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1.
《Acta Crystallographica. Section C, Structural Chemistry》2017,73(11):917-922
The synthesis and crystal structure of the multidentate PPN ligand 2‐[bis(diisopropylphosphanyl)methyl]‐6‐methylpyridine (L ), C19H35NP2, are described. In the isostructural tetrahedral Fe and Co complexes of type LM Cl2 (M = Fe, Co), namely {2‐[bis(diisopropylphosphanyl)methyl]‐6‐methylpyridine‐κ2P ,N }dichloridoiron(II), [FeCl2(C19H35NP2)], and {2‐[bis(diisopropylphosphanyl)methyl]‐6‐methylpyridine‐κ2P ,N }dichloridocobalt(II), [CoCl2(C19H35NP2)], the ligand adopts a bidentate P ,N‐coordination, whereas in the case of the octahedral Mn complex {2‐[bis(diisopropylphosphanyl)methyl]‐6‐methylpyridine‐κ2P ,P ′}bromidotricarbonylmanganese(I), [MnBr(C19H35NP2)(CO)3], the ligand coordinates via both P atoms to the metal centre. 相似文献
2.
Highly Active,Low‐Valence Molybdenum‐ and Tungsten‐Amide Catalysts for Bifunctional Imine‐Hydrogenation Reactions
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Dr. Subrata Chakraborty Dr. Olivier Blacque Dr. Thomas Fox Prof. Heinz Berke 《化学:亚洲杂志》2014,9(1):328-337
The reactions of [M(NO)(CO)4(ClAlCl3)] (M=Mo, W) with (iPr2PCH2CH2)2NH, (PNHP) at 90 °C afforded [M(NO)(CO)(PNHP)Cl] complexes (M=Mo, 1a ; W, 1b ). The treatment of compound 1a with KOtBu as a base at room temperature yielded the alkoxide complex [Mo(NO)(CO)(PNHP)(OtBu)] ( 2a ). In contrast, with the amide base Na[N(SiMe3)2], the PNHP ligand moieties in compounds 1a and 1b could be deprotonated at room temperature, thereby inducing dehydrochlorination into amido complexes [M(NO)(CO)(PNP)] (M=Mo, 3a ; W, 3b ; PNP=(iPr2PCH2CH2)2N)). Compounds 3a and 3b have pseudo‐trigonal‐bipyramidal geometries, in which the amido nitrogen atom is in the equatorial plane. At room temperature, compounds 3a and 3b were capable of adding dihydrogen, with heterolytic splitting, thereby forming pairs of isomeric amine‐hydride complexes [Mo(NO)(CO)H(PNHP)] ( 4a(cis) and 4a(trans) ) and [W(NO)(CO)H(PNHP)] ( 4b(cis) and 4b(trans) ; cis and trans correspond to the position of the H and NO groups). H2 approaches the Mo/W?N bond in compounds 3a , 3b from either the CO‐ligand side or from the NO‐ligand side. Compounds 4a(cis) and 4a(trans) were only found to be stable under a H2 atmosphere and could not be isolated. At 140 °C and 60 bar H2, compounds 3a and 3b catalyzed the hydrogenation of imines, thereby showing maximum turnover frequencies (TOFs) of 2912 and 1120 h?1, respectively, for the hydrogenation of N‐(4 ‐ methoxybenzylidene)aniline. A Hammett plot for various para‐substituted imines revealed linear correlations with a negative slope of ?3.69 for para substitution on the benzylidene side and a positive slope of 0.68 for para substitution on the aniline side. Kinetics analysis revealed the initial rate of the hydrogenation reactions to be first order in c(cat.) and zeroth order in c(imine). Deuterium kinetic isotope effect (DKIE) experiments furnished a low kH/kD value (1.28), which supported a Noyori‐type metal–ligand bifunctional mechanism with H2 addition as the rate‐limiting step. 相似文献
3.
