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1.
Gottfried Schill Claus Ulrich Priester Udo Frank Windhvel Hans Fritz 《Helvetica chimica acta》1986,69(2):438-441
A New Synthesis of the Vinblastine Derivatives 20′-Deethyl-20-deoxyvinblastine and 20′-Deethyl-20′-deoxy-C′-homovinblastine A new synthesis of vinblastine derivatives is described. In the key step, the chloroindolenine derivative 14 was reacted with vindoline ( 2 ) to give, after cyclization, stereospecifically 17/I and 20′-deethyl-20′-deoxyvinblastine ( 17/II ). In an analogous manner, the epimeric C′-homovinblastine derivatives 21/I-21/IV were synthesized. 相似文献
2.
Hyun‐Chul Kim Ja‐Min Gu Seong Huh Chul‐Hyun Yo Youngmee Kim 《Acta Crystallographica. Section C, Structural Chemistry》2015,71(10):929-935
Two new one‐dimensional CuII coordination polymers (CPs) containing the C2h‐symmetric terphenyl‐based dicarboxylate linker 1,1′:4′,1′′‐terphenyl‐3,3′‐dicarboxylate (3,3′‐TPDC), namely catena‐poly[[bis(dimethylamine‐κN)copper(II)]‐μ‐1,1′:4′,1′′‐terphenyl‐3,3′‐dicarboxylato‐κ4O,O′:O′′:O′′′] monohydrate], {[Cu(C20H12O4)(C2H7N)2]·H2O}n, (I), and catena‐poly[[aquabis(dimethylamine‐κN)copper(II)]‐μ‐1,1′:4′,1′′‐terphenyl‐3,3′‐dicarboxylato‐κ2O3:O3′] monohydrate], {[Cu(C20H12O4)(C2H7N)2(H2O)]·H2O}n, (II), were both obtained from two different methods of preparation: one reaction was performed in the presence of 1,4‐diazabicyclo[2.2.2]octane (DABCO) as a potential pillar ligand and the other was carried out in the absence of the DABCO pillar. Both reactions afforded crystals of different colours, i.e. violet plates for (I) and blue needles for (II), both of which were analysed by X‐ray crystallography. The 3,3′‐TPDC bridging ligands coordinate the CuII ions in asymmetric chelating modes in (I) and in monodenate binding modes in (II), forming one‐dimensional chains in each case. Both coordination polymers contain two coordinated dimethylamine ligands in mutually trans positions, and there is an additional aqua ligand in (II). The solvent water molecules are involved in hydrogen bonds between the one‐dimensional coordination polymer chains, forming a two‐dimensional network in (I) and a three‐dimensional network in (II). 相似文献
3.
W. Mark Barnett Russell G. Baughman Paula M. Secondo Charles J. Hermansen 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(9):o565-o567
The crystal structures of the title compounds, alternatively called 2,2′‐(2,2′‐biimidazole‐1,1′‐diyl)diacetohydrazide monohydrate, C10H14N8O2·H2O, (I), and 3,3′‐(2,2′‐biimidazole‐1,1′‐diyl)dipropionohydrazide, C12H18N8O2, (II), respectively, have been determined. The molecules consist of half‐molecule asymmetric units related by a twofold rotation in (I) and by a center of inversion in (II). The imidazole rings of both molecules crystallize in a nearly coplanar fashion [dihedral angles of 5.91 (3) and 0.0 (1)° for (I) and (II), respectively]. Both planar hydrazinocarbonylalkyl substituents are essentially planar and assume the E orientation. 相似文献
4.
