Pentamethylcyclopentadienyl-Vanadium Complexes Containing Halogeno- and Oxo-Ligands

1987 ◽  
Vol 42 (12) ◽  
pp. 1520-1526 ◽  
Author(s):  
Max Herberhold ◽  
Walter Kremnitz ◽  
Markus Kuhnlein ◽  
Manfred L. Ziegler ◽  
Karl Brunn
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
High Yield ◽  
Vanadium Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Oxygen Bond ◽  
Single Bonds ◽  
Oxo Ligands

AbstractA simple and high-yield preparation of the pentamethylcyclopentadienyl vanadium(IV) trihalides Cp*VX3 (X = CL, Br, I) from Cp*V(CO)4 as well as their conversion into the oxo-vanadium(V) compounds Cp*VOX2 (X = CL, Br) and [Cp*VOX]2(μ-O) (X = CL, Br, I) are described. The equilibrium between the two fluoride species Cp*VOF2 and [Cp*VOF]2(μ-O) has also been investigated. The complexes are characterized by their NMR (51V, l3C, 1H), IR, and mass spectra. The crystal structure of the binuclear chloro-oxo complex [Cp*VOCl]2(μ-O) has been determined by X-ray diffraction. The molecules contain two [Cp*VOCl] units combined via a bent oxo bridge (V-O-V angle of 142.2(2)°). The vanadium-oxygen bond lengths are 157.6(8) and 179.4(1) pm for the terminal and the bridging oxo ligands, respectively, corresponding to double and single bonds.

Tetrakis-pentamethylcyclopentadienyl-cyclotetrastiban (PcpSb)4 : Synthese, Molekül-und Kristallstruktur / Tetrakis-pentamethylcyclopentadienyl-cyclotetrastibane (PcpSb)4 : Synthesis, Molecular and Crystal Structure

1988 ◽  
Vol 43 (6) ◽  
pp. 744-748 ◽  
Author(s):  
Theo F. Berlitz ◽  
Heike Sinning ◽  
Jörg Lorberth ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Mass Spectra ◽  
High Yield ◽  
Crystal Data ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Tetrameric Structure ◽  
C Nmr

AbstractReaction of SbCl3 with KPcp (Pep = pentamethylcyclopentadienyl) in etheral solution at -78 °C affords dimeric pentamethylcyclopentadiene and orange-red (PcpSb)4 in high yield. 1H, 13 C NMR, IR, UV and mass spectra are reported. The tetrameric structure was found by a crystal structure determination carried out with X-ray diffraction data collected at -50 °C (928 independent observed reflexions. R = 0.055). Crystal data: tetragonal, space group I41/amd, a = 2400.0(5), c = 781.7(5) pm, Z = 4. The (PcpSb)4 molecules have a non-planar Sb4 ring with Sb -Sb bond lengths of 285.6(1) pm, one η1-Pcp ring is attached to each Sb atom. Contrary to the solid state structure, monomeric molecules are found in benzene and hexane solutions.

Pyridin-Addukte von Cyclothiazeno-Vanadiumdichlorid Die Kristallstruktur von [VCl2(N3S2)(C5H5N)] / Pyridine Adducts of Cyclo-thiazeno Vanadium Dichloride The Crystal Structure of [VCl2(N3S2)(C5H5N)]

1985 ◽  
Vol 40 (12) ◽  
pp. 1631-1637 ◽  
Author(s):  
Ruth Christophersen ◽  
Paul Klingelhöfer ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Chlorine Atom ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Independent Molecules

Abstract The pyridine complexes of cyclo-thiazeno vanadium dichloride, [VCl2(N3S2)py] and [VCl2(N3S2)(py)2] were synthesized by reactions of polymeric VCl2(N3S2) with varying amounts of pyridine in CH2Cl2. The compounds were characterized by their IR spectra as well as by their 51V NM R spectra. The crystal structure of [VCl2(N3S2)(C5H5N)] was determined by means of X-ray diffraction (1582 independent observed reflexions, R = 0.031). Crystal data: orthorhombic, space group Pnma, a = 1372, b - 2261, c - 1068 pm, Z = 12. In the lattice there are two monomeric, crystallographically independent molecules [VCl2(N3S2)(C5H5N)], which differ only slightly. The vanadium atoms have a trigonal bipyramidal coordination with the N atom of the pyridine molecule and one chlorine atom in apical positions, and with one chlorine atom and the N atoms of the cyclo-thiazeno ligand in equatorial positions. The VN bond lengths of the planar VN3S2 ring of 174 pm correspond to double bonds

