Chemical Crystallography

Very strong absorption

Crystal structure of Murdochit determined using the APEX II QUAZAR with Ag-IμS and QUAZAR optics
Crystal structure of Murdochit

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


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