Cengiz Arici Filiz Ercan Raif Kurtaran Orhan Atakol 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(7):812-814
In the title compounds, {2,2′‐[2,2‐dimethyl‐1,3‐propanediylbis(nitrilomethylidyne)]diphenolato‐κ4N,N′,O,O′}nickel(II), [Ni(C19H20N2O2)], and {2,2′‐[2,2‐dimethyl‐1,3‐propanediylbis(nitrilomethylidyne)]diphenolato‐κ4N,N′,O,O′}copper(II), [Cu(C19H20N2O2)], the NiII and CuII atoms are coordinated by two iminic N and two phenolic O atoms of the N,N′‐bis(salicylidene)‐2,2‐dimethyl‐1,3‐propanediaminate (SALPD2?, C17H16N2O22?) ligand. The geometry of the coordination sphere is planar in the case of the NiII complex and distorted towards tetrahedral for the CuII complex. Both complexes have a cis configuration imposed by the chelate ligand. The dihedral angles between the N/Ni/O and N/Cu/O coordination planes are 17.20 (6) and 35.13 (7)°, respectively. 相似文献
4.
《Acta Crystallographica. Section C, Structural Chemistry》2017,73(9):674-681
Three photoluminescent complexes containing either ZnII or CdII have been synthesized and their structures determined. Bis[4‐amino‐3,5‐bis(pyridin‐2‐yl)‐1,2,4‐triazole‐κ2N 1,N 5]bis(dicyanamido‐κN 1)zinc(II), [Zn(C12H10N6)2(C2N3)2], (I), bis[4‐amino‐3,5‐bis(pyridin‐2‐yl)‐1,2,4‐triazole‐κ2N 1,N 5]bis(dicyanamido‐κN 1)cadmium(II), [Cd(C12H10N6)2(C2N3)2], (II), and bis[4‐amino‐3,5‐bis(pyridin‐2‐yl)‐1,2,4‐triazole‐κ2N 1,N 5]bis(tricyanomethanido‐κN 1)cadmium(II), [Cd(C12H10N6)2(C4N3)2], (III), all crystallize in the space group P , with the metal centres lying on centres of inversion, but neither analogues (I) and (II) nor CdII complexes (II) and (III) are isomorphous. A combination of N—H…N and C—H…N hydrogen bonds and π–π stacking interactions generates three‐dimensional framework structures in (I) and (II), and a sheet structure in (III). The photoluminescence spectra of (I)–(III) indicate that the energies of the π–π* transitions in the coordinated triazole ligand are modified by minor changes of the ligand geometry associated with coordination to the metal centres. 相似文献
5.
Kai‐Long Zhong 《Acta Crystallographica. Section C, Structural Chemistry》2012,68(9):m259-m264
The title compounds, tris(1,10‐phenanthroline‐κ2N,N′)iron(II) bis(2,4,5‐tricarboxybenzoate) monohydrate, [Fe(C12H8N2)3](C10H5O8)2·H2O, (I), and tris(2,2′‐bipyridine‐κ2N,N′)iron(II) 2,5‐dicarboxybenzene‐1,4‐dicarboxylate–benzene‐1,2,4,5‐tetracarboxylic acid–water (1/1/2), [Fe(C10H8N2)3](C10H4O8)·C10H6O8·2H2O, (II), were obtained during an attempt to synthesize a mixed‐ligand complex of FeII with an N‐containing ligand and benzene‐1,2,4,5‐tetracarboxylic acid via a solvothermal reaction. In both mononuclear complexes, each FeII metal ion is six‐coordinated in a distorted octahedral manner by six N atoms from three chelating 1,10‐phenanthroline or 2,2′‐bipyridine ligands. In compound (I), the FeII atom lies on a twofold axis in the space group C2/c, whereas (II) crystallizes in the space group P21/n. In both compounds, the uncoordinated carboxylate anions and water molecules are linked by typical O—H...O hydrogen bonds, generating extensive three‐dimensional hydrogen‐bond networks which surround the cations. 相似文献
6.
《Acta Crystallographica. Section C, Structural Chemistry》2017,73(11):975-978
Platinum antitumour agents, containing aromatic rings, which are used for targeting DNA in effective therapies for the treatment of cancer. We have synthesized the title metallocomplex with an aromatic ligand and determined its crystal structure. In many cases, complexes of platinum and other metals have a symmetrical structure. In contrast, the platinum(II) complex with pyridine and N‐(9‐anthracenylmethyl)‐1,2‐ethanediamine as ligands (systematic name: cis‐{N‐[(anthracen‐9‐yl)methyl]ethane‐1,2‐diamine‐κ2N ,N ′}bis(pyridine‐κN )platinum(II) dinitrate), [Pt(C5H5N)2(C17H18N2)](NO3)2, is asymmetric. Of the two pyridine ligands, only one is π‐stacked with anthracene, resulting in an asymmetric structure. Moreover, the angle of orientation of each pyridine ligand is variable. Further examination of the packing motif confirms an intermolecular edge‐to‐face interaction. 相似文献
7.
