Synthesis and Structure of a Dimolybdenum Carbonyl Compound with Thiolato-Bridges [Et4N] 2 [Mo2 (CO) 8 (SC6H4-Cl -p) 2]

Reaction of Mo (CO)6 with p-Cl-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum (0) compound [Et4N]2 [Mo2 (CO)8 (SC6H4-Cl-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C36H48Cl2Mo2N2O8S2, Mr= 963.71, monoclinie, P21/c, a=9. 269(4),b=13.750(3), c=17.466(6) A ;β=104.84(3)°; V=2151.8(3) A3; Z=2; Dc=1.49 g/cm3; F(000)=984; μ=8.3 cm-1; MoKα radiation (λ=0. 71073A ); Final R = 0. 055 and Rw=0. 065 for 3287 reflections with I＞3. 0σ(I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distance is 4. 014(2) A , and this obviously indicates the absence of Mo-Mo bond.     

Synthesis and Crystal Structure of[Ni(C5H2N2O4)(2, 2'-bipy)(H2O)2]·2H2O

The crystal structure of [Ni(C5H2N2O4)(2, 2?-bipy)(H2O)2]·2H2O 1 has been determined by X-ray diffraction. Crystal data: triclinic system, space group P ī with a = 7.9424(3), b = 9.9417(3), c = 12.1867(3) (A。）, α = 84.771(1), β = 77.375(2), γ = 68.993(2)°, C15H18N4O8Ni, Mr = 440.7, V = 876.16(5) (A。）3, Z = 2, Dc = 1.672 g/cm3, F(000) = 456, ((MoK() = 1.162 mm-1, the final R = 0.0464 and wR = 0.1055 for 3026 observed reflections with I > 2((I). In the title compound, the nickel ion is coordinated by a nitrogen atom and an oxygen atom from the orotate ligand, two nitrogen atoms from 2, 2'-bipy and two oxygen atoms from the coordinated water molecules in a distorted octahedral geometry. The presence of intermolecular hydrogen bonding and (-( stacking interaction of aromatic rings from 2, 2'-bipy results in a 3D structure.     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound [Et4N ] 2 [Mo2 (CO) 8 (SC6H4-OCH3-p) 2]

Reaction of Mo(CO)6 with p-H3CO-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2 (CO)8 (SC6H4-OCH3-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C38H54Mo2N2O10S2, Mr = 954.87, triclinic, P-1, a = 11.348 (7), b =11.616(5), c=10.065(7) A, a=113.86(4), β=111.39(5), γ=91.92(5)°, V=1104.0(1) A3, Z=1, Dc=1.44 g/cm3, F(000)=492, μ=7.0cm-1, Final R=0. 046 and Rw=0. 049 for 2657 reflections with I＞3. Oσ(I). The X-ray structure analysis revealed that the Mo2S2 core of 1 is planar. The geometry around each Mo atom is a distorted octahedron, the two octahedrons form an edge-sharing bioctahedron. The bond. In addition, the 95Mo NMR chemical shift of 1 is discussed.     

OXIDATION DECARBONYLATION OF NH_4[Mo(CO)_5I]: SYNTHE-SES AND CRYSTAL STRUCTURES OF CMo(S_2CNC_4H_8)_4]I_3 · C_7H_8 and Mo_2S_2O_2(S_2CNC4H_8)_2

<正> Both of the title complexes were produced by oxidative decarbony-lation of NH4 CMO (CO)5I]. The complexes CMo(S2CNC4H8)4]I3 ?C7H8(1) and Mo2S2O2 (S2CNC4H8)2(2) both crystallize in triclinic, space group P1 with cell dimensions for (1) : a=13. 554(4), b=13. 620(4), c= 13. 058 (4) A , α=95. 58 (3), β=105. 38(2), γ=115. 49(2)°,V = 2035(1) A3, Z=2, Dc=1. 89 g. cm-3, final R=0. 054 and Rw = 0. 062 for 2926 observed reflections; and for (2): a = 8.730(2), b=16.592(6), c = 6. 688(2)A, α=97. 67(3), β=98. 10(2), γ=80. 26(2)% V = 939. 2(5) A3, Z = 2, Dc = 2. 05 g. cm-3, final R = 0. 038 and Rw = 0. 046 for 2248 observed reflections. The Mo(V) atom is bonded to eight S atoms in distorted dodecahedron for (1). The Mo atoms in compound (2) are bridged by two S atoms and each Mo atom is coordinated by two S atoms from S2CNC4H8 and one O atom to form distorted tetragonal pyramid.     

