Crystal structure, and variable temperature proton and carbon-13 NMR spectra of the 9-membered ring complex [Cr(CO)4{E,Z-PPh2CH2C(tBu)NNC(tBu)CH2PPh2}]

1993 ◽  
Vol 462 (1-2) ◽  
pp. 221-224 ◽  
Author(s):  
Sarath D. Perera ◽  
Bernard L. Shaw ◽  
Mark Thornton-Pett ◽  
Jonathan D. Vessey
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
Variable Temperature ◽  
Membered Ring ◽  
Ring Complex

scholarly journals Crystal structure and solvent-dependent behaviours of 3-amino-1,6-diethyl-2,5,7-trimethyl-4,4-diphenyl-3a,4a-diaza-4-bora-s-indacene

2017 ◽  
Vol 73 (3) ◽  
pp. 378-382
Author(s):  
Lijing Yang ◽  
Brett Drew ◽  
Ravi Shekar Yalagala ◽  
Rameez Chaviwala ◽  
Razvan Simionescu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Fluorescence Spectroscopy ◽  
Title Compound ◽  
Nmr Spectra ◽  
Membered Ring ◽  
The Other ◽  
Time Dependent ◽  
H Nmr ◽  
The Mean ◽  
Over Time

In the title compound (3-amino-4,4-diphenyl-BODIPY), C28H32BN3, the central six-membered ring has a flattened sofa conformation, with one of the N atoms deviating by 0.142 (4) Å from the mean plane of the other five atoms, which have an r.m.s. deviation of 0.015 Å. The dihedral angle between the two essentially planar outer five-membered rings is 8.0 (2)°. In the crystal, molecules are linkedviaweak N—H...π interactions, forming chains along [010]. The compound displays solvent-dependent behaviours in both NMR and fluorescence spectroscopy. In the1H NMR spectra, the aliphatic resonance signals virtually coalesce in solvents such as chloroform, dichloromethane and dibromoethane; however, they are fully resolved in solvents such as dimethyl sulfoxide (DMSO), methanol and toluene. The excitation and fluorescence intensities in chloroform decreased significantly over time, while in DMSO the decrease is not so profound. In toluene, the excitation and fluorescent intensities are not time-dependent. This behaviour is presumably attributed to the assembly of 3-amino-4,4-diphenyl-BODIPY in solution that leads to the formation of noncovalent structures, while in polar or aromatic solvents, the formation of these assemblies is disrupted, leading to resolution of signals in the NMR spectra.

Formen des Diphenylgermaniumoxids(Ph2GeO)x, x = 3, 4, n / Phases of Diphenylgermanium Oxide(Ph2GeO)x, x = 3, 4, n

1984 ◽  
Vol 39 (7) ◽  
pp. 868-875 ◽  
Author(s):  
Ludwig Roß ◽  
Martin Dräger
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Vibrational Spectra ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Tetragonal Crystals ◽  
Hydroxy Groups ◽  
C Nmr

Diphenylgermanium oxide can be obtained trimeric (6 -membered ring, monoclinic crystals), tetrameric (8 -membered ring, monoclinic and tetragonal crystals and monoclinic with half a mole of crystal ethanol) and polymeric with terminating hydroxy groups. Transitions are investigated by thermal analysis, mass spectra and 13C NMR spectra. The vibrational spectra (I. R . and Raman) of the forms are discussed . The crystal structure of the monoclinic (Ph :GeO)4 has been determined and refined to R = 0.051. The symmetry of the molecule is near to S4 (distances Ge - O 174.7 - 176.2, Ge - C 190.0 - 194.6 pm, angles Ge - O - Ge 131.2 - 136.9, O - Ge - O 107.8 -110.3 °).

Zur Chemie der 1,3,5-Triaza-2-phosphorinan-4,6-dione. Teil X. Umsetzungen von 2-Hydro-1,3,5-trimethyl-1,3,5-triaza-2-oxo-2λ4- phosphorinan-4,6-dion mit Triazin-Derivaten sowie mit einigen Aldehyden / Chemistry of the 1,3,5-Triaza-2-phosphorinan-4,6-diones. Part X. Reactions of 2-Hydro-1,3,5-trimethyl-1,3,5-triaza-2-oxo-2λ4 -phosphorinan-4,6-dione with Triazine Derivatives and with Some Aldehydes

1995 ◽  
Vol 50 (12) ◽  
pp. 1833-1838 ◽  
Author(s):  
Ion Neda ◽  
Michael Farkens ◽  
Holger Thönnessen ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Analysis ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Glyoxylic Acid ◽  
Crystal Structure Analysis ◽  
Membered Ring ◽  
X Ray ◽  
Triazine Derivatives

The reactions o f 2-hydro-1,3,5-trim ethyl-1,3,5-triaza-2-oxo-2λ4 -phosphorinan-4,6-dione 1 with the triazine derivatives, 1,3,5-trimethyl- and 1,3,5-tribenzyl-hexahydro-1,3,5-triazine, are described. The reaction of three equivalents of 1 with one equivalent of the triazine derivative gave 2 and 3. Both compounds were characterized via their 1H, 13C, and 31P NMR spectra, mass spectra and, in the case of 2, by an X-ray crystal structure analysis, which showed an almost planar six-membered ring; hydrogen bonds of the form N-H···O link the molecules in centrosymmetric pairs. The reactions of 1 with the aldehydes glyoxylic acid, 2-hydroxybenzaldehyde and 3,4,5-trimethoxybenzaldehyde gave addition products. The C (:O) group o f the aldehyde is inserted into the P -H bond o f 1. The resulting compounds 4 ,5 and 6 were characterized through their 1H, 13C, and 31P NMR spectra, and mass spectra.

