How to grow crystals for X-ray crystallography

A catalog of techniques, tips, tricks, and encouragement for growing crystals suitable for X-ray crystallography.

Using cocrystals as a tool to study non-crystallizing mol­ecules: crystal structure, Hirshfeld surface analysis and com­putational study of the 1:1 cocrystal of (E)-N-(3,4-di­fluoro­phen­yl)-1-(pyridin-4-yl)methanimine and acetic acid

Using a cocrystal of a mol­ecule that does not crystallize, we reveal that π–π inter­actions between aromatic rings are present with only two F atoms in the aromatic ring.

Crystal structure and cryomagnetic study of a mononuclear erbium(III) ox­amate inclusion com­plex

The synthesis, crystal structure and magnetic properties are reported for an erbium(III) ox­am­ate com­plex which can be considered a novel spin qubit candidate.

Synthesis of organotin(IV) heterocycles containing a xanthenyl group by a Barbier approach via ultrasound activation: synthesis, crystal structure and Hirshfeld surface analysis

An approach to form Sn—C bonds based on Barbier-type reactions assisted by sonochemical activation of the Mg surface is an easy and successful option to yield organotin mono­nuclear heterocyclic com­pounds when a xanthenyl moiety is used.

Supra­molecular inter­actions in cocrystals of benzoic acid derivatives with selective COX-2 inhibitor etoricoxib

The structures of three 1:1 cocrystal forms of etoricoxib (ETR) with benzoic acid, 4-fluoro­benzoic acid and 4-nitro­benzoic acid were characterized by X-ray diffraction (single crystal and powder) and thermal differential scanning calorimetry–thermogravimetry techniques. Due to the influence of the different acids, ETR shows different conformations.

3-[(Benzo-1,3-dioxol-5-yl)amino]-4-meth­oxy­cyclo­but-3-ene-1,2-dione: polymorphism and twinning of a precursor to an anti­mycobacterial squaramide

3-[(Benzo-1,3-dioxol-5-yl)amino]-4-meth­oxy­cyclo­but-3-ene-1,2-dione forms concomitant polymorphs, namely, block-shaped crystals of a monoclinic form I (space group P2₁/c, Z = 8, Z′ = 2) and needle-shaped crystals of a triclinic form II (space group P, Z = 4, Z′ = 2), the latter of which exhibits twinning by pseudomerohedry.

Synthesis, spectroscopic and crystallographic characterization of various cymantrenyl thio­ethers [Mn{C₅H_xBr_y(SMe)_z}(PPh₃)(CO)₂]

Several manganese com­plexes of the type [MnCp(PPh₃)(CO)₂] containing a cyclo­penta­dienyl (Cp) ligand with one to five SMe substituents were prepared and studied by X-ray crystallography. In these structures, a few S⋯S and/or S⋯Br inter­actions occur, and these are sometimes of significant importance for the arrangement of the mol­ecules in the crystal.

A novel one-dimensional thio­cyanate-bridged cobalt(III) com­plex: synthesis, crystal structure characterization and Hirshfeld surface analysis

In a new polymeric cobalt(III) coordination com­plex containing Schiff base and bridging thiocyanate ligands, the Co^III ion adopts a distorted octa­hedral shape where the metal ion is attached to two thio­cyanate ligands in the axial positions and two Schiff base ligands in the equatorial plane. Inter­molecular π–π, C—H⋯π and hydrogen-bond inter­actions are operative in the crystal packing.

Na[GeF₅]·2HF: the first quarternary phase in the H–Na–Ge–F system

trans-Penta­fluoro­germanate di­hy­dro­gen fluoride represents the first quarternary phase in the system H–Na–Ge–F, and the third Na–Ge–F phase after the X-ray structure analyses of Na₂GeF₆ and CsNaGeF₆. The crystal structure of trans-penta­fluoro­germanate di­hy­dro­gen fluoride consists of chains of [GeF₆] octa­hedra and chains of penta­gonal bipyramidal [NaF₇] polyhedra. The Raman and IR spectra show the expected vibrational modes.

Crystal structure of the cytotoxic macrocyclic trichothecene Isororidin A

The absolute configuration of Isororidin A, isolated from the fungus Myrothesium verrucaria, has been determined by X-ray crystallography.

Synthesis, structure and red-light emission of a manganese halide directed by a methyl­diphenyl­phosphine oxide com­plex

A new manganese-based halide was synthesized using methyl­diphenyl­phosphine oxide (MDPPO) and MnCl₂, where [Mn(MDPPO)₄(H₂O)₂]²⁺ served as the cation and [MnCl₄]²⁻ as the anion, demonstrating efficient red-light emission. Both spectroscopic characterization and theoretical calculations were conducted to elucidate the photoluminescence mechanism.

Crystal structure and Hirshfeld surface analysis of two iHOFs based on CH⋯NC hydrogen bonding

One of the relatively weak inter­molecular inter­actions is the CH⋯NC hydrogen-bonding inter­action of multiple cyanide groups in pyridinium-functionalized building blocks. This provides an opportunity to design ionic hydrogen-bonded organic frameworks (iHOFs) triggered by template counter-ions with hierarchical self-assembly.

Crystal structure and characterization of monascin from the extracts of Monascus purpureus-fermented rice

The com­pound monascin was extracted from Monascus purpureus-fermented rice and a novel solid form has been successfully crystallized and characterized using single-crystal X-ray diffraction.

The pattern of bifurcated hydrogen bonds in thio­urea cocrystals with diazine derivatives: experimental and quantum theoretical studies

The structures of two cocrystals were determined, i.e. thio­urea with pyrazine N-oxide and phenazine. In the crystal structures, both mol­ecular components are linked by N—H⋯N hydrogen bonds. Moreover, inter­actions of the N—H⋯S type are observed between thio­urea mol­ecules creating synthons. Furthermore, bifurcated hydrogen bonds between the thio­urea mol­ecule and azine derivatives play a significant role in both structures. This emerging motif was thoroughly examined using quantum chemistry methods.

Comparison of the crystal structures of the JAK1/2 inhibitor ruxolitinib and its hydrate and phos­phate

The crystal structures of ruxolitinib and its dihydrate and phos­phate are described in detail and com­pared through the analysis of both Hirshfeld surfaces and fingerprint plots.