Single-crystal X-ray diffraction experiments of 1 –4 were carried out with a Bruker SMART APEX II diffractometer (Bruker, Billerica, MA, United States). The APEX II software [56 ] was used to collect frames of data, index reflections, determine lattice constants, and integrate the intensities of reflections as well as for scaling and absorption correction. The structures were solved using a dual-space algorithm and refined in an anisotropic approximation for non-hydrogen atoms against F 2 (hkl). Hydrogen atoms of methyl, methylene, and aromatic fragments were calculated according to those idealized geometries and refined with constraints applied to C-H and N-H bond lengths and equivalent displacement parameters (U eq (H) = 1.2U eq (X), X—central atom of XH₂ group; U eq (H) = 1.5U eq (Y), Y—central atom of YH₃ group). All structures were solved with the ShelXT [57 (link)] program and refined with the ShelXL [58 (link)] program. Molecular graphics were drawn using the OLEX2 [59 (link)] program.
Smart apex 2 diffractometer
Manufactured by Bruker
Sourced in United States, Germany
The SMART APEX II is a single-crystal X-ray diffractometer manufactured by Bruker. It is designed for the collection and analysis of X-ray diffraction data from single-crystal samples. The instrument features advanced optics, high-precision goniometry, and state-of-the-art detectors to provide accurate and reliable data for a wide range of crystallographic applications.
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Lab products found in correlation
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D8 focus diffractometer, by Bruker (1 mentions)
Dm irb inverted fluorescence microscope, by Leica (1 mentions)
Quanta 450 sem, by Thermo Fisher Scientific (1 mentions)
Esquire 3000 plus lc ms apparatus, by Bruker (1 mentions)
Uv 1800 spectrophotometer, by Shimadzu (1 mentions)
Am 400 spectrometer, by Bruker (1 mentions)
X ray diffractometer, by Rigaku (1 mentions)
Kappa ccd diffractometer, by Bruker (1 mentions)
Spectrum two ft ir spectrometer, by PerkinElmer (1 mentions)
Chi760e electrochemical workstation, by Chenhua (1 mentions)
Evolution 220 spectrometer, by Thermo Fisher Scientific (1 mentions)
Emx plus 10 12 spectrometer, by Bruker (1 mentions)
600 mhz nuclear magnetic resonance spectrometer, by Bruker (1 mentions)
Ultraflex maldi tof ms spectrometer, by Bruker (1 mentions)
Nicolet is50 ft ir infrared spectrometer, by Thermo Fisher Scientific (1 mentions)
20 protocols using smart apex 2 diffractometer
1
Single-Crystal X-ray Diffraction of Compounds 1-4
2
Single Crystal X-ray Diffraction Analysis
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Single-crystal X-ray diffraction data were collected on a Bruker SMART APEX II diffractometer (Bruker, Ettlingen, Germany) using graphite-monochromated Cu Kα radiation (λ = 1.54178 Å). The collected data were corrected for absorption with SADABS [51 ]. The structures were solved by direct methods and refined by full-matrix least-squares on F2 using SHELXTL-2016 [52 (link)]. Non-hydrogen atoms were refined anisotropically. The H atoms on the phenolic and alcoholic –OH, water, and cationic NH2 were placed in calculated positions either by HFIX instructions or by Calc-OH program in the WinGX suite [53 (link)]. Crystallographic data for the crystal structures have been deposited in the Cambridge Crystallographic Data Centre (CCDC) with supplementary numbers of 2041676 (I ) and 2041677 (II ). These data can be obtained free of charge from the CCDC via www.ccdc.cam.ac.uk/data_request/cif . A summary of the key crystallographic data are listed in Table 1 .
3
Single-Crystal X-Ray Diffraction Analysis
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Single‐crystal X‐ray diffraction analyses were measured on a BRUKER‐AXS SMART APEX II diffractometer equipped with a CCD detector. All measurements were performed using monochromatized MoKα radiation from an Incoatec microfocus sealed tube at 100 K (cf. Table S1). Absorption corrections were performed semi‐empirical from equivalents. Structures were solved by direct methods (SHELXS‐97)75 and refined by full‐matrix least‐squares techniques against F2 (SHELXL‐2014/6).75 Full experimental details for single‐crystal X‐ray diffraction analyses of all compounds are provided in the Supporting Information.
