Synthesis and Crystal Structure of (4S)-5-(2-Methoxy-2-oxoethylamino)-5-oxo- 4-(3,4,5-trimethoxybenzamido) Pentanoic Acid

The crystal structure of (4S)-5-(2-methoxy-2-oxoethylamino)-5-oxo-4-(3,4,5- trimethoxybenzamido) pentanoic acid 5 (C18H24N2O9, Mr = 412.39) has been determined by single- crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 27.665(9), b = 5.1444(16), c = 13.907(4) ?, β = 98.401(5)o, V = 1958.0(11) ?3, Z = 4, Dc = 1.399 g/cm3, μ = 0.113 mm-1, F(000) = 872, R = 0.0606 and wR = 0.1405 (I > 2σ(I)). The results con- firmed that 5 could be assigned to the tautomeric form. The intermolecular hydrogen bonds between O(5)–H(5)…O(7), N(2)–H(2)…O(6) and N(1)–H(1)…O(4) have been observed.

Synthesis and Crystal Structure of a Hexameric Organooxotin Cluster from Benzilic Acid

The title complex [^n BuSn（O）O2C（OH）CPh2]6.2H2O has been synthesized by the reaction of n-BuSn（O）OH with benzilic acid in 1：1 molar radio and characterized by IR, ^1H NMR spectra and elemental analysis. The crystal structure was determined by X-ray diffraction. It crystallizes in triclinic, space group PI with a = 1.3543（2）, b = 1.4593（2）, c = 1.5293（2） nm, α = 102.075 （2）,β = 115.571 （2）, γ = 93.308（3）°, Z = 1, V = 2.6282（7） nm^3, Mr = 2550.21, Dc = 1.611 g/cm^3,μ = 1.477 mm^-1, F（000） = 1280, R = 0.0309 and wR = 0.0729. The structure shows a distorted octahedral configuration with six-coordination for the central tin atom.

Hydrothermal Synthesis, Crystal Structure and Thermal Analyses of Pyrazine-2,3-dicarboxylic Acid Bridged Co(II) Coordination Polymer of _∞~2[Co(phen)(μ-L)_(3/3)]·H_2O (H_2L = Pyrazine-2,3-dicarboxylic Acid)

A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- (phen)(μ-L)3/3]?H2O (H2L = pyrazine-2,3-dicarboxylic acid) has been hydrothermally synthesized, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group P21/n with a = 11.480(2), b = 11.885(2), c = 12.939(3) ?, β = 110.55(3)°, V = 1653.1(6) ?3, Mr = 423.25, Dc = 0.425 g/cm3, Z = 4, R = 0.0361 and wR = 0.1011. The title complex consists of 2D 2 ∞ [Co(phen)(μ-L)3/3] layers and crystal water molecules. Each Co atom is octahedrally coordinated by three N atoms and three O atoms to form 2D 2 ∞ [Co(phen)(μ-L)3/3] polymeric layers. Furthermore, such 2D layers are stacked into 3D supramolecular frameworks via Van der Waals’ intermolecular forces, strong and weak hydrogen-bond interactions. The coordination phen and crystal water molecules are resided into cavities of the frameworks.

Investigation on Molecular and Crystal Structures of Metal Complexes with Aminopolycarboxylic Acids(Ⅰ)─Synthesis and Structure of Na_2[Fe~Ⅲ(ida)2]2·3H_2O

The crystal structure of the title complex salt has been determined by single-crystal X-ray structure analysis. The crystal data are as follows; Monoclinic, P21/c, a=15.6480(10)A,b=16.7870(10)A, c=10.347(2)A, β=90.790(10), V=2717.7(6)A3, Z=3, and R=0.0333 for 4789 unique reflections. The complex anion has a pseudo-octahedral structure distorted more than the CrⅢand CoⅢ analogs, in which cach iminodiacetato ligand (ida2-) is coordinated in a facial fashion with the two N atoms in a cis configuration, resulting in an unsyin-fac structure.