Ivn Brito Aldo Mundaca Alejandro Crdenas Matías Lpez‐Rodríguez 《Acta Crystallographica. Section C, Structural Chemistry》2008,64(3):o117-o118
In the title compound, C10H6N4O4S2, (I), the molecule has a centre of inversion. The structure is a positional isomer of 5,5′‐dinitro‐2,2′‐dithiodipyridine [Brito, Mundaca, Cárdenas, López‐Rodríguez & Vargas (2007). Acta Cryst. E 63 , o3351–o3352], (II). The 3‐nitropyridine fragment of (I) shows excellent agreement with the bonding geometries of (II). The most obvious differences between them are in the S—S bond length [2.1167 (12) Å in (I) and 2.0719 (11) Å in (II)], and in the C—Cipso—Nring [119.8 (2)° in (I) and 123.9 (3)° in (II)] and S—C—C [122.62 (18)° in (I) and 116.0 (2)° in (II)] angles. The crystal structure of (I) has an intramolecular C—H...O interaction, with an H...O distance of 2.40 (3) Å, whereas this kind of interaction is not evident in (II). The molecules of (I) are linked into centrosymmetric R44(30) motifs by a C—H...O interaction. There are no aromatic π–π stacking and no C—H...π(arene) interactions. Compound (I) can be used as a nucleophilic tecton in self‐assembly reactions with metal centres of varying lability. 相似文献
5.
Oleg Stenzel Matthias W. Esterhuysen Helgard G. Raubenheimer 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(9):1056-1059
The crystal and molecular structures of bis(η5‐2,4,7‐trimethylindenyl)cobalt(II), [Co(C12H13)2], (I), and rac‐2,2′,4,4′,7,7′‐hexamethyl‐1,1′‐biindene, C24H26, (II), are reported. In the crystal structure of (I), the Co atom lies on an inversion centre and the structure represents the first example of a bis(indenyl)cobalt complex exhibiting an eclipsed indenyl conformation. The (1R,1′R) and (1S,1′S) enantiomers of the three possible stereoisomers of (II), which form as by‐products in the synthesis of (I), cocrystallize in the monoclinic space group P21/c. In the unit cell of (II), alternating (1R,1′R) and (1S,1′S) enantiomers pack in non‐bonded rows along the a axis, with the planes of the indenyl groups parallel to each other and separated by 3.62 and 3.69 Å. 相似文献
6.
Zhong Yu Atsuhiro Nabei Takafumi Izumi Takashi Okubo Takayoshi Kuroda‐Sowa 《Acta Crystallographica. Section C, Structural Chemistry》2008,64(5):m209-m212
4′‐Cyanophenyl‐2,2′:6′,2′′‐terpyridine (cptpy) was employed as an N,N′,N′′‐tridentate ligand to synthesize the compounds bis[4′‐(4‐cyanophenyl)‐2,2′:6′,2′′‐terpyridine]cobalt(II) bis(tetrafluoridoborate) nitromethane solvate, [CoII(C22H14N4)2](BF4)2·CH3NO2, (I), and bis[4′‐(4‐cyanophenyl)‐2,2′:6′,2′′‐terpyridine]cobalt(III) tris(tetrafluoridoborate) nitromethane sesquisolvate, [CoIII(C22H14N4)2](BF4)3·1.5CH3NO2, (II). In both complexes, the cobalt ions occupy a distorted octahedral geometry with two cptpy ligands in a meridional configuration. A greater distortion from octahedral geometry is observed in (I), which indicates a different steric consequence of the constrained ligand bite on the CoII and CoIII ions. The crystal structure of (I) features an interlocked sheet motif, which differs from the one‐dimensional chain packing style present in (II). The lower dimensionality in (II) can be explained by the disturbance caused by the larger number of anions and solvent molecules involved in the crystal structure of (II). All atoms in (I) are on general positions, and the F atoms of one BF4− anion are disordered. In (II), one B atom is on an inversion center, necessitating disorder of the four attached F atoms, another B atom is on a twofold axis with ordered F atoms, and the C and N atoms of one nitromethane solvent molecule are on a twofold axis, causing disorder of the methyl H atoms. This relatively uncommon study of analogous CoII and CoIII complexes provides a better understanding of the effects of different oxidation states on coordination geometry and crystal packing. 相似文献
7.
