Synthesis, Spectroscopic Characterization, and Structure of closo-1,10-B10H8F22- and Related Fluorinated Derivatives of B10H102-

The treatment of salts of the B10H102- anion with the commercially available N-fluoro reagent 1-chloromethyl-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) (F-TEDA) resulted in the formation of fluorinated derivatives of this ten-vertex borane dianion. The effects of changing the solvent, temperature, and reagent stoichiometry were studied. The derivatives 1-B10H9F2-, 2-B10H9F2-, 1,2-B10H8F22-, 1,6-B10H8F22-, 1,10-B10H8F22-, and 1,2,10-B10H7F32- were examined by a combination of 11B and 19F NMR spectroscopy and by IR spectroscopy. The salt [Ph4P]2[1,10-B10H8F2] . 3 CH2Cl2 was structurally characterized by single-crystal X-ray crystallography: C51H48B10Cl6F2P2, monoclinic, C2/c, a = 13.8134(9), b = 19.141(1), c = 21.136(1) Å, β = 91.546(1)°, Z = 4, T = -100 °C, R = 0.077.

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The Conformation of Some 1,6-Disulfide-Bridged D-Hexopyranoses

Australian Journal of Chemistry ◽

10.1071/ch04291 ◽

2005 ◽

Vol 58 (3) ◽

pp. 199 ◽

Cited By ~ 3

Author(s):

Ethan D. Goddard-Borger ◽

Brian W. Skelton ◽

Robert V. Stick ◽

Allan H. White

Keyword(s):

Nmr Spectroscopy ◽

Single Crystal ◽

1H Nmr ◽

1H Nmr Spectroscopy ◽

Similar Investigation ◽

X Ray ◽

X Ray Crystallography ◽

Structure Determinations ◽

Derivatives Of

The use of 1H NMR spectroscopy, in tandem with X-ray crystallography, has cast light on the conformation of the 1,6-disulfide-bridged derivatives of d-gluco-, d-manno-, d-allo-, d-galacto-, and d-talo-pyranose. A similar investigation was performed on the thiosulfinate derived from the d-gluco disulfide. Single-crystal X-ray structure determinations are reported for (1S,5S,6S,7S,8R)-6,7,8-tribenzoyloxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane, (1S,5S,6S,7R,8R)-6,7,8-tribenzoyloxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane, and (1S,2S,5S,6S,7S,8R)-6,7,8-triacetoxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane 2-oxide.

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Synthesis, Structure, and Antiproliferative Activity of Three Gallium(III) Azole Complexes

Bioinorganic Chemistry and Applications ◽

10.1155/2010/168030 ◽

2010 ◽

Vol 2010 ◽

pp. 1-10 ◽

Cited By ~ 14

Author(s):

Stergios Zanias ◽

Giannis S. Papaefstathiou ◽

Catherine P. Raptopoulou ◽

Konstantinos T. Papazisis ◽

Vasiliki Vala ◽

...

Keyword(s):

Ir Spectroscopy ◽

Single Crystal ◽

Antiproliferative Activity ◽

Bioinorganic Chemistry ◽

Anionic Complex ◽

X Ray ◽

X Ray Crystallography ◽

Mononuclear Complexes ◽

Human And Mouse ◽

Antiproliferative Activities

As part of our interest into the bioinorganic chemistry of gallium, gallium(III) complexes of the azole ligands 2,1,3-benzothiadiazole (btd), 1,2,3-benzotriazole (btaH), and 1-methyl-4,5-diphenylimidazole (L) have been isolated. Reaction of btaH or btd withGaBr3orGaCl3resulted in the mononuclear complexes[GaBr3(btaH)2](1) and[GaCl3(btd)2](2), respectively, while treatment ofGaCl3with L resulted in the anionic complex(LH)2[GaCl4](3). All three complexes were characterized by single-crystal X-ray crystallography and IR spectroscopy, while their antiproliferative activities were investigated against a series of human and mouse cancer cell lines.

