Darstellung, 11B-, 13C-, 29Si-NMR- und Schwingungsspektren von Trimethylsilylmethyl-hexahydro-closo-hexaborat, [B6H6(CH2Si(CH3)3)]- sowie Kristallstruktur von [P(C6H5)4][B6H6(CH2Si(CH3)3)] / Preparation, 11B, 13C, 29Si NMR and Vibrational Spectra of Trimethylsilylmethyl-hexahydro-clo-hexaborate, [B6H6(CH2Si(CH 3)3)]-and the Crystal Structure of [P(C6H5)4] [B6H6(CH2Si(CH3)3)]

1995 ◽  
Vol 50 (7) ◽  
pp. 1025-1029 ◽  
Author(s):  
J. Baurmeister ◽  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
29Si Nmr ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
Quadrupole Coupling ◽  
Stretching Vibration ◽  
Ir And Raman ◽  
C Nmr

By reaction of [N(C4H9 )4]2 [B6H6] with iodomethyl-trimethylsilane in acetonitrile a solution with trimethylsilylm ethyl-closo-hexaborate(1-)anions, [B6H6 (CH2Si(CH3)3)]-, is formed. The crystal structure of [P(C6H5 )4][B6H6(CH2Si(CH3)3)] has been determined by single crystal X-ray diffraction analysis; monoclinic, space group P21/n with a = 16.140(2), b = 11.646(8), c = 16.731(3) Å, β 109.664(11)°. The 11B NMR spectrum reveals features of a mono hetero substituted octahedral B6 cage. The 13C NMR spectrum exhibits a quartet at +0.18 ppm with 1J(C,H) = 118 Hz for the three methyl groups and a weak multiplet at -0.65 ppm for the methylene bridge due to quadrupole coupling with the boron atoms. In the 29Si NMR spectrum a decet at +2.25 ppm with 2J(C,H ) = 6.9 Hz is observed. The B -C stretching vibration is observed at 1155 cm-1 in the IR and 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, 11B-NMR- und Schwingungsspektren von Aminohexahydro-closo-hexaborat(1–), [B6H6(NH2)]- sowie Kristallstruktur von Cs[B6H6(NH2)] · H2O / Preparation, 11B NMR and Vibrational Spectra of Aminohexahydro-closo-hexaborate(1–), [B6H6(NH2)]-, and the Crystal Structure of Cs[B6H6(NH2)] · H2O

1995 ◽  
Vol 50 (1) ◽  
pp. 11-14 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Vibrational Spectra ◽  
Nmr Spectra ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Aqueous Alkaline Solution ◽  
Nmr Spectrum ◽  
X Ray ◽  
11B Nmr ◽  
Ir And Raman

Aminohexahydro-closo-hexaborate(1–), Crystal Structure, 11B NMR Spectra, Vibrational SpectraBy reduction of [B6H5(NO2)]2- with Fe2+ in aqueous alkaline solution [B6H6(NH2)]- is formed. The compound has been separated by extraction with dichloromethane in the presence of tetrabutylammoniumbromid and precipitated from the organic phase by adding CsCH3COO/C2H5OH. The Crystal structure of Cs[B6H6(NH2)] · H2O has been determined by single crystal X-ray diffraction analysis; monoclinic space group C2 with a = 22.1075(14), b = 6.491(2), c = 5.9570(4) A, β = 100.168(6)°. The 11B NMR spectrum is consistent with a mono-hetero-substituted octahedral B6 cage with local C4v symmetry. The IR and Raman spectra exhibit characteristic N–H, B–H and B6 vibrations.

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, 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.

Darstellung, 11B-, 13C-NMR-und Schwingungsspektren von Cyanomethylhexahydro-closo-Hexaborat(Hexaborat(1-), [B6H6(CH2CN)]– sowie Kristallstruktur von [P(C6H5)4][B6H6(CH2CN)] / Preparation, 11B, 13C NMR and Vibrational Spectra of Cyanomethylhexahydro-closohexaborate(1-), [B6H6(CH2CN)]- and the Crystal Structure of [P(C6H5)4][B6H6(CH2CN)]

1994 ◽  
Vol 49 (4) ◽  
pp. 471-476 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
13C Nmr ◽  
Exchange Chromatography ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Triclinic Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose ◽  
Ir And Raman ◽  
C Nmr

By reaction of [B6H6]2- with chloroacetonitrile in dichloromethane the cyanomethylhexahy-dro-closo-hexaborate(1-), [B6H6(CH2CN)]- is formed. The com pound has been separated from excess [B6H6]2- by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of [P(C6H5)4][B6H6(CH2CN)] has been determined by single crystal X-ray diffraction analysis; triclinic, space group P1 with a = 7.503(3), b = 12.0949(8), c = 14.6572(11) Å α = 79.399(6)°, β = 79.19(2)°, γ = 89.2(2)°. The 11B NMR spectrum is consistent with a mono hetero substituted octahedral B6 cage. In the 13C NMR spectrum of Cs2[B6H5(CH2CN)] a singlet at 131.9 ppm (CN) and a quartet at 2.97 ppm with 1J(C,B) = 54.7 Hz (CH2) are observed. The IR and Raman spectra exhibit a very strong CN stretching band at 2218 cm-1.

