吗啉二硫代氨基甲酸铁(Ⅲ)配合物Fe(S2CNC4H8O)3的合成、表征及晶体结构

合成了标题化合物Fe(S2CNC4H8O)3,得到黑色柱状晶体.晶体属三斜晶系,空间群为P-1,晶胞参数a=O.9300(2)nm,b=1.0490(2)nm,c=1.3710(3)nm,a=100.60(3)°,β=95.40(3)°,γ=106.60(3)°,V=1.2445(4)nm3,Mr=542.58,Z=2.中心Fe原子分别与来自三个吗啉二硫代氨基甲酸的六个硫原子配位形成八面体构型,由于四元螯合环的环张力,导致该八面体严重变形,六个Fe-S键的键长范围在0.2423(5)～O.2458(2)nm.热分析表明标题化合物在791.80℃完全分解.     

(R)-N-乙酰基-四氢噻唑-2-硫酮-4-甲酰TT的合成及其晶体结构

由N-乙酰(R)-四氢噻唑-2-硫酮-4-羧酸在三聚氯氰及三乙胺存在下与四氢噻唑-2-硫酮反应得到标题化合物，[α]^2^0~D +11.18°。用X射线衍射法测得其晶体结构，属单斜晶系，空间群为P2~1/c。晶体学数据：a=0.9959(4)nm，b=1.1469(4)nm，c=1.1108(3)nm，β=92.72(3)°，V=1.2673(8)nm^3，Z=4。分子中两个C=O基，两个C=S基团处于C(1)-N(1)-C(4)及C(6)-N(2)-C(7)键两侧呈反式。用PM3分子轨道方法研究了该化合物的电子结构，电荷和键序分布，得到该化合物前线轨道性质。     

N´-乙基-N-哌嗪基二硫代氨基甲酸钴(Ⅲ)配合物Co(S2CNC4H8NC2H5)3·3H2O的合成、表征及晶体结构

合成了标题化合物Co(S₂CNC₄H₈NC₂H₅)₃·3H₂O,得到黑色四棱柱状晶体。晶体属三方晶系, 空间群为R-3, 晶胞参数a=1.37700(19), b=1.37700(19), c=3.0090(6) nm, γ=120°, M_r=680.98, V= 4.9411(14) nm³, Z=6, D_c=1.373 g/cm³, F(000)=2160, R = 0.0510 和 wR = 0.1436。中心Co原子分别与来自三个N´-乙基-N-哌嗪基二硫代氨基甲酸的六个硫原子配位形成略微扭曲的八面体构型。六个Co-S键的键长范围在0.22682(13)~0.22703(14) nm, 热分析表明标题化合物在799.97°C完全分解。     

(μ-σ,π-反式-C_6H_5CH=CH)(μ-C_2H_5S)Fe_2(CO)_6的分子和晶体结构

标题化合物由[(μ-CO)(μ-C_2H_5S)Fe_2(CO)_6](C_2H_5)_3NH和反式或反式-C_6H_5CH=CHBr制得。其晶体属空间群C_c;a=1.8053 nm,b=1.0436 nm,c=1.9045 nm;β=93.68°;D_c=1.66g/cm~3;Z=8;R=0.0413。Fe—Fe键长为0.2542nm,苯乙烯基配体的C=C双键为0.1358 nm,乙基以e-键与硫桥原子相连。     

1,1,1-三[3-（2-苯并咪唑基）-2-氧杂丙基]丙烷镍配合物合成以及结构测定

合成了一个新的三脚架结构配体及其镍配合物的晶体。该晶体属单斜晶系， P2_l/n空间群，a = 1.2151(4) nm, b = 1.5535(5) nm, c = 2.1740(7) nm, β = 90.551(18)°, V = 4.103(2) nm~3, Z = 4, M_r = 834.03, R = 0.0556, wR = 0.1256, μ = 0.541 mm~(-1), F(000) = 1758。配合物中Ni与配体的三个N和 三个O构成六配位变形八面体结构。晶体中存在着分子间氢键，晶体结构依靠库仑 力和氢键作用而稳定。     

