An experiment involving a moisture-sensitive synthesis and spectroscopic characterization suitable for the advanced inorganic laboratory course is presented. The acid-base complex ammonia borane (AB) is synthesized from the heterogeneous reaction between sodium borohydride and finely ground ammonium sulfate in tetrahydrofuran solvent. AB is…

Electronic spectra often exhibit vibronic structure when vibrational and electronic transitions occur in concert. Theory reveals (1) that orbital symmetry considerations determine specific roles played by the nuclear degrees of freedom and (2) that the vibrational excitation is often highly regiospecific, that is, attributable to an identifiable…

In this experiment, the students explore the synthesis of a crystalline solid-state material, barium zirconate (BaZrO3) by two different synthetic methods: (a) the wet chemical method using BaCl[subscript 2]·2H[subscript 2]O and ZrOCl[subscript 2]·8H[subscript 2]O as the precursors, and (b) the solid-state reaction from BaCO[subscript 3] and…

In this experiment, students perform an air-free synthesis of three dichlorophosphinenickel(II) compounds, NiCl[subscript 2](PPh[subscript 3])[subscript 2], NiCl[subscript 2](PCy[subscript 3])[subscript 2], and NiCl[subscript 2](DPPE), using NiCl[subscript 2]·6H[subscript 2]O and the appropriate phosphine as the precursors. These colorful nickel…

A laboratory experiment for students in advanced inorganic chemistry is described. In this experiment, students prepare two metal complexes with a potentially bidentate-carbene ligand. The complexes are synthesized by reaction of a bisimidazolium salt with silver(I) oxide or palladium(II) acetate. Silver and palladium complexes are binuclear and…

Semiconductors are an important class of materials; preparing ZnO nanorods allows semiconducting properties to be easily observed. The week before lab, groups of four students take 15 min to setup two fluorine-doped tin oxide glass (FTO) slides in a zinc nitrate and hexamethylenetetramine solution stored at 90°C until the next lab. Hexagonal ZnO…

Undergraduate laboratories expose students to a wide variety of topics and techniques in a limited amount of time. This can be a challenge and lead to less exposure to concepts and activities in bio-inorganic chemistry and analytical chemistry that are closely-related to biochemistry. To address this, we incorporated a new iron determination by…

Laboratory experiments that demonstrate the effect of paramagnetic complexes on chemical shifts and relaxation times of protons are a useful way to introduce magnetic resonance spectroscopy (MRS) probes or magnetic resonance imaging (MRI) contrast agents. In this undergraduate inorganic chemistry experiment, a paramagnetic Co(II) cage complex is…

General chemistry courses predominantly use expository experiments that shape student expectations of what a laboratory activity entails. Shifting within a semester to course-based undergraduate research activities that include greater decision-making, collaborative work, and "messy" real-world data necessitates a change in student…

An integrated laboratory experiment applying concepts and techniques developed in organic chemistry, inorganic chemistry, and instrumental analysis is presented for use by students interested in undergraduate research. The experiment incorporates some advanced laboratory practices such as multistep organic synthesis and purification, detailed…

The aim of this simple, quick, and safe laboratory exercise is to provide undergraduate students an introduction to nanotechnology using nanoparticle (NP) synthesis. Students are provided two procedures that allow for the synthesis of different yet controlled sizes of silver NPs. After preparing the NPs, the students perform UV-visible…

This advanced undergraduate laboratory experiment involves the synthesis and characterization of a metal-organic framework with microporous channels that are held intact via hydrogen bonding of the coordinated water molecules. The hydrothermal synthesis of Co[subscript 3](BTC)[subscript 2]·12H[subscript 2]O (BTC = 1,3,5-benzene tricarboxylic acid)…

The organometallic complex Fe[subscript 2](µ-S[subscript 2])(CO)[subscript 6] has interesting biological implications. The concepts of bio-organometallic chemistry are rarely discussed at the undergraduate level, but this experiment can start such a conversation and, in addition, teach valuable synthetic techniques. The lab experiment takes a…

Experiments are described for the reliable small-scale glovebox preparation of CpMo(CO)[subscript 3](CH[subscript 3]) and acetyl derivatives thereof through phosphine-induced migratory insertion. The robust syntheses introduce students to a variety of organometallic reaction mechanisms and glovebox techniques, and they are easily carried out…

This communication is a collection of additions and modifications to two previously published classic inorganic synthesis laboratory experiments. The experimental protocol for the synthesis and isolation of enantiomerically enriched ?- (or ?-)Co(en)[subscript 3]I[subscript 3] has been modified to increase reproducibility, yield, and enantiomeric…