Syntheses and Crystal Structures of （PySe）2 and Bi2（PySe）6（HPySe=2-Pyridineselenol N-Oxide）

The title compounds(PySe)2 1(HPySe=2-pyridineselenol N-oxide,(PySe)2= bis(2-pyridine-N-oxide) diselenide) and Bi2(PySe)6 2 were prepared by the reaction of 2-bromine-N-oxide with NaHSe and Bi(NO3)3·5H2O with HPySe,and the crystal structure of 2 was studied.Compound 2 crystallizes in the monoclinic space group P21/n with a=9.840(2),b=10.204(2),c=18.395(2),β=102.926(2)°,V=1800.0(5)3,Dc=2.2687 g/cm3,Z=2,the final R=0.0319 and wR=0.0646.The Bi atoms are coordinated by four selenium and four oxygen atoms from four PySe ligands to form a slightly distorted four-column geometry.     

CRYSTAL STRUCTURE OF (C_5H_9C_5H_4)_3Er_4(μ_2-Cl)_6(μ_3-Cl)(μ_4-O)-(THF)_3

<正> The crystal of (C5H9C5H4)Er4(μ2-Cl)6(μ3-Cl)(μ4-O)(THF)3 belongs to triclinic space group P1, with a = 11. 909(4), b = 15.343(5), c=15. 619 (4)(?), α=104. 18(2), β=98. 81(3), γ= 111. 06(2)°, V = 2486(1)(?)3, Z = 2, Dc = 2. 07g/cm3, λ(MoKα) = 0.71073(?), μ= 73. 4cm-1, F(000) = 1476, Mr=1549. 25. The structure was solved by Patterson and Fourier techniques and refined by block diagonel least-squares method to final R = 0. 078 and Rw = 0. 084 for 5594 reflections with I≥1. 5σ(I). The results revealed that the complex is composed of four Er atoms bridged by seven Cl and one oxygen atoms with three of the Er atoms bonded each to a cyclopentylcyclopentadienyl group, and one Er atom, bonded to three THF. The Er atoms constitute a pseudo-tetrahedron.     

PREPARATIVE AND STRUCTURAL STUDIES ON THE SUPERCONDUCTING PHASE YBa_2Cu_3O_(7-d)

Reasonably homogeneous samples were obtained by following the formula Y_(0.334)Ba_(0.666)CuO_(3-y) andusing citric acid as a complex-forming agent to improve the dispersion of the metal oxides. We havealso found that the variant condition in preparative procedure leads to variant deviation from tetrago-nality and that more pronounced deviation gives better superconducting properties. The crystal structure determined from X-ray powder diffraction diagrams confirms the stoichiom-etry of the metal ions and gives the positions of the oxygen atoms. The orthorhombic or pseudo-tetragonal unit cell with a=3.893, b= 3.813 and c= 11.687 A contains YBa_2Cu_3O_7. It is composed ofthree perovskite cubes with three copper atoms at their corners, the two barium atoms at the centers ofthe top and bottom cubes, and the yttrium at the center of the unit cell. The oxygen atoms sit on centersof cube edges. The positions (0 0 1/2) are vacant. The vacancies represented by (0(1/2)0) cause the ar-rangement of atoms to lose tetragonal symmetry, and have far-reaching effect for this phase. The yttriumand barium atoms are coordinated in a cuboctahedron respectively with four equatoria oxygen atoms at(0 0 1/2) and two at (0 1/2 0) removed. In the light of bond valence theory we can infer from the in-teratomic distances Y-O, Ba-O and Cu-O that the occupancy of the oxygen atoms at (1/2 0 0) is wellbelow unity while the positions (0 0 1/2) are vacant, the formula of the phase is YBa_2Cu_3O_(7-d), thefraction of Cu(Ⅱ) and (Ⅲ) for the set of copper at (0 0 0) is respectively d/0.5 and (1-d/0.5), and0.2相似文献   

