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.     

Nickel Group Complexes With Thiolate or/and Phosphine Ligands.Synthesis and X-ray CrystalStructure of 〔Ni_2(pdt)_2 (PEt_3)_2〕

IINTRODUCTIONTransitionmetalcomplexesblendingbothphosphineandthiolateligandshavereceivedattentioninrecentyears,notonlyduetotheirvariationingeometricandelectronicstructuresandproperties,butalsobecauseoftheirapplicationforhomogeneousorheterogeneouscatalyticfunctionsll--33.TheearlierstudiesonthisprojeclweremainlyinthesynthesesofsimplecomplexesandsurveyoftheirpropertiesandEfewhavebeenstructurallyanalyzed"--".Althoughsomeresearchgroupscarriedculpreliminaryworkonnickelgroupcomplexeswithphosphin…     

CRYSTAL STRUCTURE OF ERBIUM (Ⅲ) COMPLEX WITH 1,2,4-BENZENETRICARBOXYLIC ACID

<正> [ErC6H3(COO)3(H2O)3] ·H2O, Mr = 446. 5, orthorhombic, space group P212121, a = 6. 072(1), b = 9.530(2), c=19. 844(4)(?) , 7 = 1148.3 (4)(?)3, Z=4, Dc = 2.58g/cm3, F(000) = 852, μ(Mo Kα) = 76. 4/cm. The final R = 0. 044 and Rw = 0. 046 for 1570 observed unique reflections with I> 3σ(I). The erbium ion is nine-coordinated by six oxygen atoms from four 1, 2, 4-benzenetri-carboxylates and three from three aqua molecules, forming a mpnocapped square an-tiprism. The Er -O distances fall in the range of 2. 31 - 2. 66 A with an average of 2. 42(?). The structures of title complex and [13] show a similar three dimensional polymeric network.     

CRYSTAL STRUCTURE OF A TRINUCLEAR COBALT COMPLEX Co_3(bdt)_3(PBu_3~n)_3 · ~2CH_2C1 (bdt = S_2C_6H_4~2- ) WITH MIXED o-BEN-ZENEDITHIOLATE AND TRIBUTYLPHOSPHINE LIGANDS

<正> Co3(S2C6H4)3{P(C4H9)3}3 ·2CH2Cl2, Mr = 1373. 45, mono-clinic, space group P21/c, a = 16. 110(5), b=36.313(10), c=13. 502(5) A , β= 105. 69(4)% V=7604. 4 A3, Z = 4, Dc = 1. 20 g. cm-3, μ=10. 03 cm-1, and F (000) = 2990. R(Rw) is 0. 086(0. 091) for 4559 observed unique reflections. The three cobalt atoms in the complex form an isosceles triangle with an average Co -Co bond distance of 2. 504(5) A. The average values of Co - S and Co - P bond distances are 2. 271(7) A , and 2. 198(8) A , respectively.     

STRUCTURE OF（C6H5COCHCOC6H5）SmI2（THF）3

<正> (C6H5COCHCOC6H5)SmI2(THF)3,Mr= 843. 75,triclinic space group P1,a=13. 274(3),b=9. 886(3),c= 12. 526(4)A,a= 110. 89(3),B=93. 98(2),y=85. 16(2) ,V=1528. 9(8)A3,Z=2,Dc=1. 83g/cm3, (MoKa) = 0. 71069A,u= 40. 3cm-1,F(000) - 810. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R value of 0.082(Rw= 0. 083). The central Sm(III) ion is coordinated by two iodine ions, two oxygen atoms from C6H5COCHCOC6H5 and three oxygen atoms from three THF molecules to form a distorted pentagonal bipyramid. The Sm-I distances are 3. 103 and 3. 092 A ,The Sm-O (O atom from C6H5COCHCOC6H5) distances are 2. 273 and 2. 307 A and the average Sm -O(THF) distance is 2. 500A.     

