THE SYNTHESIS AND CRYSTAL STRUCTURE OF A CUBANE-LIKE MOLYBDENUM-COPPER-SULFUR CLUSTER {Mo3CuS4[S2P(OC2H5)2]3(I)(μ-CCl3(00)CH3CN}

<正> The synthesis and crystal structure of the cubane-like cluste with [Mo3CuS4] core is reported herein. The title compound crystallizes i triclinic space group Pl with the following unit cell dimensions: a 11.723(3), b = 14.353(6), c = 15.533(4)A;α= 75.40(3)°,β=69.13(2)°,γ 64.93(3)°; Z = 2; V = 2196 A3; DC = 2.033 g·cm-3.7704 independent reflec tions were collected on CAM four-circle diffractoneter with MoKa radiatio in the range of 1 < <25°, with only 2083 reflections having intensitie I > 3σ(I). The structure was determined by direct methods and refined b the least-squares method to a final R index of 0.091. There are some distortion in the cubane-like [Mo3CuS4] core, with three Mo-Mo bonds and thre weak Mo-Cu bonds.     

Synthesis and Crystal Structure of 2-(2-Ethyl-1H-imidazol-1-yl)-1-hydroxy-ethane-1,1-diyldiphosphonic Acid (EIHDP)

The crystal structure of the title compound (C7H14N2O7P2, Mr = 300.14) was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a = 8.258(3), b = 8.886(3), c = 9.275(3) , α = 96.669(3), β = 115.706(3), γ = 104.467(3)°, V = 573.8(3) 3, Z = 2, Dc = 1.737 g/cm3, λ(MoKα) = 0.71073, F(000) = 720, μ(MoKα) = 0.41 mm-1, R = 0.030 and wR = 0.078. A total of 1970 unique reflections were collected, of which 1742 with I > 2σ(I) were observed. EIDHP has a structure similar to zoledronic acid (ZL). ZL is a potent bone antiresorptive bisphosphonate drug having significant activity against several parasitic protozoa. EIHDP has inner-salt character, consisting of a negatively charged PO3 group and a positively char- ged N(1) atom. The crystal structure is stabilized by intermolecular hydrogen bonds of O–H···O and N–H···O.     

CRYSTAL AND MOLECULAR STRUCTURE OF N_2-[(4-METHYLPHENYL)-SULFONYL]-CLUTAMINE (C_(12)H_(16)N_2O_5S)

<正> C12H16N2O5S, Mr = 300. 34, monbclinic, P21, a = 12. 748(4), b = 5. 240(1), c=21. 356(4)(?); β=93. 28(2)°, V = 1428. 1(7) (?)3. Z = 4, Dc = 1. 397gcm-3, λ=0. 71073(?). Full matrix least-squares refinement, final R = 0. 042, Rw = 0. 045 for 2050 unique reflexions with I≥3σ(I). The two molecules in the asymmetric unit are connected by two hydrogen bonds to form a dimer.     

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 N-[2-（4-Chlorophenyl）-1-（1-methylcarbamoyl-2-phenyl-ethylcarbamoyl）-3-phenyl-cyclopropyl]-benzamide

N-[2-(4-chlorophenyl)-1-(1-methylcarbamoyl-2-phenyl-ethylcarbamoyl)-3-phenyl-cyclopropyl]benzamide,C33H30ClN3O3,has been synthesized and characterized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 11.646(2),b = 13.795(3),c = 14.559(3),α = 76.422(4),β = 78.028(4),γ = 74.500(4)°,V = 2164.6(7)3,Z = 3,Mr = 552.05,Dc = 1.270 g/cm3,λ = 0.71073 ,μ(MoKα)= 0.171 mm–1,F(000)= 870,the final R = 0.0469 and wR = 0.0805 for 5554 observed reflections with I > 2σ(I).The N–H and oxygen atoms are involved in one-dimensional intermolecular hydrogen bonds,which further stabilize the structure.     

Synthesis and Structure of a Mononuclear Co(II) Complex Based on a Salicylideneaniline Ligand, (Z)-4-(2- Hydroxybenzylideneamino)-2-hydroxybenzoic Acid

The reaction of a new salicylideneaniline ligand, (Z)-4-(2-hydroxybenzylidenea- mino)-2-hydroxybenzoic acid (HL) with CoCl2·6H2O yields one Co(II) complex, [CoL2(CH3OH)2 (H2O)2]. This complex crystallizes in monoclinic P21/n space group, with a = 5.4992(5), b = 18.2200(15), c = 14.8678(14) , β = 98.64(1)°, V = 1472.8(2) 3, C30H32CoN2O12, Mr = 671.51, Z = 2, Dc = 1.51416 g/cm3, F(000) = 698, μ = 0.652 mm–1, T = 298(2) K, R = 0.0514 and wR = 0.1735 for all 2675 observed reflections (I > 2σ(I)). In this complex, the imine N does not link to Co(II) and a remarkable torsion around C=N bond is observed. Through hydrogen bonds, the monomers aggregate into an interesting "Z-shape" framework.     

