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1.
Tosha Barclay Wallace Cordes Fu-May Yang Shaw-Tao Lin 《Journal of chemical crystallography》1997,27(6):359-362
Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C6H4?CH2SCH2?C6H10?CH2SCH2?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP21/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)o, andZ=4. Thetrans isomer packs into the monoclinic space groupP21 witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation. 相似文献
2.
Gilbert J. Matare Kevin M. Kane Pamela J. Shapiro Ashwani Vij 《Journal of chemical crystallography》1998,28(10):731-734
cis-[(1,2-diphenyl-1,2-dicyclopentadienyl)ethanediyl]bis(tetrahydrofuran)calcium is prepared by reductively coupling phenylfulvene with activated calcium to produce cis and trans isomers which can be separately crystallized. The cis isomer crystallizes in the monoclinic space group P21/c. The cell parameters are: a = 9.7006(1), b = 18.9839(1), c = 14.2018(2) Å, = 91.263(1)°, V = 2614.70(5) Å3, D
calc = 1.252 mg/m3, and Z = 4. Spectroscopic and crystallographic data for the cis-isomer are presented and discussed. 相似文献
3.
Jason S. Overby Richard T. Woofter Arnold L. Rheingold Christopher D. Incarvito Roger D. Sommer 《Journal of chemical crystallography》2003,33(5-6):357-364
Three silyl-substituted fluorenes have been prepared by direct synthetic methods and structurally characterized by X-ray diffraction. The three silyl-substituted fluorenes studied were 9-trimethylsilylfluorene (1), 9-(tert-butyldimethyl)silylfluorene (2), and 2,7-di-tert-butyl-9-trimethylsilylfluorene (3). Complex 1 is orthorhombic, P212121, a = 6.2681(14) Å, b = 14.329(3) Å, c = 15.231(4) Å, Z = 4. Complex 2 is monoclinic, P21/c, a = 12.1953(10) Å, b = 6.9977(6) Å, c = 19.6536(17) Å, = 93.818(2), Z = 4. Complex 3 is monoclinic, P21/c, a = 11.9954(9) Å, b = 9.8978(7) Å, c = 18.5464(13) Å, = 92.456(2), Z = 4. The long carbon–silicon bonds effectively remove any significant intramolecular interactions as little distortion is exhibited around the sp
3-carbon atom and the fluorenyl backbone demonstrates near planarity. The bulky silicon substituents also prevent intermolecular interactions, as only a few close contacts less than 4.0 Å exist in all three solid state structures. 相似文献
4.
Jeffrey?E.?Fiscus Neil?Pschirer Rachael?E.?Hipp Andrea?M.?Goforth Craig?Chapman Sandra?Shotwell Ralph?C.?Layland Mark?D.?Smith Uwe?H.?F.?Bunz Hans-Conrad?zur?Loye
Using the new ligand, 2,2-bis-(4-pyridylethynyl)tolane we have synthesized five new coordination polymers: HgBr2[2,2-bis-(4-pyridylethynyl)tolane] (1), HgI2[2,2-bis-(4-pyridylethynyl)tolane] (2), Ni(acetylacetonate)2[2,2-bis-(4-pyridylethynyl)tolane] (3), Zn(acetylacetonate)2[2,2-bis-(4-pyridylethynyl)tolane] (4), and Cu(hexafluoro acetylacetonate)2[2,2-bis-(4-pyridylethynyl)tolane]CHCl3 (5). 2,2-Bis-(4-pyridyl ethynyl)tolane is a rigid ligand with a Z-shape that promotes the formation of zig-zag chains. Compounds 1– 5 were characterized by single crystal X-ray diffraction; and compounds 1– 3 were additionally characterized by IR, elemental analysis, and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic space group C2/c with a = 29.761(3) Å, b = 5.0531(5) Å, c = 16.7823(15) Å, = 104.090(2), V = 2447.9(4) Å3, Z = 4. Each mercury is bound to two tolane ligands and two bromine anions, resulting in a tetrahedral coordination environment. Compound 2 crystallizes in the monoclinic space group P2/c, with a = 20.3061(17) Å, b = 5.6303(5) Å, c = 24.5459(19) Å, = 110.338(2), V = 2631.4(4) Å3, Z = 4. Here also, each mercury is bound to two tolane ligands and two iodine anions in a tetrahedral coordination environment. The ligand orientation differs in compounds 1 and 2 being trans oriented in 1 and cis oriented in 2. Compound 3 crystallizes in the monoclinic space group P21/c with a = 14.5947(14) Å, b = 6.3082(6) Å, c = 18.3939(18) Å, = 112.112(2), V = 1568.9(3) Å3, Z = 2. Each nickel is bound to two tolane ligands and two bidentate AcAc anions, resulting in an octahedral coordination environment. Compound 4, which is isostructural with 3, also crystallizes in the monoclinic space group P21/c with a = 14.6990(9) Å, b = 6.2724(4) Å, c = 18.6433(11) Å, = 112.8610(10), V = 1583.86(17) Å3, Z = 2. Compound 5 crystallizes in the triclinic space group P-1 with a = 6.5487(4) Å, b = 11.6471(7) Å, c = 14.3225(9) Å, = 70.1360(10), = 89.3990(10), = 88.7680(10), V = 1027.18(11) Å3, Z = 1. Each copper in 5 is bound to two tolane ligands and two bidentate hfAcAc anions, resulting in an octahedral coordination environment identical to that found in 3 and 4. 相似文献
5.