S. Renganayaki E. Subramanian S. Shanmuga Sundara Raj Hoong‐Kun Fun 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(3):349-350
The aromatic ring of the cinnamic moiety in N‐benzyl‐2′‐iodocinnamanilide, C22H18INO, (I), and N‐benzyl‐2′‐iodo‐4′‐methyl‐2‐phenylcinnamanilide, C29H24INO, (II), makes a dihedral angle with the iodophenyl ring of 72.1 (2) and 81.0 (2)° in (I) and (II), respectively. In (I), molecules exist as discrete components, while in (II), they form infinite chains along the b axis, through I?O non‐bonded interactions. 相似文献
8.
Antony Bulanov Igor N. Shcherbakov Leonid D. Popov E. Y. Shasheva P. A. Belikov Zoya A. Starikova 《Acta Crystallographica. Section C, Structural Chemistry》2011,67(3):o85-o88
The structures of new oxaindane spiropyrans derived from 7‐hydroxy‐3′,3′‐dimethyl‐3′H‐spiro[chromene‐2,1′‐isobenzofuran]‐8‐carbaldehyde (SP1), namely N‐benzyl‐2‐[(7‐hydroxy‐3′,3′‐dimethyl‐3′H‐spiro[chromene‐2,1′‐isobenzofuran]‐8‐yl)methylidene]hydrazinecarbothioamide, C27H25N3O3S, (I), at 120 (2) K, and N′‐[(7‐hydroxy‐3′,3′‐dimethyl‐3′H‐spiro[chromene‐2,1′‐isobenzofuran]‐8‐yl)methylidene]‐4‐methylbenzohydrazide acetone monosolvate, C27H24N2O4·C3H6O, (II), at 100 (2) K, are reported. The photochromically active Cspiro—O bond length in (I) is close to that in the parent compound (SP1), and in (II) it is shorter. In (I), centrosymmetric pairs of molecules are bound by two equivalent N—H...S hydrogen bonds, forming an eight‐membered ring with two donors and two acceptors. 相似文献
9.
The preparation of 1′-and 3′-amino-5′,6′,7′,8′-tetrahydro-2′-acetonaphthones (IIIa and IIIb) is described, by reduction of the low temperature nitration products of 5′,6′,7′,8′-tetrahydro-2′-acetonaphtone (I). The structures of the nitro isomers (IIa and IIb), and the reduction products, IIIa and IIIb, were elucidated spectroscopically. By known reactions, a series of new heterocyclic compounds prepared from the o-aminoketones, IIIa and IIIb, resulted in two series of new heterocyclic compounds. 相似文献
10.
Vibrational Spectra of Complexes of Gold Trichloride with 2,2′-Dipyridne and 4,4′-Dipyridine, Dipyridine and 4,4′-Dipyridine By reaction of Au2Cl6 with 2,2′-Dipyridine and 4,4′-Dipyridine, respectively, the complexes [AuCl2(2,2′-Dipy)][AuCl4] (I) and [AuCl2(4,4′-Dipy)]Cl (II) are obtained. IR and Raman spectra show that (I) has a complex chelate structure, whereas (II) is polymeric with cis-configuration of the ligands. 相似文献
11.
Jian Lin Wenxiang Chai Li Song Laishun Qin Kangying Shu 《Acta Crystallographica. Section C, Structural Chemistry》2009,65(12):o621-o623
In the course of our synthesis of hybrid photochromic compounds, the unexpected new organic photochromic title compound, C29H33N3O2, (I), was obtained. It is a derivative of the parent spirooxazine 1,3,3‐trimethyl‐6′‐(piperidin‐1‐yl)spiro[indoline‐2,3′‐3′H‐naphtho[2,1‐b][1,4]oxazine], (II). The 2′‐ethoxy group gives (I) different photochromic properties from its parent spirooxazine (II). 相似文献
12.
