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 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 a Novel Aminothiourea Derivative Bearing Sugar Moiety

5-O-Benzoyl-1,2-O-isopropylidene-α-D-erythro-ketofuranose-3-ulose-3-aminothiose 3 was synthesized and characterized by spectral analysis, and its crystal structure was determined by X-ray diffraction analysis. The crystal belongs to orthorhombic, space group P212121 with a = 6.6276(13), b = 10.993(2), c = 25.027(5) , β = 90°, V = 1823.4(6)3, Z = 4, C16H20N3O5S, Mr = 366.41, Dc = 1.335 g/cm3, μ = 0.208 mm-1, F(000) = 772, S = 1.007, the final R = 0.0465 and wR = 0.1061 for 3251 observed reflections (I > 2σ(I)). Four hydrogen bonds are observed. The absolute configuration of this molecule was confirmed by comparing with that of the original material.     

Synthesis and Crystal Structure of [Mn(DPMT)2Cl2(H20)2]

The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1 -[[2-(2,4-dichlorophenyl)-1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2-4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2/c with a=23.913(4), b=7.8883(13), c=8.6291(14) (A),β=95.816(3)°,V=1619.4(5)(A)3,Z=2,C24H26Cl6MnN6O6 Mr=762.15, Dc=1.563 g/cm3, μ=0.950 mm'1, S=1.045, F(000)=774, R=0.0462 and wR=0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.     

Synthesis and Crystal Structure of 4,4＂-Diamino-N,N＇-diethyl Bisbenzenesulfamide

A new compound of 4,4'-diamino-N,N'-diethyl bisbenzenesulfamide (C18H26N4O4S2,Fw = 426.55) has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to the monoclinic system, space group P21/c with a = 10.0623(9), b =13.6759(13), c =15.5309(14) (A),β = 100.482(2)°, V= 2101.6(3)(A)3, Dc = 1.348 g/cm3, F(000) = 904,μ = 0.285 mm-1, Z = 4, the final R = 0.0512 and wR = 0.1363 for 3485 observed reflections with I ＞2σ(Ⅰ). The structure of the title compound is pseudo secondary axisymmetric, and the two sulfamide-groups show distorted tetrahedral configurations.     

Crystal Structure and Conformation of an Imino Sugar

The title compound 3 was synthesized and characterized by IR,NMR and H-RMS,and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic system (C16H23NO7S,Mr=373.41),space group P21,with a=12.000(2),b=5.5970(11),c=13.689(3),β=93.25(3)°,V=917.9(3)3,Z=2,Dc=1.351 g/cm3,F(000)=396,μ=0.213 mm-1,the final R=0.0489 and wR=0.0777 for observed reflections (I > 2σ(I)). Three intramolecular and three intermolecular hydrogen bonds were found. The absolute configuration of this molecule was confirmed by comparing with the original material.     

Synthesis and Crystal Structure of {4-[2-（9- Hexyl-9H-carbazol-3-yl）vinyl]phenyl} Dimethylamine

The title compound {4-[2-(9-hexyl-9H-carbazol-3-yl)vinyl]phenyl} dimethylamine has been synthesized by the well known Wittig reaction, and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 47.87(2), b = 10.222(4), c = 9.612(4) , β = 92.401(9)o, V = 4699(3) 3, Z = 8, C28H32N2, Mr = 396.56, Dc = 1.121 g/cm3, F(000) = 1712 and μ(MoKa) = 0.065 mm-1. The final R and wR are 0.0793 and 0.1983, respectively for 3524 observed reflections with I > 2σ(I). In the title compound, the bond lengths are normal, and the crystal is stabilized by Van der Waals’ forces.     

Synthesis and Crystal Structure of 3-Phenyi- 6-（4-methylphenyi）-1,2,4-triazolo[4,3-b]-1,2,4-triazine

1 INTRODUCTION The fused heterocycles bearing 1,2,4-triazine have attracted considerable attention in recent years owing to their biological and pharmaceutical activi- ties[1～3]. The 1,2,4-triazine core is a versatile synthe- tic platform to access a wide range of condensed heterocyclic ring systems via inter- and intramolecu- lar Diels-Alder reaction with a vast array of dieno- philes[4～6]. IBD (iodobenzene diacetate) is commer- cially available and used as benign non-metallic oxidant…     

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 4-[（1E）-（4-Hydroxy-3,5-dimethoxybenzylidene）-amino]-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

The title compound (C20H21N3O4, Mr = 367.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 7.5143(15), b = 13.901(3), c = 18.545(4) , V = 1937.1(7) 3, Z = 4, Dc = 1.260 g/cm3, μ = 0.089 mm-1, F(000) = 776, the final R = 0.0616 and wR = 0.0912. X-ray diffraction reveals that the molecule adopts an E configuration about the central C=N double bond. The intermolecular O–H…O hydrogen bond stabilizes the crystal structure by causing the formation of a supramolecular architecture.     