Synthesis and Crystal Structure of Bis（p—aminotoluene）—bis（dimethylglyoximato） Cobalt（Ⅲ） Perchlorate

The title compound (C22H32.5ClCoN6O8.25,Mr=607.42)crystallizes in the orthorhombic system,space group c222 1 with a=11.320(2),b=20.933(4),c=23.936(5)A,V=5672(2)A^3,Dc=1.423g/cm^3,Z=8,μ(MoKα）=0.754mm^-1,F(000)=2532,R=0.0512 and wR=0.1190,There are eight complex molecules [Co(C4H6N2O2)(C4H8N2O2)(C7H9N)2]ClO4.0.25H2O of C2 crystallographic symmetry in a unit cell,including two crystallographically independent molecules,in which different orientations of the MePhNH2 groups are found.Two MephNH2 groups are in trans position for molecule A,and cis for B.The central metal atom is in a distroted octahedral environment.The hydrogen bonds of O-H(oxime)…O and N-H(p-aminotoluene group)…O construct an one-dimensional chain along the c axis in the title compound.     

Synthesis,Crystal Structure and Antitumor Activities of N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline

The title compound, N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline(C16H15N3O2, Mr = 281.31), has been synthesized by the multicomponent reaction of milder Ullmann, and its structure was characterized by 1H NMR, 13 C NMR, IR, H RMS(ESI) and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group I2/c with a = 15.0212(10), b = 9.4911(6), c = 20.3075(13) A, β = 100.776(7)o, V = 2844.1(3)A3, Z = 8, Dc = 1.314 g/cm3, F(000) = 1184.0, μ = 0.089 mm-1, the final R = 0.0574 and w R = 0.1688 for 1701 observed reflections(I 2σ(I)). X-ray analysis indicates three major N(2)–H(2)···O(2), C(13)–H(13)···O(2), N(2)–H(2)···N(3) hydrogen bonds and π-π stacking interactions in the crystal structure. The preliminary biological test shows that the title compound has a good antitumor activity against A549 in vitro with the IC50 value of 35 μmol/L.     

Synthesis and Crystal Structure of 2-Ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3（2H）-one

The crystal structure of the title compound 2-ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3(2H)-one(C15H15ClN2O4,Mr = 322.74) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of orthorhombic,space group Pccn with a = 16.7246(10),b = 19.6626(12),c = 9.3013(6) ,V = 3058.7(3) 3,Z = 8,Dc = 1.402 g/cm3,μ = 0.269 mm-1,F(000) = 1344,the final R = 0.0506 and wR = 0.1464 for 2568 reflections with I 2σ(I).In addition,disordered C(14) and C(15) atoms exist in the crystal structure.     

Synthesis and Crystal Structure of Tetra（（8-quinolyl）-amido-N）ytterbium Bi（tetrahydrofuran-O）lithium

The treatment of the mixture of n-BuLi with 1 equiv.8-aminoquinoline in THF in situ,which reacted further with 1/3 equiv.of YbCl3 in THF,to give the homoleptic lanthanide amide ate complex Yb(NH-C9H6N)4Li(C4H8O)2(1).The crystal structure was determined by X-ray diffraction and the following crystallographic data were obtained:C44H44N8O2YbLi,Mr = 896.85,monoclinic,space group C2/c,a = 7.8384(16),b = 22.294(5),c = 22.668(5),β = 97.614(5)°,V = 3926.3(14)3,Z = 4,Dc = 1.517 g/cm3,F(000)= 1812,μ(MoKα)= 2.431 mm-1,R = 0.0542 and wR = 0.1523 for 3372 observed reflections with I > 2σ(I).The structure of molecule 1 consists of one ytterbium atom,one lithium atom,four 8-aminoquinoline ligands and two THF molecules.The ytterbium atom is coordinated by eight nitrogen atoms of four 8-aminoquinoline ligands,forming a distorted dodecahedral geometry.     

