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1.
A transition metal Lewis acid with metal‐centered chirality is obtained by η6:η1:η1 coordination of a 1,3‐disubstituted arene with a phosphane and a pyrazole tether (PArN) to ruthenium. The three‐legged piano‐stool complex [{η6:η1:η1‐(PArN)}Ru(H2O)]2+ (structure depicted) displays remarkable configurational stability. Its planar chiral, neutral precursor [{η6:η1‐(PArN)}RuCl2] can be resolved by preparative HPLC. 相似文献
2.
Karel Mach Jií Kubita Ivana Císaov Petr tpni
ka 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(2):m116-m118
Reacting stoichiometric amounts of 1‐(diphenylphosphino)ferrocenecarboxylic acid and [Ti(η5‐C5HMe4)2(η2‐Me3SiC[triple‐bond]CSiMe3)] produced the title carboxylatotitanocene complex, [{μ‐1κ2O,O′:2(η5)‐C5H4CO2}{2(η5)‐C5H4P(C6H5)2}{1(η5)‐C5H(CH3)4}2FeIITiIII] or [FeTi(C9H13)2(C6H4O2)(C17H14P)]. The angle subtended by the Ti/O/O′ plane, where O and O′ are the donor atoms of the κ2‐carboxylate group, and the plane of the carboxyl‐substituted ferrocene cyclopentadienyl is 24.93 (6)°. 相似文献
3.
eljko K. Jaimovi Zoran D. Tomi Gerald Giester Vukadin M. Leovac 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(10):m381-m383
In the crystal structure of the title complex, [Co(C6H8N3S)3], the CoIII atom is octahedrally coordinated by three monodeprotonated bidentate 3,5‐dimethyl‐1H‐pyrazole‐1‐thiocarboxamide ligands with two thiocarboxamide N atoms in axial positions. The asymmetric unit contains two molecules (A and B) and these molecules are arranged in chains in an alternating fashion connected by N—H⋯S interactions. 相似文献
4.
The synthesis and single crystal X‐ray structure determination are reported for the 2,2′ : 6′,2″‐terpyridine (= tpy) adduct of bismuth(III) nitrate. The hydroxide‐bridged dimer [(η2‐NO3)2(tpy)Bi(μ‐OH)2Bi(tpy)(η2‐NO3)2] with nine‐coordinate geometry about Bi was the only isolable product from all crystallization attempts in varying ratios of Bi(NO3) : terpy.; [(η2‐NO3)2(tpy)Bi(μ‐OH)2Bi(tpy) · (η2‐NO3)2] is triclinic, P 1, a = 7.941(8), b = 10.732(9), c = 11.235(9) Å; α = 63.05(1), β = 85.01(1), γ = 79.26(1)°, Z = 1, dimer, R = 0.058 for N0 = 2319. 相似文献
5.
Manfredo Hrner Julieta Saldanha de Oliveira Jairo Bordinhao Johannes Beck 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(12):m586-m587
In the centrosymmetric title complex, [Ni(C7H7N4O3)2(C5H5N)2], the coordination geometry about the Ni2+ ion is octahedral, with two deprotonated 1‐methyl‐3‐(p‐nitrophenyl)triazenide 1‐oxide ions, viz. [O2NC6H4NNN(O)CH3]?, acting as bidentate ligands (four‐electron donors). Two neutral pyridine (py) molecules complete the coordination sphere in positions trans to each other. The triazenide 1‐oxide ligand is almost planar, the largest interplanar angle of 8.80 (12)° being between the phenyl ring of the p‐nitrophenyl group and the plane defined by the N3O moiety. The Ni—Ntriazenide, Ni—O and Ni—Npy distances are 2.0794 (16), 2.0427 (13) and 2.1652 (18) Å, respectively. 相似文献
6.
Chong‐Qing Wan Zi‐Jia Wang Peng Qiao Zhi‐Wei Wang Ai‐Min Li 《Acta Crystallographica. Section C, Structural Chemistry》2012,68(5):m117-m120
In the title complex, [Ag(NO3)(C9H7N3OS)]n, η1:η1:η1:μ2‐bridging 2‐(pyridin‐4‐ylsulfinyl)pyrimidine (pypmSO) ligands with opposite chiralities are alternately arranged to link the AgI cations through two N atoms and one sulfinyl O atom of each ligand, leading to an extended zigzag coordination chain structure along the [01] direction. An FT–IR spectroscopic study shows a decreased stretching frequency for the η1‐O‐bonded S=O group compared with that of the free ligand. The parallel chains are arranged and interconnected via O(S=O)...π(pyridine/pyrimidine) and C—H(pyridine)...O(NO3−) interactions to furnish a layer almost parallel to the ac plane. Along the b axis, the layers are stacked and stabilized through anion(NO3−)...π(pyrimidine) interactions to form a three‐dimensional supramolecular framework. The ligand behaviour of the new diheterocyclic sulfoxide and the unconventional O(S=O)...π(pyridine/pyrimidine) and anion(NO3−)...π(pyrimidine) interactions in the supramolecular assembly of the title complex are presented. 相似文献
7.