(R)-N-(β-三氯锗丙酰基)四氢噻唑-2-硫酮-4-羧酸甲酯的合成及其晶体结构

三氯锗丙酰氯与(R)-四氢噻唑-2-硫酮-4-羧酸甲酯反应, 得到标题化合物1, [α]~D^2^0-89.40°。经水解得到取代丙酰四氢噻唑-2-硫酮-4-羧酸甲酯基锗倍半氧化物2, X射线衍射法测出标题化合物的晶体结构, 属于正交晶系, 晶胞参数: a=0.6192(1)nm,b=1.1147(4)nm,c=2.1796(8)nm, V=1.5045nm^3, Z=4, 空间群P2~12~12~1。分子中酰胺羰基C=O与C=S基团处于C(4)NC(3)键两侧呈反式。用MNDO分子轨道方法研究了该化合物的电子结构, 电荷和键序分布,前沿轨道性质,讨论了电子光谱性质。     

三苄基锡哌啶氨荒酸酯和二苄基锡双哌啶氨荒酸酯合成及晶体结构

利用三苄基氯化锡，二苄基二氯化锡和哌啶氨荒酸钠反应，合成了三苄基锡哌 啶氨荒酸酯（1）和二苄基锡双哌啶氨荒酸酯（2）。通过元素分析、红外光谱、核 磁共振氢谱和质谱对其结构进行了表征。用X-射线单晶衍射测定了这两个化合物的 晶体结构。化合物1为三斜晶系，空间群P-1，a=1.0271(2)nm,b=1.1131(2)nm,c=1. 2096(2)nm,α=75.56(3)°，β=81.09(3)°，γ=89.81(3)°，Z=2。化合物2为单 斜晶系，空间群P21/c,a=0.9710(3),b=2.436(1),c=1.2393(3)nm,β=90.28(2)°， Z=4。在1的晶体中， 锡原子呈五配位畸变三角双锥构型；2的晶体则是六配位的畸 变八面体构型。     

1,1,1-三[3-（2-苯并咪唑基）-2-氧杂丙基]丙烷镍配合物合成以及结构测定

合成了一个新的三脚架结构配体及其镍配合物的晶体。该晶体属单斜晶系, P2_l/n空间群,a = 1.2151(4) nm, b = 1.5535(5) nm, c = 2.1740(7) nm, β = 90.551(18)°, V = 4.103(2) nm~3, Z = 4, M_r = 834.03, R = 0.0556, wR = 0.1256, μ = 0.541 mm~(-1), F(000) = 1758。配合物中Ni与配体的三个N和 三个O构成六配位变形八面体结构。晶体中存在着分子间氢键,晶体结构依靠库仑 力和氢键作用而稳定。     

2-膦酸基-1,2,4-三羧酸丁烷的晶体结构及阻垢性能研究

合成了标题化合物,得到了晶胞中含水分子的无色柱状晶体。晶体属单斜晶系,空间群为P21/c,晶胞参数a=1.0371(2)nm,b=0.86370(17)nm,c=1.3713(3)nm,β=103.60(3)°,Mr=297.15,V=1.1939(4)nm3,Z=4,Dc=1.653g/cm3,F(000)=620,R=0.0528,wR=0.1572。P原子分别与三个O原子和一个C原子相连,形成四面体构型;2-膦酸基-1,2,4-三羧酸丁烷和水分子之间通过分子间氢键形成一维网络;三个P-O键的键长范围在0.1493(2)～0.1574(2)nm。热分析表明,标题化合物在799.65℃时,失重率为81.146%,分解为P2O3。标题化合物的结构中含有一个膦酸基、三个羧酸基,且分别在C1原子的四个不同方向,因此空间位阻小,对Ca2 的螯合能力优于HEDP和ATMP等,故其综合阻垢性能优于其它仅含有膦酸基的有机磷酸盐。     

