Synthesis and Structural Characterization of ... - Jacobs University

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Chapter 3 Published Results 3.A.2.3. X-ray Crystallography The crystals were mounted in Hampton cryoloops using light oil, for data collection at low temperature. Indexing and data collection were performed using a Bruker X8 APEX II CCD diffractometer with kappa geometry and Mo K α radiation (λ = 0.71073 Å). Data integration and routine processing were performed using the SAINT software suite. Further data processing, including multi-scan absorption corrections, was performed using SADABS. 12 Direct methods (SHELXS97) solutions successfully located the W atoms, and successive Fourier syntheses (SHELXL97) revealed the remaining atoms. 12 Refinements were full-matrix least squares against F 2 using all data. Some lanthanides, cations, and waters of hydration were modeled with varying degrees of occupancy, a common situation for polyoxotungstate structures. One disordered europium counter caion was found in addition to the nondisordered Eu 3+ ions grafted to the {W 28 } polyanion. In the final refinements, all nondisordered heavy atoms (W, Ln) were refined anisotropically, while the O and Na atoms and the disordered europium were refined isotropically. No H atoms were included in the models. The crystallographic data are provided in Table 3.3. 79
Chapter 3 Published Results Table 3.3. Crystal Data and Structure Refinement for Na-11 and NaEu-12. Code Na-11 NaEu-12 Empirical formula H 102 Sm 2 Na 14 O 145 W 28 H 116 Eu 3.5 Na 9.5 O 152 W 28 MW 8193.18 6729.17 Crystal system Triclinic Monoclinic Space group (no.) P1̅ (2) P2 1 /n aÅ 14.8727(6) 25.3862(11) bÅ 21.7762(11) 14.6364(5) cÅ 23.5751(10) 40.3264(16) ° 89.175(2) 90 ° 86.430(2) ° 75.364(2) 90 V/Å 3 7373.2(6) 14898.7(10) Z 2 4 T/ ºC -100 -100 λÅ 0.71073 0.71073 D/ Mg m -3 3.690 3.766 μ/ mm -1 22.68 23.11 R[I >2sigma(I)] a 0.056 0.072 R w (all data) b 0.158 0.203 a R = ∑|F o | – |F c | |∑| |F o |. b R w = {∑[w(F o 2 – F c 2 ) 2 ] / ∑[w(F o 2 ) 2 ]} 1/2 . 80
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