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1. Comparison of two Mn IV Mn IV -bis-μ-oxo complexes {[Mn IV (N 4 (6-Me-DPEN))] 2 (μ-O) 2 } 2+ and {[Mn IV (N 4 (6-Me-DPPN))] 2 (μ-O) 2 } 2+

   https://doi.org/10.1107/S2056989020004557  

   Coggins, Michael K. ; Downing, Alexandra N. ; Kaminsky, Werner ; Kovacs, Julie A. ( July 2020 , Acta Crystallographica Section E Crystallographic Communications)

   null (Ed.)

   The addition of tert -butyl hydroperoxide ( t BuOOH) to two structurally related Mn II complexes containing N,N -bis(6-methyl-2-pyridylmethyl)ethane-1,2-diamine (6-Me-DPEN) and N,N -bis(6-methyl-2-pyridylmethyl)propane-1,2-diamine (6-Me-DPPN) results in the formation of high-valent bis-oxo complexes, namely di-μ-oxido-bis{[ N , N -bis(6-methyl-2-pyridylmethyl)ethane-1,2-diamine]manganese(II)}( Mn — Mn ) bis(tetraphenylborate) dihydrate, [Mn(C 16 H 22 N 4 ) 2 O 2 ](C 24 H 20 B) 2 ·2H 2 O or {[Mn IV (N 4 (6-Me-DPEN))] 2 ( μ -O) 2 }(2BPh 4 )(2H 2 O) ( 1 ) and di-μ-oxido-bis{[ N , N -bis(6-methyl-2-pyridylmethyl)propane-1,3-diamine]manganese(II)}( Mn — Mn ) bis(tetraphenylborate) diethyl ether disolvate, [Mn(C 17 H 24 N 4 ) 2 O 2 ](C 24 H 20 B) 2 ·2C 4 H 10 O or {[Mn IV (N 4 (6-MeDPPN))] 2 ( μ -O) 2 }(2BPh 4 )(2Et 2 O) ( 2 ). Complexes 1 and 2 both contain the `diamond core' motif found previously in a number of iron, copper, and manganese high-valent bis-oxo compounds. The flexibility in the propyl linker in the ligand scaffold of 2 , as compared to that of the ethyl linker in 1 , results in more elongated Mn—N bonds, as one would expect. The Mn—Mn distances and Mn—O bond lengths support an Mn IV oxidation state assignment for the Mn ions in both 1 and 2 . The angles around the Mn centers are consistent with the local pseudo-octahedral geometry. 

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2. Redetermination of poly[di-μ 3 -iodido-[μ-1,2- trans -(pyridin-4-yl)ethene-κ 2 N : N ′]dicopper(I)]

   https://doi.org/10.1107/S2414314619001226  

   Neal, Henry C. ; Tamtam, Harsha ; Smucker, Bradley W. ; Nesterov, Volodymyr V. ( January 2019 , IUCrData)

   The re-investigated structure of the title compound, [Cu 2 I 2 (C 12 H 10 N 2 )] n , a two-dimensional coordination polymer crystallizing with monoclinic ( P 2 1 / n ) symmetry, is based on data collected at 100 K, while the previously reported structure was obtained with data collected at 203 K [Blake et al. (1999). Cryst. Eng. 2 , 181–195]. The refinement of the crystal structure is greatly improved; for example, the wR 2 residual converges to 0.047 for 1532 independent data, versus wR 2 = 0.179 for 992 independent data in the 1999 study. 

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3. Synthesis, structural analysis, and docking studies with SARS-CoV-2 of a trinuclear zinc complex with N -phenylanthranilic acid ligands

   https://doi.org/10.1107/S205322962200239X  

   Mbani O., Armel L. ; Bonnand, Evan F. ; Paboudam, Awawou G. ; Brannon, Jacob P. ; Gardner-Ricossa, Kevyn D. ; Stieber, S. Chantal ; Agwara, Moise O. ( April 2022 , Acta Crystallographica Section C Structural Chemistry)

   The structure of a trinuclear zinc complex, hexakis(μ 2 -2-anilinobenzoato)diaquatrizinc(II), [Zn 2 (C 13 H 10 NO 2 ) 6 (H 2 O) 2 ] or (NPA) 6 Zn 3 (H 2 O) 2 (NPA is 2-anilinobenzoate or N -phenylanthranilate), is reported. The complex crystallizes in the triclinic space group P -1 and the central Zn II atom is located on an inversion center. The NPA ligand is found to coordinate via the carboxylate O atoms with unique C—O bond lengths that support an unequal distribution of resonance over the carboxylate fragment. The axial H 2 O ligands form hydrogen bonds with neighboring molecules that stabilize the supramolecular system in rigid straight chains, with an angle of 180° along the c axis. π stacking is the primary stabilization along the a and b axes, resulting in a highly ordered supramolecular structure. Docking studies show that this unique supramolecular structure of a trinuclear zinc complex has potential for binding to the main protease (M pro ) in SARS-CoV-2 in a different location from Remdesivir, but with a similar binding strength. 

