Syntheses and Structures of Two Cadmium Complexes with Isophthaloylbisglycine Acid and 4,4'-Bipyridine

The two title complexes [{Cd（IBG-CH3）（4,4＇-bipy）（H2O）2}·NO3]n 1 and [{Cd（IBG）- （4,4＇-bipy）（H2O）2}·2H2O]n 2 （H2IBG = isophthaloylbisglycine and 4,4＇-bipy = 4,4＇-bipyridine） have been synthesized and characterized by single-crystal structure determination,IR and TG analyses. Complex 1 crystallizes in monoclinic,space group C2/c with a = 27.221（2）,b = 11.6093（7）,c = 16.3571（9）A,V = 5149.2（6） A^3,Z = 8,C23H23N5O11Cd,Mr = 657.86,Dc = 1.697 g/cm^3,F（000） = 2656.00,μ（MoKα） = 0.919 mm^-1,the final R = 0.0478 and wR = 0.0882 for 3728 observed reflections with I 〉 2σ（I）. Complex 2 crystallizes in triclinic,space group Pī with a = 9.0940（4）,b = 11.6852（5）,c = 13.1119（6）A,V = 1230.26 A^3,Z = 2,C22H26N4O10Cd,Mr = 618.87,Dc = 1.671 g/cm^3,F（000） = 628.0,μ（MoKα） = 0.951 mm^-1,the final R = 0.0567 and wR = 0.1124 for 3713 observed reflections with I 〉 2σ（I）. In both structures,the CdII metal centers are coordinated by seven atoms to form a distorted pentagonal bipyramidal geometry.     

Crystal Structures of N，N＇－Bis（4－chlorophenyl）－1，10－diaza－18－crown－6 and Its Complexwith Ba（SCN）_2

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｓｏｆＮ，Ｎ＇－Ｂｉｓ（４－ｃｈｌｏｒｏｐｈｅｎｙｌ）－１，１０－ｄｉａｚａ－１８－ｃｒｏｗｎ－６ａｎｄＩｔｓＣｏｍｐｌｅｘｗｉｔｈＢａ（ＳＣＮ）_２￥ＺｈａｎｇＬｉ－Ｊｕａｎ；ＬｉｕＸｉａｏ－Ｌａｎ；ＭａＳｈｉ－Ｋｕ?..     

Syntheses and Crystal Structures of 1,5-Disubstituted 1,3,5-Hexahydro-triazine-2-（N-nitro）imines

The title compounds,C9H13ClN6O2S 1 and C15H17ClN6O2S 2,were synthesized and structurally characterized by elemental analysis,IR,1H NMR spectra and single-crystal X-ray diffraction.Compound 1 is in the monoclinic system,space group P21/c with a=13.7711(5),b=10.3883(4),c=9.7623(2),V=1344.47(8)3,Dc=1.506 g/cm3,C9H13ClN6O2S,Mr=304.76,F(000)=632,μ=0.448 mm-1,Z=4,S=1.084,R=0.0497 and wR=0.1328 for 2640 unique reflections(Rint=0.0787) with 2089 observed ones(I2σ(I)).Compound 2 belongs to the monoclinic system,space group P21/n with a=8.3828(5),b=14.5285(7),c=14.2456(4),V=1729.74(14)3,Dc=1.462 g/cm3,C15H17ClN6O2S,Mr=380.86,F(000)=792,μ=0.364 mm-1,Z=4,S=1.057,R=0.0598 and wR=0.1582 for 3384 unique reflections(Rint=0.0469) with 2833 observed ones(I2σ(I)).Compounds 1 and 2 are homologues and stabilized by intermolecular and intramolecular hydrogen bonds.Moreover,compound 2 containing C(2)-H(2)…π(thiazole) interaction is more stable than 1.     

Hydrothermal Synthesis,Crystal Structure and Properties of a Novel Polyoxometalate {[Cu~Ⅱ(1,10-phen)]_2[PMo~Ⅵ_(11)Mo~ⅤO_(40)]} [Cu~Ⅰ(C_8N_4H_6)(C_9H_6NO)(H_2O)]

