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1. Crystal structure of bromidopentakis(tetrahydrofuran-κ O )magnesium bis[1,2-bis(diphenylphosphanyl)benzene-κ ² P , P ′]cobaltate(−1) tetrahydrofuran disolvate

   https://doi.org/10.1107/S2056989019001671  

   Girigiri, Patience B.; Carpenter, Stephanie H.; Brennessel, William W.; Neidig, Michael L. (February 2019, Acta Crystallographica Section E Crystallographic Communications)

   Structural characterization of the ionic title complex, [MgBr(THF) 5 ][Co(dpbz) 2 ]·2THF [THF is tetrahydrofuran, C 4 H 8 O; dpbz is 1,2-bis(diphenylphosphanyl)benzene, C 30 H 24 P 2 ], revealed a well-separated cation and anion co-crystallized with two THF solvent molecules that interact with the cation via weak C—H...O contacts. The geometry about the cobalt center is pseudotetrahedral, as is expected for a d 10 metal center, only deviating from an ideal tetrahedral geometry because of the restrictive bite angles of the bidentate phosphane ligands. Three THF ligands of the cation and one co-crystallized THF solvent molecule are each disordered over two orientations. In the extended structure, the cations and THF solvent molecules are arranged in (100) sheets that alternate with layers of anions, the latter of which show various π-interactions, which may explain the particular packing arrangement. 

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2. 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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3. trans -Acetyldicarbonyl(η ⁵ -cyclopentadienyl)[tris(3,5-dimethylphenyl)phosphane-κ P ]molybdenum(II)

   https://doi.org/10.1107/S2414314617000426  

   Whited, Matthew T.; Ruffer, Eli J.; Zhang, Jia; Rabaey, Dominique J.; Janzen, Daron E. (January 2017, IUCrData)

   The title compound, [Mo(C 5 H 5 )(C 2 H 3 O)(C 24 H 27 P)(CO) 2 ], was prepared by reaction of [Mo(C 5 H 5 )(CO) 3 (CH 3 )] with tris(3,5-dimethylphenyl)phosphane. The complex exhibits a four-legged piano-stool geometry with trans -disposed acetyl and phosphane ligands. The molecular geometry is nearly identical to that of the triphenylphosphane derivative, but introduction of methyl groups on the aromatic phosphane substituents significantly impacts supramolecular organization. In the crystal, non-classical C—H...O interactions involving the acetyl carbonyl group lead to a chain motif along [010], and another set of C—H...O close contacts join inversion-related molecules. 

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4. Crystal structures of three copper(II)–2,2′-bipyridine (bpy) compounds, [Cu(bpy) ₂ (H ₂ O)][SiF ₆ ]·4H ₂ O, [Cu(bpy) ₂ (TaF ₆ ) ₂ ] and [Cu(bpy) ₃ ][TaF ₆ ] ₂ and a related coordination polymer, [Cu(bpy)(H ₂ O) ₂ SnF ₆ ] _n

   https://doi.org/10.1107/S2056989021000633  

   Nisbet, Matthew L.; Hiralal, Emily; Poeppelmeier, Kenneth R. (February 2021, Acta Crystallographica Section E Crystallographic Communications)

   null (Ed.)

   We report the hydrothermal syntheses and crystal structures of aquabis(2,2′-bipyridine-κ 2 N , N ′)copper(II) hexafluoridosilicate tetrahydrate, [Cu(bpy) 2 (H 2 O)][SiF 6 ]·4H 2 O (bpy is 2,2′-bipyridine, C 10 H 8 N 2 ), (I), bis(2,2′-bipyridine-3κ 2 N , N ′)-di-μ-fluorido-1:3κ 2 F : F ;2:3κ 2 F : F -decafluorido-1κ 5 F ,2κ 5 F -ditantalum(V)copper(II), [Cu(bpy) 2 (TaF 6 ) 2 ], (II), tris(2,2′-bipyridine-κ 2 N , N ′)copper(II) bis[hexafluoridotantalate(V)], [Cu(bpy) 3 ][TaF 6 ] 2 , (III), and catena -poly[[diaqua(2,2′-bipyridine-κ 2 N , N ′)copper(II)]-μ-fluorido-tetrafluoridotin-μ-fluorido], [Cu(bpy)(H 2 O) 2 SnF 6 ] n , (IV). Compounds (I), (II) and (III) contain locally chiral copper coordination complexes with C 2 , D 2 , and D 3 symmetry, respectively. The extended structures of (I) and (IV) are consolidated by O—H...F and O—H...O hydrogen bonds. The structure of (III) was found to be a merohedral (racemic) twin. 

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5. Diisobutylammonium triphenyl(2-thiolatoacetato-κ ² O , S )stannate(IV)

   https://doi.org/10.1107/S2414314624007429  

   Song, Xueqing; Yeibyo, Woldegebriel; Li, William; Pike, Robert D (August 2024, IUCrData)

   Crystals of the title salt, (C₈H₂₀N)[Sn(C₆H₅)₃(C₂H₂O₂S)], comprise diisobutylammonium cations and mercaptoacetatotriphenylstannate(IV) anions. The bidentate binding mode of the mercaptoacetate ligand gives rise to a five-coordinated, ionic triphenyltin complex with a distortedcis-trigonal–bipyramidal geometry around the tin atom. In the crystal, charge-assisted ammonium-N—H...O(carboxylate) hydrogen-bonding connects two cations and two anions into a four-ion aggregate. Two positions were resolved for one of the phenyl rings with the major component having a site occupancy factor of 0.60 (3). 

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