CRYSTAL STRUCTURE OF [Eu(μ-CH_3COC-O)(CH3COO)_2(H_2O)_2]_2·4H_2O

<正> C12H34O20Eu2,Mr=802.30 triclinic, space group P1, a= 8.955(2), b=9.328(1), c=10.536(2) A,α= 91.74(2),β=113.87(2),γ=118.23(2), V=681.7(2)A,Dm(flotation in CC14/ BrCH2CH2Br)=1.95,DX(Z=1) =1.954g cm-3,λ(MoKα)=0.71069 A,μ=6.41 cm-1,F(OOO)=391.92, T =. 295°K,final RF= 0.032 for 7483 observed reflections with |F0|>3a(|Fo|). The compound is isostructural with the known erbium complex,the basic unit being a centrosymmetric dimer composed of two nine-coordinate polyhedra sharing a common edge. An O atom in one or the three bidentate acetato groups about each europium atom serves as a bridge between the metal centars. The dimeric units are linked by hydrogen bonds involving both ligand and lattice water molecules to form a three-dimensional network.     

CRYSTAL STRUCTURE OF [Sm(CCl_3COO)_3(H_2O)_2]·2H_2O

<正> Biaqua-trichloroacetate-samarium dihydrate, [Sm(CCl3COO)3(H2O)2]-2H2O, Mr=707.54, orthorhombic, space group Pnne, with a = 19.158(5), b = 22.176(4), c= 9.798(4)A, Z= 8, V= 4162.7A3.F{000)= 2696,λ(MoKα)=0.71069A, Dx = 2.258 g/cm3, final R=0.061. The title compound has non-molecular structural character, and its structural units Sm(μ-CCl3COO)s/2-(H2O>2 constitute 2-dinensional infinite chains of Sm(μ-CCl3COO)4Sm(μ-CCl3-COO)2Sm.The Sa(Ⅲ) atom in each unit is bound to two O atoms from aqua-molecules and six 0 atoms from six bridging CCl3COO groups (four of which are shared with the SB atom of another unit, two shared with the Sm atom of a third unit) forming a square antiprism.     

Synthesis and magnetic properties of copper(Ⅱ)-lanthanoid(Ⅲ) binuclear complexes with N,N''''-bis(3-aminopropyl) oxamido ligand

Six novel u-oxamido binuclear complexes, namely Cu(oxpn)Ln(L)2(ClO4)3 (Ln: Eu, Gd, Tb, Nd, Ho, Er), where oxpn is N,N'-bis(3-aminopropyl) oxamido, L denotes 5-nitro-1,10-phenanthroline (abbreviated as NO2-phen), have been synthesized and characterized. The magnetic susceptibility of complexes Cu(oxpn)Gd(NO2-phen)2(ClO4)3.2H2O was measured over the 4-300 K and the observed data were successfully simulated by equation based on spin Hamil-tonian operator (H = -2JS1.S2), giving the exchange integral J(Cu-Gd)=-1.62 cm-1. This indicates a weak antiferromagnetic interaction between the Cu(Ⅱ) and Gd(Ⅲ) ions.     

CRYSTAL STRUCTURE OF [Eu_2(Met)_3(Gly)(H_2O)_3](ClO_4)_6

<正> The crystal structure of [Eu2(Met)3(Gly)(H2O)2](ClO4)6(Met=CH3-S(CH2)2CHNH2COOH, Gly=NH2CH2COOH) belongs to monoclinic system with space group P21/n.The final R is 0.060. The Met and Gly are bonded as bidentate bridging ligands to Eu(III) atoms.     

Low-temperature heat capacities and thermodynamic properties of rare-earth triisothiocyanate hydrates (Ⅲ)——Sm(NCS)_3·6H_2O,Gd(NCS)_3·6H_2O,Yb(NCS)_3·6H_2O and Y(NCS)_3·6H_2O

The heat capacities of four RE isothiocyanate hydrates,Sm( NCS)3 6H2O,Gd( NCS)3 6H2O,Yb(NCS)3 6H2O and Y( NCS)3 6H2O,have been measured from 13 to 300 K with a fully-automated adiabatic calorimeter No obvious thermal anomaly was observed for the above-mentioned compounds in the experimental tem-peiatnre ranges.The polynomial equations for calculating the heat capacities of the four compounds in the range of 13-300K were obtained by the least-squares fitting based on the experimental Cp data.The Cp values below 13 K were estimated by using the Debye-Einstem heat capacity functions.The standard molar thermodynamic functions were calculated from 0 to 300 K.Gibbs energies of formation were also calculated.     

SYNTHESIS,CRYSTAL STRUCTURE AND MAGNETISM OF THE COMPLEX:GdFe(CN)_64H_2O

ＳＹＮＴＨＥＳＩＳ，ＣＲＹＳＴＡＬ　ＳＴＲＵＣＴＵＲＥ　ＡＮＤ　ＭＡＧＮＥＴＩＳＭ　ＯＦ　ＴＨＥ　ＣＯＭＰＬＥＸ：ＧｄＦｅ（ＣＮ）_６４Ｈ_２ＯＳＹＮＴＨＥＳＩＳ，ＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＡＮＤＭＡＧＮＥＴＩＳＭＯＦＴＨＥＣＯＭＰＬＥＸ：ＧｄＦ...     