Crystal structure of two brom containing aza-tetracyclic fused N-heterocycles including isoxazolidine ring compounds have been determined in single-crystal X-ray diffraction studies. The compound, C14H19BrN2O3, (1), and C12H15BrN2O3, (2), were obtained from a stereospecific[3+2] 1,3-cycloaddition of oxime based tandem nitrone generation reactions. The envelope conformation of the isoxazolidine rings are different, leading the substituents to be pseudoaxial in (1) and pseudoequatorial in (2). The stereochemistry of these fused compounds are exo- and endo-stereoisomer geometry contributed by exo and endo transition state of nitrone 1,3-dipolar cycloaddition reactions. The title compound (1) crystallizes in the monoclinic space group P2
1/n with a = 12.6221(5)Å, b = 7.5917(4) Å, c = 16.2350(9) Å, = 112.254(5)°, V = 1439.81(12) Å3, and D
calc = 1.583 Mg/m3 for Z = 4 and compound (2) crystallizes in the monoclinic space group P2
1/c with a = 11.6906(9) Å, b = 6.4255(7) Å, c = 17.2070(10) Å, = 109.264(5)°, V = 1220.2(2) Å3, and D
calc = 1.716 Mg/m3 for Z = 4. The antibacterial activity of both compounds were investigated for three Gram (+) and two Gram (–) bacteria by employing broth microdilution method and subsequently inhibitory activity against yeast-like fungi was also determined. 相似文献
6.
The structural determination by X-ray crystallography of the titled N-arylamine 4a, as well as AM1 calculations on a series of derivatives (4b–c, 5a–c), are reported. The compound 4a is monoclinic P21/c with a = 7.656(3), b = 23.655(5), c = 7.686(9) Å, = 112.59(6)°, V = 1285.2(2) Å3 and Z = 4. This structure has been used as a template for the building of some others derivatives used for AM1 calculations. The results show that the cyclization position on the aromatic rings, which can lead to two regioisomers, depends on the nature of the benzylic substituants. 相似文献
7.
X-ray crystal structure of cytochalasin D produced by Tubercularia sp., a novel endophytic fungus of Taxus mairei 总被引:2,自引:0,他引:2
Jian-Feng Wang Yao-Jian Huang Qing-Yan Xu Zhong-Hui Zheng Yu-Fen Zhao Wen-Jin Su 《Journal of chemical crystallography》2003,33(1):51-56
The crystal structure of cytochalasin D, which was isolated from Tubercularia sp., a novel endophytic fungus of Taxus mairei, and cocrystallized with dimethyl sulfoxide, is reported. The title compound crystallizes in the monoclinic space group P21, with a = 7.583(6) Å, b = 11.053(10) Å, c = 18.632(10) Å, = 95.79(6)°, V = 1553.6(3) Å3, Z = 2. The structure was solved by direct methods and refined by least-squares methods to a final R factor of 0.103 for 2937 independent reflections. 相似文献
8.
