*2.3. X-ray Crystallography*

The crystal data for compound **1** were measured on a Bruker Apex II diffractometer with graphite monochromated Mo Kα (λ = 0.71073 Å) radiation. The data for compounds **2** were measured on a Rigaku R-AXIS RAPID diffractometer with graphite monochromated Mo Kα (λ = 0.71073 Å) radiation, while the data for compound **3** were measured on an Agilent Technology SuperNova Eos Dual system with a Mo Kα (λ = 0.71073 Å) microfocus source and focusing multilayer mirror optics. None of the crystals showed evidence of crystal decay during the data collections. Refinements were carried out with SHELXS-2014/7 [73] and SHELXL-2014/7 [73] using Olex 2.0 interface via the full matrix leastsquares on F2 method. In the final refinements, all atoms were refined anisotropically in compounds **1**–**3**. The hydrogen atoms of en, phen, DETA and enMe in the three compounds were placed in calculated positions and included in the structure factor calculations but

not refined. In these heavy-atom structures with reflection data from poor-quality crystals it was not possible to see clear electron-density peaks in difference maps which would correspond with acceptable locations for the various H atoms bonded to water oxygen atoms. The refinements were then completed with no allowance for these water H atoms in the models; the CCDC number: 1,525,920 for 1, 2,024,572 for 2 and 1,525,922 for 3. The reflection intensity data for compounds **4** and **5** were also measured on a Rigaku R-AXIS RAPID diffractometer with graphite monochromated Mo Kα (λ = 0.71073 Å) radiation, and the results show that the two compounds have already been reported previously [6]. A summary of the crystallographic data and structure refinements for compounds **1**–**3** is given in Table 1.


**Table 1.** Crystal data and structure refinements for compounds **1**–**3**.

<sup>a</sup> R1 = ∑||F0| − |Fc||/∑|F0|. <sup>b</sup> ωR2 = {∑[w (F0 <sup>2</sup> − Fc 2) 2]/∑[w(F0 2) 2]}/2.