A new pseudo three-dimensional framework structure of the title compound {[CuⅡ(1,10-phen)]2[PMoⅥ11MoⅤO40]}[CuⅠ(C8N4H6)(C9H6NO)(H2O)](1) has been prepared by the hydrothermal method for the first time and characterized by elemental analyses,X-ray single-crystal diffraction and IR spectra.1 consists of two building blocks,one {[CuⅡ(1,10-phen)]2[PMoⅥ11MoⅤO40]} and one [CuⅠ(C8N4H6)(C9H6NO)(H2O)] coordinated group.Singlecrystal X-ray diffraction revealed that 1 crystallizes in the monoclinic system,space group P2/c with a=13.498(4),b=12.890(3),c=21.465(8),β=97.314o,V=3704(2)3,Mr=2693.61,Z=2,Dc=2.415 Mg/m3,μ=2.915 mm-1,F(000)=2562,S=1.009,the final R=0.0583 and wR=0.1406 for 5129 observed reflections with I2σ(I).Furthermore,compound 1 shows strong fluorescent properties in the solid state at room temperature.The electrochemical behavior of 1 has also been studied by cyclic voltammograms.     

Syntheses and Crystal Structures of Two New Compounds:[Zn(2,2'-bipy)(L)CI]_2 and [Zn(phen)(L_2)]_2(HL-3-Methylbenzoic Acid)

Compounds [Zn(2,2'-bipy)(L)CI]_2 1 and [Zn(phen)(L_2)] _2 2 (2,2'-bipy = 2,2'-bipy-ridine, HL = 3-methylbenzoic acid, phen = 1,10-phenanthroline) have been synthesized under hy-drothermal conditions. 1: monoclinic, space group C2/c, α = 20.240(4), b = 9.2960(19), c = 17.904(4) A, β = 92.63(3)°, V= 3365.1(12) A3, C_(36)H_(30)Cl_2)N_4O_4Zn_2, M_r = 784.32, Z = 4, D_c = 1.548 g/cm~3,μ = 1.631 mm~(-1), F(000) = 1600, the final R= 0.0367 and wR = 0.1289 for 3867 observed reflections (I > 2σ(I). 2: monoclinic, space group C2/c, α = 23.035(5), b = 9.0395(18), c = 23.799(5)A, β = 98.55(3)°, V= 4900.6(17) A~3, C_(56)H_(44)N_4O_8Zn_2, M_r = 1031.73, Z = 4, D_c = 1.398 g/cm~3, μ= 1.039 mm~(-1), F(000) = 2128, the final R= 0.0540 and wR = 0.1287 for 5002 observed reflections (I> 2σ(I). The two compounds have the same space group and similar isolated dinuclear structure, but different space packing structures are formed by different weak intermolecular interactions. Mo-reover, IR and luminescence spectra are also employed to study the crystal structures and pro-perties of these two compounds.     

二维网状结构双核配合物[Ca_2(C_(10)H_8N_2O_4)_2(DMSO)_2(H_2O)_4]·2DMSO的合成、热分解及晶体结构

以2-羰基丙酸水杨酰腙(C_(10)H_(10)N_2O_4)作为配体与碳酸钙在水中反应， 在DMF(N,N'-二甲基甲酰胺)和DMSO（二甲基亚砚）的混合溶剂中培养了单晶，其组 成为 [Ca_2(C_(10)H_8N_2O_4)_2(DMSO)_2(H_2O)_4]·2DMSO [C_(10)H_8N_2O~2- _4为2-羰基丙酸水杨酰腙负离子]。测字了单晶的结构，该单晶为黄色，属单斜晶 系，空间群为P2(1)/C，晶胞参数a=1.0634(3)nm, b=1.7035(5)nm, c=1.2183(3) nm, β=106.180(5)°, V=2.1192(10)nm!, Dc=1.412Mg·m~(-3), Z=2, F(000) =944, μ=0.534m~(-1)，GOF=0.867。所测单晶是以2-卷曲在丙酸水杨酰腙羧基上 的一个氧原子作为桥联的双核钙（II）配合物，两个Ca~(2+)均处于五角双锥的七 配位环境中，锥底为配体2-羰基丙酸水杨酰腙中的三个配位原子，以及另一2-羰基 丙酸水杨酰腙羧基上的桥联氧原子和一个水分子的配位氧原子，锥顶为一配位水和 一想位的DMSO分子，即溶剂DMSO也参也了配位，从晶胞结构看，晶体中除配位的 DMSO分子外，还有自由的DMSO溶剂分子，它们与配位水以氢键连接存在于晶格之中 ，在空间形成的二维网状结构。通过TG-DTG还测定了配合物的热稳定性。     

Synthesis and Crystal Structure of［Na（DB18C6）（H_2O）_2］_2Mo_6O_（19）·3DMF·2CH_3OH

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｎａ（ＤＢ１８Ｃ６）（Ｈ_２Ｏ）_２］_２Ｍｏ_６Ｏ_（１９）·３ＤＭＦ·２ＣＨ_３ＯＨＬｕＸｉａｏ－Ｍｉｎｇ；ＺｈａｏＹａ－Ｐｉｎｇ；ＱｕＥｒ－Ｌｉｎｇ；ＸｉａｏＬｉｎｇ－Ｍｅｉ；ＬｉｕＳｈｕ...     