Synthesis and Crystal Structure of 2-[(2-Chloropyridin-4-yl)oxy]-3,3-diphenyl-3-methoxypropionic Acid

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of orthorhombic system（C21H18ClNO4,Mr = 383.81）,space group Pca21 with a = 13.913（3）,b = 10.273（2）,c = 26.488（5）,V = 3786.1（13） 3,Z = 8,Dc = 1.347 g/cm3,F（000） = 1600,μ = 0.228 mm-1,the final R = 0.0550 and wR = 0.1278 for 5065 observed reflections（I 2σ（I））.The title compound in a racemic form was found to exist as a mixture of two enantiomers in an equal ratio in the unit cell.The intermolecular hydrogen bonds link the molecules in a head-to-end manner to generate an infinite chain.

Synthesis and Crystal Structure of 2-(N-Cyclohexyl)-imino-1,4-succinic Acid Dihydrate

The title compound, 2-(N-cyclohexyl)-imino-1,4-succinic acid dihydrate 4, has been prepared and structurally determined by X-ray diffraction analysis. Crystal data: monoclinic, space group Cc, a = 7.5790(15), b = 24.860(5), c = 7.1394(14) ?, β = 104.23(3)°, V = 1303.9(4) ?3, C10H21NO6, Mr = 251.28, Z = 4, Dc = 1.280 g/cm3, μ = 0.105 mm-1, F(000) = 544, R = 0.0397 and wR = 0.0918 for 1212 observed reflections with I ≥ 2σ(I). X-ray structure analysis reveals that there exist two intramolecular and six intermolecular hydrogen-bonding interactions in the crystal lattice, which can stabilize the configuration of the α-imino acid dihydrate 4.

Synthesis and Crystal Structure of Mesityl Acetic Acid 3-Mesityl-2-oxo-1-oxaspiro[4,4]non-3-en-4-yl Ester

The title compound mesityl acetic acid 3-mesityl-2-oxo-1-oxaspiro[4,4]non-3-en-4-yl ester （5, C28H32O4, Mr = 432.56）, as a spiromesifen derivative, has been synthesized by the conden- sation reaction of 2,4,6-trimethylphenylacetic chloride with 4-hydroxyl-3-mesityl-1-oxa-spiro[4,4]- non-3-en-2-one （4）, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9261（7）, b = 8.2802（8）, c = 18.7604（18） , α = 91.576（3）, β = 93.277（2）, γ = 95.306（12）o, V = 1223.3（2） 3, Z = 2, Dc = 1.174 g/cm3, F（000） = 464, μ = 0.077 mm–1, S = 1.001, the final R = 0.0624 and wR = 0.1415 for 2809 observed reflections with I 2σ（I） and 290 variable parameters. The crystal analysis results show that the five-membered cyclopentyl ring displays an envelope conformation with C（25） atom at the flap position, 0.537（3） out of the mean plane formed by the other four atoms. The dihedral angles between the two benzene and furan rings are 70.0（2） and 80.67（3）o, respectively.

Synthesis, Crystal Structure and Properties of a Europium Complex with 3-Iodobenzoic Acid and 2,2'-Bipyridine

The complex [Eu（3-IBA）3·2,2＇-bipy]2 was synthesized from 3-iodobenzoic acid （3-HIBA）, 2,2＇-bipyridine （2,2‘-bipy） and EuCl3·6H2O by hydrothermal synthesis, and its crystal structure was determined by X-ray single-crystal diffraction. It is of triclinic, space group Pi, with a = 10.958（2）, b = 12.311（3）, c = 12.556（3） A, α = 81.549（3）, β = 82.404（4）, γ = 78.348（3）°, Mr = 1049.15, V= 1631.7（6） A3, Z = 1, Dc = 2.135 g/cm^3, F（000） = 980, 2（MoKa） = 0.71073 A,μ（MoKa） = 4.804 mm^-1, the final R = 0.0329 and wR = 0.0723 for 4640 observed reflections with I 〉 2σ（I）. The Eu（Ⅲ） ion is eight-coordinated and two Eu（Ⅲ） ions are held together by four 3-iodobenzoate groups in the bidentate bridging mode. The complex was characterized by DTA-TG, IR, UV and fluorescence spectra.

