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27 protocols using 240c elemental analyzer

1

Metal-Organic Complexation and Biomolecular Interactions

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All reagents and
solvents used in this synthesis were commercially available. Reagent-grade
chemicals were used in this experiment. Hence, no further purification
was needed. Salicylaldehyde, 5-bromo Salicylaldehyde, 4-bromo aniline,
ctDNA, HSA, EB, and DAPI were obtained from Sigma-Aldrich Chemicals.
CuCl2, ZnCl2, and triethyl amine (Et3N) were purchased from Merck. Elemental analyses were performed using
a PerkinElmer 240C elemental analyzer. Electronic absorption spectral
data were collected by using a PerkinElmer UV–vis Lambda 365
spectrophotometer at room temperature. The concentration of ctDNA
per nucleotide was determined by absorption spectroscopy using a molar
extinction coefficient (€) 6600 (M–1 cm–1) at 260 nm. ctDNA interaction studies were performed
in a citrate-phosphate (CP) buffer of 10 mM [Na+] at pH
7.40 containing 0.5 mM Na2HPO4, and HSA interaction
studies were performed in Tris buffer.
Caution! Mercury salts are extremely toxic, so proper caution should be taken
before use.
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2

Structural Characterization of Compounds

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The reagents and solvents employed were commercially available and used as received without further purification. Single-crystal X-ray diffraction data were collected with a Rigaku Saturn 70 CCD, a Bruker APEX-II diffractometer or a Bruker D8 VENTURE TXS PHOTON 100 equipped with graphite monochromated Mo Kα radiation (λ = 0.71073 Å) using either the ω or the φ–ω scan mode. Elemental analyses of carbon, hydrogen and nitro­gen were performed with a Perkin Elmer 240C elemental analyzer. The infrared spectra were measured by a Magna-IR 750 spectrophotometer in the 4000–400 cm−1 region (KBr pellet). Thermogravimetric analyses (TGA) were carried out on a NETZSCH STA 449C unit at a heating rate of 10°C min−1 under a nitro­gen atmosphere. Photoluminescence analyses were performed on a Perkin Elemer LS55 fluorescence spectrometer.
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3

Characterization of Novel Compounds

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All
reagent- or analytical-grade chemicals and solvents were collected
from commercial sources and used without further purification. Elemental
analysis was carried out using a PerkinElmer 240C elemental analyzer.
Infrared spectra (400–4000 cm–1) were recorded
using KBr pellets on a Nicolet Magna IR 750 series-II FT-IR spectrophotometer.
Absorption spectral data were collected using a Cary 60 spectrophotometer
(Agilent) with a 1 cm path length quartz cell. Electron spray ionization
mass (ESI-MS positive) spectra were noted using a MICROMASS Q-TOF
mass spectrometer. A Fluromax-4 spectrofluorimeter was used to collect
emission spectral data at room temperature (298 K) in HEPES buffer
at pH = 7.4 solution under degassed condition. A time-resolved spectrofluorometer
from IBH, U.K., was used to collect the fluorescence lifetime data, 1H and 13C NMR spectral data were collected using
Bruker 400 and 300 spectrometers in DMSO-d6 solvent.
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4

Thermal and Structural Analysis of Complex 1

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All reagents are analytically pure grade in the experiment and are not further purified for use. Thermogravimetric analysis was measured on a NETZSCH STA 449 F5 Jupiter TGA analyzer (Selb, Germany) using an empty Al2O3 crucible as the standard. Measuring temperature ranges from 25 to 800 °C with a heating rate of 10 °C min−1 under N2 atmosphere. Powder X-ray diffraction patterns of the title complex were obtained using a Shimadzu XRD-6000 X-ray diffractometer (Kyoto, Japan) with Cu-Kα (λ = 1.5418 Å) radiation at room temperature and 2θ ranging from 5° to 50°. Perkin Elmer (Waltham, MA, USA) 240C elemental analyzer was used to obtain elemental analyses of complex 1. Infrared spectra were obtained on a Bruker VERTEX 80 spectrometer (Billerica, MA, USA) in the 4000–400 cm−1 region. Fluorescence data were collected on the Perkin Elmer LS55 Fluorescence Spectrophotometer.
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5

Multimodal Analysis of Magnetic Material

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Using the Nexus 870 FT-IR spectrometer, IR spectroscopy was performed with KBr particles in the range of 400–4000 cm−1. The elemental analyses of C, H, and N were recorded on a PerkinElmer 240C elemental analyzer. TGA was measured from 30 to 800 °C on a NETZSCH STA 449F3 analyzer at a heating rate of 5 °C min−1 under a N2 atmosphere. The ac magnetic susceptibility data were collected using a MPMS-XL7 Squid magnetometer (test conditions: Hac = 5 Oe, Hdc = 0 Oe, frequencies ranging from 1 to 1488 Hz). The dc magnetic susceptibility data were measured in the temperature range of 1.8–300 K. The experimental susceptibilities were corrected for the diamagnetism of the samples as estimated from Pascal's tables31d and the sample holder by a previous calibration. Pulsed-high-field magnetization measurements were performed at 1.9 K using a home-made pulsed field up to 30 T at the Wuhan National High Magnetic Field Center, P. R. China. The sweeping rate for the magnetic field was 5.0 kT s−1 on an average. The low-field magnetization data (on SQUID) were used to calibrate the high-field magnetization curve, which is a standard way to process the high field magnetization data.31e
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6

