Darstellung, 11B-, 13C-, 1H-NMR-Spektren und Schwingungsspektren von 1,2-Xylylen-pentahydro-closo-hexaborat,cis-[B6H5(CH2)2C6H4]- , sowie Kristallstrukturen von cis-[P(C6H5)4][B6H5(CH2)2C6H4] und cis-[(n-C4H9)4N][B6H5(CH2)2C6H4] / Preparation, 11B, 13C, 1H NMR Spectra and Vibrational Spectra of 1,2-Xylylene-pentahydro-closo-hexaborate, cis-[B6H5(CH2)2C6H4]-, and the Crystal Structures of cis-[P(C6H5)4][B6H5(CH2)2C6H4] and cis-[(n-C4H9)4N ][B6H5(CH2)2C6H4]

1996 ◽  
Vol 51 (5) ◽  
pp. 691-697 ◽  
Author(s):  
W. Lübbe ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Diethylaminoethyl Cellulose

By reaction of [B6H6]2- with ω,ω′-dibromo-o-xylene in acetonitrile the 1,2-xylylenepentahydro-closo-hexaborat, cis-[B6H5(CH2)2C6H4]- , is formed. The new ansa compound has been separated from excess [B6H6]2- and other reaction products by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of cis-[P(C6H5)4][B6H5(CH2)2C6H4] (I) and as-[(n-C4H9)4N][B6H5(CH2)2C6H4] (II) have been determined by single crystal X-ray diffraction analysis: I is monoclinic, space group P 21/n with a = 13.715(5), b = 11.118(1) and c = 19.702(2) Å, β = 103.47(2)°; II is orthorhombic with a = 10.204(7), b = 13.352(4) and c = 20.824(8) Å. The 11B NMR spectrum confirms the structure with a hetero disubstituted octahedral B6 cage with local C2v symmetry. The 13C and 1H NMR spectra have been assigned in term of such a configuration. The IR and Raman spectra exhibit characteristic CH, BH, BC, B6 and arene vibrations.

Darstellung, 11B-, 13C-, 1H-NMR- und Schwingungsspektren von 1.2-Trimethylenpentahydro-closo-Hexaborat(1 - ) , cis - [B6H5(CH2)3]- und 1.2-Tetramethylenpentahydro-closo-Hexaborat(1-), cis-[B6H5(CH2)4]- sowie Kristallstrukturen von [P(C6H5)4][B6H5(CH2)3] und [P(C6H5)4][B6H5(CH2)4] / Preparation, 11B, 13C, 1H NMR and Vibrational Spectra of 1.2-Trim ethylenepentahydro-closo-hexaborate(1-), cis-[B6H5(CH2)3]-, and 1.2-Tetramethylenepentahydro-closo-hexaborate(1-), cis-[B6H5(CH2)4]-, and the Crystal Structures of [P(C6H5)4][B6H5(CH2)3] and [P(C6H5)4][B6H5(CH2)4]

1994 ◽  
Vol 49 (8) ◽  
pp. 1115-1122 ◽  
Author(s):  
W. Lübbe ◽  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
1H Nmr ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Triclinic Space Group ◽  
Space Group ◽  
H Nmr ◽  
Diethylaminoethyl Cellulose

By reaction of [B6H6]2- with diiodopropane or diiodobutane in dichloromethane the 1,2- rimethylene-pentahydro-closo-hexaborate(1-), cis-[B6H5(CH2)3]-, and the 1,2-tetra-methylene- entahydro-closo-hexaborate(1-), dv-[B6H5(CH2)4]- are obtained, respectively. The compounds were separated from excess [B6H6]2- by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of [P(C6H5)4][B6H5(CH2)3] (I) and [P(C6H5)4][B6H3(CH2)4] (II) have been determined by single crystal X-ray diffraction analy­sis: I is triclinic, space group P1̅ with a = 7,388(2), b = 12,254(2), c = 14,415(2) Å, α = 85,638(12)°, β= 84,06(2)°, γ = 85,13(2)°; II is monoclinic, space group P21/c with a =9,7855(10), b = 11,0793(10), c = 25,2386(10) Å, β= 2,491(10)°. The 11B NMR spectra of oth compounds reveal the feature of a cis-disubstituted octahedral B6 cage. The 13C NMR pectrum of I exhibits a quartet at 15,46 ppm with 1J(C,B) = 121,7 Hz (B-CH2) and a triplet at 37,98 ppm with 1J(C,H) = 124,4 Hz (CH2). For II a quartet at 12,89 ppm with 1J(C,B) = 105,5 Hz (B-CH2) and a triplet at 30,00 ppm with 1J(C,H) = 124,4 Hz (CH2) are observed. In the 1H NMR spectrum of I two multiplets at 0,73 and 1,90 ppm of the CH2 groups and two singlets at 2,23 and -3,71 ppm of the BH fragments are bserved; the signals of the CH2 groups of II are at 0,60 and 1,35 ppm and of the BH fragments at 2,15 and -4,81pm,respectively. The IR and Raman spectra exhibit five very strong CH stretching bands between 2807 and 2938 cm-1 in case of I and between 2817 and 2889 cm 1 in case of II.

