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Very strong absorption
Within the same two-theta limit of ~54º a much higher number of reflections is accessible using the APEX II QUAZAR equipped with the 30 W Silver IμS. The shortest wavelength available for an in-house SC-XRD system provides an improved parameter/reflection ratio. In consequence an anisotropic refinement of the O and Cu atoms became possible. Lower absorption results in a superior signal to noise ratio of the silver data. Residual density peaks in the high-resolution Ag data set are obtained from the conventional monopol-refinement model and contain valuable information on the electron distribution within the chemical bond.
| Cu6 PbO7(Cl,Br) | APEX II QUAZAR | APEX II QUAZAR | APEX II QUAZAR |
| Source | Mo-IμS | Ag-IμS | Ag-IμS |
| Sample Size [mm3] | 0.12 x 0.09 x 0.06 | ||
| Absorption Coefficient μ [mm-1] | 38.4 | 20.6 | 20.6 |
| Exposure time [s/°] | 67 | 67 | 67 |
| Max. resolution [Å] | 0.77 | 0.77 | 0.61 |
| Unique data | 69 | 69 | 127 |
| No. of refined parameters | 9 | 9 | 12 |
| <I/sig> | 187,7 | 216,6 | 186,8 |
| R1 | 0,0198 | 0,0179 | 0,0176 |
| wR2 | 0,0551 | 0,0503 | 0,045 |
| Fo-Fc (highest/lowest peak) | 0.75 / -0.83 | 0.79 / -0.76 | 2.12 / -1.15 |
| Bond length Pb1 - O1 | 2.294(6) | 2.293(6) | 2.290(3) |
Sample courtesy of Dr. Th. Malcherek, Hamburg University, Institute of Petrography and Mineralogy