《Acta Crystallographica. Section C, Structural Chemistry》2017,73(11):923-929
Carbon monoxide (CO) has recently been identified as a gaseous signaling molecule that exerts various salutary effects in mammalian pathophysiology. Photoactive metal carbonyl complexes (photoCORMs) are ideal exogenous candidates for more controllable and site‐specific CO delivery compared to gaseous CO. Along this line, our group has been engaged for the past few years in developing group‐7‐based photoCORMs towards the efficient eradication of various malignant cells. Moreover, several such complexes can be tracked within cancerous cells by virtue of their luminescence. The inherent luminecscent nature of some photoCORMs and the change in emission wavelength upon CO release also provide a covenient means to track the entry of the prodrug and, in some cases, both the entry and CO release from the prodrug. In continuation of the research circumscribing the development of trackable photoCORMs and also to graft such molecules covalently to conventional delivery vehicles, we report herein the synthesis and structures of three rhenium carbonyl complexes, namely, fac‐tricarbonyl[2‐(pyridin‐2‐yl)‐1,3‐benzothiazole‐κ2N ,N ′](4‐vinylpyridine‐κN )rhenium(I) trifluoromethanesulfonate, [Re(C7H7N)(C12H8N2S)(CO)3](CF3SO3), ( 1 ), fac‐tricarbonyl[2‐(quinolin‐2‐yl)‐1,3‐benzothiazole‐κ2N ,N ′](4‐vinylpyridine‐κN )rhenium(I) trifluoromethanesulfonate, [Re(C7H7N)(C16H10N2S)(CO)3](CF3SO3), ( 2 ), and fac‐tricarbonyl[1,10‐phenanthroline‐κ2N ,N ′](4‐vinylpyridine‐κN )rhenium(I) trifluoromethanesulfonate, [Re(C7H7N)(C12H8N2)(CO)3](CF3SO3), ( 3 ). In all three complexes, the ReI center resides in a distorted octahedral coordination environment. These complexes exhibit CO release upon exposure to low‐power UV light. The apparent CO release rates of the complexes have been measured to assess their comparative CO‐donating capacity. The three complexes are highly luminescent and this in turn provides a convenient way to track the entry of the prodrug molecules within biological targets. 相似文献
8.
Reinaldo Atencio Gustavo Chacn Lisbeth Mendoza Teresa Gonzlez Julia Bruno-Colmenarez Merlin Rosales Briceo Alexander Edgar Ocando-Mavrez 《Acta Crystallographica. Section C, Structural Chemistry》2020,76(9):932-946
A series of related acetylacetonate–carbonyl–rhodium compounds substituted by functionalized phosphines has been prepared in good to excellent yields by the reaction of [Rh(acac)(CO)2] (acac is acetylacetonate) with the corresponding allyl‐, cyanomethyl‐ or cyanoethyl‐substituted phosphines. All compounds were fully characterized by 31P, 1H, 13C NMR and IR spectroscopy. The X‐ray structures of (acetylacetonato‐κ2O,O′)(tert‐butylphosphanedicarbonitrile‐κP)carbonylrhodium(I), [Rh(C5H7O2)(CO)(C8H13N2)] or [Rh(acac)(CO)(tBuP(CH2CN)2}] ( 2b ), (acetylacetonato‐κ2O,O′)carbonyl[3‐(diphenylphosphanyl)propanenitrile‐κP]rhodium(I), [Rh(C5H7O2)(C15H14N)(CO)] or [Rh(acac)(CO){Ph2P(CH2CH2CN)}] ( 2h ), and (acetylacetonato‐κ2O,O′)carbonyl[3‐(di‐tert‐butylphosphanyl)propanenitrile‐κP]rhodium(I), [Rh(C5H7O2)(C11H22N)(CO)] or [Rh(acac)(CO){tBu2P(CH2CH2CN)}] ( 2i ), showed a square‐planar geometry around the Rh atom with a significant trans influence over the acetylacetonate moiety, evidenced by long Rh—O bond lengths as expected for poor π‐acceptor phosphines. The Rh—P distances displayed an inverse linear dependence with the coupling constants JP‐Rh and the IR ν(C[triple‐bond]O) bands, which accounts for the Rh—P electronic bonding feature (poor π‐acceptors) of these complexes. A combined study from density functional theory (DFT) calculations and an evaluation of the intramolecular H…Rh contacts from X‐ray diffraction data allowed a comparison of the conformational preferences of these complexes in the solid state versus the isolated compounds in the gas phase. For 2b , 2h and 2i , an energy‐framework study evidenced that the crystal structures are mainly governed by dispersive energy. In fact, strong pairwise molecular dispersive interactions are responsible for the columnar arrangement observed in these complexes. A Hirshfeld surface analysis employing three‐dimensional molecular surface contours and two‐dimensional fingerprint plots indicated that the structures are stabilized by H…H, C…H, H…O, H…N and H…Rh intermolecular interactions. 相似文献
9.