CRYSTAL STRUCTURE OF Co(H_2O)_3SO_4(phen)

<正> PRELIMINARY INFORMATION. The title compound is a member of a series of cobalt complexes of polydentate ligands currently being investigated. It was prepared by the reaction of CoSO_4·7H_2O with phenanthroline in the equimolar ratio.     

THE STRUCTURAL CHEMISTRY OF PRASEODYMIUM COMPLEXES OF AMINO ACIDS I. THE CRYSTAL STRUCTURE OF COMPLEX {[Pr(Gly)_3(H_2O)_2]_2(ClO_4)_65H_2O

<正> Introduction. The title compound has been synthesized and its crystal struture determined by X-ray analysis. The crystal structure of this type of complex was reported for the first time, as far as we know.     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF A NOVEL MOLYBDENUM-SULFUR CLUSTER COMPLEX, (NH_4)_4[Mo_3(NO)_4S_(13)]·3H_2O

The title compound has been synthesized, the crystal structure of which has been detorminedby the single-crystal X-ray diffraction method. The crystal belongs to triclinic space group C-P1 with the unit cell parameters: a =9.535(2)A, b = 9.740(2)A, c = 15.795(4)A, α = 89.85(2)°, β = 91.80(2)°, γ = 99.37(1)°,ν = 1446.6A~3, Ζ = 2. The structure is refined to R = 0.075, R_w = 0.074 for 1903 reflections. There are diverse bonding modes of molybdenum and sulfur in this eompound. The twosulfur atoms at the center bond to three molybdenum atoms from respective sides and formthe two apices of a trigonal bipyramid. Besides, there are S_2~(-2) ligands and a polysulfur chaincomposed of three sulfur atoms. The coordination number for the three molybdenum atomsis seven. Their coordination polyhedra are somewhat distorted pentagonal bipyramid. Eachof the three NO ligands coordinated to molybdenum gives a linear group of Mo-N-O, whilethe fourth NO ligund bonded with a polysulfur chain forms a bent group of S-N     

CRYSTAL STRUCTURE OF RhCl(dppm)_2·H_2O

<正> C50H46OP4ClRh, RhCl(dppm)2 · H2O, Mr = 922. 2, monoclinic, P21/2, a=10. 532(3), b=22.574(8), c=18. 641(8) A, β=93. 41(3)°, V = 4424 (3) A3, Z = 4, Dc=1. 386 g. cm-3, λ(MoKα) = 0. 71073A , F(000) = 1904. The structure was determined by direct methods and difference Fourier syntheses and refined by full-matrix least-squares to final R = 0. 037 and Rw = 0. 036 for 3432 (F> 6. 0σ(F) ) observed reflections. The structure of the title compound contains RhCl-(dppm)2 and non-coordinated H2O molecules. The rhodium atom is coordinated by one chlorine atom and four phosphorus atoms of two DPPM ligands forming a tetragonal pyramidal configuration.     

稀土元素异硫氰酸盐水合物的低温热容和热力学性质研究——Ⅲ.Sm(NCS)_3·6H_2O,Gd(NCS)_3·6H_2O,Yb(NCS)_3·6H_2O和Y(NCS)_3·6H_2O

用全自动绝热量热计测定了4种稀土异硫氰酸盐六水合物,Sm(NCS)_3·6H_2O,Gd(NCS)_3·6H_2O,Yb(NCS)_3·6H_2O和Y(NCS)_3·6H_2O在13～300 K间的热容,在实验温区上述化合物均未发现反常热容.根据实验热容数据用最小二乘拟合方法得出了计算这4种化合物在13～300 K温区内的热容多项式方程.13K以下的热容用 Debye-Einstein热容函数估算而得.计算了这些化合物在0～300 K间的标准热力学函数及其标准生成Gibbs能.     

CRYSTAL STRUCTURE OF A HETERONUCLEAR LANTHANIDE COMPLEX OF ERBIUM-YTTRIUM AND GLYCINE[ErY(GlY)_6(H_2O)_4](ClO_4)_65H_2O

The title complex [ErY(Gly)_6(H_2O)_4](ClO_4)_6 5H_2O has been synthesized.Its crystalstructure has been determined by X-ray diffraction method.The crystal is triclinic with space groupP1.The unit cell parameters are as follows:a=11.518(4),b=14.105(7),c=15.530(6) ,α=96.61(3),β=102.74(3),γ=105.70(3)°,V=2327.7(17) ~3,Z=2,Dc=2.091g/cm~3.The structure has been refinedto a final R of 0.0785.The crystal is an infinite chain complex,in which four carboxyl groups fromglycine molecules bridge the Er(Ⅲ)and Y(Ⅲ)ion,other two carboxyl groups bridge two adjacentEr(Ⅲ)or two Y(Ⅲ)ions.     

