Darstellung, 11B-NMR-Spektren, Schwingungsspektren und Normalkoordinatenanalyse von conjuncto-Bis-hexahydro-closo-hexaborat, [B6H6-B6H6]2-, sowie Kristallstruktur von [P(C6H5)4]2-conjuncto-[B6H6-B6H6] / Preparation, 11B NMR Spectra, Vibrational Spectra and Normal Coordinate Analysis of conjuncto-Bis-hexahydro-closo-hexaborate, [B6H6-B6H6]2-, and the Crystal Structure of [ P(C6H5)4]2-conjuncto-[B6H6-B6H6]

1996 ◽  
Vol 51 (5) ◽  
pp. 609-618 ◽  
Author(s):  
D. Bublitz ◽  
A. Franken ◽  
W. Preetz ◽  
H. Thomsen
Keyword(s):  
Crystal Structure ◽  
Exchange Chromatography ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Vibrational Coupling ◽  
Nmr Spectrum ◽  
Triclinic Space Group ◽  
Diethylaminoethyl Cellulose ◽  
11B Nmr ◽  
Ir And Raman

By reaction of [B6H6]2- with dibenzoylperoxide in dichloromethane conjuncto-[B6H6- B6H6]2- is formed. The product could be separated from excess [B6H6]2- by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of [P(C6H5)4]2 -conjuncto- [B6H6-B6H6] has been determined by single crystal X-ray diffraction analysis; triclinic, space group P1̄ with a = 10.8315(10), b = 11,2422( 12), c = 20.340(2) Å, α = 91.278° (9), β = 90.178° (9), γ = 105.662°(9). The 11B NMR spectrum reveals three signals with the intensity ratio 1:1:4, for two equivalent moieties of the conjuncto molecule ion with local C4v symmetry. The IR and Raman spectra of the deprotonated Cs salts of the 10B, 11B and their respective D isotopomers of conjuncto-[B6H5-B6H5]4- exhibit characteristic shifts. Using averaged crystallographic data and assuming idealized D4h symmetry, normal coordinate analyses have been performed based on a modified valence force field. With a set of eleven force constants (e.g. fd(BB)conjuncto = 2.9, fd(BB)cage = 1.6 mdyn/Å) very good agreement between observed and calculated frequencies has been achieved. From strong vibrational coupling with the B6 clusters two vibrations result for the conjuncto B-B bond at 1142/1198 and 292/304cm-1 for 11B/10B species, respectively. They can be assigned as anti-phase and in-phase motions of the conjuncto B atoms related to the equatorial B4 planes.

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-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

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, 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 .

Darstellung, 11B-NMR- und Schwingungsspektren von cis-Monocyanomononitrotetrahydro-closo-hexaborat(2-) , as-[B6H4(CN)(NO2)]2- und cis-μ-Nitroso-bis(monocyanotetrahydro-closo-hexaborat)(3-), cis-[(CN)B6H4(NO)B6H4(CN)]3– sowie Kristallstruktur von [As(C6H5)4]2-cis-[B6H4(CN)(NO2)] / Preparation, n=11B-NMR and Vibrational Spectra of cis-Monocyanomononitrotetrahydro-closo-hexaborate(2-) , cis-[B6H4(CN)(NO2)]2-,cis -μ-Nitroso-bis(monocyanotetrahydro-hexaborate)(3-), cis-[(CN)B6H4(NO)B6H4(CN)]3– and the Crystal Structure of [As(C6H5)4]2-cis-[B6H4(CN)(NO2)]

1995 ◽  
Vol 50 (9) ◽  
pp. 1362-1368 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
X Ray ◽  
Diethylaminoethyl Cellulose ◽  
11B Nmr ◽  
Ir And Raman

AbstractBy electrochemical oxidation of [B6H5(CN)]2- in the presence of nitrite ions and of the base DBU in dichloromethane solution cis-[B6H4(CN)(NO2)]2- and cis- [(CN)B6H4(NO)B6H4(CN)]3- are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of the tetraphenylarsonium salt has been determined by single crystal X-ray diffraction analysis. [As(C6H5)4]2-cis-[B6H4(CN)(NO2)] is monoclinic, space group P21/a with a = 20.343(5), b = 10.896(2), c = 21.572(5) A and β = 107.30(2)°. The 11B NMR spectra are consistent with disubstituted octahedral B6 cages with local C2v symmetry. The IR and Raman spectra exhibit characteristic NO2, NO, CN, BH, and B6 vibrations.

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.

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.

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-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.

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