(Z)-1-[2-(二苯基碘化锡基)乙烯基]-1-环己醇的合成、晶体结构和性质

报道了标题化合物的合成、晶体结构及性质。该晶体属于单斜晶系，空间群为P2~1，晶胞参数a=0.9255(3)nm，b=1.0504(3)nm，c=1.0217(3)nm，β=100.99(2)°，V=0.9750nm^3，Z=2，D~c=1.790g/cm^3，R=0.025，晶体结构由直接法解出。标题化合物分子中的锡原子被配体的三个碳、一个碘和一个氧原子配位；配位原子是畸变的三角双锥构型；标题化合物具有与卤素发生取代反应而不发生加成反应的性质。     

Crystal Structure and Spectroscopic Studies of Bis (morpholine dithiocarbamate) Nickel(II) Complex,Ni(C4H8ONCS2)2

The title compound has been prepared and characterized by EA, IR and TG spectral studies. The crystal structure of nickel (H) bis(morpholine dithiocarbamate) Ni(C₄H₅ONC‐S₂)₂ is determined by X‐ray diffraction methods. It crystallizes in the monoclinic system, space group P2₁/n, with lattice parameters a = 0.4288(1), b = 2.0526(4), c = 0.8333 (2) nm, β = 97.43(3)°, and Z = 2. In the structure, central Ni atom coordination geometry is slightly distorted square‐planar with the four S atoms from two morpholine dithiocarbamate ligands. The four Ni? S bond distances are in the range of 0.2199(5)–0.2201(2) nm. The ER spectral data are in agreement with the structural ones. The TG data indicate that it decomposed completely at the 766.89°C.     

Crystal Structures and Characterizations of Bis（1-benzoyl-methyl-benzotriazole-N^3）dichoro Metal（Ⅱ） Complex： [MCl2（C6H4N3CH2COPh）2] [M=Zn（Ⅱ），Co（Ⅱ）]

The structures of [MCl₂(C₆H₄B₃CH₂COPh)₂] [M=Zn(II) (1), Co(II) (2)] have been determined by X‐ray crystallography. They were characterized by elemental analysis, IR spectrum, electronic spectrum and thermogravimetric‐differential thermal analysis. They all crystallize in the triclinic system, space pup Pi, with lattice parameters a=0.9449(2) nm, b=1.1291(2) nm, c=1.3637(3) nm, α=111.70(3)°, β= 94.33(3)°, y=90.97(3), Z=2 for compound 1; a=0.9437(2) nm, b= 1.1277(2) nm, c= 1.3650(3) nm, a=111.76(3)°, β=94.50(3)°, y=90.80(3)°, Z=2 for compound 2. The metal ions are all coordinated by two C1^?‐ anions and two nitrogen atoms of 1‐benzoylmethyl‐bentriazole ligands. forming the distorted tetrahedral geometry. The Zn—Cl and Zn—N bond lengths are 0.2209(2), 0.2210(2) nm and 0.2059(4), 0.2067(4) nm. respectively. The CO‐Cl 3 and Co–N bond lengths are 0.2215(2). 0.2222(2) nm and 0.2028(5), 0.2045(5) nm. respectively. The thermogravimetric (TG) data indicate that they are nearly similar in TG curve, and there are not structural transitions in the two compounds. They all have a high thd stability. But, there is little difference in DTG (differential thermogravimetric) curves of those two compounds. Elemental analysis, electronic and IR spectra are in agreement with the structural data.     

新型鼓状有机锡氧杂环羧酸簇合物[PhCH2Sn(O)(O2CC4H4N)]6·2CH2Cl2的合成和晶体结构

利用三苄基氧化锡与2-吡咯甲酸反应，合成六聚体-苄基锡氧2-吡咯甲酸酯簇 合物．通过元素分析、红外光谱、核磁共振氢谱和X射线单晶衍射对其结构进行了 表征．X射线单晶衍射测试结果表明：化合物为三斜晶系，空间群P1^-，α＝1． 2644(3)nm，b＝1．7416(4)nm，c＝1．9285(4)nm，α＝90．021(4)°，β＝94． 585(4)°，γ＝90．021(4)°，Z＝2，V＝4．2330(16)nm^3，Dc＝1．715g／cm^3 ，μ＝1．936mm^-1，F(000)＝2136，R＝0．0527，wR＝0．0708．该化合物为鼓型 簇状结构，锡原子为畸变的八面体构型．     