Synthesis, Crystal Structure and Antitumor Activity of a Na(Ⅰ) Coordination Polymer Based on 2-Propyl-4,5-imidazoledicarboxylic Acid and 1,10-Phenanthroline Ligands

A new Na(I) coordination polymer,[Na2(Hpimdc)(H2 pimdc)(phen)2]n(1), has been synthesized by the reaction of NaOH with 2-propyl-4,5-imidazoledicarboxylic acid(H3 pimdc)and 1,10-phenanthroline(phen). The Na(I) coordination polymer 1 was characterized by single-crystal X-ray diffraction analysis and elemental analysis. In 1, the bridged ligand H3 pimdc adopts two modes(singly deprotonated and doubly deprotonated) to coordinate with the Na(I) ion.The Na(1) ion is six-coordinated with three N atoms from a phen ligand and a H2 pimdc ligand,three O atoms from a Hpimdc ligand and two other different H2 pimdc ligands. The Na(2) ion is also six-coordinated with three N atoms from a phen ligand and a Hpimdc ligand, three O atoms from a H2 pimdc ligand and other two different Hpimdc ligands. Complex 1 exhibits a 1 D chain structure built up by μ-H2 pimdc-and μ-Hpimdc2-ligands. The antitumor activities of complex 1 against human SGC7901, A549 and H08910 cells have been tested.

Synthesis and Crystal Structure of Glycin·3,5-Dihydroxybenzoic Acid

The title compound glycin.3,5-dihydroxybenzoic acid （GDB） has been synthesized and characterized by single-crystal X-ray analysis. It crystallizes in orthorhombic, space group Pca21 with a = 25.513（10）, b = 4.668（2）, c = 9.150（4） A°, Z= 4, V= 1089.8（8） A°^3, C9H13NO7, Mr= 247.20, Dc = 1.507 g/m^3,/z（MoKa） = 0.132 mm^-1, F（000） = 520, R1 = 0.0322 and wR2 = 0.0611 for 885 observed reflections （I 〉 2σ（I））. The title compound is a 1：1 molecular complex of glycin and 3,5-dihydroxybenzoic acid, which is linked by O-H…O and N-H…O hydrogen bonds to form a three-dimensional framework. Test of SHG （second harmonic generation） indicates that NLO generation of the crystal is higher than that of KDP.

Two Dehydroabietic Acid-based Arylamines: Synthesis, Crystal Structure and Fluorescent Properties

Two dehydroabietic acid-based arylamines have been synthesized and characterized by FTIR, 1H NMR, 13C NMR, MS spectra and elemental analysis. Their spatial structures were determined by X-ray diffraction analysis. UV-Vis absorption and fluorescence spectral characteristics of these compounds in methanol were investigated. Their fluorescence emission spectra in different polarity solvents were further evaluated. Fluorescent properties and structural relationship of the compounds showed that fluorescence intensity and quantum yield inversely increase with the non-coplanar degree. In addition, the solvent polarity has different effects on the fluorescence emission spectra of two compounds.

Hydrothermal Synthesis and Crystal Structure of a Novel Polymolybdic(VI) Acid: {[H_3O]_2^+[Mo_2O_4(OH)_6]^(2-)}_n

A novel supramolecular polymolybdic（VI） acid was unexpectedly synthesized by the reaction of sodium molybdate with 1,2,4,5-benzenetetracarboxylic and trichloroacetic acids in 1：1：1 molar ratio under hydrothermal condition. The crystal belongs to tetragonal with space group P4/mbm, a = 0.88867（17）, b = 0.88867（17）, c = 0.55676（15） nm, Z = 3, V = 0.43969（17） nm^3, Dc = 4.486 g/cm^3,μ = 4.365 mm^-1, F（000） = 576, R = 0.0273 and wR = 0.0679. In the crystal, the Mo（VI） atoms are six- and five-coordinated in distorted octahedral and trigonal bipyramidal geometries, respectively. Furthermore, these Mo（VI） atoms, bearing different coordinated environments, are bridged by OH groups with disorder O atoms to form a twodimensional framework with pentagonal grids. It is worthy of notice that these adjacent twodimensional frameworks are extended into a three-dimensional supramolecular array with pentagonal large cavities＇by Van Der Waals＇ forces and hydrogen bonding interactions.

