Synthesis and Catalytic Properties of Novel Ruthenacarboranes Based on nido-[5-Me-7,8-C2B9H10]2− and nido-[5,6-Me2-7,8-C2B9H9]2− Dicarbollide Ligands

The effect of methyl substituents in the lower belt of dicarbollide ligands on the redox potential of ruthenacarboranes based thereof, as well as the ability of the metallacarboranes obtained to catalyze radical polymerization with atom transfer were studied. For this purpose, a new approach to the synthesis of closo-ruthenacarboranes based on substituted dicarbollide ligands was developed and six new complexes 3,3-(Ph2P(CH2)4PPh2)-3-H-3-Cl-9-Me-12-X-closo-3,1,2-RuC2B9H9, 3,3,8-(Ph2P(CH2)4PPh-m-(C6H4-о))-3-Cl-9-Me-12-X-closo-3,1,2-RuC2B9H8 and 3,3,4,8-(Ph2P(CH2)4P-m-(C6H4-о)2)-3-Cl-9-Me-9-X-closo-3,1,2-RuC2B9H7 (X = H, Me) were synthetized and characterized by single crystal X-ray diffraction, NMR and ESR spectroscopy and MALDI TOF mass-spectrometry. Comparison of the values of the redox potentials of the synthesized ruthenium complexes in 1,2-dichloroethane with the values previously found for the corresponding ruthenacarboranes based on the parent dicarbollide anion showed that the introduction of methyl substituents into the carborane cage led to a decrease in the redox potentials of the complexes, which made them more preferable catalysts for ATRP. Test experiments on the polymerization of MMA showed that the synthesized ruthenacarboranes were effective catalysts for ATRP, the most active being the complex with two methyl groups and two ortho-phenylenecycloboronated fragments.

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Syntheses, structures, and catalytic properties of two arene-ruthenium(II) complexes bearing N-(2-pyridinyl)aminodiphenylphosphine sulfide ligands

Zeitschrift für Naturforschung B ◽

10.1515/znb-2017-0161 ◽

2018 ◽

Vol 73 (3-4) ◽

pp. 161-166

Author(s):

Fule Wu ◽

Jiling Gu ◽

Xin Chen ◽

Ai-Quan Jia ◽

Qian-Feng Zhang

Keyword(s):

Mass Spectrometry ◽

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Single Crystal ◽

Crystal Structures ◽

Catalytic Properties ◽

Transfer Hydrogenation ◽

X Ray Diffraction ◽

X Ray ◽

Sulfide Ligands

AbstractTreatment of [(arene)Ru(μ-Cl)Cl]2with Ph2P(S)NH(2-py) in the presence or absence of base gave two arene-ruthenium(II) complexes [(η6-p-cymene)Ru{κ2-N,N-Ph2P(S)N(2-py)}Cl] (1) and [(η6-benzene)Ru{κ1-N-Ph2P(S)NH(2-py)}Cl2] (2), which have been characterized by infrared, nuclear magnetic resonance spectroscopies, and mass spectrometry along with microanalyses. Crystal structures of Ph2P(S)NH(2-py) · ¼C6H14,1and2· ½CH2Cl2were determined by single-crystal X-ray diffraction. Two arene-ruthenium(II) complexes were tested as precatalysts for the transfer hydrogenation of acetophenone to give 1-phenyl ethanol.

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A Covalent Organic Cage Compound Acting as a Supramolecular Shadow Mask for the Regioselective Functionalization of C60

10.26434/chemrxiv.12424664 ◽

2020 ◽

Author(s):

Viktoria Leonhardt ◽

Stefanie Fimmel ◽

Ana-Maria Krause ◽

Florian Beuerle

Keyword(s):