P. Staszewski J. Lipkowski J. Jaźwiński O. Staszewska L. Stefaniak Z. Urbańczyk-Lipkowska G.A. Webb 《Journal of chemical crystallography》1998,28(3):227-233
X-ray diffraction data are presented for the title mesoionic compound (I), its hydrochloride salt (II) and methylated derivative (III). The crystal of (I) is orthorombic, space group P212121, with cell dimensions: a = 5.857(1) Å, b = 12.494(2) Å, c = 16.328(3) Å, with four molecules per unit cell. The crystal of (II) is monoclinic, space group P21/n, with cell dimensions: a = 5.5720(10) Å, b = 21.5770(4) Å, c = 11.2330(2) Å, beta = 95.15(3)°, with four molecules per unit cell. The crystal of (III) is monoclinic, space group P21/n, with cell dimensions: a = 12.0886(5) Å, b = 7.9103(4), c = 104.29(1) Å, beta = 104.29(1)°, with four molecules per unit cell. Of particular interest is the fact that the C5–N6 bond appears to have a high double bond character in all three of the compounds studied. In addition, it is found that the exocyclic N-phenyl group changes from being in the cis conformation with respect to sulfur in compounds (I) and (III) to the trans conformation in the hydrochloric salt (II). 相似文献
9.
K. Simon K. Horváth D. Korbonits L. Párkányi 《Journal of chemical crystallography》1981,11(1-2):33-42
The previously reported IR study on 21 different 1-substituted 3-acylamino-2-pyrazolines assumed thecis configuration for the amide groups. In order to establish the configuration, X-ray structure determinations of two model compounds (1-phenyl-3-benzoylaminopyrazoline, monoclinic,a = 5.218,b = 8.830,c = 14.372 Å, = 90.7 °,Z = 2, P2
1; 1-benzyl-3-acetaminopyrazoline, monoclinic,a = 9.529,b = 13.679,c = 18.112 Å, = 96.7 °,Z = 8,P21/n) were performed. Both structures were solved by direct methods, and refined to a finalR = 0.075 for 710 andR = 0.122 for 2140 observed reflections. The configurations of the amide groups were found to betrans. 相似文献
10.
Four new complexes of (pn) the titled ligand have been prepared and characterized: (CO)3Mn(pn)Br, 1; (CO)3Mn(pn)N3, 2; the triazalato (tz) complex, (CO)3Mn(pn)(tz), 3 and [(CO)4Mn(pn)]BF4, 4. Crystal structures for the first three of these were determined. Crystal data for 1, monoclinic crystal system, space group = C2, a = 17.8587(6) Å, b = 7.9611(3) Å, c = 14.2349(4) Å, = 90.281(1)°, V = 2023.82(12) Å3, Z = 4; for 2, monoclinic crystal system, space group = P21/c, a = 8.8933(14) Å, b = 13.844(2) Å, c = 16.361(3) Å, = 95.712(3)°, V = 2004.4(6) Å3, Z = 4; for 3, orthorhombic crystal system, space group = Pbca, a = 17.9097(4) Å, b = 13.1308(4) Å, c = 21.2838(6) Å, V = 5005.3(2) Å3, Z = 8. 相似文献
11.
R. K. Murmann Rainer Glaser Charles L. Barnes 《Journal of chemical crystallography》2005,35(4):317-325
The X-ray structures of solid nitroguanidine (ngoH):orthorhombic, Fdd2, a = 17.6181(14), b = 24.848(2), c = 3.5901(4) Å, V = 1571.7(3) Å3, Z = 16 and nitrosoguanidine (ngH); monoclinic, P 21/n, a = 3.64510(10), b = 11.746(2), c = 8.6483(14) Å, = 99.167(2), V = 365.55(9) Å3, Z = 4 have been determined utilizing single crystal X-ray diffraction methods. The results are compared with the most stable gaseous configurations derived from ab inito calculations. The lowest energy calculated configuration for the ligands and experimentally observed crystal structures are in excellent agreement. In the solid state, both the ngoH and ngH contain discrete molecules in their unit cells which are planar (within experimental error), in the diamine configurations and are structurally identical except for an oxygen atom. In solid ngH, two ligand molecules have four nitrogen atoms arranged in a plane such that they are suitable for coordination to a nickel ion (1.945, 2.064 Å), when it is at the 1/2, 1/2, 1/2 unit-cell position giving the observed complex. As far as we are aware, this is the first instance in which a ligand crystal structure is essentially the same, with minor distance, angle and torsion angle changes, as the complex it forms and suggests some potentially unique properties and applications for this material. 相似文献
12.
Enrique Meléndez Ilia Guzei Arnold L. Rheingold 《Journal of chemical crystallography》1999,29(4):399-402
The reaction of Ru(acac)3 in ethanol in the presence of zinc and trans-stilbene affords Ru(acac)2(EtO)(EtOH) complex, co-crystallized with a half-molecule of trans-stilbene as a by-product, 1. The complex crystallizes in the monoclinic space group P21/n with a = 12.288 (3), b = 28.420(6), c = 13.285 (3) Å, = 95.63(3)° and Z = 8. The complex exhibits hydrogen bonds between the two Ru(acac)2(EtO)(EtOH) molecules. 相似文献
13.
