共查询到20条相似文献,搜索用时 31 毫秒
1.
J. M. M. Smits P. T. Beurskens R. Plate H. C. J. Ottenheijm 《Journal of chemical crystallography》1986,16(6):989-997
The structure of the title compound, C18H23N3O4, was determined by X-rays.M
r
=344.40, triclinic, space groupP¯1,a=8.163(4),b=9.230(2),c=13.297(2) Å,=102.70(2),=103.58(3)°,=102.50(3)°,V=911.3 Å3,Z=2,D
c
=1.26 Mg m–3. CuK radiation (graphite crystal monochromator,=1.54178 Å),(CuK)=7.50 cm–1,T=290 K. Final conventionalR-factor=0.068,R
w
=0.079 for 1912 unique reflections and 295 variables. The structure was solved usingMultan andDirdif. The title compound is the first example of a 3,6-tetrasubstituted dioxopiperazine adopting a folded conformation, owing to a direct interaction between the dioxopiperazine ring and the aromatic side chain. 相似文献
2.
Gregory H. Robinson Mark F. Self Samuel A. Sangokoya William T. Pennington 《Journal of chemical crystallography》1988,18(3):285-291
Reaction of an excess of trimethylaluminum with bis(diphenylphosphino)-methane in heptane affords the crystalline complex [A1(CH3)3]2[(C6H5)2PCH2P(C6H5)2]. The title compound crystallizes in the triclinic space group P¯1 with unit cell parametersa=10.053(6),b=11.017(6),c=15.908(8) Å,=85.58(4),=71.80(4), =77.49(4)°,V=1634(1) Å3, andD
c=1.07 g cm–3 forZ=2. Least-squares refinement based on 2924 observed reflection with intensitiesI3I) in the range 2.00245.0° converged atR=0.050 (R
w=0.067). The Al-P distances are 2.585(2) and 2.521(2) Å, and the P-C-P angle is 121.4(2)°. 相似文献
3.
Marek L. Główka Zbigniew J. Kamiński Valerio Bertolasi Gastone Gilli 《Journal of chemical crystallography》1989,19(4):695-700
C12H12N2O6 crystallized from methanol in the monoclinic space group P21/c (Z=4) witha=13.333(4),b=10.154(3),c=9.597(2) Å and=102.37(2)°.M
r=280.24,V=1269.1(6) Å3,D
x=1.466 g cm–3,(Mo K)=0.71069 Å,=1.29 cm–1,T=295 K. The structure was solved by direct methods and refined by full-matrix least-squares to a finalR (R
w)=0.049 (0.057) for 916 observed reflections. The molecules are linked by strong N-HO(4) hydrogen bonds with NO distance of 2.995(4) Å. The infinite racemic chains run in [001] direction. 相似文献
4.
Dianne R. Bond Luigi R. Nassimbeni Fumio Toda 《Journal of chemical crystallography》1989,19(5):847-859
The structures of the 12 molecular complexes oftrans-9,10-dihydroxy-9,10-diphenyl-9,10-dihydroanthracene with 4-methylcyclohexanone (1) and with 2-methylcyclohexanone (2) have been determined by X-ray crystallography. The crystal data are as follows: Compound (1):P22/c,a=8.838(2) Å,b=8.92(1) Å,c=20.879(8)=Å,=98.67(2)°,V=1627(2) Å3,Z=2 andR=0.062 for 2201 unique MoK reflections; Compound (2):P¯1,a=8.917(3) Å,b=9.900(2) Å,c=11.250(4) Å,a=68.72(2)°,=64.39(3)°, =74.86(2)°,V=828.1(5) Å3,Z=1 andR=0.098 for 2563 unique reflections. Both inclusion compounds exhibit O-HO=C hydrogen bonding interactions. The thermal properties of these compounds have been characterized by DTA and TGA thermograms. 相似文献
5.
