Synthesis, characterization and molecular structure of a dinuclear uranyl complex supported by N,N′,N″,N′″-tetra-(3,5-di-tert-butylsalicylidene)-1,2,4,5-phenylenetetraamine

2015 ◽  
Vol 70 (10) ◽  
pp. 757-763 ◽  
Author(s):  
René Schnorr ◽  
Marcel Handke ◽  
Berthold Kersting
Keyword(s):  
Molecular Structure ◽  
Uranium Atom ◽  
Protonated Form ◽  
Uranyl Complex ◽  
Cyclic Voltammogram ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray Crystallography ◽  
Reversible Redox ◽  
Ethanol Solvate

AbstractThe preparation, characterization and the molecular structure of a dinuclear uranyl complex [(UO2)2L(OCMe2)2] supported by the bis-salophen ligand N,N′,N″,N′″-tetra-(3,5-di-tert-butylsalicylidene)-1,2,4,5-phenylenetetraamine (L4–) is described. [(UO2)2L(OCMe2)2] was prepared by reaction of uranyl nitrate with the neutral, protonated form of the ligand (H4L) in acetone. From a saturated acetone solution [(UO2)2L(OCMe2)2]·1.5(OCMe2) crystallizes triclinically, space group P1̅ with a = 1522.7(2), b = 1751.4(2), c = 1815.4(2) Å, α = 109.16(1), β = 99.29(1), γ = 105.29(1)° and Z = 2. Each uranium atom is surrounded in a distorted pentagonal bipyramidal fashion by two O and two N atoms of the salicylidene units, one O atom of an acetone ligand, and the two oxo groups. The cyclic voltammogram of [(UO2)2L(OCMe2)2] shows two quasi-reversible redox processes centered at +0.57 V and +0.82 V vs. Fc+/Fc attributed to the sequential oxidation of the coordinating phenolates to phenoxyl radicals. The crystal structure of an ethanol solvate of H4L was also determined by X-ray crystallography. H4L·5EtOH: triclinic, space group P1̅, a = 1003.4(3), b = 1187.7(3), c = 1905.1(5) Å, α = 75.75(2), β = 78.74(2), γ = 66.66(2)°, Z = 1.

Supramoleküle aus Kronenethern und geminalen Sulfonen: Synthese von vier binären Komplexen und Kristallstruktur von (CH2CH2O)4·2H 2C(SO2C2H5)2/Supramolecules of Crown Ethers with Geminal Sulfones: Synthesis of Four Binary Complexes and Crystal Structure of (CH2CH2O )4·2H2C(SO2C2H5)2

1995 ◽  
Vol 50 (7) ◽  
pp. 1018-1024 ◽  
Author(s):  
Axel Michalides ◽  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Binary Complexes ◽  
Cyclic Polyethers ◽  
Adjacent Unit ◽  
Methylene Group

In a systematic search for supramolecular complexes involving all combinations of the cyclic polyethers 12-crown-4 (12C4), 15-crown-5 (15C 5), 18-crown-6 (18C 6) and dibenzo- 18-crown-6 (DB -18C6), and the geminal di- or trisulfones H2C(SO 2Me)2, H2C (SO2Et)2 and HC (SO2Me)3-n (SO2Et)n (n = 0 -3 ) , only the following four complexes could be isolated and unequivocally characterized by elemental analysis and 1H NMR spectroscopy: [(12C4){H2C (SO2Et)2}2] (3), [(18C6){H2C (S O2Me)2}] (4), [(DB -18C 6){H2C (SO2Et)2}] (5) and [(D B -18C 6)2{HC (SO2Me )(SO2Et)2}3] (6). The structure of 3 (triclinic, space group P1̄) consists of crystallographically centrosymmetric formula units, in which the disulfone molecules are bonded on each side of the ring by two C -H ··· O(crown) interactions originating from the central methylene group (H···O 213 pm) and from the methylene group of one EtSO2 moiety ( H ··· O 237 pm). Formula units related by translation are connected into parallel strands by a third type of reciprocal C -H ···O bond (H ···O 232 pm) between the second H atom of the central methylene group and a sulfonyl oxygen atom of the adjacent unit. The structure of 4 (monoclinic, space group C2/c) showed severe disorder of the crown ether and could not be refined satisfactorily. Compounds 5 and 6 crystallized as long and extremely thin fibres, indicative of linear-polymeric supramolecular structures; single crystals for X-ray crystallography were not available.