CRYSTAL STRUCTURE OF A LINEAR TETRANUCLEAR Mo-Fe-S CLUSTER, (Et_4N)_4C(MoS_4)_2Fe_2S_2D·(CH_3OH)_2

<正> C_34H_88O_2N_4Mo_2Fe_2S_10, Mt= 1209. 25,monoclinic, P2_1/a,a= 17. 722 (7) ,b= 11. 857(5),c= 13. 743(5) A .β= 112. 29 (3)°, V= 2672. 0A3,Z = 2,Dc = 1. 503 g·cm-33,μ(Moka) = 14. 0 cm-1,T=193 K. Final R=0. 045 for 1943 observed reflections (I≥3σ(I)). In the anion [(MoS4)_2Fe2S2]4- ,the two Fe atoms, each attached with a chelating MoS42- unit, are bridged by two sulfur atoms. The metal atoms are arranged in a linear fashion with Mo-Fe-Fe angle of 179. 1(1)°, and Fe-Fe and Fe-Mo distances of 2. 746(2) and 2. 801(2) A, respectively. The long Fe-S distances (average 2. 246A) in Fe2S2 ring could be a result of the hydrogen-bonding interaction between the sulfur atom and the methanolic hydrogen atom.     

CRYSTAL STRUCTURE OF ORGANOLANTHANIDE [{Li(THF)_2}_2 (μ-Cl)_4(η~5-C_5H_5)Pr(THF)]

<正> The title complex crystallizes in the orthorhombic space group Pna21 with Mr = 570. 8, a = 16. 927(6), b = 18.942(7), c=10. 618(5)(?) and Z = 4. The structure was solved by Patterson and Fourier techniques and refined by block-diagonal least squares techniques to R = 0. 090 and Rw = 0. 093 for 1553 reflections with I>1. 5σ(I). The Pr3+ ion is bonded to five carbon atoms of cyclopentadi-enyl ring, four μ-chlorine atoms and one oxygen atom of THF in an octahedral geometry with the Pr-C distances in the range 2. 6.7 - 2. 79(?)(av. 2. 76(?)) , the Pr-Cl distances in the range 2. 81 - 2. 92(?) (av. 2. 86(?)) and the Pr -O distance of 2. 51 (?). Each Li+ ion is coordinated by two μ-chlorine atoms and two oxygen atoms from THF in a tetrahedral geometry with the Li-Cl distances in the range 2. 24 - 2. 61(?) (av. 2. 43(?)) and the Li -O distances in the range 1. 86-1. 94(?)(av. 1. 91(?)). The Pr atom and the two Li atoms are bridged asymmetrically by the chlorine atoms.     

CRYSTAL STRUCTURE OF MIXED METAL CLUSTER Co2Nb2Te4 OBTAINED BY SOLID STATE REACTION

<正> Compound Co2Nb2Te4 obtained by heating the elements Co2 Nb anc Te at 1000℃ in a evacuated silica tube, crystallizes in nonoclinic, space group P21/c with a = 8.197(2), b = 6,258(1), c = 7.816(3) A,β=118.48(2)° Z=2, X-ray structural determination shows non-molecular 2-dimensional character of its crystal structure. In the structural unit, two Co and two Nb atoms form a rhombic plane with four Co-Nb bonds (average 2.744A) and one Co-Co bond (2.514A) and there exists no Nb-Nb interaction. The distorted tetrahedral coordination of each metal atom is completed by four Te atoms. The average distances are 2.799A for Nb-Te bonds and 2.545A for Co-Te bonds.     

Syntheses, crystal structures, and magnetic properties of one-dimensional oxalato-bridged Co(II), Ni(II), and Cu(II) complexes with n-aminopyridine (n = 2-4) as terminal ligand

