SYNTHESIS AND CRYSTAL STRUCTURE OF A NEW BINUCLEAR SIL-VER COMPLEX, [Ag_2(Py)_6(dppe)](C1O_4)_2

<正> The crystal of the title complex, Ag2Cl2P2O8N6C56H54 ,Mr= 1287. 6, belongs to triclinic system. Space group P1 with dimensions; a=10. 535(1), b= 10. 722 (3),c=12.948(2)A;α=81.25(2)°,β=81.20(1)°, γ=86.45(2)°, V=1427. 4 A3, Z= 1 ,DC= 1. 49g/cm3,F(000) = 656. 0, Mo Ka ratiation, λ=0.7107A μ = 2. 6cm-1 , The final R for 4672 reflections is 0. 043. There is a center of inversion in the molecule.     

Synthesis and Characterization of Cobalt(II), Nickel(II), and Zinc(II) Complexes with N,N ′-bis( Trans- Cinnamaldehyde)-1,2-Diiminoethane Ligand, (ca 2 en): Crystal and Molecular Structures of Co(ca 2 en)Cl 2 , Co(ca 2 en)Br 2 and Ni(ca 2 en)Br 2

A series of new complexes of the Schiff base obtained from trans- cinnamaldehyde and 1,2-diaminoethane (en) with the general formula of M(ca 2 en)X 2 (M = Co(II), Ni(II), Zn(II); X = Cl, Br, I, NCS, N 3 ; (ca 2 en) = N,N '-bis( trans- cinnamaldehyde)-1,2-diiminoethane) have been synthesized and characterized. The crystal structures of three pseudo -tetrahedral complexes, Co(ca 2 en)Cl 2 ( 1 ), Co(ca 2 en)Br 2 ( 2 ), and Ni(ca 2 en)Br 2 ( 5 ), were determined by X-ray diffraction. Crystal data for 1 , Co(ca 2 en)Cl 2 : monoclinic; space group P 2 1 / c ; a = 7.1925(14) Å, b = 20.327(4) Å, c = 14.029(3) Å; g =95.06(3)°; V = 2043.1(7) Å 3 ; Z = 4; and final R 1 = 0.0381 ( wR 2 = 0.0718) for 4653 independent reflections with I > 2 σ ( I ) and 226 parameters; 2 , Co(ca 2 en)Br 2 ; monoclinic, space group P 2 1 / c ; a = 7.3780(6) Å, b = 20.4372(17) Å, c = 14.1649(12) Å; g = 94.902(2)°; V = 2128.1(3) Å 3 ; Z = 4; and final R 1 = 0.0491 ( wR 2 = 0.1052) for 5858 independent reflections with I > 2 σ ( I ) and 227 parameters; 5 , Ni(ca 2 en)Br 2 : monoclinic, space group P 2 1 / c ; a = 7.2388(6) Å, b = 20.4651(16) Å, c = 14.2782(12) Å; g = 94.160(2)°; V = 2109.6(3) Å 3 ; Z = 4; R 1 = 0.0481 ( wR 2 = 0.0907) for 5914 independent reflections with I > 2 σ ( I ) and 227 parameters. The structures consist of discrete molecules in which the coordination polyhedra about the central metal ion are highly distorted tetrahedra with Cl(1)-Co-Cl(2), 115.51(3)°; N(1)-Co-N(2), 83.71(7)°; Br(1)-Co-Br(2), 114.58(4)°; N(1)-Co-N(2), 84.92(19)°; and Br(1)-Ni-Br(2), 125.23(3)°; N(1)-Ni-N(2), 85.11(15)° in 1 , 2 , and 5 , respectively. The stiryl groups are cis -endo with respect to the metal atom and the chelate ring is puckered. Utilization is made of electronic and vibrational spectra in structural diagnosis of other complexes.     