IR and Elemental Analysis Protocol

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IR spectra (KBr pellet) were
recorded on a PerkinElmer RXI FT-IR spectrophotometer in the range
of 4000–400 cm–1. PerkinElmer 240C elemental
analyzer was used for elemental analysis (C, H, N).
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7

Spectroscopic Characterization of Novel Compounds

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Chemicals (reagent grade)
were purchased from Sigma-Aldrich Co. Freshly boiled doubly distilled
water was used for synthesis purposes. IR spectra in the range of
4000–400 cm–1 were recorded using a Perkin-Elmer
RXI FT-IR spectrophotometer. Elemental analyses (percentages of C,
H, and N) were performed on a Perkin-Elmer 240 C elemental analyzer. 1H NMR spectra of compound (1) was recorded on
a Bruker 300 MHz instrument using deuterated dimethyl sulfoxide (DMSO).
The HRMS QTOF Micro YA263 mass spectrometer was used to obtain mass
spectra of (1). A Rigaku-TTRAX-III diffractometer (Cu
Kα radiation (λ = 1.5406 Å)) was used to collect
powder X-ray diffraction (PXRD) data of the compounds (24). Figure S5 compares
the PXRD pattern of the salts (24) with their simulated pattern.
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8

Fluorescent Nanomaterial Sensing of NACs

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All reagent-grade chemicals were purchased for the synthesis and were used as received. A PerkinElmer 240C elemental analyzer was used for carbon, hydrogen, and nitrogen elemental analysis. A PerkinElmer FT-IR spectrum RX1 spectrometer was used to record the infrared spectrum (IR) of the material using the KBr method (4000–500 cm−1). Fluorescence spectra were recorded using a PerkinElmer LS-45 fluorometer. With 1 mg of CP 1 dispersed in 5 mL of acetonitrile (ACN) solvent, the luminous properties were examined in a dispersive state for further investigation of the photophysical characteristics and sensitivity investigations. Different NACs were used in the sensing study, including 4-nitrophenol (NP), nitrobenzene (NB), 3,5-dinitrobenzoic acid (3,5-DNBA), 2,4,6-trinitrophenol (TNP), 4-nitrobenzoic acid (NBA), nitromethane (NM), 2,4-dinitrophenol (2,4-DNP) and 2,4-dinitrotoluene (2,4-DNT) in the solution of 10−4 M can.
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9

Elemental and Spectroscopic Analysis

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Elemental analyses (carbon, hydrogen and nitrogen) were performed using a Perkin Elmer 240C elemental analyzer. IR spectra in KBr (4500–500 cm−1) were recorded with a Perkin Elmer Spectrum Two spectrophotometer. Electronic spectrum of complex 1 (in DMF) and that of complexes 2–4 (in CH3CN) were recorded on a Shimadzu UV-1700 UV-Vis spectrophotometer. The magnetic susceptibility measurements were performed with an EG and PAR vibrating sample magnetometer, model 155 at room temperature (300 K) in a 5000 G magnetic field, and diamagnetic corrections were performed using Pascal's constants.
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10

Characterization of Synthesized Materials

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All reagents and solvents employed for this synthesis were purchased from commercial sources and used as received without further purification. The elemental analyses (C, H, and N) were determined with a PerkinElmer 240C elemental analyzer. Infrared spectra were recorded with a Varian 640 FT-IR spectrometer over the range of 500–4000 cm−1 with the use of KBr pellets as sample matrices. Powder X-ray diffraction (PXRD) data was collected using a Rigaku diffractometer with Cu Kα radiation. Thermogravimetric analysis (TGA) measurements were performed with a METTLER TOLEDO thermal analyzer at a heating rate of 5 °C min−1 under a N2 atmosphere. The morphology and structure of the sample was characterized via scanning electron microscopy (SEM, Nova Nano SEM 430) and high resolution transmission electron microscopy (HRTEM, JEOL 2010 at 200 kV). The specific surface area and pore structure of the sample was investigated with an automatic volumetric sorption analyzer (ASAP 2020 M) using N2 as the adsorbate at −196 °C. X-ray photoelectron spectroscopy (XPS) was performed using an Escalab 250 with an Al Kα radiation. UV-Vis absorption spectra were recorded with the use of an SP-1900 UV-Vis spectrophotometer.
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