SYNTHESIS AND CRYSTAL STRUCTURE OF La（NO3）3（16—C—5）

<正> The title complex LaC11H22O14N3 (Mr = 559. 27) crystallizes in the monoclinic space group P21/c with a=14. 452(7) ,b=8. 260(2),c= 16. 641(8) A ,β= 90. 85(4)°, Z = 4, V=1986. 2(1) A3,Dc=1. 87g·cm-3, F(000) = 1112,μ(MoKa) = 22. 7cm-1. The final refinement converged with R=0. 036 and Rw = 0. 038 for 2996 observed independent reflectios. The average La-O(crown) bond length of 2. 683 A (2. 660-2. 701A)is shorter than that in La(NO3)3(15-C-5)(2. 694A).The distances between opposite O atoms (3. 47~4. 68A) indicate that the cavity of 16-C-5 in the complex is elliptic.     

CRYSTAL STRUCTURES OF La(NO_3)_3 COMPLEXES WITH BENZO-15-C-5 AND CYCLOHEXYL-15-C-5

<正> Complex La(NO3)3(Benzo-15-C-5) (C14H20LaN3O14, Mt= 593. 28) crystallizes in the orthorhombic,space group P212121 with a=8. 393(2),b= 16. 624(5), c = 17. 326(4) A ,V = 2417. 6(6) A3,Z = 4,DC= 1. 63gcm-3,F(000) = 1176, μ= 18. 7cm~1(MoKa). The final refinement converged with R = 0. 060 and Rw=0. 065 for 2223observed independent reflections. Complex La ( NO3 )3 ( Cyclohexyl- 15- C- 5 ) (C14H26LaN3O14,MT = 599. 34) is monoclinic,P21/n space group with a=9. 917(4),b= 13. 667(5),c=16. 763(5)A,β=104. 33(3),V = 2201(1)A3,Z=4,Dc=1.81gcm-3, F(000) = 1200,μ= 20. 4cm-1(MoKa).The final refinement converged with R=0. 048 and Rw=0. 036 for 1495 observed independent reflections. In the two complexes,the La (Ⅲ) ion is 11-coordinate and bonded to six oxygen atoms from three bidentate nitrate groups and five oxygen atoms from the crown ether. The average bond lengths of La -O (crown) and La -O(nitrate)are 2. 68 and 2. 61A for La(NO3)3(Benzo-15-C-5) ,re-snectively and 2. 71 and 2. 62 A for La(NO3)3(Cyclohexyl-15-C-5) re     

SYNTHESIS AND CRYSTAL STRUCTURE OF THE LANTHANIDE COMPLEX WITH MIXED LIGANDS [Pr (CH_3COO)_2(NO_3)(Phen)]_2

<正> [Pr(CH3COO)2(NO3)(Phen)]2, Mr = 1002. 41. The crystal is monoclinic, space group I2/m, with a = 11. 725(5), b = 12. 269(5), c=12. 732(4) A, V = 1792(2)A3,β=101. 88(0)°. Z = 2, Dc=1. 86g/cm3,μ(MoKa) = 27. 5cm-1, F (000) = 984. The structure was solved by Patterson method and Fourier syntheses, and refined by full matrix least-squares method to R = 0. 033 for 1660 observed reflections with I>3σ(I). The molecule of the complex is a dimer and each praseodymium atom is eight-coordinated in a distorted square antiprism geometry.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Ta_3(Te_2)_6

<正> Ta3(Te2)6, Mr = 2074. 04, tetragonal, P4/ncc, a = 9. 204(1) A , c=20,401(8) A, V=1728. 3 A 3, Z = 4, Dc = 7. 97g/cm3, λ(MoKa) = 0. 71073 A . μ= 386, 3cm-1,F(000) = 3372, T= 296K , R= 0. 027, Rw = 0, 029 for 493 observed unique reflections. The structure is composed of infinite [TaTe4] chains along the e axis. In these chains, the Ta sequences distort in such a way that linear Ta, clusters are formed.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Nb3（Se2）6I

<正> Nb3(Se2)6I,Mr = 1353. 1, tetragonal, space group D64h-P4/mnc, a= 9. 45(1), b = 9. 45(1) , c=19. 08(3)(?), V = 1705. 6(9)(?)3, and Z = 4, Dc=5. 27g/cm3. Final R = 0. 045 and Rw = 0. 053 for 881 independent reflections with I> 3σ(I). In the structure of Nb3(Se2)6I, the Nb(Se2)4 units are almost regular rectangular antiprism, which are packed in chain forms along c axis with the I (0) atoms between these chains.     