Katarzyna
lepokura Tadeusz Lis Magorzata Bogucka Joanna Lutomska Adam Kraszewski Krzysztof Sierosawski 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(7):o405-o409
The crystal structures of triethylammonium adenosine cyclic 2′,3′‐phosphate {systematic name: triethylammonium 4‐(6‐aminopurin‐9‐yl)‐6‐hydroxymethyl‐2‐oxido‐2‐oxoperhydrofurano[3,4‐c][1,3,2]dioxaphosphole}, Et3NH(2′,3′‐cAMP) or C6H16N+·C10H11N5O6P−, (I), and guanosine cyclic 2′,3′‐phosphate monohydrate {systematic name: triethylammonium 6‐hydroxymethyl‐2‐oxido‐2‐oxo‐4‐(6‐oxo‐1,6‐dihydropurin‐9‐yl)perhydrofurano[3,4‐c][1,3,2]dioxaphosphole monohydrate}, [Et3NH(2′,3′‐cGMP)]·H2O or C6H16N+·C10H11N5O7P−·H2O, (II), reveal different nucleobase orientations, viz. anti in (I) and syn in (II). These are stabilized by different inter‐ and intramolecular hydrogen bonds. The structures also exhibit different ribose ring puckering [4E in (I) and 3T2 in (II)] and slightly different 1,3,2‐dioxaphospholane ring conformations, viz. envelope in (I) and puckered in (II). Infinite ribbons of 2′,3′‐cAMP− and helical chains of 2′,3′‐cGMP− ions, both formed by O—H⋯O, N—H⋯X and C—H⋯X (X = O or N) hydrogen‐bond contacts, characterize (I) and (II), respectively. 相似文献
13.
Susanne Stockmann Jocelyn Bruce Jorn Miller Klaus R. Koch 《Acta Crystallographica. Section C, Structural Chemistry》2008,64(3):o166-o170
In the structures of 3,3,3′,3′‐tetraethyl‐1,1′‐(propane‐1,3‐diyldicarbonyl)bis(thiourea), C15H28N4O2S2, (I), 3,3,3′,3′‐tetraethyl‐1,1′‐(butane‐1,4‐diyldicarbonyl)bis(thiourea), C16H30N4O2S2, (II), and 3,3,3′,3′‐tetrabutyl‐1,1′‐(hexane‐1,6‐diyldicarbonyl)bis(thiourea), C26H50N4O2S2, (III), compound (I) displays resonance‐assisted hydrogen bonding, (II) exhibits an inversion centre, and both (II) and (III) are characterized by intermolecular hydrogen bonds between the carbonyl O atoms and thioamide H atoms, leading to chains of hydrogen‐bonded molecules throughout the structures. The accurate structural data for these molecules is expected to assist in molecular modelling and other studies currently in progress. 相似文献
14.
Thomas M. Gdda Allison K. Nelson William P. Weber 《Journal of polymer science. Part A, Polymer chemistry》2004,42(20):5235-5243
Anionic and cationic ring‐opening polymerizations of two novel cyclotrisiloxanes, tetramethyl‐1‐(3′‐trifluoromethylphenyl)‐1‐phenylcyclotrisiloxane ( I ) and tetramethyl‐1‐[3′,5′‐bis(trifluoromethyl)phenyl]‐1‐phenylcyclotrisiloxane ( II ), are reported. Anionic ring‐opening polymerization of I or II leads to copolymers with highly regular microstructures. Copolymers obtained by cationic polymerizations of I or II , initiated by triflic acid, have less regular microstructures characteristic of chemoselective polymerization processes. The composition and microstructure of copolymers have been characterized by 1H and 29Si‐NMR, the molecular weight distributions by GPC, and the thermal properties by DSC and TGA. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 5235–5243, 2004 相似文献
15.
