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1.
Anna Laromaine Clara Vias Reijo Sillanp Raikko Kiveks 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(7):o524-o526
In the title compound, 1,2‐(SCH3)2‐1,2‐closo‐C2B10H10 or C4H16B10S2, the methylsulfanyl groups are bonded to the C atoms of the 1,2‐dicarba‐closo‐dodecaborane cage. The Ccage—Ccage distance is 1.8033 (18) Å and the S—Ccage—Ccage—S torsion angle is 1.07 (13)°. The Ccage—Ccage distance is compared with those in other 1,2‐dicarba‐closo‐dodecaborane derivatives. 相似文献
2.
Ulaganathan Venkatasubramanian David Ellis Georgina M. Rosair Alan J. Welch 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(10):o559-o561
The title compound, 1,2‐(COOH)2‐1,2‐closo‐C2B10H10·0.5C2H6O or C4H12B10O4·0.5C2H6O, forms a tetramer by incorporating ethanol (solvent) molecules through hydrogen bonding. Two eight‐membered rings [graph set R(8)] are formed by hydrogen bonding between two carboxylic acid groups, whereas two ten‐membered rings [R(10)] are formed by hydrogen bonding between two carboxylic acid groups and the OH group of an ethanol molecule (solvent). Two crystallographically independent tetramers are present in the crystal structure. 相似文献
3.
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
4.
Reijo Sillanp Jordi Llop Clara Vias Francecs Teixidor Raikko Kiveks 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(8):900-901
In the title compound, (η5‐2,5‐dimethylpyrrolyl)[(7,8,9,10,11‐η)‐7‐methyl‐7,8‐dicarba‐nido‐undecaborato]cobalt(III), [3‐Co{η5‐[2,5‐(CH3)2‐NC4H2]}‐1‐CH3‐1,2‐C2B9H10] or [Co(C3H13B9)(C6H8N)], the CoIII atom is sandwiched between the pentagonal faces of the pyrrolyl and dicarbollide ligands, resulting in a neutral molecule. The C—C distance in the dicarbollide cage is 1.649 (3) Å. 相似文献
5.
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
6.
Pierre Morel Paul Schaffer James F. Britten John F. Valliant 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(12):m601-m604
The title compounds, bis[1,2‐dicarba‐closo‐dodecaboran(12)‐1‐yl]mercury(II) dichloromethane solvate, [Hg(C2B10H11)2]·CH2Cl2, (I), and bis[1,12‐dicarba‐closo‐dodecaboran(12)‐1‐yl]mercury(II) tetrahydrofuran solvate, [Hg(C2B10H11)2]·C4H8O, (II), were prepared in excellent yields using a robust synthetic procedure involving the reaction of HgCl2 with the appropriate monolithiocarborane. X‐Ray analysis of the products revealed strong interactions between the Hg atoms in both complexes and the respective lattice solvent. The distances between the HgII centers and the Cl atoms of the dichloromethane solvent molecule in the ortho‐carborane derivative, (I), and the O atom of the tetrahydrofuran molecule in the para‐carborane complex, (II), are shorter than the sums of the van der Waals radii for Hg and Cl (3.53 Å), and Hg and O (3.13 Å), respectively, indicating moderately strong interactions. There are two crystallographically independent molecules in the asymmetric unit of both compounds, which, in each case, are related by differing relative positions of the cages. 相似文献
7.
Konstantin A. Lyssenko Gennadii V. Grintselev‐Knyazev Mikhail Yu. Antipin Sergey P. Knyazev Valerii N. Kirin Eugenii A. Chernyshev 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(7):827-829
Two phenyl‐substituted carboranes, 3‐phenyl‐1,2‐dicarba‐closo‐dodecaborane(12), C8H16B10, (I), and 1‐phenyl‐1,7‐dicarba‐closo‐dodecaborane(12), C8H16B10, (II), were found to be isostructural. Comparison of the bond angles at the ipso‐C atoms of the phenyl substituent for (I) and (II) [117.71 (3) and 118.45 (10)°, respectively] indicates that electron donation of the carborane cage for B‐ and C‐substituted carboranes is different. 相似文献
8.
Yong Nie Chun‐Hua Hu Qiang‐Jin Wu Shao‐Fang Lu Ruo‐Shui Jin Pei‐Ju Zheng 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(5):536-537
The title compound, [(PPh3)(p‐MeC6H4COO)2RuB10H8], contains an 11‐vertex closo‐type RuB10 cluster fused to two symmetric exopolyhedral Ru—O—C—O—B five‐membered rings. Principal distances include Ru—B 2.010 (5)–2.392 (4) Å and Ru—O 2.218 (5) and 2.222 (2) Å. 相似文献
9.
