Synthese, Spektren und Kristallstruktur von cis-Monobenzylmononitrotetrahydro-closo-hexaborat(2-) / Synthesis, Spectra and Crystal Structure of cis-Monobenzylmononitrotetrahydro-closo-hexaborate(2-)

1999 ◽  
Vol 54 (10) ◽  
pp. 1219-1221 ◽  
Author(s):  
C. Drewes ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Electrochemical Oxidation ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Dichloromethane Solution ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir And Raman

By electrochemical oxidation of (n-Bu4N)[B6H5Hfac(CH2Ph)] in the presence of nitrite ions in dichloromethane solution cis-[B6H4(CH2Ph)(N O2)]2- is formed. X-ray diffraction analysis has been performed on a single crystal of cis-(Ph4P)2[B6H4(CH2Ph)(NO2)] HO2CH3CN (triclinic, space group Pl̅ a = 11.338(5), b = 11.377(5), c = 21.081 (5) Å, α = 93.727(5), ß = 98.872(5), γ = 105.926(5)°, Z = 2). The 11B NMR spectrum is consistent with a disubstituted octahedral B6 cage with local C2v symmetry. The IR and Raman spectra exhibit characteristic CH, NO2, BN, BH and B6 vibrations.

Darstellung, 11B-NMR- und Schwingungsspektren von c/s-Monoethylmononitrotetrahydro- c/050-hexaborat(2-) sowie Kristallstruktur von cis (Ph4As)2[B6H4(C2H5)(NO2)] / Synthesis, 11B NMR and Vibrational Spectra of cis-Monoethylmononitrotetrahydroc-closo-hexaborate(2-) and Crystal Structure of cis-(Ph4As)2[B6 H4 (C2H5 )(NO2)]

1999 ◽  
Vol 54 (6) ◽  
pp. 772-776 ◽  
Author(s):  
C. Drewes ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Vibrational Spectra ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Dichloromethane Solution ◽  
Triclinic Space Group ◽  
X Ray ◽  
11B Nmr ◽  
Ir And Raman

By electrochemical oxidation of (n-Bu4N)[B6H5Hfac(C2H5)] in the presence of nitrite ions and of the base DBU in dichloromethane solution cis-[B6H4(C2H5)(NO2)]2- is formed. X-ray diffraction analysis has been performed on a single crystal of cis-(Ph4 As)2[B6H4(C2H5)(NO2)] (triclinic, space group P1; a = 10.673(4). b = 10.907(4), c = 21.237(4) A, α = 80.789(4), β = 83.117(4), γ = 66.548(2)°, Z = 2). The 11B NMR spectrum is consistent with a disubstituted octahedral B6 cage with local Cs symmetry. The IR and Raman spectra exhibit characteristic CH3, CH2, NO2, BN, BH and B6 vibrations

Schwingungsspektren und Normalkoordinatenanalysen der Dioxoosmate( VI) trans-[OsO2(CN)4]2-, trans-[OsO2(CN)2(0H )]22- und trans-[OsO2(CN)2(OCH3)]22 sowie Kristallstruktur von trans-(Ph3PNPPh3)2[OsO2(CN)2(OCH3)]2 / Vibrational Spectra and Normal Coordinate Analysis of the Dioxoosmates(VI) trans-[OsO2(CN)4]2-, trans-[OsO2 (CN)2(OH)]22- and trans-[OsO2(CN)2(OCH3]22- , and Crystal Structure of trans-(Ph3PNPPh3)2[OsO2(CN)2(OCH3)]2

1999 ◽  
Vol 54 (9) ◽  
pp. 1109-1115
Author(s):  
A. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Vibrational Spectra ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir And Raman