Seong Huh Young Jun Park Alan. J. Lough Moo‐Jin Jun 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(4):416-417
The title compound, [RuH(C6H8BN4)(C21H21P)2(CO)], possesses two trans‐disposed tri‐p‐tolylphosphines in axial positions and the remaining ligands in equatorial positions. The overall geometry of the RuII ion is a distorted octahedral structure. The P—Ru—P axis deviates from linearity by about 13°. This distortion arises mainly from the steric congestion between the bulky phosphine moieties and the tetrahedral dihydrobis(pyrazol‐1‐yl)borate ligands. 相似文献
8.
Alexander V. Virovets Sergey N. Konchenko 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(9):e383-e384
The structure of the title compound, hexacarbonyl‐1κ3C,2κ3C‐[3(η5)‐cyclopentadienyl]bis(μ3‐selenido)diiron(II)cobalt(II),[CoFe2(μ3‐Se)2(C5H5)(CO)6], was redetermined at room temperature and the correct C2/c space group was assumed instead of the previously reported P space group [Mathur et al. (1995). Organometallics, 14 , 2115–2118]. Analysis of the literature data showed that the previously reported triclinic parameters correspond to a primitive subcell of the actual monoclinic C‐centred cell with cell dimensions close to those found by us. The title compound appeared to be isostructural with the sulfur–selenium analogue. 相似文献
9.
Ming‐Liang Tong Shao‐Liang Zheng Xiao‐Ming Chen 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(8):960-962
The title compound, poly[[diaquadibromocadmium‐μ‐(1,3,5,7‐tetraazatricyclo[3.3.1.13,7]decane‐N1:N5)‐aquacadmium‐di‐μ‐bromo‐aquacadmium‐μ‐(1,3,5,7‐tetraazatricyclo[3.3.1.13,7]decane‐N1:N5)‐di‐μ‐bromo] dihydrate], [Cd3Br6(C6H12N4)2(H2O)4]·2H2O, is made up of two‐dimensional neutral rectangular coordination layers. Each rectangular subunit is enclosed by a pair of Cd3(μ2‐Br)6(H2O)3 fragments and a pair of (μ2‐hmt)Cd(H2O)2Br2(μ2‐hmt) fragments as sides (hmt is hexamethylenetetramine). The unique CdII atom in the Cd2Br2 ring in the Cd3(μ2‐Br)6(H2O)3 fragment is in a slightly distorted octahedral CdNOBr4 geometry, surrounded by one hmt ligand [2.433 (5) Å], one aqua ligand [2.273 (4) Å] and four Br atoms [2.6409 (11)–3.0270 (14) Å]. The CdII atom in the (μ2‐hmt)Cd(H2O)2Br2(μ2‐hmt) fragment lies on an inversion center and is in a highly distorted octahedral CdN2O2Br2 geometry, surrounded by two trans‐related N atoms of two hmt ligands [2.479 (5) Å], two trans‐related aqua ligands [2.294 (4) Å] and two trans‐related Br atoms [2.6755 (12) Å]. Adjacent two‐dimensional coordination sheets are connected into a three‐dimensional network by hydrogen bonds involving lattice water molecules, and the aqua, bromo and hmt ligands belonging to different layers. 相似文献
10.
