Hydrothermal Synthesis and Structure Characterization of Open-framework Cobalt-tungsten Phosphate[H3NCH2CH2NH3]3[Co3W4P4O28]

A new three-dimensional open-framework cobalt(Ⅱ)-tungsten(Ⅵ) phosphate,[H3NCH2CH2NH3]3·[Co3W4P4O28](1) has been synthesized from the reaction of CoCl2·6H2O,WO3,H3PO4,ethylenediamine and H2O.The title compound was fully characterized by infrared spectroscopy,elemental analysis,magnetic properties,thermogravimetric analysis,XPS and single-crystal X-ray diffraction.The compound crystallized in a tetragonal space group I4(1)/a with a=1.7118(4) nm,c=1.0773(2) nm,V =3.1568(11) nm3,Z =4.     

Synthesis,Crystal Structure and Recognition Properties of a New Benzothiazole Derivative:C_(28)H_(24)N_4O_2S

A benzothiazole-based compound 1, C_(28)H_(24)N_4O_2S, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P2_1/c with a = 9.6309(14), b = 15.230(2), c = 17.197(3) ?, β = 105.222(2)°, V = 2433.9(6) ?~3, Z = 4, F(000) = 1008, D_c = 1.311 Mg/m~3, M_r = 480.57, μ = 0.166 mm~(-1), the final R = 0.0509 and wR = 0.1481 for 6643 observed reflections with I 2σ(I). The crystal structure of compound 1 is stabilized by C–H···O, N–H···N, N–H···O, O–H···N and C–H···N hydrogen bonds. The spectroscopic studies of the title compound toward various metal ions were also investigated in 25%(V/V) ethanol aqueous solution, and the result showed that it can selectively recognize Cu~(2+) with fluorescence quenching.     

Preparation and Crystal Structure of 12β,15α-dihydroxyprogesterone

Progesterone(1) was biotransformed into the title compound 12β,15α-dihydroxy-progesterone(2) with Colletotrichum lini AS3.4486.The biotransformation process was monitored with HPLC.The structure of 2 was determined by 1H NMR,13C NMR,ESI-MS and single-crystal X-ray diffraction.The crystal of the compound belongs to orthorhombic,space group P212121 with a = 8.0671(9),b = 12.3970(15),c = 18.532(3) ,Z = 4,V = 1853.3(4)3,Dc = 1.242 mg/m3,μ = 0.084 mm-1,F(000) = 752,R = 0.0373 and wR = 0.0850.Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 2 has been constructed by multiply intermolecular O(2)-H(2)…O(4) and O(3)-H(3)…O(2) H-bonding interactions.     

Synthesis,Crystal Structure and Flame Retardance of 2-(3-Silatranylpropylamino)-4-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide

The title compound, 2-(3-silatranylpropylamino)-4-dichlorophenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide(2(C_(20)H_(33)N_2O_6Psi)·C_2H_6O·CH_4O, Mr = 991.20), has been synthesized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 10.3783(15), b = 11.2402(17), c = 12.1675(18) ?, a = 70.653(4), b = 82.908(4), g = 85.690(4)°, V = 1328.1(3) ?3, Z = 1, Dc = 1.239 g/cm~3, μ = 0.19 mm~(-1), F(000) = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 2s(I). The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si?N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H···O hydrogen bonds into dimers, generating rings with graph-set motif R22(8). Furthermore, a couple of O(7)–H(10)···O(3) hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry(TGA). The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.     

Synthesis and Crystal Structure of a New Mixed-ligand Cluster[Mo3O4(C2O4)2bipy-(H2O3)]·EtOH·2H2O(bipy=2,2'-Bipyridine)

The novel mixed-ligand neutral compound [Mo3O4(C2O4)2·bipy(H2O)3]·EtOH·2H2O (bipy = 2,2'-bipyridine) has been prepared by the reaction of oxalic acid elution of Mo(Ⅳ) and bipy, and characterized by single-crystal X-ray diffraction analysis and IR. The crystal is of triclinic, space groups P1 with a = 9.5520(2), b = 10.3730(1), c = 13.5722(2) (A), α = 74.940(12), β = 80.772(14), γ = 69.898(11)°, V = 1215.73(11) (A)3, Z = 2, C16H24Mo3N2O18, Mr = 820.19, Dc = 2.241 g/cm3, μ = 1.616 mm-1, F(000) = 808, T= 293(2) K, the final R = 0.0424 and wR = 0.0939 for 4119 observed reflections with Ⅰ> 2σ(Ⅰ). The trinuclear unit is coordinated by mixed ligands of oxalate and bipy. The intermolecular hydrogen bonding interactions among adjacent [Mo3O4(C2O4)2·bipy(H2O)3] extend the compound into a therr-dimensional supramolecular framework. The uncoordinated water molecules and ethal molecules act as space-fillers and consolidate the whole architecture through hydrogen bonding interactions.     

