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Intensity data were collected using a Bruker AXS-KAPPA APEX-II
PHOTON 100 diffractometer with graphite monochromated
Mo-Ka (l 0.71073) radiation. Data were collected using phi
and omega scans of 0.51 per frame and a full sphere of data was
obtained. Cell parameters were retrieved using Bruker SMART20
software and refined using Bruker SAINT20a on all the observed
reflections. Absorption corrections were applied using SADABS.20a
Structures were solved by direct methods by using the SHELXS-97
package20b and refined using SHELXL-97.20b Calculations were
performed using the WinGX System-Version 1.80.03.20c The
hydrogen atoms attached to carbon atoms and to the nitrogen
atoms were inserted at geometrically calculated positions and
included in the refinement using the riding-model approxi-
mation; Uiso(H) were defined as 1.2Ueq of the parent nitrogen
atoms or the carbon atoms for phenyl and methylene residues,
and 1.5Ueq of the parent carbon atoms for the methyl groups.
The hydrogen atoms of coordinated water molecules were
located from the final difference Fourier map and the isotropic
thermal parameters were set at 1.5 times the average thermal
parameters of the belonging oxygen atoms; their positions were
restrained by using DFIX and DANG. Least square refinements
using anisotropic thermal motion parameters for all the non-
hydrogen atoms and isotropic ones for the remaining atoms
were employed. In compound 2, the ethyl group was struc-
turally disordered over two orientations and were refined with
the use of PART instruction; the occupancy was refined to a
ratio of 0.66 and 0.34. Crystallographic data are summarized in
Table S1 (ESI†) and selected bond distances and angles are
presented in Table S3 (ESI†). CCDC 1040066–1040069 for 1–4.
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Acknowledgements
This work has been supported by the Foundation for Science
and Technology (FCT), Portugal (project UID/QUI/00100/2013).
Author A. Karmakar and S. Hazra express their gratitude to the
FCT for post-doctoral fellowships (Ref. No SFRH/BPD/76192/
2011 and SFRH/BPD/78264/2011). The authors acknowledge the
Portuguese NMR Network (IST-UL Centre) for access to the NMR
facility, and the IST Node of the Portuguese Network of mass-
˜
spectrometry (Dr Conceiçao Oliveira) for the ESI-MS measurements.
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