In the two title compounds, the 2-methyl-1,3-dioxoindan-2-yl and 4-(brom; ethoxy) phenyl groups aretrans with respect to one another. The phenyl ring and the azo group are not coplanar in the two molecules. The five-membered rings of the two compounds adopt an envelope conformation. The crystallographic parameters are as follows: 2-Methyl-2-(4-bromphenylazo)-1,3-indandione (I): monoclinic, P21/a witha=8.098(2),b=14.442(2),c=12.554(1)Å, =100.55(2)o, andD
calc=1.58 g cm–3 forZ=4; 2-methyl-2-(4-ethoxyphenylazo)-1, 3-indandione (II): monoclinic, P21/a witha=8.258(2),b=14.449(1),c=13.559(2)Å, =101.19(1)o, andD
calc=1.29 g cm–3 forZ=4. 相似文献
14.
Jerry P. Jasinski Heidi E. Exel Alfonso Castiñeiras Elena Bermejo Heloisa Beraldo Douglas X. West 《Journal of chemical crystallography》2003,33(1):11-18
The crystal and molecular structure of copper(II) complexes of benzil bis(3-piperidylthiosemicarbazone), [Cu(Bnzpip)] and 1-phenylpropane-1,2-dione bis(3-piperidylthiosemicarbazone), [Cu(Pmpip)] have been determined. [Cu(Bnzpip)] is monoclinic, space group P21/n with a = 13.9375(10) Å, b = 11.6621(4) Å, c = 16.4710(10) Å, = 100.667(2)°, and V = 2630.9(3) Å3 with Z = 4, for d
calc = 1.399 g/cm3. [Cu(Pmpip)] is also monoclinic, space group P21/n with a = 11.292(6) Å, b = 10.219(5) Å, c = 20.292(6) Å, = 101.50(3)°, and V = 2295(2) Å3 with Z = 4, for d
calc = 1.525 g/cm3. Both complexes involve N2S2 coordination, are relatively planar except for the phenyl rings and have similar bond distances and angles to copper(II) complexes of other 3-piperidylthiosemicarbazones. 相似文献
15.
4- and 5-nitro-2-benzoylbenzoic acid 总被引:2,自引:0,他引:2
The structures of two isomeric nitro 2-benzoylbenzoic acids have been determined. 4-Nitro-2-benzoylbenzoic acid, C14H9NO5, monoclinic, P21/c, a = 9.455(5), b = 6.632(2), c = 21.333(7)Å, = 107.96(3)°, Z = 4, V = 1270.6(9)Å3, 5-nitro-2-benzoylbenzoic acid, C14H9NO5, monoclinic, P21/c, a = 10.201(6), b = 8.515(4), c = 14.573(7)Å, = 101.35(4)°, Z = 4, V = 1241.1(11)Å3. Both carboxylic acids form the usual H-bonded dimers across crystallographic centers of inversion. The nitro groups are essentially in the ring planes, and the interplanar angle between the mean planes described by the atoms of the benzoyl substituents and those of the benzoic acid aryl rings are 69(1)° and 84(1)°, respectively. The lower cell volume, higher density, and lower solubility in ethyl ethanoate correlates with the greater packing efficiency in 5-nitro-2-benzoylbenzoic acid. 相似文献
16.
The structures of anionic pyridine-2,6-dicarboxylato (pdc2–) complexes of cobalt, nickel, and copper have been studied. The stoichiometries and structures are very much dependent on whether KOH, Et4NOH, or NaOH is used in the synthesis to deprotonate the H2pdc ligand. Crystallographic results are: (1) K2[Co(pdc)2] · 7H2O, orthorhombic, Pnna, Z = 4, a = 20.637(2)Å, b = 13.480(1)Å, c = 8.200(1)Å (2) K2[Ni(pdc)2] · 7H2O, orthorhombic, Pnna, Z = 4, a = 20.648(1)Å, b = 13.375(1)Å, c = 8.2393(8)Å (3) [Co2(H2O)5(pdc)2] · 2H2O, monoclinic, P21/c, Z = 4, a = 8.3880(6)Å, b = 27.384(2)Å, c = 9.6110(8)Å, = 98.271(6)° (4) [Ni(Hpdc)2] · 3H2O, monoclinic, P21/c, Z = 4, a = 13.679(1)Å, b = 10.0450(9)Å, c = 13.767(2)Å, = 115.184(7)° (5) Na6[Co(H2O)6][Co(pdc)2]4 · 28H2O, monoclinic, P21/n, Z = 2, a = 13.363(1)Å, b = 8.437(1)Å, c = 40.689(3)Å, = 91.288(5)° (6) Na[Ni(Hpdc)(pdc)] · 11.5H2O, monoclinic, C2/m, Z = 4, a = 15.200(2)Å, b = 22.299(2)Å, c = 8.3596(7)Å, = 118.894(7)° (7) Na[Cu(Hpdc)(pdc)] · 3H2O, monoclinic, P21/n, Z = 4, a = 9.516(4)Å, b = 14.917(6)Å, c = 12.247(5)Å, = 92.00(5)°. The potassium and sodium complexes have extensive K+—H2O and Na+—H2O networks. The fact the Et4N+ ion does not appear in any of the complexes is likely due to the fact that it is incapable of forming the intricate cation—water and hydrogen-bonding networks observed in all of the other structures. 相似文献
17.
