TY - JOUR

T1 - Solvothermal Approach to the Synthesis of Triangular Re(III) Iodide and Bromide Cluster Complexes

AU - Mikhailov, M. A.

AU - Sukhikh, T. S.

AU - Sokolov, M. N.

N1 - Funding Information: We dedicate this manuscript to the memory of Pamela Sklar, whose guidance and wisdom we miss daily. We strive to continue her legacy of thoughtful, innovative, and collaborative science. Data were generated as part of the CommonMind Consortium supported by funding from Takeda Pharmaceuticals Company Limited, F. Hoffman-La Roche Ltd and NIH grants R01MH085542, R01MH093725, P50MH066392, P50MH080405, R01MH097276, RO1-MH-075916, P50M096891, P50MH084053S1, R37MH057881 and R37MH057881S1, HHSN271201300031C, AG02219, AG05138 and MH06692. Brain tissue for the study was obtained from the following brain bank collections: the Mount Sinai NIH Brain and Tissue Repository, the University of Pennsylvania Alzheimer’s Disease Core Center, the University of Pittsburgh NeuroBioBank and Brain and Tissue Repositories and the NIMH Human Brain Collection Core. CMC Leadership: P. Sklar, J. Buxbaum (Icahn School of Medicine at Mount Sinai), B. Devlin, D. Lewis (University of Pittsburgh), R. Gur, C.-G. Hahn (University of Pennsylvania), K. Hirai, H. Toyoshiba (Takeda Pharmaceuticals Company Limited), E. Domenici, L. Essioux (F. Hoffman-La Roche Ltd), L. Mangravite, M. Peters (Sage Bionetworks), T. Lehner, B. Lipska (NIMH). ROSMAP study data were provided by the Rush Alzheimer’s Disease Center, Rush University Medical Center, Chicago. Data collection was supported through funding by NIA grants P30AG10161, R01AG15819, R01AG17917, R01AG30146, R01AG36836, U01AG32984, U01AG46152, the Illinois Department of Public Health, and the Translational Genomics Research Institute. The iPSYCH-GEMS team acknowledges funding from the Lundbeck Foundation (grant no. R102-A9118 and R155-2014-1724), the Stanley Medical Research Institute, an Advanced Grant from the European Research Council (project no. 294838), the Danish Strategic Research Council the Novo Nordisk Foundation for supporting the Danish National Biobank resource, and grants from Aarhus and Copenhagen Universities and University Hospitals, including support to the iSEQ Center, the GenomeDK HPC facility, and the CIRRAU Center. The Genotype-Tissue Expression (GTEx) Project was supported by the Common Fund of the Office of the Director of the National Institutes of Health, and by NCI, NHGRI, NHLBI, NIDA, NIMH, and NINDS. The data used for the analyses described in this manuscript were obtained from the GTEx Portal on September 5, 2016. BrainSpan: Atlas of the Developing Human Brain (Internet). Funded by ARRA Awards 1RC2MH089921-01, 1RC2MH090047-01, and 1RC2MH089929-01. H.K.I. was supported by R01 MH107666-01. Publisher Copyright: © 2021, Pleiades Publishing, Ltd. Copyright: Copyright 2021 Elsevier B.V., All rights reserved.

PY - 2021/7

Y1 - 2021/7

N2 - Crystalline Re3I9 (1) is formed in a quantitative yield upon the hydrothermal reaction of NaReO4 with concentrated HI at 200°C. The reaction of Re3I9 with HBr at 200°C results in complete replacement of iodide ligands with bromide ligands with retention of the cluster core. The addition of pyridine to the reaction mixture leads to crystallization of the pyridinium salt (PyH)2[Re3Br11(H2O)] · 4H2O (2). In the presence of phosphoric acid, (PyH)2[Re3Br9(PO4H)]·H2O (3) and (Et4N)2[Re3Br9(PO4H)]·2H2O (4) were isolated. The crystal structures of the compounds 2–4 were determined by single crystal X-ray diffraction. Complexes 1 and 4 were characterized by powder X-ray diffraction. The Re/halogen ratio for compounds 1–4 was determined by energy dispersive spectroscopy. Elemental analysis and 31P NMR spectroscopy data were obtained for compound 4, and vibrational spectra were measured for 1 (far-IR range) and 4 (near-IR range). The data for thermal stability in inert atmosphere were obtained for 1.

AB - Crystalline Re3I9 (1) is formed in a quantitative yield upon the hydrothermal reaction of NaReO4 with concentrated HI at 200°C. The reaction of Re3I9 with HBr at 200°C results in complete replacement of iodide ligands with bromide ligands with retention of the cluster core. The addition of pyridine to the reaction mixture leads to crystallization of the pyridinium salt (PyH)2[Re3Br11(H2O)] · 4H2O (2). In the presence of phosphoric acid, (PyH)2[Re3Br9(PO4H)]·H2O (3) and (Et4N)2[Re3Br9(PO4H)]·2H2O (4) were isolated. The crystal structures of the compounds 2–4 were determined by single crystal X-ray diffraction. Complexes 1 and 4 were characterized by powder X-ray diffraction. The Re/halogen ratio for compounds 1–4 was determined by energy dispersive spectroscopy. Elemental analysis and 31P NMR spectroscopy data were obtained for compound 4, and vibrational spectra were measured for 1 (far-IR range) and 4 (near-IR range). The data for thermal stability in inert atmosphere were obtained for 1.

KW - aqua complexes

KW - bromides

KW - clusters

KW - iodides

KW - phosphate complexes

KW - rhenium

KW - X-ray diffraction analysis

UR - http://www.scopus.com/inward/record.url?scp=85109843066&partnerID=8YFLogxK

U2 - 10.1134/S0036023621070081

DO - 10.1134/S0036023621070081

M3 - Article

AN - SCOPUS:85109843066

VL - 66

SP - 969

EP - 974

JO - Russian Journal of Inorganic Chemistry

JF - Russian Journal of Inorganic Chemistry

SN - 0036-0236

IS - 7

ER -