Mass Spectrometry ◽

Single Crystal ◽

High Selectivity ◽

Shadow Mask ◽

X Ray Diffraction ◽

X Ray ◽

Trigonal Bipyramidal ◽

Cage Compound ◽

Vis Spectroscopy ◽

Regioselective Functionalization

<div><div><div><p>A trigonal-bipyramidal covalent organic cage compound serves as an efficient host to form stable 1:1-complexes with C60 and C70. Fullerene encapsulation has been comprehensively studied by NMR and UV/Vis spectroscopy, mass spectrometry as well as single-crystal X-ray diffraction. Exohedral functionalization of encapsulated C60 via threefold Prato reaction revealed high selectivity for the symmetry-matched all-trans-3 addition pattern.</p></div></div></div>

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The Molecular Geometry of Diastereoisomeric Bis[α-(9-anthryl)ethyl] Ethers

Australian Journal of Chemistry ◽

10.1071/ch9851417 ◽

1985 ◽

Vol 38 (9) ◽

pp. 1417 ◽

Cited By ~ 3

Author(s):

H Becker ◽

VA Patrick ◽

BW Skelton ◽

AH White

Keyword(s):

Single Crystal ◽

Least Squares ◽

Dihedral Angle ◽

Molecular Geometry ◽

Dihedral Angles ◽

Methyl Groups ◽

X Ray Diffraction ◽

X Ray ◽

Meso Form ◽

Aromatic Systems

The crystal structures of racemic bis [α-(9-anthryl)] ether and its meso form have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to residuals of 0.053 and 0.041 for 1868 and 3568 independent 'observed' reflections respectively. Crystals of the racemate are orthorhombic, Pcab, a 23.07(1), b 19.85(2), c 10.241(8) Ǻ, Z 8. Crystals of the meso form are triclinic, Pī , a 19.032(12), b 14.207(11), c 9.451(8) Ǻ, α 79.46(6), β 89.68(6), γ 68.97(5)°, Z 4. In the racemate , the dihedral angle between the methyl groups along the ether bonds is 12°, and the short axes of the anthracene moieties lie at an angle of about 120°. In the meso compound, for the two molecules the dihedral angles between the methyl groups along the ether bonds are 90 and 93°, the angle between the two anthracene moieties is 90°, and the interplanar angles between the partly overlapping aromatic systems are 46 and 43°.

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[Ni(OH)3W6O18(OCH2)3CCH2OH]4−: the first tris-functionalized Anderson-type heteropolytungstate

Chemical Communications ◽

10.1039/c6cc04326g ◽

2016 ◽

Vol 52 (59) ◽

pp. 9263-9266 ◽

Cited By ~ 21

Author(s):

Nadiia I. Gumerova ◽

Alexander Roller ◽

Annette Rompel

Keyword(s):

Mass Spectrometry ◽

Ir Spectroscopy ◽

Single Crystal ◽

Electrospray Ionization ◽

Electrospray Ionization Mass Spectrometry ◽

Ionization Mass Spectrometry ◽

Ionization Mass ◽

X Ray Diffraction ◽

X Ray

Na2[TMA]2[Ni(OH)3W6O18(OCH2)3CCH2OH]·9H2O represents the first covalent tris-functionalized Anderson-type heteropolytungstate and was characterized by single-crystal X-ray diffraction, electrospray ionization mass spectrometry, TGA and IR spectroscopy.

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1,3,5-Tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane

Zeitschrift für Naturforschung B ◽

10.1515/znb-2015-0148 ◽

2016 ◽

Vol 71 (1) ◽

pp. 81-84 ◽

Cited By ~ 4

Author(s):

Eugen Weisheim ◽

Hans-Georg Stammler ◽

Norbert W. Mitzel

Keyword(s):

Mass Spectrometry ◽

Ir Spectroscopy ◽

Single Crystal ◽

Elemental Analysis ◽

X Ray Diffraction ◽

X Ray ◽

Ft Ir ◽

Ft Ir Spectroscopy

AbstractThe reaction of 1,3,5-triethynyl-1,3,5-trimethyl- 1,3,5-trisilacyclohexane with (dimethylamino)trimethylstannane afforded 1,3,5-tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane with tin-functionalised ethynyl groups. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, mass spectrometry, NMR and FT-IR spectroscopy.

