Oxford diffraction supernova diffractometer

Diffraction data for compound 1-2 were collected using a Rigaku Oxford Diffraction SuperNova diffractometer with MoK α radiation (Table 1). An Oxford Cryosystems Cryostream 700+ low temperature device was used to maintain a crystal temperature of 120 K. The structures were solved using ShelXT and refined with ShelXL interfaced through Olex2. 12, 13 All nonhydrogen atoms were refined using anisotropic displacement parameters. H atoms were placed in calculated positions geometrically and refined using the riding model. CCDC: 1847956 and 1847957. † Powder XRD measurements were performed using a Bruker D2 PHASER spectrometer, and are shown in Fig. S1. †

Diffraction data for samples 1-9 were collected using a Rigaku Oxford Diffraction SuperNova diffractometer with MoK α (1-4, 6-9) and CuK α (5) radiation, and are given in Tables S1 andS2. † An Oxford Cryosystems Cryostream 700+ low temperature device was used to maintain a crystal temperature of 120 K. The structures were solved using ShelXT or ShelXS by direct (2-7, 9) or intrinsic phasing solution methods (1, 8) and refined with version 2016/6 of ShelXL interfaced with Olex2. 25, 26 All non-hydrogen atoms were refined using anisotropic displacement parameters. C-bound H atoms were placed in calculated positions geometrically and refined using the riding model. In structures 1, 2, 4, 6 and 9, O-bound H atoms were identified from a difference Fourier map and refined freely. In 3, 5, 7 and 8, O-bound H atoms were identified from a difference Fourier map and refined as riding, with geometric restraints. CCDC 1579642-1579645 & 1579647-1579651. †

Details about data collection and solution refinement are given in Table S1. Data collections were performed on a Rigaku Oxford Diffraction SuperNova diffractometer equipped with an Atlas CCD detector and micro-focus Cu-Kα radiation (λ = 1.54184 Å). The structures were solved by intrinsic phasing and refined on F² by full matrix least-squares techniques with SHELX programs (SHELXT 2018/2 and SHELXL 2018/3) [50, 51] using the ShelXle and the Olex2 graphical user interfaces. [52, 53] All non-H atoms were refined anisotropically and absorption was corrected by multiscan empirical absorption using spherical harmonics with CrysAlisPro program for 1-CuCl2, 1-ZnCl2, 1-CdCl2 and 1-HgCl2. The H atoms were placed at calculated positions and refined using a riding model. Crystallographic data for the five structures have been deposited with the Cambridge Crystallographic Data Centre, deposition numbers CCDC for 1-CuCl2 : 2203496; 1-ZnCl2 : 2203494 ; 1-CdCl2: 2203493; 1-HgCl2: 2203497; 1-CdCl2-I3 : 2203495.These data can be obtained free of charge from CCDC, 12 Union road, Cambridge CB2 1EZ, UK (e-mail: deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk).