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.

Reactions of Transition-Metal Sigma-Acetylides. V. Synthesis and X-Ray Structure of Co2(µ-η2-PhC2Fe(Co)2(η-C5h5))(Co)6

1986 ◽  
Vol 39 (1) ◽  
pp. 159 ◽  
Author(s):  
MI Bruce ◽  
DN Duffy ◽  
MG Humphrey
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Single Crystal ◽  
Diffraction Study ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Independent Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The reaction between Co2(CO)8 and Fe(C2Ph)(CO)2(η-C5H5) gave the title complex in 44% yield. The molecular structure was determined from a single-crystal X-ray diffraction study, and consists of the transition metal acetylide acting as a conventional μ- alkyne ligand to a Co2(CO)6 unit. Crystals are monoclinic, space group P21/n, with a 11.610(8), b 14.657(4), c 12.526(6)Ǻ, β 90.30(5)°, and Z 4; 1683 independent data were refined to R 0.080, Rw 0.087.

Late metal salicylaldimine complexes derived from 5-aminosalicylic acid — Molecular structure of a zwitterionic mono Schiff base zinc complex

2005 ◽  
Vol 83 (8) ◽  
pp. 1063-1070 ◽  
Author(s):  
Tara A Bourque ◽  
Megan E Nelles ◽  
Teri J Gullon ◽  
Christian N Garon ◽  
Melissa K Ringer ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Schiff Base ◽  
Diffraction Study ◽  
Monoclinic Space Group ◽  
Aminosalicylic Acid ◽  
X Ray Diffraction ◽  
Compound A ◽  
Space Group ◽  
X Ray ◽  
New Compounds

Condensation of salicylaldehyde (2-HOC6H4C(O)H) with 5-aminosalicylic acid (5-H2NC6H3-2-(OH)-CO2H) afforded the Schiff base 2-HOC6H4C(H)=NC6H3-2-(OH)-5-CO2H (a). Similar reactivity with 5-bromosalicylaldehyde was also observed to give 5-Br-2-HOC6H3C(H)=NC6H3-2-(OH)-5-CO2H (b). Reaction of these salicylaldehydes with Pd(II), Cu(II), and Zn(II) salts gave the corresponding bis(N-arylsalicylaldiminato)metal complexes (M = Pd (1), Cu (2), Zn (3)). The molecular structure of the Schiff base compound a has been confirmed by an X-ray diffraction study. Crystals of a were monoclinic, space group P2(1)/c, a = 7.0164(7) Å, b = 11.0088(11) Å, c = 14.8980(15) Å, β = 102.917(2)°, Z = 4. The molecular structure of a novel zwitterionic conformer of 3a was also characterized by an X-ray diffraction study. Crystals of 4 were monoclinic, space group P2(1)/c, a = 9.5284(5) Å, b = 19.5335(11) Å, c = 8.6508(5) Å, β = 90.596(1)°, Z = 4. All new compounds have been tested for their antifungal activity against Aspergillus niger and Aspergillus flavus. Key words: 5-aminosalicylic acid (5-ASA), antifungal, copper, palladium, salicylaldimines, Schiff base, zinc.

The crystal structure of dibutyl-bis(pentamethylenedithiocarbamato)tin(IV)

1986 ◽  
Vol 51 (11) ◽  
pp. 2521-2527 ◽  
Author(s):  
Jan Lokaj ◽  
Eleonóra Kellö ◽  
Viktor Kettmann ◽  
Viktor Vrábel ◽  
Vladimír Rattay
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Coordination Polyhedron ◽  
Crystal And Molecular Structure ◽  
Distorted Octahedron ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal and molecular structure of SnBu2(pmdtc)2 has been solved by X-ray diffraction methods and refined by a block-diagonal least-squares procedure to R = 0.083 for 895 observed reflections. Monoclinic, space group C2, a = 19.893(6), b = 7.773(8), c = 12.947(8) . 10-10 m, β = 129.07(5)°, Z = 2, C20H38N2S4Sn. Measured and calculated densities are Dm = 1.38(2), Dc = 1.36 Mg m-3. Sn atom, placed on the twofold axes, is coordinated with four S atoms in the distances Sn-S 2.966(6) and 2.476(3) . 10-10 m. Coordination polyhedron is a strongly distorted octahedron. Ligand S2CN is planar.