The crystal structure of trans-(Ph3PNPPh3)2[OsO2(CN)2(OCH3)]2 (triclinic, space group P1̄, a = 11.816(2), b = 13.480(3), c = 13.610(5) Å, α = 83.46(2), ß = 77.09(2), γ = 71.06(2)°, Z = 1) has been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra of the (n-Bu4N)-salts of trans-[OsO2(CN)4]2- (1), trans-[OsO2(CN)2(OH)]22- (2) and trans-[OsO2(CN)2(OCH3)]22- (3) were measured at room temperature. Based on the molecular parameters of the X-ray determination normal coordinate analyses have been performed and the vibrations are assigned. The valence force constants of 1 are fd(Os=O) = 6.5, fd(Os-C) = 2.62 and fd(C≡N ) = 16.85 mdyn/A, of 2 and 3 are fd(Os=O) = 6.7, fd(Os-C) = 2.55 and fd(C≡N ) = 16.95 mdyn/Å. fd(Os-O) ranges from 2.0 - 2.2 and for the methoxy bridge is fd(C-O) = 4.00 mdyn/Å

Darstellung, 11B-, 13C-NMR- und Schwingungsspektren von Cs2[B6Cl5(p-C6H4(NI-I2))] sowie Kristallstruktur von (Ph4P)2[B6Cl5(p-C6H4(NH2))]·2CH3CN · 0,5 Et2O / Preparation, 11B, 13C NMR and Vibrational Spectra of Cs2[B6Cl5(p-C6H4(NH2))] and Crystal Structure of (Ph4P)2[B6Cl5(p-C6H4(NH2))]· 2CH3CN · 0.5 Et2O

2001 ◽  
Vol 56 (1) ◽  
pp. 85-89
Author(s):  
S. Zander ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
13C Nmr ◽  
Vibrational Spectra ◽  
Amino Derivative ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Triclinic Space Group ◽  
X Ray

Abstract By reduction of [B6Cl5(p-C6H4 (NO2))]2- with hydrazine in the presence of Raney nickel in dichlorom ethane solution the amino derivative [B6Cl5(p-C6H4(NH2)]2-is formed. X -ray diffraction analysis has been performed on a single crystal of (Ph4P)2[B6Cl5(p-C6H4(NH2] ·2CH3CN-0,5Et2O(triclinic, space group P1̅, a = 12.870(6), b = 12.9406(5), c = 35,870(7) Å , a = 91,63(4), ß = 93,22(7), γ = 98,04(8)°, Z = 2). The 11B NMR spectrum is consistent with a monosubstituted B6 cluster. The IR and R am an spectra exhibit characteristic BB, CH , CC, and NH vibrations, respectively.

Darstellung, spektroskopische Charakterisierung und Kristallstruktur von Dicyclopentadienylcobalt-hexahydro-closo-hexaborat [(C5H5)Co(C5H4)B6H5Hfac]/ Synthesis, Spectroscopic Characterization and Crystal Structure of Dicyclopentadienyl- cobalt-hexahydro-closo-hexaborate [(C5H5)Co(C5H4)B6H5Hfac]

1998 ◽  
Vol 53 (8) ◽  
pp. 819-822 ◽  
Author(s):  
T. Schaper ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Raman Spectra ◽  
Spectroscopic Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
Ir And Raman

Abstract By reaction of [B6H6Hfac]- with cobaltocene in acetonitrile [(C5H5)Co(C5H4)B6H5Hfac] is formed. Its crystal structure has been determined by single crystal X-ray diffraction analysis (monoclinic, space group P21/n with a = 9.786(2), b = 9.726(2), c = 13.938(2) A, β = 107.2850(3)°, Z = 4). The B6 octahedron is slightly compressedoin the direction of the B-C bond by about 1%, with B-B bond lengths between 1.69 and 1.87 A. The 11B NMR spectrum exhibits a 1:4:1 pattern of a monosubstituted B6 cage. In the IR and Raman spectra characteristic B-H vibrations are observed.

