4-cdc crystal

4-CDC / 4-cdc crystals / 4-cdc crystals Buy . Chemicals and reagents used in analyses were acetonitrile, methanol, water (Chem Solve LC–MS, Witko, Łódź, Poland), ammonium formate (Fluka, Seelze, Germany), formic acid (Sigma-Aldrich, Darmstadt, Germany) and DMSO-d₆ (Sigma-Aldrich, Darmstadt, Germany).

Analyzed compounds have been seized by the police during the search of an apartment. Secured evidence (Figure 2) in the form of a white crystalline powder was packed in sachets of two different sizes: one of them contained 1 g, the other 0.5 g. Performed analyzes showed that each of the evidence contained only one of the psychoactive substances described in this paper.

4-CDC / 4-cdc crystals / 4-cdc crystals Buy . X-ray quality crystals were taken directly from crude sample (sachet content). Single-crystal data collection was performed on a KUMA diffractometer (Rigaku Americas Holding Company, Inc. The Woodlands, Texas, TX, USA) with a Saphire CCD detector, equipped with an Oxford Cryosystems open-flow nitrogen cryostat, using ω-scan and graphite-monochromated Mo K_α (λ = 0.71073 Å) radiation at 100 K. Cell refinement, data reduction, analysis and absorption correction were carried out with CRYSALIS^Pro [27] software. The structures were solved by direct methods with SHELXS [21], and refined with full-matrix least-squares techniques on F² with SHELXL [28]. All hydrogen atoms were calculated in idealized geometry riding on their parent atoms. The molecular structure plots were prepared using Diamond [29]. Full details can be found in the CIF files CCDC 1945259–1945262.

NMR spectra were recorded in DMSO-d₆ at room temperature on a Bruker 500 MHz Avance II spectrometer (Billerica, Massachusetts, MA, USA) (¹H frequency 500.13 MHz, ¹³C 125.7 MHz). Spectra were referenced to the residual solvent signals (2.50 and 39.5 ppm). 2D experiments (COSY, HSQC, HMBC) were performed by means of standard Bruker software, recorded with 2048 data points in the t₂ domain and up to 1024 points in the t₁ domain, with a 0.5–1 s recovery delay.

A total of 100 mg of the sample was dissolved in 5 mL of methanol and diluted 1000-fold with MeOH. A total of 10 μL of diluted solution was transferred to a 150 μL insert containing 80 μL of MeOH and 10 μL of IS (4-MMC-d₃, c = 1 μg/mL), mixed on a vortex and analyzed with UHPLC-QQQ-MS/MS.

Analyses were performed using an ultra-high-performance liquid chromatograph (Nexera X2, Shimadzu, Kyoto, Japan). The separation was done using a Kinetex XB-C18 2.6 μm 2.1 mm × 150 mm column (Phenomenex, Torrance, California, CA, USA) with the thermostat set at 40 °C. The mobile phase consisted of a mixture of 10 mM ammonium formate and 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B). The gradient elution was carried out at a constant flow of 0.4 mL/min. The gradient applied was as follows: 0 min, 5% B; 12 min, 98% B; 14 min, 98% B; and 15 min, 5% B. A return to the initial gradient compositions (95% A and 5% B) was performed at 5 min.

Detection of the investigated compounds was achieved using a triple-quadrupole mass spectrometer (LCMS-8050, Shimadzu, Kyoto, Japan). The spectrometer was equipped with an ESI source; determination of the investigated substances was carried out in the Scan mode with positive ionization, and mass range of 50–1000 m/z. The following MS parameters were fixed: nebulizing gas flow, 3 L/min; heating gas flow, 10 L/min; interface temperature, 250 °C; DL temperature, 200 °C; heat block temperature, 350 °C; and drying gas flow, 10 L/min.

A 100 mg sample was dissolved in 5 mL of methanol and analyzed with GC-MC. Gas chromatography–mass spectrometry (GC-MS) analyses were performed using a gas chromatograph coupled with a triple quadrupole mass spectrometer (GC-MS-TQ8040; Shimadzu, Kyoto, Japan). The injector was maintained at 250 °C. Sample injection (2 μL) was in the direct mode. Separation of sample components was conducted using the ZB-5MSi column (30 m length, 0.25 mm inner diameter and 0.25 µm film thickness; Phenomenex, Torrance, California, CA, USA). Helium was used as a carrier gas at the flow rate of 2 mL min⁻¹. The mass detector was set to positive electron ionization (EI) mode and the electron beam energy was 70 eV. The mass detector was operating in a full scan mode in the 50–650 amu range.

The molecular structures of 4-CDC / 4-cdc crystals / 4-cdc crystals Buy(1), MDPT(2), 4F-PHP(3) and 3-MEC(4) are presented in Figures 3, 5, 7 and 9, while representative bond lengths and angles are given in Tables S1–S4 (Supplementary Information). Crystal data and structure refinement details for 4-CDC / 4-cdc crystals / 4-cdc crystals Buy(1), MDPT(2), 4F-PHP(3) and 3-MEC(4) are presented in Table 1. Compounds 1–3 crystallize in the triclinic P-1 space group whereas compound 4 in the monoclinic P2₁/c space group. All distances and angles are in normal range. The C=O bond distance is in a range 1.208(9)–1.225(3) Å.