2(C12H26O3N3·C2H3O2)·C2H4O2·H2O,M
r
=350.44, triclinic, P1,a=5.576,b=12.574(3),c=14.946(2) Å, =107.80(2), =96.34(2), =89.89(2)°.B=991.04(6) Å3,Z=2,D
x
=1.201 g/cm3, (KCu)=1.5418, Å, =7.4 cm–1, room temperature.R=0.074 for 2645 observed reflections. In the unit cell there are two peptide molecules, three acetic acid molecules, two of them likely to be present as acetate anions, and one water molecule. Each peptide exists in zwitterionic form with the carboxylic group deprotonated, and with positive charges both in the amino terminal and -amino groups of lysine. The two peptide molecules have almost identical conformations. The dipeptide backbone is folded. 相似文献
6.
V. Ferretti P. Gilli V. Bertolasi G. Spalluto G. Gilli 《Journal of chemical crystallography》1993,23(3):195-201
(3(Z),4,6a,9a,9b)-(±)-3a,4,6a,7,8,9,9a,9b-octahydro-4,7,7, 9b-tetramethyl-3a-[3-(methoxymethyloxy)-3-methyl-1-butenyl]-5H-naphto[1,8-de]-1,3-dioxin-6-one (I), C22H36O5,M
r=378.51, monoclinic,P21/n,a=6.330(1),b=14.576(2),c=22.837(2)Å,=93.04(1)°,V=2104.1(2)Å3,Z=4,D
c=1.19 Mg/m3, (MoK)=0.71069Å,=0.8 cm–1,F(000)=832,T=298 K,R=0.054 for 1971 observed reflections; (7a,10a,10b,12)-(±)-7a,9, 10,10a,10b,11,12,12a-octahydro-2,2,10,10,10b,12a-hexamethyl-2H,8H-1-benzopyrano[4a,5,6,-de][1,3,2]-benzodioxin-11-one (II), C20H29O4,M
r=334.5, triclinic,P-1,a=10.595(2),b=12.152(1),c=8.073(1)Å,=106.53(1),=105.65(1), =66.29(1)°,V=897.9(2)Å3,Z=2,D
c=1.24 Mg/m3, (MoK)=0.71069Å,=0.8 cm–1,F(000)=362,T=298 K,R=0.046 for 2848 observed reflections; (7a,10a,10b,12, 12a)-(±)-7a,9,10,10a,10b,11,12,12a-octahydro-2,2,10,10,10b,12a-hexamethyl-2H,8H-1-benzopyrano[4a,5,6-de][1,3,2]-benzodioxin-11, 12-diol (III), C20H32O5 (two molecules in the asymmetric unit),M
r=352.2, triclinic,P-1,a=12.948(3),b=13.615(3),c=12.197(4)Å,=101.16(2),=111.88(2), =69.48(2)°,V=1863.8(9)Å3,Z=2,D
C=1.26 Mg/m3,(MoK)=0.71069 Å,=0.8 cm–1,F(000)=768,T=298 K,R=0.060 for 4570 observed reflections; 4-acetoxy-4-[[(4a,5,8a)-(±)-hexahydro-4a,6,6-trimethyl-4H-1,3-benzodioxin-4-one]-5-yl]butan-2-one (IV), C17H26O6,M
r=326.4, monoclinic,P21/c,a=10.495(2),b=12.050(2),c=14.216(2)Å,=108.51(1)°,V=1704.8(5)Å3,Z=4,D
c=1.27 Mg/m3,(MoK)=0.71069 Å,=0.9 cm–1,F(000)=704,T=298 K,R=0.049 for2455 observed reflections; (3a,4,5,6,6a,9a,9b)-(±)-4,5-epoxy-decahydro-3, 3a-dihydroxy-2-ethoxy-4,7,7,9b-tetramethyl-naphto-[1,8-bc]-pyran-6-ol-acetate (V), C20H32O7,M
r=383.5, monoclinic,C2/c,a=10.353(2),b=17.975(3),c=21.188(3)Å,=91.29(1)°,V=3942(1)Å3,Z=8,D
c=1.29 Mg/m3,(MoK)=0.71069 Å,=0.8 cm–1,F(000)=1664,T=298 K,R=0.051 for 2120 observed reflections. We report here the complete structures of four decalin derivatives (compoundsI, II, III, V) and one related compound (compoundIV) synthetized in order to find an efficient synthetic approach for the natural productforskolin. 相似文献
7.