Crystal Structure of [Et_4N][Sm(S_2CNEt_2)_4]

The crystal structure of .[Et4N][Sm(S2CNEt2)4] was determined by X-ray diffraction technique. The crystal crystallizes in monoclinic system, space group P21/n with a= 1. 1695(3), b=2.0821(6), c=1.7420(7) nm, β=99. 79(3)°? Z=4, Dc= 1. 39 g/ cm3, μ(Mo/KTσ) = 18. 4 cm-1, F(000) = 1812. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R of 0. 053 for 3116 (Ⅰ> 3σ- (Ⅰ)) reflections. Each asymmetric unit contains two ions [Sm (S2CNEt2)4]-1 and [Et4N] +1, having distance between central atoms N5 and Sm3+ to be 0. 6522 nm. The atom Sm is coordinated by eight sulphur atoms. The Sm-S distance lies in the range of 0. 285-0. 290 nm with an average of 0. 288 nm.     

CRYSTAL AND MOLECULAR STRUCTURE OF MOLYBDENUM COM-PLEX MoO_2Cl_2(C_4H_3OCOOH)_2

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction method. The complex crystallizes in the mono-clinic space group P21/n with a = 10. 306 ( 3) , b = 10. 161 (2), c = 14. 798 ( 4) A . β= 108. 52(2)°, V= 1469. 4(6)A3,Z= 4. The structure was solved by direct methods. Least-squares refinement converged to a final value of R = 0. 043 and Rw= 0. 040 for 1237 reflections. The molybdenum (Ⅵ) ion is bonded to two chlorine atoms, two oxo atoms and two oxygen atoms from two monodentately and weakly coordinated carboxyl groups of molecules C4H3OCOOH, forming a octahedron. The Mo-O distances are in the range 1. 66 - 2. 39A ,the Mo-Cl distances fall in the range 2. 33-2. 34A.     

CRYSTAL STRUCTURE OF ORGANOLANTHANIDE COMPLEX [Li~+(DME)_3]_2[(CpNd)_4(μ_2-CH_3)_2(μ_4-O)(μ_2-Cl)_6]~(2-)

<正> The crystal and molecular structure of [Li+(DME)3]2[(CpNd)4 (μ2-CH3)2(μ4-O) (μ2-Cl)6]2~was determined from single crystal X-ray diffraction. The complex crystallizes in the monoclinic space group P21/n with lattice parameters a= 14. 614(5), b= 18. 683 (5),c= 24. 595 (6) A, β = ,91-85(2)°, V = 6712(3) A3,2 = 4,DC = 1. 63g/cm3,F(000) = 3256,Mr=1650. 85. The structure was solved by direct methods and Fourier techniques and refined by least-squares to a final R=0. 047,RW = 0. 049 for 3761 with I>3σ(I). The result revealed that the anion [(CpNd)4(μ4-O) (μ2-Cl)6(μ2-CH3)2]2- is composed of four neodymium (Ⅲ) atoms bridged by six Cl atoms, two methyl groups and one oxygen atom, and every Nd is bonded to a cyclopentadienyl group. The four Nd atoms form a distorted tetrahedron. The cations are composed of two Li+(DME)3 with average Li-O distance of 2. 120(40) A.     

CRYSTAL AND MOLECULAR STRUCTURE OF BINUCLEAR Ni(Ⅱ) COMPLEX--CNi(OC_6H_4CHNCH_2CH_2OH) (CH_3COO) (H_2O)_2

<正> The title complex crystallizes in the monoclinic space group P21/n,with a = 9. 509(2),b=17. 614(6),c=15. 013(3)A ,β=95. 21(1)°,V = 2504. lA3,Mr = 599.91,Z = 4, Dx= 1. 59g/cm3, μ= 15. 66cm-1F (000) = 1248. The structure was solved by direct method and the final R=0. 060. The crystal consists of discrete molecules with symmetric center at the center of the four-member ring consisting of two Ni atoms and two 0 atoms.     

