Studies on the Synthesis,Crystal Structure and Quantum Chemistry of Di（o-cyanobenzyl）tin Bis（quinoline-2-carboxylate）

Di（o-cyanobenzyl）tin bis（quinoline-2-carboxylate） was synthesized by the reaction of tri（o-cyanobenzyl）tin chloride with quinoline-2-carboxylic acid. The molecular structure of the compound was characterized by elemental analysis, IR, 1H NMR and X-ray diffraction. Crystal data for the compound： tficlinic, space group P1, a = 0.80734（7）, b = 1.00681（9）, c = 1.04811（9） nm, a = 81.7570（10）, β = 7.7240（10）,γ = 81.2850（10）°, V = 0.77581（12） nm3, Z = 1, Dc = 1.488 g/cm3, μ（MoKa） = 0.870 mm^-1 and F（000） = 350. The final R= 0.0204 and wR= 0.0530 for 2677 observed reflections with I 〉2σ（I）, and R = 0.0208 and wR = 0.0532 for all reflections. The molecular structure adopts a distorted octahedral geometry around the Sn atom. The title compound molecules are connected via hydrogen bonding interactions to form a 3D network structure. Quantum chemistry calculation study on the title compound has been performed by means of G98W package at the Lanl2dz basis set. The stability of the compound, orbital energies and some frontier molecular orbital composition characteristics have also been investigated.     

Synthesis and Crystal Structure of 2-（4-Fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H- 1,2,4-triazol-1-ylmethyl）-3-methoxy-isopropy Alcohol

The title compound 2-（4-fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H-1,2,4-triazol- 1-ylmethyl）-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-（4-fluoro- 2-（4-fluorophenoxy）phenyl）-2,3-epoxypropyl]-1H-1,2,4-triazole with sodium methoxide. It belongs to orthorhombic, space group P212121, with a = 9.7229（19）, b = 11.516（2）, c = 16.047（3）A, C18H17F2 N3O3, Mr = 361.35, V = 1796.7（6）A^3, Z = 4, Dc = 1.3359 g/cm^3, F（000） = 752, p = 0.106 mm^-1, the final R = 0.0329 and wR = 0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56（3） and 54.78（2）°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

Synthesis and Crystal Structure of 2,3,4,6-tetra-O-Acetyl-1-{4-chloro-3-[1-（4-ethoxyphenyl）-1-methylethyl]phenyl}-1-deoxy-β-D-glucopyranose

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system(C31H37ClO10,Mr = 605.06),space group P21 with a = 11.882(5),b = 10.106(5),c = 13.816(6),V = 1545.9(12)3,Z = 2,Dc = 1.300 g/cm3,F(000) = 640,μ = 0.179 mm-1,the final R = 0.0430 and wR = 0.0595 for 4960 observed reflections(I > 2σ(I)).The title compound was confirmed to be a β-anomer by single-crystal X-ray diffraction and 1H NMR.The proximal benzene ring is nearly orthogonal to the glucopyranoside ring,and the two benzene rings are also almost orthogonal to each other.Four non-classical intermolecular hydrogen bonds observed in the crystal lattice help to stabilize the crystal.     

Synthesis and Crystal Structure of N-（1′-H-Pyrrol- 2′-ylcarbonyl）-5-amino- 1,10-phenanthroline

The title compound, N-（1′-H-pyrrol-2′-ylcarbonyl）-5-amino-1,10-phenanthroline, was synthesized by the reaction of a-pyrrolyl carbonyl chloride and 5-amino-1,10-phenanthroline in pyridine. Determined by X-ray structure analysis, it crystallizes in triclinic system, space group P1 with the following crystallographic data： C20H21N5O3, Mr = 379.42, a = 7.8559（4）, b = 9.1681（6）, c = 14.6818（9） A, α= 73.254（10）,β= 88.938（15）, γ= 68.080（10）°, V= 934.66（10） A3, Z = 2, F（000） = 400, Dc = 1.348 g/cm^3 and p = 0.094 mm-1. The final R = 0.0680 and wR = 0.1419 for 2142 observed reflections with I 〉 2σ（/）, and R = 0.1084 and wR = 0.1643 for all reflections. Two aromatic ring planes （pyrrole and phenanthroline rings） are connected by the amide plane. Two different types of intermolecular hydrogen bonds, O-H…N and N-H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 3-D supramolecule.     

