Synthesis and Crystal Structure Analysis of 4-Dibenzaldehydeamino-4H-1,2,4-triazole Diacetate

The new title compound 4-dibenzaldehydeamino-4H-1,2,4-triazole diacetate （C16H18N8O4,Mr = 386.38） has been prepared and its crystal structure was determined by single- crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 8.1371（17）,b = 7.1237（12）,c = 16.325 （2）A,β = 100.366（2）°,V = 930.9（3） A^3,Z = 2,Dc = 1.378,F（000） = 404,μ = 0.104 mm^-1,MoKa radiation （λ = 0.71073 ）,R = 0.0307 and wR = 0.1196 for 4632 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the molecule is not flat and the crystal structure is stabilized mainly by van der Waals interactions.     

Synthesis and Crystal Structure of N,N′,N″- Tris-（2-aminophenyltriphenylphosphium）- benzene- 1,3,5-tricarboxamide

A new tripodal P,N ligand （C63H48N3O3P3） was prepared and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 13.013（3）, b = 28.406（6）, c = 14.911（3） A^°, β= 111.04（3）°, V= 5144.6（18） A^°^3 Z = 4, Dc = 1.276 g/cm^3, Mr = 987.95, λ（MoKa） = 0.71073 A^°,μ = 0.17 mm^-1, F（000） = 2064, R = 0.0786 and wR = 0.1545. A total of 43260 unique reflections were collected, of which 5112 with I 〉 2σ（I） were observed. The title compound has a central benzene ring, which is linked by -NH-CO- bonds to three 2-aminophenyltriphenylphosphium moieties, of which two with P（1） and P（2） centers are pointing to the same face of the central aryl ring, while the third one directs oppositely, forming a pseudo-propeller. In the crystal structure, there exist face-to-face π-π stacking interactions which increase the stability of the crystal structure.     

Synthesis and Crystal Structure of Ethyl 3-（4-Chlorophenyl）-3,4-dihydro-6-methyl-4-oxo-2- （pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate

The crystal structure of the title compound ethyl 3-（4-chlorophenyl）-3,4-dihydro-6- methyl-4-oxo-2-（pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate （C20H20ClN3O4, Mr= 401.84） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215（9）, b = 8.5311（4）, c = 21.6886（9） A^°, β = 91.607（1）°, V = 3814.0（3）A^°^3, Z = 8, Dc = 1.400 g/cm^3, F（000） = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.     

A Layered Vanadium Oxide with Cobalt（Ⅱ） Coordination Complex： Hydrothermal Synthesis and Crystal Structure of （py）5Co2（H2O）3[V4O12]

A novel layered mixed metal vanadium-cobadt complex, （py）5Co2（H2O）3[V4O12] 1 （py = pyridine）, was hydro（solvo）thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pca21 with a = 17.473（4）, b = 11.447（2）, c = 17.509（4）A^°, V = 5005.3（7）A^°3, Z = 4, Mr = 3502.1（12）, Z = 4, Dc = 1.827 g/cm^3,μ（MoKα） = 2.023 mm^-1, F（000） = 1928, S = 1.020, the final R = 0.0400 and wR= 0.1063 for 6035 observed reflections with I 〉 2σ（I） and 460 variables. Complex 1 consists of tetrahedral VO4 groups to form the large layers which are alternately bonded by two cobalt complex species Co（py）2（H2O）2 and Co（py）3（H2O）.     

Synthesis and Crystal Structure of a New 3-Amino-3-deoxy Derivative from 3-Keto-D-xylose

The title compound 2 was synthesized by the reaction of 3-keto-D-xylose with O-C6H4NH2NH2 and characterized by IR, NMR and HRMS, and its crystal structure was determined by X-ray diffraction analysis. The crystal is of orthorhombic system （C21H22N2O5, Mr = 382.41）, space group P2 1 2 1 2 1 with α = 10.140（2）, b = 10.802（2）, c = 17.840（4） A, β = 90°, V = 1954.1（7）A^3, Z = 4, Dc = 1.300 g/cm^3, F（000） = 808, μ = 0.094 mm^-1, the final R = 0.0354 and wR = 0.0514 for 1924 observed reflections （I 〉 2σ（I））. One intermolecular and one intramolecular hydrogen bonds were found. The absolute configuration of this molecule was confirmed by comparison with that of the original material.     