David Martínez Majid Motevalli Michael Watkinson 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(4):m258-m260
The title compound, aquachloro{2,2′‐[1,2‐ethanediylbis(nitrilomethylidyne)]diphenolato‐κ4O,N,N′,O′}manganese(III),[MnCl(C16H14N2O2)(H2O)], is a neutral manganese(III) complex with a pseudo‐octahedral metal centre. The equatorial plane comprises the four donor atoms of the tetradentate Schiff base ligand [Mn—O 1.886 (4) and 1.893 (4) Å, and Mn—N 1.978 (5) and 1.982 (5) Å], with a water molecule [Mn—O 2.383 (4) Å] and a Cl? ligand [Mn—Cl 2.4680 (16) Å] completing the coordination sphere. The distorted geometry is highlighted by the marked displacement of the MnIII ion out of the least‐squares plane of the four Schiff base donor atoms by 0.165 (2) Å. These monomeric MnIII centres are then linked into a polymeric array via hydrogen bonds between the coordinated water molecule and the phenolic O‐atom donors of an adjacent MnIII centre [O—H?O 2.789 (5) and 2.881 (5) Å]. 相似文献
10.
《Acta Crystallographica. Section C, Structural Chemistry》2017,73(6):486-491
Luminescent CuI complexes have emerged as promising substitutes for phosphorescent emitters based on Ir, Pt and Os due to their abundance and low cost. The title heteroleptic cuprous complex, [9,9‐dimethyl‐4,5‐bis(diphenylphosphanyl)‐9H‐xanthene‐κ2P ,P ](2‐methylquinolin‐8‐ol‐κ2N ,O )copper(I) hexafluorophosphate, [Cu(C10H9NO)(C39H32OP2)]PF6, conventionally abbreviated as [Cu(Xantphos)(8‐HOXQ)]PF6, where Xantphos is the chelating diphosphine ligand 9,9‐dimethyl‐4,5‐bis(diphenylphosphanyl)‐9H‐xanthene and 8‐HOXQ is the N ,O‐chelating ligand 2‐methylquinolin‐8‐ol that remains protonated at the hydroxy O atom, is described. In this complex, the asymmetric unit consists of a hexafluorophosphate anion and a whole mononuclear cation, where the CuI atom is coordinated by two P atoms from the Xantphos ligand and by the N and O atoms from the 8‐HOXQ ligand, giving rise to a tetrahedral CuP2NO coordination geometry. The electronic absorption and photoluminescence properties of this complex have been studied on as‐synthesized samples, whose purity had been determined by powder X‐ray diffraction. In the detailed TD–DFT (time‐dependent density functional theory) studies, the yellow emission appears to be derived from the inter‐ligand charge transfer and metal‐to‐ligand charge transfer (M +L ′)→LCT excited state (LCT is ligand charge transfer). 相似文献
11.
