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1.
Jan Janczak Mayura M. M. Rubinger Leandro C. Alves Marcelo R. L. Oliveira 《Acta Crystallographica. Section C, Structural Chemistry》2012,68(11):m312-m316
The rigid organic linkers N‐(4‐bromophenylsulfonyl)dithiocarbimate(2−) and N‐(4‐iodophenylsulfonyl)dithiocarbimate(2−) crystallize with two potassium cations and two water molecules in their asymmetric units, forming the title coordination polymers, [K2(C7H4BrNO2S3)(H2O)2]n and [K2(C7H4INO2S3)(H2O)2]n. The anions and the water molecules link the potassium cations into broad two‐dimensional networks, which are further linked by K...halide interactions. 相似文献
2.
Thomas D. McGrath Mark A. Fox Alan J. Welch 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(4):487-488
The title compound, 9‐iodo‐1,2‐diphenyl‐1,2‐dicarba‐closo‐dodecaborane(9), C14H19B10I, has the expected pseudo‐icosahedral cluster geometry, with a cage C—C distance of 1.724 (4) Å, comparable to that in the non‐iodinated parent. However, the twist angles, θ, of the phenyl rings are 2.1 (6) and 27.6 (5)°, the latter being unusually large. 相似文献
3.
Paloma Sevillano Sven Koenig Daniel Himmel Olaf Fuhr Dieter Fenske 《无机化学与普通化学杂志》2005,631(11):2236-2240
The reactions of [Co2(CO)8] with E(SiMe3)2 (E = Se, Te) in CH2Cl2 result in the formation of the compounds [Co4Se2(CO)10]> ( 1 ) and [Co4Te2(CO)11] ( 2 ), respectively. Both cluster complexes have similar molecular structures in which the cobalt atoms form four‐membered rings with μ4‐bridging chalcogen atoms (Se and Te) above and below the plane of the metal atoms and the carbonyl ligands as either terminal or μ2‐bridging ligands. DFT‐calculations for both compounds have been carried out in order to obtain some more information about their electronic distribution. In the presence of the phosphine Ph2PC≡CPPh2 (dppa), the reaction of [Co2(CO)8] with Se(SiMe3)2 leads to the formation of [Co8Se4(CO)16(μ‐dppa)2] ( 3 ). During the reaction two molecules of [Co2(CO)8] have been added to the acetylene groups of the dppa ligands, whilst the remaining cobalt atoms coordinate to the phosphorus atoms of the phosphine. In this compounds the selenium atoms act as μ3‐ligands, bridging the metal atoms bonded to the phosphorus with those bonded to the acetylene groups. 相似文献
4.
John Bacsa Hanhua Zhao Kim R. Dunbar 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(12):m561-m564
Two new iron–oxo clusters, viz. di‐μ‐trifluoroacetato‐μ‐oxo‐bis[(2,2′‐bipyridine‐κ2N,N′)(trifluoroacetato‐κO)iron(III)], [Fe2O(CF3CO2)4(C10H8N2)2], and bis(2,2′‐bipyridine)di‐μ3‐oxo‐hexa‐μ‐trifluoroacetato‐bis(trifluoroacetato)tetrairon(III) trifluoroacetic acid solvate, [Fe4O2(CF3CO2)8(C10H8N2)2]·CF3CO2H, contain dinuclear and tetranuclear FeIII cores, respectively. The FeIII atoms are in distorted octahedral environments in both compounds and are linked by oxide and trifluoroacetate ions. The trifluoroacetate ions are either bridging (bidentate) or coordinated to the FeIII atoms via one O atom only. The fluorinated peripheries enhance the solubility of these compounds. Formal charges for all the Fe centers were assigned by summing valences of the chemical bonds to the FeIII atom. 相似文献
5.
