Syntheses and Crystal Structures of Two Coordination Compounds CuLCl（H2O） and Ni（L）2 （HL = 2-Carboxy-1,10-phenanthroline）

Two complexes CuLCl（H2O） 1 and Ni（L）2 2 （HL = 2-carboxy-1,10-phenanthroline） have been synthesized and characterized by single-crystal X-ray crystallography. The structure of 1 has a monoclinic space group P21/n with a = 7.985（2）, b = 16.067（3）, c = 9.694（2） A, β = 98.189（30）°, V= 1231.0（4） A^3, Z = 4, Dc = 1.836 g/cm^3,μ =1.998 mm^-1, F（000） = 684, the final R = 0.0301 and wR = 0.0810. The structure of 2 （C26H14N4NiO10） adopts an orthorhombic system, space group Pbea with a = 9.410（2）, b = 23.2410（5）, c = 23.8680（5） A, V = 5219.9（18） A^3, Z = 8, Mr = 601.12, Dc = 1,530 g/cm^3,μ = 0.809 mm^-1, F（000） = 2448, the final R = 0.0448 and wR = 0.1427. The Cu center of complex 1 exhibits a square pyramidal coordination environment with one oxygen and two nitrogen atoms from deprotonated 2-carboxy-1,10-phenanthroline, one oxygen atom from water and one chloride ion. The Ni center of complex 2 assumes a distorted octahedral coordination geometry consisting of two oxygen atoms and four nitrogen atoms of two deprotonated 2-carboxy-1,10-phenanthroline molecules. Supramolecular assembly has been found via noncovalent bonds, such as hydrogen bonds and π-π stacking interactions.     

[（phen）2Mn2（μ—O）（μ—Ac）2（H2O2）]（ClO4）2·4H2O双核锰？…

MnAc3.2H2O在pH=4.0的HAc-NaAc缓冲溶液中和邻菲罗啉(phen)反应, 制得了双核锰(Ⅲ)合物[(phen)2Mn2(μ-O)(μ-Ac)2 (H2O)2](ClO4)2.H2O, 并进行了红外光谱表征. X射线单晶衍射表明, 该晶体属单斜晶系, 空间群P21/n, 晶胞参数: a=1.025 28(5) nm, b=1.792 75(9) nm, c=1.984 14(10) nm, β=94.843 0(10)°, V=3.634 0(3) nm3, Z=4, Dc=1.669 g.cm-3. 紫外可见光谱在480 nm处有一个吸收峰. 循环伏安实验说明, 此配合物在乙腈溶液中经历了一个半可逆的一电子氧化还原过程.     

Synthesis and Crystal Structure of （H3O）2[Cu3Cl3（H2O）3（NC9H12.5O6）2]

1 INTRODUCTION The polydentate ligand nitrilotripropionic acid, H3ntp[N(CH2CH2COOH)3], has attracted conside- rable research interest in constructing coordination polymers, designing organic-inorganic hybrid mate- rials[1], synthesizing supramolecular compounds[2], etc. due to its high degree of flexibility with three carboxylic acid moieties allowing for a variety of coordination through oxygen atoms[3]. It also pro- vides other versatile properties such as the possibili- ty of inter-…     

Synthesis and Crystal Structure of a Novel Heterometallic Complex [Na2Cu2Gd2（pdc）4（H2O）14·2H2O]

A novel heterometallic complex [Na2Cu2Gd2（pdc）4（H2O）14·2H2O] （H3pdc = 1H- pyrazole-3,5-dicarboxylic acid） has been synthesized and characterized by 1R spectra, elemental analysis, and single-crystal X-ray analysis. The crystal belongs to the monoclinic system, space group P2 1/c with a = 7.9521（18）, b = 12.251（3）, c = 22.293（5） A, β = 110.173（5）°, V= 2038.5（8） A^3, Mr = 1388.13, Z = 2, F（000） = 1352, Dc = 2.261 g/cm^3,/2 = 4.380 mm^-1, the final R = 0.0409 and wR = 0.0622 for 2453 observed reflections with I 〉 2σ（I）. The structural analysis shows that the Na^I, Cu^II and Gd^II ions are linked together by two kinds of bridging ligands （pdc^3- and H2O） to form a main moiety [Na2Cu2Gd2（pdc）4（H2O）14], which can be regarded as a centrosymmetric dimmer of [NaCuGd（pdc）2（H2O）7]. Many hydrogen bonds exist in the complex to build a 3D supramolecular framework.     