scholarly journals Darstellung, 11B-, 13C-, 1H-NMR- und Schwingungsspektren von μ-Dimethylen-bis-hexahydro-closo-hexaborat, [B6H6(CH2)2B6H6]2-, sowie Kristallstrukturen von [As(C6H5)4]2[B6H6(CH2)2B6H6]·[(CH3)2CO] und [P(C6H5)4]2[B6H6(CH2)2B6H6]·[C2H5OH]/Preparation, 11B , 13C, 1H NMR and Vibrational Spectra of μ-Dimethylene-bis-hexahydro-closo-hexaborate, [B6H6(CH2)2B6H6]2- , and the Crystal Structures of [As(C6H5)4]2[B6H6(CH2)2B6H6]·[(CH3)2CO] and [P(C6H5)4]2[B6H6(CH2)2B6H6]·[C2H5OH]

1996 ◽  
Vol 51 (3) ◽  
pp. 363-369 ◽  
Author(s):  
W. Lübbe ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
1H Nmr ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
Nmr Spectrum ◽  
Triclinic Space Group ◽  
Space Group ◽  
H Nmr ◽  
Diethylaminoethyl Cellulose ◽  
Stretching Vibration

Abstract By reaction of [B6H6]2- with dibromoethane in acetonitrile μ-dimethylene-bis-hexahydro-closo-hexaborate(2-), [B6H6(CH2)2B6H6]2-, is formed. The compound was separated from excess [B6H6]2- by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of [As(C6H5)4]2[B6H6(CH2)2B6H6]·[(CH3)2CO] (I) and [P(C6H5)4]2[B6H6(CH2)2B6H6]·[C2H5OH] (II) have been determined by single crystal X-ray analysis: I is triclinic, space group P1̄ with a = 10.264(2), b = 13.804(2) and c = 20.242(2) Å, α = 97.857(10)°, β = 92.734( 11)° and γ = 103.024( 13)°; II is monoclinic, space group P21/n with a = 12.742(2), b = 7.532(2) and c = 26.887(3) Å, β = 95.765( 10)°. The 11B NMR spectrum of this compound reveals the feature of monosubstituted octahedral B6 cages. The 13C NMR spectrum exhibits a triplet at 16.20 ppm with 1J(C,H) = 120.4 Hz. In the 1H NMR spectrum a singulet at 0.72 ppm of the CH2-groups and two singulets at 1.72 and -4.95 ppm of the BH fragments are observed. The IR and Raman spectra exhibit strong CH stretching bands between 2908 and 2789 cm-1, BH stretching bands between 2463 and 2396 cm-1, and the BC stretching vibration at 1144 in the IR and at 1150 cm-1 in the Raman spectrum.

scholarly journals Darstellung, 11B-, 13C-NMR- und Schwingungsspektren der closo-Hexaborate [B6H5(CN)12- und cis-[B6H4(CN)2]2− sowie Kristallstruktur von Cs2[B6H5(CN)] / Preparation, 11B,13C NMR and Vibrational Spectra of the closo-Hexaborates [B6H5(CN)]2- and cis-[B6H4(CN)2]2-, and the Crystal Structure of Cs2[B6H5(CN)]

1993 ◽  
Vol 48 (5) ◽  
pp. 598-602 ◽  
Author(s):  
W. Preetz ◽  
A. Franken ◽  
M. Rath
Keyword(s):  
Crystal Structure ◽  
13C Nmr ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Diethylaminoethyl Cellulose ◽  
Ir And Raman ◽  
C Nmr