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2-(3,5-Dimethyl-1H-pyrazol-1-yl)thiazolo[4,5-b]pyridine

Molbank ◽

10.3390/m1077 ◽

2019 ◽

Vol 2019 (3) ◽

pp. M1077

Author(s):

Lan ◽

Zheng ◽

Wang

Keyword(s):

Nmr Spectroscopy ◽

Single Crystal ◽

1H Nmr ◽

Structure Determination ◽

1H Nmr Spectroscopy ◽

Pyrazole Ring ◽

Hydrogen Atoms ◽

X Ray ◽

X Ray Crystallography

The compound 2-(3,5-dimethyl-1H-pyrazol-1-yl)thiazolo[4,5-b]pyridine (1) was synthesized with a yield of 71% by the reaction of 1-(thiazolo[4,5-b]pyridine-2-yl)hydrazine and acetylacetone. The structure was characterized by a single-crystal X-ray structure determination as well as 1H and 13C{1H} NMR spectroscopy. X-ray crystallography on 1 confirms the molecule consists of a pyridine–thiazole moiety and the pyrazole ring, and all non-hydrogen atoms are planar.

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Synthesis and Characterization of Tetrakis(pentafluoroethyl)germane

Synthesis ◽

10.1055/s-0036-1589005 ◽

2017 ◽

Vol 49 (11) ◽

pp. 2389-2393 ◽

Cited By ~ 3

Author(s):

Stefanie Pelzer ◽

Beate Neumann ◽

Hans-Georg Stammler ◽

Nikolai Ignat’ev ◽

Reint Eujen ◽

...

Keyword(s):

Mass Spectrometry ◽

Nmr Spectroscopy ◽

Ir Spectroscopy ◽

Diffraction Analysis ◽

Spectroscopic Characterization ◽

Synthesis And Characterization ◽

X Ray Diffraction ◽

X Ray ◽

Comprehensive Characterization

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.

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Trigold(I) Phosphine Derivatives of Clusters Containing Octahedral Rh2Ru4B-Boride Cores: The X-Ray Structure of [Rh2Ru4(CO)15Rh2Ru4B{AuPCy3}3] (Cy = cyclohexyl)

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc19990959 ◽

1999 ◽

Vol 64 (6) ◽

pp. 959-970 ◽

Cited By ~ 2

Author(s):

Andrew D. Hattersley ◽

Catherine E. Housecroft ◽

Arnold L. Rheingold

Keyword(s):

Nmr Spectroscopy ◽

Single Crystal ◽

Boron Atom ◽

Variable Temperature ◽

Mass Spectrometric ◽

X Ray Diffraction ◽

X Ray ◽

The Third ◽

Phosphine Derivatives ◽

Derivatives Of

The reaction of [Rh(CO)2Cl]2 with [HRu4(CO)12BH]- followed by treatment with an excess (at least three-fold) of [Cy3PAuCl] (Cy = cyclohexyl) leads to the formation of [Rh2Ru4(CO)16B{AuPCy3}] (previously prepared by another route) and [Rh2Ru4(CO)15B{AuPCy3}3]. The new trigold derivative has been characterized by spectroscopic and mass spectrometric methods, and by single crystal X-ray diffraction. It possesses an octahedral Rh2Ru4 core containing an interstitial boron atom; two of the gold(I) phosphine units cap two adjacent faces and the third bridges an edge of the octahedral cage. There are no close Au···Au contacts. Reactions of [Rh2Ru4(CO)16B]- with [(R3PAu)3O]+ (R = Ph, 2-MeC6H4) resulted in the formation of [Rh2Ru4(CO)15B{AuPR3}3]; for R = Ph, two isomers in respect of the arrangements of the AuPPh3 were isolated. Fluxional processes involving the gold(I) phosphine fragments have been observed using solution variable-temperature 31P NMR spectroscopy.