Three dinuclear copper(I) complexes, [Cu2(µ‐Cl)2(1,2‐(PPh2)2‐1,2‐C2B10H10)2]·2CH2Cl2 ( 1 ), [Cu2(µ‐Br)2(1,2‐(PPh2)2‐1,2‐C2B10H10)2]·2THF ( 2 ) and {Cu2(µ‐I)2[1,2‐(PPh2)2‐1,2‐C2B10H10]2} ( 3 ) have been synthesized by the reactions of CuX (X = Cl, Br and I) with the closo ligand 1,2‐(PPh2)2‐1,2‐C2B10H10. All these complexes were characterized by elemental analysis, FT‐IR, 1H and 13C NMR spectroscopy and X‐ray structure determination. Single crystal X‐ray structure determinations show that every complex contained di‐µ‐X‐bridged structure involving a crossed parallelogram plane formed by two Cu atoms and two X atoms (X = Cl, Br, I). The geometry at the Cu atom was a distorted tetrahedron, in which two positions were occupied by two P atoms of the PPh2 groups connected to the two C atoms of carborane (Cc), and the other two resulted from two X atoms which bridged the other Cu atom at the same time. To the best of our knowledge, this is the first example of copper(I) complexes with 1,2‐diphenylphosphino‐1,2‐dicarba‐closo‐dodecaborane as ligand characterized by X‐ray diffraction. The catalytic property of the complex 3 for the amination of iodobenzene with aniline was also investigated. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
10.
Hong‐Ping Xiao Sai‐Zhen Yang Xin‐Hua Li 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(2):m112-m114
The title compound, [Co2(C12H11N2)2(C12H10N2)(H2O)8][Co(H2O)6](SO4)4·8H2O, consists of bis(4‐pyridyl)ethenedicobalt(II) cations, hexaaquacobalt cations, sulfate anions and water solvent molecules that are linked by hydrogen bonds into a network structure. In the hexaaquacobalt cation, the six water molecules are coordinated in an octahedral geometry to the Co atom, which lies on an inversion centre. The other cation is a 1,2‐bis(4‐pyridyl)ethene‐bridged centrosymmetric dimer, consisting of protonated 1,2‐bis(4‐pyridyl)ethene cations, a bridging 1,2‐bis(4‐pyridyl)ethene ligand and tetraaquacobalt cations. Each Co atom is six‐coordinated by four water molecules and two N atoms from a protonated 1,2‐bis(4‐pyridyl)ethene cation and the bridging 1,2‐bis(4‐pyridyl)ethene ligand, and the geometry around each Co atom is octahedral. 相似文献
11.
Pan
e Naumov Gligor Jovanovski Sheng‐Zhi Hu Il‐Hwan Suh Ibrahim Abdul Razak Suchada Chantrapromma Hoong‐Kun Fun Seik Weng Ng 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(9):1016-1019
The short carbonyl bond in the title compound, [Cu2(C7H4NO3S)4(C3H4N2)4] [Liu, Huang, Li & Lin (1991). Acta Cryst. C 47 , 41–43], is an artifact of disorder in the isothiazol‐3(2H)‐one 1,1‐dioxide part of the 1,2‐benzisothiazol‐3(2H)‐one entity. In the present redetermination, all bond dimensions in the centrosymmetric dinuclear molecule are normal. The five‐coordinate Cu atom shows trigonal–bipyramidal coordination. Hydrogen bonds from the imidazole donor ligand link adjacent molecules into a two‐dimensional layer structure. 相似文献
12.
