Crysalis program package

X-ray measurements on the selected crystal of 1 were performed on an Oxford Diffraction Xcalibur™ 2 equipped with a Sapphire2 CCD detector using Mo-Kα radiation. The CrysAlis program package (version 1.171.33.52, Oxford Diffraction) was used for data collection and reduction. 39 X-ray measurements on the single-crystals of 2 and 3 were performed on a Bruker D8 Quest diffractometer equipped with a Photon 100 CMOS detector using the Mo-Kα radiation. Data collection, data reduction, and cell parameters refinements were performed using the Bruker Apex III software package. 40 The molecular structures were solved by direct methods SHELXS-2014 and all non-hydrogen atoms were refined anisotropically on F 2 using full-matrix least-squares procedure SHELXL-2014. 41 All hydrogen atoms were found in differential Fourier maps and their parameters were refined using a riding model with U iso (H) = 1.2(CH) or 1.5(CH 3 )U eq . The X-ray powder diffraction patterns of all solid samples were recorded on an MiniFlex600 (Rigaku) instrument equipped with the Bragg-Brentano geometry, and with iron-filtered Cu Kα 1,2 radiation.

Single crystal X-ray diffraction data are listed in Table S1. † The data were recorded on an Oxford diffraction Xcalibur 2 CCD diffractometer with a Sapphire CCD detector, sealed tube (Mo Kα radiation, Kα = 0.71073 Å) and equipped with an Oxford Cryosystems nitrogen gas-flow apparatus. The CrysAlis program package (version 1.171.33.52, Oxford Diffraction) was used for data collection and reduction. 27 The molecular structures were solved by direct methods SHELX-2014 and all nonhydrogen atoms were refined anisotropically on F 2 using the full-matrix least-squares procedure SHELXL-97. 28 All the hydrogen atoms were found in differential Fourier maps and their parameters were refined using a riding model with U iso (H) = 1.2 (CH, CH 2 , OH) or 1.5U eq (CH 3 ).

X-ray measurements on the selected single crystals of 1a-c and 2b-c were performed on an Oxford Diffraction Xcalibur™ 2 equipped with a Sapphire 2 CCD detector using the Mo-Kα radiation (λ = 0.71073 Å) and Oxford Cryosystems nitrogen gasflow apparatus. The CrysAlis program package (version 1.171.33.52, Oxford Diffraction) was used for data collection and reduction. 32 X-ray measurement on the single-crystal of 2a was performed on a Bruker D8 Quest diffractometer equipped with a Photon 100 CMOS detector using the Mo-Kα radiation. Data collection, data reduction, and cell parameter refinements were performed using the Bruker Apex III software package. 33 The molecular structures were solved by direct methods SHELXS-2014 and all non-hydrogen atoms were refined anisotropically on F 2 using the full-matrix least-squares procedure SHELXL-2014. 34 All hydrogen atoms were found in differential Fourier maps and their parameters were refined using the riding model with U iso (H) = 1.2 (CH, CH 2 , and OH) or 1.5U eq (CH 3 ).
The shape of coordination polyhedra was calculated using the program Shape (version 2.1). 24