APPLICATION OF DITHIO - MOLYBDATE IN THE SYNTHESES OF Mo-Cu CLUSTERS: SYNTHESES AND CRYSTAL STRUC-TURES OF MoOS_3(CuPPh_3)(Cu(PPh_3)_2 AND (Ph_4P)_2[Mo_2Cu_5S_6O_2-(S_2CNEt_2)_3] ·DMF

<正> The reactions of (NH4)2MoO2S2 with Cu(PPh3)3Cl in CH3CN in the air, or with CuCl, Ph4PBr, and NaS2CNEt2 in DMF under anaerobic condition, afforded the cluster complexes MoS3OCu2 (PPh3)3 (Ⅰ) and (Ph4P)2 CMo2Cu5S6O2-(S2CNEt2)33 · DMF (Ⅱ), respectively. Compound (Ⅰ), MoOS3Cu2P3C54H45(Mr = 1121. 0) , crystallizes in the triclinic, space group P1 with cell parameters a = 14. 103 (3), b = 17.906(3), c=11.503(2)(?), α=107. 76(1), β=111.81(2), γ = 74.93 (2)°, F = 2532. 9(?)3 and Z=2, Dc=1. 471 g/cm3, F (000) = 1140, μ(MoKα) = 13. 215 cm-1, final R = 0. 060 (Rw = 0.064) for 5959 independent reflections with I >3σ(Ⅰ). Complex (IⅡ), Mo2O3S12Cu5P2N4C66H77 (Mr = 1930. 67) , crystallizes in monoclinic, space group P2/c with cell parameters a = 25. 325(19) , 6 = 22. 506(9) , c =14. 066(8)(?) , β =100. 96(6)°, V =7871. 16 (?)3, Z = 4, D,= 1. 629 g/cm3, F(000) = 3904, μ(MoKα) = 20. 216 cm-1, R = 0. 097 (Rw = 0. 095) for 5677 reflections with I>3σ(Ⅰ). The core structure of complex (Ⅰ) is defective cub     

CRYSTAL STRUCTURE OF Mo_2(u-S)_2(S_2P(OEt)_2)_4

<正> Mr=996.91, triclinic, P1, a=8.773(2), b=9.712(3), c=13.652(1) A; α=69.24(0), β=70.43(3), γ=66.87(l)°; Z=l, Dx=1.699 g/cm 3. Final R=0.053 for 3186 reflections with I≥3a(I). There is an interesting trans influence of μ-s bridge in this binuclear cluster. Mo-Mo distance is 2.752(1) A.     

Crystal Structure of Methyl 3- (2-chlorophenyl )-3- (5, 5-dimethyl-3-hydroxy-2-cyclohexene- 1-one-2-yl) propionate

1INTRODUCTIONInorganicsolidsupportsascatalystshavebeenwellstudied,becauseoftheirap-plicationsinorganicsynthese('~".Recently,wehavereportedtheKnoevenagelcon-densationcatalysedbyKF-Al,O,['i.Inthispaper,wediscussedthecrystalstruc-tureofthetitlecomPoundsynthesizedbythereactionof2-chlorobenzaldehydey5,5-dimethyl-1,3-cyclohexanedioneandisopropylidenemalonateinmethanolcatalyzedbyKF-Alzo,'Inordertoconfirmthestructureofthetitlecompound,theX-raycrys-tallOgraphicstudywascarriedout.2EXPER1MEN…     

CRYSTAL STRUCTURE OF BID[N-t-BUTYLBUTEN-2-YLIDENE] DICHLOROPALLADIUM(II)

<正> The title compound, C15H30N2PdCl2 (Mr=427.73), crystallizes in two kinds of crystal forms I and II.I : monoclinic, P21/c, a = 8.234(1), b = 13.702(3), c = 8.939(2) A, β = 93.90(1)°, V = 1010.55 A3, DC = 1.407g/cm3, R = 0.032 for 2098 observed reflections.II: triclinic, Pl, a=8.179(1), b=8.182(1). c=8.231(2) A, α=91.89(1)°, β=91.90(2)°, α=113.80(1)°, V =503.09A3, DC =1.413 g/cm3, R = 0.036 for 1770 observed reflections.The molecules in both crystals I and II possess the identical configurations but there are two orientations of molecules in the crystal II.     