Tullio Pilati Gianluigi Casalone 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(3):o178-o180
The title diastereoisomers, methyl 5‐(S)‐[2‐(S)‐methoxycarbonyl)‐2,3,4,5‐tetrahydropyrrol‐1‐ylcarbonyl]‐1‐(4‐methylphenyl)‐4,5‐dihydropyrazole‐3‐carboxylate and methyl 5‐(S)‐[2‐(R)‐methoxycarbonyl)‐2,3,4,5‐tetrahydropyrrol‐1‐ylcarbonyl]‐1‐(4‐methylphenyl)‐4,5‐dihydropyrazole‐3‐carboxylate, both C19H23N3O5, have been studied in two crystalline forms. The first form, methyl 5‐(S)‐[2‐(S)‐methoxycarbonyl)‐2,3,4,5‐tetrahydropyrrol‐1‐ylcarbonyl]‐1‐(4‐methylphenyl)‐4,5‐dihydropyrazole‐3‐carboxylate–methyl 5‐(S)‐[2‐(R)‐methoxycarbonyl)‐2,3,4,5‐tetrahydropyrrol‐1‐ylcarbonyl]‐1‐(4‐methylphenyl)‐4,5‐dihydropyrazole‐3‐carboxylate (1/1), 2(S),5(S)‐C19H23N3O5·2(R),5(S)‐C19H23N3O5, contains both S,S and S,R isomers, while the second, methyl 5‐(S)‐[2‐(S)‐methoxycarbonyl)‐2,3,4,5‐tetrahydropyrrol‐1‐ylcarbonyl]‐1‐(4‐methylphenyl)‐4,5‐dihydropyrazole‐3‐carboxylate, 2(S),5(S)‐C19H23N3O5, is the pure S,S isomer. The S,S isomers in the two structures show very similar geometries, the maximum difference being about 15° on one torsion angle. The differences between the S,S and S,R isomers, apart from those due to the inversion of one chiral centre, are more remarkable, and are partially due to a possible rotational disorder of the 2‐(methoxycarbonyl)tetrahydropyrrole group. 相似文献
13.
Maik Finze Dr. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2009,15(4):947-962
The first primary 2‐aminocarba‐closo‐dodecaborates [1‐R‐2‐H2N‐closo‐CB11H10]? (R=H ( 1 ), Ph ( 2 )) have been synthesized by insertion reactions of (Me3Si)2NBCl2 into the trianions [7‐R‐7‐nido‐CB10H10]3?. The difunctionalized species [1,2‐(H2N)2‐closo‐CB11H10] ( 3 ) and 1‐CyHN‐2‐H3N‐closo‐CB11H10 (H‐ 4 ) have been prepared analogously from (Me3Si)2NBCl2 and 7‐H3N‐7‐nido‐CB10H12. In addition, the preparation of [Et4N][1‐H2N‐2‐Ph‐closo‐CB11H10] ([Et4N]‐ 5 ) starting from PhBCl2 and 7‐H3N‐7‐nido‐CB10H12 is described. Methylation of the [1‐Ph‐2‐H2N‐closo‐CB11H10]? ion ( 2 ) to produce 1‐Ph‐2‐Me3N‐closo‐CB11H10 ( 6 ) is reported. The crystal structures of [Et4N]‐ 2 , [Et4N]‐ 5 , and 6 were determined and the geometric parameters were compared to theoretical values derived from DFT and ab initio calculations. All new compounds were studied by NMR, IR, and Raman spectroscopy, MALDI mass spectrometry, and elemental analysis. The discussion of the experimental NMR chemical shifts and of selected vibrational band positions is supported by theoretical data. The thermal properties were investigated by differential scanning calorimetry (DSC). The pKa values of 2‐H3N‐closo‐CB11H11 (H‐ 1 ), 1‐H3N‐closo‐CB11H10 (H‐ 7 ), and 1,2‐(H3N)2‐closo‐CB11H10 (H2‐ 3 ) were determined by potentiometric titration and by NMR studies. The experimental results are compared to theoretical data (DFT and ab initio). The basicities of the aminocarba‐closo‐dodecaborates agree well with the spectroscopic and structural properties. 相似文献
14.
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
15.
Sergiusz Lulinski Janusz Serwatowski 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(5):o301-o303
The structure of the title compound, 2(CH3OCO)C6H4B(OH)2 or C8H9BO4, involves two crystallographically independent conformers, A and B, in a 1:2 ratio; molecules of conformer A are located on a crystallographic mirror plane. The most striking difference between the two independent molecules is the opposite orientation of the methoxycarbonyl groups, while the conformations of the boronic acid groups vary more subtly. Molecules of both types are ordered to produce a specific hydrogen‐bonding network that can be interpreted in terms of a layer lying parallel to (100). Within the layer, B molecules are linked with each other by two different O—H⋯O bonds to form an infinite chain where two centrosymmetric dimeric motifs can be distinguished. 相似文献
16.
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
17.