Synthesis and Crystal Structure of a Cr（Ⅲ） Dimer [Cr2（8-hqn）2Cl4（H2O）2]·2（CH3）2CO （8-hqn = 8-Hydroxyoxyquinolate）

The title complex [Cr2（8-hqn）2Cl4（H2O）2]·2（CH3）2CO （8-hqn = 8-hydroxyoxyquinolate） has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in the triclinic system, space group P^-1 with a = 8.719（1）, b = 9.226（1）, c = 9.717（1） A^°, α = 71.916（2）, β= 78.072（2）, γ = 76.014（2）°, V= 713.72（15） A^°^3, Z= 1, Dc= 1.597g/cm^3, F（000） = 350 and μ（MoKa） = 1.177 mm^-1, the final R = 0.0490 and wR = 0.1055 for 1616 observed reflections with I 〉 2σ（I）. It is a dimer constructed by two monomeric units [Cr（8-hqn）Cl2（H2O）] bridged by phenoxide-like oxygen atom from 8-hydroxyoxyquinolate, where the two six-coordinated Cr（Ⅲ）atoms exhibit an octahedral coordination geometry.     

Syntheses and Crystal Structures of Two New Organically Templated Borates： [（C2H10N2）]2[B14O20（OH）6] and [C8H22N4][B5O6（OH）4]2

Two new nonmetal borates, [（C2H10N2）]2[B14O20（OH）6] 1 and [C8H22N4][B5O6（OH）4]2 2, have been synthesized under mild conditions and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis and thermogravimetric analysis. Crystal data for compound 1： triclinic, space group P^-1, a = 8.4979（17）, b = 8.8498（18）, c = 10.065（2）A^°, α = 95.01（3）, β = 96.99（3）, γ = 116.82（3）°, V= 661.8（3）A^°^3, Z= 1, Mr = 697.63, Dc = 1.751 g/cm^3,μ = 0.163 mm^-1, F（000） = 356, the final R = 0.0372 and wR = 0.0968 （I 〉 2σ（I））; and those for compound 2： monoclinic, space group P21/c, a = 9.1867（18）, b= 14.118（3）, c = 10.334（2）A^°, β = 91.48（3）°, V = 1339.8（5）A^°^3, Z = 2, Mr = 610.46, Dc = 1.513 g/cm^3,μ = 0.135 mm^-1, F（000） = 632, the final R = 0.0350 and wR = 0.0912 （I 〉 2σ（I））. For both 1 and 2, the anionic units are interlinked via O-H…O hydrogen bonds to form a 3D supramolecular network, while the protonated cations are located in the free space of the inorganic borate framework and interact with the anions by electrostatic attraction and extensive N-H…O hydrogen bonds.     

Synthesis,Crystal Structure and Biological Activity of 1-（β-D-Glucopyranosyl）-3- amino-5-methyl-1H-1,2,4-triazole

The title compound 1-（β-D-glucopyranosyl）-3-amino-5-methyl- 1H- 1,2,4-triazole was synthesized and characterized by IR, 1H-NMR and elemental analysis. Its single crystals of 2H2O adduct suitable for X-ray analysis were obtained by the slow evaporation of a H2O solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 7.7490（15）, b = 10.424（2）, c = 17.447（4） A^°, V = 1409.3（5） A^°^3, Z= 4, C9H20N4O7, Mr = 296.29, Dc = 1.396 g/cm^3,μ = 0.120 mm^-1, S = 1.007, F（000） = 632, R = 0.0686 and wR = 0.1560 for 1217 observed reflections with I 〉 20（I）. The title molecules are linked through intermolecular hydrogen bonds to form two 1-D chain structures, and such adjacent chains are further linked by intermolecular hydrogen bonds and H2O bridges to form a 3-D supramolecular network structure. The preliminary bioassay results showed that the title compound exhibits fungicidal activities against Gibberella zeae and Colletotrichum orbiculare.     

A New Eight-connected Three-dimensional Network Based on a Tetranuclear Zinc Cluster Building Block

One interesting coordination polymer, [Zn2（1,2,4-BTC）（OH）（H2O）2]2·2H2O 1, has been synthesized from 1,2,4-BTC （1,2,4-BTC = 1,2,4-bentricarboxylate） under hydrothermal conditions and characterized by elemental analyses, IR, TG and single-crystal X-ray diffraction. Complex I crystallizes in triclinic, space group P^-1, with a = 6.5200（13）, b = 9,0600（18）, c = 10.968（2） A^°, α = 111.55（3）, β = 92.07（3）,γ= 95.03（3）°, C9H10O10Zn2, Mr = 408.91, V= 598.7（2） A^°^3, Dc = 2.268 g/cm^3, F（000） = 408 and Z = 2. X-ray diffraction analysis reveals that complex 1 is a three-dimensional network built from tetranuclear Zn（Ⅱ） building unit. In this complex, the Zn4 unit is an eight-connected knot, while 1,2,4-BTC a four-connected knot. This results in a CaF2 topology. To the best of our knowledge, such Zn4 unit is the first 8-connected building block built from asymmetry ligand.     