Synthesis and Crystal Structure of a Novel Lactone Derived from Dehydroabietic Acid

A novel lactone derived from dehydroabietic acid,C20H21BrO4,has been charac-terized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction method.It crystallizes in orthorhombic,space group P212121 with a = 6.4195（15）,b = 11.535（3）,c = 24.654（6） ,V = 1825.5（7） 3,Z = 4,Mr = 405.28,Dc = 1.475 g/cm3,λ = 0.71075 ,μ（MoKα） = 2.27 mm-1,F（000） = 832,the final R = 0.024 and wR = 0.045 for 2152 observed reflections with I 2σ（I）.The molecules of lactone are mainly linked through intermolecular hydrogen bonds.

Synthesis and Crystal Structure of 2,2'-Dihydroxy-[1,1']binaphthalenyl-3,3'-bis-hydroxamic Acids

The first synthesis and structural characterization by X-ray crystallography of racemic 2,2＇-dihydroxy-[1,1＇]binaphthalenyl-3,3＇-bis-hydroxamic acids were reported.The com-pound（C28H30N4O8,Mr = 550.56） crystallizes in orthorhombic system,Fdd2 space group with a = 13.055（3）,b = 34.871（7）,c = 12.570（3） ,V = 5722（2） 3,Z = 8,Dc = 1.278 g/cm3,λ = 0.71073 ,μ（MoKα） = 0.095 mm-1,F（000） = 2320,S = 1.021,R = 0.0349 and wR = 0.0802 for 1757 observed reflections with I 〉 2σ（I）.The N-H and O atom are involved in two-dimensional intermolecular hydrogen bond nets,which further stabilize the structure.

Synthesis and Crystal Structure of a New Silver(I) Isonicotinate Coordination Polymer:[(Ag_3L_2)(ClO_4)]_n(HL=Isonicotinic Acid)

The title complex [(Ag3L2)(ClO4)]n 1, where HL = isonicotinic acid, has been prepared from the reaction of isonicotinic acid with AgClO4?H2O at room temperature and its struc- ture was determined by single-crystal X-ray diffraction. The crystal of 1 is of triclinic, space group P1 with a = 8.429(3), b = 10.694(4), c = 10.840(4) ?, α = 119.063(4), β = 100.474(5), γ = 99.901(5)°, V = 800.4(5) ?3, Mr = 1334.53, Dc = 2.769 g/cm3, Z = 2, μ(MoKα) = 3.848 mm-1, F(000) = 632, R = 0.0250 and wR = 0.0582 for 2872 observed reflections with I > 2σ(I). Complex 1 is a two-dimensional network consisting of adjacent one-dimensional chains through Ag–Ag inter- actions.

Synthesis and Crystal Structure of a Novel 1D Magnesium(II) Coordination Polymer Constructed by L-Cysteic Acid

A novel coordination polymer [Mg（L）（H2O）2]·H2O] （LH2=L-cysteic acid） has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction.The crystal crystallizes in orthorhombic system, space group P212121, with a=5.962（3）, b=11.224（6）, c=13.664（7）A, V=914.3（8）A^3, Z=4, Mr=245.50, Dc=1.783 g/cm^3,μ=0.445 mm-1,flack parameter=0.32（16）, F（000）=512, the final R=0.0458 and wR=0.1172 for 1578 observed reflections with I 〉 2σ（Ⅰ）. The Mg（Ⅱ） atom shows an octahedral geometry defined by two carboxyl O atoms from two different L-cysteic acid ligands, one carboxyl O atom and one amino N atom from the adjacent ligand, and two aqua ligands. The Mg（Ⅱ） atoms are bridged by L-cysteic acid ligands, leading to a 1D infinite zigzag chain. In the structure there are extensive hydrogen bonds,through which the complex completes its 3D framework structure.