Synthesis,Crystal Structure and Antifungal Activities of 3-Methyl-l-（4-methylphenyl）-4- （N-4-trifluoromethylphenyl）-aminomethyl- 5-（4-methoxyphenylthio）-lH-pyrazole

The title compound 3-methyl-l-（4-methylphenyl）-4-（N-4-trifluoromethylphenyl） aminomethyl-5-（4-methoxyphenylthio）-lH-pyrazole has been synthesized via a four-step reaction and characterized by IR, 1H NMR, elemental analysis and X-ray crystallography. The compound crystallizes in monoclinic, space group P21/c with a = 8.7170（15）, b = 18.355（3）, c = 15.292（3） A, fl = 103.445（3）°, V= 2379.7（7） A3, Dc = 1.350 g/cm3, Z = 4, p = 0.184, F（000） = 1008, and the final R = 0.0491 and wR = 0.1339 for 4160 observed reflections （I 〉 2a（/））. The results demonstrate that there is a face-to-face π-π stacking interaction between one benzene ring （C（19）-C（24）） and another （C（I 3）-C（! 8）） at a plane-plane distance of 3.3539 A. The ring normal and vector between the ring centroids form an angle of 18.2° up to the centroid-to-centroid distance of 3.5273 A. The crystal structure is stabilized by the intermolecular hydrogen bond of N（3）-H（3A）...N（2） （symmetry code： A -x＋l, -y＋l, -z）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis,Crystal Structure and Biological Activities of N-（4-Cyanopyrazole-3-yl）- α-（3,5-difluorophenyl）- O,O-diisopropyl- α-aminophosphonate

The title compound has been synthesized by the addition reaction of N-（4-cyanopyrazole-3-yl）-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959（14）, b = 9.2212（7）, c = 22.1108（16）A^°, β= 90.1540（10）°, V = 3873.0（5） A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F（000） = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections （I 〉 2σ（I））. The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N（3）. The crystal structure is stabilized by two intermolecular hydrogen bonds of N（1）-H（1）…O（3） and N（3）-H（3A）…N（4）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Studies on the Synthesis,Crystal Structure and Quantum Chemistry of Di(o-cyanobenzyl)tin Bis(quinoline-2-carboxylate)

Di(o-cyanobenzyl)tin bis(quinoline-2-carboxylate)was synthesized by the reaction of tri(o-cyanobenzyl)tin chloride with quinoline-2-carboxylic acid.The molecular structure of the compound Was characterized by elemental analysis,IR,1H NMR and X-ray diffraction.Crystal data for the compound:triclinic,space group P1,a=0.80734(7),b=1.00681(9),c=1.04811(9)nm,α=81.7570(10),β=7.7240(10),γ=81.2850(10)°,V=0.77581(12)nm3,Z=1,Dc=1.488 g/cm3,μ(MoKa)=0.870 mm-1 and F(000)=350.1 The final R=0.0204 and wR=0.0530 for 2677 observed reflections with I＞2σ(I),and R=0.0208 and wR=0.0532 for all reflections.The molecular structure adopts a distorted octahedral geometry around the Sn atom.The title compound molecules are connected via hydrogen bonding interactions to form a 3D network structure.Quantum chemistry calculation study on the title compound has been performed by means of G98W package at the Lanl2dz basis set.The stability of the compound,orbital energies and some frontier molecular orbital composition characteristics have also been investigated.     

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.     