CRYSTAL STRUCTURE OF [(C_4H_9)_4N][O_2Mo~(VI)S_2Cu~Itu](tu=(NH_2)_2CS)

<正> Crystal and molecular structure of [(C4H9)4N][O2MoS2Cutu] (tu-thiourea) has been determined by X-ray diffraction technique. The crystal is monoclinic, space group P21/n, with a = 11.871(4), b=13.920(2), c= 15.814(11)A;β= 90.22(4)°,V=2613.2A3,Z = 4, DC= 1.459, Do = 1.46g/cm3. The final R and Rw are 0.049 and 0.056, respectively. The title complex has a rhombic planar MoCu(μ-S)2 core with Mo-Cu distance of 2.647A.The Ho atom is tetrahedrally coordinated by two 0 atoms and two u-S atoms. The Cu-S(tu) bond length of 2.191 A is significantly shorter than the Cu-S(bridge) in analogues.     

TRINUCLEAR BASIC CARBOXYLATE COMPOUNDS OF TRANSITION METALS PART 2. SYNTHESIS AND CRYSTAL STRUCTURE OF [Fe_3O (EtCO_2)_3(MeCO_2)_3(H_2O)_3]NO3·H_2O

<正> The title complex crystallizes in monoclinic system,space group C 2/m with α=19. 870(5),b=13. 070(2),c=18. 246(4)A ,β=134. 32(1)°,Mr = 707. 88, V=3390. 0A3.Z = 4,DC=1. 387g/cm3,F(000) = 1468,final R=0. 066 for 2244 independent reflections with Ⅰ >3σ(Ⅰ). The cation was shown to contain three Fe (Ⅲ) atoms at the apices of an equilateral triangle with a 3-O bridge.The Fe (1)-(μ3-O)and Fe(2)-(μ3-O) distances are 1. 907(6) and 1. 87(1) A , respectively. And mixed ligands of acetato and propionyloxy lato are bridged to each pair of the Fe(Ⅲ) atoms.     

CRYSTAL STRUCTURE OF (NH_4)_(11)[Na(H_2O)_2P_4W_(14)O_(58)] ·12H_2O

<正> (NH4)11[Na(H2O)2P4W14O58)·12H2O, Mr = 4099. 39, triclinic, space group P1, a = 14. 376(2), b = 19.861(9), c=13. 010(3)(?) , α=104. 68(2), β=91. 37(1), γ= 104. 05(2)°, V = 3471. 1 (?)3, Z = 2, Dc=3. 922g/cm3, μ (MoKα) = 238. 274cm-1, F(000) = 3664, R = 0.0510, Rw = 0. 0665 for 9260 observed reflections with I> 3σ(I). The polyanion [Na(H2O)2P4W14O58]11- consists of two PW7O29 subunits anisostructurally, two linkage phosphorous atoms and one sodium ion with two water ligands as well. The geometries of tungsten atoms within these two subunits are almost the same as those in K12P4W14O58· 21H2O[2]. The four phosphorous atoms are in PO4 coordinations. The sodium ion locates nearly at the center of the polyanion, and is coordinated by two water molecules, five oxygen atoms of the anion and one phosphorous atom with Na-P = 3. 053(3) (?). Due to the presence of the sodium atom, the interactions between oxygen and tungsten atoms in the polyanion are somewhat weakened.     

Crystal Structure of [Cd（pom）2Cl2]

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｃｄ（ｐｏｍ）_２Ｃｌ_２］ＷｕＷｅｎ－Ｓｈｉ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，Ｈｕａ－ｑｉａｏＵｎｉｖｅｒｓｉｔｙ，Ｆｕｊｉａｎ，Ｃｈｉｎａ，３６２０１１）ＤｏｎｇＭｅｉ－Ｂｉｎ；ＬｉＳｏｎｇ－Ｘｉａ...     