Krzysztof Burak Zbigniew Ciunik Tadeusz Głowiak 《Journal of chemical crystallography》1994,24(8):503-506
The structures of racemic 2-hydroxy-4-hydroxyiminopinan-3-one (1) and 3-hydroxyimino-cis-pinan-4-one monohydrate (2) have been determined by X-ray diffraction. The crystals of1 are monoclinic:P21/c, a=7.838(2),b=10.776(3),c=12.025(3) Å, =105.09(1)°,Z=4, room temp.; the crystals of2 are orthorhombic;P212121,a=8.181(3),b=9.250(3),c=14.085(6)Å,Z=4, T=80K. Both structures were solved by direct methods, and refined toR=0.037 for 1920 reflections (1) and 0.032 for 1776 reflections (2). The absolute configuration of2 was not established. The hydroxyimine groups in both crystals and water molecules in2 participate in the network O–H...O of hydrogen bonds. 相似文献
18.
G. C. Das M. B. Hursthouse K. M. A. Malik M. M. Rahman M. T. Rahman T. Olsson 《Journal of chemical crystallography》1994,24(8):511-515
1,3,5-triphenyl-1,5-pentanedione, C23H20O2, has been prepared and characterized by spectroscopic methods and single crystal X-ray analysis. Crystals are monoclinic, space groupP21/n, a=28.124(4),b=5.997(1),c=10.434(1)Å, -98.42(1)Å,Z=4. The structure has been refined to a finalR-value of 0.040 for 1625 reflections withF
o>3(F
o). The compound contains the two carbonyl groups in a mutuallycis arrangement. 相似文献
19.
The crystal structure of trispotassium [cis-trioxo(nitrilotriacetato)molybdate (VI)] monohydrate, C6H8K3MoNO10, has been determined. The crystals are monoclinic, space groupP21/c,a = 9.700(4),b = 19.628(6),c = 7.608(2) Å, = 110.58(4) ° andZ = 4. X-ray data were collected by counter methods using MoK. radiation, and least-squares refinement led toR = 0.055 for the 2234 independent reflections for which ¦F
0¦2 > (¦F
0¦2). The anion contains acis-trioxo metal system, while the ligand coordinates as a tridentate through its nitrogen atom and two of the three carboxylate oxygen atoms, the Mo atom being in a distorted octahedral environment. The two glycinato rings involved in the coordination are mutuallycis. The mean Mo-O (terminal) bond length is 1.74 Å and the lengths of the metal-ligand bonds are Mo-O 2.18, 2,25 Å; Mo-N 2.39 Å. 相似文献
20.
The titled covalent tetrafluoroborato dppfe complex was prepared by treating the precursor hydride, (CO)3(dppfe)MnH, with tetrafluoroboric acid. Similar treatment of analogous hydrido complexes with other chelating phosphines always gave ionic tetrafluoroborates, presumably via similar intermediate FBF3 covalent complexes, which however could not be isolated. Crystal structures for the covalent complex (CO)3(dppfe)MnFBF3.3/2CH2Cl2, 3, and the ionic complex [(CO)4(dppfe)Mn]BF4.CH2Cl2, 4, were determined. Crystal data for 3, monoclinic crystal system, space group = P21/n, a = 11.458(2) Å, b = 19.348(3) Å, c = 17.810(3) Å, = 104.410(4), V = 3823.9(12) Å3, Z = 4; for 4, monoclinic crystal system, space group = P21/n, a = 15.6521(2) Å, b = 14.3107(4) Å, c = 17.0933(5) Å, = 95.075(1), V = 3813.8(2) Å3, Z = 4. 相似文献