Synthesis, characterization, and thermal properties of benzylammonium pentaborate [C6H5CH2NH3][B5O6(OH)4]

2010 ◽  
Vol 75 (9) ◽  
pp. 971-980 ◽  
Author(s):  
Michael A. Beckett ◽  
Peter N. Horton ◽  
Michael B. Hursthouse ◽  
James L. Timmis ◽  
K. Sukumar Varma
Keyword(s):  
Thermal Properties ◽  
Solid State ◽  
Low Temperature ◽  
Boric Acid ◽  
Single Crystal ◽  
High Yield ◽  
Dsc Analysis ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray

[C6H5CH2NH3][B5O6(OH)4] was obtained as colourless crystals in high yield from a MeOH/ H2O (1:1) solution of benzylamine and boric acid (1:5). A single-crystal X-ray study confirmed that the solid-state structure was comprised of a supramolecular H-bonded pentaborate anion lattice, templated by the benzylammonium cations which occupy positions within the lattice cavities. Each pentaborate anion formed 4 H-bonds to 4 neighbouring pentaborate anions at α,α,α,β acceptor sites. Additionally, each cation H-bonds to 3 pentaborate anions. Crystals were monoclinic, P21/c, with a = 9.3511(2) Å, b = 14.5157(4) Å, c = 10.4670(2) Å, β = 90.778(2)°, T = 120 K, V = 1420.64(6) Å3, and Z = 4. TGA/DSC analysis showed that [C6H5CH2NH3][B5O6(OH)4] thermally decomposed in air at 800 °C to 2.5B2O3, via a low-temperature (200–250 °C) dehydration step to a condensed pentaborate.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

Structural Study of an Acyclic Diterpene From Eremophila Species

1996 ◽  
Vol 49 (6) ◽  
pp. 701 ◽  
Author(s):  
YM Syah ◽  
EL Ghisalberti ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Structural Study ◽  
Room Temperature ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of the semicarbazone derivative (3) of the aldehyde diacid (1), an acyclic diterpene isolated from Eremophila species, has been determined by a single-crystal room-temperature X-ray study. Crystals of (3) are triclinic, Pī , a 14.642(7), b 14.371(6), c 12.823(6) Ǻ, α 76.59(4), β 66.09(4), γ 72.97(4)°, Z = 4; R was 0.052 for 2265 independent 'observed' (I > 3σ(I)) diffractometer reflections.

N–O Bond Cleavage During the Deprotonation of N,O-Bis(trimethylsilyl)hydroxylamine

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Bond Cleavage ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Potassium Hydride ◽  
Oxygen Atoms

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

Synthesis of Triferrocenylbenzenes by Tantalum(V)-Catalyzed Cyclotrimerization of Ethynylferrocene. The Crystal Structure of 1,3,5-Triferrocenylbenzene

1997 ◽  
Vol 62 (10) ◽  
pp. 1577-1584 ◽  
Author(s):  
Petr Štěpnička ◽  
Ivana Císařová ◽  
Jan Sedláček ◽  
Jiří Vohlídal ◽  
Miroslav Polášek
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
High Yield ◽  
Isomer Mixture ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Yield Formation

Exclusive, high-yield formation of the cyclotrimers of ethynylferrocene (1) was observed when TaCl5 in benzene was employed as catalyst. Analysis of the resulting isomer mixture by means of HPLC and 1H NMR revealed the presence of 1,3,5-triferrocenylbenzene (sym-2) and 1,2,4-triferrocenylbenzene (asym-2) in the ratio of 4 : 6. A small amount of pure sym-2 isomer was isolated, and its solid-state structure was established by single-crystal X-ray diffraction. The molecules of sym-2 possess a distorted up-up-down arrangement of the ferrocenyl groups attached to the benzene ring.