X-RAY STRUCTURE AND MOLECULAR MECHANICS CALCULA-TIONS OF N-(2-CHLOROPHENYL)-2-PYRIDINECAR-BOTHIOAMIDE

<正> C12H9N2SCl, Mr= 248. 74, monoclinic, P21/n, a = 3. 902(2), b = 11.547(1), c = 25. 132(4)(?), β =93. 71(2)°, V = 1131. 1(?)3, Z = 4, Dc = 1.461, Do= 1. 45gcm-3, λ(MoKα) = 0, 71073A, μ = 4.84cm-1, F(000) = 512, R = 0. 041 for 1755 unique observed reflections. In comparison of the title molecular structure with that of N-(2-methylphenyl)-2-Pyridinecarbothipamide, the difference is insignificant. Intramolecular hydrogen bonds and short contacts are formed to the utmost extent, and the intermolecular hydrogen bonds such as C - H… S and C-H…Cl play an important role in the molecular packing. Molecular mechanics calculations (MMPM) is informative on the feature of the molecular conformation observed.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE ADDUCT OF BIS [4, 4, 4-TRIFLUORO-1-(2-THIENYL) BUTANEDIONE-1, 3] NICKEL (Ⅱ) WITH DIMETHYLSULFOXIDE, [Ni(TTA)_2(DMSO)]

<正> The title complex [Ni(TTA)2(DMSO)] (TTA = thenoyl trifluo-roacetone, DMSO=dimethyl sufloxide) belongs to triclinic, space group P1, parameters of crystal cell: a = 9.447(l), b = 10.505(1), c=11. 912(1)(?) , α=97. 42(1), β= 84. 00(1), γ = 102. 08(1)°, V = 1143. 3(?)3, Z = 2, Mr = 581. 22 [Ni (C8H4O2F3S)2(CH3)2SO)], Dc=1. 688g. cm-3, F(000) = 588, final R = 0. 065 and Rw = 0. 072 for 2873 reflections with I≥3σ(I). In the title complex the nickel atom has a square pyramidal geometry with four short Ni-O bonds and one long Ni -O (DMSO) bond.     

Crystal Structures of (18-Crown-6)-(2-Hydroxyethylammonium) Tetracyanonickelate(Ii) and 10-Amino-Decylammonium Tetracyanonickeltate(II)

Abstract

The crystal structures of the two title tetracyanonickelate(II) salts of organic ammonium ions, (18-crown-6)-(2-hydroxyethylammonium) tetracyanonickelate(II), I, and 10-aminodecylammonium tetracyano nick-elate(II), II, have been analyzed. I crystallizes in the monoclinic space group P2₁/n with a = 10.458(2), b = 8.267(3), c = 24.045(2) Å, β = 94.09(1)°, V = 2074(1) ų, Z = 2, R = 0.061 for 2274 reflections; II is triclinic P ₁ with a = 9.437(3), b = 10.094(3), c = 9.205(3)Å,a = 110.16(2), β = 112.72(3), γ = 69.16(2)°, V = 733.7(5) ų 2=1, R = 0.040 including all the hydrogen atoms refined for 2724 reflections. The square planar tetracyanonickelate(II) anion is in a favourable position to form hydrogen bonds via N with the hydroxyl group in I and the ammonio group in II, respectively.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Mo_3(μ_3-O)(μ-S)_3[S_2P(OEt)_2]_4(C_3H_3N_2)

<正> Mr=1164, space group C2/c, a=14.954(13)A,b=22.323(6)A,c=27.003(18)A,β=98.23(7)°,V=8920 A3, Z=8. Final R=0.069 for 2818 unique diffraction data with I≥30(I). The title cluster compound is of Ml configuration with a triple bridging atom O and with a 'loosely coordinated site' occupied by an imidazole ligand. Three Mo-Mo bond lengths are 2.657 (2), 2.649(2),and 2.646(2)A,respectively. The average bond length of Mo-(μ3-O) bonds is 2.052 A.     

CRYSTAL STRUCTURE OF A NEW STEROIDAL ALKALOID FROM PEIMINE,C_(27)H_(43)NO_2·H_2O

<正> Mr = 431,.6 orthorhombic,P212121,a = 8.526(2), b = 9.970(2), c= 29.787(6)X,Z=4,V=2532.0A3,Dc=1.132g.cm-3,λ(MoKα)=0.71073A,μ=0.67cm-1, F(000) = 952, final R= 0.069 for 1733 observed reflections with I>1σ(I). All six-membered rings in this free base are in the chair form and the five-membered ring C takes the envelope conformation, with the ring fusions A/B traps, B/C trans, C/D cis, D/E trans and E/F trans. There is one crystal water whose oxygen atom joins the adjacent alkaloid molecules by the inter-molecular hydrogen bonds O(1)-H... 0(3)-H(31)...0(2)=C(6). Pertinent parameters for the hydrogen bonding system are: .0(1)...0(3) 2.878(6), 0(2)...O(3) 2.917(6)A,O(1)-H...O(3) 178.3(3)°,and 0(3)-H(31)...0(2) 165.6(3)°.     