Darstellung, 11B-, 13C-, 1H-NMR- und Schwingungsspektren von μ-Methylen-bis-hexahydro-closo-hexaborat, [B6H6(CH2)B6H6]2-, und Kristallstruktur von [As(C6H5)4]2[B6H6(CH2)B6H6]· ½(CH3)2CO / Preparation, 11B- , 13C-, 1H NMR and Vibrational Spectra of μ-Methylene-bis-hexahydro-doso-hexaborate, [B6H6(CH2)B6H6]2- and Crystal Structure of [As(C6H5)4]2[B6H6(CH2)B6H6]· ½(CH3)2CO

1996 ◽  
Vol 51 (4) ◽  
pp. 545-550 ◽  
Author(s):  
W. Lübbe ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Exchange Chromatography ◽  
Nmr Spectrum ◽  
Triclinic Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose ◽  
Stretching Vibration ◽  
Ir And Raman ◽  
C Nmr

Abstract By reaction of [B6H6]2- with dibromomethane in acetonitrile μ-Methylene-bis-hexahydro-closo-hexaborate, [B6H6(CH2)B6H6]2-, is formed which can be separated from excess [B6H6]2- by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of [As(C6H5)4]2[B6H6(C H2)B6H6] · (CH3)2CO has been determined by single crystal X-ray analysis: triclinic, space group P1 with a = 10.779(2), b = 10.8003(12) and c = 23.077(3) Å, a = 99.147(10), β = 91.569(13) and y = 91.288(11)°. The 11B NMR spectrum reveals the features of a monosubstituted octahedral B6 cage. The 13C NMR spectrum exhibits a multiplet at -5.44 ppm. In the 1H NM R spectrum a singlet of the methylene protons at 0.23 ppm and two singlets at 1.97 and -4.52 ppm of the BH fragments are observed. The IR and Raman spectra exhibit strong CH stretching bands between 2873 and 2762 cm-1, BH stretching bands between 2443 and 2403 cm-1, and a BC stretching vibration at 1138 cm-1 in the Raman spectrum.

A New Bis-Tröger's Base: Synthesis, Spectroscopy, Crystal Structure and Isomerization

2006 ◽  
Vol 71 (9) ◽  
pp. 1278-1302 ◽  
Author(s):  
Martin Valík ◽  
Pavel Matějka ◽  
Eberhardt Herdtweck ◽  
Vladimír Král ◽  
Bohumil Dolensky
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Data ◽  
The Other ◽  
X Ray Diffraction ◽  
One Pot ◽  
Molecular Tweezers ◽  
X Ray ◽  
Troger's Base ◽  
Ir And Raman ◽  
C Nmr

A new bis-Tröger's base was prepared from a tetraamine precursor as a mixture of two diastereoisomers. One of the isomers has a chair-like geometry, and the other possesses a boat-like geometry, embodying molecular tweezers. A one-pot preparation of bis-TB isomers and their interconversion under acid conditions was also studied. Structures of both isomers were confirmed by single-crystal X-ray diffraction. Extensive spectroscopic data, including 1H and 13C NMR, IR and Raman spectra of the isomers, are given.

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

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, 11 B-NMR-, Schwingungsspektren und Kristallstruktur von Bis(tetraphenylphosphonium)-2-[2-(2-pyridyl-amino)-pyrid-5-yl]-closo-decaborat, [P(C6H5)4]2[2-{2-(2-(C5H4N)-NH)-(C5H3N)-5}B10H9] / Preparation, 11B NMR, Vibrational Sprectra and Crystal Structure of Bis(tetraphenylphosphonium) 2-[2-(2-Pyridyl-amino)-pyrid-5-yl]-closo-decaborate, [P(C6H5)4]2 [2-{2-(2-(C5H4N)-NH)-(C5H3N)-5}B10H9]

1996 ◽  
Vol 51 (11) ◽  
pp. 1559-1562 ◽  
Author(s):  
C. Nachtigal ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Deae Cellulose ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
Closo Decaborate Anion ◽  
11B Nmr ◽  
Stretching Vibrations ◽  
Ir And Raman

By reaction of [N(C4H9)4]2[B10H10] with 2, 2′-(C5H5N)2NH at 160 °C the 2-[2-(2-pyridylamino)- pyrid-5-yl]-closo-decaborate anion [2-{2-(2-(C5H4N)-NH)-(C5H3N)-5 }B10H9]2− is obtained which can be separated from excess [B10H10]2− by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The crystal structure of [P(C6H5)4]2[2-{2-(2-(C5H4N)- NH)-(C5H3N)-5 }B10H9] has been determinated by single crystal X-ray diffraction analysis: monoclinic, space group P21/n with a = 11.435(3), b = 22.923(2), c = 20.094(4) Å, β = 95,27(2)°, Z = 4. By influence of the substituent the B10 cage is strongly distorted with B-B distances ranging from 1.522 to 2.188 Å. The 11B NMR spectrum reveals the feature (2:1:7) of a B10 cage with the substituent in the 2 position with a downfield shift of the ipso B atom at −20.2 ppm. The IR and Raman spectra exhibit characteristic BH stretching vibrations between 2416 and 2499 cm −1 and the (C-C) and (C-N) stretching vibrations in the range of 1306 to 1584 cm −1 .

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