Crystal and Molecular Structure of Methylene－bis［benzobicyclo（diaza－diphenyl）stannoxide］，［o－O■n（C_6H_5）_2］_2CH_2·1／2C_6H_6

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆＭｅｔｈｙｌｅｎｅ－ｂｉｓ［ｂｅｎｚｏｂｉｃｙｃｌｏ（ｄｉａｚａ－ｄｉｐｈｅｎｙｌ）ｓｔａｎｎｏｘｉｄｅ］，［ｏ－Ｏ■ｎ（Ｃ_６Ｈ_５）_２］_２ＣＨ_２·１／２Ｃ_６Ｈ_６ＷａｎｇＪｉ－Ｔａｏ；?..     

Crystal Structure of Catena-poly-[2,2'-bisbenzimidazole Mn(Ⅱ)-μ-Benzene-1,3-dicarboxylato]

The title complex,[(BBI)Mn(BDC)]n 1(BBI = 2,2'-bisbenzimidazole(C14H10N4),BDC=benzene-1,3-dicarboxylate dianion(C8H10O4)),crystallizes in the monoclinic system,space group C2/c,with a=17.822(8),b=16.181(7),c=13.355(6),β=92.112(5)°,V=3848.67(304)3,Z=8,C22H14MnN4O4,Mr=453.31,Dc=1.565 g/cm3,F(000)=1848,μ=0.725 mm-1,S=1.000,the final R=0.0310 and wR=0.0589.1 contains hydrogen bonds and π-π stacking interactions between the neighboring aryl-ring of BBI's,which helps to form a three-dimensional crystal structure.     

二维无机－有机杂化层网骨架晶体的合成与结构

在温和条件下合成了二维层网结构的无机－有机杂化晶体Zn(BDC)(C_3H_3N_2) ·(DMF)(1)和Co_2(BDC)_2(C_5H_5N)_4·2(DMF)·(C_5H_5N)·(C_5H_5N) (2)，并 通过ICP和X射线单晶衍射分析等手段对其结构进行了表征。1的晶胞数据：C_(14) H_(14)N_3O_5Zn, M_r = 369.65，单斜晶系，C2/c空间群，晶胞参数a = 2.1059 (4) nm, c = 1.4836(3) nm, β = 99.09(3)°，V = 3.1826(11) nm~3, Z = 4, D_X = 1.543 Mg/m~3, μ = 1.571 mm~(-1), F(000) = 1512。最后的一致性因子 为R = 0.0697, R_w = 0.2018。2的晶胞数据：C_(47)H_(47)N_7O_(10)Co_2, M_r = 987.78，单斜晶系，P2(1)/n空间群，晶胞参数a = 1.0829(2) nm, b = 1. 5431(3) nm, c = 1.4428(3) nm, β = 101.65(3)°，V = 2.3612(8) nm~3, Z = 2, D_X = 1.391 Mg/m~3, μ = 0.767 mm~(-1), F(000) = 1024。最后的一致性 因子为R = nm, β = 101.65(3)°, V = 2.3612(8) nm~3, Z = 2, D_X = 1.391 Mg/m~3, μ = 0.767 mm~(-1), F(000) = 1024。最后的一致性因子为R = 0. 0652，R_w = 0.1888。1和2的结构都是由无机簇M_2(CO_2)_4(M = Zn, Co)通过苯 环连接而形成的层网结构。它们都存在由4个无机簇与4个苯环形成的环，其大小约 为0.9 nm * 0.9 nm。由于咪唑和吡啶分别与1和2无机簇的两极配位，阻止了它们 形成三维骨架结构。     