Synthesis and Crystal Structure of a One-dimensional Infinite Chain Organotin Complex [(n-Bu)_3Sn(OCOC_5H_4NO)]_n

1 INTRODUCTION Organotin esters of carboxylic acid are widely used as biocides and fungicides and as homogeneous cata- lysts in industry[1~3]. In recent years, the pharmaceu- tical properties of carboxylic acid have been investi- gated for the antitumour activity[4~6]. In general, bio- cidcal activities of organotin complexes are greatly influenced by the molecular structures and coordina- tion numbers of the tin atom[7, 8]. It is revealed that organotin complexes containing carboxylate l…     

镧系金属高氯酸盐与1.8-萘啶氮氧化物配合物的合成、性质和结构

本文合成了镧系金属高氯酸盐与1,8-萘啶氮氧化物形成的Ln(C8H6N2O)4(ClO4)3(Ln=Sm-Lu)的固体配合物. 进行了元素分析、红外光谱、差热-热重分析和摩尔电导测定, 并作了Eu(ClO4)2与1,8-萘啶氮氧化物配合物的X射线单晶结构分析. 结果表明Eu^3^+离子与4个配体的氧原子和氮原子配位, 配位数为8.     

Synthesis and Crystal Structure of Fe（aapo）2Cl3 （aapo=2—Acetylamino Pyridine N—Oxide

1INTRODUCTIONComplexesofpyridineN-oxideligandshavereceivedmoreandmoreattention,andwehavereportedsomeofthemcontainingadonorsubstituteatthe2-positioninanattempttobroadentherangeofpyridineN-oxidecomplexes[1,2].MostcrystalstructuresofpyridineN-oxidesreportedareaboutdivalenttransitionmetalionsM(Ⅱ)[1～4],withonlyaveryfewontrivalenttransitionmetalionsM(Ⅲ)[5].Asthecontinuingworkofsystematicresearch,herewewillpresentthesynthesisandstructureofthetitlecompound.Toourknowledge,itisthefirstexamplet…     

氧化-4-吡啶甲酸桥联的一维链状三丁基锡配合物的合成与晶体结构

利用双三丁基氧化锡与氧化-4-吡啶甲酸(HOCOC5H4NO)以物质的量比1∶2反应,合成了有机锡配合物[Bu3Sn(OCOC5H4NO)]n。通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征,用X射线单晶衍射测定了它的晶体结构。结果表明,该配合物晶体属单斜晶系,空间群为C2/c,晶胞参数a=2.002 8(9)nm,b=1.224 7(6)nm,c=1.913 6(12)nm,β=119.145(6)°,Z=8,V=4.166(4)nm3,Dc=1.365 g.cm-3,μ=1.239 mm-1,F(000)=1 760,R=0.052 9,wR=0.192 1,GOF=1.013。在配合物中锡原子由氧化-4-吡啶甲酸桥联为五配位的畸变的三角双锥构型。氧化-4-吡啶甲酸配体中N-O基团中的氧原子和另一配体中的羧基氧原子与中心锡原子配位,形成无限一维链状有机锡配合物。该配合物具有良好的热稳定性和较高的抗肿瘤活性。     

铜配合物[Cu(2,2''''-bipy)(pydco)(H2O)]·4H2O的合成与晶体结构

配合物[Cu(2,2’-bipy)(pydco)(H2O)].4H2O(2,2’-bipy=2,2’联吡啶,pydco=氮氧化-2,6-二甲酸吡啶)的结构由X-射线测定,配合物属三斜晶系,P墿空间群,晶胞参数:a=0.68120(14),b=1.1850(2),c=1.2554(3)nm,α=86.06(3),β=81.60(3),γ=86.16(3)°,V=0.99854(4)nm3,Z=2。2,2’联吡啶提供两个配位原子(N1,N2),氮氧化-2,6-二甲酸吡啶提供两个配位氧原子以及一个配位水提供一个氧原子参与了配位,中心Cu(II)离子是一个畸变的四角锥结构。有趣的是,配合物的结晶水组成了一条条的水带,配合物分子正是由这些水带中的氢键连接在一起的。     

