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C3H11N2I, monoclinic, P21/n (no. 14), a = 5.0152(2) Å, b = 10.1470(4) Å, c = 14.1852(5) Å, β = 96.501(2)°, V = 717.23(5) Å3, Z = 4, Rgt(F) = 0.0174, wRref(F2) = 0.0411, T = 100 K.

We present the results of the analysis of 2,2,6,6-tetramethyl-4-oxo-piperidinium nitrate isolated from the stem bark of Vitex doniana, a tree growing in Nigeria. The low-temperature molecular structure comprises one 2,2,6,6-tetramethyl-4-oxopiperidinium cation and one nitrate anion as one molecule in the asymmetric unit. The compound crystallizes in the monoclinic space group P 2 1 / n . A portion of the nitrate anion exhibits positional disorder with the main disorder component present 66.253(2) % of the time and the minor disorder component present 33.279(2) % of the time. In comparison with the previously reported room-temperature structure of C 9 H 18 N 2 O 4 . The low-temperature structure shows similarity with the piperidinium ring adopting a slightly deformed chair conformation while the nitrate anion is disordered. DFT method was used to complement the experimental study.

Tumour cells maintain a local hypoxic and acidic microenvironment which plays a crucial role in cancer progression and drug resistance. Urease is a metallohydrolases that catalyses the hydrolysis of urea into ammonia and carbon dioxide, causing an abrupt increase of pH. This enzymatic activity can be employed to target the acidic tumour microenvironment. In this study, we present the anticancer activities of urease mimetic cobalt (III) complexes on A549 cells. The cells were treated with different doses of cobalt (III) complexes to observe the cytotoxicity. The change in cellular morphology was observed using an inverted microscope. The cell death induced by these complexes was analysed through ATP proliferation, LDH release and caspase 3/7 activity. The effect of extracellular alkalinization by the cobalt (III) complexes on the efficacy of the weakly basic drug, doxorubicin (dox) was also evaluated. This combination therapy of dox with cobalt (III) complexes resulted in enhanced apoptosis in A549 cells, as evidenced by elevated caspase 3/7 activity in treated groups. The study confirms the urease mimicking anticancer activity of cobalt (III) complexes by neutralizing the tumour microenvironment. This study will motivate the applications of transition metal-based enzyme mimics in targeting the tumour microenvironment for effective anticancer treatments.

In the title compound, C 20 H 19 N 3 O 4 , the dihedral angles between the central pyrazole ring and the pendant phenyl and substituted benzene rings are 50.95 (8) and 3.25 (12)°, respectively, and an intra-molecular C-H⋯O link generates an S (6) ring. The benzodioxolyl ring adopts a shallow envelope conformation with the methyl-ene C atom as the flap. In the crystal, the mol-ecules are linked by non-classical C-H⋯O inter-actions, which generate a three-dimensional network. Solvent-accessible voids run down the c- axis direction and the residual electron density in these voids was modelled during the refinement process using the SQUEEZE algorithm [Spek (2015 ▸). Acta Cryst. C 71 , 9-18] within the structural checking program PLATON ., (© Arderne et al. 2021.)

A single pot, wet chemical route has been applied for the synthesis of polymer supported copper azide, CuN 3 , nanoparticles (CANP). The hybrid system was used as 'catalyst-cum-reagent' for the azide-alkyne cyclo-addition reaction to construct triazole molecules using substituted benzyl bromide and terminal alkyne. The electron donating group containing terminal alkyne produced 5-alkynyl 1,4-disubstituded triazole product whereas for alkyne molecule with terminal electron withdrawing group facilitate the formation of 1,4-disubstituted triazole molecule.