The reaction of M(ox) x 2H(2)O (M = Co(II), Ni(II)) or K(2)(Cu(ox)(2)) x 2H(2)O (ox = oxalate dianion) with n-ampy (n = 2, 3, 4; n-ampy = n-aminopyridine) and potassium oxalate monohydrate yields one-dimensional oxalato-bridged metal(II) complexes which have been characterized by FT-IR spectroscopy, variable-temperature magnetic measurements, and X-ray diffraction methods. The complexes M(mu-ox)(2-ampy)(2) (M = Co (1), Ni (2), Cu (3)) are isomorphous and crystallize in the monoclinic space group C2/c (No. 15), Z = 4, with unit cell parameters for 1 of a = 13.885(2) A, b = 11.010(2) A, c = 8.755(1) A, and beta = 94.21(2) degrees. The compounds M(mu-ox)(3-ampy)(2).1.5H(2)O (M = Co (4), Ni (5), Cu (6)) are also isomorphous and crystallize in the orthorhombic space group Pcnn (No. 52), Z = 8, with unit cell parameters for 6 of a = 12.387(1), b = 12.935(3), and c = 18.632(2) A. Compound Co(mu-ox)(4-ampy)(2) (7) crystallizes in the space group C2/c (No. 15), Z = 4, with unit cell parameters of a = 16.478(3) A, b = 5.484(1) A, c = 16.592(2) A, and beta = 117.76(1) degrees. Complexes M(mu-ox)(4-ampy)(2) (M = Ni (8), Cu (9)) crystallize in the orthorhombic space group Fddd (No. 70), Z = 8, with unit cell parameters for 8 of a = 5.342(1), b = 17.078(3), and c = 29.469(4) A. All compounds are comprised of one-dimensional chains in which M(n-ampy)(2)(2+) units are sequentially bridged by bis-bidentate oxalato ligands with M.M intrachain distances in the range of 5.34-5.66 A. In all cases, the metal atoms are six-coordinated to four oxygen atoms, belonging to two bridging oxalato ligands, and the endo-cyclic nitrogen atoms, from two n-ampy ligands, building distorted octahedral surroundings. The aromatic bases are bound to the metal atom in cis (1-6) or trans (7-9) positions. Magnetic susceptibility measurements in the temperature range of 2-300 K show the occurrence of antiferromagnetic intrachain interactions except for the compound 3 in which a weak ferromagnetic coupling is observed. Compound 7 shows spontaneous magnetization below 8 K, which corresponds to the presence of spin canted antiferromagnetism.     

THE CRYSTAL STRUCTURE OF TR1S (μ-SULFJDO)-(U3-SULFJDO)-TETRAKTS (O,O-DIETHYLPHOSPHORODITHIOATO-S,S)-OXAZOLE-TRI-MOLYBDENUM-ANTIMONOUSCHLORID {Mo_3(U3-S)[u-S)_3·SbCl_3][S_2P(OEt)_2]_4·(C_3H_3ON)}

<正> Mr = 1445.67, triclinic. The space group is P1 with the unit cell parameters: a = 10.342(3), b = 11.994(3), c = 21.352(4) A; (?)= 76.27(2), β - 88.55(2)°, r = 73.26(2)°; V = 246lA3, Z = 2, DC = 1.959 g.cm-3. The final R factor is 0.068 based on 4053 reflectioons with I≥3(?)(Ⅰ). The title compound may be regarded as the result of that a molecule of trinuclear Mo cluster {Mo3S4[S2P(OEt)2]4·(C3H3ON)}[1] connects with a molecule of SbCl3 by three bridging S atoms. The skeleton {Mo3SbS4} is a distorted cube. The distances of Mo-Mo bonds are 2.728(2), 2,743(2) and 2.751(2) A, respectively, and the distances between Sb and Mo atoms are 3.814(2), 3.815(2) and 3.847(2) A, respectively.     

Synthesis and Crystal Structure of a Novel Tetranuclear Zinc（Ⅱ） Coordination Polymer [Zn4（o-bda）4（p-pbim）4]n

A novel tetranuclear zinc（H） coordination polymer [Zn4（o-bda）a（p-pbim）4]n 1 （p-pbim = 4-pyridylbenzimidazole, o-bda2 = o-phenylenediacetic acid dianion） has been synthesized by a hydrothermal method and characterized by elemental analysis, IR and X-ray singlecrystal diffraction. The title complex crystallizes in monoclinic, space group of P21/n with α = 14.231（1）, b = 16.257（1）, c = 16.794（1） ]k, β = 100.26（1）°, V = 3823.1（2）A3, Z = 8, Dc = 1.573 g/cm^3,β = 1.321 mm^-1, F（000） = 1856, R = 0.0420 and wR = 0.111. The Zn（1） atom assumes a distorted trigonal bipyramidal geometry, involving three carboxyl O atoms from two different o-bda ligands and two N atoms from two p-pbim ligands. The Zn（2） atom is coordinated by two oxygens from two distinct bda2- anions and two nitrogen atoms from two p-pbim ligands to form a distorted tetrahedral geometry. The Zn（Ⅱ） atoms are alternately interlinked by o-bda ligands in bis-monodentate or chelating-bidentate and monodentate modes into one-dimensional undulate chains along axis c with the adjacent Zn…Zn distances of 8.32 and 8.47 A. Such neighboring chains are further extended into a 1D bi-chain structure with two different subrings A and B, which are 32- and 14-membered rings through interchain p-pbim ligands. There exists a 2D supramolecular network linked by intermolecular hydrogen-bonding interactions between the uncoordinated carboxylate 0（4） atom or coordinated carboxylate 0（7） atom and the uncoordinated imidazolyl N（2） and N（5） atoms with the O...N distances to be 2.695 and 2.807A.     