[（C6n5NO2）Pr（H2O）4]（CrMo6O24H6）·（C6H5NO2）·2．5H2O的合成与晶体结构

用常规合成方法制备了基于Anderson结构阴离子的二维层状化合物[（C6n5NO2）Pr（H2O）4]（CrMo6O24H6）·（C6H5NO2）·2．5H2O,通过红外光谱和X射线单晶衍射对其进行了表征．结果表明,该化合物属于单斜晶系,C2/c空间群．a=2．3442（9）nm,b=1．3291（5）nm,c=2．458（1）nm,β=103．08（1）°,V=7．460（5）nm^3,R1=0．0727,wR2=0．1903．结构分析表明,[CrMo6O24H6]^3-阴离子通过端氧担载一个配位的Pr^3＋离子形成中性的（C6H5NO2）Pr（H2O）4（CrMo6O24H6）基团,相邻的中性基团在O1-Pr-O1桥联下形成一维链,链与链又通过异烟酸的桥联形成二维层状结构．     

In Situ Hydrothermal Synthesis of a Mononuclear Copper（Ⅱ） Complex： Cu（H2SIP-O）（bpy）（H2O） （H4SIP-O = 4-Hydroxyl-5-sulfoisophthalic Acid）

The mononuclear complex, Cu（H2SIP-O）（bpy）（H2O） （H4SIP-O = 4-hydroxyl- 5-sulfoisophthalic acid and bpy = 2,2＇-dipyridyl）, has been synthesized by the hydrothermal reaction of Cu（OH）2 with NaH2SIP and bpy at 160 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis and IR spectrum. The new ligand 4-hydroxyl-5-sulfoisophthalic acid derived from 5-sulfoisophthalic acid ligand under an in situ hydrothermal condition. The crystal of the complex crystallizes in a triclinic system, space group P1, with a = 7.757（4）, b = 10.663（6）, c = 11.727（7）A, α = 94.272（4）, β = 104.067（7）, γ = 97.400（7）°, V= 927.4（9）A^3, Z = 2, C18H14N2O9SCu, Mr= 497.93, Dc= 1.783 g/cm^3,μ = 1.350 mm^-1, F（000） = 506, the final R = 0.0518 and wR = 0.1513 for 4180 observed reflections with I 〉 2σ（I）. The central Cu（II） ion is five-coordinated by two oxygen atoms from the H2SIP-O^2- ligand and two nitrogen atoms of bpy ligand in a distorted square-planar geometry as well as a water oxygen atom in the apical position to complete a distorted square-pyramidal coordination geometry. The mononuclear copper molecules are linked by hydrogen bonds between coordinated water molecules and sulfonate groups to form a one-dimensional double-chain structure. The chains are further held together through extensive π-π stacking interactions between the aromatic rings to form a three- dimensional supramolecular structure.     

三缺位杂多化合物K8[P2W18Mo2CO2（H2O）2O68].MoO6.15H2O…

合成了杂多化合物Ｋ８［Ｐ２Ｗ１８Ｍｏ２Ｃｏ２（Ｈ２Ｏ）Ｏ６８］．ＭｏＯ６．１５Ｈ２Ｏ，依据ＸＲＤ、ＩＲ、ＵＶ－Ｖｉｓ及ＸＰＳ确定了其晶体结构的晶位原子价态，考察了该化合物催化Ｈ２Ｏ２分解动力学行为。     

