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While Δ9-tetrahydrocannabinolic acid A (THCA-A) has been reported to be difficult to crystallize and/or amorphous, we have obtained THCA-A in a pure crystalline form by extraction of marijuana and selective fractionation with liquid CO2. THCA-A (systematic name 1-hydroxy-6,6,9-trimethyl-3-pentyl-6a,7,8,10a-tetrahydro-6H-benzo[c]isochromene-2-carboxylic acid, C22H30O4) crystallizes in the orthorhombic space group P212121, with Z = 8 and Z' = 2. The two independent molecules are related by a pseudo-twofold axis centered between the two -CO2H groups, but the conformations of the two -C5H11 chains are quite different (tgt and ttg; t is trans and g is gauche). The carboxylate groups form an intermolecular R22(8) hydrogen-bonded ring; the two C2O2 carboxylate planes are twisted out of the planes of the attached arene rings in opposite directions by 13.59 (8) and 18.92 (8)°, respectively, with a resultant interplanar angle of 28.89 (8)°. Each molecule also has an intramolecular S(6) hydrogen-bond motif between the ortho -OH group and the dihydropyran-ring O atom. Other conformational aspects of the two independent molecules are quite similar to those found in the previously determined structure of THCA-B. THCA-A has shown promise in a number of medical applications. Demonstration of the crystallinity and details of the crystal structure are expected to provide a standard point of departure for chemical and medical experiments.Single crystals of dicerium trialuminium tetragermanide, Ce2Al3Ge4, have been synthesized from a high-temperature reaction using an eutectic mixture of Al and Ge as a metal flux. Through single-crystal X-ray diffraction it was established that Ce2Al3Ge4 crystallizes in the centrosymmetric space group Cmce (No. 64) with the Ba2Cd3Bi4 structure type (Pearson code oC36). Five atoms compose the asymmetric unit, i.e. one Ce, two Al, and two Ge atoms, all in special positions with Wyckoff symbols 8f (Ce), 4a and 8e (Al), and 8e and 8f (Ge). The structure can be described as a three-dimensional network of Al and Ge atoms, with Ce atoms occupying the cavities of the framework.The conformational flexibilities are studied in two new organotin(IV) complexes, namely, trans-dichloridodimethylbis[N,N',N''-tris(2-chlorobenzyl)phosphoric triamide]tin(IV), [Sn(CH3)2(C21H21Cl3N3OP)2Cl2] or Sn(CH3)2Cl2OP[NHCH2C6H4(2-Cl)]32, (I), and bis(dipropylammonium) tetrachloridodimethylstannate(IV), [(CH3CH2CH2)2NH2]2[Sn(CH3)2Cl4], (II), and their analogous structures from the Cambridge Structural Database (CSD). The conformations are considered based on the N-P=O-Sn torsion angles for (I) and the C-C-C-N, C-C-N-C, C-N-C-C and N-C-C-C torsion angles for the two symmetry-independent [CH3CH2CH2NH2CH2CH2CH3]+ cations in (II), and the ±ac±sp±ac (ac = anticlinal and sp = synperiplanar) and ±ap±ap±ap±ap (ap = antiperiplanar) conformations are observed, respectively. In both structures, the four atoms in the corners of the square-planar segment of the octahedral shape around the Sn atom participate in normal hydrogen-bonding interactions as acceptors, which include two O and two Cl atoms for (I), and four Cl atoms for (II). However, the phosphoric triamide ligands block the environment around the Sn atom and limit the hydrogen-bond pattern to form a supramolecular ribbon assembly, while in the presence of small organic cations in (II), a two-dimensional hydrogen-bonded architecture is achieved. The weak interactions π-π, C-H...π and C-Cl...π in (I), and C-H...Cl in (II) do not change the dimensionality of the hydrogen-bond pattern. The 62 CSD structures analogous to (I), i.e. with an SnOPN3 segment (including 83 entries) fall into four categories of conformations based on the N-P=O-Sn torsion angles. The 132 [(CH3CH2CH2)2NH2]+ cations from 85 CSD structures are classified into seven groups based on the torsion angles noted for (II). Most of the CSD structures adopt the same associated conformations noted for (I) and (II). 15 [Sn(CH3)2Cl4]2- anions extracted from the CSD are compared with the structure of (II).Two copper(I) iodide tetramers, namely, [μ2-1,3-bis(diphenylphosphanyl)propane-κ2PP']di-μ3-iodido-di-μ2-iodido-[1-(pyridin-3-yl)ethan-1-one-κN]tetracopper(I) dichloromethane disolvate, [Cu4I4(C6H7NO)2(C27H26P2)2]·2CH2Cl2 (CuL3), and [μ2-1,3-bis(diphenylphosphanyl)propane-κ2PP']di-μ3-iodido-di-μ2-iodido-[1-(pyridin-4-yl)ethan-1-one-κN]tetracopper(I), [Cu4I4(C6H7NO)2(C27H26P2)2] (CuL4), have been synthesized from reactions of CuI, 1,3-bis(diphenylphosphanyl)propane (dppp) and 3- or 4-acetylpyridine (3/4-acepy). The complexes were characterized by elemental analysis, IR spectroscopy, single-crystal X-ray diffraction (XRD), powder XRD and photoluminescence spectroscopy. Both complexes possess a stair-step [Cu4I4] cluster structure with a crystallographic inversion centre located in the middle of a Cu2I2 ring (Z' = 1/2). The dppp ligands each adopt a bidentate coordination mode that bridges two CuI centres on one side of the [Cu4I4] cluster and the acepy ligands act as terminal ligands. The solid-state samples of similar complexes show highly efficiency thermally activated delayed fluorescence (TADF) at room temperature. At ambient temperature, both CuL3 and CuL4 exhibit photoluminescence, with a maximum emission in the region 560-580 nm and with short emissive decay times, but only phosphorescence was observed at 77 K. The narrow gaps between the higher lying singlet state and the triplet state, ΔE(S1 - T1), also confirm the presence of TADF. Structure analysis and consideration of photoluminescence indicates that the position of the acetyl group on the heterocyclic ligand has an obvious influence on the structural arrangement, on intermolecular interactions and on the observed photophysical properties.Pretransplant crossmatch (XM) testing is widely used for detecting preformed donor-specific antibodies (DSAs) against human leukocyte antigen (HLA). However, in some cases, there is a positive XM result in the absence of HLA-DSAs, the cause of which was rarely identified. Golvatinib nmr We reviewed the causes of sequential positive XM results at a single center and analyzed the presence of non-HLA antibodies in patients with an unexplained positive pretransplant XM result. Among 251 patients with T-cell/B-cell complement-dependent cytotoxicity (CDC) or flow cytometric crossmatch (FCXM) positivity, HLA-DSAs were confirmed in 88 (35.1%) by a single antigen bead (SAB) assay, 150 (59.8%) used rituximab (anti-CD20), and 13 (5.2%) had neither HLA-DSAs nor a desensitization history. Anti-angiotensin II type 1 receptor IgG and 33 non-HLA antibodies were tested in the 13 patients with an unexplained positive pretransplant XM result, and more than one non-HLA antibody were revealed in all these patients; 11 patients had non-HLA antibodies reported to be associated with graft rejection, and two patients experienced rejection episode after kidney transplantation.
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