Synthesis, x-ray crystal structure, and temperature-dependent NMR spectrum of tetraethylammonium (.alpha.-methoxybenzyl)pentacarbonyltungstate

1978 ◽  
Vol 17 (11) ◽  
pp. 3045-3049 ◽  
Author(s):  
Charles P. Casey ◽  
Stanley W. Polichnowski ◽  
Hendrik E. Tuinstra ◽  
Loren D. Albin ◽  
Joseph C. Calabrese
Keyword(s):  
Crystal Structure ◽  
Temperature Dependent ◽  
Nmr Spectrum ◽  
X Ray

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.

Solid state stereochemistry of crown ethers: X-ray crystal structure and 13C NMR studies of the LiNCS complex of 1,4,7,11-tetraoxacyclotetradecane

2000 ◽  
Vol 78 (3) ◽  
pp. 316-321
Author(s):  
G W Buchanan ◽  
A B Driega ◽  
G PA Yap
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crown Ether ◽  
13C Nmr ◽  
Title Complex ◽  
Nmr Studies ◽  
Nmr Spectrum ◽  
X Ray ◽  
Large Amplitude Motion ◽  
C Nmr

The title complex is asymmetric in the crystal due to the spatial orientation of the NCS function. The space group has been determined to be P21 with a = 9.496(3), b = 8.736(3), c = 9.676(3) Å, β = 117.859(5)°, and Z = 2. The solid state 13C NMR spectrum is consistent with the lack of symmetry in the crystal and there is little evidence for large amplitude motion in the macrocycle as determined from the dipolar dephased spectrum.Key words: macrocyclic crown ether, lithium complex.

Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ5-phosphaspiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige 1H-NMR-Spektren: The 7, 8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ).5-phosphaspiro[4.4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable 1H NMR Spectra

1992 ◽  
Vol 47 (6) ◽  
pp. 755-759 ◽  
Author(s):  
Thomas Kaukorat ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Acceptor Interaction ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Donor Acceptor

The 1H NMR spectrum of the spirophosphorane 3 at room temperature indicates dynamic behaviour of the cation. The low-temperature 1H NMR spectra of 3 exhibit two sets of doublets for the protons of the diastereotopic N(CH3)2 groups. The free enthalpy of activation for the dynamic process was determined (58.6 KJ/mole). In the reaction of 3 with sodium tetraphenylborate the crystalline compound, 4, involving the non-coordinating anion, [B(C6H5)4]-, was obtained. The X-ray crystal structure analysis of 4 reveals the presence of a five-membered ring, formally as a result of intramolecular donor-acceptor interaction between the nitrogen atom of the N(CH3)2 group and phosphorus. The geometry at phosphorus deviates somewhat from ideal trigonal bipyramidal.

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

Darstellung, 11B-und 19F-NMR-Spektren des Monofluoropentaiodo- closo-hexaboratanions sowie Kristallstruktur von (CH2Py2)[B6FI5]/ Synthesis, 11B and 19F NMR Spectra of the Monofluoropentaiodo-closo-hexaborate Anion and the Crystal Structure of (CH2Py2)[B6FI5]

1998 ◽  
Vol 53 (8) ◽  
pp. 829-832 ◽  
Author(s):  
H. Thomsen ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
19F Nmr ◽  
Coupling Constant ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
19F Nmr Spectra ◽  
Nmr Spectrum ◽  
X Ray ◽  
Excess Iodine

Abstract By reaction of closo-[B6H5F]2- in alkaline solution with excess iodine the monofluoropentaiodo- closo-hexaborate anion [B6FI5]2- is formed in good yield. The crystal structure of (CH2Py2)[B6FI5] has been determined by single crystal X-ray diffraction analysis (orthorhombic, space group Pnma, a = 13.803(2), b = 11.759(2), c = 13.936(2) Å, Z = 4). The B-F-bond length is 1.41 Å, the B-I distances range from 2.13 to 2.17 Å, the B-B distances from 1.69 to 1.76 A. According to the C4v point symmetry the 11B NMR spectrum of the anion exhibits three singlets at +3.8,-30.1 and-33.3 ppm with the intensity ratio 1:4:1, the 19F NMR spectrum one quartet at -247.6 ppm with the coupling constant 1J (19F, 11B) = 54 Hz.

scholarly journals Effects of Cr Doping and Water Content on the Crystal Structure Transitions of Ba2In2O5

Crystals ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 1548
Author(s):  
Raphael Finger ◽  
Marc Widenmeyer ◽  
Thomas C. Hansen ◽  
Dirk Wallacher ◽  
Stanislav Savvin ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Water Content ◽  
Structural Changes ◽  
Equimolar Amount ◽  
Co2 Conversion ◽  
Temperature Dependent ◽  
X Ray ◽  
Photocatalytic Co2 Conversion ◽  
Cr Doping

Temperature-dependent crystal structure alterations in the brownmillerite-type material Ba2In2O5 play a fundamental role in its applications: i) photocatalytic CO2 conversion; ii) oxygen transport membranes; and iii) proton conduction. This is connected to a reversible uptake of up an equimolar amount of water. In this study, in situ X-ray and neutron diffraction were combined with Raman spectroscopy and solid-state nuclear magnetic resonance experiments to unravel the effects of Cr doping and water content on the crystal structure transitions of Ba2In2O5(H2O)x over a wide temperature range (10 K ≤ T ≤ 1573 K, x < 1). A mixture of isolated and correlated protons was identified, leading to a highly dynamic situation for the protons. Hence, localisation of the protons by diffraction techniques was not possible. Cr doping led to an overall higher degree of disorder and stabilisation of the tetragonal polymorph, even at 10 K. In contrast, a further disordering at high temperatures, leading to a cubic polymorph, was found at 1123 K. Cr doping in Ba2In2O5 resulted in severe structural changes and provides a powerful way to adjust its physical properties to the respective application.

X-Ray Structure and Magnetic Properties of the Tetracupferronato-bis(μ-methoxy)-diiron(III) Complex

1995 ◽  
Vol 50 (11) ◽  
pp. 1587-1590 ◽  
Author(s):  
Yalcin Elerman ◽  
Mehmet Kabak ◽  
Ingrid Svoboda ◽  
Hartmut Fuess ◽  
Klaus Griesar ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Magnetic Susceptibility ◽  
Exchange Interaction ◽  
Monoclinic Space Group ◽  
Antiferromagnetic Exchange ◽  
Temperature Dependent ◽  
Space Group ◽  
X Ray ◽  
Antiferromagnetic Exchange Interaction

The tetracupferronato-bis(μ-methoxy)-diiron(III) complex has been synthesized in acetonitrile and its crystal structure determined. C26H26N8O10Fe2, monoclinic, space group C2/c, a =18.425(3), b = 12.999(2), c = 15.046(3) Å, β = 124.66(2)°,V = 2964(1) Å3, Z = 4, wR(2) = 0.097 from 1491 reflections (F2). Two iron(III) atoms are at special positions in six-fold coordination, bridged by O with a Fe-O-Fe angle of 102.4(1)° and a distance between two iron(III) centers of 3.075(1) Å. Temperature-dependent magnetic susceptibility measurements reveal a antiferromagnetic exchange interaction (J = -14 cm-1) between the iron(III) centers.

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.

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