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9 protocols using equinox 55 s ft ir spectrophotometer

1

Characterization of UPSN Nanoparticles

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As-synthesized UPSN and UPSN-CHX were characterized using transmission electron microscopy (TEM) on FEI Tecnai TF30 at an acceleration voltage of 300 kV. Images were processed and particle diameter and pore sizes were measured using ImageJ software. Hydrodynamic diameters and surface charge were measured using dynamic light scattering (DLS, Malvern Zetasizer Nano ZS). Nitrogen adsorption-desorption isotherms were measured at 77 K on a Quantachrome Nova 4000e system. The samples were freeze-dried for 48 h and surface area was determined using the BET method. Pore size distribution data was collected by the Barrett-Joyner-Halenda (BJH) method of the desorption branch of the isotherm. Fourier transmission infrared spectroscopy measurements were carried out on a Bruker Equinox 55/S FT–IR Spectrophotometer.
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2

Spectroscopic Analysis of Organic Compounds

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Optical rotations were measured on a Perkin–Elmer 241 Polarimeter. UV spectra were recorded on an Aminco/OLIS UV-Vis Spectrophotometer. ECD spectra were recorded on an AVIV Model 420 Circular Dichroism Spectrometer. IR spectra were measured with a Bruker Equinox 55/S FT–IR Spectrophotometer. Both 1D and 2D NMR spectra were obtained using a Bruker Avance 600 MHz spectrometer with 1H{13C/15N} cryoprobe and a 500 MHz spectrometer with 13C/15N{1H} cryoprobe; chemical shifts were referenced to the residual solvent peaks (CD3OD: δH = 3.31, δC = 49.15). HRMS and MS/MS data were acquired with a Bruker MaXis 4G QTOF mass spectrometer. RP HPLC was performed using a Shimadzu Prominence HPLC system and a Phenomenex Luna C18 column (250 × 10 mm, 5 µm).
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3

Spectroscopic Characterization of Compounds

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UV spectra were recorded on an Aminco/OLIS UV-Vis Spectrophotometer (Bogart, GA, USA). IR spectra were measured with a Bruker Equinox 55/S FT–IR Spectrophotometer (Santa Barbara, CA, USA). Both 1D and 2D NMR spectra were obtained using a Bruker Avance 500 MHz spectrometer (Billerica, MA, USA) with 1H{13C/15N} cryoprobe and a 500 MHz spectrometer with 13C/15N{1H} cryoprobe; chemical shifts were referenced to the residual solvent peaks (CD3OD: δH = 3.31, δC = 49.15; DMSO-d6: δH = 2.50, δC = 39.51). HRMS data were acquired with a Bruker MaXis 4G QTOF mass spectrometer (Billerica, MA, USA). RP HPLC was performed using a Shimadzu Prominence HPLC system and a Phenomenex Luna C18 column (250 × 10 mm, 5 µm) (Torrance, CA, USA).
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4

Comprehensive Analytical Characterization Protocol

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Optical rotations were measured with a Perkin-Elmer 241 polarimeter. UV spectra were recorded with an Aminco/OLIS UV-Vis spectrophotometer. IR spectra were measured with a Bruker Equinox 55/S FT-IR spectrophotometer. 1D and 2D NMR data were recorded using a Bruker Avance 600 MHz spectrometer with a 1H{13C/15N} cryoprobe and a 500 MHz spectrometer with a 13C/15N{1H} cryoprobe, AVANCE-500, or DRX-400 spectrometers. Chemical shift values were referenced to the residual solvent peaks (CDCl3: δH7.26, δC 77.18; methanol-d4: δH 3.31, δC 49.15) HRMS data were acquired with a Bruker Maxis 4G QTOF mass spectrometer. Reverse phase (RP) HPLC was performed using a Shimadzu Prominence HPLC System and a Phenomenex Luna C-18 semi-prep column (250 × 10 mm, 5 μm), Phenomenex Luna phenyl-hexyl semi-prep column (250 × 10 mm, 5 μm) or a Phenomenex Luna phenyl-hexyl analytical column (250 × 4.6 mm, 5 μm).
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5

Spectroscopic and Microscopic Analysis

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Attenuated total reflectance Fourier-transform infrared spectroscopy (ATR FT-IR) analysis was performed on an Equinox 55/S FT-IR spectrophotometer (Bruker, Germany). The surface morphologies were measured by a Zeiss Gemini 450 field emission scanning electron microscope (SEM) (Carl Zeiss, Germany). Energy-dispersive spectroscopy (EDS) elemental mapping were performed using the Thermo Noran Energy dispersive X-ray microanalysis system (Thermo Fisher Scientific, San Jose, CA).
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6