Synthesis,Structure and Magnetic Property of a Binuclear Nickel(Ⅱ) Complex

A new binuclear complex [Ni2(2,2'-bpy)2(C8H3NO6)2(H2O)4] 1 (2,2'-bpy = 2,2'- bipyridine, C8H3NO6 = 4-nitrophthalate) has been synthesized by a hydrothermal reaction and characterized by X-ray single-crystal diffraction analysis. The complex crystallizes in triclinic, space group P1 with a = 7.206(2), b = 10.337(4), c = 12.480(4) , α = 89.887(11), β = 77.033(9), γ = 78.349(6)o, V = 886.3(5) 3, Z = 1, C36H30Ni2N6O16, Mr = 920.08, Dc = 1.724 g cm-3, F(000) = 472, μ = 1.152 mm-1, the final R = 0.0458 and wR = 0.1163 for 3372 observed reflections with I 2σ(Ⅰ). The two Ni(Ⅱ) ions are bridged by two 4-nitrophthalates both in a bis-monodentate mode. Magnetic measurements reveal that the intramolecular exchange couplings in the dimer are ferromagnetic with 2J/k = 2.32 K, D =-1.44 K and g = 2.18.     

Synthesis and Crystal Structure of 1，5－Bis（1＇－phenyl－3＇－methyl－5＇－pyrazolone－4＇）－1－（4＇－aminobutand－1＇－imino）－5－pentaneone

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ１，５－Ｂｉｓ（１＇－ｐｈｅｎｙｌ－３＇－ｍｅｔｈｙｌ－５＇－ｐｙｒａｚｏｌｏｎｅ－４＇）－１－（４＇－ａｍｉｎｏｂｕｔａｎｄ－１＇－ｉｍｉｎｏ）－５－ｐｅｎｔａｎｅｏｎｅ￥ＹａｎｇＬｕ－Ｑ...     

顺式-二 (乙二胺 )二硝基合钴 (Ⅲ ) (d,l)酒石酸盐的合成与晶体结构

合成顺式 -二 (乙二胺 )二硝基合钴 (Ⅲ )酒石酸盐cis [Co(en) 2 (NO2 ) 2 ]·1/2C4 H4 O6超分子化合物 ,(C6H18N6O7Co ,Mr=345 .2 ) ,用X射线衍射方法确定了晶体结构。晶体学参数 :单斜晶系 ,空间群P2 1/a ,a =13.90 1(3) ,b =6 .5 2 5 (5 ) ,c=14 483(4 ) ,β =10 1.13(2 )°,V =12 89.1(4 ) 3,Z =4,Dc=1.779g/cm3,μ(CuKα) =10 6 .6 9cm- 1,F(0 0 0 ) =72 0。结构由重原法、直接法和Fourier合成法解出 ,最终偏离因子R =0 .117,Rw=0 .0 74。Co(Ⅲ )与 6个N原子形成变形八面体构型 ,酒石酸阴离子处在 4个Co(Ⅲ )正离子所包围的空穴中。     

Template Synthesis and Structure of Dinuclear Zinc Complex with Three Kinds of Pyrazole Ligands

ＴｅｍｐｌａｔｅＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆＤｉｎｕｃｌｅａｒＺｉｎｃＣｏｍｐｌｅｘｗｉｔｈＴｈｒｅｅＫｉｎｄｓｏｆＰｙｒａｚｏｌｅＬｉｇａｎｄｓＺＨＡＮＧＷｅｎ－Ｘｉｎｇ；ＭＡＣｈａｎｇ－Ｑｉｎ；ＷＡＮＧＸｕ－Ｎｉｎｇ；ＹＵＺｈｅ...     

A 3D Supramolecular Framework Based on 1D {[Co（proH）（H2O）3]2[P2Mo5O23]}n Chains and 1D Helical Water Chains

A three-dimensional supramolecular architecture, {[Co（proH）（H2O）3]2[P2Mo5O23]}·7H2O （1, pro = praline）, has been synthesized and characterized by IR, elemental analysis, thermogravimetric analysis, and single-crystal X-ray diffraction. 1 crystallizes in monoclinic, space group C2 with a = 20.600（3）, b = 11.6980（11）, c = 9.2944（10）A, β = 107.837（4）°, V = 2132.1（4） A^3, Z = 2, C10H46Co2Mo5N2O40P2, Mr = 1493.99, Dc = 2.327 g/cm^3, F（000） = 1468, μ（MoKα） = 2.375 mm^-1, the final R = 0.0339 and wR = 0.0844 for 4169 observed reflections with I 〉 2σ（I）. Singlecrystal X-ray crystallographic analysis reveals that the helical water chains and {[Co（proH）- （H2O）3]2[P2Mo5O23]}n chains are perpendicular to each other and extend into an overall three-dimensional supramolecular architecture by hydrogen-bonding interactions. The magnetic investigation indicates weak antiferromagnetic interactions in the compound.     