Schwingungsspektrum und Kristallstruktur des fünffach-koordinierten cis-Dioxo-dipicolinato-vanadat(V)-Anions / Vibrational Spectrum and Crystal Structure of the cis-Dioxo-dipicolinato-vanadium(V) Anion

1978 ◽  
Vol 33 (3) ◽  
pp. 265-267 ◽  
Author(s):  
Bernhard Nuber ◽  
Johannes Weiss ◽  
Karl Wieghardt
Keyword(s):  
Crystal Structure ◽  
Raman Spectrum ◽  
Vibrational Spectrum ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Distorted Trigonal Bipyramid ◽  
Ir And Raman

Abstract cis-Dioxo-dipicolinato-vanadate(V), Crystal Structure, IR, Raman The crystal structure of Cs[V(O)2(dipic)]·H2O (dipic = pyridine-2,6-dicarboxylate) has been determined by single crystal x-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/a, with cell constants a =737.8(3), 6=1917.5(5), c = 792.9(3) pm, β= 94.87(6)°, and Z = 4. The geometry about vanadium is a distorted trigonal bipyramid containing a cis-dioxo moiety (∢ O-V-O 109.9(3)°, V=O bond lengths 161.0(6) and 161.5(6) pm). Vibrational absorptions νs(V - 0) and νas(V=O) were found at 956 and 947 cm-1 in the IR and Raman spectrum, resp.

Darstellung und 11B-NMR-Spektrum von Heptabromo-closo-heptaborat, [B7Br7]2- sowie Kristallstruktur von [(C5H5N)2CH2][B7Br7] / Preparation and 11B NMR Spectrum of Heptabromo-closo-heptaborate, [B7Br7]2-, and the Crystal Structure of [(C5H5N)2CH2][B7Br7]

1996 ◽  
Vol 51 (5) ◽  
pp. 744-746 ◽  
Author(s):  
A. Franken ◽  
H. Thomsen ◽  
W. P reetz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Alkaline Solution ◽  
Intensity Ratio ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
11B Nmr

By reaction of conjuncto-[B6H6-B6H6]2- in alkaline solution with excess bromine the heptabromo-closo-heptaborate, [B7Br7]2 is formed. The crystal structure of [(CsH3N)2CH2][B7Br7] has been determined by single crystal X-ray diffraction analysis (monoclinic, space group P21/a with a = 15.0843(14), b = 9.8882(14), c = 17.057(2) Å, β = 114.039°(7)). In accordance with the D5h point symmetry, the anion shows two singlets at -23.3 and -0.1 ppm with the intensity ratio 2:5 in its 11B NMR spectrum.

Die Kristallstruktur des Tetraphenylphosphonium-Monoiodohexahydroc/ oso-Hexaborats [P(C6H5)4][B6H6I] / The Crystal Structure of Tetraphenylphosphonium Monoiodohexahydro-closo-hexaborate [P(C6H5)4][B6H6I]

1994 ◽  
Vol 49 (12) ◽  
pp. 1809-1812 ◽  
Author(s):  
W. Preetz ◽  
D. Sonnak
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The crystal structure of [P(C6H5)4][B6H6I] has been determined by single crystal X-ray diffraction analysis; triclinic, space group P1 with a = 7.5137(9), b = 12.623(2), c = 13.6363(13) Å, α = 87.787(13)°, β = 83.836(13)°, γ = 88.156(10)°. The additional H atom could be refined with B-H distances of 1.13 to 1.31 A above one of the facettes of the B6 octahedron opposite to the I substituent.