4
Single-crystal X-ray Diffraction Analysis
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Single-crystal X-ray diffraction data were collected on a Bruker SMART APEX II diffractometer using graphite-monochromated Mo Kα radiation (λ = 0.71073 Å). The collected data were corrected for absorption with SADABS [39 (link)]. The structures were solved by direct methods and refined by full-matrix least-squares on F2 using SHELXTL-2016 [40 ]. Non-hydrogen atoms were refined anisotropically. The H atoms on the phenolic and alcoholic –OH and the cationic NH2 were placed in calculated positions either by HFIX instructions or with the Calc-OH program in the WinGX suite [41 (link)]. Crystallographic data for the crystal structures were deposited in the Cambridge Crystallographic Data Centre (CCDC) with supplementary numbers of 2090218 (RSV), 2090219 (RSV-L-Pro), 2090216 (PD), and 2090217 (PD-L-Pro). These data can be obtained free of charge from the CCDC via https://www.ccdc.cam.ac.uk/structures/ .
5
X-ray Diffraction Structural Analysis
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X-ray diffraction data for
all complexes were collected on single crystals mounted on a glass
fiber using Paratone oil. Data was acquired with a Bruker SMART APEX
II diffractometer equipped with a charge-coupled device detector cooled
to 88 K and using Mo Kα radiation (λ = 0.71073 Å).
The SMART program package was used to determine unit-cell parameters
and for data collection. Raw frame data were processed using SAINT
and SADABS to yield the reflection data file. Subsequent calculations
were carried out using the SHELXTL program suite. The structures were
solved by direct methods and refined on F2 using full-matrix least-squares techniques. Analytical scattering
factors for neutral atoms were used throughout the analyses. Hydrogen
atoms were generated at calculated positions and refined using a riding
model. ORTEPs were generated using ORTEP-3 for Windows.
all complexes were collected on single crystals mounted on a glass
fiber using Paratone oil. Data was acquired with a Bruker SMART APEX
II diffractometer equipped with a charge-coupled device detector cooled
to 88 K and using Mo Kα radiation (λ = 0.71073 Å).
The SMART program package was used to determine unit-cell parameters
and for data collection. Raw frame data were processed using SAINT
and SADABS to yield the reflection data file. Subsequent calculations
were carried out using the SHELXTL program suite. The structures were
solved by direct methods and refined on F2 using full-matrix least-squares techniques. Analytical scattering
factors for neutral atoms were used throughout the analyses. Hydrogen
atoms were generated at calculated positions and refined using a riding
model. ORTEPs were generated using ORTEP-3 for Windows.
6
High-Pressure Single-Crystal Diffraction of 1
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Single crystal diffraction data for a crystal of 1 mounted on a Kapton loop were collected at room temperature using a Bruker D8 Venture diffractometer. For high pressure studies, a crystal of 1 (0.15 × 0.10 × 0.05 mm3) was loaded into a Merrill–Bassett diamond anvil cell (DAC) equipped with 600 mm culet-cut diamonds and conically-ground WC backing plates.27 The hydrostatic medium was Fluorinert FC-77, and the pressure was calibrated using a ruby chip. High pressure single-crystal X-ray diffraction data were collected at room temperature on a Bruker SMART APEX II diffractometer with graphite-monochromated Mo Kα radiation (λ = 0.71073 Å). The data were integrated using the program SAINT28 while employing dynamic masks to account for regions shaded by the pressure cell, and absorption corrections were carried out with SADABS.29 The ambient pressure structure was solved using SUPERFLIP.30 This solution was used as the basis for the solution of the high pressure data, and all refinements were against F2 using CRYSTALS.31 All non-H atoms were refined anisotropically. For the MeDABCO ligands at high pressure, the bond distances were restrained and the anisotropic displacement parameters of the ligands were subject to similarity restraints. All metal–ligand distances, angles, and torsion angles were refined freely. H atoms were fixed in geometrically calculated positions.
7
X-ray Crystallographic Structural Analysis
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A Bruker SMART APEX II diffractometer was used to
collect all data. The APEX28 program package
was used to determine the unit-cell parameters and for data collections.
