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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. 5-([( Z )-Methoxyimino]{2-[(2-methylphenoxy)methyl]phenyl}methyl)-1,3,4-oxadiazole-2(3 H )-thione dimethyl sulfoxide monosolvate

   https://doi.org/10.1107/S2414314623002377  

   Shripanavar, Chetan Shrimandhar ; Balerao, Rishik ; Butcher, Ray J. ( March 2023 , IUCrData)

   The title compound, C 18 H 17 N 3 O 3 S·C 2 H 6 OS, crystallizes in the monoclinic space group P 2 1 /c . In the crystal, C 1 1 (9) chains of C—H...O interactions are formed, propogating in the c -axis direction. The N—H hydrogen atom forms a strong hydrogen bond with the oxygen atom of a DMSO solvate molecule. 

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3. 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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4. N -(5-Cyanononan-5-yl)benzamide

   https://doi.org/10.1107/S2414314623006399  

   Song, Xueqing ; Li, William ( July 2023 , IUCrData)

   N -(5-Cyanononan-5-yl)benzamide, C 17 H 24 N 2 O, synthesized from the reaction between benzoyl chloride and 2-amino-2-butylhexanenitrile, is an important intermediate in amino acid synthesis. Intermolecular N—H...O and C—H...O hydrogen bonds with N...O and C...O distances of 3.083 (2) and 3.304 (2) Å, respectively, link adjacent molecules into chains along the a axis. The dihedral angle between the mean plane of the phenyl group and the plane of the amide group is 19.504 (4)°. 

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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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