Oxofluoro-oxalato-vanadate des vierwertigen Vanadins: Schwingungsspektrum und Struktur von Na3[VOF(C2O4)2] • 6 H2O.

1976 ◽  
Vol 31 (5) ◽  
pp. 537-540 ◽  
Author(s):  
Helmut Rieskamp ◽  
Rainer Mattes
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Fluorine Atom ◽  
Direct Methods ◽  
Terminal Oxygen Atom ◽  
Triclinic Space Group ◽  
Trans Effect ◽  
Space Group ◽  
X Ray ◽  
In Cis

The Na and NH4 salts of the [VOF(C2O4)2]3--ion have been prepared. The crystal structure of the former has been determined from X-ray diffractometer data. The crystals are triclinic, space group P with Z = 2. The structure was solved by `direct methods' and refined to R 0.050 for 1749 reflections. In the anion, vanadium(IV) is octahedrally coordinated by a terminal oxygen atom, a fluorine atom in cis-position to the former, and two bidentate oxalate ligands. The terminal V—O-bond exhibits a strong ‘trans’ effect.

Fluorreiche Oxofluorovanadate(V): Die Kristallstruktur von [enH2][VOF5]. / Fluorine-Rich Oxofluorovanadates(V): Crystal Structure of [enH2][VOF5]

1976 ◽  
Vol 31 (11) ◽  
pp. 1453-1455 ◽  
Author(s):  
Helmut Rieskamp ◽  
Rainer Mattes
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Bonds ◽  
Oxygen Atom ◽  
Fluorine Atom ◽  
Terminal Oxygen Atom ◽  
X Ray

The crystal structure of triclinic [enH2][VOF5], prepared in aqueous solution, has been determined from X-ray diffractometer data (R = 0.076 for 527 reflections). The structure contains monomeric [VOF5]2--ions. The bond distances are 1.54(1) Å (terminal oxygen), 1.80(1) (average for the cis-fluorine atoms) and 2.10(1) Å for the fluorine atom in transposition to the terminal oxygen atom. This fluorine atom is involved in strong hydrogen bonds originating from the [NH3CH2CH2NH3]2+ cation with cisoid conformation. Earlier results about the existence of K2VOF5 could not be confirmed

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

Structure of 3α,4α:5β,6β-Diepoxyandrostan-17-one

1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.

Bildung von Arsensäure aus [As2Cl8]2Ionen und Ozon. Die Kristallstruktur von PPh4Cl · H3AsO4 / Formation of Arsenic Acid from [As2Cl8]2- Ions and Ozone. Crystal Structure of PPh4Cl · H3AsO4

1992 ◽  
Vol 47 (12) ◽  
pp. 1677-1680 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Alfred-Dirk Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Low Temperatures ◽  
X Ray Diffraction ◽  
Arsenic Acid ◽  
Subsequent Reaction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Reaction of ozone with (PPh4)2[As2Cl8] in CH2C12 at low temperatures yields a red compound, possibly an ozonide. Upon evaporation of the solvent at –78 °C the ozone is released again. At -40 °C or above a subsequent reaction yields PPh4[AsCl6], PPh4Cl · H3AsO4, and other products. The crystal structure of PPh4Cl · H3AsO3 was determined by X-ray diffraction (4253 observed reflexions, R = 0.031). It is triclinic, space group P1̅, and consists of H3AsO4 molecules joined to dimer units via H bridges and associated via O–H · · · Cl- bridges to strands. The packing of the PPh4+ ions is discussed. Products of the reaction of (PPh4)2[Sb2Cl8] with ozone in CH2C12 are PPh4[SbCl6] and (PPh4)2[SbOCl4]2 · 2 CH2Cl2.

Synthese und Kristallstruktur von l,13-Bis(8-chinolyl)- 1,4,7,10,13-pentaoxatridecan-diquecksilber(I)-diperchlorat

1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Torsional Angles ◽  
L 13 ◽  
Oxygen Atoms

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.

Synthesis and X -Ray Crystal Structure of the Heterobimetallic Complex [FeRh (μ-CO)(CO)3((μ-PBut2)((μ-Ph2PCH2PPh2)]

1997 ◽  
Vol 52 (7) ◽  
pp. 810-814 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Kurt Merzweiler ◽  
Clemens Bruhn
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Room Temperature ◽  
Metal Carbonyl ◽  
Homogeneous Catalyst ◽  
Catalyst Precursor ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Heterobimetallic Complex

Abstract The reaction of the phosphido-bridged metal carbonyl [FeRh(CO)6(μ-PBut2)] (1) with dppm [dppm = bis(diphenylphosphino)methane] leads to the heterobimetallic complex [FeRh(μ-CO)(CO)3(μ-PBut2)(μ-dppm)] (2) in good yields. The molecular structure of 2 was determined at room temperature [triclinic, space group P1̄, a = 9.509(6), b = 13.637(5), c = 14.926(8) Å, α = 81.38(4), β = 82.75(4), γ = 71.25(4)°]. The compound acts as a homogeneous catalyst precursor in the hydroformylation reaction of ethylene, but it decomposes during this process.

