Crystalline monomeric alkyltin(II) compounds were prepared using the β-N-functionalised ligand 2-pyridylbis(trimethylsilyl)methyl, C5H4N[C(SiMe3)2]-2 (R): (a) SnR21 from (LiR)2 and SnCl2 or Sn(OC6H3But2-2,6)2(b) SnR(Cl)2 from SnCl2 and SnR2 or ½(LiR)2; and (c) SnR[N(SiMe3)2]3 from Sn[N(SiMe3)2]2 and ½(LiR)2. Single-crystal X-ray diffraction data showed that in each of 1–3 R– behaves as a chelating, C,N-centred ligand, and that the lone pair on tin is stereochemically active. The mean Sn–C [and Sn–NC5H4] bond lengths (A) are 2.35(2)[2.42(2)] in 1, 2.32(2)[2.27(3)] in 2, and 2.356(8)[2.299(5)] in 3. Variable-temperature multinuclear (1H, 13C, 29Si and 119Sn) NMR spectral data were obtained for 1–3 in [2H8]toluene. These showed that dynamic processes were operative, believed to be Sn–N(C5H4) dissociations, with ΔG‡Tc= 43.5 ± 0.8 for 2 or 42.7 ± 0.8 kJ mol–1 for 3(the coalescence temperature Tc being 220 ± 2 for 2 and 214 ± 2 K for 3); for 3 a further fluxion with ΔG‡Tc= 76.1 ± 0.8 kJ mol–1(Tc= 368 ± 2 K) is attributed to the barrier to rotation about the tin–amide nitrogen bond. Attempts were made to reduce 2[evidence for (SnR)n], and to prepare analogues of GeII and PbII of 1 and 2. A further β-functionalised complex, SnCl(OCBut2CH2PMe2)4, was obtained from SnCl2 and ½2[Li(OCBut2CH2PMe2)]2; there was no evidence for 31P–119Sn coupling, and a plausible structure is [Sn(µ-Cl)(OCBut2CH2PMe2)]2. A similar metathetical reaction between SnCl2 and Sn(OC6H3But2-2,6)2 in tetrahydrofuran (thf) gave 1//m[SnCl(OC6H3But2–2,6)(thf)n]m, whereas SnCl2+ SnR′2[R′= CH(SiMe3)2] yielded SnR′2Cl2+ Sn.

Subvalent Group 14 metal compounds. Part 16. Synthesis, crystal structure and characterisation of some β-functionalised-alkyltin(II) complexes, SnR(X){R = C5H4N[C(SiMe3)2]-2; X = R, Cl or N(SiMe3)2}

Main Group and Group 11, 12, 2-pyridyl-(trimethylsilyl)methyl and -bis(trimethylsilyl)-methyl chemistry

Synthesis and Structures of Iron(II) Alkyl and Thiolate Compounds Containing Sterically Hindered N-Functionalized Alkyl Ligands

6.1 – Cobalt

Organometallic Complexes of the η2 (N, C)-Coordinated Derivatives of Pyridine

Synthesis and X-ray structure of a highlyhindered N-functionalized alkyl-cobalt(II) complex trans-[-2}2]

Abstract Calreticulin (CRT) is a protein found mainly in the endoplasmic reticulum (ER) that maintains calcium levels and controls protein folding, but has recently been found at the cell surface, cytoplasm, and in the extracellular matrix. CRT participates in multiple physiological processes such as gene expression, the immune response, and cancer. Calreticulin has been shown to autoacetylate with the binding of preferred ligand 7,8‐diacetoxy‐4‐methylcoumarin (DAMC). This project aims to develop a chemical biology approach to investigate importance of CRT acylating abilities on its nonendoplasmic reticulum functions by targeting the downstream substrates of CRT acetylation. Our goal was to use CRT to transfer a pentynoyl tag (using a novel ligand, DPeMC) to its substrates, which can then be used as a handle for protein identification. Molecular modelling using available data in the literature was used to approximate the binding interface between CRT and the acylation ligands. Molecular Operating Environment (MOE) software was used to perform sequence alignment, simulated annealing, positional refinement, and blind docking of acylated coumarins with the CRT model. Docking studies pointed to the P domain as the most thermodynamically and sterically favourable region for acylated coumarin binding with tryptophan residue 200 within the active site on CRT. Absorption and fluorescence spectra of all coumarin compounds in ethanol:PBS (1:9 v/v) solution were investigated. Stern–Volmer quenching constant (KSV), binding constant (K), and number of binding sites (n) of each coumarin compound with CRT was determined. Our studies demonstrated that acyl coumarin compounds bind to CRT using a dynamic quenching mechanism, bind to a single binding site on the P domain, and that the protein–ligand interaction is spontaneous and exothermic.

Spectroscopic studies of 7,8‐diacetoxy‐4‐methylcoumarin and 7,8‐dipentynoyl‐4‐methylcoumarin binding with calreticulin

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Synthesis and X-ray structure of a highlyhindered N-functionalized alkyl-cobalt(II) complex trans-[-2}2]

Spectroscopic studies of 7,8‐diacetoxy‐4‐methylcoumarin and 7,8‐dipentynoyl‐4‐methylcoumarin binding with calreticulin