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D8 goniometer

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The D8 goniometer is a versatile X-ray diffraction (XRD) instrument designed for a wide range of applications. It features high-precision angular positioning and advanced optics for accurate and reliable measurements. The core function of the D8 goniometer is to perform XRD analysis on various materials, providing valuable insights into their structural properties.

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Lab products found in correlation

Apex 2 ccd diffractometer, by Bruker (3 mentions) Mz 75 microscope, by Leica (3 mentions) Saint software package, by Bruker (1 mentions) Shelxtl software, by Bruker (1 mentions) Sadabs, by Bruker (1 mentions)

7 protocols using d8 goniometer

1

Single Crystal X-Ray Diffraction Analysis

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Methanol was distilled from KOH and stored over 4Å molecular sieves. Other solvents and chemicals were purchased from commercial sources and used as received. A Leica MZ 75 microscope was used to identify samples suitable for analysis. A Bruker APEX-II CCD diffractometer was employed for crystal screening, unit cell determination, and data collection, which were obtained at 100 K. The Bruker D8 goniometer was controlled using the APEX3 software suite.22 The samples were optically centered with the aid of a video camera so that no translations were observed as the crystal was rotated through all positions. The X-ray radiation employed was generated from a Mo Kα sealed X-ray tube (λ = 0.71076 Å) with a potential of 50 kV and a current of 30 mA, fitted with a graphite monochromator in the parallel mode (175 mm collimator with 0.5 mm pinholes). A full matrix least squares refinement based on F2 was carried out within the Olex223 using SHEXL-201824 , 25 . All hydrogen and non-hydrogen atoms were refined using anisotropic thermal parameters. CrysAlisPro 1.171.41.31a (Rigaku Oxford Diffraction, 2019) was used for empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. The thermal ellipsoid molecular plots (50%) were produced using Olex2.23
Hoffer E., Niebuhr B.P., Pota K., Schwartz T.M., Burnett M.E., Prior T.J., Puschmann H, & Green K.N. (2021). pH-dependent concatenation of an inorganic complex results in solid state helix formation. Inorganica chimica acta, 531, 120740.
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2

Single Crystal Structure Determination

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Single crystals were prepared by slow evaporation from a mixed solvent system (hexane and CH2Cl2). Each crystal was mounted on a glass fiber, and the reflection data were collected with the omega scanning technique using a D8 goniometer (Bruker, Billerica, MA, USA). Monochromatic Mo Kα radiation (λ = 0.71075 Å) was used to analyze the complexes and all measurements were performed at room temperature (298 K). The initial structures of all the complexes were determined using a direct method using APEX3. The structural model was refined by a full-matrix least-squares method using SHELXL-2014/6. All calculations were conducted using SHELXL programs. The crystal data are summarized in Table S1, and are included in the Cambridge Crystallographic Data Centre (CCDC) database as reference numbers CCDC: 2,123,806 for B2-4, 2,123,807 for B2-5, and 2,123,809 for B3-5, respectively. The indexed database contains additional supplementary crystallographic data for this paper and may be accessed without charge at http://www.ccdc.cam.ac.uk/conts/retrieving.html (accessed on 6 November 2021).
Furoida A., Daitani M., Hisano K, & Tsutsumi O. (2021). Aggregation-Enhanced Room-Temperature Phosphorescence from Au(I) Complexes Bearing Mesogenic Biphenylethynyl Ligands. Molecules, 26(23), 7255.
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3

Crystal Structure Determination Protocol

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A Leica MZ 75 microscope was used to identify samples suitable for analysis. A Bruker APEX-II CCD diffractometer was employed for crystal screening, unit cell determination, and data collection, which was obtained at 100 K. The Bruker D8 goniometer was controlled using the APEX3 software suite, version 1.119 The samples were optically centered with the aid of a video camera, so that no translations were observed as the crystal was rotated through all positions. The X-ray radiation employed was generated from a Mo Kα sealed X-ray tube (λ = 0.71076) with a potential of 50 kV and a current of 30 mA and fitted with a graphite monochromator in the parallel mode (175 mm collimator with 0.5 mm pinholes).
Johnston H.M., Pota K., Barnett M.M., Kinsinger O., Braden P., Schwartz T.M., Hoffer E., Sadagopan N., Nguyen N., Yu Y., Gonzalez P., Tircsó G., Wu H., Akkaraju G., Chumley M.J, & Green K.N. (2019). Enhancement of the Antioxidant Activity and Neurotherapeutic Features through Pyridol Addition to Tetraazamacrocyclic Molecules. Inorganic chemistry, 58(24), 16771-16784.
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4

