Synthesis of Gold Complexes From Diphosphine Ligands and Screening Reactions of Heterocyclic Acetylacetonato (ACAC) Ligands with Transitional Metal Complexes Page: 41
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The following are the 'H-NMR results from the reactions; note that all chemical shifts (6)
are in ppm: 6, 9.04-9.03 (d, J= 4 Hz), 6, 8.33-8.31 (d, J= 8.4 Hz), 6, 7.96-7.94, (dd, J=1.6, .4.8
Hz,), 6, 7.78-7.76, (dd, J=1.2, 8.4 Hz) and 6, 7.42-7.40, (dd, J=0.8, 1.2, 8.0 Hz). The IR
vibrational peaks of the products are: 1900 cm-, 2025 cm-, and a small sharp peak at 2300 cm-.
ReBr(CO)5
N Ethanol, Reflux N NCO
OCRt
O O CH3 O } CO
/O O
0 O
O---\
CH3
Scheme 3.2. Synthesis of Rhenium Complex 2
3.2 X-Ray Crystallography
The crystal structure determination of compounds diphosphine gold(I) complex 1 or
[Au2Cl2(bpcd)], [Au2Cl2(bppm)], ligand A, and rhenium complex 1 were carried out using a
Bruker SMART APEX2 CCD-based X-ray diffractometer. The instrument was equipped with an
Oxford low-temperature cryostat and a Mo-target X-ray tube (wavelength = 0.71k). The X-ray
data for the compounds were collected at 100(2) K. Data collections, indexing, and initial cell
refinements were carried out using APEX2.68 The frame integrations and final cell refinements
were carried out using SAINT.69 An absorption correction was applied using the program
SADABS70, and all non-hydrogen atoms were refined anisotropically. H- Atoms in the
investigated compounds were placed in idealized positions and were refined using a riding
model. The structures were examined using the Addsym subroutine of PLATON to ensure that41
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Nyamwihura, Rogers. Synthesis of Gold Complexes From Diphosphine Ligands and Screening Reactions of Heterocyclic Acetylacetonato (ACAC) Ligands with Transitional Metal Complexes, thesis, August 2015; Denton, Texas. (https://digital.library.unt.edu/ark:/67531/metadc804890/m1/54/: accessed July 16, 2024), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; .