Synthesis and Crystal Structure of 1-（N,N-Di-（p-toluenesulfonyl））-amino- 2-（N＇-p-toluenesulfonyl）-amino-3,5-dinitrobenzene

The title compound, 1-(N,N-di-(p-toluenesulfonyl))-amino-2-(N'-p-toluenesulfonyl)-amino-3,5-dinitrobenzene, was synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in orthorhombic, space group Pna21 with a = 13.723(2), b =25.354(4), c = 8.6565(12)(A), V= 3011.9(8)(A)3, Z= 4, Mr = 660.68, F(000) = 1368, Dc = 1.457 g/cm3,μ = 0.309, the final R = 0.0609 and wR = 0.1042. The H atom of N2-H group, which is the unique recognition site to anion, is enveloped by two oxygen atoms and one benzene from two and one p-toluenesulfonyl moieties, respectively.     

Synthesis and Crystal Structure of 3,5-Diphenyl- 1,2- di（4- chlorophenyl）pyrrole

1 INTRODUCTION The pyrrole ring constitutes a basic heteroaro- matic structure. It is a vital building block for the construction of porphyrins and alkloids[1]. Several substituted pyrroles have potential applications as fungicides and bactericides and as active compo- nents of nonsteroidal anti-inflammatory drugs inhi- biting human cyclooxygenase[2, 3]. Besides the clas- sical Knorr’s method, there are a number of poten- tially useful methods for the synthesis of pyrrole he- terocyclic …     

Synthesis and Crystal Structure of 1,2-Bis（2-benzimidazolyl）benzene

The title compound C6H4(C7H5N2)2 was prepared by the condensation of o-phenylenediamine with o-phthalic acid and characterized by elemental analysis, IR, UV and ^1H NMR spectra, and its structure was determined by single-crystal X-ray diffraction,showing the compound molecule belongs to (72 point group. A ID chain structure was formed by the intermolecular hydrogen bonds (N(2)H…N(I)).     

Synthesis and Crystal Structure of Tetra（o-cyanobenzyl）tin

The tetra（o-cyanobenzyl）tin compound has been synthesized by the reaction of cyanobenzyl chloride with tin, and its molecular structure was characterized by elemental analysis, IR spectra, ^1H NMR and X-ray diffraction. Crystal data for this compound： monoclinic, space group C2/c, Mr = 583.24, a = 1.9629（2）, b = 1.05967（13）, c = 1.41249（18） nm, β= 118.180（2）^o, V = 2.5898（5） nm^3, Z = 4, Dc =1.496 g/cm^3, μ（MoKa） = 1.015 cm^-1, F（000） = 1176, R = 0.0189, wR = 0.0497 （observed reflections with I 〉 20（I）） and R = 0.0218, wR = 0.0513 （all reflections）. The molecular structure adopts a distorted tetrahedral geometry around the tin atom. The Sn＇＂N weak interaction between the Sn and N atoms of cyano forms an intermolecular H-bonding, and the bond length is 0.3570 nm; the interaction between hydrogen of methylene and benzene ring of benzyl forms C-H…C with its bond length of 0.2817 nm; and the interaction among hydrogen of benzene ring and carbon of cyano forms Ph-H…C bond （0.2897 nm） Of the σ…π interaction. A 3D chain structure is formed by the above weak intermolecular interactions.     

Synthesis and Crystal Structure of a Novel Ion-pair Compound Consisting of 1-（4-Bromobenzyl）pyridinium Cation and 7,7,8,8-Tetracyanoquinodimethanide Anion

The title compound [BrBzPy][TCNQ] （BrBzPy^＋=1-（4-bromobenzyl）pyridinium cation, TCNQ = 7,7,8,8-tetracyanoquinodimethanide anion） was synthesized by the reaction of [BrBzPy]Br and LiTCNQ in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 14.067（3）, b = 7.3089（14）, c = 23.796（4）A, β = 122.011（9）°, V= 2074.6（7）A^3, Z = 4, C24H15BrN5, Mr = 453.32, Dc = 1.451 g/cm^3,μ = 2.002 mm^-1, S = 1.047, F（000） = 916, R = 0.0398 and wR = 0.0921. The most prominent structural features are the completely segregated stacking columns of the TCNQ- anions and [BrBzPy]^＋ cations. In a TCNQ column, the centroid-to-centroid distances of the neighboring anions of TCNQ are 3.2693 and 4.9464 A, respectively.     