Synthesis of Diferrocenylethyne by Molybdenum-Catalyzed Metathesis of 1-Ferrocenylprop-1-yne

2003 ◽  
Vol 68 (10) ◽  
pp. 1897-1903 ◽  
Author(s):  
Martin Kotora ◽  
David Nečas ◽  
Petr Štěpnička
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
State Structure ◽  
X Ray Diffraction ◽  
Catalytic Systems ◽  
Solid State Structure ◽  
X Ray

Diferrocenylethyne (1) was synthesized by metathesis of 1-ferrocenylprop-1-yne using various catalytic systems based on [Mo(CO)6] (5 mole %) and a chlorophenol (30 mole %) in toluene. The yields varied for different chlorophenols; the best conversions were obtained with 2,5-dichlorophenol (66%) and 4-chlorophenol (55%). Alkyne 1 was further reduced to the known (E)-1,2-diferrocenylethene and 1,2-diferrocenylethane, and its solid-state structure determined by single-crystal X-ray diffraction.

Structural Study of Dehydrocurvularin, an Inhibitor of Microtubule Assembly

1994 ◽  
Vol 47 (6) ◽  
pp. 1193 ◽  
Author(s):  
F Almassi ◽  
EL Ghisalberti ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Structural Study ◽  
Room Temperature ◽  
Microtubule Assembly ◽  
State Structure ◽  
Fungal Metabolite ◽  
Solid State Structure ◽  
X Ray ◽  
Opposite Helicity

The solid-state structure of the fungal metabolite E-dehydrocurvularin (2), an inhibitor of microtubule assembly, has been determined by a single-crystal room-temperature X-ray study for comparison with curvularin (1). Crystals of (2) are orthorhombic, P212121, a 17.757(9), b 10.031(6), c 8.069(4) Ǻ, Z = 4; R was 0.060 for 988 independent 'observed' [I > 3σ(I)] diffractometer reflections. The results of this study show that (1) and (2) adopt opposite helicity in the solid state.

scholarly journals Investigating Differences and Similarities between Betaxolol Polymorphs

Crystals ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 509 ◽  
Author(s):  
Patrizia Rossi ◽  
Paola Paoli ◽  
Stella Milazzo ◽  
Laura Chelazzi ◽  
Andrea Ienco ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Blocking Agent ◽  
Rotational Isomer ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Β Blocker ◽  
Adrenergic Blocking

Betaxolol belongs to the class of β1-adrenergic blocking agent. Several polymorphs of racemic betaxolol have been reported in the literature, but only one of them (BE_I) had the crystal structure determined from single-crystal X-ray diffraction. Here, we present a new crystalline phase of betaxolol (BE_IV). Its solid-state structure has been obtained from single-crystal X-ray diffraction data. The molecular and crystal arrangements of betaxolol in BE_IV have been further investigated by molecular modelling, by Cambridge Structural Database (CSD) surveys and by Hirshfeld surface analysis. A comparison with the solid-state structure of BE_I have been carried out. In the two polymorphs the 2-hydroxy-3-(isopropylamino)-propoxy chain, which is common to other β-blocker drugs, adopts a different conformation. In addition, the rotational isomer found in BE_IV is different with respect to the four already observed in the solid-state structure of analogous compounds. In both the polymorphs, the most significant interaction is due to the H-bonds involving the OH group as donor and the NH as acceptor, while the interaction where OH works as acceptor (NH acts as donor) is definitely less important. The resulting H-bond patterns are however different: Alternate R2,2(10) a > a (OH donors) and R2,2(10) b > b (OH acceptors) in BE_I vs. alternate R4,4 (8) a > b > a > b (OH donors) and R2,2 (10) b > b (OH acceptor) in BE_IV.

Structural Study of Torquatone, an Acylphloroglucinol Derivative From Eucalyptus Species

1995 ◽  
Vol 48 (10) ◽  
pp. 1771 ◽  
Author(s):  
EL Ghisalberti ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Solid State ◽  
Essential Oils ◽  
Single Crystal ◽  
Structural Study ◽  
Room Temperature ◽  
Eucalyptus Species ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of torquatone (1), an acylphloroglucinol derivative from the essential oils of a number of Eucalyptus species, has been determined by a single-crystal room-temperature X-ray study. Crystals of (1) are monoclinic, P21/c, a 10.470(8), b 20.53(1), c 7.696(6) Ǻ, β 95.91(7)۰, Z = 4; R was 0.054 for 1877 independent 'observed' [I > 3σ(I)] diffractometer reflections.

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