CRYSTAL STRUCTURE OF ADDUCT OF BIS(O,O''''-DIBUTYLDITHIOPHOSPHATO)-NICKEL (II) WITH BIPYRIDYL

<正> Ni[(C8H9O)2PS2]2 bipy, Mr=697.57, triclinic, Ci-Pl, a=9.469(1)A, b=14.638(3)A, c=14.637(2)A, α=69.64(1)° , β=71.16(1)°, r=89.99(1)°, V= 1785.6A3, Z=2, Dc=1.297g.cm-3, Mo kα radiation, λ=0.71073A, F(000)=736e, R=0.081 for 4986 independent reflections. Ni(II) is coordinated by four sulfur atoms and two nitrogen atoms to form a distorted octahedron. The angles between each two among planes N2Ni, NiS(11)S(12) and NiS(21)S(22) are nearly 90°.     

AFFINITY LABELLING OF E.coil LEUCYL-tRNA SYNTHETASE WITH 3''''-OXIDIZED tRNA~(Leu)

The E.coli leucyl-tRNA synthetase (E. C. 6. 1. 1. 4) was specifically labelled with 3'-oxidized tRNA~(Leu) (tRNA_(ox)~(Leu)).The procedure involves a Schiff's base formation and its subsequent reduction by sodium cyanoborohydride. Stoichiometric inactivation of aminoacylation was achieved with the incorporation of 1 mol of tRNA_(ox)~_(Leu) per mol LeuRS.On the other hand, the amino acid activation activity of LeuRS-tRNA_(ox) complex was partially inhibited. After extensive digestion of the complex by pancreatic ribonuclease, the amino acid activation activity was fully recovered, while the aminoacylation activity was not restored at all.The results suggest that the active sites responsible for the activities of LeuRS correlate with each other as well as differ from each other.     

STRUCTURES OF COPPER(I) AND ZINC(II) COMPLEXES WITH N,N′-BIS(2-PYRIDINYL)THIOUREA (BPT)

Abstract

Copper(I) and zinc(II) complexes with N,N′-bis(2-pyridinyl)thiourea (BPT), [Cu(BPT)₂]ClO₄ (1) and [Zn(BPT)₂](ClO₄)₂ (2) were synthesized by reaction of M(ClO₄)₂ (M = Cu, Zn) with BPT in methanol solution. The crystal structures of complexes (1) and (2) were characterized by X-ray diffraction: (1) is triclinic, space group P, with a = 10.162(2), b=14.483(6), c = 9.496(2) Å, α = 105.80(2)°, β = 106.94(2)°, γ = 82.71(3)°, V = 1284.4(7) ų, Z = 2, and final R = 0.047, R _w = 0.061; (2) is monoclinic, space group C2/c, with a = 15.15(1), b = 6.299(3), c = 30.16(1)Å, β = 93.49(7)°, V = 2872(2)ų, Z=4, and final R = 0.049, R_w = 0.070. Both of the complexes exhibit novel structures. Two N atoms and two S atoms from two BPT groups coordinate to one M atom. The M atom shows distorted tetrahedral geometry. IR spectra and ther-moanalyses of BPT and its complexes (1) and (2) are briefly discussed.     

SYNTHESIS AND STRUCTURE OF EUROPIUM (Ⅲ) WITH N,N'''' BISSALICYLIDENE ETHYLENEDIAMINE (H_2salen)

<正> A europium (Ⅲ) complex with N, N' - bissalicylidene-ethylenediamine (H2salen) has the formula Eu(Hsalen)(salen)4H2O,where water molecules are in the outer sphere and do not coordinate with Eu (Ⅲ), was synthesized and structurally studied. The central atom Eu is coordinated by four nitrogen atoms and four oxygen atoms in a deltadodecahedron arrangement. The crystal is monoclinic,space group P21/a with cell constants a=16. 441(2),b=20. 599(3),c=10. 719(2) A ,β=84. 16(1)°,Z=4 and V = 3611. 5(8) A3,Dc=1. 392g/cm3.The final standard deviation R is 0. 093.     

STUDIES ON POLYHALOALKANES Ⅳ. THE REACTION OF POLYFLUOROALKYL IODIDES WITH SILVER(I) SALTS

The conversion of polyfluoroalkyl iodides into the corresponding carboxylic acids by the reaction with silver (I) salts is described.     