An X-ray structural examination of an intermediate from the cleavage of a vic-diol by iodine(I) acetate

1980 ◽  
Vol 33 (3) ◽  
pp. 671 ◽  
Author(s):  
PG Beckingsale ◽  
JM Waters ◽  
TN Waters
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Structural Examination ◽  
Space Group ◽  
X Ray

The crystal structure of a compound isolated after reaction of iodine(1) acetate with cis-cyclohexane-1,2-diol has been determined by direct methods. It is identified as 2,2'-(butane-1,4-diyl)bis(hexahydro-1,3-benzodioxole). Crystals are orthorhombic, a 8.625(2), b 7.589(1), c 26.187(5) Ǻ, space group Pbca, Z 4. Least- squares refinement brought R to 0.046.

Crystal Structure and Spectroscopic Behaviour of a Binuclear Copper(II) Complex of Mefenamic Acid and Dimethylsulfoxide

1998 ◽  
Vol 53 (8) ◽  
pp. 871-874 ◽  
Author(s):  
G. Facchin ◽  
M. H. Torre ◽  
E. Kremer ◽  
O. E. Piro ◽  
E. J. Baran
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Mefenamic Acid ◽  
Electronic Spectra ◽  
Anthranilic Acid ◽  
Binuclear Copper ◽  
Triclinic Space Group ◽  
Spectroscopic Behaviour ◽  
Space Group ◽  
X Ray

Abstract The crystal structure of the binuclear Cu(II) complex [Cu(mef)2DMSO]2 (mef = deprotonated N-2,3-dimethylphenyl-anthranilic acid; DMSO = dimethylsulfoxide) has been determined by single-crystal X-ray diffractometry. It crystallizes in the triclinic space group P1̄ with Z = 1. IR and electronic spectra of the compound are also discussed briefly.

Organoamido- and Aryloxo-Lanthanoids. II. Preparation of Tris(2,6-diphenylphenoxo)-lanthanoid(III) Complexes and the X-Ray Structures of Low-Coordinate [Yb(O-2,6-Ph2C6H3)3] Containing an Intramolecular Chelate Yb…π-Arene Interaction, and [Yb(O-2,6-Ph2C6H3)3(thf)2].thf (thf = Tetrahydrofuran)

1990 ◽  
Vol 43 (7) ◽  
pp. 1245 ◽  
Author(s):  
GB Deacon ◽  
S Nickel ◽  
P Mackinnon ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Analogous Reaction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Oxygen Donor ◽  
Homoleptic Complexes

Bulky monomeric lanthanoid(III) aryl oxides Ln(Odpp)3(Odpp = 2,6- diphenylphenoxide; Ln = Nd, Sm, Er, Yb or Lu) have been prepared by reaction between the lanthanoid metal, Hg(C6F5)2, and HOdpp in tetrahydrofuran (thf), and Yb(Odpp)3 has also been obtained from an analogous reaction of (PhCC)2Hg. Cleavage of Ln(η5-C5H5)3 (Ln = Nd or Yb) with HOdpp also yields Ln(Opdd)3. The aryl oxides have been isolated as [Ln(Odpp)3(thf)2] (Ln = Nd, Sm or Yb) or as the homoleptic complexes Ln(Odpp)3 (Ln = Nd, Er, Yb or Lu). The X-ray crystal structure of [Yb(Odpp)3(thf)2].thf [crystals monoclinic, space group P21/n, a 11.009(4), b 32.134 (7), c 15.498(6)Ǻ, β 96.72(3)°, Z 4; 2785 data refined to R 0.039] shows the complex to have distorted square pyramidal stereochemistry with apical and transoid basal Odpp ligands, (Yb-Odpp) 2.078(9)Ǻ, and transoid basal thf ligands, {Yb-O(thf)} 2.305(8)Ǻ. Similarly, Yb(Odpp)3 [crystals triclinic, space group Pī, a 15.934(2), b 13.563(1), c 10.968(2)Ǻ, α 116.71(1), β 92.90(2), γ 103.38(1)°, Z 2; 6236 data refined to R 0.031] was shown to have a trigonal pyramidal arrangement of oxygen donor atoms [{Yb-O} 2.065(4) Ǻ;{O-Yb-O} 117.5(1)°], a novel intramolecular chelate Yb…π-arene interaction, {Yb...C} 2.978(6)Ǻ, and an agostic Yb…CH interaction.

The Crystal and Molecular Structure of Butorphanol Hydrogen Tartrate

1994 ◽  
Vol 59 (6) ◽  
pp. 1361-1367 ◽  
Author(s):  
Alexandr Jegorov ◽  
Roman Sobotík ◽  
Svetlana Pakhomova ◽  
Jan Ondráček ◽  
Jiří Novotný ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Triclinic Space Group ◽  
Space Group

The structure of butorphanol hydrogen tartrate {(9R,13S,14S)-(-)-17-(cyclobutylmethyl)morphinan-3,14-diol (2S,3S)-(-)-hydrogen tartrate} (C21H29NO2 .C4H6O6) was solved by direct methods and refined anisotropically to the R value of 0.029 for 2 069 observed reflections. The title morphine analogue crystallizes in the triclinic space group P1 with lattice parameters a = 7.620(1), b = 9.140(1), c = 9.591(1) Å, α = 105.48(1), β = 112.91(1), γ = 84.29(1)°, Z = 1. The butorphanol B ring possesses the 3E envelope conformation with small 3H2 distortion, C and D rings have a regular chair conformation. The intramolecular N17-H17...O2 hydrogen bond is observed in crystal structure of the title compound. The butorphanol and hydrogen tartrate molecules are joined together by means of O2-H(O2)...O7, O1-H(O1)...O7' and O3-H(O3)...O8" hydrogen bonds to form networks.

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