Synthesis and Crystal Structure of 3-（Trichloroacetyl） Indole

1 INTRODUCTION Indole and its derivatives have attracted much at-tention due to their chemical properties as well asbiological activities[1, . They have been widely used 2]as the materials for producing pigment, perfume,plant growth regulators, etc. Recently, it has alsobeen found that some indole derivatives present anti-tumor and antiviral activities[3～5]. During our sear-ches for bioactive compounds, a series of indole deri-vatives were synthesized, among …     

Synthesis, Crystal Structure and AbsoluteConfiguration of （＋）-O-Phenyl Cyclophosphorodiamidate

The title compound, ( )-O-phenyl cyclophosphorodiamidate (C28H33N202P, Mr=460.53), has been synthesized and characterized by 31p NMR, 1H NMR and elemental analysis. X-ray diffraction analysis at 273(2) K indicates that it belongs to orthorhombic system, space group P212121 with a=11.518(4), b=13.449(4), c=16.539(5)A, V=2562(1)A3, Z=4, Dc=1.194g/cm3, F(000)=984 and μ(MoKα)=0.134mm-l. The structure parameters were refined by full-matrix least-squares on F2 to R=0.0459 and wR=0.0640. The flack χ parameter is 0.03(10), and the absolute configuration of the phosphorus atom in the title compound is S.     

Synthesis and Crystal Structure of 5-N-i-Propyl-2- （ 2＇ -nitrobenzenesulfonyl） -glutamine

The title compound, 5-N-i-propyl-2-(2′-nitrobenzenesulfonyl)-glutamine, was synthesized and its structure was confirmed by IR, MS, ¹H NMR, and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P2 (1), with a = 0.69281(11) nm, b = 0.76508(12), c = 1.5843(3) nm, = 90°, β = 90.941(3)°, γ = 90°, V = 0.8397(2) nm³, Z = 2, D_c = 1.477 g/cm³, μ = 0.236 mm^-1, F(000) = 392, R = 0.0297, and wR = 0.0664.     

Synthesis and Crystal Structure of N-Phenylbis（ferrocenecarboxyl）imide

The ferrocenyl compound,N-phenylbis(ferrocenecarboxyl)imide (C28H23NO2Fe2,Mr=517.17),was synthesized and structurally characterized by means of X-ray single-crystal dif-fraction. It crystallizes in monoclinic,space group C2/c with a=21.374(14),b=10.430(7),c= 10.741(7) ,β=114.184(8)°,V=2184(2) 3,Z=4,Dc=1.573 g/cm3,F(000)=1064,μ(MoKα)= 1.355 mm–1,T=291(2) K,the final R=0.0548 and wR=0.1437 for 1524 observed reflections with I > 2σ(I). In this compound,the nitrogen atom links two ferrocenyl groups and one phenyl group forming a novel imido derivative.     

Synthesis and Crystal Structure of 1-(N,N-Di-(p-toluenesulfonyl))-amino-2-(N'-p-toluenesulfonyl)-amino-3,5-dinitrobenzene

The title compound,1-(N,N-di-(p-toluenesulfonyl))-amino-2-(N'-p-toluenesulfonyl)-amino-3,5-dinitrobenzene,was synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in orthorhombic,space group Pna21 with a=13.723(2),b=25.354(4),c=8.6565(12) ,V=3011.9(8) 3,Z=4,Mr=660.68,F(000)=1368,Dc=1.457 g/cm3,μ=0.309,the final R=0.0609 and wR=0.1042. The H atom of N2-H group,which is the unique recognition site to anion,is enveloped by two oxygen atoms and one benzene from two and one p-toluenesulfonyl moieties,respectively.     

Synthesis and Crystal Structure of 4-（4-Bromophenyl）- 3,4-dihydro-6-methyl quinolin-2（1H）-one

The title compound (C16H14BrNO) has been synthesized by the reaction of p-tolylamine, Meldrum’s acid and 4-bromo-benzaldehyde, and its structure was characterized by IR, 1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 7.6850(11), b = 8.3004(11), c = 21.301(3) , β = 95.110(2)°, V = 1353.4(3) 3, Mr = 316.19, Z = 4, Dc = 1.552 g/cm3, μ(MoKα) = 3.028 mm-1, F(000) = 640, the final R = 0.0345 and wR = 0.0768. X-ray analysis reveals that the atoms of C(1), C(2), C(3), C(4), C(5) and N(1) form a six-membered ring of boat conformation.     