CRYSTAL STRUCTURES OF COPPER (Ⅱ) AND COBALT (Ⅲ) COM- PLEXES OF o-HYDROXYBENZYLGLYCINATE (HBG)

<正> The structures of two complexes C(CuOC6H4CH2NHCH2COO)2 (H2 O)]·H2P(1) and [Co(NH3)6[Co(OC6H4CH2NHCH2COO)2]2[C1]·10H2O (2) were determined by X-ray analyses. Compound (1) crystallizes in the orthorhombic space group P212121 with a=11. 357(1),b= 24. 304(2),c=7.317(4) A,Z= 4;While compound (2) in the monoclinic space group A2/a(C2/c) with a=23. 486(9) ,b=26. 605(6) ,c= 10. 542(1) A,γ= 128. 42(4)°,Z= 4. In compound (1),two Cu(Ⅱ) ions are bonded together by the phenolic oxygen atoms of two tridentate chelating ligands and each of them is separately coordinated by the carboxyl oxygen,amino nitrogen of each chelate ligand and by the fifth oxygen atom as well (from aqua or the carbonyl group in adjacent molecule). Thus the coordination of each Cu(Ⅱ) is a square pyramid with distances of 1. 93- 1. 97A to the four corner atoms and 2. 30 and 2. 32 A to the apex atoms. The whole molecule has an approximately planar configuratioir with the two pyramid apexes pointing towards one side. Compound (2) consists of     

Synthesis and Structural Characterization of a Tetranuclear Copper Complex with 2-Amino-1,3-thiazole

The title tetranuclear complex,(μ4-oxo)-hexakis(μ2-chloro)-tetrakis(2-amino-1,3-thiazole-N)-tetra-copper(ii) [Cu4(μ4-O)(μ-Cl)6L4](1,L=2-amino-1,3-thiazole) was synthesized by the reaction of CuCl2·2H2O with 2-amino-1,3-thiazole in methanol and characterized by IR spectra and X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1 with a=9.7137(2),b=10.7005(2),c=14.6505(2),α=83.9550(10),β=82.0930(10),γ=67.1640(10)°,V=1387.84(4)3,Mr=883.43,Z=2,μ=3.927 mm-1,Dc=2.1144 g/cm3,F(000)=868,R=0.0332 and wR=0.0814.The complex contains a tetrahedron of four CuII atoms coordinating to a central μ4-O atom,with the six edges of the tetrahedron bridged by six Cl atoms.The Cu-O bond distances range from 1.910(2) to 1.918(2),Cu-Cl from 2.3501(11) to 2.5924(10),and Cu-Cu from 3.1003(6) to 3.1663(6).The coordination geometries of the four coppers distort from trigonal bipramid to tetragonal pyramid with different distortion factors.The free animo groups of the ligands result in a lot of N-H···Cl and N-H···N intra-and intermolecular hydrogen bonds.     

Synthesis and Structure of K_6PMo_7V_2W_3O_(40)(H_2O)_(16)

1INTRODUCTIONHeteropolycompoundsareacidsaswellasoxidizingagents"'.Takingadvantageoftheseproperties,heteropolycompoundshavebeenusedascatalystsforvarioussyntheticreaction(bothinhomogeneousandheterogeneoussystems).Hydrationofpropeneinaliquidphasecatalyzedbyheteropolyacidshasbecomeacommercializedprocess.Oxidationofmethacroleinorisobutyricacidtoproducemethacrylicacidisanexampleofindustrialprocessestowhichthesecompoundsareapplied"--'>.Theoxidationpotential(oroxidizingability)decreaseslinearlywi…     

Synthesis and Structure of Nickel(II) Compound with Tetradentate Schiff-base Ligand and Diazido Monohydrate