Single-Crystal X-Ray Diffraction Analysis

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A Leica MZ 75 microscope was used to identify samples suitable for analysis. A Bruker APEX-II CCD diffractometer was employed for crystal screening, unit cell determination, and data collection; which was obtained at 100 K. The Bruker D8 goniometer was controlled using the APEX2 software suite, v2014.11-0. The samples were optically centered with the aid of video camera so that no translations were observed as the crystal was rotated through all positions. The X-ray radiation employed was generated from a MoKα sealed X-ray tube (λ = 0.71076) with a potential of 50 kV and a current of 30 mA; fitted with a graphite monochromator in the parallel mode (175 mm collimator with 0.5 mm pinholes). The crystal-to-detector distance was set to 50 mm, and the exposure time was 10 s per degree for all data sets at a scan width of 0.5°. The frames were integrated with the Bruker SAINT Software package using a narrow frame algorithm. Data were corrected for absorption effects using the multi-scan method SADABS. Using Olex2 the structure was solved with the ShelXS structure solution program using Direct Methods and refined with the SHELXL refinement package using Least Squares minimization. All hydrogen and non-hydrogen atoms were refined using anisotropic thermal parameters. The thermal ellipsoid molecular plots (50%) were produced using Olex2.
Freire D.M., Beeri D., Pota K., Johnston H.M., Palacios P., Pierce B.S., Sherman B.D, & Green K.N. (2020). Hydrogen Peroxide Disproportionation with Manganese Macrocyclic Complexes of Cyclen and Pyclen. Inorganic chemistry frontiers, 7(7), 1573-1582.
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5

Single-Crystal X-Ray Diffraction of C₆₇F₆

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Crystals of 2 were grown by slow evaporation of a carbon disulfide solution. Data were collected on the Advanced Photon Source synchrotron instrument on beamline 15ID-B at Argonne National Laboratory, using a wavelength of 0.41328 Å, a diamond 111 monochromator, and a Bruker D8 goniometer. Unit cell parameters were obtained from a least-squares fit to the angular coordinates of all reflections. Intensities were integrated from a series of frames from ω and φ rotation scans. Absorption and other corrections were applied using TWINABS.112 The structure was solved as a non-merohedral twin using direct methods and refined on F2 against one major and two minor twin components. Standard Bruker control and integration software (APEX II) was employed,113 ,114 and Bruker SHELXTL software was used with Olex 2 for the structure solution, refinement, and molecular graphics.115 ,116 For C67F6: M = 918.67, orthorhombic, a = 9.9998(6), b = 20.6538(12), c = 31.3512(18) Å, V = 6475.1(7) Å3, T = 15(2) K, space group Pbca (no. 61), Z = 8, 9670 reflections measured, 8340 unique which were used in all calculations. The final R and wR values are 0.073 (observed reflections) and 0.163 (all reflections), respectively.†
San L.K., Bukovsky E.V., Larson B.W., Whitaker J.B., Deng S.H., Kopidakis N., Rumbles G., Popov A.A., Chen Y.S., Wang X.B., Boltalina O.V, & Strauss S.H. (2014). A faux hawk fullerene with PCBM-like properties †Electronic supplementary information (ESI) available: Additional figures and tables described in the text. CSD-428507. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c4sc02970d Click here for additional data file. Click here for additional data file.. Chemical Science, 6(3), 1801-1815.
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6

X-ray Crystallography of Microscopic Crystals

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A small colorless platelet with approximate dimensions 0.02×0.01×0.01 mm3 was mounted on a glass fiber and placed into the cold N2 stream of the diffractometer. An Oxford Cryostream 700 instrument was used to maintain a data‐collection temperature of 100 K. Intensity data were collected on a Bruker D8‐Goniometer equipped with an APEX CCD detector. An Incoatec I‐μS micro focus tube with focussing multilayer optics supplied MoKα radiation (λ=0.71073 Å). 1886 intensities were measured in the ω‐scan mode at room temperature and integrated with SAINT+.20 SADABS21 was used for scaling and absorption correction.
Benz S., Missong R., Ogutu G., Stoffel R.P., Englert U., Torii S., Miao P., Kamiyama T, & Dronskowski R. (2019). Ammonothermal Synthesis, X‐Ray and Time‐of‐Flight Neutron Crystal‐Structure Determination, and Vibrational Properties of Barium Guanidinate, Ba(CN3H4)2. ChemistryOpen, 8(3), 327-332.
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7

Single Crystal X-ray Structural Analysis

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Bruker D8 goniometer with APEX area detector

Absorption correction: multi-scan (SADABS; Bruker, 2009 ▶ ) Tmin = 0.687, Tmax = 0.935

15474 measured reflections

2772 independent reflections

2563 reflections with I > 2σ(I)

Rint = 0.069

Sarr M., Merkens C., Diassé-Sarr A., Diop L, & Englert U. (2014). Bis(cyclo­hexyl­ammonium) tetra­chlorido­diphenyl­stannate(IV). Acta Crystallographica Section E: Structure Reports Online, 70(Pt 6), m220-m221.
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