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Synthesis and Structure of an Aluminum Bis(3-chloropentanedionate) Isopropoxide: [Al(μ-OiPr)(3-Clacac)2]2

Zeitschrift für Naturforschung B ◽

10.5560/znb.2014-3332 ◽

2014 ◽

Vol 69 (7) ◽

pp. 799-803 ◽

Cited By ~ 1

Author(s):

Kiran Gupta ◽

Peter Mayer ◽

Ashutosh Pandey

Keyword(s):

Ir Spectroscopy ◽

Ambient Temperature ◽

Single Crystal ◽

Molar Ratio ◽

Monoclinic Space Group ◽

Space Group ◽

X Ray ◽

X Ray Crystallography ◽

Elemental Analyses

1A[Al(OiPr)3]4 was reacted at ambient temperature with 3-chloropentanedione (3-ClacacH) in 1 : 1 molar ratio in toluene, to obtain the mono-substituted product. However, the bis-substituted dinuclear tetrakis(3-chloropentanedionato)-di-m-isopropoxy-dialuminum(III) [Al(μ-OiPr)(3-Clacac)2]2 () was isolated in 46% yield upon aging of the reaction mixture at −10 °C. The supernatant upon aging yielded a crop of tris-3-chloroacetylacetonate Al(3-Clacac)3·H2O (1) in 13% yield. Complexes 1A (monoclinic, space group P21/c with Z = 2) and 1(cubic, space group P43n with Z = 8) were characterized by elemental analyses, NMR and IR spectroscopy and single-crystal X-ray crystallography.

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Preparation, Crystal Structure and Spectroscopic Characterization of [Ga(OH)(SO4)(terpy)(H2O)] · H2O (terpy=2,2’:6’,2-Terpyridine): The First Characterized Gallium(III) Sulfato Complex

Zeitschrift für Naturforschung B ◽

10.1515/znb-2004-0310 ◽

2004 ◽

Vol 59 (3) ◽

pp. 291-297 ◽

Cited By ~ 11

Author(s):

Andreas Sofetis ◽

Giannis S. Papaefstathiou ◽

Aris Terzis ◽

Catherine P. Raptopoulou ◽

Theodoros F. Zafiropoulos

Keyword(s):

Crystal Structure ◽

Hydrogen Bonding ◽

Nmr Spectroscopy ◽

Good Yield ◽

Spectroscopic Data ◽

Spectroscopic Characterization ◽

X Ray ◽

X Ray Crystallography ◽

H Nmr

The reaction of Ga2(SO4)3·18H2O and excess 2,2′:6′,2″-terpyridine (terpy) in MeOH / H2O leads to [Ga(OH)(SO4)(terpy)(H2O)]·H2O (1·H2O] in good yield. The structure of the complex has been determined by single-crystal X-ray crystallography. The GaIII atom in 1·H2O is 6-coordinate and ligation is provided by one terdentate terpy molecule, one monodentate sulfate, one terminal hydroxide and one terminal H2O molecule; the coodination polyhedron about the metal is described as a distorted octahedron. There is an extensive hydrogen-bonding network in the crystal structure which generates corrugated layers parallel to bc. The new complex was characterized by IR and 1H NMR spectroscopy. The spectroscopic data are discussed in terms of the nature of bonding

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4-Bromophenylboronate Derivatives of Ring and Cage Borosilicates

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc20021051 ◽

2002 ◽

Vol 67 (7) ◽

pp. 1051-1060 ◽

Cited By ~ 17

Author(s):

Anthony G. Avent ◽

Simon E. Lawrence ◽

Margaret M. Meehan ◽

Tom G. Russell ◽

Trevor R. Spalding

Keyword(s):

Single Crystal ◽

Single Crystal Diffraction ◽

X Ray ◽

X Ray Crystallography ◽

Work Up ◽

Derivatives Of

The reactions between equimolecular amounts of 4-bromophenylboronic acid and di-tert-butylsilanediol or tert-butylsilanetriol in toluene solutions at reflux temperatures afforded the borosilicate ring compound [(4-BrC6H4B)O2Si(t-Bu)2]2 (1), and the cube-based species [(t-BuSi)4(4-BrC6H4B)4O10] (2), in medium (62%) and low (13%) yields, respectively. These compounds were characterised by microanalysis, IR and NMR (1H, 11B, 13C and 29Si) spectroscopy and single crystal X-ray crystallography. During the work-up of 2, a sample of the boroxine, [(4-BrC6H4BO)3] (3), was isolated and was characterised by single crystal diffraction.

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