S. Bamidele Sanni H. Behm Paul T. Beurskens E. Kayode Adesogan James I. Durodola 《Journal of chemical crystallography》1988,18(5):575-582
A new cytotoxic macrocyclic diterpenoid named Japodagrol, C20H28O4, has been isolated from the ornamental plantJatropha podagrica, family Euphorbiaceae, grown in Nigeria. The structure of the title compound, C20H28O4, was solved by X-ray analysis.M
r
=332.44, monoclinic space groupC2,a=23.285(4),b=6.5105(12),c=12.505(3) Å,=98.504(17),V=1874.8 Å3,Z=4,D
c
=1.178 Mg/m3. CuK radiation (graphite crystal monochromator, =1.54184 A), (CuK)=6.13 cm–1,F(000)=720,T=290 K. Final conventionalR factor=0.035,R
w
=0.038 for 3349 observed reflections. The structure was solved with the programDirdif. The 5-membered ring is closed to a half-chair form. The compound contains inter- and intramolecular hydrogen bonds. 相似文献
8.
V. Parthasarathi Paul T. Beurskens H. J. J. Behm S. Garcia-Granda M. Krishna Pillay 《Journal of chemical crystallography》1986,16(6):833-840
The structure of the the title compound, C30H29NO, was determined by X-rays.M
r
=419.57, triclinic, space groupP1,a=5.8922(12),b=8.5855(11),c=12.2216(20) Å,=78.145(12)°,=79.181(15)°, =76.108(14)°,V
c
=581.1(1) Å3,Z=1,D
x
=1.199 Mg m–3. CuK radiation (graphite crystal monochromator, =1.54184 Å),(CuK)=5.17 cm–1,T=290K. Final conventionalR-factor=0.039,R
w
=0.042 for 2795 observed reflections and 377 variables. The structure was solved usingMultan andDirdif. With a view to determining the conformational preference of the piperidine ring when it is highly sustituted with a bulky group like the phenyl group, the present X-ray investigation was undertaken. 相似文献
9.
Kaiyuan Yang Simon G. Bott Michael G. Richmond 《Journal of chemical crystallography》1995,25(5):263-266
The reaction betweencis-Ru(bpy)2Cl2 (where bpy=bipyridine) and the diphosphine ligand 1,1-bis(diphenylphosphino)ferrocene (dppf) in the presence of AgBF4 has led to the isolation of the title compound [Ag(dppf)Cl]2. [Ag(dppf)Cl]2 has been structurally characterized by X-ray diffraction analysis, which confirms the bridging mode adopted by the ancillary dppf ligand and the centrosymmetric nature of this molecule. Dimeric [Ag(dppf)Cl]2 crystallizes in the triclinic space group
,a=11.426(1) Å,b=11.509(1) Å,c=12.786(1) Å, =68.96(2)°, =70.66(2)°, =71.24(2)°,V=1441(1) Å3,Z=1,d
calc=1.608 g·cm–3;R=0.0445,R
w=0.0566 for 4486 observed reflections withl>3(l) 相似文献
10.
Laila H. Abdel-Rahman Luigi Pietro Battaglia Paolo Sgarabotto Mohamed R. Mahmoud 《Journal of chemical crystallography》1994,24(9):567-571
A series of ternary complexes of copper(II), cobalt(II) and zinc(II) with L-histidine, 1,10-phenanthroline, 2,2-dipyridyl or imidazole having perchlorate or acetate as counterions were synthesized and characterized by conventional methods and for [Cu(bipy)(L-hist)]ClO4·1.5H2O and X-ray crystal structure was determined. The crystals belong to the monoclinic space groupC2 witha=18.843(3),b=10.582(2),c=11.020(2), =115.20(10)°,Z=4,R=0.0535. The structure is consistent of [Cu(bipy)(L-hist)]+ cations, perchlorate ions and water molecules. The geometry around copper is trigonal bipyramidal with one N,N,O tridentate L-histidine molecule and one 2,2-dipyridyl ligand, the apical sites are occupied by the -amino nitrogen [Cu–N(71) 1.995(8)] and by N(11) of 2,2-dipyridyl [Cu–N(11) 1.983(7)], the equatorial plane is formed by the N(3) imidazole -nitrogen [Cu–N(3) 2.140(6)], O(82) carboxylic oxygen [Cu–O(82) 2.009(5)] and N(22) [Cu–N(22) 2.010(7)]. 相似文献
11.
