Reactions of aminoboron compounds with palladium and platinum complexes

1999 ◽  
Vol 77 (7) ◽  
pp. 1196-1207 ◽  
Author(s):  
Christopher M Vogels ◽  
Heather L Wellwood ◽  
Kumar Biradha ◽  
Michael J Zaworotko ◽  
Stephen A Westcott
Keyword(s):  
Diffraction Study ◽  
Boronic Acid ◽  
Methylene Chloride ◽  
Palladium Complex ◽  
Bond Cleavage ◽  
Platinum Complexes ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Palladium And Platinum Complexes

Reactions of 3-NH2C6H4B(OH)2 (1, APBA) with [MCl4]2- (M = Pd, Pt) give the boronic acid-containing complexes, MCl2(APBA)2 (M = Pd, 2; M = Pt, 3). Addition of 1 to [PdCl2(COE)]2 (COE = η2-C8H14) ultimately led to PdCl2(APBA)2 (2). The pinacol derivative PdCl2(APBpin)2 (5, pin = O2C2Me4) was characterized by an X-ray diffraction study. Crystals of 5 were monoclinic, a = 13.836(5), b = 14.937(5), c = 11.287(5) Å, β = 99.042(9)°, Z = 2, with space group P21/c. Monoalkene complexes PtCl2(COE)(APBA) (8) and PtCl2(COE)(APBpin) (9) were generated from the addition of APBA and APBpin, respectively, to [PtCl2(COE)]2. Reactions of 2-NMe2CH2C6H4B(OH)2 (10) with palladium complex [PdCl2(COE)]2 proceed via selective B—C bond cleavage to give the cyclopalladated dimer [PdCl(2-NMe2CH2C6H4)]2 as the major amine-containing product. Likewise, reactions with borinic esters H2NCH2CH2OBR2 (R = Bu, 14; R = Ph, 15) give products derived from cleavage of the B—O bond. The unique palladium complex PdCl2[3-NC5H4B(OH)2]2 (19) was prepared by addition of (3-NC5H4BEt2)4 (18) to [PdCl2(COE)]2 in wet methylene chloride, where adventitious water was used to convert the organoborane product into the corresponding boronic acid moiety.Key words: aminoboronic acids, platinum, palladium, cyclomηllation.

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.

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).

scholarly journals Addition of boranes to (E)-(η5-C5H5)2Zr(CH=CHPh)Cl

2013 ◽  
Vol 11 (5) ◽  
pp. 811-816
Author(s):  
Patrick Ferland ◽  
Kathleen Prosser ◽  
Jeremy Bourque ◽  
Ian Edwards ◽  
Nathan Hamilton ◽  
...  
Keyword(s):  
Carbon Atom ◽  
Diffraction Study ◽  
Zirconium Oxide ◽  
Organic Molecule ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

AbstractIn this study, the addition of boranes to (E)-(η5-C5H5)2Zr(CH=CHPh)Cl (3) has been examined in order to investigate the regioselectivity of these ‘hydroboration’ reactions. We have found that these additions proceed with remarkable selectivity to give exclusive formation of a saturated organic molecule where one carbon atom has both the boron and the zirconium fragments. These reactions do not proceed via a conventional hydroboration reaction, but instead go through an initial transmetalation step to generate (E)-(η5-C5H5)2Zr(H)Cl (1) and the corresponding alkenyl boron intermediate, whereupon subsequent hydrozirconation of this latter species gives the geminal products. An x-ray diffraction study has been conducted on gem-(η5-C5H5)2Zr(CH(Bpin)CH2Ph)Cl (pin = 1, 2-O2C2Me4) (2). Crystals of 2 were orthorhombic with a = 18.545(3) Å, b = 15.713(3) Å, c = 16.157(3) Å in the space group Pccn. An x-ray diffraction study has also been conducted on the trinuclear zirconium oxide species (η5-C5H5)2ZrO2[ZrCl(η5-C5H5)2]2(4). Crystals of 4 were orthorhombic with a = 13.6000(8) Å, b = 14.2252(8) Å, c = 17.6500(10) Å in the space group P2(1)2(1)2(1).