Synthesis,Crystal Structure and Antifungal Activities of 3-Methyl-1-(4-methylphenyl)-4-(N-4-trifluoromethylphenyl)-aminomethyl-5-(4-methoxyphenylthio)-1H-pyrazole

The title compound 3-methyl-1-(4-methylphenyl)-4-(N-4-trifluoromethylphenyl) aminomethyl-5-(4-methoxyphenylthio)-1H-pyrazole has been synthesized via a four-step reaction and characterized by IR,1H NMR,elemental analysis and X-ray crystallography.The compound crystallizes in monoclinic,space group P21/c with a = 8.7170(15),b = 18.355(3),c = 15.292(3) ,β = 103.445(3)°,V = 2379.7(7) 3,Dc = 1.350 g/cm3,Z = 4,μ = 0.184,F(000) = 1008,and the final R = 0.0491 and wR = 0.1339 for 4160 observed reflections(I 2σ(I)).The results demonstrate that there is a face-to-face π-π stacking interaction between one benzene ring(C(19)~C(24)) and another(C(13)~C(18)) at a plane-plane distance of 3.3539 .The ring normal and vector between the ring centroids form an angle of 18.2o up to the centroid-to-centroid distance of 3.5273 .The crystal structure is stabilized by the intermolecular hydrogen bond of N(3)-H(3A)···N(2)(symmetry code:A –x+1,–y+1,–z).The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis and Crystal Structure of Cis-syn Cyclobutane 1-（Carboxyethyl）thymine Dimer Monopentyl Amide Monotryptophan Methyl Ester Amide

The crystal structure of the title compound (C34H47N7O9, Mr = 697.79) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21 with a = 9.000(8), b = 11.360(10), c = 17.841(15) , β = 97.083(14)°, V = 1810(3) 3, Z = 2, F(000) = 744, Dc = 1.280 g/cm3, μ = 0.094 mm-1, the final R = 0.0721 and wR = 0.1942 for 2479 observed reflections with I > 2σ(I). The two methyl groups attached to the cyclobutane ring are cis oriented. An intramolecular hydrogen bond (N(6)-H(6)…O(8)) introduces rigidity into the title molecule and the crystal structure is stabilized by intermolecular N-H…O hydrogen bonds.     

Synthesis and Crystal Structure of Methyl 3-（5- Bromo-1-ethyl-1H-indole-3-carbonyl）aminopropionate

Methyl 3-(5-bromo-1-ethyl-1H-indole-3-carbonyl)aminopropionate has been syn-thesized by the acylation of 5-bromo-3-trichloroacetylindole with β-alanine methyl ester,followed by alkylation with ethyl iodide,in 82.6% yield.Its crystal structure was gotten and determined by X-ray diffraction method.The crystal is of monoclinic,space group P2 1 /c with a=11.7927(8),b=14.9342(8),c=9.0060(5),β=101.558(6)°,V=1553.93(16)3,Z=4,D c=1.510 g/cm 3,λ=0.71073,μ(MoKα)=2.656 mm-1,M r=353.22 and F(000)=720.The structure was refined to R=0.0401 and wR=0.0825 for 1704 observed reflections with I > 2σ(I).In the crystal structure,intermolecular N(2)-H(2)···O(1) hydrogen bond and weak intermolecular bonds (C(1)-H(1) O(1) and C(10)-H(10B) O(2)) are formed,and π-π stacking also exists.     

Synthesis, Crystal Structure Analysis and DFT Calculation of 1-Benzoyl-3,6-diphenyl-1,4-dihydro-1,2,4,5-tetrazine

The new title compound, 1-benzoyl-3,6-diphenyl-1,4-dihydro-1,2,4,5-tetrazine (C21H16N4O, Mr = 340.38), has been prepared and its crystal structure can not be confirmed by the results of MS, elemental analysis, IR spectrum and 1H NMR spectrum, but determined by X-ray diffraction. The title compound crystallizes in an orthorhombic space group P212121 with a = 7.1100(19), b = 12.115(3), c = 19.884(6), V = 1712.7(8)3, Z = 4, Dc = 1.320 g/cm3, F(000) = 712, μ = 0.085 mm-1, MoKa radiation (λ = 0.71073), R = 0.0334 and wR = 0.0845 for 2254 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the central tetrazine adopts an unsymmetrical boat conformation. According to the bond lengths of tetrazine ring, the molecule should be 1,4-dihydro-1,2,4,5-tetrazine, rather than 1,2-dihydro-1,2,4,5-tetrazine. The crystal structure is stabilized mainly by intermolecular N–H···O hydrogen bonds.     

