A comment on the formation of N-C bonds via reactions of anionic dinitrogen complexes with organic halides: X-ray crystallographic structure of trans-

Author:

Hughes David L.,Ibrahim Saad K.,Ali Hapipah Mohd,Pickett Christopher J.

Publisher

Elsevier BV

Subject

Materials Chemistry,Inorganic Chemistry,Organic Chemistry,Physical and Theoretical Chemistry,Biochemistry

Reference7 articles.

1. Preparation and properties of molybdenum and tungsten dinitrogen complexes. 47. Bimetallic arylation of molecular nitrogen

2. Redox potential–structure relationships in metal complexes. Part 2. The influence of trans-substituents upon the redox properties of certain dinitrogen complexes of molybdenum and tungsten and some carbonyl analogues: inner-sphere versus outer-sphere electron transfer in the alkylation of co-ordinated dinitrogen

3. Transformation of a methyleneamide ligand at molybdenum: electrochemical oxidation to a cyanide, reactions with elemental oxygen, sulphur or selenium and X-ray crystal structures of trans-[Mo(CN)Cl(dppe)2]·MeOH and trans-[Mo(NCS)Cl(dppe)2]; electroreduction of the cyanide to an aminocarbyne, trans-[Mo(CNH2)Cl(dppe)2](dppe = Ph2PCH2CH2PPh2)

4. Crystal structure analysis oftrans-[W(CN)(NNCHO-CH2CH2CH2)(dppe)2]. Et2O. Crystal data: C57H55N3-OP4W,C4H10O, M = 1180.0. Tetragonal, space group P42/n (no. 86, origin on an inversion centre),a = 29.444(2), c = 12.944(1) Å, U = 11221.7 Å3.Z = 8, Dc = 1.397 g cm−3,F(000) = 4816, μ(Mo-Kα) = 22.6 cm−1, λ(Mo-Kα) = 0.71069 Å. Very thin, long, orange needles which deteriorate slowly in air. After photographic examination, crystal mounted on CAD4 diffractometer for accurate cell dimensions and intensity measurements (θmax = 20°). Intensities corrected for Lorentz-polarisation and absorption effects. 5220 Unique reflections (3199 with I > 2σ1) entered into shelx system for structure determination (heavy atom method) and refinement (large-block-matrix least-squares methods) to R = 0.067 and Rg = 0.049 (G.M. Sheldrick, shelx-Program for crystal structure analysis, University of Cambridge, 1976; also extended version, shelxn, 1977) for 3838 reflections (I > σ1) weighted w = (σF2 + 0.000063F2−1. All non-hydrogen atoms in W complex refined anisotropically; H atoms included in idealised positions. Solvent molecule disordered, not fully resolved. Tables of atom coordinates, thermal parameters, and bond lengths and angles have been deposited at the Cambridge Crystallographic Data Centre

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