CRYSTAL STRUCTURE OF {Ni[(C_4H_9O)_2PS_2](C_(12)H_8N_2)_2} -[(C_4H_9O)_2PS_2]

<正> {Ni C(C4H9O)2PS2] (C12H8N2)2} [C(C4H9O)2PS2], Mr= 795. 60, Monocinic,P2,/n,a=16. 806(2), b=12. 720(2), c=21. 248(2) A. β=98. 454(7)°, V = 4493A3,Z=4,Dc= 1. 18g·cm-3,Mo Ka radiation,A=0. 71069A ,F(000) = 1664, R=0. 102 for 4154 reflections with I≥3σ(I).The crystal structure consists of complex cation {NiC(C4H9O)2PS2](C12H8N2)2}+ and complex anion C(C4H9O)2PS2]-. In the cation, nickel (Ⅱ) atom is coordinated by four nitrogen atoms and two sulfur atoms to form a distorted octahedron.     

CRYSTAL STRUCTURE OF 3-NITRO-2, 6-BIS(4''''-BENZO-15-CROWN-5)-AMINOPYRIDINE POTASSIUM PICRATE HYDRATE METHANOL, (C_(33)H_(42)N_4o_(12)K)C_6H_2N_3o_7·H_2O ·CH_3OH

<正> The title compound, (C33H42N4O12K)C6H2N3O7·H2O·CH3OH,Mr = 1003. 98,space group P1,a=11. 458(2) ,b= 14. 565(6) ,c=15. 828(3) A ;α=63. 34 (2),β=74. 06(1),γ=81. 03(2)°,V=2268. 1 A3;Z = 2,Dx = l. 47g/cm3,λ=0. 71069 A (MoKa).The final R = 0. 041 for 1700 observed reflections (I≥3σ(I)). The molecule is sandwich-like, and the cation K+ is sandwiched between the two crown rings.     

Synthesis, Crystal Structure and Pyrolysis of a Heterobimetallic Peroxo-titanium（IV） Nitrilotriacetate Complex

A new heterobimetallic nitrilotriacetatoperoxotitanate complex with the formula of [Mn(H2O)5]2[Ti(O2)2O(nta)2]·7H2O (1, C6H6O6N = H3nta) has been isolated in pure crystals. It was characterized by elemental analyses, IR, thermal analysis (TGA) and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic, space group C2/c with a = 15.088(3), b = 13.311(3), c = 17.741(4) , β = 100.92(3)°, Z = 4, V = 3498.6(12) 3, Mr = 968.19, Dc = 1.838 g/cm3, μ = 1.266 mm-1, F(000) = 1992, R = 0.0337 and wR = 0.0819. Single-crystal X-ray analysis reveals that the titanium atom is N,O,O',O'-chelated by the nitrilotriacetate and O,O'-chelated by the peroxo group, and is coordinated to the bridging O atom in an overall pentagonal-bipyramidal geometry. The manganese ions in the compound are both 6-coordinated by five water molecules and one bridged carboxylato oxygen atom. A decameric water cluster consisting of a cyclic water hexamer in a boat fashion is also found in complex 1. The TGA and XRD results prove that 1 undergoes facile thermal decomposition to form the mixture of Mn2O3 and TiO2 at 600～800 ℃, and pure MnTiO3 at 900 ℃.     

STRUCTURE OF A Cu (Ⅱ) COMPLEX WITH MIXED LIGANDS, DIETHYLENETRIAMINE ETH YLENEDIAMINE COPPER (Ⅱ) DIPERCHLORATE

<正> CuC6H21N5O8Cl2, Mr = 425. 5, monoclinic, P21/n, a = 8. 418 (2), b = 14.450(4), c= 12. 940(3)A, β=98. 13(2)% V = 1572. 9A3,Z = 4, Dx= 1. 797g. cm-3,μ(MoKa) = 18. 3cm-1. The crystal structure consists of discrete complex cations and perchlorate anions. The coordination geometry around Cu(Ⅱ) atom is a distorted square pyramid. The complex cations are disordered in the crystal,the ethylenediamine ligand chelates to the Cu(Ⅱ ) atom in δ arid λ conformation in different cells. The average Cu-N distance is 2. 03 A in the equatorial plane while the Cu -N distance is 2. 25 A in the axial direction.     

SYNTHESIS AND CRYSTAL STRUCTURE OF (DIETHYLENETRIA-MINE) (ACETATE) ZINC PERCHLORATE

<正> The preparation and molecular structure of the novel five-coordinate zinc compound CZn(C4H13N3) (C2H3O2)]ClO4(Mr= 327. 04) are described. The crystal belongs to orthorhombic space group Pn21a with a=8. 352(2) ,6=8. 642(2) ,c=17. 758 (4)A,V=1282A3,Z=4,0c=1.69gcm-3,Dm=1.70gcm-3,F(000) = 672,u(MoKa)= 22.01cm-1.The complex cation has a distorted trigonal bipyramidal geometry wifr each acetat anion C2H3O2- bridging two zinc atoms so that a chain structure along a axis is formed by the complex cations [Zn(C4H13N3)(C2H3O2)]+.     