Synthesis and molecular structure of tetraphenylarsonium Tetrakis(benzenethiolato)-oxorhenate(V)-Acetonitrile (1/1)

1983 ◽  
Vol 36 (2) ◽  
pp. 253 ◽  
Author(s):  
AC McDonell ◽  
TW Hambley ◽  
MR Snow ◽  
AG Wedd
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Crystal Data ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography

The salts Ph4As [ReO(SPh)4].MeCN and Ph4As [ReO(SePh)4] have been synthesized and characterized. The crystal and molecular structure of the thiolate compound has been determined by X-ray crystallography which reveals a square-pyramidal arrangement of ligand atoms around the central rhenium atom of the [ReO(SPh)4]- anion. Crystal data: a 9.756(4), b 18.171(3), c 25.684(4) �, space group P212121, Z 4.

The Structures of the Decaphenylmetallocenium Cations of Chromium and Cobalt

1997 ◽  
Vol 50 (11) ◽  
pp. 1035 ◽  
Author(s):  
Leslie D. Field ◽  
Trevor W. Hambley ◽  
Taian He, ◽  
Anthony F. Masters ◽  
Peter Turner
Keyword(s):  
Methylene Chloride ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography

Decaphenylchromocenium and decaphenylcobaltocenium cations [M(η5-C5Ph5)2]+, M = Cr and Co, were synthesized by oxidation of the corresponding neutral decaphenylchromocene and decaphenylcobaltocene respectively with nitrosyl tetrafluoroborate. The complexes are air-stable and were fully characterized; decaphenylchromocenium tetrafluoroborate (1) and decaphenylcobaltocenium tetrafluoroborate (2) were structurally characterized by X-ray crystallography. Crystals of (1) (as a water/methylene chloride solvate), C70·5H50BClCrF4O0·5, M 1079·42, are triclinic, space group P -1 (No. 2), a 13·634(5), b 17·424(5), c 13·298(4) Å, α 106·45(2), β 101·83(3), γ 74·56(2)°, Z 2. Crystals of (2) (as a water/methylene chloride solvate), C70·5H50BClCoF4O0·5, M 1086·36, are triclinic, space group P-1 (No. 2), a 13·633(2), b 17·683(3), c 13·255(3) Å, α 107·95(1), β 102·71(1), γ 73·23(1)°, Z2.

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.

Organoamido- and Aryloxo-lanthanoids. III. Preparation and X-Ray Structure of Bis(μ-3,5-dimethylpyrazolato-N:N′)bis(μ-tetrahydrofuran-O)-bis[bis(η2-3,5-dimethylpyrazolato-N,N')neodymium(III)]

1991 ◽  
Vol 44 (4) ◽  
pp. 613 ◽  
Author(s):  
GB Deacon ◽  
BM Gatehouse ◽  
S Nickel ◽  
SN Platts
Keyword(s):  
Trigonal Prism ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Dimeric Structure

Reaction of neodymium metal with bis ( pentafluorophenyl )mercury and pyrazole ( Hpz ) or 3,5-dimethylpyrazole ( Hdmpz ) in tetrahydrofuran ( thf ) yields Nd ( pz )3 or [ Nd ( dmpz )3( thf )]2. X-Ray crystallography has shown that [Nd (dmpz )3( thf )]2 [triclinic, space group Pī (No. 2), a 11.070(4), b 11.364(3), c 10.867(2)Ǻ, α 103.00(1), β 120.78(3), γ 97.68(2)°, R 0.0235, Rw 0.0247 for 5575 observed reflections] has a novel centrosymmetric dimeric structure. Each neodymium is eight-coordinate (4,4 bicapped trigonal prism) with two terminal chelating dmpz ligands [ Nd -N 2.400(2), 2.413(3), 2.422(3), 2.426(3)Ǻ], two bridging dmpz ligands [ Nd -N 2.509(2), 2.511(2)Ǻ], and, unexpectedly, two bridging tetrahydrofuran ligands [ Nd -O 2.792(2), 2.757(2)Ǻ].

Structure cristalline et moléculaire du cyclopentadiényle dicarbonyle triphénylphosphine manganèse, MnC5H5(CO)2P(C6H5)3

1973 ◽  
Vol 51 (18) ◽  
pp. 3027-3031 ◽  
Author(s):  
Claude Barbeau ◽  
Klaus Sorrento Dichmann ◽  
Louis Ricard
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Least Squares Method ◽  
Three Dimensional ◽  
Triphenyl Phosphine ◽  
Triclinic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Atomic Parameter

The crystalano molecular structure of cyclopentadienyl manganese dicarbonyl-triphenyl phosphine has been determined by means of three dimensional data obtained by a Buerger precession camera. 2931 independent intensities were utilized in the refinement of the structure using the least-squares method. The final disagreement factor is 0.11. MnC5H5(CO)2P(C6H5)3 crystallizes in the triclinic space group.[Formula: see text]The molecule shows atomic parameter almost identical to those of MnC5H5(CO)3 except for the Mn—C bond lengths which change from 1.80 to 1.73 Å. The Mn—P distance (2.236 Å) and the unchanged parameters for the Mn—C5H5 group confirm the strong donating power of the cyclopentadienyl group. [Journal translation]