[（t—BuCp）2GdCl]2的合成及晶体结构

Wayda最近报道,无水氯化稀土LnCl_3和叔丁基环戊二烯钠(t-BuCp)Na进行交换反应时,由于歧化反应得不到单取代或双取代的轻稀土氯化物衍生物,只能得到中稀土和重稀土氯化物衍生物,并且没有测得这些配合物的晶体结构。我们采用提高反应温度和延长反应时间,使交换反应进行完全,有效地避免了歧化反应的发生,成功地分离到了单取代或双取代的叔丁基环戊二烯基轻稀土氯化物。并测得(t-BuCp)_2LnCl·nTHF(Ln=Pr,n=2;Ln=Yb,n=1)     

SYNTHESIS AND CRYSTAL STRUCTURE OF Eu[（CH3O）2PO2]3

<正> The title complex has been synthesized and characterized by elementary analysis,FT-IR and Raman spectra. The crystal and molecular structure was determined by X-ray diffraction analysis. The crystal of this complex C6H18O12P3Eu(Mr = 527. 08) is monoclinic with space group P21/c and cell parameters a= 10. 418(2) ,b= 16. 596(6) ,c =10. 766(2) A ,β=111. 67(2)°,V=1729. 8(8) A3 and Z=4. Dimethyl phosphate an-ions coordinate with europium ions through double O-P-O bridges to form a special network of rings-linking-rings. The local coordination geometry of Eu is a slightly distorted octahedron.     

(C5H7S2)2[Cu3I5]的合成和晶体结构

我们曾经对二硫代乙酰丙酮和多种金属离子的配合反应进行了系统的研究.在成功合成(C_5H_7S_2)_2[CuBr_3]的基础上,最近我们试图用类似方法合成(C_5H_7S_2)[CuI_3].但对产物晶体的X 射线衍射分析结果却表明,所得到的化合物的分子式为(C_5H_7S_2)_2[Cu_3I_5].[Cu_3I_5]~(2-)是以[CuI_3]配位三角形和两个相邻[CuI_4]配位四面体连接的无限链状配合阴离子形式存在.     

SYNTHESIS AND CRYSTAL STRUCTURE OF （C5H5）2Ti（o—NHPhC6H4CO2）2

<正> Cp2Ti(o-NHPhC6H4CO2)2, Mr = 602. 54, space group C2/c, a = 33. 77(2), b = 12. 611(6), c=14. 486(9) A ,β=103. 28(4)°,V = 6004(5) (?)3,Z = 8, Dc= 1. 33gcm-1, MoKa(λ=0. 71069(?)) radiation, μ = 3. 21cm-1, F(000) = 2512e, R = 0. 066, Rw= 0. 085 for 2511 radiations. The Ti atom in the molecule is coordinated by two C5H5 groups and two monodentate carboxyl ligands in a distorted tetrahedral geometry with the bonds in the range of Ti-C = 2. 334 - 2. 41(?) ; Ti-O = 1. 914(5) and 1. 919(5)(?);and the bond angles O-Ti-O = 91. 7(2)°; (cent-C5H5)-Ti-(cent-C5H5) = 135. 9(6)°.     