Syntheses and Crystal Structures of Two Trinuclear Iron(Ⅲ) Carboxylate Complexes:〔Fe_3(μ_3-O)(μ-O_2CEt)_6(H_2O)_3〕Cl·3H_2O and 〔Fe_3(μ_3-O)(μ-O_2CEt)_6Py_3〕Cl(Py=pyridine)

１ＩＮＴＲＯＤＵＣＴＩＯＮＴｒｉｎｕｃｌｅａｒｏｘｏ ｃｅｎｔｅｒｅｄｍｅｔａｌｃａｒｂｏｘｙｌａｔｅａｓｅｍｂｌｉｅｓｏｆｔｈｅｇｅｎｅｒａｌｃｏｍｐｏｓｉｔｉｏｎ〔Ｍ３（μ３ Ｏ）（μ２ Ｏ２ＣＲ）６（Ｌ）３〕ｎ＋ｈａｖｅｂｅｎｏｆｉｎｔｅｎｓｅ...     

Crystal Structure and Inhibitory Activity against Xanthine Oxidase of Bis(μ_2-chloro)-chloro-(μ-N,N'-(2-pyridylmethylene) Furanmethanoamine Copper(II) Complex

A chloro-bridged dinuclear copper(II) complex with ligand 2-pyridylme-thylene-furfurylamine has been synthesized and characterized by single-crystal X-ray diffraction, and its inhibitory activity on xanthine oxidase (XO) was also evaluated. It crystallizes in the triclinic system, space group P1 with a=8.0441(16), b=8.5663(17), c=10.060(2), α=77.52(3), β= 72.04(3), γ=70.12(3)°, V=615.3(2)3, Z=1, Dc=1.731 g/cm3, F(000)=322, the final R= 0.0401 and wR=0.0934 for 1971 observed reflections with I > 2σ(I). X-ray analysis reveals that the Cu(II) cation is five-coordinated by two N atoms of Schiff base and three Cl anions. The C-H…Cl intermolecular and intramolecular hydrogen bonds connect the molecules to form a three-dimensional network. This copper(II) complex shows more potent inhibitory activity against XO with IC50=3.48 μM than the standard inhibitor allopurinol.     

Crystal Structure of Calix［4］（dioxo） crown－6 Acetonitrile（1：3） Inclusion Complex

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＣａｌｉｘ［４］（ｄｉｏｘｏ）ｃｒｏｗｎ－６Ａｃｅｔｏｎｉｔｒｉｌｅ（１：３）ＩｎｃｌｕｓｉｏｎＣｏｍｐｌｅｘＺＨＯＮＧＺｈｅｎ－Ｌｉｎ；ＣＨＥＮＹｕａｎ－Ｙｉｎ；ＬＵＸｕｅ－Ｒａｎ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅ...     

SYNTHESIS AND MOLECULAR STRUCTURE OF Co（Ph2pyPO—N,O）2Cl2[Ph2pyPO=DIPHENYL（2—PYRIDYL）PHOSPHINE OXIDE]

<正> Complex Co(Ph2pyPO-N,O)2Cl2 was synthesized and its crystal and molecular structure was determined. Crystal data: Co(Ph2C5H5NPO-N,O)2Cl2, Mr = 688.4, monoclinic, space group A 2/a, a = 13.085(2), b = 11.134(3), c = 21.769(4)A,β=102.29(1)°,Z = 4, V = 3098.6 A3, DC = 1.476 g/cm3, final R= 0.049 and Rw=0.057 for 2804 independent reflections. The cobalt atom in the title molecules is coordinated by two chlorine atoms and two nitrogen and two oxygen atoms from the two phosphine oxide ligands, forming a distorted octahedron.     