1 INTRODUCTION Complexes of ligands which bind two or more metal centers in close proximity are important as potential catalysts[1], as models for a number of metalloproteins[2], and because of the opportunity they provide for the investigation of magnetic interactions. The structural and magnetic properties of binuclear and polymetallic nickel (II) complexes with various bridging ligands have received considerable attention in the past three decades[3～6]. At present, there is a spectacu…     

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 and Molecular Structure of OMPCTF

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STUDIES ON SOLID STATE REACTIONS OF COORDINATION COMPOUNDS XXXXV. SOLID STATE SYNTHESIS AND CRYSTAL STRUCTURE OF [MoAg_3BrS_4I_3][(n-Bu)_4N]_3

<正> C48H108Ag3BrI3MoN3S4, Mr=1735. 84, cubic, F43c, a = b = c = 24. 577(4) A.V= 14845. 2A3, Z = 8, Dc=1. 553g/cm3, Dv = 1. 560g/cm3. Final R = 0. 061 for 307 unique diffraction data with I≥3σ(I). The anion of the title cluster compound can be viewed as a cubane like structure situated at specific equivalent positions in the unit cell with Td symmetry. One Mo and three Ag atoms, one Br and three Sb atoms, one S, and three I atoms are statistically distributed, individually. The distances of Mo....Ag (or Ag....Ag), Mo-Sb(or Ag -Sb, Ag -Br), and Mo-St(or Ag-I) are 3. 303(3), 2. 701(4) and 2. 741(3) A , respectively.     

Cs3AgAs4Se8 and CsAgAs2Se4: selenoarsenates with infinite 1 infinity[AsSe2]- chains in different Ag+ coordination environments

Two quaternary silver selenoarsenates Cs3AgAs4Se8 (I) and CsAgAs2Se4 (II) have been discovered by methanothermal reaction of Li3AsSe3 with AgBF4 in the presence of the respective alkali metal sources Cs2CO3 and CsCl. Orange crystals of Cs3AgAs4Se8 (I) were formed after reaction at 120 degrees C for 72 h, whereas red CsAgAs2Se4 (II) was obtained under slightly different conditions at 140 degrees C for 70 h. Both compounds possess novel two-dimensional (2D) polyanions consisting of infinite 1 infinity[AsSe2]- chains that are interconnected by Ag+ ions in different coordination patterns. In I, a double layer of 1 infinity[AsSe2]- chains is bridged by distorted trigonal planar coordinated Ag+ atoms to form a 2 infinity[AgAs4Se8]3- layer with a thickness of about 11.3 A. The nonbonding Ag...Ag distances are about 4.220 A, and large cavities within the layers accommodate for three of the four crystallographic Cs+ cations. The double amount of Ag+ atoms per AsSe2 chain unit in II leads to simple layers 2 infinity[AgAs2Se4]- [=[Ag2As4Se8]2-] in which the Ag+ atoms are arranged in rows between the 1 infinity[AsSe2]- chains, with alternating Ag...Ag distances of 3.053(3) and 3.488(3) A. Hereby the 1 infinity[AsSe2]- polyanions show a disorder within the central (-As-Seb)- chain (b = bridging), while the positions of the terminal Se atoms (Set) remain unaffected. The thermal, optical, and spectroscopic properties of the compounds are reported. Both I and II melt with decomposition and are wide band gap semiconductors with values of 2.07 and 1.79 eV, respectively. Raman spectroscopic data show typical band patterns expected for infinite [AsSe2]- chains. Crystal Data: Cs3AgAs4Se8 (I), monoclinic, C2/c, a = 25.212(2) A, b = 8.0748(7) A, c = 22.803(2) A, beta = 116.272(2) degrees, Z = 8; CsAgAs2Se4 (II), monoclinic, P2(1)/n, a = 10.9211(1) A, b = 6.5188(2) A, c = 13.7553(3) A, beta = 108.956(1) degrees, Z = 4.     

Synthesis and 2D H-bonded Cd（ Ⅱ ） Network Structure of [Cd（C10H15N3）Cl2]

1 INTRODUCTION Transition metal Schiff base complexes have been extensively studied in the past two decades for their various crystallographic features, enzymatic reactions, steric effects[1～4], catalysis and magnetic properties[5, 6] as well as their important role in organisms[7, 8]. Most of these first-row materials are biologically essential with a number of their complexes showing bioactivities[9, 10]. Herein we describe the synthesis and X-ray structure of the cadmium (Ⅱ) compl…