Synthesis and Crystal Structure of 5,17-Diformyl-11,23-di（tert-butyl）25,26,27,28-tetrapropoxy-calix[4]arene

The title compound 5,17-diformyl-11,23-di（tert-butyl）-25,26,27,28-tetrapropoxycalix[4]arene has been synthesized by selective formylation of 5,11,17,23-tetra（tert-butyl）25,26,27,28-tetrahydroxycalix[4]arene in three steps and characterized by1H NMR and X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group C2/c with a = 25.760（3）,b = 10.9952（10）,c = 18.630（2）,β = 119.985（4）°,V = 4570.4（9）3,Z = 4,Dc = 1.106 g/cm3,Mr = 761.01,F（000） = 1648,μ = 0.071 mm-1,MoKa radiation（λ = 0.71073）,R = 0.0710 and wR = 0.2411 for 3234 observed reflections with I 2σ（I）.X-ray analysis reveals that the title compound adopts a pinched cone conformation which leads to an open cavity.Intermolecular C–H O weak interactions link the molecules along the bc plane,which are effective in the stabilization of the crystal structure.     

Solvothermal Synthesis of a 3D Luminescent Cadmium-organic Framework with msw Topological Net

A new cadmium-organic framework, [Cd2（TBDC）2（DMF）2（H2O）]n （1）, was synthesized by solvothermal reaction of rigid carboxylate ligand 2,3,5,6-tetramethyl-l,4-ben- zenedicarboxylate （H2TBDC） and cadmium nitrate and characterized by elemental analysis, infrared spectrum, thermal analysis, PXRD, single-crystal X-ray diffraction and photoluminescence in the solid state. Compound 1 crystallizes in orthorhombic, space group Pca21 with a = 21.487（6）, b = 7.790（2）, c = 20.666（6） A, C30H40Cd2N2O11, Mr = 829.44, V= 3459.3（16） A3, Z = 4, Dc = 1.593 g.cm-3,μ = 1.29 mm-1, F（000） = 1672, 2.7〈θ〈27.2°, λ（MoKa） = 0.71073 A, T= 293（2） K, the final R = 0.026, wR = 0.0548 and S = 1.027. X-ray diffraction analysis reveals that complex 1 possesses a 3D framework and exhibits rnsw net. Thus, the solid-state luminescent spectrum of 1 displays that the emission of cadmium（lI） complex shows a peak at 317 nm upon 250 nm excitation at room temperature.     

A New Two-dimensional Cd（Ⅱ） Coordination Polymer Constructed by Pyridine-2,5-dicarbohydrazide

A new two-dimensional Cd（Ⅱ） coordination polymer, [Cd（2,5-pdch）（H2O）]n·2n（ClO4）·nH2O （2,5-pdch = pyridine-2,5-dicarbohydrazide）, was prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 10.905（2）, b = 11.602（1）, c = 15.034（2） A, β = 117.794 （10°, V = 1682.8（4A3, Z = 4, C7H13CdCl2NsO12, Mr = 542.52, Dc = 2.141 g/cm^3,/μ = 1.691 mm^-1, F（000） = 1072, 2（MoKa） = 0.71073A, the final R = 0.0608 and wR = 0.1329 for 2972 observed reflections with I 〉 2σ（I）. Single-crystal X-ray diffraction analysis reveals that the Cd（Ⅱ） atom displays a distorted pentagonal-bipyramidal geometry coordinated by three N atoms and three O atoms from three different 2,5-pdch ligands, and one water molecule. Interestingly, each two Cd（Ⅱ） atoms are bridged by two carbohydrazide groups of the 2,5-pdch ligands to form a dimeric unit, and such dimeric units are further connected by the 2,5-pdch ligand to generate a two-dimensional （4,4）-network.     

