scholarly journals Novel Enantiomerically Pure Ferrocenes

1996 ◽  
Vol 51 (3) ◽  
pp. 437-440 ◽  
Author(s):  
Adolphus A . H. van der Zeijden ◽  
J. Sieler ◽  
E. Hovestreydt
Keyword(s):  
Solid State ◽  
Ammonium Salt ◽  
State Structure ◽  
X Ray Diffraction ◽  
Dimethylamino Group ◽  
Enantiomerically Pure ◽  
Solid State Structure ◽  
X Ray ◽  
Cyclopentadienyl Ligand

Abstract A chiral ferrocene (CpE2Fe) was synthesized by reaction of CpELi with FeCl2(THF)1.5 The cyclopentadienyl ligand CpE contains a dimethylamino group that is separated from the Cp backbone by two stereogenic carbon centres. Reaction of CpE2Fe with excess Mel affords the ammonium salt CpE2Fe.2MeI. Its solid state structure was determined by X-ray diffraction methods.

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.

The two solid-state conformations of nefopam methiodide, a quaternary ammonium salt of the analgesic drug

1990 ◽  
Vol 68 (7) ◽  
pp. 1128-1134 ◽  
Author(s):  
Robert Glaser ◽  
André Michel ◽  
Marc Drouin
Keyword(s):  
Solid State ◽  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
State Structure ◽  
X Ray Diffraction ◽  
Analgesic Drug ◽  
X Ray ◽  
Positional Disorder ◽  
X Ray Crystallography

The solid-state structure of nefopam methiodide, a quaternary ammonium salt of nefopam hydrochloride (a non-narcotic analgesic drug), has been determined by single crystal X-ray diffraction analysis. Nefopam methiodide gives crystals belonging to the monoclinic P21/c space group and, at 298 K, a = 10.001(1), b = 9.928(1), c = 17.598(1) Å, β = 94.41(1)°, V = 1742.2(2) Å3, Z = 4, R(F) = 0.086, and Rw(F) = 0.108. Due to disorder, the boat (flattened chair) and twist-chair (flattened chair) conformations of the 2,5-benzoxazocine eight-membered ring were both observed in the crystal with 55:45 occupancy, respectively. Positional disorder was also observed for the iodide counterion, which showed occupancies of 81:9.5:9.5. Keywords: nefopam, analgesic, X-ray crystallography, conformation.

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.

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.

scholarly journals Synthesis and structure of the donor-free potassium silanide K[SiPh3]

2019 ◽  
Vol 74 (2) ◽  
pp. 153-158 ◽  
Author(s):  
Edith Alig ◽  
Isabelle Georg ◽  
Inge Sänger ◽  
Lothar Fink ◽  
Matthias Wagner ◽  
...  
Keyword(s):  
Solid State ◽  
Room Temperature ◽  
State Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray ◽  
Phenyl Rings ◽  
Short Contacts

AbstractThe donor-free potassium silanide K[SiPh3] was prepared by the reaction of hexaphenyldisilane, Ph3Si–SiPh3, with potassium metal in benzene at room temperature. The solid-state structure, determined by powder X-ray diffraction consists of {K[SiPh3]}2 units, which interact with adjacent dimers to form an infinite chain along the crystallographic c axis (orthorhombic, space group Cmc21, Z=4). The structure features short contacts between the π system of the phenyl rings and the potassium atoms of neighbouring K[SiPh3] units.

Synthesis and Crystal Structures of Dimethylsilylene-Bridged (Amidocyclopentadienyl)dichlorotitanium(IV) Complexes with Various Substituents on the Cyclopentadienyl Ligand

2001 ◽  
Vol 66 (4) ◽  
pp. 605-620 ◽  
Author(s):  
Jaroslav Zemánek ◽  
Petr Štěpnička ◽  
Karla Fejfarová ◽  
Róbert Gyepes ◽  
Ivana Císařová ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Single Crystal ◽  
Spectral Methods ◽  
Nmr Spectra ◽  
Bulky Substituent ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cyclopentadienyl Ligand

(Amidocyclopentadienyl)dichlorotitanium(IV) complexes of the general formula [TiCl2{η5:η1(N)-C5(1-SiMe2Nt-Bu-2,3,4-Me3-5-R)}], where R = H (6b), Ph (6c), 4-fluorophenyl (6d) and 1-methylallyl (6e) were synthesized and characterized by spectral methods. Solid-state structure of [TiCl2{η5:η1(N)-C5Me4(SiMe2Nt-Bu)}] (6a) and 6d determined by single-crystal X-ray diffraction showed that variation of the ring substituent R has only a negligible effect on the molecular structure of the complexes. The NMR spectra indicate that motion of the bulky substituent R in compounds 6c, 6d and 6e is hindered below ca 50 °C.

Phosphine chalcogenide complexes of antimony(III) halides

2015 ◽  
Vol 93 (3) ◽  
pp. 375-379 ◽  
Author(s):  
Karlee L. Bamford ◽  
Alasdair P.M. Robertson ◽  
Hilary A. Jenkins ◽  
Brian O. Patrick ◽  
Neil Burford
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Phosphine Oxide ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Derivatives Of

Three series of phosphine chalcogenide complexes of the antimony(III) halides SbX3 (X = F, Cl, Br, or I) have been synthesized and characterized by spectroscopic and crystallographic methods. Complexes of the generic formulae (Cy3PO)SbX3 (X = F (1a), Cl (1b), or Br (1c)), (Cy3PO)2SbX3 (X = F (2a), Cl (2b), or Br (2c)), and (Cy3PS)SbX3 (X = Cl (3b), Br (3c), or I (3d)) were synthesized via the treatment of solutions of SbX3 with OPCy3 and SPCy3, respectively. Derivatives of (Cy3PO)SbX3 were characterized by single crystal X-ray diffraction for 1a and 1b and crystallize as dimers through symmetry related intermolecular Sb–X interactions, providing the first structurally characterized examples of this class of complex. Derivatives of (Cy3PS)SbX3 (3b–3c) adopt analogous dimeric structures in the solid state. The solid-state structure of (Cy3PO)2SbCl3 (2b) is consistent with the previously reported structures of bis-phosphine oxide complexes of antimony(III), with a square pyramidal Sb center and cis-configured OPCy3 ligands. The phosphine chalcogenide complexes of SbX3 display configurations that are consistent with the perceived trans-labilizing properties of the ligands/substituents.

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