Synthesis and Crystal Structure of Metronidazole-derived Compound

A MET-OH derivative,MET-OTs 1,was designed,prepared and structurally charac-terized by single-crystal X-ray diffraction. X-ray structure analysis reveals that 1 crystallizes in the monoclinic system,space group P21/c,with a=16.1178(14),b=7.5473(6),c=13.4161(11),V= 1520.3(2)3,β=111.3210(10)o,Z=4,Dc=1.421 g/cm3 and F(000)=680.     

Synthesis and Crystal Structure of 1,2-Bis-（p-nitrophenylsulfonamido）-4,5-dinitrobenzene

The title compound, 1,2-bis-(p-nitro-phenylsulfonamido)-4,5-dinitrobenzene, was synthesized and characterized by elemental analysis, IR and 1H NMR. A pale yellow prism crystal of C23H26N8O13S2 (Mr = 686.64) was obtained in DMF solution and determined by single-crystal X-ray diffraction method. It crystallizes in triclinic system, space group P1 with a = 10.346(4), b = 12.210(5), c = 12.976(5) , α = 108.220(8), β = 99.482(4), γ = 95.490(4)°, V = 1516.7(10) 3, Z = 2, Dc = 1.504 g/cm3, F(000) = 712, μ = 0.254, Mr = 686.64, the final R = 0.0561 and wR = 0.1487. One sulfonamido group of the title compound is deprotoned and forms N(3)=C(13). The crystal involves N,N-dimethylamine from the decomposition of DMF and the proton is transferred to N,N- dimethylamine. It is a strong proof for the characterization of deprotoned recognition compound by X-ray single-crystal structure.     

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 4-Bromo-5-ethoxy-3-methyl-5- （naphthalen- 1-yl）- 1-tosyl- 1H-pyrrol-2（5H）- one

The title compound 4-bromo-5-ethoxy-3-methyl-5-(naphthalen-1-yl)-1-tosyl-1H- pyrrol-2(5H)-one 1 (C24H22BrNO4S, Mr = 500.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/n with a = 8.8562(15), b = 18.118(3), c = 14.055(2) , β = 99.855(3)o, V = 2221.9(6) 3, Z = 4, Dc = 1.496 g/cm3, μ = 1.975 mm-1, λ = 0.71073 , F(000) = 1024, R = 0.0607 and wR = 0.1371.     

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).     

Crystal Structure of Trans-2-Amino-3-Cyano-4-(3',4'-Methylenedioxyphenyl)-1-Phenyl-2-Cyclopentene-r-1-ol

1INTRODUCTIONIntheearlyseventiesthreegroupsofinvestigators('--"establishedthatlow--va-lenttitanium,preparedbythereactionofstrongreducingagentsontitaniumtrichlo-rideortitaniumtetrachlorideintetrahydrofuran,canabstractoxygenfromketonesoraldehydes,leadingtotheformationofolefins.Anincreasinginterestinthereac-tioninducedbylow--valenttitaniumreagentsisobservedandalargenumberoffunc-tionalgroupscanbereducedt4--6).However,thereactionoflow-valenttitaniumreagentwith4,4--dicyano--1,3--diaryl--l-butano…     

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.     

Synthesis and Crystal Structure of a 2-D Hydrogen-bonded Supramolecular Network {[Cu4(OH)4(2,2''-bpy)4(bqdc)]·2ClO4}n

The title compound {[Cu4(OH)4(2,2'-bpy)4(bqdc)]·2ClO4}n 1 (bqdc = 2,2'-biquinoline-4,4'-dicarboxylic acid) has been synthesized by hydrothermal method. Its crystal structure is of triclinic, space group P-1 with a = 7.6561(5), b = 12.4652(8), c = 15.7501(10) (A), α= 80.0480(10), β= 87.7900(10), γ = 74.0800(1)°, V = 1423.65(16) (A)3, Z = 2, C30H23ClN5O8Cu2, Mr = 744.06, Dc = 1.736 g/cm3, μ = 1.651 mm-1, F(000) = 754, the final R = 0.0421 and wR = 0.1163 for 4973 observed reflections with Ⅰ＞ 2σ(Ⅰ). In 1, tetra-copper chair-like clusters of [Cu4(OH)4(2,2'-bpy)4]4 are connected by bqdc ligands to form one-dimensional chains, which are further connected by hydrogen bonds to generate a two-dimensional supramolecular network .     

Synthesis and Crystal Structure of 2-p-Methyloxyphenyl- 3a-（2-phenyl-1,2,3-triazole-4-yl）-3,4-dihydro-1,2,4- oxa-diazolo[4,5-d][1,5] Benzothiazepine

The title compound2-p-methyloxyphenyl-3a-(2-phenyl-1,2,3-triazole-4-yl)-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine (C31H25N5O2S, Mr = 531.63) has been syn- thesized and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a = 10.888(2), b = 15.115(3), c = 16.702(3), α = 99.90(3), β = 95.21(3), γ = 100.41(3)o, V = 2642.1(9) nm3, Dc = 1.336 g/cm3, Z = 4, F(000) = 1112, μ = 0.162 mm-1 ,λ(MoKα) = 0.071073 nm, R = 0.0357 and wR = 0.1126 for 10620 observed reflections with I > 2σ(I). X-ray analysis reveals that the molecular backbone consists of a tricyclic system with the central seven- membered ring in a twisted boat-like conformation.