Chi Nguyen Thi Thanh Thong Pham Van Hai Le Thi Hong Luc Van Meervelt 《Acta Crystallographica. Section C, Structural Chemistry》2016,72(10):758-764
Crystallization experiments with the dinuclear chelate ring complex di‐μ‐chlorido‐bis[(η2‐2‐allyl‐4‐methoxy‐5‐{[(propan‐2‐yloxy)carbonyl]methoxy}phenyl‐κC1)platinum(II)], [Pt2(C15H19O4)2Cl2], containing a derivative of the natural compound eugenol as ligand, have been performed. Using five different sets of crystallization conditions resulted in four different complexes which can be further used as starting compounds for the synthesis of Pt complexes with promising anticancer activities. In the case of vapour diffusion with the binary chloroform–diethyl ether or methylene chloride–diethyl ether systems, no change of the molecular structure was observed. Using evaporation from acetonitrile (at room temperature), dimethylformamide (DMF, at 313 K) or dimethyl sulfoxide (DMSO, at 313 K), however, resulted in the displacement of a chloride ligand by the solvent, giving, respectively, the mononuclear complexes (acetonitrile‐κN)(η2‐2‐allyl‐4‐methoxy‐5‐{[(propan‐2‐yloxy)carbonyl]methoxy}phenyl‐κC1)chloridoplatinum(II) monohydrate, [Pt(C15H19O4)Cl(CH3CN)]·H2O, (η2‐2‐allyl‐4‐methoxy‐5‐{[(propan‐2‐yloxy)carbonyl]methoxy}phenyl‐κC1)chlorido(dimethylformamide‐κO)platinum(II), [Pt(C15H19O4)Cl(C2H7NO)], and (η2‐2‐allyl‐4‐methoxy‐5‐{[(propan‐2‐yloxy)carbonyl]methoxy}phenyl‐κC1)chlorido(dimethyl sulfoxide‐κS)platinum(II), determined as the analogue {η2‐2‐allyl‐4‐methoxy‐5‐[(ethoxycarbonyl)methoxy]phenyl‐κC1}chlorido(dimethyl sulfoxide‐κS)platinum(II), [Pt(C14H17O4)Cl(C2H6OS)]. The crystal structures confirm that acetonitrile interacts with the PtII atom via its N atom, while for DMSO, the S atom is the coordinating atom. For the replacement, the longest of the two Pt—Cl bonds is cleaved, leading to a cis position of the solvent ligand with respect to the allyl group. The crystal packing of the complexes is characterized by dimer formation via C—H…O and C—H…π interactions, but no π–π interactions are observed despite the presence of the aromatic ring. 相似文献
12.
《Acta Crystallographica. Section C, Structural Chemistry》2017,73(4):357-361
PhotoCORMs (photo‐active CO‐releasing molecules) have emerged as a class of CO donors where the CO release process can be triggered upon illumination with light of appropriate wavelength. We have recently reported an Mn‐based photoCORM, namely [MnBr(pbt)(CO)3] [pbt is 2‐(pyridin‐2‐yl)‐1,3‐benzothiazole], where the CO release event can be tracked within cellular milieu by virtue of the emergence of strong blue fluorescence. In pursuit of developing more such trackable photoCORMs, we report herein the syntheses and structural characterization of two MnI–carbonyl complexes, namely fac‐tricarbonylchlorido[2‐(pyridin‐2‐yl)‐1,3‐benzothiazole‐κ2N ,N ′]manganese(I), [MnCl(C12H8N2S)(CO)3], (1), and fac‐tricarbonylchlorido[2‐(quinolin‐2‐yl)‐1,3‐benzothiazole‐κ2N ,N ′]manganese(I), [MnCl(C16H10N2S)(CO)3], (2). In both complexes, the MnI center resides in a distorted octahedral coordination environment. Weak intermolecular C—H…Cl contacts in complex (1) and Cl…S contacts in complex (2) consolidate their extended structures. These complexes also exhibit CO release upon exposure to low‐power broadband visible light. The apparent CO release rates for the two complexes have been measured to compare their CO donating capacity. The fluorogenic 2‐(pyridin‐2‐yl)‐1,3‐benzothiazole and 2‐(quinolin‐2‐yl)‐1,3‐benzothiazole ligands provide a convenient way to track the CO release event through the `turn‐ON' fluorescence which results upon de‐ligation of the ligands from their respective metal centers following CO photorelease. 相似文献
13.
