Combined solid state NMR and ONIOM studies of reversible crystalline phase reaction for nickel coordination compounds

Paluch, Piotr; Potrzebowski, Marek J.

doi:10.1016/j.ssnmr.2009.07.001

Cited by 5 publications

(5 citation statements)

References 34 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Repetition delay was set to 60 s which was equal to at least three times the measured T 1 of each sample. 15 N chemical shifts were calibrated indirectly with respect to liquid ammonia using the signal of finely powdered -glycine at 32.1 ppm (Paluch & Potrzebowski, 2009). 32, 9120 or 12208 scans were coherently added giving total measurement times equal to 32 min, 154 h and 208 h for Y NH 4 Cl , P NH 4 Br and P NH 4 I , respectively.…”

Section: N Ssnmr Spectroscopymentioning

confidence: 99%

Arsenic(III) oxide intercalate with ammonium chloride: crystal structure revision and thermal characterization

Wrześniewska

Paluch²,

Guńka

2023

Acta Crystallogr Sect B

Self Cite

View full text Add to dashboard Cite

According to the crystal structure determination by Edstrand & Blomqvist [Ark. Kemi (1955), 8, 245–256], intercalate NH4Cl·As2O3·0.5H2O ({\bf Y_{{NH}_{4}Cl}}) is not isostructural with compound KCl·As2O3·0.5H2O. This is very unlikely because both NH4Br·2As2O3 and KBr·2As2O3 as well as NH4I·2As2O3 and KI·2As2O3 are isostructural. Hence, intercalate {\bf Y_{{NH}_{4}Cl}} has been studied using single-crystal X-ray diffraction in addition to attenuated total reflection Fourier transform infrared (ATR-FTIR) and 15N solid-state magic-angle spinning nuclear magnetic resonance (ssNMR) spectroscopies. These techniques indicate that revising the previous crystal structure model is necessary. Compound {\bf Y_{{NH}_{4}Cl}} crystallizes in space group P6/mmm with unit-cell parameters a = 5.25420 (10) Å and c = 12.6308 (3) Å and is isostructural with KCl·As2O3·0.5H2O. The presence of two symmetry-independent ammonium cations in the structure has been unequivocally confirmed using 15N ssNMR spectroscopy. The 15N ssNMR spectrum of intercalate {\bf Y_{{NH}_{4}Cl}} has been compared with analogous spectra of NH4Br·2As2O3 and NH4I·2As2O3 which allowed for a probable assignment of signals to ammonium cations occupying particular sites in the crystal structures. Thermogravimetry, differential scanning calorimetry and variable-temperature ATR-FTIR spectra have revealed that intercalate {\bf Y_{{NH}_{4}Cl}} is dehydrated between 320 and 475 K. Upon cooling or standing in moist air water is re-absorbed. Dehydration leads to significant shortening of the c unit-cell parameter as revealed by powder X-ray diffraction [c = 12.1552 (7) Å at 293 K]. Compound {\bf Y_{{NH}_{4}Cl}} decomposes on prolonged heating above 490 K to arsenic(III) oxide and ammonium chloride.

show abstract

Section: N Ssnmr Spectroscopymentioning

confidence: 99%

Arsenic(III) oxide intercalate with ammonium chloride: crystal structure revision and thermal characterization

Wrześniewska

Paluch²,

Guńka

2023

Acta Crystallogr Sect B

Self Cite

View full text Add to dashboard Cite

show abstract

“…For paramagnetic inorganic materials 2 H NMR is preferred over 1 H NMR due to a reduction of the strong electron–nuclear dipolar interaction by a factor of ∼1/6 (γ( 2 H)/γ( 1 H)), no background signals, and additional structural information from the 2 H quadrupole interaction. Diamagnetic Ni(II) complexes have previously been investigated by SSNMR to obtain structural information and monitor single crystal to single crystal transformation . Paramagnetic Ni(II) coordination compounds are much less studied by NMR.…”