Synthesis, Crystal Structure and Antidepressant Activity of 5-[4-(Benzyloxy)phenyl]-9-(n-propyl)-4,6-dioxa-1-azabicyclo[3.3.1]nonane Hydrochloride 0.5Hydrate

The title compound 2(C22H28N+O3)·H2O·2Cl-was synthesized by the reaction of 2-bromo-1-[4-(benzyloxy)phenyl]-1-pentone with 2,2'-azanediyldiethanol. The crystal determined by X-ray diffraction analysis belongs to the monoclinic system, space group Pc with a = 18.312(3), b = 14.838(3), c = 7.6227(14) , β = 97.981(4)°, Z = 2, Mr = 797.82, V = 2051.1(6) 3, Dc = 1.292 g/cm3, S = 0.956, μ = 0.21 mm-1, F(000) = 852, the final R = 0.0625 and wR = 0.1428 for 5683 observed reflections (Ⅰ > 2σ(Ⅰ)). Flack parameter is 0.10(9). The title compound is composed by four non-coplanar ring systems, two benzenes and two morpholines. One morpholine ring (C(3)-C(4)-N(1)-C(1)-C(2)-O(1)) forms a chair conformation, while the other (C(4)-C(3)-O(2)-C(6)-C(5)-N(1)) assumes a boat conformation. X-ray crystal structure displays extensive N-H…Cl and O-H…Cl intermolecular hydrogen bonds. The preliminary antidepressant activity test indicates that the inhibition ratio of SERT (5-HT Transporter) was 35.9% at the dosage of 10.0 mg/L.     

Synthesis,Characterization and Crystal Structure of a Trinuclear Diorganotin(Ⅳ) Complex with N'-acetylsalicylhydrazide

A diorganotin(IV) complex [(CH3)2Sn]3L2(L=N'-acetylsalicyl-hydrazide) 1 has been successfully synthesized and structurally characterized by elemental analysis,FT-IR,NMR(1H,13C and 119Sn) spectra and X-ray crystallography.The crystal structure belongs to an orthorhombic system,space group Pnma with a=8.5047(16),b=28.466(5),c=12.842(2) ,V=3109.1(10)3,C24H32N4O6Sn3,Mr=828.61,Dc=1.770 g/cm3,μ(Mo-Kα)=2.432 mm-1,Z=4,F(000)=1608,the final R=0.0378 and wR=0.0973 for 2125 observed reflections(Ⅰ 2σ(Ⅰ)).The complex is a trinuclear organotin(Ⅳ) containing five-and six-coordinated tin atoms.And weak but significant Sn···O intermolecular interactions lead to the assembly of complex into a 1D linear polymeric chain supramolecular framework.     

Syntheses and Crystal Structures of Two Diethyltin Complexes of N-Salicylidene-α-amino Acid

Two novel diethyltin（IV） complexes of N-salicylidenevaline （H2L1） and N-Sali- cylidenetryptophan （H2L^2）, Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730（5）, c = 23.6890（13）A^°, V= 7620.4（5） A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F（000） = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550（8）, b = 11.5425（7）, c = 12.7876（7）A^°, β= 93.585（1）°, V = 2026.3（2） A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F（000） = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.     

Synthesis and Crystal Structure of (9S)-2'-O-Benzoyl-9,11-[carbonylbis(oxy)]-9-deoxo-5-O-(β-D-desosaminyl)-12,21-anhydro-9-hydroxy-erythronolide A

The title compound (9S)-2'-O-benzoyl-9,11-[carbonylbis(oxy)]-9-deoxo-5-O-(-D-desosaminyl)-12,21-anhydro-9-hydroxyerythronolide A 1 was synthesized. The crystal structure of the acetone solvate of 1, C37H55NO11·C3H6O, was determined by single-crystal X-ray diffraction analysis. It belongs to monoclinic system, space group P21 with a = 14.4691(10), b = 8.2626(6), c = 17.5990(11) A, β = 94.167(1)°, V = 2098.4(2)A3, M,= 748, Z = 2, De= 1.184 g/cm3,μ = 0.087 mm-1, F(000) = 808, S = 1.026, R= 0.0542 and wR = 0.1322 for 3331 observed reflections (I > 2σ(Ⅰ)). In the solid state, molecules of 1 are linked into spirals along the b axis by O(25)-H(25)…O(29) intermolecular hydrogen bond.     