STEREOCHEMISTRY OF A DERIVATIVE OF QINGHAOSU - ARTESUNATE, C_(19)H_(28)O_8

<正> Artesunate, C19H28O8, is orthorhombic and crystallizes in the space group D24 -P212121 with a = 18.781(4), b = 10.528(5), c = 9.853(5) A, Z =4, V = 1948 A3, DC = 1.310 g.cm-3, Mr = 384, F(000) = 824, m.p.= 134°-5°, dD21.5= +12.5 (c:2%, CHCl3), μ(CuKd) = 0.0867mm-1, λ(CuKd) = 1.5418A, T =293K. The X-ray study was carried out to determine the stereochemistry at the four chiral centers and to compare the skeleton of the title compound with that of Qinghaosu. The structure was solved by direct methods and refined for the 1620 reflections with I > 2σ(I) to a final R factor of 0.067.     

Synthesis and Crystal Structure of a [Cu(HTren)Cl_2]ClO_4·H_2O Complex (Tren = Tris(2-aminoethyl)amine)

1INTRODUCTION Investigation of the coordination chemistry of copper(II)continues to be stimulated by interest in developing modes for copper proteins and in under-standing the factors which give rise to the seemingly infinite variety of distortions from regular stereo-chemistry observed in Cu(II)complexes[1,2].For more than decades,due to the unique coordination polyhedra and their easy preparation,tripodal copper complexes have attracted much attention in addition to their special chemi…     

STRUCTURE OF A NOVEL METHYLENE-BRIDGED TETRAPYRIMIDINIUM MACROCYCLIC COMPOUND (C_(24)H_(22)N_(12))·4C1·5H_2O

<正> Attempt to prepaie thiamine-metal complex resulted in a cyclic te-trapyrimidinlum tetrachloride. The retracationic macrocycle consists of four substituted pyrimidinium rings connected by methylene bridges. The cation interacts with two chloride anions at two sides of the macrocycle respectively, through the C-H....Cl hydrogen bonds and pyrimidinium ring-chloride electrostatic forces. Crystallographic data: (C24H32N12)4+·4Cl-·5H2O, Mr = 720. 49, monoclinic, C2/c, a = 10. 746 (5), b = 16.612(5), c=19. 263(4)A, β=100. 43(3)°,V = 3382(2)A3, Z = 4, Dv = 1. 41gcm-3, μ(MoKa) = 4. 1cm-1, F (000) = 1512, R = 0.057 for 1505 observed reflections (I>2σ(I)).     

THE CRYSTAL STRUCTURE OF BIS(TETRAETHYLAMMONIUM)(μ-OXO)BIS[TRIPHENYL-THIOLATO-IRON(Ⅲ)],(Et_4N)_2[Fe_2O(SPh)_6]

<正> Fe_2OSsN_2C_(52)H_(70),Mr=1043.23,monoclinic, P21/a, a=18.121(3), b=15.249(3), c=20.369(4)A,β=102.49(8)°,V=5495(1)A3, Z=4, Dc=1.261g.cm-3,MoKα(λ =0.710691), μ=17.816mm-1, F(000)=2208. R=0.073 for 4374 observed reflections with I≥3.0σ(I). The structure of the anion contains a linear Fe-O-Fe unit, with mean Fe-O distance of 1.766(2)A. The coordination geometry about each iron atom is close to tetrahedral with the angles O-Fe-S and S-Fe-S being 115.3° and 103.1°, respectively.     

STRUCTURE OF 3-(IMIDAZOLIDIN-2-YLIDENE)-4,5-DIMETHYL-4,5-DIHYDRO-2(3H)-FURANONE, C_9H_(14)O_2N_2

<正> Mr=182.25, Orthorhombic, Pna21, a=10.698(4), b=9.779(4), c=8.872(5)A, Z=4, V=928.1(7)A3, Dx=1.3 Mgm-3, λ(MoKα)=0 . 71069A, μ(MoKα) = 1.0cm-1, F(000)=392, room temperature, R=0.034 for 637 reflections. The lactone ring and imidazolidine ring are twisted mutually by 12.3°. The two methyl groups are in cis positions relative to the lactone ring. There exist intramolecular and intermolecular hydrogen bonds in the structure.