CRYSTAL STRUCTURE OF SODIUM ETHYLENEDIAMINETETRA-ACETATOANTIMONY (Ⅲ) TRIHYDRATE Na[Sb(edta)]·3H_2O

<正> C10H18N2O11NaSb, Mr = 487. 0,orthorhombic, space group Pnna,a = 7. 047(1),b= 20. 915(3),c= 11. 152(2) A ,V= 1643. 7 A3,Z = 4,Dm= 1. 97,Dc = 1. 968gcm-3,λ(MoKa) = 0. 71073A ,μ=17. 7cm-1 ,F(000) = 968,final R=0. 040 for 1256 observed reflections. The [Sb(edta)]- ion has a diad symmetry, which differs from the structure of analog [Sb(Hedta)] in [Sb(Hedta)]·2H2O phase.     

SYNTHESIS AND CRYSTAL STRUCTURE OF THE MACROCYCLOOCTAONE, C_(28)H_(40)O_8

<正> INTRODUCTION. Macrocyclic compounds have attracked a lot of chemistsbecause of their diverse physical and chemical properties. There was anidealized method to synthesis macrocyclo polyketones compounds. Product(Ⅱ)was obtained by condensation reactions of furan with acetone followed byOxidative opening of furan rings in (Ⅰ) . The 2,2,7,7,12,12,17,17-octamethylcycloeicosan-1,3,6,8,11,13,16,18-octaone(Ⅲ) was obtained byhydrogenation of (Ⅱ) with 20% Pd carried on carbon.     

MOLECULAR AND CRYSTAL STRUCTURE OF (μ-4,4'-DIPYRIDYL)-BIS [DIAQUA-IMINODIACETATO-COBALT(Ⅱ)] TETRAHYDRATE {[CoNH(CH_2COO)_2(H_2O)_2]_2C_10H_8N_2}·4H_2O

<正> Mr=679.8,monoclinic, C2/m,a = 21.146(3), b = 12.613(1), c = 5.202(3)A,β= 93.26(2) ,V= 1385.1A3,Z = 2,Dx=1.63,Dm=1.64 g.cm-3 λ(MoKα)=0.71073A,μ=13.3cm-1,final R=0.036 for 1427 observed reflections. Bach cobalt atom in the title complex is in six-coordination environment with one bridging dipy ligand, two terminal H2O ligands and one tridentate ininodiacetic acid ligand. The "facial configuration" of the coaplex is compared with "the meridional one" found in corresponding Cu(II) complex.The bridge ligand dipy is tilted out of the coordination plane (N(1)-N(2)-O(1)-O(2) or N(1)-N(2)-0(1')-0(2')) by 47°,which may provide a spin-spin exchange pathway. Another possible magnetic exchange pathway is in the hydrogen-bonding linkage.     

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.     

CRYSTAL AND MOLECULAR STRUCTURE OF IPOHARDINE PICRATE, C_(15)H_(16)NO·C_6H_2N_3O_7

<正> INTRODUCTION. Ipomoea Hardwickii Hemsl (Ⅰ) belongs to Convolvulaceae, and its seed may be used as an anodyne. Ipoharine and Ipohardine were obtained by Reinickate method from the aqueous solution of Ⅰ. The structure of the title compound has been determined by X-ray crystal structure analysis. The structure of the cation (C_(15)H_(16)NO)~+ is reported here for the first time.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A TRITUNGSTEN CLUS-TER COMPOUND [W_3O_2(O_2CCH_3)_6(H_2O)_3]ZnBr_4·8H_2O

<正> C12H40O25Br4W3Zn, Mr = 1520. 71, monoclinic, space group P1, a = 10. 470(4) b=17. 669(6),c=14. 477(2) A ,α=99. 80(2),αB=101. 51(2),γ=99. 78 (4)°,V=1829A3,Z = 2,DX = 2. 66g/cm3,λ(MoKa) = 0. 71073A,μU= 146. 9cm-1,F (000) = 1408. Final R=0. 038,Rw = 0. 049 for 4088 independent observable reflections.     