Syntheses, Structures, and Some Properties of Three Vanadium Selenites

Three novel vanadium selenites with the formulae [（VO2）（1,10-phenanthtoline）（SeO3H）]2 1, [（VO2）（2,2′-bipyridine）]2（SeO3） 2 and [（VO）（H2O）（SeO3）2]2（HaEDD） 3 （EDD = N1,N1′-（ethane-1,2-diyl）diethane-1,2-diamine） were hydrothermally synthesized, and characterized with elemental analysis, FT-IR spectrum, Raman spectrum, TG-DTA analysis, EPR spectra, and single-crystal X-ray diffraction analysis. Compound I belongs to the triclinic system, space group P1^- with a = 7.7527（5）, b = 9.5345（10）, c = 9.8192（8） A^°, α = 92.712（3）, β = 105.540（3）, γ = 108.154（4）°, V = 657.66（1） A^°^3, Mr = 782.22, Z = 1, F（000） = 384,μ（MoKa） = 3.544 mm^-1, R = 0.0432 and wR = 0.1142; Compound 2 is of orthorhombic system, space group F212121 with a = 7.6574（15）, b = 14.916（3）, c = 19.085（4） A, V = 2179.8（8） Aa, Mr = 605.21, Z = 4, F（000） = 1200, μ（MoKa） = 2.579 mm^-1, R = 0.0338 and wR = 0.0658; Compound 3 belongs to the triclinic system, space group P1^- with a = 9.247（2）, b = 9.659（2）, c = 7.2651（19） A^°, α = 98.171（7）, β = 103.709（5）, γ = 114.712（13）°, V = 550.9（2） A^°^3, Mr = 828.03, Z = 1, F（000） = 400, μ（MoKa） = 7.537 mm^-1, R = 0.0641 and wR = 0.2118. Compound 1 is constructed from alternating corner-shared [VO4N2] octahedra and SeO3H units, forming a dimeric vanadium unit. These assemblies are further linked into an infinite chain via hydrogen bonds along the a axis. In the structure of 2, two distinct V centers form centrosymmetric [V2O6N4] clusters through edge-sharing, and the SeO3 unit serves as a capping unit to fix the oxovanadate cluster. In the structure of 3, each [VO6] octahedron shares four oxygen atoms with adjacent Se atoms, while every SeO3 unit shares two oxygen atoms with neighboring V atoms. This connectivity of alternating VO6 and SeO3 units results in a joint-like chain. Based on the TGA analysis, these three compounds are thermally stable under 200℃ .     

Synthesis and Crystal Structure of 1,4,7,10-Tetrakis （2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10- tetraazacyclododecane

A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.     

A New Terbium（III） Coordination Compound with 2-Thiophenecarboxylic Ligand： Synthesis and Crystal Structure①

A new coordination compound with formula [Tb（2-TC）3（DMF）]n （1, 2-TC = 2-thio- phenecarboxylic ligand and DMF = dimethylformamide） was synthesized by solvothermal method. The structure of compound 1 was determined by single-crystal X-ray diffraction analyses, and characterized by elemental analyses, IR and powder X-ray diffraction. Structure analysis reveals compound 1, exhibiting a one-dimensional chain structure, crystallizes in triclinic space group P21/c, with a = 9.2751（19）, b = 16.490（3）, c = 15.865（5） A, β = 118.98（2）°, V= 2122.7（9）A3, D,. = 1.916 g/cm3, Mr= 612.45 （C18H15NO7S3Tb）, F（000） = 1196,μ（MoKa） = 3.67 mm-1, Z = 4, R = 0.0616 and wR = 0.0962 for 3865 observed reflections （I 〉 2o（I））, and R = 0.1092 for all data. Meanwhile, the photoluminescent properties of compound 1 were also investigated in the solid state at room temperature.     

Crystal Structure of 2-Amino-5,10-dioxo-4-aryl-5,10-dihydro-4H-naphtho [2,3-b]pyran-3-carboxylic Acid Ethyl Ester

The title compounds have been synthesized via a three-component reaction and their structures were characterized by IR, ^1H NMR, ^13C NMR and X-ray single-crystal diffraction. The crystal of compound 4a belongs to monoclinic, space group P121/c1 with a = 8.575（3）, b = 9.590（3）, c = 21.431（6）A, β = 91.172（3）°, V = 1762.1（9）A^3, Mr = 393.36, Z = 4, Dc= 1.483 g/cm^3, μ（MoKα） = 0.113 mm^-1, F（000） = 816, the final R = 0.0366 and wR = 0.0941. The crystal of compound 4b is of triclinic, space group P-1 with a = 8.6420（17）, b = 9.761（2）, c = 11.132（2） A, α = 97.51（3）, β = 97.86（3）, γ = 92.85（3）°, V = 920.1（3） A^3, Mr = 393.36, Z = 2, Dc = 1.420 g/cm^3, μ（MoKα） = 0.108 mm^-1, F（000） = 408, the final R = 0.0612 and wR = 0.1781. In each molecular structure, the naphthalene rings and pyran rings are almost coplanar with the latter in an envelope conformation. The rings formed by the N-H…O intramolecular hydrogen bonds are almost planar in these compounds. Their crystal packing is stabilized by intermolecular hydrogen bonds together with C-H…π and π-π stacking interactions.     