Robert T. Stibrany Harvey J. Schugar Joseph A. Potenza 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(6):o354-o357
Two of the title compounds, namely (E)‐1,2‐bis(1‐methylbenzimidazol‐2‐yl)ethene, C18H16N4, (Ib), and (E)‐1,2‐bis(1‐ethylbenzimidazol‐2‐yl)ethene, C20H20N4, (Ic), consist of centrosymmetric trans‐bis(1‐alkylbenzimidazol‐2‐yl)ethene molecules, while 3‐ethyl‐2‐[(E)‐2‐(1‐ethylbenzimidazol‐2‐yl)ethenyl]benzimidazol‐1‐ium perchlorate, C20H21N4+·ClO4−, (II), contains the monoprotonated analogue of compound (Ic). In the three structures, the benzimidazole and benzimidazolium moieties are essentially planar; the geometric parameters for the ethene linkages and their bonds to the aromatic groups are consistent with double and single bonds, respectively, implying little, if any, conjugation of the central C=C bonds with the nitrogen‐containing rings. The C—N bond lengths in the N=C—N part of the benzimidazole groups differ and are consistent with localized imine C=N and amine C—N linkages in (Ib) and (Ic); in contrast, the corresponding distances in the benzimidazolium cation are equal in (II), consistent with electron delocalization resulting from protonation of the amine N atom. Crystals of (Ib) and (Ic) contain columns of parallel molecules, which are linked by edge‐over‐edge C—H⋯π overlap. The columns are linked to one another by C—H⋯π interactions and, in the case of (Ib), C—H⋯N hydrogen bonds. Crystals of (II) contain layers of monocations linked by π–π interactions and separated by both perchlorate anions and the protruding ethyl groups; the cations and anions are linked by N—H⋯O hydrogen bonds. 相似文献
18.
Sari Paavola Francesc Teixidor Clara Vias Raikko Kiveks 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(4):m237-m239
The asymmetric unit of the title complex, [PtCl2(C14H38B10P2)]·0.5CH2Cl2 or cis‐[PtCl2{1,2‐(PiPr2)2‐1,2‐C2B10H10}]·0.5CH2Cl2, contains one disordered solvent molecule and two molecules of the complex, in which each PtII atom displays slightly distorted square‐planar coordination geometry. The P atoms connected to the cage C atoms are coordinated to the PtII atom. The Pt—P distances vary slightly [2.215 (3) and 2.235 (4) Å] and the Pt—Cl distances are equal [2.348 (3) and 2.353 (5) Å]. 相似文献
19.
Süheyla
zbey Nesrin Gkhan 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(10):o737-o739
A new type of benzothiazolinone derivative with potential pharmacological activity, viz. 6‐(3,4‐difluorobenzoyl)‐3‐[2‐(4‐pyridyl)ethyl]‐1,3‐benzothiazol‐2(3H)‐one, C21H14F2N2O2S, has been prepared and studied by NMR, IR and single‐crystal X‐ray diffraction techniques. The molecule is not planar, the pyridine and difluorobenzene moieties being located above and below the benzothiazole ring system. The carbonyl O atoms are involved in an intramolecular hydrogen‐bond‐type interaction. 相似文献
20.
V. I. Bregadze S. A. Glazun P. V. Petrovskii Z. A. Starikova A. G. Buyanovskaya R. U. Takazova M. Gielen D. de Vos M. Kemmer M. Biesemans R. Willem 《应用有机金属化学》2004,18(4):191-194
Sodium bis[2‐(3′,6′,9′‐trioxadecyl)‐1,2‐dicarba‐closo‐dodecaborane‐1‐carboxylato]triphenylstannate, [(CH3OCH2CH2OCH2CH2OCH2CH2)‐1,2‐C2B10H10‐9‐COO)2SnPh3]? Na+, compound 1, was synthesized by the 1:1 condensation of triphenyltin(IV) hydroxide with 2‐(3′,6′,9′‐trioxadecyl)‐1,2‐dicarba‐closo‐dodecaborane‐1‐carboxylic acid and crystallized in the presence of sodium bicarbonate. Its structure was determined by spectroscopy, elemental analysis and X‐ray diffraction. The structure of 1 consists of trigonal bipyramidal [Sn(Ph)3(L)2]? anions and Na+ cations coordinated by oxygen atoms of polyoxaalkyl chains of different stannate anions, forming cation–anion chains elongated along the c axis. Compound 1 is significantly more active in vitro against seven tumour cell lines of human origin than 5‐fluorouracil, cis‐platin, carboplatin, and previously reported organotin carboranecarboxylates, but is less active than organotin polyoxaalkylcarboxylates. Copyright © 2004 John Wiley & Sons, Ltd. 相似文献