CRYSTAL STRUCTURE OF [PdCl_2 (DMAF)_2]·C_7H_8

<正> C33H42 Fe2PdCl2N2 (dichloro-bis (dimethylaminomethylferrocene) pal-ladium(Ⅰ) toluene solvate) ,Mr = 755. 72,monoclinic,P21/c,a=7. 521(1),b= 11. 128 (2),c=19. 260(7) A ,β=91. 77(2)°,V=1611. 1A3,Z=2,Dc = 1. 56g·cm-3,D0 = 1. 58g·cm-3,μ=76. 3cm-1, The least-squares refinement gave a final R value of 0. 062 for 2192 observed reflections. The Pd atom is of squareplanar coordination. The ferrocene ligand of in DMAF has an approximately eclipsed conformation.     

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 Ba[Co(EDTA)]_2·6H_2O

<正> INTRODUCTION. The crystal structures of a number of metal complexes of ethlenediaminetetraacetic acid (EDTA) have been reported. As a versatile ligand, EDTA molecule is known to have several different coordination forms.     

Non-Isothermal Decomposion Kinetics of Supermolecule Compound [Eu(C_(10)H_9N_2O_4)(C_(10)H_8N_2O_4)(H_2O)_3]_2·phen·4H_2O

Europium(Ⅲ) compound with 2-oxopropionic acid salicyloyl hydrazone (C_(10)H_(10)N_2O_4,H_3L) and 1,10-phenan-throline (C_(12)H_8N_2,phen) has been prepared.A yellow prismatic crystal of the compound was obtained,and themolecule crystallized in the triclinic space group P-1.There are two 9-coordinated complex molecules in everystructure unit,where every Eu atom is coordinated by three water molecules and two tridentate C_(10)H_(10)N_2O_4 ligands,forming two stable pentacycles.The coordination polyhedron around Eu~(3+) was described as a single cap squareantiprism.In the crystal cell,there are one free 1,10-phenanthroline and four water molecules.The thermaldecomposition of the compound and its kinetics were studied by non-isothermal thermogravimetry.The Kissinger'smethod and Ozawa's method were used to calculate the activation energy value of the first-step decomposition.Thestages of the decompositions were identified by TG-DTG-DSC curve.The non-isothermal kinetic data were ana-lyzed by means of integral and differential methods.The possible reaction mechanism and the kinetic equationswere investigated by comparing the kinetic parameters.     

STRUCTURE OF MACROSPEGATRINE, [C_(40)H_(46)N_4O_3]Cl_2·3(H_2O)

<正> Mr=322.9, orthorhombic, P212121,a=19.867(4), b=15.793(3),c= 12.997(2)A, Z=4, Dc=1.23gcm-3,λ(CuKα)=1.5418A,μ=17.06cm-1, F(000)=1552. Final R=0.096 for 2764 unique diffractions with I≥3σ(I). Macrospegatrine obtained from the root of raurolfia Verticillata(Lour) Baill.f.rubrocarpa H. T.Chang.mss is a complex which involves double skeletons. It is a new alkaloid.     

CRYSTAL STRUCTURE OF Na_2Mo_2O_4(EDTA)·5H_2O

<正> Introduction. Mo(V)-EDTA compounds have been widely studied. Recently, the title compound has been investigated by magnetic anisotropic method. In order to provide a detailed information on its structure, the crystal structure, of the title compound has been determined.     

CRYSTAL AND MOLECULAR STRUCTURE OF K(C_3H_(12)N_2)_2(HV_(10)O_(28_).8.5H_2O

<正> Preliminary information. Vanadium compounds plays an important role in catalysis since they have a property of easily changeable oxidation states. As a part of our study on vanadium compounds, the crystal structure of the title compound is reported, which is prepared by the reaction of (C_3H_(12)N_2)_2-V_2O_7, NaVO_3 with KOH in an aqueous solution.     

SYNTHESIS OF LANSFORDITE MgCO_3·5H_2O AND ITS CRYSTAL STRUCTURE INVESTIGATION

Euhedral crystals of the uncommon low-temperature mineral lansfordite have been obtained by the synthetic method, and the crystal structure analysis has been accomplished correspondingly. The structural parameters and the general view of structure were presented for the first time. The results obtained show that the coordination configuration of two magnesium ions in the unit cell is octahedral arrangement and the coordination number is 6, but in two forms: one in the complex ion Mg(CO_3)_2(H_2O)_4~(2-) and the other in the Mg(H_2O)_6~(2+). There is only a CO_3~(2-) group in the structure, not three distinct groups as reported by Hill et al. previously based on the IR absorption spectrum research data. The authors of this paper believe that the exact chemical formula of lansfordite should be expressed as "Mg(H_2O)_6. Mg(CO_3)_2 (H_2O)_4", and MgCO_3-5H_2O is only a simple chemical expression.     