The raw frame data was processed using SAINT9 and SADABS10 to yield the reflection
data file. Subsequent calculations were carried out using the SHELXTL11 program. Structures were solved by direct methods
and refined on F2 by full-matrix least-squares
techniques. Analytical scattering factors12 for neutral atoms were used throughout the analysis. Hydrogen atoms
were included using a riding model. Hydrogen atoms H(1) of NMe4[FeIIITST(OH)] and H(1) and H(2) NMe4[FeIIMST(OH2)] were located from a difference-Fourier
map and refined (x, y, z, and Uiso). Data sets of both NMe4[FeIIITST(OH)] and NMe4[FeIII–O–MST] contained several high residuals in the final
difference-Fourier map. It was not possible to determine the nature
of the residuals, although it is probable that a pentane or DCM solvent
molecule was present. The SQUEEZE routine in the PLATON13 program package was used to account for the
electrons in the solvent-accessible voids. In the NMe4[FeIIMST(OH2)] structure, the (NMe4)+ counterion was disordered. Carbon atoms C(35)–C(40)
were included using multiple components with partial site-occupancy
factors.
collect all data. The APEX28 program package
was used to determine the unit-cell parameters and for data collections.
The raw frame data was processed using SAINT9 and SADABS10 to yield the reflection
data file. Subsequent calculations were carried out using the SHELXTL11 program. Structures were solved by direct methods
and refined on F2 by full-matrix least-squares
techniques. Analytical scattering factors12 for neutral atoms were used throughout the analysis. Hydrogen atoms
were included using a riding model. Hydrogen atoms H(1) of NMe4[FeIIITST(OH)] and H(1) and H(2) NMe4[FeIIMST(OH2)] were located from a difference-Fourier
map and refined (x, y, z, and Uiso). Data sets of both NMe4[FeIIITST(OH)] and NMe4[FeIII–O–MST] contained several high residuals in the final
difference-Fourier map. It was not possible to determine the nature
of the residuals, although it is probable that a pentane or DCM solvent
molecule was present. The SQUEEZE routine in the PLATON13 program package was used to account for the
electrons in the solvent-accessible voids. In the NMe4[FeIIMST(OH2)] structure, the (NMe4)+ counterion was disordered. Carbon atoms C(35)–C(40)
were included using multiple components with partial site-occupancy
factors.
8
Comprehensive Characterization of Novel Materials
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Scanning electron microscope (SEM) images were captured by a FEI Quanta 450 SEM. Differential scanning calorimetry (DSC) heating curves were acquired by a Setaram μDSC7-Evo instrument (heating rate, 1.0 °C min−1). 1H NMR spectra were obtained by using a Bruker AM400 spectrometer. Powder X-ray diffraction (PXRD) patterns were recorded on a Bruker D8 Focus diffractometer with Cu-Kα radiation (λ = 1.5418 Å). Single-crystal X-ray diffraction (SCXRD) data were collected on a Bruker Smart APEX II diffractometer. Fourier transform infrared (FT-IR) spectra were recorded by using a Nicolet AVATAR 360 spectrometer in the region between 4000 and 400 cm−1 at 4 cm−1 spectral resolution. Mass spectra were collected on a Bruker Dalton Esquire 3000 plus LC-MS apparatus. Rheological data were obtained by a HAAKE RheoStress 6000 stress-controlled rheometer with parallel plate type geometry (plate diameter, 3.5 cm). Ultraviolet-visible (UV-vis) absorption spectra were recorded by using a Shimadzu UV-1800 spectrophotometer. Cell viability was observed under a Leica DMIRB inverted fluorescence microscope.
9
Single Crystal Diffraction Analysis of Compound 1
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A Bruker SMART APEX II diffractometer with graphite-monochromated MoKα radiation (λ = 0.71073 Å) was used for obtaining single crystal data on compound 1 with acceptable dimensions. The molecular structure was solved using the SHELXT 2014/4 structure solution program.44 (link) Least squares refinements of all reflections within the hkl range −7 ≤ h ≤ 7, −19 ≤ k ≤ 19, −27 ≤ l ≤ 27 were used to figure out the unit cell parameters and crystal-orientation matrices. The collected data (I > 2σ(I)) was integrated using the SAINT45 program, and the absorption correction was performed using SADABS.46 Anisotropic thermal parameters were used to refine non-hydrogen atoms. Each hydrogen atom was positioned in its geometrically ideal location and forced to ride on its parent atom. Table S1 (ESI† ) provides a summary of the crystallographic data for compound 1, and Table S2 (ESI† ) lists the specific bond lengths and bond angles.
10
Molecular Structure Determination by XRD
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