Synthesis,Spectroscopic Properties and Crystal Structure of 3,3＇-（Anthracene-9,10-diyl）bis（1-phenylpropan-1-one）

The compound 3,3'-(anthracene-9,10-diyl)bis(1-phenylpropan-1-one)(C32H26O2,Mr=442.55) has been synthesized by the reaction of 2,2'-(anthracene-9,10-diylbis(methy-lene))bis(1,3-diphenylpropane-1,3-dione) with CsCO3,and its structure was characterized by 1H NMR and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic,space group P21/c with a=9.154(3),b=5.2777(16),c=24.897(7) nm,β=107.337(10)°,Z=2 and V=1.1482 nm3.X-ray analysis indicates that an intermolecular hydrogen bond C(8)-H(8A)…O(1),weak C-H···π between H(9A) and the centre of anthracene rings and weak π-π interactions between two anthracene ring planes are observed.     

4-Tert-butyl-N?-((2-Hydroxynaphthalen-1-yl)methylene) Benzohydrazide: Synthesis,Crystal Structure and Recognition Properties

A new naphthol-based compound 1, C22 H_22 N2 O2, has been designed and synthesized. The structure of the title compound 1 was confirmed by IR, ~1 H NMR, ~(13) C NMR, H RMS, and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2_1/c, with a = 12.888(9), b = 15.543(10), c = 9.119(6) ?, β = 94.05(3)°, V = 1822(2) ?~3, Z = 4, D_c = 1.263 g/cm~3, M_r = 346.41, μ = 0.081 mm-1, F(000) = 736.0, the final R = 0.0452 and wR = 0.1142 for 3404 observed reflections with(I 2σ(I)). The crystal structure of 1 is stabilized by O–H···N, N–H···O, C–H···O hydrogen bonds and π-π interactions. The spectroscopic studies of 1 toward various metal ions were also investigated in 25%(V/V) ethanol aqueous solution, and the result showed that it can selectively recognize Zn~(2+) with fluorescence enhancement.     

Synthesis and Crystal Structure of (Z)-N-(2-(diethylamino)ethyl)-7-(5-fluoro-2-oxoindolin-3-ylidene)-2-methyl-4,5,6,7-tetrahydro-1H-indole-3-carboxamide Methanol Solvate

The crystal structure of a new compound (Z)-N-(2-(diethylamino)ethyl)-7-(5- fluoro-2-oxoindolin-3-ylidene)-2-methyl-4,5,6,7-tetrahydro-1H-indole-3-carboxamidemethanol solvate (C24H29FN4O2CH4O, Mr = 456.55) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 14.560(3), b = 7.3200(2), c = 22.233(4) , β = 101.78(3)°, V = 2319.7(8) 3 , Z = 4, Dc = 1.307 g/cm 3 , F(000) = 976, μ = 0.092 mm -1 , MoKa radiation (λ = 0.71073), R = 0.0604 and wR = 0.1644 for 4262 observed reflections with I > 2 (I). X-ray diffraction analysis reveals that the indole and pyrrole are almost coplanar. Intramolecular C-H···O and N-H···O hydrogen bonds together with π-π interactions are found in the structure.     

UV Assisted Preliminary DNA Binding Studies and Single-crystal X-ray Structure of 4-{(4-Nitrophenyl-sulfonamido)methyl}cyclohexanecarboxylic Acid

A new sulfonamide, 4-{(4-nitrophenylsulfonamido)methyl}cyclohexanecarboxylic acid(C14H18N2O6S), has been synthesized by the reaction of tranexamic acid and 4-nitrobenzenesulfonyl chloride in basic medium at room temperature. The molecular structure was determined by FT-IR, NMR, elemental analysis and single-crystal X-ray technique. X-ray diffraction shows that the compound crystallizes in the monoclinic system, space group P21/c with a = 13.5980(7), b = 4.9877(2), c = 23.3878(13) ?, β = 93.254(3)o, Z = 4, V = 1583.67(14) ?3, μ = 0.237 mm-1, F(000) = 720, R = 0.0471 and w R = 0.1182. The molecules are related by inversion and paired into dimers via C–H···O interactions. The dimmers are interlinked due to strong N–H···O bonds, where O-atoms are of sulfonyl groups. The molecules are stabilized in the form of infinite two-dimensional network with base vectors [0 1 0] and [0 0 –1] in the plane(1 0 2). The existence of good intermolecular interactions suggests the biological importance of the synthesized molecule. The compound was screened for its interaction with FS-DNA using UV-visible spectroscopy. UV-visible spectroscopic results depict that the compound interacts with DNA by mixed binding mode intercalation along with hydrogen bonding. Negative values of ΔG(–23.34, –17.79 k J·mol-1) indicate spontaneity of the compound-DNA adduct formation.     