The Crystal Structure of the Tetrameric Adduct of Antimony Trichloride and Phosphoryl Isothiocyanate, [SbCl3·OP(NCS)3]4

1994 ◽  
Vol 49 (4) ◽  
pp. 441-444 ◽  
Author(s):  
Alexander V. Sienkiewicz ◽  
Anatoliy A. Kapshuk
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Antimony Trichloride ◽  
Cage Structure ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Cubic System ◽  
Tetrameric Complex

The crystal and molecular structure of the tetrameric complex of the composition [SbCl3·OP(NCS)3]4 synthesized from SbCl3 and OP(NCS)3 in CCl4 waso determined by X-ray crystallography [143 m space group, cubic system with a = 13.927(4) Å]. The complex exhibits a tetranuclear "cage" structure with a [Sb4O4] core which consists of μ3-bridging oxygen and six coordinate antimony(III) atoms; the Sb-O distance, 3.060 Å, is exceptionally long.

Metal-selenolate chemistry: stereochemistry of adamantane-type clusters of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd)

1992 ◽  
Vol 70 (3) ◽  
pp. 792-801 ◽  
Author(s):  
Jagadese J. Vittal ◽  
Philip A. W. Dean ◽  
Nicholas C. Payne
Keyword(s):  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Space Groups ◽  
X Ray Crystallography ◽  
Cell Dimensions ◽  
Minimum Number

The structures of three tetramethylammonium salts containing anions of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd) were determined by single crystal X-ray diffraction techniques. The Zn salt crystallizes in different space groups depending upon the solvent combination used in the synthesis. Thus crystals of (Me4N)2[Zn4(SePh)10], 1, grown from a mixture of methanol, acetonitrile, and acetone are triclinic, space group [Formula: see text] with cell dimensions a = 13.214(2), b = 23.859(2), c = 13.072(1) Å, α = 91.134(8), β = 113.350(8), γ = 79.865(9)°, and Z = 2. In the absence of acetone, a solvated crystal (Me4N)2[Zn4(SePh)10]•CH3CN, 2, is formed, which belongs to the monoclinic space group P21/n with a = 14.248(1), b = 39.722(2), c = 13.408(1) Å, β = 97.132(5)°, and Z = 4. The Cd salt (Me4N)2[Cd4(SePh)10], 3, crystallizes in the monoclinic space group P21/c, with a = 20.830(2), b = 14.282(1), c = 25.872(1) Å, β = 99.626(6)°, and Z = 4. These three salts are the first examples of homoleptic, tetranuclear selenolatometal(II) anions with (μ-Se)6M4 cages of adamantane-type stereochemistry. In each case the phenyl substituents of the bridging ligands adopt the configuration [aae, aae, aee, aee], which has the minimum number of two 1,3-axial–axial non-bonding substituent interactions. Keywords: selenolate complexes, synthesis, X-ray crystallography, isomerism, adamantane stereochemistry.

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.

Silaheterocyclen: Molekülstruktur eines 3-Oxa-2,4,6,7-tetrasilabicyclo[3.1.1]heptans / Silaheterocycles: Molecular Structure of a 3-Oxa-2,4,6,7-tetrasilabicyclo[3.1.1]heptane

1989 ◽  
Vol 44 (7) ◽  
pp. 796-799 ◽  
Author(s):  
Gabriele Reber ◽  
Jürgen Riede ◽  
Nils Wiberg ◽  
Gerhard Wagner ◽  
Gerhard Müller
Keyword(s):  
Molecular Structure ◽  
Dihedral Angle ◽  
Structure Analysis ◽  
Membered Ring ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

According to an X-ray structure analysis 1,5-bis(di-tert-butylmethylsilyl)-2,2,4,4,6,6,7,7-octamethyl-3-oxa-2,4,6,7-tetrasilabicyclo[3.1.1]heptane (1) is a rigid bicyclic molecule consisting of a 1,3-disilacyclobutane ring whose 2,4 positions are bridged by a Me2Si—O—SiMe2 fragment. The four-membered ring is non-planar with a dihedral angle of 33.8° along the C—C axis. The intraring valence angles at carbon are significantly smaller than those at silicon leading to a transannular Si ··· Si distance of only 2.558(1) Å (triclinic, space group P 1̄ with a = 9.125(2), b = 12.668(2), c = 15.499(3) Å, α = 101.25(1), β = 87.87(1), γ = 96.88(1)°, V = 1744.4 Å3 R (wR) = 0.044 (0.051) for 316 refined parameters and 5156 observables).

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