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIX. Crystal Structure Determinations of Tetrakis(trimethylphosphine)copper(I) Halides and Tetrakis(triphenylphosphine)-copper(I) and -silver(I) Hexafluorophosphates

1990 ◽  
Vol 43 (10) ◽  
pp. 1697 ◽  
Author(s):  
GA Bowmaker ◽  
PC Healy ◽  
LM Engelhardt ◽  
JD Kildea ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Bond Lengths ◽  
Cu Complex ◽  
Structure Determinations

The crystal structures of [Cu(Pme3)4]X (X = Cl , Br, I) and of [M(PPh3)4] [PF6] (M = Cu, Ag) have been determined by single-crystal X-ray diffraction methods at 295 K. The former compounds contain nearly tetrahedral [Cu(PMe3)4]+ ions on sites of m symmetry with mean Cu-P bond lengths of 2.270, 2.271 and 2.278 Ǻ for X = Cl , Br and I respectively. The latter compounds contain [M(PPh3)4]+ ions on sites of 3 symmetry. In the M =Ag complex the coordination environment is close to tetrahedral, but in the M =Cu complex the length of the axial Cu-P bond [2.465(2)Ǻ] is significantly shorter than that of the off-axis bonds [2.566(2)Ǻ]. Possible reasons for this are discussed.

Brom- und Chlorthionitrenkomplexe des Rheniums. Die Kristallstruktur von (PPh4)2 [ReBr4(NS)(NSBr)]·CH2Br2 Bromo- and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh4)2[ReBr4(NS)(NSBr)]·CH2Br2

1986 ◽  
Vol 41 (7) ◽  
pp. 825-830 ◽  
Author(s):  
Hans-Günter Hauck ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Ring Cleavage ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Pyridine Complex ◽  
Subsequent Addition

AbstractThe thionitrosyl-halothionitrene com pounds (PPh4)2[ReX4(NS)(NSX)]·2 CH2X2, X = Cl or Br, are obtained by nucleophilic ring cleavage of the Re(N2S2) rings of complexes [ReX4(N2S2)]⊖ with PPh4X in CH2X2. (AsPh4)2[ReCl4(NS)(NSCl)] · CH2Cl2 can also be obtained by the reaction of [ReCl4(NSCl)(POCl3)] with S(NSiMe3)2 and subsequent addition of AsPh4Cl. The pyridine complex [ReBr2(NS)(NSBr)(NC5H5)2] · CH2Br2 forms by bromination of the corresponding chloro compound with Me3SiBr. The IR spectra are reported. The crystal structure of (PPh4)2[ReBr4(NS)(NSBr)] · CH2Br2 was determ ined by X-ray diffraction (4158 independent observed reflexions, R = 0.059). Crystal data: a = 1039.7, b - 1232.5, c - 2158.4 pm, α = 81.59, β = 87.05, γ = 77.06°, Z = 2, space group P1̄. The compound consists of PPh4⊕ ions, CH2Br2 molecules, and anions [ReBr4(NS)(NSBr)]2⊖ in which the rhenium atoms are coordinated by four bromine atoms, one thionitrosyl and one brom othionitrene group. The latter have cis arrangement and ReN bond lengths of 186 pm. W hereas the thionitrosyl group is nearly linear, the R = N = SBr group has an ReNS angle of 165°.