The crystal and molecular structure of a platinum-silatrane complex

1977 ◽  
Vol 30 (5) ◽  
pp. 1007 ◽  
Author(s):  
GR Scollary
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

A structural analysis of the platinum-silatrane complex, PtCl [Si(OCH2CH2)3N] [PMe2Ph]2, has been carried out by X-ray diffraction. Crystals are monoclinic, space group P21/c, a 6.630(4), b 17.465(6), c 22.297(6) Ǻ, β 97.4(2)�, Z 4. The structure has been refined by a full- matrix least-squares procedure to R 0.048 for 2165 reflections. Basic geometries are square (platinum), tetrahedral (silicon) and trigonal (nitrogen). Within the silatrane ligand, the Si-N non-bonding distance is 2.89(1) Ǻ.

scholarly journals Efficient Synthesis and X-ray Structure of [1,2,4]Triazolo[4,3-a]pyriaadines via Oxidative Cyclization Using N-Chlorosuccinimide (NCS)

Crystals ◽  
2021 ◽  
Vol 11 (10) ◽  
pp. 1156
Author(s):  
Said El-Kurdi ◽  
Bassam Abu Thaher ◽  
Kanan Wahedy ◽  
Dieter Schollmeyer ◽  
Levin Nopper ◽  
...  
Keyword(s):  
Biological Activity ◽  
Oxidative Cyclization ◽  
Monoclinic Space Group ◽  
Efficient Synthesis ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Mild Conditions ◽  
Pharmaceutical Applications

Triazolopyridines are a family of compounds that, owing to their biological activity, have many pharmaceutical applications. In this study, 3-(pyridine-4-yl)-[1,2,4]triazolo[4,3-a]pyridine and 6-bromo-3-(pyridine-4-yl)-[1,2,4]triazolo[4,3-a]pyridine were synthesized by using the chlorinated agent NCS for hydrazones under very mild conditions. The characterization of these compounds was achieved by 1H NMR, 13C NMR, FTIR, MS and X-ray diffraction. The compound 3-(pyridine-4-yl)-[1,2,4]triazolo[4,3-a]pyridine was crystallized in the monoclinic space group P 21/c with a = 15.1413(12), b = 6.9179(4), c = 13.0938(8) Å, β = 105.102(6)°, V = 1324.16(16)Å3, Z = 4, and R = 0.0337. Also compound 6-bromo-3-(pyridine-4-yl)-[1,2,4]triazolo[4,3-a]pyridine was crystallized in the monoclinic space group P 21/c with a = 14.3213(11), b = 6.9452(4) (4), c = 12.6860(8)Å, β = 100.265(6)°, V = 1241.62(14)Å3, Z = 4, and R = 0.0561.

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.

Synthesis, characterization, and bioactivities of platinum(II) complexes bearing pyridinecarboxaldimines containing aliphatic groups

2013 ◽  
Vol 91 (2) ◽  
pp. 131-136 ◽  
Author(s):  
Erin L. Stewart ◽  
Alyssa E. Patterson ◽  
Taryn O'Neill ◽  
Haoxin Li ◽  
Andrew Flewelling ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Platinum Complexes ◽  
Primary Amines ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

Condensation of 2-pyridinecarboxaldehyde with six primary amines containing aliphatic groups gave the corresponding pyridinecarboxaldimines (N-N′R). Addition of these ligands to [PtCl2(coe)]2 (coe = cis-cyclooctene) gave complexes of the type cis-PtCl2(N-N′R) (1: R = propyl, 2: R = hexyl, 3: R = octyl, 4: R = nonyl, 5: R = hexadecyl, and 6: R = octadecyl) in moderate yields. The molecular structure of the hexyl derivative (2) has been confirmed by an X-ray diffraction study. Crystals of 2 were triclinic with a = 8.6858(19) Å, b = 8.7567(19) Å, c = 9.5080(19) Å, α = 76.546(3)°, β = 87.151(3)°, and γ = 78.586(3)° in the space group P1. All platinum complexes show considerable anti-bacterial and anti-mycobacterial properties.