SYNTHESIS AND CRYSTAL STRUCTURE OF [(PPh_3)_3(Cu_3S_3MoBr)O]-0. 5CH_2C1_2

<正> [(Ph3P)3 (Cu3S3MoBr)O] 0. 5CH2C12, Mr = 1308. 00, monoclinic, P21/c,a=11. 831(3),b = 28. 471(8),c=19. 232(5) A ,β= 101. 05(3)°,V = 6358 A3,Z = 4,DC=1.37 g/cm3,F(000) = 2620,μ(MoKa) = 20. 47 cm-1. Final R=0. 085 for 4271 observede reflections. The core [Cu3S3MoBr] has a distorted cubic configuration. Two dichloromethane molecules distribute statistically in a unit cell.     

SYNTHESIS AND CRYSTAL STRUCTURES OF {Pr[(C_2H_5O)_2POO]_3}_n

The synthesis, characterization and crystal structure of rare earth coordination complex of {Pr[(C_2H_5O)_2POO]_3}_n has been studied. It is triclinic with space group P1 in a unit cell of dimensions a=11.788(5), b=12.536(3), c=10.262(2.) , α=112.21(2), β=93.01(3), γ=109.94(3)°; V=1290.9(8)~3, Z=2. As shown in Fig. 1, each Pr atom is connected with other two Pr atoms through three "O-P-O" bridging groups to form a long chain polymer. The coordination number of Pr is six. The six coordinated O atoms form an octahedron. The average bond distance of Pr-O is 2.333 A. The complex has been also studied by infrared spectroscopy and thermal analyses.     

[Tb(CH_3COO)_3(H_2O)_2]_2的合成及其结构测定

2-羟基吡啶、希土高氯酸盐和乙酸钴在乙腈中反应,制备了九配位化合物[Tb(CH_3COO)_3·2H_2O]_2该晶体为三斜晶系,P~(?)空间群,其晶胞参数为a=8.870(4)(?),b=9.247(1)(?),c=10.586(1)(?),α=65.13(1)°,β=64.43(2)°,γ=62.16(4)°,V=665.97(?)~3,Z=1,F(000)=394。测定了配合物的红外光谱。讨论了它的生成机制。     

TRINUCLEAR BASIC CARBOXYLATE COMPOUNDS OF TRANSITION METALS PART 1. SYNTHESIS AND CRYSTAL STRUCTURE OF {Fe_2MnO(EtCO_2)_5(H_2O)_4}·NO_3

<正> The title complex crystallizes in the tetragonal system,space guoup I 4 with α = b=22. 41(1), c=12. 920(3) A. Mr = 682. 06,V = 6488. 5A3,Z=8,Dc= 1. 396g/cm3,F(000) = 2808,final R=0. 098 for 2668 independent reflection with Ⅰ > 3σ( Ⅰ ). This complex was Shown to contain two Fe(Ⅲ ) and one Mn( Ⅱ ) at the apices of an approximately equilateral triangle with a μ3-O bridge. The Mn (Ⅱ)atom and one Fe (Ⅲ )atom are each octahedrally coordinated by six oxygen atoms,while the other Fe atom coordinated by five oxygen atoms to form a square pyramid. The μ3-O is in the centre of the Fe2Mn triangle with the Fe(1)-O, Fe(2)-O and Mn-O distances of 1. 89(1), 1. 90(1) ,and 1. 91(1) A ,respectively. The IR spectrum was also studied.     

四核钼簇合物的配体取代反应及产物Mo_4S_4(μ-OAc)_2(dtp)_4的晶体结构

标题化合物(Ⅰ)经由Mo_4S_4(μ-dtp)_4(Ⅱ)[dtp=S_2P(OEt)_2]和Ni(OAc)_2反应而得。(Ⅰ)晶体属单斜晶系,空间群P2/c,a=13.176(4),b=11.699(3),c=18.526(4)(?),β=116.11(3)°,V=2564(3)(?)~3,Z=2,D_c=1.776g·cm~(-3)。晶体结构由直接法解出,最终偏离因子R=0.085。本文结果表明,可由已知的四核钼簇合物经过配体置换反应,合成得到其簇骼中心[Mo_4S_4]保持不变并具有-OAc作为桥式配体和-dtp作为端基配体的混合配体类立方烷[Mo_4S_4]簇合物。     

SYNTHESIS AND CRYSTAL STRUCTURE OF Mo_20_2S_2(Py)_4(Mo0_4)

<正> Introduction. A series of trinuclear molybdenum clusters has been synthesized and identified. Most of them have almost the sameMo-Mo distance. We have synthesized another kind of trinuclear molybdenum complex which has different Mo-Mo distances and can be comsidered as composed of the complex (Mo_2O_2S_2(py)_4)~2+ and the molbdenic ion (MoO_4)~2-. This paper reports the synthesis and structure of the title compound.     