Article

1998 ◽  
Vol 76 (3) ◽  
pp. 301-306
Author(s):  
Sengen Sun ◽  
James F Britten ◽  
Christopher N Cow ◽  
Chérif F Matta ◽  
Paul HM Harrison
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
The Other ◽  
Methyl Groups ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Form Part ◽  
Two Sides ◽  
Opposite Helicity

The crystal structure of 3,4,7,8-tetramethylglycoluril (5) was determined by X-ray diffraction. The structure reveals a hydrogen-bonding motif in the crystal lattice that differs from that present in related glycolurils. The two sides of each molecule form part of two independent, but parallel, infinite helical chains. These chains are formed by the NH donor and C==O acceptor on one side of a glycoluril molecule, forming H-bonds to two different molecules at adjacent positions within the helix. On the other side of the same molecule, a similar motif generates another helix of opposite helicity to the first. The molecule has a crystallographic plane of symmetry through the two bridgehead carbon atoms and the two bridgehead methyl groups, which are syn-periplanar. Thus, 5 is similar to 3,4-dimethylglycoluril (3), but differs from some glycolurils, where there is a significant dihedral angle between the two bridgehead-to-bridgehead substituent bonds. Bond lengths and angles in 5 resemble those reported for 3, but bond lengths around the bridgehead positions are slightly lengthened relative to 3.Key words: glycoluril, 1,2,5,8-tetramethyl-2,6,7,8-tetraazabicyclo[3.3.0]octane-3,7-dione, X-ray diffraction, crystal structure, hydrogen-bond array.

Reactions of the tetrasulfur pentanitride(-1) ion with halogens: synthesis, spectroscopic characterization, and crystal structure of pentasulfur hexanitride

1979 ◽  
Vol 57 (11) ◽  
pp. 1286-1293 ◽  
Author(s):  
T. Chivers ◽  
J. Proctor
Keyword(s):  
Crystal Structure ◽  
Thionyl Chloride ◽  
Mass Spectra ◽  
Methylene Chloride ◽  
Spectroscopic Characterization ◽  
The Other ◽  
X Ray ◽  
Yellow Orange ◽  
Uv Visible ◽  
Single Bonds

Pentasulfur hexanitride, S5N6, has been prepared in good yield by the reaction of [n-Bu4N+][S4N5−] with bromine (or iodine) in methylene chloride at 0 °C. In contrast, the tetrasulfur pentanitride(−1) ion reacts smoothly with chlorine to give S4N5Cl, while the reaction with sulfuryl chloride produces S4N5Cl and S5N6 and the reaction with thionyl chloride produces a mixture of S3N2O, S3N2O2, S4N4, and S5N6. Pentasulfur hexanitride is an air-sensitive, explosive, yellow-orange solid which sublimes at ca. 45 °C/10−2 Torr without significant decomposition. It has been characterised by infrared, Raman, uv–visible, and mass spectra and by a single crystal X-ray structure determination. The crystals are monoclinic and belong to the space group C2/c, a = 8.787(2), b = 11.190(2), c = 7.427(2) Å, β = 106.46(2)°, V = 700.3(5) Å3, Z = 4, Dc = 2.317 g cm−3. The refined structure (Rw = 0.040) has twofold symmetry and resembles a basket in which an —N=S=N— unit (d(S—N) = 1.54 Å) is the handle which bridges an S4N4 cradle via S—N single bonds (d(S—N) = 1.70 Å). The introduction of this bridge widens one of the [Formula: see text] transannular separations in S4N4 to 3.94 Å while the other is shortened to 2.43 Å. Thus, the S4N4 cradle can be viewed as two five-membered rings fused at the S—S bond.

Synthese, Schwingungs- und Massenspektren von Et2Sn(O2PR2)2 (R = Me, Ph); Kristallstruktur von Et2Sn(O2PPh2)2 / Synthesis, Vibrational Spectra and Mass Spectra of Et2Sn(O2PR2)2 (R = Me, Ph); Crystal Structure of Et2Sn(O2PPh2)2

1996 ◽  
Vol 51 (8) ◽  
pp. 1111-1116 ◽  
Author(s):  
Abdel-Fattah Shihada ◽  
Frank Weller
Keyword(s):  
Crystal Structure ◽  
Vibrational Spectra ◽  
Mass Spectra ◽  
Structure Refinement ◽  
Base Peak ◽  
Trans Position ◽  
X Ray Diffraction ◽  
X Ray ◽  
Octahedral Environment ◽  
In Trans