Hans‐Christian Bttcher Marion Graf Kurt Merzweiler Christoph Wagner 《无机化学与普通化学杂志》2001,627(5):903-908
Heterobinuclear Complexes: Synthesis and X‐ray Crystal Structures of [RuRh(μ‐CO)(CO)4(μ‐PtBu2)(tBu2PH)], [RuRh(μ‐CO)(CO)3(μ‐PtBu2)(μ‐Ph2PCH2PPh2)], and [CoRh(CO)4(μ‐H)(μ‐PtBu2)(tBu2PH)] [Ru3Rh(CO)7(μ3‐H)(μ‐PtBu2)2(tBu2PH)(μ‐Cl)2] ( 2 ) yields by cluster degradation under CO pressure as main product the heterobinuclear complex [RuRh(μ‐CO)(CO)4(μ‐PtBu2)(tBu2PH)] ( 4 ). The compound crystallizes in the orthorhombic space group Pcab with a = 15.6802(15), b = 28.953(3), c = 11.8419(19) Å and V = 5376.2(11) Å3. The reaction of 4 with dppm (Ph2PCH2PPh2) in THF at room temperature affords in good yields [RuRh(μ‐CO)(CO)3(μ‐PtBu2)(μ‐dppm)] ( 7 ). 7 crystallizes in the triclinic space group P 1 with a = 9.7503(19), b = 13.399(3), c = 15.823(3) Å and V = 1854.6 Å3. Moreover single crystals of [CoRh(CO)4(μ‐H)(μ‐PtBu2)(tBu2PH)] ( 9 ) could be obtained and the single‐crystal X‐ray structure analysis revealed that 9 crystallizes in the monoclinic space group P21/a with a = 11.611(2), b = 13.333(2), c = 18.186(3) Å and V = 2693.0(8) Å3. 相似文献
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Investigations on Metal Catalysts. XXII. Chemisorption of Hydrogen on Pt? Ru and η-Al2O3 Supported Pt? Ru Catalysts Measurements of the H2 chemisorption by volumetric method were carried out on several series of Pt? Ru and η-Al2O3 supported Pt? Ru catalysts. Addition of Ru to Pt and vice versa effects a remarkable influence on the sorption behaviour of the starting samples. For mixtures of carrier-free catalysts and η-Al2O3 as well as Pt? Ru/η-Al2O3 catalysts a hydrogen-spillover effect was found. 相似文献
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10.
John Nicolson Low Justo Cobo Braulio Insuasty Manuel Nogueras Angela Salcedo Adolfo Snchez 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(2):o125-o128
The title compounds, 2‐(4‐bromophenyl)‐1,2‐dihydropyrimido[1,2‐a]benzimidazol‐4‐(3H)‐one, C16H12BrN3O, (IVa), and 4‐(4‐methylphenyl)‐3,4‐dihydropyrimido[1,2‐a]benzimidazol‐2‐(1H)‐one, C17H15N3O, (Vb), both form R(8) centrosymmetric dimers via N—H?N hydrogen bonds. The N?N distance is 2.943 (3) Å for (IVa) and 2.8481 (16) Å for (Vb), with the corresponding N—H?N angles being 129 and 167°, respectively. However, in other respects, the supramolecular structures of the two compounds differ. Both compounds contain different C—H?π interactions, in which the C—H?π(centroid) distances are 2.59 and 2.47 Å for (IVa) and (Vb), respectively (the latter being a short distance), with C—H?π(centroid) angles of 158 and 159°, respectively. The supramolecular structures also differ, with a short Br?O distance of 3.117 (2) Å in bromo derivative (IVa), and a C—H?O interaction with a C?O distance of 3.2561 (19) Å and a C—H?O angle of 127° in tolyl system (Vb). The dihydropyrimido part of (Vb) is disordered, with a ratio of the major and minor components of 0.9:0.1. The disorder consists of two non‐interchangeable envelope conformers, each with an equatorial tolyl group and an axial methine H atom. 相似文献
11.
Cai‐Xia Yu Feng Zhao Min Zhou Dan‐Feng Zhi Lei‐Lei Liu 《Acta Crystallographica. Section C, Structural Chemistry》2014,70(3):277-280
In the title coordination polymer, [Zn2(C14H8N2O4)2(C12H10N2)]n, the asymmetric unit contains one ZnII cation, two halves of 2,2′‐(diazene‐1,2‐diyl)dibenzoate anions (denoted L2−) and half of a 1,2‐bis(pyridin‐4‐yl)ethene ligand (denoted bpe). The three ligands lie across crystallographic inversion centres. Each ZnII centre is four‐coordinated by three O atoms of bridging carboxylate groups from three L2− ligands and by one N atom from a bpe ligand, forming a tetrahedral coordination geometry. Two ZnII atoms are bridged by two carboxylate groups of L2− ligands, generating a [Zn2(CO2)2] ring. Each loop serves as a fourfold node, which links its four equivalent nodes via the sharing of four L2− ligands to form a two‐dimensional [Zn2L4]n net. These nets are separated by bpe ligands acting as spacers, producing a three‐dimensional framework with a 4664 topology. Powder X‐ray diffraction and solid‐state photoluminescence were also measured. 相似文献
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Narayan S. Hosmane Chong Zheng 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(5):525-527
The title dimer, bis[1‐cyclopentadienyl‐2‐methyl‐1‐titana‐3‐trimethylsilyl‐2,3‐dicarba‐closo‐hexaborane(6)], [Ti(C5H5)(C6H16B4Si)]2, reveals that the centrosymmetric molecule consists of two bent‐sandwich titanacarboranes bridged by the B—H—Ti bonds. The average bond distances are Ti—B 2.445 (3), Ti—C(cage) 2.334 (2) and Ti—C(Cp) 2.376 (3) Å, and the corresponding bond angles are Cp—Ti—Cp 163.2 (1) and Cp—Ti—Cb (Cb = C2B3 face) 139.9 (1)°; the Ti—H separations are 2.10 (2) and 2.19 (2) Å. 相似文献
14.
