Photon 100 cmos

Single crystal X-ray diffractions of bulk NbOCl₂ and NbOI₂ crystals are measured using a four circles goniometer Kappa geometry, Bruker AXS D8 Venture, equipped with a Photon 100 CMOS active pixel sensor detector. A molybdenum monochromatized (λ = 0.71073 Å) X-Ray radiation is used for the measurement. The frames are integrated with the Bruker SAINT software using a narrow-frame algorithm. Data are corrected for absorption effects using the Multi-Scan method (SADABS). The structures are solved in the monoclinic unit cell and refined using the SHELXT, VERSION 2014/5 Software. The final anisotropic refinement of the structures is performed by least squares procedures on weighted F² values using the SHELXL-2014/7 (Sheldrick, 2014) included in the APEX3 v2016, 9.0, AXS Bruker program.

All experiments were carried out under a nitrogen atmosphere using standard Schlenk techniques and a glove box. 1,2,4,5-tetrakis(isopropyl-thio)benzene (TPB) and NOSbF₆ (Alfa Aesar) were purchased and used upon arrival. 1,2,4,5-tetrakis(ethylthio)benzene (TEB) were prepared according to literatures25 . Solvents were dried prior to use. EPR spectra were obtained using Bruker EMX-10/12 at room temperature. UV-Vis spectra were recorded on Lambda 35 spectrometers. Element analyses were performed on Elementar Vario EL III at Shanghai Institute of Organic Chemistry, the Chinese Academy of Sciences. X-ray crystal structures were obtained by Bruker APEX-II CCD and PHOTON100 CMOS detectors. Single crystals were coated with Paratone-N oil and mounted using a glass fiber. Crystal data and structure refinement details are listed in the supporting information (Table 1, SI). For conductivity measurements, single-crystal samples were affixed on glass carriers and silver paste was used to connect samples and electrodes along the crystallogarphic axises. I-V curves were measured by using a computer-controlled Keithley 2400 source meter.