By reaction of Cs2[B6H6] with in situ generated dicyanogen in aqueous alkaline solution the monocyanohydrohexaborate Cs2[B6H5(CN)] and the dicyanohydrohexaborate cis-Cs2[B6H4(CN)2] are formed. The compounds have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of Cs2[B6H5(CN)] was determined from single crystal X-ray diffraction analysis; monoclinic, space group P21/a with a = 9.540(8), b = 9.977(3), c = 10.578(2)Å, β = 105.06(2)°. The B6 octahedron is compressed in the direction of the nearly linear B—CN bond by about 5%, with bond lengths between 1.71 and 1.76Å. The "B NMR spectra of the two compounds reveal the features of substituted B6 cages with C4v and C2v point symmetry. In the 13C NMR spectrum of Cs2[B6H5(CN)] a quartet at -139 ppm with 1J(C,B) 92 Hz is observed. The IR and Raman spectra exhibit very strong CN stretching bands for Cs2[B6H5(CN)] at 2149, and for cis-Cs2[B6H4(CN)2] at 2170 cm-1.

Darstellung, Schwingungsspektren und Normalkoordinatenanalyse von bindungsisomeren Halogenoselenocyanatorhenaten(IV) sowie Kristallstrukturen von mer-(Ph4P)2[ReCl3(NCSe)2cis (SeCN)] und mer-(n-Bu4N)2[ReCl3I(NCSe)2cis] / Synthesis, Vibrational Spectra and Normal Coordinate Analysis of Linkage Isomeric Halogenoselenocyanatorhenates(IV) and Crystal Structures of mer-(Ph4P)2[ReCl3(NCSe)2cis (SeCN)] and mer-(n-Bu4N)2[ReCl3I(NCSe)2cis]

1999 ◽  
Vol 54 (10) ◽  
pp. 1222-1228 ◽  
Author(s):  
S. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Exchange Chromatography ◽  
Normal Coordinate Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By treatment of fac-[ReCl3I3]2- with (SeCN)2 indichloromethane fac-[ReCl3(NCSe)3]2- (1), mer-[ReCl3(NCSe)2cis (SeCN)]2- (2) and mer-[ReCl3I(NCSe)2cis]2- (3) are formed which have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of mer-(Ph-P)2[ReCl3(NCSe)2cis(SeCN)] (triclinic, space group Pl̅, a = 16.099(1), b = 16.729(3), c =21.026(2) Å, α = 70.194(10), ß = 73.958(10), γ = 83.929(10)°, Z = 4) and mer-(n-Bu4N)2[ReCl3|(NCSe)2cis] (monoclinic, space group P21/c, a = 11.838(1), b = 12.796(2), c = 30.767(2) Å, ß = 97.419(6)°, Z = 4) have been determined by single crystal X-ray diffraction analysis. Based on the molecular parameters of the X-ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis. The valence force constants are fd(ReN) = 1.79 (1), 1.71 (2), 1.71 (3) and fd(ReSe) = 1.15 (2) mdyn/Å.

Darstellung, 11B-,13C-,1H-NMR- und Schwingungsspektren von Phenylundecahydro-closo-dodecaborat(2-) sowie Kristallstruktur von [As(C6H5)4]2[(C6H5)B12H11] / Preparation, 11B-, 13C-, 1H-NMR- and Vibrational Spectra of Phenylundecahydro-closo-dodecaborate(2-) and Crystal Structure of [As(C6H5)4]2[(C6H5)B12H11]

1997 ◽  
Vol 52 (8) ◽  
pp. 935-938 ◽  
Author(s):  
T Koch ◽  
W Preetz
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Deae Cellulose ◽  
Phenyl Group ◽  
Exchange Chromatography ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Triclinic Space Group ◽  
H Nmr ◽  
Stretching Vibrations

By reaction of [N(C4H9)4]2[B12H12] with chlorotriphenyltin at 170 °C the phenylundecahydro-closo-dodecaborate anion [(C6H5)B12H11]2- is formed which can be isolated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The crystal structure of [As(C6H5)4]2[(C6H5)B12H11] has been determined by single crystal X-ray diffraction analysis; triclinic, space group P1̄ with a = 11,0066(11), b = 11.1371(6), c = 22.236(2) Å, α = 93.040(6), β = 92.981(8), γ = 100.254(6)°, Z = 2. The 11B NMR spectrum reveals the features (1:5:5:1) of a monosubstituated B12 cage with the ipso B atom at - 6.1 and the antipodal B at -17.4 ppm. The 13C and 1H NMR spectra show the characteristic patterns of the phenyl group. The IR and Raman spectra exhibit characteristic BH stretching vibrations between 2464 and 2519 cm-1 and the CC stretching vibrations in the range of 1405 to 1592 cm-1.