Interaction of the methylmercury cation with glycine and alanine: a vibrational and X-ray diffraction study

1986 ◽  
Vol 64 (9) ◽  
pp. 1876-1884 ◽  
Author(s):  
Marie-Claude Corbeil ◽  
André L. Beauchamp ◽  
Serge Alex ◽  
Rodrigue Savoie
Keyword(s):  
Aqueous Solutions ◽  
Diffraction Study ◽  
Raman Spectra ◽  
Infrared Spectra ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Carboxylate Oxygen

The complexes (CH3Hg)Gly, (CH3Hg)(L-Ala), and (CH3Hg)(DL-Ala) were prepared by reacting CH3HgOH with glycine (HGly) and alanine (HAla). Crystals of (CH3Hg)(DL-Ala) are monoclinic, space group P21/c, a = 9.460(2), b = 8.794(2), c = 8.723(2) Å, β = 97.49(2)°, Z = 4. The structure was refined on 935 MoKα reflections to R = 0.042. The complex results from displacement of an alanine NH3+ proton by the CH3Hg+ ion, which is linearly bonded to the —NH2 group. An intramolecular Hg … O contact of 2.63 Å is also formed with a carboxylate oxygen. The Raman and infrared spectra of solid (CH3Hg)Gly and (CH3Hg)(L-Ala) are compared with those of the ligands. Raman spectra of aqueous solutions at different pH indicate that the NH2-bonded structure is retained in solution, although no complexation via the carboxylate occurs.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

New mixed-valent alkali chain sulfido ferrates A1+x[FeS2] (A = K, Rb, Cs; x = 0.333–0.787)

2020 ◽  
Vol 235 (8-9) ◽  
pp. 275-290
Author(s):  
Michael Schwarz ◽  
Pirmin Stüble ◽  
Katharina Köhler ◽  
Caroline Röhr
Keyword(s):  
Alkali Metal ◽  
General Structure ◽  
Variable Number ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Modulated Structure ◽  
Space Group ◽  
X Ray ◽  
Local Coordination ◽  
Natural Pyrite

AbstractFour new mixed-valent chain alkali metal (A) sulfido ferrates of the general structure family ${A}_{1+x}\left[{\text{Fe}}_{x}^{\text{II}}{\text{Fe}}_{1-x}^{\text{III}}{\text{S}}_{2}\right]$ were synthesized in the form of tiny green-metallic needles from nearly stoichiometric melts reacting elemental potassium with natural pyrite (A = K) or previously prepared Rb2S/Cs2S2 with elemental iron and sulfur (A = Rb/Cs). The crystal structures of the compounds were determined by means of single crystal X-ray diffraction: In the (3+1)D modulated structure of K7.15[FeS2]4 (space group Ccce(00σ3)0s0, a = 1363.87(5), b = 2487.23(13), c = 583.47(3) pm, q = 0,0,0.444, R1 = 0.055/0.148, x = 0.787), a position modulation of the two crystallographically different undulated ${}_{\infty }{}^{1}\left[{\text{FeS}}_{4/2}\right]$ tetrahedra chains and the surrounding K cations is associated with an occupation modulation of one of the three potassium sites. In the case of the new monoclinic rubidium ferrate Rb4[FeS2]3 (x = $\frac{1}{3}$; space group P21/c, a = 1640.49(12), b = 1191.94(9), c = 743.33(6) pm, β = 94.759(4)°, Z = 4, R1 = 0.1184) the undulation of the tetrahedra chain is commensurate, the repetition unit consists of six tetrahedra. In the second new Rb ferrate, Rb7[FeS2]5 (x = 0.4; monoclinic, space group C2/c, K7[FeS2]5-type; a = 2833.9(2), b = 1197.36(9), c = 744.63(6) pm, β = 103.233(4)°, Z = 4, R1 = 0.1474) and its isotypic mixed Rb/Cs-analog Rb3.6Cs3.4[FeS2]5 (a = 2843.57(5), b = 1226.47(2), c = 759.890(10) pm, β = 103.7170(9)°, R1 = 0.0376) the chain buckling leads to a further increased repetition unit of 10 tetrahedra. For all mixed-valent ferrates, the Fe–S bond lengths continuously increase with the amount (x) of Fe(II). The buckling of the chains is controlled through the local coordination of the S atoms by the variable number of A cations of different sizes.

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