William Raven Irmgard Kalf Ulli Englert 《Acta Crystallographica. Section C, Structural Chemistry》2012,68(8):m223-m225
The enantiomerically pure title complex, [SP‐4‐4]‐(R)‐[2‐(1‐aminoethyl)phenyl‐κ2C1,N]chlorido(quinoline‐κN)palladium(II) acetone hemisolvate, [Pd(C8H10N)Cl(C9H7N)]·0.5C3H6O, crystallizes with four molecules of the organopalladium complex and two molecules of acetone in the asymmetric unit. This corresponds to a discrete hydrogen‐bonded aggregate and to the content of the unit cell in the space group P1. Pronounced pseudo‐inversion symmetry relates pairs of these objects in the asymmetric unit. 相似文献
14.
Yoshio Wada Nobuo Okabe Yasunori Muranishi 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(10):m511-m513
In trans‐bis(5‐n‐butylpyridine‐2‐carboxylato‐κ2N,O)bis(methanol‐κO)copper(II), [Cu(C10H12NO2)2(CH4O)2], the Cu atom lies on a centre of symmetry and has a distorted octahedral coordination. The Cu—O(methanol) bond length in the axial direction is 2.596 (3) Å, which is much longer than the Cu—O(carboxylate) and Cu—N distances in the equatorial plane [1.952 (2) and 1.977 (2) Å, respectively]. In mer‐tris(5‐n‐butylpyridine‐2‐carboxylato‐κ2N,O)iron(III), [Fe(C10H12NO2)3], the Fe atom also has a distorted octahedral geometry, with Fe—O and Fe—N bond‐length ranges of 1.949 (4)–1.970 (4) and 2.116 (5)–2.161 (5) Å, respectively. Both crystals are stabilized by stacking interactions of the 5‐n‐butylpyridine‐2‐carboxylate ligand, although hydrogen bonds also contribute to the stabilization of the copper(II) complex. 相似文献
15.
Chi Nguyen Thi Thanh Ngan Nguyen Bich Luc Van Meervelt 《Acta Crystallographica. Section C, Structural Chemistry》2014,70(3):297-301
The crystal structures of cis‐dichlorido(ethylamine‐κN)(piperidine‐κN)platinum(II), [PtCl2(C2H7N)(C5H11N)], (I), cis‐dichlorido(3‐methoxyaniline‐κN)(piperidine‐κN)platinum(II), [PtCl2(C5H11N)(C7H9NO)], (II), and cis‐dichlorido(piperidine‐κN)(quinoline‐κN)platinum(II), [PtCl2(C5H11N)(C9H7N)], (III), have been determined at 100 K in order to verify the influence of the nonpiperidine ligand on the geometry and crystal packing. The crystal packing is characterized by N—H...Cl hydrogen bonding, resulting in the formation of chains of molecules connected in a head‐to‐tail fashion. Hydrogen‐bonding interactions play a major role in the packing of (I), where the chains further aggregate into planes, but less so in the case of (II) and (III), where π–π stacking interactions are of greater importance. 相似文献
16.
Günter Reck Roland Becker 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(3):m134-m136
Bis(N,N‐di‐n‐butyldithiocarbamato‐κ2S,S′)(1,10‐phenanthroline‐κ2N,N′)zinc(II) ethanol hemisolvate, [Zn(C9H18NS2)2(C12H8N2)]·0.5C2H6O, (I), and bis(N,N‐di‐n‐hexyldithiocarbamato‐κ2S,S′)bis(1,10‐phenanthroline‐κ2N,N′)calcium(II), [Ca(C13H26NS2)2(C12H8N2)2], (II), are mixed‐ligand complexes. In the first compound, the Zn atom has a distorted octahedral coordination, while in the second compound, the Ca atom is eight‐coordinate, with four S and four N atoms forming a highly distorted cube. 相似文献
17.
Pierre Haquette Franck Lebideau Samuel Dagorne Jrme Marrot Grard Jaouen 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(11):m551-m552
The crystal structure of the title compound, chloro(η5‐cyclopentadienyl){(1R,2S)‐2‐[(diphenylphosphino)methylamino]‐1‐phenylpropyl diphenylphosphinite‐κ2P,P′}ruthenium(II), [Ru(C5H5)Cl(C34H33NOP2)], is reported. The pseudo‐octahedral complex is chiral and the configuration at the Ru atom is S. The seven‐membered metallacycle adopts a boat‐like conformation. 相似文献
18.