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ISOLATION AND STRUCTURAL ELUCIDATION OF A NEW DEPSIDE OF LICHEN Everniopsis trulla

Revista de la Sociedad Química del Perú ◽

10.37761/rsqp.v87i2.340 ◽

2021 ◽

Vol 87 (2) ◽

pp. 97-106

Author(s):

Olivio Nino Castro ◽

Jesús López Rodilla ◽

Sofia Pombal ◽

Francisca Sanz González ◽

Julio Santiago Contreras

Keyword(s):

Mass Spectrometry ◽

Melting Point ◽

Hydrogen Bonds ◽

Single Crystal ◽

Spectroscopic Data ◽

Intermolecular Forces ◽

X Ray Diffraction ◽

Intermolecular Hydrogen Bonds ◽

X Ray ◽

Uv Visible

In this research, a new depside of the lichen Everniopsis trulla has been isolated. The extraction was carried out to 400 g of dry sample and ground with ethanol for 3 repetitions, then, it was fractionated by applying column chromatography with the CHCl3-MeOH system and purified by recrystallization with MeOH-Acetone (1: 1); Finally, white crystals in the form of needles (solid C) with a melting point of 198 ° C were obtained, whose structure was elucidated based on spectroscopic data (UV-Visible, IR, NMR-H1, NMR-C13, mass spectrometry and single crystal X-ray diffraction). According to the Science Finder databases, it is a new depside, called trullarin, and it is observed that molecular packing is influenced by both intramolecular and intermolecular forces. Intermolecular hydrogen bonds of O - H -O type binds neighboring molecules forming dimers.

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Die Kristallstruktur von Tricarbonyl(2.6-di-tert-butyl-pyridin)chrom(0) bei 200 K / Crystal Structure of Tricarbonyl(2,6-di/tert-butyl-pyridine)chromium(0) at 200 K

Zeitschrift für Naturforschung B ◽

10.1515/znb-1984-0216 ◽

1984 ◽

Vol 39 (2) ◽

pp. 213-216 ◽

Cited By ~ 7

Author(s):

Roland E. Schmidt ◽

Werner Massa

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Diffraction Data ◽

Pyridine Ring ◽

Chromium Atom ◽

Methyl Groups ◽

X Ray Diffraction ◽

X Ray ◽

Lattice Constants ◽

Tert Butyl

Based on single crystal X-ray diffraction data the crystal structure of tricarbonyl(2,6-dwmbutyl- pyridine)chromium(0) has been determined at 200 K: space group P 21/n, Z = 4, lattice constants a = 680.6(5), b - 1383.3(10), c = 1763.0(16) pm, β = 96.53(8)°, refinement to Rw - 0.048 for 1672 independent reflections with FO > 2 σ. The chromium atom is η6π6- bonded to the essentially planar pyridine ring (Cr-C: 219-222 pm, Cr-N: 221 pm). The CO ligands show “eclipsed” orientation with respect to the 2, 4 and 6 position of the pyridine ring. Two CO groups fit into the gaps formed by two methyl groups of the tert-butyl substituents in 2 and 6 position, respectively. The results are discussed in context with related arene and λ3-phosphorine complexes

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Crystal structures of titanium–aluminium and –gallium complexes bearing twoμ2-CH3units

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989017004856 ◽

2017 ◽

Vol 73 (5) ◽

pp. 691-693 ◽

Cited By ~ 9

Author(s):

Tim Oswald ◽

Mira Diekmann ◽

Annika Frey ◽

Marc Schmidtmann ◽

Rüdiger Beckhaus

Keyword(s):