Darstellung und spektroskopische Charakterisierung von (η3-Hexahydro-closo-hexaborato)phenylquecksilber(1-) [Hg(η3-B6H6)Ph] sowie Kristallstruktur von [PPh4][Hg(η3-B6H6)Ph] / Preparation and Spectroscopic Characterization of (η3-Hexahydro-closo-hexaborato)phenylmercury(1 -) [Hg(η3-B6H6)Ph]- and Crystal Structure of [PPh4][Hg(η3-B6H6)Ph]

1997 ◽  
Vol 52 (1) ◽  
pp. 57-60 ◽  
Author(s):  
T. Schaper ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Spectroscopic Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Lower Field ◽  
Nmr Spectrum ◽  
X Ray ◽  
Ir And Raman

By reaction of [B6H7]- with PhHg(CH3COO) in dichloromethane [Hg(η3-B6H6)Ph]- is formed. The crystal structure of [PPh4][Hg(η3-B6H6)Ph] has been determined by single crystal X-ray diffraction analysis; monoclinic space group P 21/c with a = 9.567(5) Å, b = 22.213(5) Å, c = 14.296(5) Å, β = 94.484(5)°. The 11B NMR spectrum exhibits a doublet at -9.9 ppm shifted to lower field as compared with [B6H7]- and the 199Hg NMR spectrum a singlet at -74.5 ppm. In the IR and Raman spectra characteristic B-H vibrations are observed

Darstellung, 11 B-NMR- und Schwingungsspektren von cis-Dinitrotetrahydro-closo-hexaborat(2–), cis-[B6H4( NO2)2]2- sowie Kristallstruktur von cis-Cs2[B6H4(NO2)2] / Preparation, 11 B NMR and Vibrational Spectra of cis-Dinitrotetrahydro-closo-hexaborate(2–),cis-[B6H4(NO2)2]2-, and the Crystal Structure of cis-Cs2[B6H4(NO2)2]

1995 ◽  
Vol 50 (7) ◽  
pp. 1030-1034 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Dichloromethane Solution ◽  
X Ray ◽  
Diethylaminoethyl Cellulose ◽  
Ir And Raman

By electrochemical oxidation of [B6H6,]2 in the presence of nitrite ions and of the base DBU in dichloromethane solution apart from [B6H5 (NO2)]2- and [B6H5(NO)B 6H5]3- the dinitro anion cis-[B6H4( NO2)2]2- is formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of the Cs salt has been determined from single crystal X-ray diffraction analyses. cis-Cs2[B6H4 ( NO2)2] is tetragonal, space group P4̄21 m with a = 10.0656(4), c = 11.0127(13) Å. The 11B NMR spectrum is consistent with a disubstituted octahedral B6 cage with local C2v symmetry. The IR and Raman spectra exhibit characteristic NO2, B - H and B6 vibrations.

Darstellung, 11B-NMR- und Schwingungsspektren von μ-Amido-bis(hexahydro-closo-hexaborat)(1-), und Kristallstruktur von [As(C6H5)4][B6H6(NH2)B6H6] / Preparation, 11B NMR and Vibrational Spectra of μ-Amido-bis(hexahydro-closo-hexaborate)(1-) and Crystal Structure of [As(C6H5)4][B6H6(NH2)B6H6]

1995 ◽  
Vol 50 (5) ◽  
pp. 767-771 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Neutral Medium ◽  
X Ray Diffraction ◽  
Aqueous Alkaline Solution ◽  
Nmr Spectrum ◽  
Triclinic Space Group ◽  
X Ray ◽  
11B Nmr ◽  
Brønsted Base ◽  
Ir And Raman

Abstract By reduction of [B6H3(NO)B6H5]3- with Fe2+ in aqueous alkaline solution [B6H3(NH2)B6H3]3- is formed. It reacts as a Brönsted base and becomes protonated in neutral medium to give the mono anion [B6H6(NH2)B6H 6]-. The crystal structure of the salt [As(C6H3)4][B6H6(NH2)B6H6] has been determined by single crystal X-ray diffraction analysis; triclinic space group P1̄ with a = 8.284(2), b = 12.619(2), c = 15.5 4 3 (3 )Å and α = 69.193(13)°; β = 88.59(2)°, γ = 87.24(2)°. The 11B NMR spectrum is consistent with mono hetero substituted octahedral B6 cages with local C4v symmetry. The IR and Raman spectra exhibit characteristic N-H , B-H and B6 vibrations.

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