X-RAY DIFFRACTION STUDY OF THE MODULATED STRUCTURE IN SUPERCONDUCTING SINGLE-CRYSTAL Bi2Sr2CaCu2Oy

1988 ◽  
Vol 02 (08) ◽  
pp. 985-991 ◽  
Author(s):  
X. CHU ◽  
Z.H. MAI ◽  
Y.F. YAN ◽  
J.H. WANG ◽  
D.N. ZHENG ◽  
...  
Keyword(s):  
Experimental Data ◽  
Single Crystal ◽  
Diffraction Study ◽  
Basic Structure ◽  
X Ray Diffraction ◽  
Modulated Structure ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Average Structure

X-ray precession technique1 has been utilized to study the reciprocal space of the superconducting single crystal Bi 2 Sr 2 CaCu 2 O y. An average structure with space group of Pnnn and a real structure with the superspace group of [Formula: see text] or [Formula: see text] have been found for this one dimensional modulated incommensurate material. As well, a basic structure with the space group of Fmmm is derived from the experimental data.

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.

Synthesis and characterization of hydrophilic hydroxy-pyridinones and their complexes with molybdenum(VI)

2000 ◽  
Vol 53 (8) ◽  
pp. 687 ◽  
Author(s):  
Noah A. Epstein ◽  
Jennifer L. Horton ◽  
Christopher M. Vogels ◽  
Nicholas J. Taylor ◽  
Stephen A. Westcott
Keyword(s):  
Diffraction Study ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Hydroxy Groups

We have prepared four N-substituted hydroxypyridinones containing alcohol and morpholine groups. Complexes of the type cis-MoO2L2, where L represents the hydroxypyridinonato ligands have also been synthesized. The ethanolamine derivative, cis-MoO2(hep)2 (5), has been characterized by an X-ray diffraction study whereby the pyridinone ligands are bound to molybdenum in a cis bidentate fashion via the deprotonated hydroxy groups and the ketone moieties. Crystals of (5) are triclinic, with a 9.1930(7), b 14.2718(8), c 14.6219(9) Å, α 106.816(5), β 95.902(5), γ 96.350(5)°, Z 4, space group P–1.

scholarly journals Synthesis, reactivity, and antimicrobial properties of boron-containing 4-ethyl-3-thiosemicarbazide derivatives

2018 ◽  
Vol 96 (10) ◽  
pp. 906-911 ◽  
Author(s):  
Ryan S. Scott ◽  
Alex J. Veinot ◽  
Darcie L. Stack ◽  
Patrick T. Gormley ◽  
B. Ninh Khuong ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Saccharomyces Cerevisiae ◽  
Pseudomonas Aeruginosa ◽  
Aspergillus Niger ◽  
Diffraction Study ◽  
Boronic Acid ◽  
Antimicrobial Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thiosemicarbazide Derivatives

The addition of 4-ethyl-3-thiosemicarbazide to benzaldehyde and boronic acid containing derivatives afforded the corresponding thiosemicarbazones (1–3) or benzodiazaborines (4–6) depending on the position of the boronic acid within the ring. All compounds have been characterized fully including an X-ray diffraction study of the methoxy-containing benzodiazaborine 6. Attempts to coordinate thiosemicarbazones 2 and 3 to palladium(II) acetate were unsuccessful; however, addition of the non-boron-containing derivative 1 to palladium afforded complex 7 whose molecular structure was determined by an X-ray diffraction study. The initial bioactivities of compounds 1–7 were examined against two fungi, Aspergillus niger and Saccharomyces cerevisiae, and two bacteria, Bacillus cereus and Pseudomonas aeruginosa.

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.

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