scholarly journals Synthesis of N,O-Chelating Hydrazidopalladium Complexes from 1,2-Bis(trifluoroacetyl)hydrazine

Inorganics ◽  
2021 ◽  
Vol 9 (10) ◽  
pp. 76
Author(s):  
Yoshihito Kayaki ◽  
Tomohiro Hayakawa ◽  
Takao Ikariya
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Nmr Spectra ◽  
Structural Changes ◽  
Variable Temperature ◽  
Palladium Complexes ◽  
Electron Donors ◽  
Crystal Structure Determination ◽  
X Ray ◽  
Square Planar

N,O-chelating dicarbonylhydrazido-palladium complexes were synthesized by treatment of 1,2-bis(trifluoroacetyl)hydrazine with a mixture of a Pd(0) source, [Pd(dba)2] (DBA = dibenzylideneacetone), and four-electron donors including 1,3-bis(diphenylphosphino)propane (DPPP), N,N,N’,N’-tetramethylethylenediamine (TMEDA), and two equivalents of triphenylphosphine. The same products from DPPP and TMEDA could be obtained alternatively by using Pd(OAc)2 through deprotonation of the diacylhydrazine. The five-membered chelate structure was confirmed by NMR spectra and X-ray crystal structure determination. The X-ray structures indicate that the products are formally considered as Pd(II) complexes with a hydrazido(2–) ligand. In the case of the triphenylphosphine-coordinated complex, a fluxional behavior in dichloromethane-d2 was observed by variable temperature NMR experiments, possibly due to structural changes between the square planar and pseudo-tetrahedral geometries.

The crystal structure of 1-azoniatricyclo[4.4.4.01,6]tetradecane and 1-azoniatricyclo[4.4.3.01,6]tridecane bromides

1982 ◽  
Vol 60 (9) ◽  
pp. 1073-1077 ◽  
Author(s):  
John M. McIntosh ◽  
Masood A. Khan ◽  
Louis T. J. Delbaere
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Unit Cell ◽  
Space Group ◽  
The One

The crystal structures of 1-azoniatricyclo[4.4.4.01,6]tetradecane bromide (1) and 1-azoniatricyclo[4.4.3.01,6]tridecane bromide (2) are reported. Compound 1, C13H24NBr, crystallizes in space group P63/mmc with a = 8.383(2) Å, c = 10.092 Å, γ = 120°, Z = 2. Compound 2, C12H22NBr, crystallizes in space group P63/mmc with a = 8.283(2) Å, c = 10.046(2) Å, γ = 120°, Z = 2. The crystal structures of 1 and 2 are statistically disordered with both enantiomers occurring in the unit cell. Compound 2 is further disordered with the one five-membered ring and the two six-membered rings of the cation being averaged over the same site in the unit cell.The structures confirm the previously reported conclusions based on the 400 MHz nmr spectra of 1.

Substituted 1,2-diaza-7-oxaspiro[4,4]nonen-6-ones; Preparation, NMR spectra, and crystal structure

1991 ◽  
Vol 56 (5) ◽  
pp. 973-983 ◽  
Author(s):  
Jaroslav Jonas ◽  
Tadeusz Głowiak ◽  
Zdirad Žák ◽  
Petr Trška ◽  
Ctibor Mazal
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra

Diazomethane adds to substituted 3-methylene-2-(3H)-dihydrofuranones (Ia-Ii) to give the corresponding title dihydropyrazolospirodihydrofuranones (IIa-IIf, IIi,andIIj) or (IIIa, IIIg, and IIIh). NMR spectra of the adducts are discussed in some detail and the crystal structure has been solved for (4R, 5S)-5-benzoyloxy-1,2-diaza-7-oxaspiro[4.4]non-1-en-6-one (IIa).

scholarly journals Heteroleptic [Cu(P^P)(N^N)][PF6] Complexes: Effects of Isomer Switching from 2,2′-biquinoline to 1,1′-biisoquinoline

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 185
Author(s):  
Nina Arnosti ◽  
Marco Meyer ◽  
Alessandro Prescimone ◽  
Edwin C. Constable ◽  
Catherine E. Housecroft
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Nmr Spectra ◽  
Phenyl Ether ◽  
Quantum Yields ◽  
Dynamic Processes ◽  
Electrochemical Behaviors ◽  
Ambient Temperatures ◽  
Π Stacking

The preparation and characterization of [Cu(POP)(biq)][PF6] and [Cu(xantphos)(biq)][PF6] are reported (biq = 1,1′-biisoquinoline, POP = bis(2-(diphenylphosphanyl)phenyl)ether, and xantphos = (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphane). The single crystal structure of [Cu(POP)(biq)][PF6] 0.5Et2O was determined and compared to that in three salts of [Cu(POP)(bq)]+ in which bq = 2,2′-biquinoline. The P–C–P angle is 114.456(19)o in [Cu(POP)(biq)]+ compared to a range of 118.29(3)–119.60(3)o [Cu(POP)(bq)]+. There is a change from an intra-POP PPh2-phenyl/(C6H4)2O-arene π-stacking in [Cu(POP)(biq)]+ to a π-stacking contact between the POP and bq ligands in [Cu(POP)(bq)]+. In solution and at ambient temperatures, the [Cu(POP)(biq)][PF6]+ and [Cu(xantphos)(biq)]+ cations undergo several concurrent dynamic processes, as evidenced in their multinuclear NMR spectra. The photophysical and electrochemical behaviors of the heteroleptic copper (I) complexes were investigated, and the effects of changing from bq to biq are described. Short Cu···O distances within the [Cu(POP)(biq)]+ and [Cu(xantphos)(biq)]+ cations may contribute to their very low photoluminescent quantum yields.

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