J. M. M. Smits Paul T. Beurskens A. J. H. Klunder M. J. F. M. Crul 《Journal of chemical crystallography》1986,16(5):665-671
The structure of the title compound, C12H16O3, was determined by X-rays.M
r
=208.26, triclinic, space groupP¯1,a=7.802(2),b=8.449(2),c=9.069(1) Å,=90.79(1)°,=105.57(1)°, =106.07(1)°,Z=2,D
x
=1.26 Mg m–3; MoK radiation (graphite crystal monochromator, =0.71069 Å),(MoK)=0.96 cm–1,T=290 K. Final conventionalR-factor=0.046,R
w
=0.067 for 3009 observed reflections and 184 variables. The structure was solved using Patterson methods andDirdif, and the resulting all cis-endo configuration of the alcohol group on C(3) and the ethoxy group on C(5) shows that the stereochemistry of the metal-mediated addition reaction involved is solely determined by steric factors. 相似文献
12.
J. Gabriel Garcia Yen-Hsiang Liu Frank R. Fronczek 《Journal of chemical crystallography》1996,26(9):607-613
The crystal structures of two conjugated ene-yne derivatives of thiophene are described, 2,5-di-(trimethylsilylethynyl)-3,4-dibromothiophene (1), is triclinic P
witha=6.3281(4)Å,b=9.7421(6)Å,c=16.3669(9)Å; =80.516(5)°, =84.810(5)°, =74.072(5)°,Z=2,R=0.054; 2,3,4,5-tetra(trimethylsilylethynyl)thiophene (2), is monoclinic, P21/c with a=20.928(2)Å b=5.852(1)Å,c=23.907(2)Å; =100.245(6)°,Z=4,R=0.049. The ethynylic C atoms of both compounds lie near the thiophene plane, with deviations in the range 0.010(3)–0.455(4)Å. The phenyl groups of2 form a dihedral angle of 13.0(4)°. 相似文献
13.
A. K. Das S. K. Mazumdar V. Bertolasi A. Van Aerschot 《Journal of chemical crystallography》1993,23(6):455-458
The title compound, 1-(2,3-dideoxy-3-fluoro--d-erythro pentofuranos-1-yl)-5-chlorocytosine, crystallises in the orthorhombic space groupP212121 witha=5.142(1),b=14.177(2),c=15.721(2) Å,Z=4. The crystal structure was solved by the heavy atom method and refined by full-matrix least-squares method to a finalR value of 0.031 for 1629 unique observed reflections. The N-glycosidic torsion angle is –156.1(2)° and the sugar moiety is anti to the cytosine base. The sugar pucker is
2
3
T withP=178.2(1)° and=31(1)°. The atom 05 is in a +sc conformation with respect to the furanose ring. The molecular packing in the crystal is stabilized by N-HN, N-HO, O-HO hydrogen bonds and C-HO close contacts. 相似文献
14.
The spectroscopic and X-ray investigation of the N-(2-phenylethyl) amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid are reported. The1H NMR spectra for the title structure and for the N-(p-methoxybenzyl) amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid are given. The N-(2-phenylethyl)amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid, C16H23O4N, crustallizes in the monoclinic space groupP2
1/c witha=21.547(5),b=6.333(2),c=11.822(3) Å and =101.01(2)°. The dioxolane ring has a half-chair conformation with C2(O3)=2.4° and ||av=18.2°. The inconsiderable deviations from planarity of the six atoms of the amide group are caused mainly by twist around the C4–N1 bond and out-of-plane bending at the N1 atom ((C4–N1)=4°, XN =7°, Xc =0.4° ). The amide group plane is nearly coplanar with the phenyl ring. The molecules are connected by two intermolecular hydrogen bonds. 相似文献
15.