[Cu(Phen)_3][DTB]·6H_2O的合成与晶体结构

利用螯合配体1,10-邻菲咯啉(Phen)与2,2′-二硫代二苯甲酸(H2DTB)的钠盐及氢氧化铜反应合成了一种新型配合物[Cu(Phen)3][DTB].6H2O,通过元素分析、红外光谱和X射线单晶衍射等技术对其进行了表征.配合物属单斜晶系,空间群P2(1)/c,晶胞参数:a=1.822(2)nm,b=3.053(4)nm,c=2.016(3)nm,α=90°,β=106.28(4)°,γ=90°,Z=8,V=10.762(25)nm3,Dc=1.255 g/cm3,Mr=1016.57.该配合物晶体结构由配阳离子[Cu(Phen)3]2+和未配位的反荷阴离子[DTB]2-和晶格水分子组成.每个Cu(Ⅱ)原子与来自三个Phen的6个N原子配位,形成畸变的八面体结构单元.     

有机锡氧羧酸簇合物[PhCH_2Sn(O)(O_2CCH=CHAr)]_6的合成、表征和[PhCH_2Sn(O)(O_2CCH=CHPh)]_6的晶体结构

利用(PhCH_2)_3Sn]_2O与ArCH=CHCO_2H反应，合成6个新的[PhCH_2Sn(O) (O_2CCH=CHAr)]_6簇合物。通过元素分析、红外光谱和X射线单晶衍射对其结构进 行了表征。用X射线单晶衍射测定了[PhCH_2Sn(O)(O_2CCH=CHPh)]_6的晶体结构， 结果表明，该簇合物为三斜晶系，空间群P1, a = 1.6771(3) nm, b = 1.8020(4) nm, c = 2.1073(4) nm, α = 108.111(3)°β = 103.614(3)°,γ = 104.679 (3)°,Z = 2, V = 5.5033(18) nm~3, D_c = 1.350 g/cm~3, μ = 1.396 mm~(-1) , F(000) = 2208, R = 0.0606, wR = 0.698。该化合物为鼓型簇状结构，锡原子 呈畸变的八面体构型。     

A zinc(II) coordination polymer, [Zn4( o -bda)4( p -pbim)4] n,with strong blue fluorescence

A zinc(II) coordination polymer, [Zn₄(o-bda)₄(p-pbim)₄] _n (1) (p-pbim = 4-pyridylbenzimidazole, o-bda^2? = o-phenylenediacetic acid dianion), has been synthesized by hydrothermal method and characterized by elemental analysis, IR, TG, photoluminescence and X-ray single crystal diffraction. Complex 1 crystallizes in a monoclinic system and space group P2₁ /n, with a = 14.231(3) Å, b = 16.257(4) Å, c = 16.794(4) Å, β = 100.262(1)°, and Z = 8; R ₁ for 6475 observed reflections [I > 2σ(I)] was 0.0420. Complex 1 shows a bi-chain structure fabricated by the tetranuclear zinc unit. Two zinc(II) ions are five coordinate with distorted trigonal-bipyramid geometry; the other two zinc(II) ions are four coordinate with distorted tetrahedral geometry. Complex 1 builds the 1-D bi-chain structure with two different subrings A and B, which are 32-member and 14-member rings, respectively. There exists a 2-D supramolecular network linked by hydrogen-bonding interactions (2.695 and 2.807 Å). A 3-D supramolecular network is further constructed by non-covalent interactions between the 1-D bi-chain structure. The TG/DTG shows that the chain skeleton is thermally stable to 356°C. Blue fluorescent emission of the complex was determined at 404 nm in the solid state with short decay lifetime of 1.67 ns.     

