Abstract

Erdmann’s anion [1,6-diammino tetranitrocobaltate(III)] is useful in the isolation and crystallization of recently confiscated street drugs needing to be identified and catalogued. The protonated form of such drugs forms excellent crystals with that anion; moreover, Erdmann’s salts are considerably less expensive than the classically used AuCl4− anion to isolate them, while preparation of high-quality crystals is equally easy in both cases. We describe the preparation and structures of the K+CoH6N6O8− and NH4+CoH6N7O8−, salts of Erdmann’s. In addition, herein are described the preparations of this anion’s salts with cocaine (C17H28CoN7O12), with methamphetamine (C10H22CoN7O8), and with methylone (C22H34CoN8O14), whose preparation and stereochemistry had been characterized by the old AuCl4− salts methodology. For all species in this report, the space groups and cell constants were determined at 296 and 100 K, looking for possible thermally induced polymorphism—none was found. Since the structures were essentially identical at the two temperatures studied, we discuss only the 100 K results. Complete spheres of data accessible to a Bruker ApexII diffractometer with Cu–Kα radiation, λ = 1.54178 Å, were recorded and used in the refinements. Using the refined single crystal structural data for the street drugs, we computed their X-ray powder diffraction patterns, which are beneficial as quick identification standards in law enforcement work.

Highlights

  • In collaboration with the Ocean County Sheriff’s Office Forensic Science Laboratory (NJ, USA), we have been engaged in studies of the nature of the street drugs commonly known as bath salts [4,5], the addictive principle of which are positively charged amino species, per se, or have been converted into hydrohalides (Cl− or Br−, or mixtures thereof) in order to make them water soluble

  • Complex (3): A sample of a few milligrams of crystalline cocaine·HCl was dissolved on a glass slide in H2 O, and a single drop of a 5% Erdmann’s potassium salt solution in Chemistry 2021, 3 water was added

  • Complex (4): Several milligrams of crystalline methamphetamine·HCl were reacted with a drop of the previously prepared 5% solution of potassium Erdmann’s salt on a pre-cleaned microscope slide

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Summary

Introduction

Notes: (a) Erdmann’s salt should not be confused with Erdmann’s reagent (sulfuric acid containing dilute nitric acid), which has been used as an alkaloid color test [1]. (b). AuCl4 − anion, we decided to find alternative, inexpensive anions, which would be simple to make even by our first-year chemistry major or nonmajor, students Those salts should provide good, hopefully better, microscopic and X-ray diffraction quality crystals with those of the traditional gold anion samples. Since a number of these drugs contain oxygen moieties that can act as bases to proton donors, an ideal crystallization partner would be one that can function well as either an acid or a base Such a reagent is Erdmann’s anion, which is simple to prepare in multigram quantities at a very low cost and can act both as a proton acceptor and as a proton donor to various cationic drugs. Representative samples (cocaine, methamphetamine, methylone) were selected in order to demonstrate the practical use of the reagent They were crystallized as Erdmann’s salts by the addition of a 5% aqueous solution of either ammonium or potassium Erdmann’s anion and a few milligrams of the target drug compound. We describe the crystal structures of both the potassium and ammonium salts at 100K using complete spheres of data and give a detailed description of the structures of complexes of three cationic drugs with Erdmann’s anion

Materials and Methods
Syntheses and Crystallization
Preparation of the Drug Crystals
Crystallographic Studies
Structures
Structure of the Ammonium
Structures of Structures the Erdmann’s
A Caveat
Packing Considerations in the Three Drug Complexes
The program
Racemic
Summary of Experimental Results
Conclusions
Full Text
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