Section: Introductionmentioning

confidence: 99%

Solid State ¹³C and ²H NMR Investigations of Paramagnetic [Ni(II)(acac)₂L₂] Complexes

et al. 2013

View full text Add to dashboard Cite

Nine structurally related paramagnetic acetylacetonato nickel(II) complexes: [Ni(acac)2] and trans-[Ni(acac)2(X)2]nH/D2O, X = H2O, D2O, NH3, MeOH, PMePh2, PMe2Ph, or [dppe]1/2, n = 0 or 1, dppe = 1,2-bis(diphenylphosphino)ethane, as well as cis-[Ni(F6-acac)2(D2O)2], F6-acac = hexafluoroacetylonato, have been characterized by solid state (13)C MAS NMR spectroscopy. (2)H MAS NMR was used to probe the local hydrogen bonding network in [Ni(acac)2(D2O)2]D2O and cis-[Ni(F6-acac)2(D2O)2]. The complexes serve to benchmark the paramagnetic shift, which can be associated with the resonances of atoms of the coordinated ligands. The methine (CH) and methyl (CH3) have characteristic combinations of the isotropic shift (δ) and anisotropy parameters (d, η). The size of the anisotropy (d), which is the sum of the chemical shift anisotropy (CSA) and the paramagnetic electron-nuclei dipolar coupling, is much more descriptive than the isotropic shift. Moreover, the CSA is found to constitute up to one-third of the total anisotropy and should be taken into consideration when (13)C anisotropies are used for structure determination of paramagnetic materials. The (13)C MAS NMR spectra of trans-[Ni(acac)2(PMe2Ph)2], trans-[Ni(acac)2(PMePh2)2], and the noncrystallographically characterized trans-[Ni(acac)2(dppe)]n were assigned using these correlations. The complexes with L = H2O, D2O, NH3, and MeOH can be prepared by a series of solid state desorption and sorption reactions. Crystal structures for trans-[Ni(acac)2(NH3)2] and trans-[Ni(acac)2(PMePh2)2] are reported.

show abstract

“…Solid-state NMR is a versatile tool for studying the different interactions present in porous co-ordination frameworks, which is increasingly used for the characterization of structure and dynamics in these materials. [20][21][22][23][24] NMR spectra of solid samples provide information on the detailed local electronic structure of each nucleus reflected as chemical shift without the need of long-range order. Therefore, non-crystalline materials can be characterized with solid-state NMR which is increasingly used for the characterization of structure and dynamics in these materials.…”

Section: Introductionmentioning

confidence: 99%

“…A better understanding of the various interactions present in the metal–ligand framework is inevitable to explore its potential applicability. Solid-state NMR is a versatile tool for studying the different interactions present in porous coordination frameworks, which is increasingly used for the characterization of structure and dynamics in these materials. − NMR spectra of solid samples provide information on the detailed local electronic structure of each nucleus reflected as a chemical shift without the need of long-range order. Therefore, noncrystalline materials can be characterized with solid-state NMR, which is increasingly used for the characterization of structure and dynamics in these materials. − Furthermore, using this method, it is easy to determine the presence of small mobile molecules, while X-ray analysis is more complicated or impossible …”

Section: Introductionmentioning

confidence: 99%

Synthesis, Crystal Structure, and Solid-State NMR Investigations of Heteronuclear Zn/Co Coordination Networks — A Comparative Study

et al. 2013

View full text Add to dashboard Cite

show abstract

Combined solid state NMR and ONIOM studies of reversible crystalline phase reaction for nickel coordination compounds

Cited by 5 publications

References 34 publications

Arsenic(III) oxide intercalate with ammonium chloride: crystal structure revision and thermal characterization

Arsenic(III) oxide intercalate with ammonium chloride: crystal structure revision and thermal characterization

Solid State ¹³C and ²H NMR Investigations of Paramagnetic [Ni(II)(acac)₂L₂] Complexes

Synthesis, Crystal Structure, and Solid-State NMR Investigations of Heteronuclear Zn/Co Coordination Networks — A Comparative Study

Contact Info

Product

Resources

About

Combined solid state NMR and ONIOM studies of reversible crystalline phase reaction for nickel coordination compounds

Cited by 5 publications

References 34 publications

Arsenic(III) oxide intercalate with ammonium chloride: crystal structure revision and thermal characterization

Arsenic(III) oxide intercalate with ammonium chloride: crystal structure revision and thermal characterization

Solid State 13C and 2H NMR Investigations of Paramagnetic [Ni(II)(acac)2L2] Complexes

Synthesis, Crystal Structure, and Solid-State NMR Investigations of Heteronuclear Zn/Co Coordination Networks — A Comparative Study

Contact Info

Product

Resources

About

Solid State ¹³C and ²H NMR Investigations of Paramagnetic [Ni(II)(acac)₂L₂] Complexes