Mihaela Cibian Andr Bessette Andrew O'Connor Janaina G. Ferreira Garry S. Hanan 《Acta Crystallographica. Section C, Structural Chemistry》2015,71(2):122-127
The crystal structures of fac‐(acetonitrile‐κN)(2‐{[3,5‐bis(4‐methoxyphenyl)‐2H‐pyrrol‐2‐ylidene‐κN1]amino}‐3,5‐bis(4‐<!?tlsb=0.2pt>methoxyphenyl)‐1H‐pyrrol‐1‐ido‐κN1)tricarbonylrhenium(I)–hexane–acetonitrile (2/1/2), [Re(C36H30N3O4)(CH3CN)(CO)3]·0.5C6H14·CH3CN, (2), and fac‐(2‐{[3,5‐bis(4‐methoxyphenyl)‐2H‐pyrrol‐2‐ylidene‐κN1]amino}‐3,5‐bis(4‐methoxyphenyl)‐1H‐pyrrol‐1‐ido‐κN1)tricarbonyl(dimethyl sulfoxide‐κO)rhenium(I), [Re(C36H30N3O4)(C2H6OS)(CO)3], (3), at 150 K are reported. Both complexes display a distorted octahedral geometry, with a fac‐Re(CO)3 arrangement and one azadipyrromethene (ADPM) chelating ligand in the equatorial position. One solvent molecule completes the coordination sphere of the ReI centre in the remaining axial position. The ADPM ligand shows high flexibility upon coordination, while retaining its π‐delocalized nature. Bond length and angle analyses indicate that the differences in the geometry around the ReI centre in (2) and (3), and those found in three reported fac‐Re(CO)3–ADPM complexes, are dictated mainly by steric factors and crystal packing. Both structures display intramolecular C—H...N hydrogen bonding. Intermolecular interactions of the Csp2—H...π and Csp2—H...O(carbonyl) types link the discrete monomers into extended chains. 相似文献
19.
Daniel T. Marake Penny P. Mokolokolo Hendrik G. Visser Alice Brink 《Acta Crystallographica. Section C, Structural Chemistry》2015,71(6):423-429
Two tricarbonyl complexes of rhenium(I) and manganese(I) coordinated by the ligand 2‐{[2‐(1H‐imidazol‐4‐yl)ethyl]iminomethyl}‐5‐methylphenolate are reported, viz. fac‐tricarbonyl(2‐{[2‐(1H‐imidazol‐4‐yl‐κN3)ethyl]iminomethyl‐κN}‐5‐methylphenolato‐κO)rhenium(I) methanol monosolvate, [Re(C16H14N3O4)(CO)3]·CH3OH, (I), and fac‐tricarbonyl(2‐{[2‐(1H‐imidazol‐4‐yl‐κN3)ethyl]iminomethyl‐κN}‐5‐methylphenolato‐κO)manganese(I), fac‐[Mn(C16H14N3O4)(CO)3], (II), display facial coordination in a distorted octahedral environment. The crystal structure of (I) is stabilized by O—H...O, N—H...O and C—H...O hydrogen‐bond interactions, while that of (II) is stabilized by N—H...O hydrogen‐bond interactions only. These interactions result in two‐dimensional networks and π–π stacking for both structures. 相似文献
20.
Tomoko Harada Satoko Wada Hidetaka Yuge Takeshi Ken Miyamoto 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(2):m37-m39
In the two ruthenium(II)–porphyrin–carbene complexes (dibenzoylcarbenyl‐κC)(pyridine‐κN)(5,10,15,20‐tetra‐p‐tolylporphyrinato‐κ4N)ruthenium(II), [Ru(C15H10O2)(C5H5N)(C48H36N4)], (I), and (pyridine‐κN)(5,10,15,20‐tetra‐p‐tolylporphyrinato‐κ4N)[bis(3‐trifluoromethylphenyl)carbenyl‐κC]ruthenium(II), [Ru(C15H8F6)(C5H5N)(C48H36N4)], (II), the pyridine ligand coordinates to the octahedral Ru atom trans with respect to the carbene ligand. The C(carbene)—Ru—N(pyridine) bonds in (I) coincide with a crystallographic twofold axis. The Ru—C bond lengths of 1.877 (8) and 1.868 (3) Å in (I) and (II), respectively, are slightly longer than those of other ruthenium(II)–porphyrin–carbene complexes, owing to the trans influence of the pyridine ligands. 相似文献