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4. Synthesis and crystallographic characterization of diphenylamide rare-earth metal complexes Ln (NPh 2 ) 3 (THF) 2 and [(Ph 2 N) 2 Ln (μ-NPh 2 )] 2

   https://doi.org/10.1107/S2056989020009998  

   Palumbo, Chad T. ; Kotyk, Christopher M. ; Ziller, Joseph W. ; Evans, William J. ( September 2020 , Acta Crystallographica Section E Crystallographic Communications)

   null (Ed.)

   Studies of the coordination chemistry between the diphenylamide ligand, NPh 2 , and the smaller rare-earth Ln III ions, Ln = Y, Dy, and Er, led to the structural characterization by single-crystal X-ray diffraction crystallography of both solvated and unsolvated complexes, namely, tris(diphenylamido-κ N )bis(tetrahydrofuran-κ O )yttrium(III), Y(NPh 2 ) 3 (THF) 2 or [Y(C 12 H 10 N) 3 (C 4 H 8 O) 2 ], 1-Y , and the erbium(III) (Er), 1-Er , analogue, and bis[μ-1κ N :2(η 6 )-diphenylamido]bis[bis(diphenylamido-κ N )yttrium(III)], [(Ph 2 N) 2 Y(μ-NPh 2 )] 2 or [Y 2 (C 12 H 10 N) 6 ], 2-Y , and the dysprosium(III) (Dy), 2-Dy , analogue. The THF ligands of 1-Er are modeled with disorder across two positions with occupancies of 0.627 (12):0.323 (12) and 0.633 (7):0.367 (7). Also structurally characterized was the tetrametallic Er III bridging oxide hydrolysis product, bis(μ-diphenylamido-κ 2 N : N )bis[μ-1κ N :2(η 6 )-diphenylamido]tetrakis(diphenylamido-κ N )di-μ 3 -oxido-tetraerbium(III) benzene disolvate, {[(Ph 2 N)Er(μ-NPh 2 )] 4 (μ-O) 2 }·(C 6 H 6 ) 2 or [Er 4 (C 12 H 10 N) 8 O 2 ]·2C 6 H 6 , 3-Er . The 3-Er structure was refined as a three-component twin with occupancies 0.7375:0.2010:0.0615. 

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5. Crystallographic characterization of rare-earth cyanotriphenylborate complexes and the cyanoborates [NCBPh 3 ] 1− , [NCBPh 2 Me] 1− , and [NCBPh 2 (μ-O)BPh 2 ] 1−

   https://doi.org/10.1107/S2056989021006861  

   Dumas, Megan T. ; White, Jessica R. ; Ziller, Joseph W. ; Evans, William J. ( August 2021 , Acta Crystallographica Section E Crystallographic Communications)

   The investigation of the coordination chemistry of rare-earth metal complexes with cyanide ligands led to the isolation and crystallographic characterization of the Ln III cyanotriphenylborate complexes dichlorido(cyanotriphenylborato-κ N )tetrakis(tetrahydrofuran-κ O )lanthanide(III), [ Ln Cl 2 (C 19 H 15 BN)(C 4 H 8 O) 4 ] [lanthanide ( Ln ) = dysprosium (Dy) and yttrium Y)] from reactions of LnCl 3 , KCN, and NaBPh 4 . Attempts to independently synthesize the tetraethylammonium salt of (NCBPh 3 ) − from BPh 3 and [NEt 4 ][CN] in THF yielded crystals of the phenyl-substituted cyclic borate, tetraethylazanium 2,2,4,6-tetraphenyl-1,3,5,2λ 4 ,4,6-trioxatriborinan-2-ide, C 8 H 20 N + ·C 24 H 20 B 3 O 3 − or [NEt 4 ][B 3 (μ-O) 3 (C 6 H 5 ) 4 ]. The mechanochemical reaction of BPh 3 and [NEt 4 ][CN] without solvent produced crystals of tetraethylazanium cyanodiphenyl-λ 4 -boranyl diphenylborinate, C 8 H 20 N + ·C 25 H 20 B 2 NO − or [NEt 4 ][NCBPh 2 (μ-O)BPh 2 ]. Reaction of BPh 3 and KCN in THF in the presence of 2.2.2-cryptand (crypt) led to a crystal of bis[(2.2.2-cryptand)potassium] 2,2,4,6-tetraphenyl-1,3,5,2λ 4 ,4,6-trioxatriborinan-2-ide cyanomethyldiphenylborate tetrahydrofuran disolvate, 2C 18 H 36 KN 2 O 6 + ·C 24 H 20 B 3 O 3 − ·C 14 H 13 BN − ·2C 4 H 8 O or [K(crypt)] 2 [B 3 (μ-O) 3 (C 6 H 5 ) 4 ][NCBPh 2 Me]·2THF. The [NCBPh 2 (μ-O)BPh 2 ] 1− and (NCBPh 2 Me) 1− anions have not been structurally characterized previously. The structure of 1-Y was refined as a two-component twin with occupancy factors 0.513 (1) and 0.487 (1). In 4 , one solvent molecule was disordered and included using multiple components with partial site-occupancy factors. 

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