Synthesis and Structure of bis(μ-2-aminopyridine N-oxide)-bis[dichlorocopper(II)]

1 INTRODUCTIONMany complexes of 2-aminopyridine N-oxide (apo) have been characterized by infrared spectra, X-ray powder diffraction spectra, and by magnetic measurements and electronic spectra at liquid nitrogen temperature, but very few of them are their crystal X-ray studies[1~3]. Recently, a number of bridged binuclear copper (II) complexes have been reported, some of which have important potential applications in bioinorganic chemistry and materials[4~6]. Particularly, the complexes …     

Synthesis and Crystal Structure of a New Chain Coordination Polymer [Cu（inio）2（H2O）]∞ （Inio = Isonicotinic Acid N-Oxide）

1 INTRODUCTION With deep studies on the complex biology system and syntheses of new functional complexes, people have paid more and more attention to the polynuclear complexes. In the construction of one to three dimensional frameworks, multi-dentate ligands are usually used to bridge the metal centers to form polymeric structures[1, 2]. The isonicotinic acid N-oxide can function as a good mono-dentate ligand[3～8] through one oxygen atom from the group of -NO or carboxyl, and the dep…     

Synthesis and structure of two lanthanide complexes with isonicotinic acid N-oxide (HL): [Ln(L)2(H2O)4]n·(NO3)n·n(H2O) (Ln = Sm or Tb)

Two new lanthanide complexes of isonicotinic acid N-oxide (HL), namely [Ln(L)₂(H₂O)₄]_n·(NO₃)_n·n(H₂O) for Ln = Sm or Tb, have been synthesized and characterized by spectroscopic and crystallographic methods. IR spectra suggest that isonicotinic acid N-oxide acts as a O,O′-bidentate ligand, the N-oxide group as well as the nitrate group are not involved in coordination. Single crystal analyses have shown that both complexes are isomorphous, where the Ln(III) centers are eight coordinated by four O atoms of four water ligands and other four O atoms of two isonicotinic acid N-oxide ligands. The carboxylate groups are only involved in the bidentate syn–syn bridging mode into infinite chains. Hydrogen bonds between aqua ligands, lattice molecules, nitrate and N-oxide groups are formed giving a three-dimensional network.     

First structural authentication of third-sphere coordination: [p-sulfonatocalix[4]arene]5- as a third-sphere ligand for Eu3+

Abstract

The central feature of the complicated structure of Na[Eu₃(p-sulfonatocalix[4]arene)₂(OH₂)18(ONC₅H₅)₃]·14 H₂O is the coordination sphere of one of the three independent europium atoms. Its first coordination sphere consists of seven water molecules, the oxygen atom of a pyridine N-oxide molecule, and a sulfonate oxygen atom from one of the two independent calix[4]arenes. The second-sphere coordination consists of the second calix[4]arene which is bound to the coordinated pyridine N-oxide via hydrophobic interactions, and a second pyridine N-oxide which is hydrogen bonded to a coordinated water molecule. The third-sphere coordination consists of the binding of the second-sphere coordinated pyridine N-oxide to the cavity of the first-sphere coordinated calix[4]arene. Na[Eu₃(p-sulfonatocalix[4]arene)₂(OH₂)₁₈(ONC₅H₅)₃]·14 H₂O crystallizes in the monoclinic space group P2₁/c with a = 20.973(2), b = 18.678(2), c = 29.502(4)Å, β = 109.19(1)°, and D_c = 1.74 g cm^?3 for Z = 4. Refinement based on 10,043 observed reflections led to a final R value of 0.091.