The orthorhombic crystal structure of [Co2(CO)6(μ‐CO)(μ‐C4O2H2)] ( 1 ) was determined at 150 K (Fig. 1). Two C−H⋅⋅⋅O bonds connect the molecules, forming waving ribbons along the b axis. The experimental electron density, determined with the aspherical‐atom formalism, was analyzed with the topological theory of molecular structure. The presence of the Co−Co bond critical point indicates for the first time the existence of a metal−metal bond in a system with bridged ligands. The bond critical properties of the intramolecular bonds and of the intermolecular interactions show features similar to those found in [Mn2(CO)10], confirming our previously established bonding classification for organometallic and coordination compounds. 相似文献
15.
Coordinatively Unsaturated Diiron Complexes: Synthesis and Crystal Structures of [Fe2(CO)4(μ‐H)(μ‐PtBu2)(μ‐Ph2PCH2PPh2)] and [Fe2(CO)4(μ‐CH2)(μ‐H)(μ‐PtBu2)(μ‐Ph2PCH2PPh2)] [Fe2(μ‐CO)(CO)6(μ‐H)(μ‐PtBu2)] ( 1 ) reacts spontaneously with dppm (dppm = Ph2PCH2PPh2) to give [Fe2(μ‐CO)(CO)4(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 2 c ). By thermolysis or photolysis, 2 c loses very easily one carbonyl ligand and yields the corresponding electronically and coordinatively unsaturated complex [Fe2(CO)4(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 3 ). 3 exhibits a Fe–Fe double bond which could be confirmed by the addition of methylene to the corresponding dimetallacyclopropane [Fe2(CO)4(μ‐CH2)(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 4 ). The reaction of 1 with dppe (Ph2PC2H4PPh2) affords [Fe2(μ‐CO)(CO)4(μ‐H)(μ‐PtBu2)(μ‐dppe)] ( 5 ). In contrast to the thermolysis of 2 c , yielding 3 , the heating of 5 in toluene leads rapidly to complete decomposition. The reaction of 1 with PPh3 yields [Fe2(CO)6(H)(μ‐PtBu2)(PPh3)] ( 6 a ), while with tBu2PH the compound [Fe2(μ‐CO)(CO)5(μ‐H)(μ‐PtBu2)(tBu2PH)] ( 6 b ) is formed. The thermolysis of 6 b affords [Fe2(CO)5(μ‐PtBu2)2] and the degradation products [Fe(CO)3(tBu2PH)2] and [Fe(CO)4(tBu2PH)]. The molecular structures of 3 , 4 and 6 b were determined by X‐ray crystal structure analyses. 相似文献
16.
The potassium salt of the [1‐H2N‐2‐F‐closo‐1‐CB11H10]– anion ( 1 ) was obtained from an insertion reaction of Li3[7‐H2N‐nido‐7‐CB10H10] with BF3 · OEt2. Anion 1 was protonated to the neutral species 1‐H3N‐2‐F‐closo‐1‐CB11H10 (H 1 ) and it was iodinated with ICl to the [1‐H2N‐2‐F‐closo‐1‐CB11I10]– anion ( 2 ). All species were characterized by multinuclear NMR, IR, and Raman spectroscopy as well as by elemental analysis. The structure of H 1· (CH3)2CO was studied by single‐crystal X‐ray diffraction and the experimentally determined bond lengths are compared to values derived from density functional calculations. 相似文献
17.
Rafa Petrus Piotr Sobota 《Acta Crystallographica. Section C, Structural Chemistry》2012,68(10):m275-m280
The zinc alkoxide molecules in di‐μ3‐ethanolato‐diethyltetrakis(μ2‐2‐methyl‐4‐oxo‐4H‐pyran‐3‐olato‐κ3O3,O4:O3)tetrazinc(II), [Zn4(C2H5)2(C2H5O)2(C6H5O3)4], (I), and bis(μ3‐2‐ethoxyphenolato‐κ4O1,O2:O1:O1)bis(μ2‐2‐ethoxyphenolato‐κ3O1,O2:O1)bis(μ2‐2‐methyl‐4‐oxo‐4H‐pyran‐3‐olato‐κ3O3,O4:O3)bis(2‐methyl‐4‐oxo‐4H‐pyran‐3‐olato‐κ2O3,O4)tetrazinc(II) toluene disolvate, [Zn4(C6H5O3)4(C8H9O2)4]·2C7H8, (II), lie on crystallographic centres of inversion. The asymmetric units of (I) and (II) contain half of the tetrameric unit and additionally one molecule of toluene for (II). The ZnII atoms are four‐ and six‐coordinated in distorted tetrahedral and octahedral geometries for (I), and six‐coordinated in a distorted octahedral environment for (II). The ZnII atoms in both compounds are arranged in a defect dicubane Zn4O6 core structure composed of two EtZnO3 tetrahedra and ZnO6 octahedra for (I), and of four ZnO6 octahedra for (II), sharing common corners. The maltolate ligands exist mostly in a μ2‐bridging mode, while the guetholate ligands prefer a higher coordination mode and act as μ3‐ and μ2‐bridges. 相似文献
18.