Robert J. Brown Donna S. Amenta John W. Gilje Glenn P. A. Yap 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(10):1104-1107
The aminophosphane ligand 1‐amino‐2‐(diphenylphosphanyl)ethane [Ph2P(CH2)2NH2] reacts with dichloridotris(triphenylphosphane)ruthenium(II), [RuCl2(PPh3)3], to form chloridobis[2‐(diphenylphosphanyl)ethanamine‐κ2P,N](triphenylphosphane‐κP)ruthenium(II) chloride toluene monosolvate, [RuCl(C18H15P)(C14H16NP)2]Cl·C7H8 or [RuCl(PPh3){Ph2P(CH2)2NH2}2]Cl·C7H8. The asymmetric unit of the monoclinic unit cell contains two molecules of the RuII cation, two chloride anions and two toluene molecules. The RuII cation is octahedrally coordinated by two chelating Ph2P(CH2)2NH2 ligands, a triphenylphosphane (PPh3) ligand and a chloride ligand. The three P atoms are meridionally coordinated, with the Ph2P– groups from the ligands being trans. The two –NH2 groups are cis, as are the chloride and PPh3 ligands. This chiral stereochemistry of the [RuCl(PPh3){Ph2P(CH2)2NH2}2]+ cation is unique in ruthenium–aminophosphane chemistry. 相似文献
11.
The η2‐thio‐indium complexes [In(η2‐thio)3] (thio = S2CNC5H10, 2 ; SNC4H4, (pyridine‐2‐thionate, pyS, 3 ) and [In(η2‐pyS)2(η2‐acac)], 4 , (acac: acetylacetonate) are prepared by reacting the tris(η2‐acac)indium complex [In(η2‐acac)3], 1 with HS2CNC5H10, pySH, and pySH with ratios of 1:3, 1:3, and 1:2 in dichloromethane at room temperature, respectively. All of these complexes are identified by spectroscopic methods and complexes 2 and 3 are determined by single‐crystal X‐ray diffraction. Crystal data for 2 : space group, C2/c with a = 13.5489(8) Å, b = 12.1821(7) Å, c = 16.0893(10) Å, β = 101.654(1)°, V = 2600.9(3) Å3, and Z = 4. The structure was refined to R = 0.033 and Rw = 0.086; Crystal data for 3 : space group, P21 with a = 8.8064 (6) Å, b = 11.7047 (8) Å, c = 9.4046 (7) Å, β = 114.78 (1)°, V = 880.13(11) Å3, and Z = 2. The structure was refined to R = 0.030 and Rw = 0.061. The geometry around the metal atom of the two complexes is a trigonal prismatic coordination. The piperidinyldithiocarbamate and pyridine‐2‐thionate ligands, respectively, coordinate to the indium metal center through the two sulfur atoms and one sulfur and one nitrogen atoms, respectively. The short C‐N bond length in the range of 1.322(4)–1.381(6) Å in 2 and C‐S bond length in the range of 1.715(2)–1.753(6) Å in 2 and 3 , respectively, indicate considerable partial double bond character. 相似文献
12.
Manfredo Hrner Vanessa S. Carratu Jairo Bordinhao Angela Silva Elke Niquet 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(3):m140-m142
In the title compound, [Cd(C12H8F2N3)2(C5H5N)2], the Cd atom lies on a crystallographic twofold axis in space group Iba2. The coordination geometry about the CdII ion corresponds to a rhombically distorted octahedron, with two deprotonated 1,3‐bis(2‐fluorophenyl)triazenide ions, viz. FC6H4NNNC6H4F−, acting as bidentate ligands (four‐electron donors). Two neutral pyridine (py) molecules complete the coordination sphere in positions cis with respect to one another. The triazenide ligand is not planar (r.m.s. deviation = 0.204 Å), the dihedral angle between the phenyl rings of the terminal 2‐fluorophenyl substituents being 24.6 (1)°. The triazenide and pyridine Cd—N distances are 2.3757 (18)/2.3800 (19) and 2.3461 (19) Å, respectively. Intermolecular C—H⋯F interactions generate sheets of molecules in the (010) plane. 相似文献
13.
The η1‐thiocarbamoyl palladium complexes [Pd(PPh3)(η1‐SCNMe2)(η2‐S2R)] (R = P(OEt)2, 2 ; CNEt2, 3 ) and trans‐[Pd(PPh3)2(η1‐SCNMe2)(η1‐Spy)], 4 , (pyS: pyridine‐2‐thionate) are prepared by reacting the η2‐thiocarbamoyl palladium complex [Pd(PPh3)2(η2‐SCNMe2)][PF6], 1 with (EtO)2PS2NH4, Et2NCS2Na, and pySK in methanol at room temperature, respectively. Treatment of 1 with dppm (dppm: bis(diphenylphosphino)methane) in dichloromethane at room temperature gives complex [Pd(PPh3)(η1‐SCNMe2)(η2‐dppm)] [PF6], 5 . All of the complexes are identified by spectroscopic methods and complex 1 is determined by single‐crystal X‐ray diffraction. 相似文献
14.