Synthesis and Crystal Structure of 2-Amino-4- chloro-5-（4-methylbenzyl）-6-methylpyrimidine

The title compound 2-amino-4-chloro-5-(4-methylbenzyl)-6-methylpyrimidine (C26H28Cl2N6, Mr = 495.44) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 14.892(7), b = 6.129(3), c = 14.889(7) , β = 109.795(8)°, V = 1278.7(10) 3, Z = 2, F(000) = 520, Dc = 1.287 g/cm3, μ = 0.280 mm-1, the final R = 0.0577 and wR = 0.1589 for 1357 observed reflections with I > 2σ(I). A total of 6091 reflections were collected, of which 2257 were independent (Rint = 0.033). The X-ray analysis reveals that the chlorine atom and methyl of the title compound are disordered.     

Synthesis and Crystal Structure of 3-（4-Ethoxyphenyl）-6-（phenoxymethyl）-1,2,4-triazolo[3,4-b][1,3,4]thiadiazole

The title compound C18H16N4O2S has been synthesized by the reaction of 4-amino-3-(4-ethoxyphenyl)-5-mercapto-1,2,4-triazole with phenoxyacetic acid in phospho- rus oxychloride, and characterized by IR, NMR spectra and elemental analysis. Its structure was determined by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a = 1.4903(3), b = 1.5230(2), c = 0.9615(16) nm, Z = 4, V = 1.7769(5) nm3, Dc = 1.317 g/cm3, μ = 0.201 mm-1, F(000) = 736, R = 0.0795 and wR = 0.2233. In the title compound, all rings are essentially planar.     

Synthesis and Crystal Structure of 3-Benzoyl-7,7-dimethyl-4-phenyl-2-phenylamino-4,6,7,8-tetrahydro-chromen-5-one

The title compound (C30H27NO3) was synthesized via a one-pot procedure starting from β-benzoylthioacetanilide, benzaldehyde and 5,5-dimethyl-1,3-cyclohexanedione, and its struc- ture was determined by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic system, space group P, with a = 6.325(2), b = 11.243(3), c = 17.553(4) , α = 87.306(4), β = 80.822(4), γ = 77.798(4)°, V = 1204.2(5) 3, Z = 2, Mr = 449.53, Dc = 1.240 g/cm3, μ = 0.080 mm-1, F(000) = 476, the final R = 0.0459 and wR = 0.0970 for 2301 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of 7-Acetamido-5-chloro-8-（p-methyl- oxybenzenesulfonyloxy）-2-styrylquinoline

The title compound 7-acetamido-5-chloro-8-(p-methyloxybenzenesulfonyloxy)-2- styrylquinoline 4 (C26H21ClN2O5S, Mr = 508.96) has been synthesized and characterized by 1H- NMR, IR, ESI-MS and single-crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pca21, with a = 7.920(3), b = 10.672(5), c = 28.008(12) , V = 2367.3(17) 3, Z = 4, Dc = 1.425 g/cm3, μ = 0.290 mm-1, F(000) = 1056, R = 0.0323 and wR = 0.0692 for 3895 unique reflections with 3127 observed ones (I > 2σ(I)). X-ray analysis reveals that the styrylquinoline subunit adopts a coplanar conformation, where the benzene ring and quinoline are in trans configuration.     

Synthesis and Crystal Structure of a Mo-S Cluster Compound Coordinated by Isonicotinate

A cluster compound, Mo3S4(DTP)3(IN)(Py)·EtOH I (DTP = diethyl dithiophospha- te, IN = isonicotinate) has been rationally synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 13.6345(2), b = 13.7805(2), c = 14.5400(1) , α = 107.078(1), β = 113.380(1), γ = 96.310(1)o, C25H45Mo3- N2O9P3S10, Mr = 1218.96, V = 2315.75(5) 3, Z = 2, Dc = 1.748 g/cm3, μ = 1.399, F(000) = 1224, R = 0.0425 and wR = 0.1144 for 6335 observed reflections (I > 2σ(I)). 31P NMR spectrum has been measured with the resonance 110.050 and 108.783 (2:1).     

Synthesis and Crystal Structure of 3,6-Dimethyl- 9-（4-b rom o p h enyl）- 1,8-oxo-2,7,10-trioxanth ene

The crystal structure of the title compound (C19H13BrO5) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/c,with a=10.508(4),b=11.354(4),c=14.522(5),β=106.255(4)°,V=1663.4(10)3,Mr=401.20,Z=4,Dc=1.602 g/cm3,λ=0.71073,F(000)=808,μ= 2.498 mm-1,R=0.0337 and wR=0.0837 for 2200 observed reflections (I>2σ(I)). X-ray analysis reveals that the dihedral angles between planes 1 and 2,1 and 3,1 and 4,2 and 3,2 and 4,and 3 and 4 are 78.6,82.5,87.4,5.6,9.5 and 4.9°,respectively. There exists a conjugated system in the molecular structure.