Darstellung, 11B-, 13C -, 1H-NMR- und Schwingungsspektren von 2,2' -Bipyridylundecahydro-closo-dodecaborat(1-) sowie Kristallstruktur von (Ph4As)[(2,2′-C10H8N2)B12Hn ]·CH3CN / Synthesis, 11B, 13C, 1H NMR and Vibrational Spectra of 2 ,2'-Bipyridyl-undecahydro-closo-dodecaborate(1-) and Crystal Structure of (Ph4As)[(2 ,2'-C10H8N2)B12H11]-CH3CN

1997 ◽  
Vol 52 (10) ◽  
pp. 1165-1168 ◽  
Author(s):  
T. Koch ◽  
W. Preetz
Keyword(s):  
1H Nmr ◽  
Deae Cellulose ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Ir And Raman

By reaction of (n-Bu4N)2[B12H12] with 2,2′-bipyridine at 190 °C the 2,2′-bipyridyl-undecahydro- closo-dodecaborate anion [(2,2′-C10H8N2)B12H11]− is formed which can be seperated from excess [B12H12]2− by ion exchange chromatography on diethylaminoethyl (DEAE) cellulose. The X-ray structure determination of (Ph4As)[(2, 2′-C10H8N2)B12H11] (monoclinic, space group P21/c with a = 13.3190(9), b = 10.1532(14), c = 28.788(3′) Å, β = 96.761(7)°, Z = 4) reveals that the bipyridyl substituent is bonded via one nitrogen atom. The 11B NMR spectrum exhibits a 1:5:5:1 pattern with ipso-B1 at -0.3, B2-B6 at -14.5, B7-B11 at -15.3 and antipodal-B12 at -15.9 ppm. The 13C and 1H NMR spectra show the characteristic patterns of the bipyridyl group in the range of 124.5 to 158.6 (13C) and 7.4 to 9.6 ppm (1H) respectively. The IR and Raman spectra exhibit characteristic BH stretching vibrations between 2445 and 2568 cm-1 and the stretching of the CC and CN bonds in the range of 1427 to 1619 cm-1 .

A 15N, 13C, and 1H NMR study of reaction products from arylguanidines and chloroformate esters

1991 ◽  
Vol 56 (7) ◽  
pp. 1505-1511 ◽  
Author(s):  
Antonín Lyčka ◽  
Karel Palát
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Reaction Products ◽  
H Nmr ◽  
Nmr Study

The 15N, 13C, and 1H NMR spectra of the reaction products from arylguanidines with two mols of chloroformate esters have been measured. With application of the corresponding 15N isotopomer it has been proved that the reaction products have the structures IIIa-IIIc.

Organometallic oxides: preparation of the cluster [(η-C5Me5)Mo]4O7 by reduction of [(η-C5Me5)MoCl(O)]2(μ-O) or (η-C5Me5)MoCl2(O)

2000 ◽  
Vol 78 (3) ◽  
pp. 383-394
Author(s):  
Frank Bottomley ◽  
Victor Sanchez ◽  
Robert C Thompson ◽  
Olusola O Womiloju ◽  
Zhiqiang Xu
Keyword(s):  
Nmr Spectra ◽  
Chloroform Solution ◽  
X Ray Diffraction ◽  
Broad Resonance ◽  
Nmr Spectrum ◽  
X Ray ◽  
Temperature Range ◽  
H Nmr ◽  
Tributyltin Hydride ◽  
Effective Moment

Reduction of [(η-C5Me5)MoCl(O)]2(μ-O) or (η-C5Me5)MoCl2(O) with sodium or magnesium amalgam, magnesium turnings, or tributyltin hydride produced [(η-C5Me5)Mo]4O7, with [(η-C5Me5)Mo(O)(μ-O)]2 as a co-product. [(η-C5Me5)Mo]4O7 was characterized by X-ray diffraction, mass spectrometry, 1H NMR and IR spectroscopies, and magnetism. Crystals of [(η-C5Me5)Mo]4O7 contained a tetrahedral [(η-C5Me5)Mo]4 unit (Mo-Mo = 2.909 (3) Å) with the Mo4O7 core having the structure Mo4(μ2-O(b))3(µ2-O(c))3(µ3-O(a)) (3). Microcrystalline samples of [(η-C5Me5)Mo]4O7 were paramagnetic over the temperature range 2-300 K, with an effective moment of 1.26 μB at 300 K. [(η-C5Me5)Mo]4O7 was also paramagnetic in chloroform solution, over the temperature range 223-298 K, with an effective moment of 1.43 µB at 298 K. The 1H NMR spectrum showed a broad resonance at 16.3 ppm (Δν 1/2 = 113 Hz) and two narrow resonances at 1.89 ppm and 1.69 ppm (Δν 1/2 = 5 Hz). The magnetism and NMR spectra showed that [(η-C5Me5)Mo]4O7 existed in two forms which were in equilibrium in solution. One form was paramagnetic (S = 1), with the Mo4O7 core having the geometry 3, and the other was diamagnetic (S = 0), with the Mo4O7 core having the geometry 4.Key words: cluster, cyclopentadienyl, molybdenum, oxide, paramagnetism.