镍配合物[Ni(C_(10)H_8N_2)(C_7H_4O_5N_3)(H_2O)]·ClO_4的合成及晶体结构

含C=N结构的过渡金属配合物具有抗肿瘤、抗细菌、抗癌等多种生物活性[1].亚胺金属配合物大多具有优异的光电性能和功能性,而且可以通过扩充配合物中心离子的种类、调整自由配体的结构及取代基效应、立体效应和溶剂效应等使其具有结构多样性和性质可调变性,是合成大环配合物、自组装分子及分子器件的重要原料,日益受到物理、化学和材料科学家的关注[2-11].     

SYNTHESIS AND CRYSTAL STRUCTURE OF A SCHIFF BASE: 2-CHLORO-4-NITRO-N-(5-BROMOSALICYLIDENE) ANILINE (C_(13)H_8BrClN_2O_3)

<正> The title compound 2-chloro-4-nitro-N-(5-bromosalicylidene) aniline is preparedby condensation of 5-bromosalicylidehyde and 2-chloro-4-nitro-aniline. C_(13)H_8BrClN_2O_3, M_r=355.58, monoclinic space group P 2_1/n, a=7.4927 (7), b=16.389(5), c=11.013(5), β=98.2(6)°, V=1338.4, Z=4, D_c=1.764g.cm~(-3), MoK_a(λ=0.71073),μ=34. 569cm~(-1), F.(000)=704, room temperature,final R=0. 053, R_w=0. 057 for 1453 reflections with I≥3σ(I). A total of 2948 in-     

SYNTHESIS AND CRYSTAL STRUCTURE OF HETEROPOLY MOLYBDOSILICIC LANTHANIDE K_(10)H_3[Pr(SiMo_(11)O_(39))_2]·18H_2O

The intensity data of the title complex were collected at a low temperature of -90℃. Thecompound crystallizes in the monoclinic space group P2_1/n, a = 17.504(2), b = 27.323 (5),c = 21 .616(4)A, β= 104.49 (2)°, Z=4. The structure was solved by Patterson and Fouriertechniques and refined by least- squares to an R = 0.088 for 8320 independent reflections.The central Pr ion is bonded to eight oxygen atoms from two molybdosilicic heteropolyligands to form a square antiprism. The Pr- O average distance is 2.44 (2)A. Both molyb-dosilicic heteropoly ligands are of a defective α- Keggin structure.     

CRYSTAL STRUCTURE OF CK(C_(12)H_(24)O_6)]_2Pd(SCN)_4(H_2O)

<正> [K(C_12H_24O_6)]_2Pd(SCN)_4(H_2O),MT=963.59,monoclinic, P21/n,a= 11. 075(1),b= 12. 231(1),c= 15. 863(2) A ,β=93. 25(1)°,V=2145. 3A3,Z=2, Dc=1. 492gcm-3,λ(MoKa) = 0. 71073A μ=8. 64cm-1,F(000) = 996,final R=0. 045 for 1835 observable reflections. The Pd2+ ion coordinates with four S atoms from SCN- groups forming a regular square planar configuration. The K+ ion is surrounded by six ether oxygen atoms,one O atom from water molecule coordinated to two K+ions and one N atom from SCN- group to form a distorted hexagonal bipyramid. Two K atoms are linked with one Pd atom by two bridging SCN- groups forming a chain molecular array in the crystal.     

SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [Cu_2(CH_3COO)_4(C_8H_(11)NO)_2] · (C_6H_(11)NO)_2 · (C_8H_(12))

<正> SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [Cu_2(CH_3COO)_4(C_8H_(11)NO)_2] · (C_6H_(11)NO)_2 · (C_8H_(12)), where C6H11 = caprolactam, Mr = 900. 07, triclinic,space group P1, a = 11. 103(4), b= 11. 865(6), c=9. 912(3)(?), α=94. 85(4), β=115.20(2), γ=103. 25(4)°, V = 1125(2)(?)3, Z = l, Dx = 1. 33g. cm-3, λ(MoKa) = 0. 71069(?), T = 295K , μ = 10. 45cm-1, F(000) = 478, final R=0. 063 for 2098 observed reflections with I>3σ (I). The two Cu atoms in the molecule are held together by four carboxylate groups. Each Cu atom is bound in a square-pyramidal configuration to four carboxyl oxygen atoms and to the O atom of a caprolactam molecule.     

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