2C6H3) undergo replacement of the coordinated nitrile by halides, diethyldithiocarbamate, and dicyanomethanide to give [Fe2{μ-CN(Me) (R)}(μ-CO)(CO)(X)(Cp)2] complexes (R = Me, X = Br, 4a; R = Me, X = I, 4b; R = CH2Ph, X = Cl, 4c; R = CH2Ph, X = Br, 4d; R = CH2Ph, X = I, 4e; R = Xy1, X = SC(S)NEt2, 5a; R = Me, X = SC(S)NEt2, 5b; R = Xy1, X = CH(CN)2, 7), in good yields. The molecular structure of 5a shows an unusual η1 coordination mode of the dithiocarbamate ligand. Similarly, treatment of [M2{μ-CN(Me) (R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (M = Fe, R = Xy1, 1a; M = Fe, R = Me, 1b; M = Ru, R = Xy1, 2a; M = Ru, R = Me, 2b) with a series of phosphanes generates the cationic complexes [M2{μ- CN(Me)(R)}(μ-CO)(CO)(P)(Cp)2][SO3CF3] (M = Fe, R = Xy1, P = PPh2H, 6a; M = Fe, R = Xy1, P = PPh3, 6b; M = Fe, R = Xy1, P = PMe3, 6c; M = Fe, R = Me, P = PMe2Ph, 6d; M = Fe, R = Me, P = PPh3, 6e; M = Fe, R = Me, P = PMePh2, 6f; M = Ru, R = Xy1, P = PPh2H, 6g; M = Ru, R = Me, P = PPh2H, 6h), in high yields. The molecular structure of 6a has been elucidated by an X-ray diffraction study. The reactions of [Fe2{μ-CN(Me)(Xyl)}(μ-CO)(CO)(NCR′)(Cp)2][SO3CF3] [R′ = Me, 1a; R′ = tBu, 3] with PhLi and PPh2Li yield [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(Ph)(Cp)2] (8) and [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(PPh2)(Cp)2] (9), respectively. The molecular structure of 8 has been ascertained by X-ray diffraction. Conversely, the reaction of 1a with MeLi generates the aminoalkylidene compound [Fe2{C(Me)N(Me)(Xy1)}(μ-CO)2(CO)(Cp)2] (10).Finally, the acetone complex [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(OCMe2)(Cp)2][SO3CF3] (12) reacts with lithium acetylides to give complexes [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(C≡CR)(Cp)2] (R = p-C6H4Me, 11a; R = Ph, 11b; R = SiMe3, 11c), in high yields. Filtration through alumina of a solution of 11a in CH2Cl2 results in hydration of the acetylide group and C-Si bond cleavage, affording [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO){C(O)Me}(Cp)2] (12).

X-ray powder diffraction data for compound DyNiSn

1997 ◽  
Vol 12 (3) ◽  
pp. 134-135
Author(s):  
Liangqin Nong ◽  
Lingmin Zeng ◽  
Jianmin Hao
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Figure Of Merit ◽  
Room Temperature ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Diffraction Patterns

The compound DyNiSn has been studied by X-ray powder diffraction. The X-ray diffraction patterns for this compound at room temperature are reported. DyNiSn is orthorhombic with lattice parameters a=7.1018(1) Å, b=7.6599(2) Å, c=4.4461(2) Å, space group Pna21 and 4 formula units of DyNiSn in unit cell. The Smith and Snyder Figure-of-Merit F30 for this powder pattern is 26.7(0.0178,63).

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