Purple coloured single crystals of 1 suitable for X-ray analysis were obtained by slow diffusion of Et2O into an acetone solution of 1 . Crystallographic data collections were carried out on a Bruker SMART AXS diffractometer equipped with a monochromator in the Mo Kα (λ=0.71073 Å) incident beam. Single crystals of 1 were mounted on a glass fibre tip with epoxy cement. The diffraction data for 1 were collected at 100 K on a Bruker SMART AXS diffractometer equipped with a monochromator in the Mo Kα (λ=0.71073 Å) incident beam. The CCD data were integrated and scaled using the Bruker-SAINT software package, and the structure was solved and refined using SHEXTL V 6.12 (ref. 56 ). The crystallographic data and selected bond distances and angles for 1 are listed in Supplementary Tables 1 and 2 .
Smart axs diffractometer
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The SMART AXS diffractometer is a laboratory instrument designed for X-ray diffraction analysis. Its core function is to measure and analyze the diffraction patterns of various materials, providing insights into their structural properties.
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7 protocols using smart axs diffractometer
1
Single Crystal Structure Determination
2
Single-Crystal Diffraction Structural Analysis
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Single-crystal diffraction experiments were collected at 90 K using a Bruker AXS SMART diffractometer with an APEX-II CCD detector with Mo-Kα radiation. The datasets were recorded as ω-scans with a 0.4° step width and integrated with the Bruker SAINT software package.27 Multi-scan absorption corrections were applied.27 The solution and refinement of the crystal structure were carried out using the SHELX-2014 suite of programs.28 The final refinements were performed using anisotropic atomic displacement parameters for all atoms. A summary of pertinent information relating to unit cell parameters, data collection, and refinements is provided in Table 1 and the atomic parameters and interatomic distances are provided in Tables S1 and S2.† Further details of the crystal structure determination may be obtained from Fachinformationszentrum Karlsruhe, Germany, by quoting the depository number CSD-433052.
3
Single-crystal X-ray Diffraction of [Co(NH3)5N3](MnO4)2
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Single-crystal diffraction data for [Co(NH3)5N3](MnO4)2× H2O have been collected on a Bruker AXS SMART diffractometer equipped with CCD detector. More than a hemisphere of data was collected on each crystal over three batches of exposure using MoK
aradiation (l = 0.71073 Å). A fourth set of data was measured and compared to the initial set to monitor and correct for decay, which was negligible. Data processing was performed using the program SAINT [3].The absorption correction was done using an empirical method (SADABS) [3]. The structure was solved by the direct method and refined by the full-matrix least-squares method on all F12 2 data using SHELX-97 [3]. All other information regarding the refinement is also recorded in Table 1.
aradiation (l = 0.71073 Å). A fourth set of data was measured and compared to the initial set to monitor and correct for decay, which was negligible. Data processing was performed using the program SAINT [3].The absorption correction was done using an empirical method (SADABS) [3]. The structure was solved by the direct method and refined by the full-matrix least-squares method on all F12 2 data using SHELX-97 [3]. All other information regarding the refinement is also recorded in Table 1.
4
Structural Elucidation of Manganese Complexes
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Single crystals of [Mn(HN3O2)(Cl)2], 1, and 2 suitable for X-ray crystallographic analysis were obtained by the slow diffusion of Et2O into a CH3CN solution of each metal complex. These crystals were taken from the solutions by a nylon loop (Hampton Research Co.) on a handmade cooper plate and mounted on a goniometer head in a N2 cryostream. The diffraction data for [Mn(HN3O2)(Cl)2], 1, and 2 were collected at 120 K on a Bruker SMART AXS diffractometer equipped with a monochromator in the Mo Kα (λ = 0.71073 Å) incident beam. The cell parameters were determined and refined by the SMART program.77 The CCD data were integrated and scaled using the Bruker-SAINT software package.78 An empirical absorption correction was applied using the SADABS program.79 The structures were solved by direct methods, and all non-hydrogen atoms were subjected to anisotropic refinement by full-matrix least squares on F2 using SHELXTL Ver. 6.14.80 The crystallographic data and selected bond distances and angles are listed in Tables S1 and S2,† respectively.
5
Synthesis and Structural Characterization of (TMG3tren)CoII Complex
6
Synthesis and Characterization of Co(II) Complex
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Complex 1 was synthesized as follows: H2L (212 mg, 0.80 mmol, 2 equiv.) and Co(BF4)2 6 H2O (136 mg, 0.40 mmol, 1 eqequiv.) were dissolved in acetonitrile (10 ml) and NEt3 (0.5 ml) was added. The reaction mixture was stirred at room temperature. Diffusion of diethylether into the acetonitrile solution yielded pink crystals (250 mg, 0.32 mmol, 80%) of the desired complex. Those were also suitable for X-ray analysis. Elem. Anal. Calc. for C28H50CoN6O8S4 0.15 H2O C 42.65; H 6.41; N 10.66% found C 42.66; H 6.75; N 10.63%. ESI-MS calc. for C16H23CoN4O8S4 (M – 2 HNEt3+3 H+): m/z 585.9731 found 585.9713.
Elemental analysis was performed on a Perkin Elmer Analyser 240. Mass spectrometry experiments were carried out on a Bruker Daltronics Mictrotof-Q mass spectrometer.
Single crystals of1 were grown by the slow diffusion of diethylether into an acetonitrile solution. The X-ray diffraction measurement was performed on a BRUKER Smart AXS diffractometer (graphite-monochromated Mo Kα radiation, λ=0.71073 Å). SHELXS-97 and SHELXL-97 were used to solve and refine the structure49 . The CCDC deposition number is CCDC 971167.
Elemental analysis was performed on a Perkin Elmer Analyser 240. Mass spectrometry experiments were carried out on a Bruker Daltronics Mictrotof-Q mass spectrometer.
Single crystals of
7
Characterization of Nanomaterials by XRD, SEM, and TGA
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Powder X-ray diffraction (XRD) measurements were performed on a Rigaku DMAX 2500 diffractometer (Rigaku, Japan) with Cu Kα radiation (λ = 1.5406 Å) operated at 40 kV and 150 mA. The UV-visible absorption spectra were recorded using a Lambda 950 spectrophotometer (PerkinElmer, USA). High-resolution scanning electron microscopy analyses were carried out using a Hitachi S-5500 microscope (Hitachi, Japan). The operating acceleration voltage is 15 kV. Thermogravimetric analysis was carried out using a TGA 2050 instrument (TA Instruments, USA). The sample was placed on a platinum pan for each run and analyzed in air or oxygen from 25 to 900 °C at a heating rate of 5 °C min−1. GC/MS data were recorded on Agilent 5973N, and elemental analyses were obtained using a Carlo Erba EA1180 at the Organic Chemistry Research Center at Sogang University. 1H NMR and 13C NMR spectra in solution were recorded on a Varian 400 MHz Gemini operating at 400 MHz for 1H and 100 MHz for 13C, respectively. All chemical shifts were referenced to tetramethylsilane. Single-crystal X-ray diffraction data were collected using a Bruker SMART AXS diffractometer equipped with a monochromator with a Mo Kα (λ = 0.71073 Å) incident beam.
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