Synthesis and Crystal Structure of Diaquabis{2,4-dibromo-6-[(2-ethylaminoethylimino)methyl]-phenolato}nickel(Ⅱ) Dinitrate Diacetonitrile

The title mononuclear Schiff base nickel(Ⅱ) complex [Ni(C11H14Br2N2O)2(H2O)2]· 2NO3·2C2H3N was prepared and characterized by elemental analysis,IR spectrum,and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system,space group P21/n with a=15.534(2),b=7.647(1),c=16.435(2),β=103.252(2)o,V=1900.3(4)3,Z=2,Dc=1.750 g/cm3,Mr=1000.99,λ(MoKα)=0.71073,μ=4.776 mm-1,F(000)=996,the final R=0.0368 and wR=0.0724. A total of 3988 unique reflections were collected,of which 2764 with I > 2σ(I) were observed. The complex consists of a mononuclear [Ni(C11H14Br2N2O)2(H2O)2]2+ cation,two nitrate anions and two acetonitrile molecules. The Ni atom,lying on the inversion centre,is six-coordinated by two Schiff bases and two water molecules to assume an octahedral coordination geometry. The molecules in the crystal are linked through intermolecular hydrogen bonds of N–H…O,N–H…Br,O–H…O,O–H…N and C–H…O to form layers.     

SYNTHESIS AND STRUCTURE OF EUROPIUM (Ⅲ) WITH N,N'''' BISSALICYLIDENE ETHYLENEDIAMINE (H_2salen)

<正> A europium (Ⅲ) complex with N, N' - bissalicylidene-ethylenediamine (H2salen) has the formula Eu(Hsalen)(salen)4H2O,where water molecules are in the outer sphere and do not coordinate with Eu (Ⅲ), was synthesized and structurally studied. The central atom Eu is coordinated by four nitrogen atoms and four oxygen atoms in a deltadodecahedron arrangement. The crystal is monoclinic,space group P21/a with cell constants a=16. 441(2),b=20. 599(3),c=10. 719(2) A ,β=84. 16(1)°,Z=4 and V = 3611. 5(8) A3,Dc=1. 392g/cm3.The final standard deviation R is 0. 093.     

Synthesis and Crystal Structure of Bis{2-bromo- 4-chloro-6-[（2-isopropylammonioethylimino）- methyl]phenolato}bisthiocyanatozinc（Ⅱ）

A Schiff base zinc(Ⅱ) complex [Zn(C12H16BrClN2O)2(NCS)2] was prepared and characterized by elemental analysis,IR and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a=8.414(1),b=9.124(1),c=22.212(3),α=79.177(2),β=86.296(2),γ=89.899(2)o,V=1671.3(4)3,Z=2,Dc=1.631 g/cm3,Mr=820.79,λ(MoKα)= 0.71073,μ=3.444 mm-1,F(000)=824,R=0.0646 and wR=0.1179. A total of 7371 unique reflections were collected,of which 3904 with I > 2σ(I) were observed. The complex crystallizes with two half-molecules per asymmetric unit and each mononuclear molecule is centrosymmetric. The Zn atom lying at the inversion centre is six-coordinated in a slightly distorted octahedral geometry by two phenolate O atoms and two imine N atoms from two Schiff base ligands,as well as two N atoms from two thiocyanate anions. In the crystal structure,the combination of π-π stacking interactions and intermolecular hydrogen bonds (N–H…Br,N–H…O,N–H…N,C–H…O,C–H…S and C–H…Cl) leads to a three-dimensional network.     