Crystal Structure of N－（N－Phenylthiazotone）imino－O－ethyl－N－isopropylaminothiophosphate

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＮ－（Ｎ－Ｐｈｅｎｙｌｔｈｉａｚｏｔｏｎｅ）ｉｍｉｎｏ－Ｏ－ｅｔｈｙｌ－Ｎ－ｉｓｏｐｒｏｐｙｌａｍｉｎｏｔｈｉｏｐｈｏｓｐｈａｔｅ￥ＹａｎｇＨｕａ－Ｚｈｅｎｇ；ＬｉｕＨｕａ－Ｙｉｎ；ＷｕＹｅ（Ｉｎｓｔｉｔｕｔｅｏｆ...     

Synthesis,Crystal Structure and Fluorescent Property of 2,2＇-Bipyridyl-3,3＇- bis（N,N＇-disalicylidene）-formyhydrazone

A binicotinic biscarbohydrazone compound,2,2＇-bipyridyl-3,3＇-bis（N,N＇-disali- cylidene）-formyhydrazone,1 has been prepared and characterized by elemental analysis,FT-IR,1H- NMR,ESI-MS and single-crystal X-ray diffraction analysis. The crystal belongs to triclinic,space group P1 with a = 9.419（3）,b = 11.745（4）,c = 12.035（5）A,V = 1178.8（7）A^3,Z = 2,Dc = 1.354 g/cm^3,μ = 0.095 mm^-1,F（000） = 500,λ（MoKα） = 0.71073 ,C26H20N6O4,Mr = 480.48,the final R = 0.0480 and wR = 0.1084 for 3634 observed reflections with I 〉 2σ（I）. Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 1 has been constructed by multiply intermolecular N–H···N and O–H···O H-bonding interactions. Besides,compound 1 exhibits a strong green-light emission in the solid state at room temperature.     

氰尿酸镍的晶体结构

标题化合物Ｎｉ（Ｃ＿３Ｈ＿２Ｎ＿３Ｏ＿３）＿２（Ｈ２Ｏ）＿４属正交晶系，空间群为Ｆｍｍｍ（编号６９）。晶胞参数：ａ＝７．２８２（４），ｂ＝１２．０５７（２），ｃ＝１６．０７２（２），Ｖ＝１４１１（１），Ｄ＿ｃ＝１．８２ｇ／ｃｍ￣３，Ｚ＝４，Ｍ＿ｒ＝３８６．８９，λ（ＭｏＫα）＝０．７１０６９，μ＝１４．４３ｃｍ￣（－１），Ｆ（０００）＝７９２。最终偏离因子Ｒ＝０．０４５，Ｒ＿ｗ＝０．０６０。独立可观测点数（Ｉ≥３σ（Ｉ））为３８５个。在配合物中，镍离子与来自氰尿酸的两个氮原子和来自水分子的四个氧原子配位。     

Crystal Structure of Bis(3-hydroxy-2-pyridyl)disulfide

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＢｉｓ（３－ｈｙｄｒｏｘｙ－２－ｐｙｒｉｄｙｌ）ｄｉｓｕｌｆｉｄｅＣｈｅｎＸｕｅ－Ｔａｉ；ＫａｎｇＢｅｉ－Ｓｈｅｎｇ；ＸｕＹｏｎｇ－Ｊｉｎ；ＨｕＹｏｎｇ－Ｈａｎ（ＳｔａｔｅＫｅｙＬａｂｏｒａｔｏｒｙｏｆＳｔｒｕｃｔ...     

Synthesis and Crystal Structure of a New Tetracopper Complex [Cu(H_2O)_3Cu(HCDTA)]_2(ClO_4)_2·H_2O

A new tetracopper complex [Cu(H2O)3Cu(HCDTA)]2(ClO4)2·H2O (CDTA = transcyclohexane-1,2-diamine-N,N,N′,N′-tetraacetate) has been prepared and characterized by singlecrystal X-ray diffraction analysis. The crystal adopts space group C2/c with a = 16.990(10), b = 9.150(5), c = 29.318(17) , β = 104.289(9)°, V = 4417(4) 3, Z = 4, C28H52Cl2Cu4N4O31, Mr = 1265.80, Dc = 1.904 g/cm3, μ = 2.130 mm-1, F(000) = 2584, T = 293(2) K, the final R = 0.0328 and wR = 0.0809 for 4938 observed reflections (I 2σ(I)). The tetracopper units are interconnected by weak covalent bonds into a layered structure.