STRUCTURE OF A Cu (Ⅱ) COMPLEX WITH MIXED LIGANDS, DIETHYLENETRIAMINE ETH YLENEDIAMINE COPPER (Ⅱ) DIPERCHLORATE

<正> CuC6H21N5O8Cl2, Mr = 425. 5, monoclinic, P21/n, a = 8. 418 (2), b = 14.450(4), c= 12. 940(3)A, β=98. 13(2)% V = 1572. 9A3,Z = 4, Dx= 1. 797g. cm-3,μ(MoKa) = 18. 3cm-1. The crystal structure consists of discrete complex cations and perchlorate anions. The coordination geometry around Cu(Ⅱ) atom is a distorted square pyramid. The complex cations are disordered in the crystal,the ethylenediamine ligand chelates to the Cu(Ⅱ ) atom in δ arid λ conformation in different cells. The average Cu-N distance is 2. 03 A in the equatorial plane while the Cu -N distance is 2. 25 A in the axial direction.     

CRYSTAL AND MOLECULAR STRUCTURES OF SCHIFF BASE COM-PLEXES WITH TRANSITION METAL IONS Ⅱ . BIS-( N-( 4-CHLQRO-PHENYL)-SALICYLALDIMINATO)COBALT (Ⅱ)

<正> The crystal and molecular structure of the title compound was determined by means of Patterson and Fourier synthesis based on three-dimensional X-ray data. The crystallographic parameters are as follows; (C13H8NOCl)2Co, monoclinic, space group A2/a,a = 11. 722 (8) , b = 8. 726 (5) , c = 21. 810 (8) A ,β= 95. 90 (6)°, V = 2219. OA3,Z= 4, Dc=1.55g/cm3,μ= 10. 71cm-1, F(000) = 1052, R= 0.042, Rw = 0. 051. Two iminato ligands are attached to the center atom Co through their donor atoms N(1),O(1),N(1)* ,and O(1)* to form a distorted tetrahedral configuration. The bond lengths of Co-O and Co-N are 1. 891 and 1. 988 A , respectively.     

COPPER(II), NICKEL(II) AND COBALT(II) COMPLEXES WITH N,N′-BIS(2-N,N-DIMETHYLAMINOETHYL)PYRIDINE-2,6-DICARBOXAMIDE 1-OXIDE. BINUCLEATING BEHAVIOUR BY A DEPROTONATED PYRIDINE N-OXIDE LIGAND

Abstract

New copper(II), nickel(II), and cobalt(II) complexes are described with the potentially binu-cleating pyridine N-oxide ligand N,N′-bis(2-N,N-dimethylaminoethyl)pyridine-2,6-dicarboxamide 1-oxide (medpco). Electronic spectra and X-ray powder diffraction measurements indicate that metal complexes of the type M(medpco)Hal₂(H₂O) _x (Hal = Cl, Br) are five-coordinate. Monomeric structures are proposed with ONN-bonded ligand and coordinated halide. This is analogous to the coordination to one of the coppers in the previously reported X-ray structure of Cu₂(medpco)Cl₄. Complexes of the type M′₂(medpco-2H)Hal₂(H₂O) _z (M′ = Ni, Co), involving deprotonated ligand, are reported. These appear to have N-oxide-bridged structures, involving binucleating ligand, analogous to the previously reported X-ray structure of Cu₂(medpco-2H)Cl₂. Variable temperature magnetic data for the complexes are discussed.     

VARIATION OF C_(60) SOLUBILITY WITH TEMPERATURE

ＶＡＲＩＡＴＩＯＮＯＦＣ_（６０）ＳＯＬＵＢＩＬＩＴＹＷＩＴＨＴＥＭＰＥＲＡＴＵＲＥＹｏｎｇＪｕｎＬＥＮＧ；ＷａｎＸｉＣＨＥＮ；ＺｈｕＤｅＸＵ；ａｎｄＷｅｎＺｈｕＬＩＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙａｎｄＤｅｐａｒｔｍｅｎｔｏｆＰｈｙｓｉｃ?..     

