Zinc Carbazole Diphosphonate

CAU-57

The following submission contains the data collection and processing for the sample CAU-57 in the framework of the publication: Synthesis and Structure Evolution in Metal Carbazole Diphosphonates Followed by Electron Diffraction. Felix Steinke, Laura Gemmrich Hernandéz, Stephen J. I. Shearan, Maxi Pohlmann, Marco Taddei, Ute Kolb, and Norbert Stock. Inorganic Chemistry 2023 62 (1), 35-42.

Precession Electron Diffraction (PED) was used to collect the dataset on the target crystal.  The dataset was processed with PETS2 and eADT software. The table below summarizes the data collection parameters for the dataset.

General information:

Project

NanED (www.naned.eu)

ESR Project

ESR8

Project Label

CAU-57

Sample Label

CAU-57

Data set Label

ZnDPC_Cry7

Instrumental:

Instrument

FEI TECNAI F30 STWIN

Radiation source

FEG

Accelerating voltage

300 kV

Wavelength

0.0197 Å

Probe Type

Nanodiffraction

Beam Diameter

200nm

Beam Convergence

Semi-parallel beam

Detector

US4000 - CCD camera GATAN (16-bit) (bottom mounted)

Number of pixels in the image

2048 x 2048

Pixel size

15 µm x 15 µm

Camera Length / Effective Camera Length

1500 mm / 1500 mm

Calibration constant (not corrected for Effective Camera length)

0.00074 Å-1/pixel

 Hardware Binning

2 

Sample description:

Name

CAU-57

Chemical composition

[Zn6.75(H2O)1.5(HL)2.5(L)1.5]∙8H2O

3,6-diphosphono-9H-carbazole (H4L)

Sample source

Synthesized

Sample preparation

Grinded in an Agatha mortar and suspended in 1ml of EtOH. 4 µL of the suspension were dropped with a pipette on the carbon side of a carbon-coated copper grid (300 mesh).

Experimental:

Data Type

Electron diffraction data - 3D ED

Data collection method

Precession

Temperature (K) used during data collection

293 K

Number of crystals contributing to the data set

1

Number of experimental frames

106

tilt range, tilt step, tilt per frame

-45° to +60°, 1°, 0°

Precession angle

1°

Exposure time per frame

4 s

Software:

Software used for the data collection

Gatan Digital Micrograph software

Software used for processing

PETS2 and eADT

Authorship and bibliography

Author(s) of the data

Laura Gemmrich Hernández (ESR8)

Related data

CAU-37-as & CAU-37-act

Publication(s)

https://doi.org/10.1021/acs.inorgchem.2c02599

Files and data formats

Image folder

img: Folder containing images of the diffraction pattern from each frame.

Image format

tiff_16bit_unsigned