The reactivity of the cobalt(III) complexes dichlorido[tris(2-aminoethyl)amine]cobalt(III) chloride, [CoCl 2 (tren)]Cl, and dichlorido(triethylenetetramine)cobalt(III) chloride, [CoCl 2 (trien)]Cl, towards different amino acids (L-proline, L-asparagine, L-histidine and L-aspartic acid) was explored in detail. This study presents the crystal structures of three amino acidate cobalt(III) complexes, namely, (L-prolinato-κ 2 N,O)[tris(2-aminoethyl)amine-κ 4 N,N',N'',N''']cobalt(III) diiodide monohydrate, [Co(C 5 H 8 NO 2 )(C 6 H 18 N 4 )]I 2 ·H 2 O, I, (L-asparaginato-κ 2 N,O)[tris(2-aminoethyl)amine-κ 4 N,N',N'',N''']cobalt(III) chloride perchlorate, [Co(C 4 H 7 N 2 O 3 )(C 6 H 18 N 4 )](Cl)(ClO 4 ), II, and (L-prolinato-κ 2 N,O)(triethylenetetramine-κ 4 N,N',N'',N''')cobalt(III) chloride perchlorate, [Co(C 4 H 7 N 2 O 3 )(C 6 H 18 N 4 )](Cl)(ClO 4 ), V. The syntheses of the complexes were followed by characterization using UV-Vis spectroscopy of the reaction mixtures and the initial rates of reaction were obtained by calculating the slopes of absorbance versus time plots. The initial rates suggest a stronger reactivity and hence greater affinity of the cobalt(III) complexes towards basic amino acids. The biocompatibility of the complexes was also assessed by evaluating the cytotoxicity of the complexes on cultured normal human fibroblast cells (WS1) in vitro. The compounds were found to be nontoxic after 24 h of incubation at concentrations up to 25 mM.

The title compound, C 10 H 13 Cl 2 NO 2 ·C 6 H 4 Cl 2 O, was formed from the incomplete Mannich condensation reaction of 3-amino-propan-1-ol, formaldehyde and 2,4-di-chloro-phenol in methanol. This resulted in the formation of a co-crystal of the zwitterionic Mannich base, 2,4-di-chloro-6-{[(3-hy-droxy-prop-yl)azaniumyl]-meth-yl}phenolate and the unreacted 2,4-di-chloro-phenol. The compound crystallizes in the monoclinic crystal system (in space group Cc ) and the asymmetric unit contains a mol-ecule each of the 2,4-di-chloro-phenol and 2,4-di-chloro-6-{[(3-hy-droxy-prop-yl)azaniumyl]-meth-yl}phenolate. Examination of the crystal structure shows that the two components are clearly linked together by hydrogen bonds. The packing patterns are most inter-esting along the b and the c axes, where the co-crystal in the unit cell packs in a manner that shows alternating aromatic di-chloro-phenol fragments and polar hydrogen-bonded channels. The 2,4-di-chloro-phenol rings stack on top of one another, and these are held together by π-π inter-actions. The crystal studied was refined as an inversion twin., (© Uprety and Arderne 2019.)

The acidity of the amine H atoms and the consequent salt formation ability of ethylenedinitramine (EDNA) were analyzed in an attempt to improve the thermal stability of EDNA. Two short-chain alkanediamine bases, namely propane-1,3-diamine and butane-1,4-diamine, were chosen for this purpose. The resulting salts, namely propane-1,3-diaminium N,N'-dinitroethylenediazanide, C 3 H 12 N 2 ·C 2+ ·C 2 H 4 N 4 , and butane-1,4-diaminium N,N'-dinitroethylenediazanide, C 4 2- , and butane-1,4-diaminium N,N'-dinitroethylenediazanide, C 4 ·C 14 N 2 2+ ·C 2 H 4 /n, respectively. The resulting salts display extensive hydrogen-bonding networks because of the presence of ammonium and diazenide ions in the crystal lattice. This results in an enhanced thermal stability and raises the thermal decomposition temperatures to 202 and 221 °C compared to 180 °C for EDNA. The extensive hydrogen bonding present also plays a crucial role in lowering the sensitivity to impact of these energetic salts.4 O 4 2- , crystallize in the orthorhombic space group Pbca and the monoclinic space group P2 1 /n, respectively. The resulting salts display extensive hydrogen-bonding networks because of the presence of ammonium and diazenide ions in the crystal lattice. This results in an enhanced thermal stability and raises the thermal decomposition temperatures to 202 and 221 °C compared to 180 °C for EDNA. The extensive hydrogen bonding present also plays a crucial role in lowering the sensitivity to impact of these energetic salts.