[（C6n5NO2）Pr（H2O）4]（CrMo6O24H6）·（C6H5NO2）·2．5H2O的合成与晶体结构

用常规合成方法制备了基于Anderson结构阴离子的二维层状化合物[（C6n5NO2）Pr（H2O）4]（CrMo6O24H6）·（C6H5NO2）·2．5H2O,通过红外光谱和X射线单晶衍射对其进行了表征．结果表明,该化合物属于单斜晶系,C2/c空间群．a=2．3442（9）nm,b=1．3291（5）nm,c=2．458（1）nm,β=103．08（1）°,V=7．460（5）nm^3,R1=0．0727,wR2=0．1903．结构分析表明,[CrMo6O24H6]^3-阴离子通过端氧担载一个配位的Pr^3＋离子形成中性的（C6H5NO2）Pr（H2O）4（CrMo6O24H6）基团,相邻的中性基团在O1-Pr-O1桥联下形成一维链,链与链又通过异烟酸的桥联形成二维层状结构．     

Synthesis and Crystal Structure of [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O

The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (phen = 1,10-phe-nanthroline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10)(A), α = 80.6830(10), β = 66.6480(10), γ = 64.0480(10)o, V = 1554.63(4) (A)3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm3, μ = 0.845 mm-1, F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (I > 2σ(I)). The compound contains a six-coordinated copper(II) center, which is surround by four N atoms of two phen ligands (Cu-N distances in the range of 1.997(2)～2.225(2)(A)), one sulfate O atom (Cu-O = 2.0037(17) (A)) and one water O atom (Cu-O(5w) = 2.719(2) (A)) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.     

Supramolecular Terbium-SIP Complex Pillared by 4,4＇-Bipyridyl, {[Tb（SIP）（H2O）5]2（bpy）3（H2O）}n： Synthesis,Crystal Structure and Photoluminescence

The supramolecular terbium complex, {[Tb（SIP）（H2O）5]2（bpy）3（H2O）}n （NaH2SIP = 5-sulfoisophthalic acid monosodium salt and bpy = 4,4＇-bipyridyl）, has been synthesized by the hydrothermal reaction of Tb4O7 with NaH2SIP and bpy at 165 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, powder X-ray diffraction and photoluminescence spectrum. It crystallizes in a monoclinic system, space group C2/c, with a = 30.6840（1）, b = 10.9206（2）, c = 17.4967（3） A, β= 111.931（1）°, V = 5438.65（14） A^3, Z = 4, C46H52N6O25S2Tb2, Mr = 1470.90, Dc = 1.796 g/cm^3, p = 2.747 mm^-1, F（000） = 2928, the final R = 0.0654 and wR = 0.1322 for 3806 observed reflections with I 〉 2σ（I）. In the neutral [Tb（SIP）（H2O）5]2 motif, the Tb（III） ions are linked by the SIP ligands to form a one-dimensional zigzag chain propagating along the c axis. The zigzag chains are linked together by hydrogen bonds and π-π stacking interactions to form a two-dimensional supramolecular framework. The uncoordinated bpy molecules act as pillars to extend the two-dimensional sheets into a distinctive pillared three-dimensional supramolecular structure through O-H...N hydrogen bonds. The photoluminescence of the complex was investigated at room temperature in the solid state.     

Synthesis and Characterization of Diorganotin Compounds {[R2Sn（ON =CHC6H5）]2O}2 and Crystal Structure of {[（C6H5CH2）2Sn（ON=CHC6H5）]2O}2

Introduction Dimeric tetraorganodistannoxanes are a kind of in-teresting organotin oxo clusters and have attracted con-siderable attention during the last several decades, in view of their unique structural features1-5 as well as their applications as biocides6,7 and in homogenous cataly-sis.8,9 In the solid state, they contain characteristic Sn4O2X2Y2 structural motifts with staircase or ladder arrangements, a planar four-membered Sn2O2 ring and, generally, penta-coordination around the tin…     

Synthesis and Structure of a New Mixed-polyoxometalate （W/Mo） Compound： H5K{[Co（H2O）5]2（H2Mo3.24W8.76O42）}·19H2O

