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Photon 2

Manufactured by Bruker

The PHOTON II is a high-performance X-ray diffractometer designed for advanced materials research and structural analysis. It features a state-of-the-art X-ray source and detector system, providing high-quality data for a wide range of sample types and applications. The PHOTON II is capable of performing a variety of X-ray diffraction techniques, including powder, single-crystal, and thin-film analysis.

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7 protocols using photon 2

1

X-Ray Diffraction of Single Crystals

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X-ray diffraction data on single crystals with dimensions of 0.30 × 0.19 × 0.09 (1) and 0.45 × 0.13 × 0.09 mm3 (2) were collected on a Bruker D8 Venture diffractometer with a PHOTON II detector (Bruker, Mannheim, Germany) and by using monochromatized Mo-Kα radiation (λ = 0.71073 Å). Crystal parameters and refinement results for 1 and 2 are summarized in Table 1. The structures were solved by standard direct methods and subsequently completed by Fourier recycling using the SHELXTL (SHELXTL-2013/4) [56 ] software packages and refined by the full-matrix least-squares refinements based on F2 with all observed reflections. Compound 2 reveals the pseudosymmetric space group P21/n, but this symmetry breaks due to the slightly different positions of the counterions and water molecules, which lack hydrogen atoms. The final graphical manipulations were performed with the DIAMOND program [57 ]. The CCDC Deposition Numbers are 2286941 and 2286942 for 1 and 2, respectively.
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2

Single Crystal X-Ray Diffraction Protocol

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Single crystals of the complex 1 were obtained by slow cooling of a concentrated solution of the species in CH2Cl2/heptane. X-ray diffraction data were collected on a Bruker D8 Venture single crystal x-ray diffractometer equipped with a CPAD detector (Bruker Photon II), an IMS microsource with MoKα radiation (λ = 0.71073 Å) and a Helios optic using the APEX3 Version 2019-1.0 software package. For additional details about collection and refining of data, see the Supporting Information. CCDC 2302606 contains the supplementary crystallographic data for this paper. These data are provided free of charge by The Cambridge Crystallographic Data Centre.
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3

X-ray Structural Analysis of Zinc Complexes

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Single crystals for X-ray structural analyses of [ZnL3]n(BF4)2n and [Zn2(NO3)4L3]n were collected on a Bruker APEX III coated with Paraton-N oil at 100 K. Data were collected in-house on a Bruker PHOTON II equipped with an INCOATEC microfocus sealed tube (IμS 3.0) using Mo Kα. The resolution was cut off at 0.80 Å for [ZnL3]n(BF4)2n, and at 0.77 Å for [Zn2(NO3)4L3]n, after which the signal-to-noise ratio had dropped below I/σ(I) < 2.0. The data were integrated with APEX III. For [ZnL3]n(ClO4)2n, diffraction data were obtained on the 2D beamline at PAL.33 (link) Diffraction data were collected by a Rayonix MX225HS CCD area detector controlled by the PAL BL2D-SMDC Program.34 HKL3000sm was used for cell refinement and data reduction.35 The structures were resolved by intrinsic phasing/direct methods using SHELXT36 (link) and refined with SHELXL (2018/3)37 (link) for full-matrix least-squares routines on F2 and ShelXle38 (link) as a graphical user interface.
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4

Single Crystal X-Ray Diffraction Analysis

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The single crystals of 1, 2, and 4 were immersed in FOMBLIN oil (HVAC 140/13, Sigma-Aldrich), mounted on a glass fiber, and examined on a Bruker D8 VENTURE diffractometer equipped with an Oxford Cryostream 800 low-temperature device using a nickel-filtered Cu K¦Á radiation source (λ = 1.54178 Å) and a Bruker PHOTON II detector at 150 K and 298 K, respectively. All data were integrated with SAINT and a multi-scan absorption correction using TWINABS was applied. The structures were solved by direct methods using SHELXT and refined by full-matrix least-squares methods against F2 by SHELXL-2018/1. All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were refined their pivot atoms for terminal sp3 carbon atoms and 1.2 times for all other carbon atoms.
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5

Single Crystal X-Ray Diffraction Analysis

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Single crystal X-ray diffraction analysis was performed on 1–4 using either a Bruker PHOTON-II or Bruker APEX-II diffractometer. Details of the measurements are provided in the ESI.
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6

Single-Crystal X-ray Diffraction Protocol for ZIF-UC-6

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Single-crystal diffraction
data were collected using a Bruker D8 VENTURE diffractometer equipped
with a Bruker PHOTON II detector at 150 K using graphite monochromated
Mo Kα radiation (λ = 0.71073). Data reduction was done
using the APEX3 program. Absorption correction based on multiscan
was obtained by SADABS. The structure was solved and refined using
SHELXT and SHELXL packages correspondingly, using the OLEX2 program.51 (link)−53 (link) The electron density within the voids was accounted for using the
SQUEEZE program implemented in PLATON.54 (link)Crystal data for ZIF-UC-6: C13.59H12.78N8.39Zn2, Mr =
424.36, crystal dimensions 0.195 × 0.156 × 0.077 mm, Orthorhombic, a = 15.839(2) Å, b = 15.599(2) Å, c = 17.984(2) Å, α = β = γ = 90°, V = 4443.3(9) Å3, space group, Pbca, (no. 61), T = 150 K, Z = 8, 24514
measured reflections, 4524 independent reflections (Rint = 0.0593), which were used in all calculations. The
final R1 = 0.053 for 3285 observed data R[F2 > 2σ(F2)] and wR(F2) = 0.139 (all data). CSD deposition 2115059.
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7

Tibia Cortical Bone Mineral Characterization

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Tibia cortical mineral crystallinity and crystal orientation were measured by X-ray diffraction (XRD), as described in more detail in [22 (link)]. A 1-cm2 portion of cortical bone that was cut from the tibia mid-shaft was analysed in transmission mode with a X-ray single crystal diffractometer (D8 VENTURE, Bruker) equipped with an area detector (PHOTON II) and a Mo radiation (0.2 mm collimator). Measurements related to bone mineral crystallinity (maturity) and mineral organization (apatite crystal orientation) were determined from XRD data, as described in Table 1.
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