Darstellung von Mononitropentahydrohexaborat(2-) und Kristallstruktur von M2[B6H5(NO2)], M = K, Cs / Preparation of Mononitropentahydrohexaborate(2—) and Crystal Structure of M2[B6H5(NO2)], M = K, Cs

1993 ◽  
Vol 48 (12) ◽  
pp. 1727-1731 ◽  
Author(s):  
A. Franken ◽  
W. Preetz ◽  
M. Rath ◽  
K.-F. Hesse
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and the base DBU in dichloromethane solution mononitropentahydrohexaborate [B6H5(NO2)]2- ions are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of the K and Cs salt were determined from single crystal X-ray diffraction analyses. K2[B6H5(NO2)] is monoclinic, space group P21/m with a = 5.953(1), b = 8.059(4), c = 8.906(1) Å, β = 109.553(9)°; Cs2[B6H5(NO2)] is monoclinic, space group P21/a with a = 9.438(6), b = 9.644(7), c = 11.138(9) Å, β = 101.44(9)°. The B6 octahedron is compressed in the direction of the B—NO2 bond by about 5%, with bond lengths between 1.67 and 1.77 A.

Photoreaktionen von Dekacarbonyldirhenium mit Allen und unverzweigten Allenderivaten / Photoreactions of Decacarbonyldirhenium with Allene and Unbranched Derivatives of Allene

1995 ◽  
Vol 50 (4) ◽  
pp. 649-660 ◽  
Author(s):  
Cornelius G. Kreiter ◽  
Wolfgang Michels ◽  
Gerhard Heeb
Keyword(s):  
Nmr Spectra ◽  
Crystal And Molecular Structure ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Oxidative Rearrangement ◽  
Dirhenium Complexes ◽  
Derivatives Of ◽  
By Products

Decacarbonyldirhenium (1) reacts upon UV irradiation with allene (2), 1,2-butadiene (3) and 2,3-pentadiene (4) preferentially by CO substitution and oxidative rearrangement to the corresponding enneacarbonyl-μ-η1:3-endiyl-dirhenium complexes 5, 9, and 15 and to the octacarbonyl-μ-η2:2-allene-dirhenium complexes 6, the stereoisomers 10, 11, and 16. At elevated temperature 5, 9, and 15 loose CO and yield by a reductive rearrangement also the complexes 6, 10, 11, and 16. In addition to these main products, depending upon the allene derivative used, various by-products are obtained.By-products of the reaction o f 1 with 2 are octacarbonyl-μ-η3:3-(2,3-dimethylene-buta-1,4- diyl)dirhenium (7) and μ-η2:2-allene-hexacarbonyl-μ-η1:3-1-propene-1,3-diyl-dirheniurn (8). The photo reaction of 1 with 3 yields, in addition to 9-11, tetracarbonyl-η3-(E-5-ethylidene- 4-methyl-2-cyclopenten-1-yl)rhenium (12) and tetracarbonyl-η3-(Z-5-ethyliden-4- methyl-2-cyclopenten-1-yl)rhenium (13) as a mixture of isomers. 1 and 4 form the by-products tetracarbonyl-η3-(EZ-3-penten-2-yl)rhenium (17), tetracarbonyl-η3-(EE-3-penten-2-yl)rhenium (18) and heptacarbonyl-μ-η1:2:1:2-(4,5-dimethyl-2,6-octadiene-3,6-diyl)dirhenium (19) with an unusually bridging and chelating ligand. The constitutions of the reaction products have been concluded from the IR and 1H NMR spectra. For 19 the crystal and molecular structure has been determined by X-ray diffraction analysis.

Sign in / Sign up

Export Citation Format

Share Document