SYNTHESIS, SPECTRAL AND MAGNETIC CHARACTERISATION OF SOME BIMETALLIC ALKOXIDES OF NICKEL(Ⅱ)WITH GALLIUM(Ⅲ)AND ZIRCONIUM(IV)

Some interesting bimetallic isopropoxides of nickel(Ⅱ) with gallium(Ⅲ) and zirconium(Ⅳ), Ni[Ga(OPr~1)_4]_2 and Ni[Zr_2(OPr_1)_9]_2 have been synthesized by the interaction of NiCl_2·2Pr~1OH with K[Ga(OPr~1)_4],and K[Zr_2(OPr~1)_9] respectively, in 1:2 molar ratio. These bimetallic isopropoxides undergo facile alcohol interchange reactions with primary alcohols. However, reactions with tertiary alcohols result in the isolation of partially substituted derivatives with the compositions, Ni[Ga(OPr~1)(OBu~t)_3]_2 and Ni[Zr_2(OPr~1)_3(OBu~t)_6]_2. Characterisation of these derivatives has been made on the basis of elemental analyses, infrared, electronic spectral and magnetic susceptibility measurements. These studies suggest an octahedral geometry for nickel(Ⅱ) in the primary bimetallic alkoxides, while in the case of secondary and tertiary derivatives, an equilibrium is suggested between octahedral and tetrahedral forms.##属性不符     

Protoberberine ausReissert-Verbindungen, 4. Mitt. Eine neue Synthese des (±)-Alamaridins und des (±)-epi-Alamaridins

Summary A novel synthesis of 8-methylisoquino[2,1-b][2,7]naphthyridinium salts7 is reported using the intramolecular cyclization of the 1-substituted isoquinolines5 as the key step, which in turn are obtained by alkylation of theReissert compounds1. The salts7 can be reduced by NaBH₄ yielding the 8- and 8-methylstereomers (±)-alamaridine and (±)-epi-alamaridine9c and11c, respectively.

     

PEARL-NECKLACE-POLYMER: COPOLYMERIZATION OF C_(60) WITH PARACYCLOPHANE

ＰＥＡＲＬ－ＮＥＣＫＬＡＣＥ－ＰＯＬＹＭＥＲ：ＣＯＰＯＬＹＭＥＲＩＺＡＴＩＯＮＯＦＣ_（６０）ＷＩＴＨＰＡＲＡＣＹＣＬＯＰＨＡＮＥ￥ＳｈａｏＭｉｎｇＨＵＡＮＧ；ＸｕｅＨａｉＹＵ；ＣｈａｎｇＺｈｅｎｇＹＡＮＧａｎｄＬｉＦｅｎＷＵ（ＣｈｅｍｉｓｔｒｙＤｅ?..     

REACTION OF METHANE WITH CARBON DIOXIDE OVER SrNiAl_(11)O_(19)

合成了六铝酸盐ＳｒＮｉＡｌ１１Ｏ１９并用ＸＲＤ、ＵＶＤＲＳ、ＴＧＤＴＡ和ＴＥＭ等技术对其进行了表征。在７５０℃于ＳｒＮｉＡｌ１１Ｏ１９上进行的甲烷与二氧化碳重整反应表明，这类催化剂较Ｎｉ／ＳｒＡｌ１２Ｏ１９具有较大活性和低积碳能力，在催化反应过程中可有效地抑制Ｎｉ颗粒的增大。     

PREPARATIONS OF COPPER (Ⅰ) COMPLEXES WITH NOVEL PYRAZOLYLBORATES

ＰＲＥＰＡＲＡＴＩＯＮＳ　ＯＦ　ＣＯＰＰＥＲ（Ⅰ）ＣＯＭＰＬＥＸＥＳ　ＷＩＴＨ　ＮＯＶＥＬ　ＰＹＲＡＺＯＬＹＬＢＯＲＡＴＥＳＰＲＥＰＡＲＡＴＩＯＮＳＯＦＣＯＰＰＥＲ（Ⅰ）ＣＯＭＰＬＥＸＥＳＷＩＴＨＮＯＶＥＬＰＹＲＡＺＯＬＹＬＢＯＲＡＴＥＳ￥ＫｅＷｕＹ...     

ASYMMETRIC REDUCTION OF S-ALKYL-S-ARYL-N-p-TOSYLSULFILIMINES WITH L(–)CYSTEINE

Abstract

Partial reduction of racemic mixture of S-alkyl-S-aryl-p-tosyl sulfilimines with L(–)cysteine affords optically active recovered sulfilimine. In the case of S-methyl-S-p-tolyl-N-p-tosylsuifilimine the absolute configuration and the optical yield were determined.