Et2Sn(O2PPh2)2 has been synthesized by the reaction of (Et2ClSn)2O with Ph2POCl in toluene and by the treatment of (Et2ClSn)2O or Et2SnCl2 with HO2PPh2 in methanol. The reaction of Et2SnO with HO2PMe2 in toluene was used to prepare Et2Sn(O2PMe2)2. An X-ray diffraction study of Et2Sn(O2PPh2)2 (space group P1̅, Z = 1, a = 559,9( 1), b = 983,7(1), c = 1262,4(l)pm, α = 81,85( 1 )°, β = 79,79( 1)°, γ = 75,00(1)°; structure refinement with 2662 independent reflections, R = 0.055) shows that the structure is polymeric and the O2PPh2 ligands function as double bridges between the tin atoms leading to the formation of centrosymmetric Sn2O4P2 eight-membered rings. The ethyl groups are in trans-position in the resulting octahedral environment around tin. The I. R. and Raman spectra of Et2Sn(O2PR2)2 (R = Ph, Me) have been discussed and assigned. The mass spectra of Et2Sn(O2PR2)2 show Sn(O2PR2)+ as the base peak.

Cobalt(III) Complexes of the 10-Membered Macrocycle 1,4,7-Triazacyclodecane. The Structure of trans-Bis(1,4,7-triazacyclodecane)cobalt(III) Perchlorate

1993 ◽  
Vol 46 (12) ◽  
pp. 1955 ◽  
Author(s):  
TW Hambley ◽  
TW Hambley ◽  
GH Searle ◽  
GH Searle
Keyword(s):  
Crystal Structure ◽  
Membered Ring ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

The crystal structure of trans-[Co( tacd )2](ClO4)3 has been determined by X-ray diffraction methods and refined to a residual of 0.054 for 2477 independent observed reflections. The crystals are monoclinic, P 21/c, a 18.627(2), b 9.3438(5), c 16.057(2)Ǻ, β 119.45(2)°. Two complex cations are located at centres of symmetry and the ligands adopt λ,δ,chair conformations. Bond lengths from cobalt to nitrogen atoms in the six- membered ring (average 1.995 Ǻ) are significantly longer than those only associated with five- membered rings (average 1.961 Ǻ).

EXAFS and XRD investigations of zeunerite and meta-zeunerite

2003 ◽  
Vol 218 (1) ◽  
Author(s):  
C. Hennig ◽  
G. Reck ◽  
T. Reich ◽  
A. Roßberg ◽  
W. Kraus ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

AbstractIn this paper EXAFS was used to determine bond lengths in the structures of zeunerite and meta-zeunerite. The atomic distances between heavy and light scatterers observed using EXAFS in meta-zeunerite deviate approximately 0.1 Å from literature data of single-crystal X-ray diffraction measurements. Because this difference is significant higher than the error limits of EXAFS measurements, the complete crystal structure of meta-zeunerite, Cu[UO

Preparation and Crystal Structure of Genistein Benzenesulfonate Prodrugs

2008 ◽  
Vol 2008 (10) ◽  
pp. 555-558 ◽  
Author(s):  
You Peng ◽  
Zeyuan Deng ◽  
Shaojie Lang ◽  
Yawei Fan
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Sulfonic Acid ◽  
Nmr Spectra ◽  
High Yield ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
H Nmr ◽  
Ester Prodrugs

In order to improve bioavailability and anticancer activity of genistein, a series of novel sulfonic acid ester prodrugs of the isoflavone genistein were synthesised in high yield with excellent regioselectivity. Their structures were characterised by IR, MS, elemental analysis and 1H NMR spectra. The crystal structure was examined by X-ray diffraction. X-ray structure determination revealed that all the aromatic rings in the compound are not coplanar. In the crystal structure, molecules are linked through intermolecular C-H···O hydrogen bonds, forming layers parallel to the ab plane.

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