The crystal structure of [SnBu2(TNEE)2], (HTNEE=5-ethyl ester of 2-mercaptopyridine-5-carboxylic acid) has been determined by X-ray single crystal diffraction study. The crystal is triclinic, space groupP,a=10.042(1),b=18.421(2),c=7.979(1) Å, =98.7(1), =107.3(1), =87.7(1)o,V=1393(1) Å3, and Z=2 The tin center is coordinated to two butyl groups and to the nitrogen and the sulfur atoms of two ligand molecules in a very distorted trapezoidal bipyramid. 相似文献
16.
Lingqin Han Wen-Hua Sun Leyong Wang Honggen Wang Yong Cui 《Journal of chemical crystallography》2003,33(3):159-163
Bis(2,6-(2,6-diisoproylanil)diformyl-4-chloro-phenolate) nickel(II) was prepared by the reaction of 2,6-(2,6-diisoproylanil)diformyl-4-chloro-phenol with nickel chloride. The title complex crystallized in P21/c, with cell dimensions a = 9.962(2) Å, b = 12.087(3) Å, c = 24.445(6) Å, and = 97.032(5), giving a volume of 2921.4(13) Å3. The bis(2,6-(2,6-diisoproylanil)diformyl-4-chloro-phenolate) nickel(II) adapts an ideal parallelogram, in which the Ni atom is coordinated with two phenolic oxygen atoms [O(1), O(1A)] and two imino nitrogen atoms [N(1), N(1A)]. 相似文献
17.
J. M. M. Smits P. T. Beurskens R. Plate H. C. J. Ottenheijm 《Journal of chemical crystallography》1986,16(6):941-948
The structure of the title compound, C22H22N2O3, was determined by X-rays atT=290 K.M
r
=362.427, orthorombic, space groupPbca,a=11.666(4),b=15.691(1),c=20.931(1) Å,V=3831.4 Å3,Z=8,D
x
=1.257 Mgm–3. CuK radiation (graphite crystal monochromator, =1.54178 Å),(CuK)=6.42 cm–1. Final conventionalR-factor=0.050,R
w
=0.062 for 2552 observed reflections and 301 variables. The structure was solved usingMultan. 相似文献
18.
A. K. Das S. K. Mazumdar V. Bertolasi A. Van Aerschot 《Journal of chemical crystallography》1993,23(5):353-357
The title compound crystallizes in the orthorhombic space groupP212121 witha=5.084(1),b=14.322(3),c=16.065(2)Å,Z=4. The structure was solved by the heavy atom method and refined by full-matrix least-squares calculations to a finalR value of 0.033 for 1106 unique observed reflections. The N-glycosidic torsion anglex has a value of –153.7(4)°, in the anti-range. The sugar pucker is2T3 withP=175(1)° and=30(1)°. The C4-C5 conformation is + sc with =46.7(7)°. The structure is stabilized by N-HN, N-HO and O-HO hydrogen bonds and C-HO close contacts. 相似文献
19.
Charles R. Ojala William H. Ojala Doyle Britton 《Journal of chemical crystallography》1996,26(3):191-194
2-Nitroresorcinol is triclinic, space group P; at –100°Ca=7.083(2),b=7.696(2),c=6.607(2) Å, =74.61(2), =77.81(2), =68.64(2)°,V=320.8(2) Å3,D
x=1.606(1) g cm–3,Z=2. The two hydroxyl groups form symmetric intramolecular hydrogen bonds to the nitro group. The molecules pack in stacks held together by - interaction with adjacent molecules in a head-to-tail arrangement. 相似文献
20.
J. M. M. Smits P. T. Beurskens R. Plate H. C. J. Ottenheijm 《Journal of chemical crystallography》1986,16(6):957-966
The structure of the title compound, C18H20N2O5, was determined by X-rays atT=290 K.M
r
=344.366, monoclinic, space groupP21/c,a=13.7850(8),b=8.8951(7),c=15.1603(11) Å, =111.410(6)°,V
c
=1730.7 Å3,Z=4,D
x
=1.322 Mgm–3. Cu K radiation (graphite crystal monochromator, =1.54178 Å),(Cu K)=7.69 cm–1. Final conventionalR-factor=0.057,R
w
=0.076 for 2160 observed reflections and 271 variables. The structure was solved usingMultan. 相似文献