Syntheses of Halogenated Polyhedral Phosphaboranes: Crystal Structure of conjuncto‐3,3′‐(closo‐1,2‐P2B4Br3)2
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Willi Keller 《无机化学与普通化学杂志》2017,643(8):517-522
Co‐pyrolysis of B2Br4 with PBr3 at 480 °C gave, in addition to the main product closo‐1,2‐P2B4Br4, conjuncto‐3,3′‐(1,2‐P2B4Br3)2 ( 1 ) and the twelve‐vertex closo‐1,7‐P2B10Br10 ( 2 ), both in low yields. X‐ray structure determination for 1 [triclinic, space‐group P1 with a = 7.220(2) Å, b = 7.232(2) Å, c = 8.5839(15) Å, α = 97.213(15)°, β = 96.81(2)°, γ = 94.07(2)° and Z = 1] confirmed that 1 adopts a structure consisting of two symmetrically boron–boron linked distorted octahedra with the bridging boron atoms in the 3,3′‐positions and the phosphorus atoms in the 1,2‐positions. The intercluster 2e/2c B–B bond length is 1.61(3) Å. The shortest boron–boron bond within the cluster framework is 1.68(2) Å located between the boron atoms antipodal to the phosphorus atoms. The icosahedral phosphaborane 2 was characterized by 11B‐11B COSY NMR spectroscopy showing cross peaks indicative for the isomer with the phosphorus atoms in 1,7‐positions. Both the X‐ray data of 1 and the NMR spectroscopic data of 1 and 2 give further evidence for the influence of an antipodal effect of heteroatoms to cross‐cage boron atoms and, vice versa, of an additional shielding of the phosphorus atoms caused by B‐Hal substitution at the boron positions trans to phosphorus. 相似文献
19.
Syntheses and Crystal Structures of new Amido- und Imidobridged Cobalt Clusters: [Li(THF)2]3[Co3(μ2-NHMes)3Cl6] (1), [Li(DME)3]2[Co18(μ4-NPh)3(μ3-NPh)12Cl3] (2), [Li(DME)3]2[Co6(μ4-NPh)(μ2-NPh)6(PPh2Et)2] (3), and [Li(THF)4][Co8(μ3-NPh)6(μ2-NPh)3(PPh3)2] (4) The reactions of cobalt(II)-chloride with the lithium-amides LiNHMes and Li2NPh leads to an amido-bridged multinuclear complex [Li(THF)2]3[Co3(μ2-NHMes)3Cl6] ( 1 ) as well as to the imido-bridged cobalt cluster [Li(DME)3]2[Co18(μ4-NPh)3(μ3-NPh)12Cl3] ( 2 ). In the presence of tertiary phosphines two imido-bridged cobalt clusters [Li(DME)3]2[Co6(μ4-NPh)(μ2-NPh)6(PPh2Et)2] ( 3 ) and [Li(THF)4][Co8(μ3-NPh)6(μ2-NPh)3(PPh3)2] ( 4 ) result. The structures of 1 – 4 were characterized by X-ray single crystal structure analysis. 相似文献
20.
DFT‐calculations of the geometries of the closo‐anion [B11H11]2– in its ground state and in the transition state of its skeletal rearrangement and of the protonated species [B11H12]– in its ground state were performed at the B3LYP/6‐31++G(d,p) level. The corresponding NMR shifts were computed on the basis of the optimized geometry by the GIAO method at the same level. Calculated and observed NMR data are in good agreement and thus prove the structure of [B11H12]–, previously deduced from 2 D‐NMR spectra. The addition of water, ethanol, and pyridine to [B11H12]– at low temperature gave the nido‐species [B11H13(OH)]–, [B11H13(OEt)]–, and [B11H12(py)]–, respectively. The structures of these anions were investigated by NMR methods and the last two of them by crystal structure analyses of appropriate salts. The course of the addition reactions can be rationalized on the basis of the structurally characterized reaction components. 相似文献