Synthesis and Crystal Structure of the Ring-opening of Amino-oxazoline

The compound C12H19Cl2N20·1/2H2O was obtained as the by-product of synthesizing silylene-bridged amino-oxazoline, and its structure was determined by X-ray diffraction. The crystal is of triclinic, space group P1, with a = 12.132（5）, b = 12.231（5）, c = 16.435（6） A^°, α = 97.485（8）, β = 106.106（7）,γ = 98.538（7）°, λ = 0.7103 A^°, V = 2279.0（15）A^°3, Z = 6, Dc = 1.251 g/cm^3, Mr = 286.19, F（000） = 906, R = 0.0846 and wR = 0.2295 for 6290 observed reflections with I 〉 2σ（I）. It is a Cl-salt. The compound was composed of phenyl, amino ion and amido derivatives. The aforementioned components were held together into a complicated three-dimensional network through three types of hydrogen bonding interactions.     

Synthesis and Crystal Structure of a New Mo/Au/S Cluster [Et4N][Mo2S4（AuPPh3）（edt）2]· 0.25Et2O·0.25MeOH （edt = Ethanedithiolate）

Reactions of the preformed cluster precursor [Et4N]2[Mo2S2（μ-S）2（edt）2] （edt = ethanedithiolate） （1） with [Au（PPh3）Cl] in MeOH/MeCN gave rise to a new heterobimetallic Mo/Au/S cluster [Et4N][Mo2S4（AuPPh3）（edt）2]·0.25Et2O·0.25MeOH （2·0.25Et2O·0.25MeOH）. It was characterized by elemental analysis, IR spectrum and X-ray analysis. 2·0.25Et2O·0.25MeOH crystallizes in the monoclinic system, space group C2/c with a = 20.117（4）, b = 9.2705（19）, c = 44.418（9） A^°, β= 93.19（3）°, V = 8271（3） A^°^3, Z = 8, Dc = 1.794 g/cm^3, T = 193 K, C31.25H43AuMo2NO0.50PS8, Mr = 1116.96, F（000） = 4380, μ（MoKa） = 4.603 mm^-1, S = 1.019, R = 0.0672 and wR = 0.1708 for 7243 observed reflections with I 〉 2σ（I）. The anion of 2 consists of a butterfly-shaped Mo2S4Au core in which one [AuPPh3]^＋ cation is coordinated by one bridging S and two terminal S atoms of the [（edt）2Mo2（S）2（μ-S）2] moiety. The Au（I） center adopts a pseudo-tetrahedral coordination geometry, and the Au-S bond lengths vary from 2.425（2） to 2.898（3）A^°.     

Synthesis and Structural Characterization of a Ruthenium Complex： trans-RuCle（COD）Py2

A new ruthenium complex trans-RuCl2（COD）Py2 has been synthesized and characterized by elemental analysis, IR, IH NMR and single-crystal X-ray diffraction. Crystal data： trans- RuCl2（COD）Py2, Mr = 438.35, monoclinic, space group P21/c, a = 8.9116（9）, b = 14.6175（15）, c = 13.7582（14）A, β = 101.994（1）°, V= 1753.1（3）A^3, Z= 4, Dc= 1.661 g/cm^3, F（000）= 888,μ = 1.199 mm^-1, R = 0.0376 and wR = 0.0789 for 2492 observed reflections with I 〉 2σ（I）.     

Synthesis and Crystal Structure of NaeTiO3

The crystal structure of a sodium titanium oxide Na2TiO3 obtained by high temperature solid state reaction method was determined from single-crystal X-ray diffraction study. The compound crystallizes in the monoclinic system, space group C2/c, Mr = 141.88, a = 9.885（1）, b = 6.4133（8）, c = 5.5048（7） A, β = 115.50（3）°, V = 314.99（7） A^3, Z = 4, Dc = 2.992 g/cm^3, 2 = 0.71073A,μ = 27.80 cm^-1, F（000） = 272, T= 295 K, R = 0.0189 and wR = 0.0512 for 30 variables and 370 contributing unique reflections. The three-dimensional structure in Na2TiO3 is constructed by the TiO（1）4O（2） and NAO（1）3O（2）2 groups. The titanium atoms are grouped in the form of trigonal bipyramid and arranged along the c axis by sharing the edges. The structure is compared with other structures of related A2BO3 compounds.