X-ray diffraction experiments for 1, 3–5 were carried out at 120 K with a Bruker APEX2 DUO CCD diffractometer, those for 2 at 150 K with a Bruker AXS Smart Apex II CCD diffractometer, both using graphite monochromated Mo-Kα radiation (l = 0.71073 Å). Using Olex2,36 (link) the structures were solved with the ShelXT37 (link) structure solution program using Intrinsic Phasing and refined with the olex2.refine38 (link) refinement package using Gauss–Newton minimization against F2 in anisotropic approximation for non-hydrogen atoms. Hydrogen atoms of NH groups in 2 were located from difference Fourier synthesis; positions of other hydrogen atoms were calculated, and they all were refined in isotropic approximation within the riding model. Crystal data and structure refinement parameters for 1–5 are given in Table S1. CCDC 2112367 (1), 2112368 (2), 2112369 (3), 2112370 (4) and 2115090 (5) contain the supplementary crystallographic data for this paper (Table S1† ).
Axs smart apex 2 ccd diffractometer
Manufactured by Bruker
Sourced in United States
The AXS SMART APEX II CCD diffractometer is a laboratory instrument designed for single-crystal X-ray diffraction analysis. It utilizes a CCD (Charge-Coupled Device) detector to collect diffraction data from crystalline samples. The core function of this diffractometer is to determine the crystal structure of materials by analyzing the pattern of X-ray diffraction produced by the sample.
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Lab products found in correlation
6 protocols using axs smart apex 2 ccd diffractometer
1
X-ray Diffraction Structural Analysis
2
X-ray Structural Characterization of Metal Complexes
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A Bruker AXS SMART APEX II CCD diffractometer, which was equipped with graphite-monochromated MoKα (λα = 0.71073 Å) radiation, was used to collect the diffraction data for complexes 1 –3 [16 ], and the data were reduced by using the well-established computational procedures. The structure factors were treated with Lorentz and polarization corrections and an empirical absorption correction based on “multi-scan” [17 (link)]. The Direct or Patterson method was applied to locate the positions of some of the heavier atoms, and the remaining atoms were identified in several alternating difference Fourier maps and least-square refinements. Hydrogen atoms were added by using the HADD command in SHELXTL. The coordinated water molecule, O(8), of complex 2 is disordered such that two orientations of the oxygen atom can be found, and the occupancy of each orientation was set to be 0.5 and were refined isotropically. Moreover, the occupancy of O(8) of 3 was refined to be 0.5. Table 1 lists the basic information regarding the crystal parameters and structure refinement.
3
Single Crystal X-ray Structural Analysis
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The single crystal X-ray structures were performed on a Bruker AXS SMART APEX II CCD diffractometer (MoKα radiation, λ = 0.71073 Å, graphite monochromator) (Bruker AXS, Madison, WI, USA). Lorentz–polarization and empirical absorption correction based on a “multi-scan” were then applied to reduce and correct the reflections collected for each crystal [20 ]. While some of the heavier atoms were located by using the direct method or Patterson method, the remaining atoms were found in a series of alternating difference Fourier maps and least-square refinements and the hydrogen atoms were added by using the HADD command in SHELXTL 6.1012 [21 (link)]. Because of the serious disorder of the co-crystallized solvents in 5b ·H2O, the SQUEEZE/PLATON technique [22 (link)] was applied to remove the solvent contribution, while the elemental analysis indicates the cocrystallization of one water molecule. Table 1 lists the basic crystal parameters and structure refinement results for 1 –5b ·H2O.
4
Single-Crystal X-Ray Diffraction Analysis
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Single-crystal X-ray diffraction data for complexes 1 –9 were collected on a Bruker AXS SMART APEX II CCD diffractometer with graphite-monochromated MoKα (λα = 0.71073 Å) radiation at 296 K [30 ]. Data reduction and absorption correction were performed by using standard methods with well-established computational procedures [31 (link)]. Some of the heavier atoms were located by the direct or Patterson method, and the remaining atoms were found in a series of Fourier maps and least-squares refinements, while the hydrogen atoms were added by using the HADD command in SHELXTL. Basic information pertaining to crystal parameters and structure refinement is listed in Table 6 .
5
Single-Crystal X-Ray Diffraction of Complexes 1-8
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Single-crystal X-ray diffraction data for complexes 1 –8 were collected on a Bruker AXS SMART APEX II CCD diffractometer with graphite-monochromated MoKα (λα = 0.71073 Å) radiation at 296 K [23 ]. Data reduction and absorption correction were performed by using standard methods with well-established computational procedures. Some of the heavier atoms were located by the direct or Patterson method, and the remaining atoms were found in a series of Fourier maps and least-squares refinements, while the hydrogen atoms were added by using the HADD command in SHELXTL [24 (link)]. Table 2 lists the basic information pertaining to crystal parameters and structure refinement. CCDC no. 2238099–2238106 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/retrieving.html or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336 033; e-mail: deposit@ccdc.cam.ac.uk ; or at: http://www.ccdc.cam.ac.uk .
6
Structural Characterization of Complexes 1-6
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A Bruker AXS SMART APEX II CCD diffractometer, equipped with a graphite-monochromated MoKα radiation (0.71073 Å), was used to collect diffraction data for complexes 1 –6 . The diffraction data were then reduced by using standard methods [23 ], followed by empirical absorption corrections based on a “multi-scan”. The positions of some of the heavier atoms were located by the direct method or Patterson method, and the remaining atoms were found in a series of alternating difference Fourier maps and least-square refinements. The hydrogen atoms, except those of the water molecules, were added by using the HADD command in SHELXTL 6.1012 [24 ]. Due to the serious disordering, the solvent molecules in 3 were squeezed by using the PLATON program [20 (link)] and their diffraction data were reported without solvent contribution. Table 3 lists the crystal and structure refinement parameters for 1 –6 . The CCDC no. 2311169-2311174 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/retrieving.html or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336 033; e-mail: deposit@ccdc.cam.ac.uk ; or at http://www.ccdc.cam.ac.uk .
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