镨,钕量法测定有机磷化合物中的磷含量

有机磷化合物中的磷含量可以先将样品放入氧瓶燃烧分解,再以Pr(NO_3)_3或Nd(NO_3)_3作为PO_4~(3-)的沉淀剂,并用EDTA回滴过量的Pr~(3+)或Nd~(3+)来测定。文中还介绍了消除氟,硫,硼干扰的简单方法。测定误差为±0.20%。     

SYNTHESIS AND CRYSTAL STRUCTURE OF AZACROWN (2, 2) DINITRATE [C_(12)H_(28)O_4N_2] (NO_3)_2

<正> [C12H28O4N2](NO3)2, Mr = 388. 45, monoclinic space group P21/ n,a = 7. 811(2), b = 10.626(4), c= 11. 823(6) A , β=106.51(3)°, Z = 2, Dc = 1.37 gem-3, V = 940. 8(7) (?)3 F(000) = 416, μ(MoKα) =1. 3 cm-1, R =0. 044 for 1373 reflections. The structure contains prdtonated azacrown [H2(2,2)]2+ and two (NO3-) which are bridged by four hydrogen bonds O(nitrate) ...H-N(crown). The ion [H2(2,2)]2+ in the title crystal lies on the crystallographic center of symmetry. There is half a [H2(2,2)]2+ and one NO3- in an asymmetric unit.     

SYNTHESIS AND CRYSTAL STRUCTURE OF [C8H8NdCl（THF）2]2

<正> The title complex was prepared from the reaction of NdClLi0.3 and C8H8, its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/c with cell dimensions o = 11. 819(3), 6=12.651(3), c=13. 478(3)A, β=122.99(2)°, Mr = 856. 00, Z = 2, Dc=1. 68g/cm3, F(000) = 636. 89, V = 1690. 33A3. The structure was solved by direct methods and Fourier techniques. Least squares refinement on the basis of 1842 observed reflections led to final R = 0. 038 and Rw = 0. 040. The molecule is a dimer of C3H8NdCl(THF)2 bridged by two Cl atoms with Nd -Cl bond lengths of 2. 832(2) A and 2. 917(3)A.     

CRYSTAL STRUCTURE OF GdCl_3(DIMETHOXYETHANK)_2

<正> C8H2oCl3GdO4,Mr=443.80,monoclinic, space group P21/c, a=11.442 (3),b= 8.849(2), c= 15.575(5)A,β=104.8l(2)° ,V=1521.9(7)A3,Z= 4, DC = 1.94 g/cm3,λ(MoKα) =0.71069A,F(000)=860. The structure was solved by Patterson and Fourier techniques and refined by least-squares nethod to a final conventional lvalue of 0.051 (Rw=0.054). The central ion Gd(III) is bonded to three chlorine atoms and four oxygen atoms froa two dimethoxye-thane molecules to form a distorted pentagonal bipyramid. The Qd-Cl distances are in the range of 2.460-2.628A (average 2.571A). The Gd-O distances are in the range of 2.408-2.493A (average 2.458A).     

SYNTHESIS AND CRYSTAL STRUCTURE OF POLYMERIC STRUCTURE CONFLEX [Ag_2(C6H5CS_2)_2]_n

<正> Structural units Ag2(C6H5CS2)2,in which the distance between the unbridged silver atoms is only 2.890A, are connected by Ag...S interactions of neighbouring units along a and b axes to form a nonmolecular poly-meric structure [Ag2(C6H5CS2)2]n.