CRYSTAL STRUCTURE OF [Tm_4(p-NO_2C_6H_4CO_2)_(12)(H_2O)_(10)·2H_2O

<正> [Tm4 (p-NO2C6H4CO2)12 (H2O)10]·2H2O, Mr = 2885. 28, triclinic, space group P1 with a=14. 109(4) ,b= 14. 594(3) ,c= 13. 638(3) A ,α= 107. 04 (2), β=103. 36(2),γ= 93. 93(2)°, Z=1,V = 2584(1) A3.F(000) = l416,μ = 36. 4cm-1(Moka) ,Dc=1. 85g·cm3. The final R factor is 0. 034. The crystal structure is composed of tetrameric units in which four metal ions are bridged by carboxyl groups in chain form.     

CRYSTAL STRUCTURE OF MOLYBDENUM-CARBENE COMPLEX (CO)_5Mo=C(OC_2H_5)C_6H_4-p-CH_3

<正> INTRODUCTION. Recently, researches on carbene metal complexes are very active, as they are of great importance in both theoretical study and catalytic activity. In a systematic research, the crystal structure of the title complex was analyzed and reported here to the advantage of understanding the catalytic action and searching for new and better carbene catalysts of novel kinds.     

SYNTHESIS AND STRUCTURE OF A COBALT DIMER COMPLEX (Bt_4N)_2 [Co(SOC_6H_4 )(HOSC_6H_4)]_2

<正> The title compound was obtained by reaction of CoCl2.6H2O and mp2- (σ-C6H4SO2-) in MeCN,crystallized as Et4N+ salt in monoclinic system with space group P21/c, Mr=877.040. The cell parameters are:a =16.606(2), b=15.575(1),c=17.725(2)A,β=111.07(1)°,V=4277.8A3,Z=4,Dx= 1.36g/cm3.It is a dimer of [Co(mp)(Hmp)]- connected by two strong hydrogen bonds with a twist angle of about 36.94 .     

CRYSTAL STRUCTURE OF UO_2(PMBP)_2(H_2O) THF

<正> C34H28N407U·C4H4O Mr=910.7, monoclinic, Cc, a=12.999(1), b=15.448(2), c=18.481(2) A, β=100.18(2)°, Z=4, DC=1.656 g/cm-3, V=3652.3 A3, final R = 0.035 for 3457 observable reflections. Uranyl ion is coordinated equatorially by four oxygen atoms of PMBP and one oxygen atom of water in a distorted pentagonal bi-pyramid.     

CRYSTAL STRUCTURE OF (Br(μ-Met)(μ-Gly)(H_2O)_4]_2[Er(μ-Net)_2(H_2O)_4]_2(ClO_4)_(12)

<正> [Er(u-Met)(u-Gly)(H2O)4]2[Er(u-Met)2(HaO)4]2(ClO4)12(NMet=CH3S-(CH2)2CH(NH2)COOH,Gly=NH2CH2COOH), Mr=3194, trilinic, space group P1, a = 12.375(6),b= 14.041(13), c=19.074(13)A,α=80.85(6),β=80.72(6).γ=62.82(6)° ,Z=1,V= 2896A3,Dc=1.83 g/cm3,R=0.091. The carboxyl groups of Met and Gly in the title complex are bonded to Er atoms as bidentate bridging ligands.There are two different cations located at crystallographic symmetry centers in one unit cell.     

SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [CrMo_3 (μ_3-O)_3(μ-O)(μ-O_2CCH_3)_5(O_2CCH_3)_3]Na2 · H_2O

<正> The title complex C CrMo3 (μ3-O )3 (μ-O) (μ-O2CCH3 )5 (O2CCH3)3]2Na2 · H2O (Mr=1814. 32) crystallizes in monoclinic, space group P21/ n with a=11.209(5), b=18. 05(1), c=14. 44(1) A , β= 98. 30(5)°. V=2890 (3) A3, Z=2, A = 2. 08 g/cm3, F(000) -1780, Final R = 0. 049, Rw = 0. 058 for 2622 independent reflectons with I>3σ(I). The complex anion contains two Mo3O4 cores which connect two chromium atoms through four μ3-O atoms and eight bridging CH3COO- groups. Each of the Cr atoms and the Mo atoms is coordinated by six oxygen atoms. The anions are linked by Na cations to form one-dimensional infinite chain structure.     

CRYSTAL STRUCTURE OF A NOVEL TETRANUCLEAR MIXED-METAL CLUSTER Mo_2Fe_2Te_3(CO)_6(C_3H_3)_2

<正> Mr = 984. 63, orthorhombic Imm2, a = 14.562(3), b = 10.391(1), c = 7.139(4) A; V = 1080.2(1) A3, Z = 2, DC = 3.027 g.cm-3. Final R= 0.022 for 620 reflections with I > 20(Ⅰ). In the title compound, four metal atoms form a butterfly configuration, one ,μ-Te is bonded to these four metals and two μ3-Te cap two Fe-Mo-Mo faces. All these atoms as a whole give a bicapped trigonal bipyramidal structure.