Single Crystal ◽

Crystal Structures ◽

Lewis Acids ◽

Methyl Groups ◽

X Ray Diffraction ◽

X Ray ◽

Methyl Methyl ◽

Low Valent ◽

Titanium Aluminium ◽

Gallium Complexes

The isotypic crystal structures of two titanocene complexes containing anEMe3unit (E =Al, Ga; Me = methyl) with twoμ2-coordinating methyl groups, namely [μ-1(η5)-(adamantan-1-yl-2κC1)cycylopentadienyl]di-μ2-methyl-methyl-2κC-[1(η5)-pentamethylcyclopentadienyl]aluminiumtitanium(III), [AlTi(CH3)3(C10H15)(C15H18)], and [μ-1(η5)-(adamantan-1-yl-2κC1)cycylopentadienyl]di-μ2-methyl-methyl-2κC-[1(η5)-pentamethylcyclopentadienyl]galliumtitanium(III), [GaTi(CH3)3(C10H15)(C15H18)], are reported. Reacting a dinuclear nitrogen-bridged low-valent titanium(III) complex with the Lewis acids AlMe3or GaMe3results in the loss of molecular dinitrogen and the formation of two monomeric titanocene(III) fragments bearing twoμ2-bridging methyl groups. Single crystal X-ray diffraction reveals the formation of a newE—C bond involving the pentafulvene ligand while the bridging and terminal methyl groups remain intact.

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Study on the Acid-Induced Ring-Expansion of an Oxaphosphirane Complex with an Electron-Withdrawing C-Substituent

Australian Journal of Chemistry ◽

10.1071/ch16609 ◽

2017 ◽

Vol 70 (4) ◽

pp. 442 ◽

Cited By ~ 1

Author(s):

Cristina Murcia García ◽

Gregor Schnakenburg ◽

Rainer Streubel

Keyword(s):

Mass Spectrometry ◽

Single Crystal ◽

Elemental Analysis ◽

Ring Expansion ◽

X Ray Diffraction ◽

X Ray ◽

Multinuclear Nmr ◽

Fluorinated Ligands ◽

Ring Expansion Reaction

A study on the acid-induced ring-expansion reaction of the first oxaphosphirane complexes bearing an electron-withdrawing C-substituent is described. The stereoselectively obtained 1,3,4-dioxaphospholane complexes 4a–c, representing the first examples of such fluorinated ligands, were unambiguously characterized by multinuclear NMR, elemental analysis, mass spectrometry, and single-crystal X-ray diffraction studies.

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Trinodal Self-Penetrating Nets from Reactions of 1,4-Bis(alkoxy)-2,5-bis(3,2’:6’,3’’-terpyridin-4’-yl)benzene Ligands with Cobalt(II) Thiocyanate

Crystals ◽

10.3390/cryst9100529 ◽

2019 ◽

Vol 9 (10) ◽

pp. 529 ◽

Cited By ~ 1

Author(s):

Giacomo Manfroni ◽

Alessandro Prescimone ◽

Stuart R. Batten ◽

Y. Maximilian Klein ◽

Dariusz J. Gawryluk ◽

...

Keyword(s):

Mass Spectrometry ◽

Crystal Growth ◽

Single Crystal ◽

Crystal Lattice ◽

1H Nmr ◽

Room Temperature ◽

X Ray Diffraction ◽

X Ray

The tetratopic ligands 1,4-bis(2-ethylbutoxy)-2,5-bis(3,2’:6’,3’’-terpyridin-4’-yl)benzene (1) and 1,4-bis(3-methylbutoxy)-2,5-bis(3,2’:6’,3’’-terpyridin-4’-yl)benzene (2) have been prepared and characterized by 1H and 13C{1H} NMR, IR, and absorption spectroscopies and mass spectrometry. Reactions of 1 and 2 with cobalt(II) thiocyanate under conditions of crystal growth at room temperature result in the formation of [{Co(1)(NCS)2}·MeOH·3CHCl3]n and [{Co(2)(NCS)2}·0.8MeOH·1.8CHCl3]n. Single-crystal X-ray diffraction reveals that each crystal lattice consists of a trinodal self-penetrating (62.84)(64.82)(65.8)2 net. The nodes are defined by two independent cobalt centres and the centroids of two crystallographically independent ligands which are topologically equivalent.

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