A complementary application of three analytical techniques, viz. multidimensional nuclear magnetic resonance spectroscopy (NMR), mass spectrometry (MS), and single-crystal X-ray diffractometry was required to identify and refine two natural products isolated from Millettia versicolor and solvent of crystallization. The two compounds, namely 3-(2H-1,3-benzodioxol-5-yl)-6-methoxy-8,8-dimethyl-4H,8H-pyrano[2,3-h]chromen-4-one, or durmillone, (I), and (2E)-1-(4-{[(2E)-3,7-dimethylocta-2,6-dien-1-yl]oxy}-2-hydroxyphenyl)-3-(4-hydroxyphenyl)prop-2-en-1-one, (II), could not be separated by routine column chromatography and cocrystallized in a 2:1 ratio with 0.13 molecules of ethanol solvent. Compound (II) and ethanol could not be initially identified by single-crystal X-ray analysis due to complex disorder in the aliphatic chain region of (II). Mass spectrometry ensured that (II) represented only one species disordered over several positions in the solid state, rather than several species cohabitating on the same crystallographic site. The atomic identification and connectivity in (II) were established by several 2D (two-dimensional) NMR techniques, which in turn relied on a knowledge of its exact mass. The derived connectivity was then used in the single-crystal analysis to model the disorder of the aliphatic chain in (II) over three positions and allowed identification of a partially occupied ethanol solvent molecule that was disordered over an inversion center. The disordered moieties were refined with restraints and constraints.

The title compound, [Cd 2 (C 7 H 10 NS 2 ) 4 ], is a neutral dinuclear cadmium(II) complex bearing four bis N , N -di-allyl-di-thio-carbamate ligands coordinating to two Cd II cations. In each of the monomeric subunits, there are four S atoms of two di-thio-carbamate ligands [Cd-S = 2.5558 (3), 2.8016 (3), 2.6050 (3) and 2.5709 (3) Å] that coordinate to one Cd II atom in a bidentate mode. The dimers are located over an inversion centre bridged by two additional bridging Cd-S bonds [2.6021 (3) Å], leading to a substantial distortion of the geometry of the monomeric subunit from the expected square-planar geometry. The five-coordinate environment around each of the Cd II ions in the dimer is best described as substanti-ally tetra-gonally distorted square pyramidal. The di-thio-carbamate groups are themselves planar and are also coplanar with the Cd II ions. The negative charge on these groups is delocalized by resonance across the S atoms bound to the Cd II cation. This delocalization of the π electrons in the di-thio-carbamate groups also extends to the C-N bonds as they reveal significant double bond character [C-N = 1.3213 (16) and 1.3333 (15) Å].

Three polymorphs of bis(nitrito-κN)[tris(2-aminoethyl)amine-κ(4)N,N',N'',N''']cobalt(III) chloride, [Co(NO2)2(C6H18N4)]Cl, have been structurally characterized in the 100-300 K temperature range. Two orthorhombic polymorphs are related by a solid-state enantiotropic order-disorder k2 phase transition at ca 152 K. The third, monoclinic, polymorph crystallizes as a nonmerohedral twin. In the structure of the high-temperature (300 K) orthorhombic polymorph, the Co(III) complex cation resides on a crystallographic mirror plane, whereas the Cl(-) anion occupies a crystallographic twofold axis. In the unit cell of the monoclinic polymorph, the cationic Co(III) complex is in a general position, whose charge is balanced by two halves of two Cl(-) anions, each residing on a crystallographic twofold axis.

The 100 K structures of two salts, namely 2-amino-1H-benzimidazolium 3-phenylpropynoate, C7H8N3(+)·C9H5O2(-), (I), and 2-amino-1H-benzimidazolium oct-2-ynoate, C7H8N3(+)·C8H11O2(-), (II), both have monoclinic symmetry (space group P21/c) and display N-H...O hydrogen bonding. Both structures show packing with corrugated sheets of hydrogen-bonded molecules lying parallel to the [001] direction. Two hydrogen-bonded ring motifs can be identified and described with graph sets R(2)(2)(8) and R(4)(4)(16), respectively, in both (I) and (II). Computational chemistry calculations performed on both compounds show that the hydrogen-bonded ion pairs are more energetically favourable in the crystal structure than their hydrogen-bonded neutral molecule counterparts.