Aerobic Synthesis and Characterization of Multidentate Ligand Complexes

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All manipulations were performed under aerobic conditions using materials as received (Aldrich Co). All chemicals and solvents were of reagent grade. The ligand OH-C6H4-CH=NC(CH2OH)3, H4L was synthesized as described previously [57 (link)]. Elemental analysis for carbon, hydrogen, and nitrogen was performed on a Perkin Elmer 2400/II automatic analyzer. Infrared spectra were recorded as KBr pellets in the range 4000–400 cm−1 on a Bruker Equinox 55/S FT-IR spectrophotometer. Variable-temperature magnetic susceptibility measurements were carried out on polycrystalline samples of 14 by using a SQUID magnetometer (Quantum Design MPMS 5.5). Diamagnetic corrections were estimated from Pascal′s constants. The program PHI was used for simulations of the magnetic susceptibility data of 3 [58 (link)].
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7

Comprehensive Analytical Characterization Workflow

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UV spectra were recorded on an Aminco/OLIS UV-Vis spectrophotometer. IR spectra were measured with a Bruker Equinox 55/S FT–IR spectrophotometer. NMR spectra were obtained in CD3OD (δH 3.34 ppm, δC 49.0 ppm) with a Bruker Avance 600 III MHz (Billerica, MA, USA) spectrometer equipped with a 1H{13C/15N/31P} cryoprobe, a Bruker Avance III 500 MHz (Billerica, MA, USA) spectrometer equipped with a 13C/15N{1H} cryoprobe, and a Bruker Avance III HD 400 MHz (Billerica, MA, USA) spectrometer. HRMS data were acquired with a Bruker MaXis™ 4G ESI-QTOF (Billerica, MA, USA) mass spectrometer. RP HPLC was performed using a Shimadzu Prominence HPLC system and a Phenomenex Gemini C18 column (250 × 30 mm). UHPLC-HRMS was acquired using a Bruker MaXis™ 4G ESI-QTOF (Billerica, MA, USA) mass spectrometer coupled with a Waters Acquity UPLC system operated by Bruker Hystar software and a C18 column (Phenomenex Kinetex 2.6 μm, 2.1 mm × 100 mm). Bruker timsTOF Pro instrument (Billerica, MA, USA) was used for the trapped ion mobility MS analysis using direct infusion with 0.003 mL/min of flow rate and ESI+ ionization source. Nebulizer gas 0.4 bar, dry gas 3.5 L/min, source temperature 220 °C, ESI voltage 4200V (+). MS spectra were collected using the following parameters: tims ramp time = 350 ms, PASEF on, scan range (m/z, 20–1000; 1/k0, 0.70–1.00 V·s/cm2.
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8

Comprehensive Analytical Characterization

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Melting points were measured on a MEL-TEMP micromelting point apparatus and were uncorrected. Optical rotations were measured on a PerkinElmer 241 polarimeter. UV spectra were recorded using an Aminco/OLIS UV–vis spectrophotometer. IR spectra were measured with a Bruker Equinox 55/S FT-IR spectrophotometer. NMR spectra were obtained in CDCl3 with a Bruker Avance 600 MHz spectrometer equipped with a 1H{13C/15N} cryoprobe and a Bruker Avance 500 MHz spectrometer equipped with a 13C/15N{1H} cryoprobe. HRMS data were acquired with a Bruker MaXis 4G QTOF mass spectrometer. Normal-phase flash chromatography was performed using a Combi Flash Rf 200 HPLC system and a 4 g gold silica gel column (Teledyne Isco).
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9

Comprehensive Analytical Characterization of Compounds

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Optical rotations were measured on a Perkin–Elmer 241 polarimeter. UV spectra were recorded on an Aminco/OLIS UV–vis spectrophotometer. ECD spectra were recorded on an AVIV model 420 circular dichroism spectrometer. IR spectra were measured with a Bruker Equinox 55/S FT-IR spectrophotometer. 1D and 2D NMR spectra were obtained on a Bruker Avance 600 MHz spectrometer with a 1H{13C/15N} cryoprobe and a 500 MHz spectrometer with a 13C/15N{1H} cryoprobe; chemical shifts were referenced to the residual solvent peaks (CDCl3: δH 7.26, δC 77.23; DMSO-d6: δH 2.50, δC 39.51). HRMS and MSMS data were acquired with a Bruker MaXis 4G QTOF mass spectrometer. RP HPLC was performed using a Shimadzu Prominence HPLC system and a Phenomenex Luna C18 column (250 × 10 mm, 5 µm). The Marfey’s method utilized a Shimadzu Prominence HPLC coupled with a Waters Micromass LCT TOF mass spectrometer.
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