Synthesis and Crystal Structure of Diaquabis{2,4-dibromo-6-[(2-ethylaminoethylimino)methyl]phenolato}nickel(Ⅱ) Dinitrate Diacetonitrile

The title mononuclear Schiff base nickel(Ⅱ) complex [Ni(C11H14Br2N2O)2(H2O)2]·2NO3·2C2H3N was prepared and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/n with a = 15.534(2), b = 7.647(1), c = 16.435(2) (A), β = 103.252(2)o, V = 1900.3(4) (A)3, Z = 2, Dc = 1.750 g/cm3, Mr = 1000.99, λ(MoKα) = 0.71073 (A), μ = 4.776 mm-1, F(000) = 996, the final R = 0.0368 and wR = 0.0724. A total of 3988 unique reflections were collected, of which 2764 with I＞2σ(I) were observed. The complex consists of a mononuclear [Ni(C11H14Br2N2O)2(H2O)2]2 cation, two nitrate anions and two acetonitrile molecules. The Ni atom, lying on the inversion centre, is six- coordinated by two Schiff bases and two water molecules to assume an octahedral coordination geometry. The molecules in the crystal are linked through intermolecular hydrogen bonds of N-H…O, N-H…Br, O-H…O, O-H…N and C-H…O to form layers.     

Synthesis and Crystal Structure of Diaquabis{2,4- dibromo-6-[（2-ethylaminoethylimino）methyl]- phenolato}nickel（II） Dinitrate Diacetonitrile

The title mononuclear Schiff base nickel(Ⅱ) complex [Ni(C11H14Br2N2O)2(H2O)2]·2NO3·2C2H3N was prepared and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/n with a = 15.534(2), b = 7.647(1), c = 16.435(2) (A), β = 103.252(2)o, V = 1900.3(4) (A)3, Z = 2, Dc = 1.750 g/cm3, Mr = 1000.99, λ(MoKα) = 0.71073 (A), μ = 4.776 mm-1, F(000) = 996, the final R = 0.0368 and wR = 0.0724. A total of 3988 unique reflections were collected, of which 2764 with I＞2σ(I) were observed. The complex consists of a mononuclear [Ni(C11H14Br2N2O)2(H2O)2]2 cation, two nitrate anions and two acetonitrile molecules. The Ni atom, lying on the inversion centre, is six- coordinated by two Schiff bases and two water molecules to assume an octahedral coordination geometry. The molecules in the crystal are linked through intermolecular hydrogen bonds of N-H…O, N-H…Br, O-H…O, O-H…N and C-H…O to form layers.     

PREPARATION AND CRYSTAL STRUCTURE OF CYCLOPENTADI-ENYL TETRAMETHYLETHENE-BRIDGED DICYCLOPENTA-DIENYLSAMARIUM(Ⅲ) TETRAHYDROFURANATE

<正> (CH3)4C2(C5H4)2Sm(C5H5)(OC4H8),Mr=499.4,orthorhom-bic,Cc2a,a=11.696(6),b=12.539(5),c=29.432(15)A,V=4316(4)A3,Z=8,Dc=1.54g/cm3,μ(MoKa)=27.8cm-1,F(000)=2024,R=0.077 for 1833 observed reflections.The samarium atom in the molecule is bonded to three cyclopen-tadienyl rings and one oxygen atom of tetrahydrofuran(THF)to form a tetrahedral configuration.The average Sm-C(η5-Cp)distances for the three cyclopentadienyl groups are 2.72(3),2.76(3)and 2.78(3)A,respectively,and the Sm-O bond is 2.53(1)A.     

Synthesis and Crystal Structure of a New Complex [Cd（C20H14N4）2Cl2]

The title compound [Cd(C20H14N4)2Cl2] 1 was synthesized via the hydrothermal reaction of CdCl2·7H2O and NaOH with 1,3-bis(benzimidazol-2-yl)benzene (BMB), and characterized by elemental analysis and infrared spectra. The crystal of 1 crystallizes in monoclinic, space group C2/c with a = 21.021(6), b = 9.489(3), c = 18.302(6), β = 108.686(6)o, V = 3458.2(19)3, Z = 4, C40H28CdN8Cl2, Mr = 804.01, Dc = 1.544 g/cm3, F(000) = 1624 and μ(MoKα) = 0.829 mm-1. The final R = 0.0306 and wR = 0.0779 for 3334 observed reflections with I > 2σ(I) and R = 0.0796 and wR = 0.0360 for all data. The cadmium atom is four-coordinated by the BMB ligands and Cl atom with a tetrahedral geometry. The extensive N-H···N hydrogen bonding interactions are observed in the structure, which further extend the [Cd(C20H14N4)2Cl2] units into a 1D structure. The thermogravimetric analysis measurement showed that compound 1 has thermal stability as no strictly clean weight loss step occurred below 425 ℃.