Jan W. Bats Aleksandra
ivkovi Jrg Parsch Joachim W. Engels 《Acta Crystallographica. Section C, Structural Chemistry》2014,70(4):400-404
Crystal structures are reported for three fluoro‐ or chloro‐substituted 1′‐deoxy‐1′‐phenyl‐β‐D‐ribofuranoses, namely 1′‐deoxy‐1′‐(2,4,5‐trifluorophenyl)‐β‐D‐ribofuranose, C11H11F3O4, (I), 1′‐deoxy‐1′‐(2,4,6‐trifluorophenyl)‐β‐D‐ribofuranose, C11H11F3O4, (II), and 1′‐(4‐chlorophenyl)‐1′‐deoxy‐β‐D‐ribofuranose, C11H13ClO4, (III). The five‐membered furanose ring of the three compounds has a conformation between a C2′‐endo,C3′‐exo twist and a C2′‐endo envelope. The ribofuranose groups of (I) and (III) are connected by intermolecular O—H...O hydrogen bonds to six symmetry‐related molecules to form double layers, while the ribofuranose group of (II) is connected by O—H...O hydrogen bonds to four symmetry‐related molecules to form single layers. The O...O contact distance of the O—H...O hydrogen bonds ranges from 2.7172 (15) to 2.8895 (19) Å. Neighbouring double layers of (I) are connected by a very weak intermolecular C—F...π contact. The layers of (II) are connected by one C—H...O and two C—H...F contacts, while the double layers of (III) are connected by a C—H...Cl contact. The conformations of the molecules are compared with those of seven related molecules. The orientation of the benzene ring is coplanar with the H—C1′ bond or bisecting the H—C1′—C2′ angle, or intermediate between these positions. The orientation of the benzene ring is independent of the substitution pattern of the ring and depends mainly on crystal‐packing effects. 相似文献
16.
Bernardo Masci Stefano Levi Mortera Luca Seralessandri Pierre Thury 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(2):o107-o109
Two related compounds containing p‐tert‐butyl‐o‐methylene‐linked phenol or phenol‐derived subunits are described, namely 5,5′‐di‐tert‐butyl‐2,2′‐dihydroxy‐3,3′‐methylenedibenzaldehyde, C23H28O4, (I), and 6,6′‐di‐tert‐butyl‐8,8′‐methylenebis(spiro[4H‐1,3‐benzodioxin‐2,1′‐cyclohexane]), C35H48O4, (II). Both compounds adopt a `butterfly' shape, with the two phenol or phenol‐derived O atoms in distal positions. Phenol and aldehyde groups in (I) are involved in intramolecular hydrogen bonds and the two dioxin rings in (II) are in distorted half‐chair conformations. 相似文献
17.
Vijay Mahadevan Iyer Helen Stoeckli‐Evans Anthony D'Alo Luisa De Cola Peter Belser 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(4):o259-o261
Structure analyses of 4,4′‐bis(4‐hydroxybutyl)‐2,2′‐bipyridine, C18H24N2O2, (I), and 4,4′‐bis(4‐bromobutyl)‐2,2′‐bipyridine, C18H22Br2N2, (II), reveal intermolecular hydrogen bonding in both compounds. For (I), O—H·N intermolecular hydrogen bonding leads to the formation of an infinite two‐dimensional polymer, and π stacking interactions are also observed. For (II), C—H·N intermolecular hydrogen bonding leads to the formation of a zigzag polymer. The two compounds crystallize in different crystal systems, but both molecules possess Ci symmetry, with one half molecule in the asymmetric unit. 相似文献
18.
Bai-Chuan Pan Zum-Yao Weng Zhi-Hao Chen Elizabeth C. Rowe Shih-Hsi Chu 《Journal of heterocyclic chemistry》1990,27(6):1569-1574
5-Benzyl and 5-benzyloxybenzyl-substituted 3′-azido-2′,3′-dideoxyuridine, ( 8a and 8b ), 3′-halogeno-2′,3′-dideoxyuridine, 9a, 9b, 10a, 10b, 11a and 11b , and 2′,3′-dideoxyuridine, 12a and 12b , of Scheme I were synthesized as potential anti AIDS agents. Synthesis of epimers of 8a and 8b , 5-benzyl- and 5-benzyloxybenzyl-1-(3′-azido-2′,3′-dideoxy-β-D-threo-pentafuranosyl)uracil, 15a and 15b , and 5-benzyl- and 5-benzyloxy-5′-azido-2′,5′-dideoxyuridine, 16a and 16b , shown in Scheme II, were also reported. 相似文献
19.