The Crystal and Molecular Structure of Acetatochlorobis(4-methylpyridine) oxovanadium (IV)

The crystal and molecular structure of the title compound, VOCl(O₂CCH₃)(4-CH₃C₅H₄N)₂, has been determined by single-crystal X-ray diffraction. The material crystallizes in the space group P1(#2) with a = 7.822(2), b = 8.023(1), c = 14.841(2) Å, α = 99.73(1)°, β = 91.41(1)°, and γ = 117.13(1)°. The coordination geometry around the vanadium is a highly distorted octahedron. The molecule is remarkable for being a monomeric oxovanadium(IV) carboxylate. A generalized synthetic strategy is proposed for the preparation of oxovanadium(IV) monomers.     

由己二酸根桥联的新颖双U形四核铜配合物: [Cu4(phen)4(NO3)2(H2O)2(adip)4/4(Hadip)4/2](NO3)2•2H2O

邻菲罗啉、己二酸和硝酸铜在水溶液中反应得到一种新颖的四核铜配合物[Cu4(phen)4(NO3)2(H2O)2- (adip)4/4(Hadip)4/2](NO3)2•2H2O (其中H2adip＝己二酸), 并经元素分析, IR, UV, TG和X射线单晶衍射分析表征. 该配合物晶体属三斜晶系, 空间群, a＝1.0146(2) nm, b＝1.0261(2) nm, c＝1.8285(4) nm, α＝91.66(3)°, β＝92.19(3)°, γ＝112.76(3)°, V＝1.7520(6) nm3, Z＝1, Dc＝1.639 g/cm3, C66H66Cu4N12O28, Mr＝1729.47, F(000)＝886, μ＝1.294 mm－1, R1和wR2分别为0.0447和0.1141. 己二酸根通过4个羧基O将两个U形双核亚单元联接成具有一个对称中心的双U形四核结构, 其中每个U型亚单元包含晶体学上不对称的2个Cu(II)原子. 每个Cu(II)离子均处于畸变的四方锥配位环境, 除与己二酸氢根(Hadip)、己二酸根(adip)和邻菲罗啉(Phen)的N, O配位形成锥底平面外, 其中的1个Cu(II)与水配位, 而另一个Cu(II)则与硝酸根配位. 配合物晶体结构中存在着广泛的氢键和p×××p作用.     

水杨醛缩糠胺合钴（Ⅲ）配合物的合成,表征与晶体结构

合成了水杨醛缩糠胺合钴（Ⅲ）配合物Co（SF）3[HSF=水杨醛缩糠胺Schiff碱],通过IR和单晶X射线衍射测定了其结构.配合物属三斜晶系,空间群P墿,晶体学参数a=0.900 64（8）nm,b=1.061 13（9）nm,c=1.636 23（14）nm,α=93.989 0（10）°,β=94.886 0（10）°,γ=93.627 0（10）°.分子式C36H30CoN3O6,V=1.550 5（2）nm3,Z=2,Dc=1.413 g/cm3,F（000）=684,R1=0.0350,wR2=0.0958[I〉2sigma（I）],S=1.068.在配合物分子中,Co原子处于三个N原子、三个酚O原子形成的变形八面体场中.     

超分子化合物[Ni(C_6H_4O_2N)_2·(H_2O)_4]_n的水热合成及晶体结构

用皮考林酸和六水合氯化镍反应制备了一种三维氢键超分子配合物,经X射线衍射分析确定了单晶结构.该晶体属单斜晶系,P21/m空间群,晶胞参数为:a=0.976 0(2)nm,b=0.522 54(10)nm,c=1.450 1(3)nm,Mr=374.98,α=90.08(3)°,β=90.08(3)°,γ=90°,V=0.739 63(3)nm3,Z=2,ρ=1.684 g/cm3,F(000)=388,μ=1.357 mm-1,R=0.039 0,wR=0.090 8.共收集2 656个衍射数据,其中1 569个为独立衍射点(Rint=0.033 2),可观测点数1 382个(I>2σ(I)).结果表明,在组成该超分子体系的基本结构单元[N i(C6H4O2N)2.(H2O)4]中,N i(Ⅱ)离子形成六配位的稍拉长的八面体构型,配合物单元之间通过氢键相互连接,形成了无限延伸的具有网状结构的三维超分子体系.