One new polyoxometalate compound connected via cobalt/potassium cations,namely H5K{[Co（H2O）5]2（H2Mo3.24W8.76O42）}·19H2O 1,was prepared and characterized by ele- mental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis result reveals that anions of {[Co（H2O）5]2（H2Mo3.24W8.76O42）}6- in compound 1 are linked by potassium cations to form one- dimensional chain,based on which a three-dimensional network is further constructed with the help of hydrogen bonds. Crystal data： H67Co2KMo3.24O72W8.76,Mr = 3297.87,monoclinic,C2/c,a = 19.0126（10）,b = 16.6025（5）,c = 19.1908（10）A,β = 106.713（1）°,V = 5801.8（5） A^3,Z = 4,Dc = 3.755 g/cm^3,F（000） = 5961,μ = 18.730 mm^-1,R = 0.0569 and wR = 0.1437 （I 〉 2σ（I））.     

Rapid Thermolysis Studies of [Pb2（TNR）2（CHZ）2（H2O）2]·4H2O and Cd（CHZ）2（TNR）（H2O）

T-jump/FT-IR spectroscopy was used to study the rapid thermal decomposition activity of [Pb2（TNR）2（CHZ）2（H2O）2]·4H2O and Cd（CHZ）2（TNR）（H2O） under 0.1 MPa Ar atmosphere. The results show that the main gaseous products of [Pb2（TNR）2（CHZ）2（H2O）2]·4H2O are NH3, H2O and HONO, while CO and NO are the major gaseous products of flash pyrolysis of Cd（CHZ）2（TNR）（H2O）. Thus Cd（CHZ）2（TNR）（H2O） is not an eco-friendly and chemically compatible primary explosive. Both compounds liberate volatile metal carbonate, oxide and isocyanate compounds. The combustion temperature and products of the two compounds were calculated by Real code. The results of theoretical calculation show that the combustion temperature of [Pb2（TNR）2（CHZ）2（H2O）2].4H2O is higher than that of Cd（CHZ）2（TNR）（H2O）, there is no HNCO in the combus- tion products and the amount of NO is less than the experiment result from T-jump/FTIR.     

配位化合物[Cd（hca）2（H2O）3]（H2O）2,[Cu（hca）2（phen）]的合成与表征

配合物1由醋酸镉和Nahca(对羟基肉桂酸钠)在水溶液中反应得到,配合物2由醋酸铜,Hhca和phen在水和乙醇混合溶液中反应得到.配合物1属正交晶系,Pbcn空间群.配合物2属单斜晶系,C2/c空间群.配合物1和2中配体中的羧酸根与金属离子都是螯合配位的,末端羟基没有参与配位.配合物1和2的结构中都包含了丰富的氢键.通过氢键作用,配合物1形成了三维网状超分子结构,配合物2形成了二维层状超分子结构.     

A New Chain-like Copper（Ⅱ） Polymer： [Cu（MOPIP）（BDC）]n·0.5n（H2O）

A metal-organic coordination compound formulated as [Cu（MOPIP）（BDC）]n·0.5n（H2O） 1 （MOPIP - 2-（4-methoxyphenyl）-1H-imidazo[4,5-f][1,10] phenanthroline, BDC = 1,4-benze Nedicarboxylate） has been hydrothermally synthesized and structurally characterized by elemental analysis, thermogravimetric analysis, IR spectrum, and single-crystal X-ray diffraction. The title compound crystallizes in the triclinic system, space group P1^-, with a = 8.872（5）, b = 11.163（6）, c = 12.589（6）A, α = 94.687（7）, β = 99.930（6）, γ = 103.074（7）°, V = 1186.7（12）A^3, C28H19CuN4O5.5, Mr= 563.01, Dc = 1.576 g/cm^3,μ（MoKa） = 0.973 mm^-1, F（000） = 576, Z = 2, the final R = 0.0607 and wR = 0.1618 for 3419 observed reflections （I 〉 2σ（I））.