Syntheses, structures and flexible coordination of sterically demanding di- and “tri”-lithiated methandiides

2014 ◽  
Vol 43 (38) ◽  
pp. 14334-14345 ◽  
Author(s):  
Christian P. Sindlinger ◽  
Andreas Stasch

Sequential lithiation of a sterically demanding bis(iminophosphoranyl)methane afforded di- and trianionic methandiide lithium complexes and their structures and coordination behaviour have been studied with solid state and solution methods.

2018 ◽  
Vol 74 (8) ◽  
pp. 951-960 ◽  
Author(s):  
Chong Zhang ◽  
Kou-Lin Zhang

The bromo-substituted aromatic dicarboxylic acid 5-amino-2,4,6-tribromoisophthalic acid (H2ATBIP) was used to assemble with CdII ions in the presence of the N-donor flexible bipyridyl ligands 3,3′-(diazene-1,2-diyl)dipyridine (mzpy) and 1,3-bis(pyridin-3-ylmethyl)urea (3bpmu), leading to the formation of two chain coordination polymers by adopting solution methods, namely, catena-poly[[[triaqua(5-amino-2,4,6-tribromoisophthalato-κO)cadmium(II)]-μ-3,3′-(diazene-1,2-diyl)dipyridine-κ2 N 1:N 1′] dihydrate], {[Cd(C8H2Br3NO4)(C10H8N4)(H2O)3]·2H2O} n or {[Cd(ATBIP)(mzpy)(H2O)3]·2H2O} n , (1), and catena-poly[[[tetraaquacadmium(II)]-μ-1,3-bis(pyridin-3-ylmethyl)urea-κ2 N 1:N 1′-[diaquabis(5-amino-2,4,6-tribromoisophthalato-κO)cadmium(II)]-μ-1,3-bis(pyridin-3-ylmethyl)urea-κ2 N 1:N 1′] octahydrate], {[Cd(C8H2Br3NO4)(C12H12N4O)(H2O)3]·4H2O} n or {[Cd(ATBIP)(3bpmu)(H2O)3]·4H2O} n , (2). Both complexes were characterized by FT–IR spectroscopic analysis, thermogravimetric analysis (TGA), solid-state diffuse reflectance UV–Vis spectroscopic analysis, and single-crystal and powder X-ray diffraction analysis (PXRD). The mzpy and 3bpmu ligands bridge the CdII metal centres in (1) and (2) into one-dimensional chains, and the ATBIP2− ligands show a monodentate coordination to the CdII centres in both coordination polymers. A discrete water tetramer exists in (1). Within the chains of (1) and (2), there are halogen bonds between adjacent ATBIP2− and mzpy or 3bpmu ligands, as well as hydrogen bonds between the ATBIP2− ligands and the coordinated water molecules. With the aid of weak interactions, the structures of (1) and (2) are further extended into three-dimensional supramolecular networks. An analysis of the solid-state diffuse reflectance UV–Vis spectra of (1) and (2) indicates that a wide indirect band gap exists in both complexes. Complexes (1) and (2) exhibit irreversible and reversible dehydration–rehydration behaviours, respectively, and the solid-state fluorescence properties of both complexes have been studied.


1989 ◽  
Vol 4 (5) ◽  
pp. 1099-1102 ◽  
Author(s):  
E. A. Hayri ◽  
M. Greenblatt ◽  
K. V. Ramanujachary ◽  
M. Nagano ◽  
J. Oliver ◽  
...  

Samples of YBa2Cu3O7 were prepared by sol-gel, co-precipitation, and solid state processes. Sol-gel samples were prepared from a solution of yttrium, barium, and copper nitrates dissolved in ethylene glycol, co-precipitated samples were made by the amorphous citrate method, and solid state samples were prepared by conventional high temperature reaction of the appropriate metal oxides and carbonates. The sol-gel process was shown to yield superconducting samples of superior Meissner effect, critical current, and critical field. The co-precipitated samples contain impurities that affect the critical properties. The sol-gel and co-precipitated processes yield materials with well-formed, plate-like particles with a fairly uniform size of about 10 μm. The grains in the solid state sample are smaller but have a much wider distribution of sizes than the samples prepared by solution methods.


Polyhedron ◽  
2019 ◽  
Vol 171 ◽  
pp. 412-422 ◽  
Author(s):  
Anastasios Peppas ◽  
Evanthia Papadaki ◽  
Gregor Schnakenburg ◽  
Victoria Magrioti ◽  
Athanassios I. Philippopoulos

2014 ◽  
Vol 43 (12) ◽  
pp. 4838-4846 ◽  
Author(s):  
Graeme J. Moxey ◽  
Fabrizio Ortu ◽  
Leon Goldney Sidley ◽  
Helen N. Strandberg ◽  
Alexander J. Blake ◽  
...  

Reaction between N,N′-bis(aryl)amidines and di-n-butylmagnesium affords magnesium amidinates, where the steric bulk of the ligand influences both the solid state and solution behaviour of these complexes.


Inorganics ◽  
2021 ◽  
Vol 9 (10) ◽  
pp. 75
Author(s):  
Shogo Morisako ◽  
Kohsuke Noro ◽  
Takahiro Sasamori

A spirogermabifluorene that bears sterically demanding 3,3′,5,5′-tetra(t-butyl)-2,2′-biphenylene groups (1) was obtained from the reaction of in-situ-generated 2,2′-dilithiobiphenylene with GeCl2·(dioxane). The solid-state structure and the redox behavior of 1 were examined by single-crystal X-ray diffraction analysis and electrochemical measurements, respectively. The sterically hindered biphenyl ligands endow 1 with high redox stability and increased electron affinity. The experimental observations were corroborated by theoretical DFT calculations.


2009 ◽  
Vol 62 (10) ◽  
pp. 1207 ◽  
Author(s):  
Ying Dong ◽  
Leonard F. Lindoy

A cyclic, tetra-linked macrocyclic species incorporating four 1,4,8,11-tetraazacyclotetradecane (cyclam) subunits has been synthesized employing Boc amine-group protecting chemistry coupled with high dilution conditions for the cyclization step. A series of 4:1 (metal:ligand (M:L)) complexes with nickel(ii), copper(ii), zinc(ii), and cadmium(ii) has been synthesized. Visible spectophotometric (including spectrophotometric titration), EPR, NMR, and electrochemical studies are reported for individual complexes and are in general accord with similar 4:1 (M:L) coordination behaviour occurring in both the solid state and in solution. The study makes available an example of a new category of large cyclic receptors whose cavity can be tuned electronically through variation of the metal centres incorporated in the cavity walls.


2021 ◽  
Author(s):  
Jessica E. Waters ◽  
Schirin Hanf ◽  
Marina Rincón-Nocito ◽  
Andrew David Bond ◽  
Raúl García-Rodríguez ◽  
...  

The effects of moving the donor N-atom from the 2-position in lithium (2-pyridyl)- and (2-quinolyl)aluminates to the more remote position in (8-quinolyl)aluminates have been investigated by solid-state structural and DFT...


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