A Multi-Technique Experimental and Computational Approach To Study the Dehydration Processes in the Crystals of Endomorphin Opioid Peptide Derivative
PBN-AR
Instytucja
Centrum Badań Molekularnych i Makromolekularnych Polskiej Akademii Nauk
Informacje podstawowe
Główny język publikacji
angielski
Czasopismo
CRYSTAL GROWTH & DESIGN
ISSN
1528-7483
EISSN
Wydawca
AMER CHEMICAL SOC
DOI
URL
Rok publikacji
2016
Numer zeszytu
9
Strony od-do
5312-5322
Numer tomu
16
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Język
angielski
Treść
When molecular crystals undergo partial dehydration, determining the crystal contents and precise localization of the remaining water in the crystal lattice becomes challenging, especially when the quality of crystals after dehydration is not suitable for X-ray diffraction studies. In this work, we describe a methodology that allows the determination and refinement of the structures of partially dehydrated crystals employing complementary experimental (advanced solid-state NMR techniques, differential scanning calorimetry, elemental analysis) and computational (gauge-including projector-augmented wave density functional theory) techniques. We present the power of the methodology using an opioid peptide derivative, endomorphin-2-OH (EM2-OH) heptahydrate. The advanced solid state NMR techniques 2D-PASS, inv-HETCOR, and cross polarization variable contact (CP-VC) carried out with very fast magic angle spinning were used as a source of the constraints showing differences and similarities in the structures and local molecular dynamics for crystallized and dehydrated samples. A crystal structure prediction employing the gauge-including projector-augmented wave (GIPAW) method was used for the determination and refinement of dehydrated EM2-OH. After dehydration, three out of the initial seven water molecules remain in the lattice of the EM2-OH crystals, with two water molecules located in the pockets made by the pseudocyclic conformations and one forming a bridge between two independent EM2-OH molecules.
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System-identifier
PX-58a6e634d5de215850509b22
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