Uwe‐Christoph Knig Michael Berkei Claudia Hirsch Hans Preut Terence Nigel Mitchell 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(10):e450-e451
The synthesis and the X‐ray structural analysis of the title compound, μ‐chloro‐1:2κ2Cl‐trichloro‐1κCl,2κ2Cl‐tetramethyl‐1κ2C,2κ2C‐(N‐methylpyrrolidin‐2‐one)‐1κO‐ditin(IV), [Sn2Cl4(CH3)4(C5H9NO)], are described. The title compound is found to exhibit a distorted trigonal–bipyramidal geometry at both SnIV atoms. The Sn—Cl—Sn angle involving the bridging chlorine ligand is 135.56 (5)°, with the Sn—Cl bond lengths being 2.5704 (13) and 3.1159 (13) Å. 相似文献
15.
2, 4‐Dimethylpenta‐1, 3‐diene and 2, 4‐Dimethylpentadienyl Complexes of Rhodium and Iridium The complexes [(η4‐C7H12)RhCl]2 ( 1 ) (C7H12 = 2, 4‐dimethylpenta‐1, 3‐diene) and [(η4‐C7H12)2IrCl] ( 2 ) were obtained by interaction of C7H12 with [(η2‐C2H4)2RhCl]2 and [(η2‐cyclooctene)2IrCl]2, respectively. The reaction of 1 or 2 with CpTl (Cp = η5‐C5H5) yields the compounds [CpM(η4‐C7H12)] ( 3a : M = Rh; 3b : M = Ir). The hydride abstraction at the pentadiene ligand of 3a , b with Ph3CBF4 proceeds differently depending on the solvent. In acetone or THF the “half‐open” metallocenium complexes [CpM(η5‐C7H11)]BF4 ( 4a : M = Rh; 4b : M = Ir) are obtained exclusively. In dichloromethane mixtures are produced which additionally contain the species [(η5‐C7H11)M(η5‐C5H4CPh3)]BF4 ( 5a : M = Rh; 5b : M = Ir) formed by electrophilic substitution at the Cp ring, as well as the η3‐2, 4‐dimethylpentenyl compound [(η3‐C7H13)Rh{η5‐C5H3(CPh3)2}]BF4 ( 6 ). By interaction of 2, 4‐dimethylpentadienyl potassium with 1 or 2 the complexes [(η4‐C7H12)M(η5‐C7H11)] ( 7a : M = Rh; 7b : M = Ir) are generated which show dynamic behaviour in solution; however, attempts to synthesize the “open” metallocenium cations [(η5‐C7H11)2M]+ by hydride abstraction from 7a , b failed. The new compounds were characterized by elemental analysis and spectroscopically, 4b and 5a also by X‐ray structure analysis. 相似文献
16.
Eleonora Freire Sergio Baggio Juan Carlos Muoz Ricardo Baggio 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(8):m299-m301
The structure of the title compound, [Ni(ths)(bbip)(dmf)]·H2O [ths is thiosulfate, S2O3; bbip is 2,6‐bis(1H‐benzimidazol‐2‐yl)pyridine, C21H13N5; and dmf is dimethylformamide, C3H7NO], is monomeric, with the nickel ion octahedrally surrounded by an N,N′,N′′‐tridentate bbip molecule, an S,O‐bidentate ths molecule and an O‐monodentate dmf molecule. The H atoms of the hydration water molecule and the amino groups of bbip are involved in hydrogen bonding and determine a spatial organization of broad layers parallel to (001), which are connected by weak interactions. 相似文献
17.
Dr. Michael P. Boone Prof. Dr. Douglas W. Stephan 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(12):3333-3341
The reactivity of [{(Ph2PC6H4)2B(η6‐Ph)}RuCl][B(C6F5)4] ( 1 ) as a Lewis acid was investigated. Treatment of 1 with mono and multidentate phosphorus Lewis bases afforded the Lewis acid–base adducts with the ortho‐carbon atom of the coordinated arene ring. Similar reactivity was observed upon treatment with N‐heterocyclic carbenes; however, adduct formation occurred at both ortho‐ and para‐carbon atoms of the bound arene with the para‐position being favoured by increased steric demands. Interestingly treatment with isocyanides resulted in adduct formation with the B‐centre of the ligand framework. The hydride‐cation [{(Ph2PC6H4)2B(η6‐Ph)}RuH] [B(C6F5)4] was prepared via reaction of 1 with silane. This species in the presence of a bulky phosphine behaves as a frustrated Lewis pair (FLP) to activate H2 between the phosphorus centre and the ortho‐carbon atom of the η6‐arene ring. 相似文献
18.