Crystal Structure and Antitumor Activity of Tri[2-[N-（4′-methyl-benzylsulfonyl）amino]ethyl]-amine

The crystal structure of the title compound (C27H38N4O7S3, Mr = 626.79) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pīwith a = 9.411(1), b = 11.645(2), c = 14.672(2) (A。), α = 91.80(1), β = 95.36(1), γ =104.56(1)o, V = 1547.0 (A。)3, Z = 2, Dc = 1.346 g/cm3, λ = 0.71073 (A。), μ(MoKα) = 0.289 mm－1 and F(000) = 664. The structure was refined to R = 0.0406 and wR = 0.1177 for 4103 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the title compound is a practically distorted tetrahedron and each molecule contains one lattice H2O by hydrogen bond. The antitumor activity of the title compound against HL-60 human leukemia cells has also been studied by MTT method.     

Synthesis, Crystal Structure and Luminescent Property of a One-dimensional Europium Citrate Complex

A new compound, [Eu(Hcit)(H2O)2]·H2O]n (1, Hcit3-= C(OH)(COO-)(CH2COO-)2), has been synthesized under hydrothermal reactions of europium oxide, MnCl2·4H2O and citric acid at 120 ℃ for three days. The compound was characterized by single-crystal X-ray diffraction analyses, IR and TGA. Complex 1 crystallizes in monoclinic, space group P21/n with a = 6.179(1), b = 9.688(2), c = 16.990(3) , β = 91.98(3)°, Z = 4, V = 1016.4(3) 3, C6H11EuO10, Mr = 395.11, Dc = 2.582 g/cm3, μ = 6.218 mm-1, F(000) = 760, R = 0.0183 and wR = 0.0411. Single-crystal X-ray analysis reveals that complex 1 displays 1D ladder chains along the a axis, with dinuclear Eu2O2 units serving as "steps" and carboxylate groups as "uprights", which are connected by hydrogen bonds. The solid-state luminescent property of complex 1 was investigated at room temperature. Upon excitation at 394 nm, compound 1 exhibits interesting luminescent properties with several intense bands in the visible region and the most intense and sharp emission being in the red region at 615 nm. The TGA and XRD results prove that complex 1 undergoes facile thermal decomposition to form Eu2O3 at about 870 ℃.     

Crystal Structure and Properties of the Calix[4]arene Derivative Containing Ethyl 2-Diazo-3-(ethylamino)-3-oxopropanoate Moieties

The target compound(C58H74N6O10) has been structurally determined by singlecrystal X-ray diffraction. The crystal is in the monoclinic system, space group C2/c, with a = 22.08(3), b = 12.628(19), c = 21.73(3) , β = 106.78(3)°, C58H74N6O10, Mr = 1015.23, Dc = 1.16239 g/cm3, V = 5801(14)3, Z = 4, F(000) = 2176, μ(MoKa) = 0.080 mm-1, T = 293(2) K, 5107 independent reflections with 3125 observed ones(I 2σ(I)), R = 0.0768 and w R = 0.2305 with GOF = 1.025(R = 0.1129 and w R = 0.2674 for all data). The calixarene moiety maintains the symmetric cone conformation through intramolecular O–H···O and N–H···O hydrogen bonds. The thermal analysis showed that the decomposition mechanism of compound 3 is complex. Fluorescence spectra of 3 exhibited an emission band at 423 nm when excited with 360 nm radiation at room temperature in DMF.     