混合三烃基锡有机酸酯化合物构效关系 （Ⅰ）二环己基－甲基－2，4－二溴－β－甲基苯氧乙酸锡酯 及二环己基－甲基－2－甲氧基－4－丙烯基苯氧乙酸锡酯的晶体结构和分子结构

报道２，４－Ｂｒ２Ｃ６Ｈ３ＯＣＨ（ＣＮ３）ＣＯ２Ｓｎ（Ｃ６Ｈ１１）２ＣＵ３（１）和２－ＯＣＨ３－４－ＣＨ３ＣＨ＝ＣＨＣ６Ｈ３ＯＣＨ２ＣＯ２Ｓｎ（Ｃ６Ｈ１１）２ＣＨ３（Ｈ２Ｏ）（Ⅱ）的晶体结构和分子结构。（Ⅰ）单斜晶系，空间群Ｐ２１／ｃ，ａ＝１３．０６７（３），ｂ＝１０．５９４（３），ｃ＝１８．１５７（４），β＝１０６．９９（２）°，Ｚ＝４，Ｄｃ＝１．６７２ｇ／ｃｍ３，Ｖ＝２４０３．７３，μ＝４３．７３１ｃｍ－１，Ｍｒ＝６２２．９９，Ｆ（０００）＝１２３２；（Ⅱ）单斜晶系，空间群Ｐ２１／ｎ，ａ＝１０．４０９（１），ｂ＝　１２．５７０（２），ｃ＝２０．６６４（２），β＝８３．５１（１）°，Ｚ＝４，Ｄｃ＝１．２８１ｇ／ｃｍ３，Ｖ＝２６８６．４Ａ３，μ＝９．７６１ｃｍ－１，Ｍｒ＝５３９．２８，Ｆ（０００）＝１１２０．最后的偏离因子，化合物（Ⅰ）Ｒ＝０．０４６，Ｒω＝０．０４６；化合物（Ⅱ）Ｒ＝０．０４９，Ｒω＝０．０４７。晶体结构解析表明，化合物（Ⅰ）和（Ⅱ）中的锡均被配体的３个碳和２个氧原子配位，配位原子呈畸变三角双锥构型；化合物中的环己基均为椅式构象；化合物（Ⅱ）中，配位水分子和另一分子的羰基氧与芳环上的甲基氧?     

STUDIES ON THE CRYSTAL STRUCTURE OF THIS(HYDROXYMETHYL)METHYLAMMONIUM SALT Ⅰ.THE CRYSTAL STRUCTURE OF THIS(HYDROXYMETHYL)METHYLAMMONIUM DIHYDROGEN PHOSPHATE(HOH2C)3CNH3H2PO4

<正> The crystal structure of tris(hydroxymethyl)methylammonium di-hydrogen phosphate(TAMP) has been determined by X-ray structural analysis.Mr = 219.13, nonoclinic, space group P21, a=8.179(l), b=6.170(2), c=9.576(5)A,β=106.32(3)°,DC= 1.57g·cm-3, Do = 1.56 g·cm3, Z = 2, MoKα radiation,λ=0.71073A, F(000)=232e,R=0.033,Rw=0.050 for 1102 reflections (I)3σ(I)).     

SYNTHESIS AND CRYSTAL STRUCTURE OF (β-PHENYL) CAR-BOXYLETHYLTRICHLOROGERMANIUM

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction. The complex crystallizes in the triclinic space group P1,a=8. 450(4),b=11. 730(3),c=14. 718(6)A ,α=104. 50(3),β=103. 71 (4),γ=69. 20(3)°,Z=4,V=1302. 4(9) A3,Dc,= 1.67g/cm3, λ(MoKa) = 0. 71069 A ,μ=30. 7/cm,F(000) = 646,Mr = 327. 6,final R=0. 037 for 2198 reflections with I<3σ(I). There are two molecules of different conformation in an asymmetric unit. Atom Ge is coordinated by three chlorine atoms and one carbon atom to form an irregular tetrahedron.     