2-[(2-溴苯胺基)甲基]-4-氯苯酚Schiff碱及其铜配合物的合成及晶体结构

以5-氯水杨醛和邻溴苯胺为原料合成了一种新的Schiff碱配体2-[(2-溴苯胺基)甲基]-4-氯苯酚(1)(C₁₃H₉BrClNO,H₂L),继而与过渡金属铜离子配合,得到其配合物2 ([Cu(C₁₃H₈BrClNO)₂],CuL₂)。通过X-射线衍射法对配体及其配合物进行了结构表征。化合物1属正交晶系,Pbca空间群,晶胞参数a=0.710 19(12) nm,b=1.308 2(2) nm,c=2.533 3(5) nm,M_r=310.57,V=2.353 6(7) nm³,D_c=1.753 g·cm^-3,Z=8,μ=3.700 mm^-1,Z=8,F(000)=1 232,R=0.025 0,wR=0.055 5;化合物1依靠分子间的C-H…N,C-H…O,C-H…Cl 氢键及π-π堆积作用进一步联结成二维网状结构。化合物2属单斜晶系,P2₁/c空间群,晶胞参数a=0.956 8(2) nm,b= 1.085 3(3) nm,c=1.204 7(3) nm,β=105.965(7)°,M_r=682.67,V=1.202 8(6) nm³,D_c=1.885 g·cm^-3,Z=2,μ=4.481 mm^-1,F(000)=670,R=0.045 0,wR=0.122 5。2依靠分子间C-H…π作用及卤素…卤素作用进一步联结成三维网状结构。     

丙酰皮考林酰肼(C_9H_(11)N_3O_2 )的合成和晶体结构

合成了标题化合物(C9H11N3O2,Mr=193.21),晶体属于单斜晶系,空间群为C2/c, a=13.703(1),b = 9.142(1), c = 16.437(2)?, ( = 105.547(3)(,V = 1983.8(4)?,Z = 8, Dc=1.294g/cm3, F(000)= 816,(??o?α)=0.094 mm-1,R=0.0527, wR=0.1517,I(2((I)的可观察衍射点1596个。有机分子间以氢键相联并形成网状结构,N(2)-H...N(1a)(a: -x+1, y, -z+1/2)和N(3)-H…O(2b)(b: -x+1/2, y-1/2, -z+1/2)键键长分别为3.007(2)和2.786(2)?。     

Synthesis and Crystal Structure of (4R, 5R)(5-Hydroxymethyl-2,2-dimethyl- [1,3]dioxolan-4-yl)-bis-(4-methoxy-phenyl)-methanol

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅα ,α ,α′,α′ ｔｅｔｒａａｒｙｌ 1 ,3 ｄｉｏｘｏｌａｎｅ 4,5 ｄｉｍｅｔｈａｎｏｌｓ (ＴＡＤＤＯＬＳ)ｄｉｏｌｓｗｈｉｃｈａｒｅｒｅａｄｉｌｙａｖａｉｌａｂｌｅｆｒｏｍａｌｋｙｌｔａｒｔｒａｔｅｓ ,ｈａｖｅｂｅｅｎｗｉｄｅｌｙｕｓｅｄａｓｃｈｉｒａｌｌｉｇａｎｄｓｉｎｅｎａｎｔｉｏｓｅｌｅｃｔｉｖｅａｄｄｉｔｉｏｎｒｅａｃｔｉｏｎｓｏｆｃａｒｂｏｎ ｃｅｎｔｅｒｅｄｎｕｃｌｅｏｐｈｉｌｅｓｔｏａｌｄｅｈｙ ｄｅｓ[1 ] ,ｉｎ [2 +2 ]ｃｙｃｌｏａｄｄｉｔｉｏｎｓ[2 ] …