Synthesis,Crystal Structure,and Biological Activity of 4-Chlorobenzaldehyde (2-trifluoromethylTrifluoromethyl-5,6,7,8-tetrahydrobenzo[4 ,5]-thieno[2,3-d]pyrimidin-4-yl)hydrazone Monohydrate

The novel title compound 4-chlorobenzaldehyde (2-trifluoromethyl-5,6,7,8- tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-4-yl)hydrazone monohydrate (C18H14ClF3N4SH2O, Mr = 428.86) has been synthesized by a condensation reaction of 4-chlorobenzaldehyde with (2-trifluoromethyl-5,6,7,8-tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-4-yl)hydrazine, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 7.4252(7), b = 26.344(2), c = 10.3095(9) , = 109.407(2)°, V = 1902.0(3) 3 , Z = 4, Dc = 1.498 g/cm3 , μ = 0.356 mm-1 , F(000) = 880, the final R = 0.0564 and wR = 0.1681 for 2343 observed reflections with I > 2 (I). X-ray diffraction analysis reveals that the title hydrazone molecule is nearly planar except for the cyclohexene and trifluoromethyl moieties. In the crystal packing, the molecules form stacks by a three-dimensional framework, which results from intermolecular N(3)-H(3)···O(1), O(1)-H(1B)···N(2), O(1)- H(1B)···N(4) and O(1)-H(1A)···F(1) hydrogen bonds via water molecules together with π-π stacking interactions. Molecular geometry of the title compound in the ground state optimized by B3LYP functional with 6-311G** basis sets indicates that the calculations are in agreement with the experimental data. The preliminary bioassay suggested that the title compound exhibits relatively good fungicidal activity against Fusarium oxysporium f.sp.vasinfectum and Dothiorella gregaria.     

Synthesis, Crystal Structure and Antiproliferative Activity of 2,2-Dimethyl-4-oxochroman-3-ylmorpholine-4-carbodithioate

The crystal structure of the new title compound 2,2-dimethyl-4-oxochroman-3-ylmorpholine-4-carbodithioate(C16H19NO3S2,Mr = 337.44) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 9.5518(7),b = 9.7172(7),c = 11.0220(8),α = 67.08(1),β = 74.66(1),= 61.31(1)°,V = 822.72(10)3,Z = 2,Dc = 1.362 g/cm3,F(000) = 356,μ = 0.092 mm-1,MoKa radiation(λ = 0.71073),R = 0.0515 and wR = 0.1389 for 2623 observed reflections with I > 2(I).X-ray diffraction analysis reveals that the chroman ring adopts a half-chair conformation while the morpholine ring shows a chair conformation.Intramolecular and intermolecular C-H···S and C-H···O hydrogen bonds together with π-π interations are found in the structure.The result of MTT assay shows the title compound displays good antiproliferative activity against two human cancer cell lines.     

Synthesis,Crystal Structure and Antitumor Activities of N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline

The title compound, N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline(C16H15N3O2, Mr = 281.31), has been synthesized by the multicomponent reaction of milder Ullmann, and its structure was characterized by 1H NMR, 13 C NMR, IR, H RMS(ESI) and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group I2/c with a = 15.0212(10), b = 9.4911(6), c = 20.3075(13) A, β = 100.776(7)o, V = 2844.1(3)A3, Z = 8, Dc = 1.314 g/cm3, F(000) = 1184.0, μ = 0.089 mm-1, the final R = 0.0574 and w R = 0.1688 for 1701 observed reflections(I 2σ(I)). X-ray analysis indicates three major N(2)–H(2)···O(2), C(13)–H(13)···O(2), N(2)–H(2)···N(3) hydrogen bonds and π-π stacking interactions in the crystal structure. The preliminary biological test shows that the title compound has a good antitumor activity against A549 in vitro with the IC50 value of 35 μmol/L.     

Synthesis,Crystal Structure and Biological Activity of 8-（（4-（（2,3-diaminopyridin-4-yl）oxy）-3-fluorophenyl）-amino）-2-（4-fluorophenyl）-3-methyl-2,7-naphthyridin-1（2H）-one

The new title compound 8-((4-((2,3-diaminopyridin-4-yl)-oxy)-3-fluorophenyl)-amino)-2-(4-fluorophenyl)-3-methyl-2,7-naphthyridin-1(2H)-one(C26H20F2N6O2, Mr = 486.48) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 15.365(3), b = 13.144(2), c = 11.863(2), β= 108.882(3)°, Z = 4, V = 2267.0(7)3, Dc = 1.425 g/cm3, F(000) = 1008, μ = 0.105 mm-1, MoKa radiation(λ = 0.71073), R = 0.0480 and wR = 0.1294 for 3197 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the region C(substituents of 8-amino group and 3-methyl group on the 2,7-naphthyridin-1(2H)-one ring) of compound 6 are effectively planar. Intramolecular and intermolecular hydrogen bonds together with π···π interations are found in the structure. In addition, compound 6 shows potent c-Met and c-Kit kinase inhibition activities.     