对位取代苯甲酸酯晶体结构研究——Ⅱ.对氨基苯甲酸甲酯p-(H_2N)C_6H_4CO_2CH_3的晶体结构

对氨基苯甲酸甲酯(简写为p—MAB)晶体结构已用X射线衍射法测定。晶体属单斜晶系,空间群为C2/c,晶胞参数a=16.242(2),b=8.113(2),c=12.724(2),β=69.17(1)°;V=1567.1~3。ρobs=1.284gcm~(-3)(ρcal=1.281gcm~(-3)),Z=8。使用CAD4四圆衍射仪和MOKα射线收集强度数据,晶体结构用直接法解出,经全矩阵最小二乘修正,对于1215个I>3σ(I)的衍射点最后偏离因子R=0.050。     

THE CRYSTAL AND MOLECULAR STRUCTURE OF N,N~'-DI-n-BUTYL-29,30-DIMBTHOXY-13,27-DICHLORO-6,20-DIAZA-3,9,17,23-TETRAOXA TRICYCLIC (23.3.1.1~(11,15))-CYCLOTRIACONTANE-1(29),11,13,15(30),25,27-HEXENE

<正> C34H52N2O6Cl2, Mr=655.70, triclinic, Pl,a=8.909(5),b=9.158(5), c=11.841(9) A,α=73.41(5)°,β=76.51(8)°,γ=80.38(6)°, V = 895.1 A3, Z=l, DC=1.223 gcm-3,λ= 0.7107 A,μ=2.299 cm-1.Full matrix least-squares refinement, final R = 0.088, Rw= 0.084 for 1039 (I>36) unique reflections. The crystal is composed of separate molecules having an approximate inversion center. The molecule is shaped like an ellipse. The distances of 0(31)-0(32), 0(41)-0(42), and N(31)-N(41) are 4.254, 4.136 and 10.930 A, respectively.     

STEREOCHEMICAL STUDIES ON CYCLOHEXANONE SEMICARBAZONE DERIVATIVES II. CRYSTAL AND MOLECULAR STRUCTURES OF 4-METHYL-CYCLOHEXANONE SEMICARBAZONE AND 4-CYCLOHEXYL-CYCLOHEXANONE SEMICARBAZONE

<正> The crystal and molecular structures of 4-methyl-cyclohexanone semicarbazone (MCSC) and 4-cyclohexyl-cyclohexanone semicarbazone (CHCSC) have been determined by X-ray diffraction methods. MCSC, monoclinic, space group C2/c with a=19. 788(5), b=8.328(2), c=14. 372(4) A , β=127. 44(1)°, final R = 0. 051, Rw = 0. 057 for 801 unique reflections. CHCSC, triclinic, space group P1 with a = 5. 874(5), b = 7. 026(3), c=17. 93(1)A, α=88. 57(4)°,β = 83.08(5)°,γ=111. 66(5)°, final R = 0. 063, Rw = 0. 057 for 2144 unique reflections. The cyclohexane ring of both compounds has a slightly distorted chair conformation. The NH CONH group in both molecules shows a configuration with the C = O bonds trans to the N-NH bond with respect to the C-NH bond. The molecules in the crystals interacted with each other forming infinite ribbons through the O....H -N hydrogen bonds.     

Synthesis,Crystal Structure and Fluorescence of a Three-dimensional Cd(II) Coordination Polymer [Cd(μ_(1,3)- SCN~-)_2(μ-dmpo)]_n (dmpo = 3,5-Dimethylpyridine N-Oxide)

1 INTRODUCTION For a long time much research interest has been focused on coordination polymeric compounds[1] be- cause they may afford new materials with useful properties, such as catalytic activity, micro-porosity, electrical conductivity, non-linear optical activity, magnetic coupling behavior and so on[2]. Thiocya- nate anion, pyridine N-oxide and its derivatives be- long to very useful bridge ligands and many com- plexes[3～5] with one of them as bridge ligand exhibit special propert…     

Synthesis,Structure,Characterization and Electrochemistry of a New Dinuclear W(0)-complex 〔Et_4N〕_2〔W_2(CO)_8(SCH_2COOMe)_2〕

１ＩＮＴＲＯＤＵＣＴＩＯＮＲｅｃｅｎｔｌｙ,ｔｈｅｃｈｅｍｉｓｔｒｙｏｆｃｏｍｐｌｅｘｅｓｃｏｎｔａｉｎｉｎｇｌｏｗ ｖａｌｅｎｃｅｍｅｔａｌａｔｏｍｓｈａｓｉｎｃｒｅａｓ ｉｎｇｌｙａｔｒａｃｔｅｄｔｈｅａｔｅｎｔｉｏｎｆｒｏｍｃｈｅｍｉｓｔｓａｎ...     