Pablo Romo Jairo Quiroga Justo Cobo Christopher Glidewell 《Acta Crystallographica. Section C, Structural Chemistry》2020,76(8):779-785
The synthesis and characterization of three new dispiro[indoline‐3,3′‐pyrrolizine‐1′,5′′‐thiazolidine] compounds are reported, together with the crystal structures of two of them. (3RS,1′SR,2′SR,7a′SR)‐2′‐(4‐Chlorophenyl)‐1‐hexyl‐2′′‐sulfanylidene‐5′,6′,7′,7a′‐tetrahydro‐2′H‐dispiro[indoline‐3,3′‐pyrrolizine‐1′,5′′‐thiazolidine]‐2,4′′‐dione, C28H30ClN3O2S2, (I), (3RS,1′SR,2′SR,7a′SR)‐2′‐(4‐chlorophenyl)‐1‐benzyl‐5‐methyl‐2′′‐sulfanylidene‐5′,6′,7′,7a′‐tetrahydro‐2′H‐dispiro[indoline‐3,3′‐pyrrolizine‐1′,5′′‐thiazolidine]‐2,4′′‐dione, C30H26ClN3O2S2, (II), and (3RS,1′SR,2′SR,7a′SR)‐2′‐(4‐chlorophenyl)‐5‐fluoro‐2′′‐sulfanylidene‐5′,6′,7′,7a′‐tetrahydro‐2′H‐dispiro[indoline‐3,3′‐pyrrolizine‐1′,5′′‐thiazolidine]‐2,4′′‐dione, C22H17ClFN3O2S2, (III), were each isolated as a single regioisomer using a one‐pot reaction involving l ‐proline, a substituted isatin and (Z)‐5‐(4‐chlorobenzylidene)‐2‐sulfanylidenethiazolidin‐4‐one [5‐(4‐chlorobenzylidene)rhodanine]. The compositions of (I)–(III) were established by elemental analysis, complemented by high‐resolution mass spectrometry in the case of (I); their constitutions, including the definition of the regiochemistry, were established using NMR spectroscopy, and the relative configurations at the four stereogenic centres were established using single‐crystal X‐ray structure analysis. A possible reaction mechanism for the formation of (I)–(III) is proposed, based on the detailed stereochemistry. The molecules of (I) are linked into simple chains by a single N—H…N hydrogen bond, those of (II) are linked into a chain of rings by a combination of N—H…O and C—H…S=C hydrogen bonds, and those of (III) are linked into sheets by a combination of N—H…N and N—H…S=C hydrogen bonds. 相似文献
20.
3′:5′‐Cyclic nucleotides play an outstanding role in signal transduction at the cellular level but, in spite of comprehensive knowledge of the biological role of cyclic nucleotides, their structures are not established fully. Two hydrated sodium salts of thymidine 3′:5′‐cyclic phosphate (cdTMP, C10H12N2O7P), namely sodium thymidine 3′:5′‐cyclic phosphate heptahydrate, Na+·C10H12N2O7P−·7H2O or Na(cdTMP)·7H2O, (I), and sodium thymidine 3′:5′‐cyclic phosphate 3.7‐hydrate, Na+·C10H12N2O7P−·3.7H2O or Na(cdTMP)·3.7H2O, (II), have been obtained in crystalline form and structurally characterized, revealing one nucleotide in the asymmetric unit of (I) and eight different nucleotides in (II). All the cyclic nucleotide anions adopt a similar conformation with regard to nucleobase orientation, sugar conformation and 1,3,2‐dioxaphosphorinane ring puckering. In (I), no direct inter‐nucleotide hydrogen bonds are present, and adjacent nucleotide anions interact via water‐mediated and Na+‐mediated contacts. In contrast, in (II), direct thymine–phosphate N—H...O inter‐nucleotide hydrogen bonds occur and these are assisted by numerous inter‐nucleotide C—H...O contacts, giving rise to the self‐assembly of cdTMP− anions into three different ribbons. Two of these three ribbons run in the same direction, while the third is antiparallel. 相似文献