A twofold interpenetrating three‐dimensional CdII coordination framework, [Cd(C8H3NO6)(C14H14N4)]n, has been prepared and characterized by IR spectroscopy, elemental analysis, thermal analysis and single‐crystal X‐ray diffraction. The asymmetric unit consists of a divalent CdII atom, one 1,3‐bis(2‐methyl‐1H‐imidazol‐1‐yl)benzene (1,3‐BMIB) ligand and one fully deprotonated 5‐nitrobenzene‐1,3‐dicarboxylate (NO2‐BDC2−) ligand. The coordination sphere of the CdII atom consists of five O‐donor atoms from three different NO2‐BDC2− ligands and two imidazole N‐donor atoms from two different 1,3‐BMIB ligands, forming a distorted {CdN2O5} pentagonal bipyramid. The NO2‐BDC ligand links three CdII atoms via a μ1‐η1:η1 chelating mode and a μ2‐η2:η1 bridging mode. The title compound is a twofold interpenetrating 3,5‐connected network with the {42.65.83}{42.6} topology. In addition, the compound exhibits fluorescence emissions in the solid state at room temperature. 相似文献
19.
Dinuclear Rare‐Earth Metal Alkyl Complexes Supported by Indolyl Ligands in μ‐η2:η1:η1 Hapticities and their High Catalytic Activity for Isoprene 1,4‐cis‐Polymerization 下载免费PDF全文
Guangchao Zhang Yun Wei Liping Guo Prof. Dr. Xiancui Zhu Prof. Dr. Shaowu Wang Prof. Dr. Shuangliu Zhou Xiaolong Mu 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(6):2519-2526
Two series of new dinuclear rare‐earth metal alkyl complexes supported by indolyl ligands in novel μ‐η2:η1:η1 hapticities are synthesized and characterized. Treatment of [RE(CH2SiMe3)3(thf)2] with 1 equivalent of 3‐(tBuN?CH)C8H5NH ( L1 ) in THF gives the dinuclear rare‐earth metal alkyl complexes trans‐[(μ‐η2:η1:η1‐3‐{tBuNCH(CH2SiMe3)}Ind)RE(thf)(CH2SiMe3)]2 (Ind=indolyl, RE=Y, Dy, or Yb) in good yields. In the process, the indole unit of L1 is deprotonated by the metal alkyl species and the imino C?N group is transferred to the amido group by alkyl CH2SiMe3 insertion, affording a new dianionic ligand that bridges two metal alkyl units in μ‐η2:η1:η1 bonding modes, forming the dinuclear rare‐earth metal alkyl complexes. When L1 is reduced to 3‐(tBuNHCH2)C8H5NH ( L2 ), the reaction of [Yb(CH2SiMe3)3(thf)2] with 1 equivalent of L2 in THF, interestingly, generated the trans‐[(μ‐η2:η1:η1‐3‐{tBuNCH2}Ind)Yb(thf)(CH2SiMe3)]2 (major) and cis‐[(μ‐η2:η1:η1‐3‐{tBuNCH2}Ind)Yb(thf)(CH2SiMe3)]2 (minor) complexes. The catalytic activities of these dinuclear rare‐earth metal alkyl complexes for isoprene polymerization were investigated; the yttrium and dysprosium complexes exhibited high catalytic activities and high regio‐ and stereoselectivities for isoprene 1,4‐cis‐polymerization. 相似文献
20.
Nack‐Do Sung Ki‐Seob Yun Jin‐Gyu Kim Il‐Hwan Suh 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(9):e370-e371
The title compound, μ‐aqua‐1:2κ2O‐pentaaqua‐1κ2O,2κ3O‐μ‐3,6‐bis(6‐methyl‐2‐pyridyl)pyridazine‐1κ2N1,N6:2κ2N2,N3‐chloro‐1κCl‐dinickel(II) trichloride trihydrate, [Ni2Cl(C16H14N4)(H2O)6]Cl3·3H2O, consists of two NiII atoms, a 3,6‐bis(6‐methyl‐2‐pyridyl)pyridazine molecule, four Cl atoms and nine water molecules. The two Ni atoms are octahedrally coordinated by N and Cl atoms, and by water molecules, and the three six‐membered rings, a pyridazine and two picolines, are planar to within 0.181 (3) Å. The crystal structure is stabilized by an intra‐ and intermolecular hydrogen‐bonding scheme involving water–water and water–chlorine interactions. 相似文献