主体分子2,2′-二羟基-1,1′-二萘与客体分子乙酸乙酯晶态包结物的研究

用X射线单晶衍射分析法研究主体分子2，2’-二羟基-1，l’-二萘与客体分子乙酸乙酯（3：1）晶态包结物的晶体结构。其化学式为C64H50O8，Mr=947．08。晶体属三斜晶系，空间群为P1。晶胞参数：个独立衍射点，5823个可观察点（F≥3σF）。2，2’-二羟基-1，1’-二萘与乙酸乙酯形成以氢键联系的包结物3个主体分子中的6个羟基形成21环的氢键体系。     

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 a Three-dimensional Cd(II) Coordination Polymer [Cd(μ_(1,3)-SCN)(μ_3-pco)]_n(pco=Pyrazine-2-carboxylate 4-oxide Anion)

1 INTRODUCTION For a long time much research interest has been focused on coordination polymeric compounds[1] because these new coordination polymers may afford new materials with useful properties, such as catalytic activity, micro-porosity, electrical conduc- tivity, non-linear optical activity, magnetic coupling behavior and so on[2]. Thiocyanate anion is a very useful bridging ligand, and many complexes[3～5] are synthesized with it as bridging ligand and some of them exhibit interesti…     

Synthesis and Crystal Structure of a Novel Hetero-bimetallic Complex with a Three-dimensional Network Structure: Bis(malonato)tetra(aqua)calcum(II)cobalt(II)

1INTRODUCTION There has been considerable interest in the designand synthesis of transition metal complexes withcarboxylate ligands in coordination chemistry due tothe fact that this type of complexes has potentialapplications in molecule-based magnets,catalysis,supramolecular chemistry and biological systems[1～3].As an important flexibility dicarboxylate ligand,malonate dianion may act as momodentate,chelatedbidentate and tridentate bridging ligands to formvarious1D,2D and3D structures[…     

Crystal Structure of 2-〔(P,P-Diphenoxy)phosphono(p-methyl)benzyl〕-1,2-benzisoselenazol-3(2H)-one

１ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｒｅｃｅｎｔｙｅａｒｓｂｉｏｌｏｇｉｃａｌｙａｃｔｉｖｅｏｒｇａｎｏｓｅｌｅｎｉｕｍｃｏｍｐｏｕｎｄｓｈａｖｅｂｅｇｕｎｔｏａｔ ｔｒａｃｔｃｏｎｓｉｄｅｒａｂｌｅｉｎｔｅｒｅｓｔｄｕｅｔｏｔｈｅｉｒｕｎｉｑｕｅａｎｄｄ...     

STRUCTURE OF NEODYMIUM TRINITRATE WITH DIPHENYL SULFOXIDE LIGANDS, Nd(N0_3)_3·[(C_6H_5SO]_4

<正> Mr=2278, triclinic, Pl, a=11.154(1), b=14.310(2), c=17.295(2) A, α=84.09(1)°, β=72.97(1)°, r=69:37(1)°, V=2470.2(5)A3, Z=2; 2(MoKα)=12.9cm-1 F(000)=1154, Dx=1.53 g/cm3, room temperature. The final R=0.039, Rw=0.039 with wt=1, S=2.57 for 5710 independent reflections with | Fα|≥2.5σ(F0). The molecular configuration of the Nd-complex is similar to those of the Sm-complex and Pr-complex except for the difference in distances between central metal and the coordinated oxygen atoms.