Synthesis,Crystal Structure and Biological Activity of 2-(1-(3-Bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbonyl)piperidin-4-yl)-N-isopropyl-1,3-thiazole-4-carboxamide

The title compound 2-(1-(3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbonyl)piperidin-4-yl)-N-isopropylthiazole-4-carboxamide(C21H22Br Cl N6O2 S,Mr = 536.04) has been synthesized,and its structure was characterized by IR spectra,1H-NMR,13C-NMR,EA,and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic system,space group P/c with a = 15.146(3),b = 11.573(2),c = 26.937(5) ?,β = 103.64(3)°,V = 1839.0(6) ?3,Z = 4,Dc = 1.557 g/cm3,μ(Mo Ka) = 0.71073 mm-1,F(000) = 2192,R = 0.0601 and w R = 0.1392.There exist one intramolecular hydrogen bond at N–H···N and four intermolecular weak interactions at O(2)···H(1),Cl(1)···H(12),O(1)···Cl(1) and S(1)···O(2).Bioassay results indicated that the title compound had good fungicidal and antiviral activities against tobacco mosaic virus.     

A 3D Hydrogen-bonded 2-Fold Interpenetrated Supramolecular Structure of Cyclen Derivative

The title compound 1,4,7,10-tetrakis(2-(4-methoxyphenoxy)ethyl)-1,4,7,10-tetraazacyclododecane hydrobromide derivated from cyclen has been synthesized by 4-methoxyphenol via two steps and characterized by ~1H NMR and X-ray single-crystal diffraction. The crystal belongs to the orthorhombic system, space group Pbcn with a = 17.3174(15), b = 12.9891(11), c = 19.3379(17) ?, V = 4349.8(7) ?3, Z = 4, Dc = 1.304 g/cm3, Mr = 853.87, F(000) = 1808, μ = 1.001 mm~(-1), Mo Ka radiation(λ = 0.71073 ?), R = 0.0467 and w R = 0.1045 for 2774 observed reflections with I 2σ(I). X-ray structural analysis reveals that the molecular structure of the title compound is stabilized by intramolecular C–H···O and C–H···Br hydrogen-bonding interactions, and a 3D 2-fold interpenetrated supramolecular framework is constructed by intermolecular C–H···O and C–H···Br hydrogen-bonding interactions.     

Synthesis and Crystal Structure of 1-Ethyl 3-Methyl 6-Benzyl-2-methyl-5-oxo-5,6-dihydropyrrolo[1,2-c]quinazoline-1,3-dicarboxylate

The crystal structure of the title compound(C24H22N2O5, Mr = 418.44) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P21/c with a = 7.751(2), b = 12.392(4), c = 21.326(6), V = 2048.4(1)3, Z = 4, Dc = 1.357 g/cm3, F(000) = 880, μ(MoKα) = 0.096 mm-1, the final R = 0.0731 and wR = 0.1982 for 3335 observed reflections(I 2σ(I)). Intermolecular C(24)–H(24B)···O(1) hydrogen bond is observed in the structure.     

Synthesis,Crystal Structure and Antitumor Activity of 4-(tert-butyl)-5-(1H-1,2,4-triazol-1-yl)-N-(2-hydroxy-3,5-diiodinebenzyl)-thiazol-2-amine

The title compound, 4-(tert-butyl)-5-(1H-1,2,4-triazol-1-yl)-N-(2-hydroxy-3,5-diiodinebenzyl)thiazol-2-amine, was synthesized via the reduction of 4-(tert-butyl)-5-(1H-1,2,4-triazol-1-yl)-N-benzylidene-thiazol-2-amine with Na BH4, and its crystal structure was determined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a = 7.91944(19), b = 10.5250(3), c = 24.4985(6) , Z = 4, V = 2041.66(9) 3, Mr = 599.22, Dc = 1.949 Mg/m3, S = 1.120, μ = 3.203 mm-1, F(000) = 1152, the final R = 0.0283 and wR = 0.0592 for 3490 observed reflections(Ⅰ 2σ(Ⅰ)). X-ray analysis displays that the crystal water takes part in three intermolecular hydrogen bonds of O(2)–H(2A)···O(1), O(2)–H(2B)···N(1) and N(5)–H(5)···O(2), and an octatomic ring is formed via intramolecular hydrogen bond of O(1)–H(1A)···N(4). Furthermore, the Ⅰ···Ⅰ contacts are involved in stabilizing the overall three-dimensional network structure. The preliminary biological test shows the title compound has good antitumor activity with the IC50 value of 26 μM against the Hela cell line.