Synthesis, Crystal Structure and Antioxidant Activity of 5,6-O-(4-bromophenyl)-L-ascorbic Acid

The title compound 5,6-O-（4-bromophenyl）-L-ascorbic acid （C13H11BrO6, Mr = 343.13） has been synthesized and its structure was characterized by IR, 1H NMR and single-crystal X-ray diffraction. The product is a mixture of two diastereomer compounds （a （7S） and b （7R））. The crystal of a （7S） belongs to orthorhombic system, space group P212121 with a = 6.5362（10）, b = 7.8226（11）, c = 25.294（4） ？, V = 1293.3（3） ？3, Z = 4, Dc = 1.762 g/cm3, μ（MoKα） = 3.202 mm-1, F（000） = 688, R = 0.0235 and wR （I 〉 2σ（I）） = 0.0566. The hydrogen bonding interactions link the molecules to form a three-dimensional system. In addition, 5,6-O-（4-bromophenyl）-L-ascorbic acid （BPAA） exhibits strong free-radical scavenging activities in vitro against 2,2-diphenyl-1-picrylhy- drazyl and superoxide anion. BPAA should be investigated further as a worthy antioxidant.

Synthesis and Crystal Structure of a Two-dimensional Cadmium(Ⅱ) Coordination Polymer:[Cd(AIP)(Bpy)]_n·nBpy(H_2AIP=5-Aminoisophthalic Acid, Bpy=2,2′-Bipyridyl)

A two-dimensional coordination polymer, [Cd（AIP）（Bpy）]n.nBpy, was hydrothermally synthesized by the reaction of hydrate cadmium acetate with 5-aminoisophthalic acid, lithium hydroxide, vanadiumpentoxide, sodium chloride and 2,2′-bipyridyl in water solution. It crystallizes in orthorhombic, space group C222 1, absolute structure parameter 0.00（7）, with a = 15.336（4）, b = 22.390（6）, c = 14.257（3）A, V = 4896（2）/~3, C28H21CdNsO4, Mr = 603.90, Z = 8, F（000） = 2432, Dc = 1.639 g/cm^3, μ = 0.939 mm^-1, T= 298（2） K, S = 1.001, R = 0.0296 and wR = 0.0813 for 5522 observed reflections （I 〉 2a（/））. In the title complex, each 5-aminoisophthalate ligand bridges three cadmium（Ⅱ） ions to form a two-dimensional layer structure.

Hydrothermal Synthesis and Crystal Structure of a 2D Zinc(Ⅱ) Coordination Polymer with 5-Hydroxynicotinic Acid

The title compound, [Zn（5-hydroxynicotinate）22H2O]n, has been synthesized by reacting zinc sulfate vitriol with 5-hydroxynicotinic acid under hydrothermal conditions, and its structure was determined by X-ray crystallography with the following data： monoclinic, space group C2/c, C12H12N2O8Zn, Mr = 377.61, a = 10.223（3）, b = 10.319（3）, c = 13.613（4）A, β = 105.922（6）°, Z = 4, V = 1380.9（8） A3, F（000） = 768, Dc = 1.816 g/cm3, μ（MoKα ） = 1.826 mm^-1, the final R = 0.0401 and wR = 0.1380 for 1157 observed reflections （I 〉 2σ（I））. In the structure of the title compound, the ZnⅡ ion located in an inversion center lies in a distorted tetrahedral environment at a N2O2 coordination mode, and the 5-hydroxynicotinic acid ligand linkssymmetry-related ZnⅡ ions at aμ2-N,O bridging way forming a two-dimensional covalent structure. In the crystal, solvent water molecules form intermolecular O-H-O hydrogen bonds and pyridine rings of adjacent layers form n-n-stacking （3.346 A）, which connect adjacent two-dimensional sheets into a three-dimensional supramolecular network.