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1. Crystal structure of bromido­penta­kis­(tetra­hydro­furan-κO)magnesium bis­[1,2-bis­(di­phenyl­phosphan­yl)benzene-κ2P,P′]cobaltate(−1) tetra­hydro­furan disolvate

   https://doi.org/S2056989019001671  

   Girigiri, P. B. (January 2019, Acta crystallographica)

   Structural characterization of the ionic title complex, [MgBr(THF)5][Co(dpbz)2]·2THF [THF is tetra­hydro­furan, C4H8O; dpbz is 1,2-bis­(di­phenyl­phosphan­yl)benzene, C30H24P2], 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 d10 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. 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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3. Bis(catecholato-κ ² O , O ′)bis(dimethyl sulfoxide-κ O )titanium(IV)

   https://doi.org/10.1107/S2056989022002638  

   Hewage, Nisansala; Mastriano, Carolyn; Brückner, Christian; Zeller, Matthias (April 2022, Acta Crystallographica Section E Crystallographic Communications)

   Bis(benzene-1,2-diolato-κ 2 O , O ′)bis(dimethyl sulfoxide-κ O )titanium(IV), [Ti(C 6 H 4 O 2 ) 2 (C 2 H 6 OS) 2 ], crystallizes with two crystallographically independent molecules in the space group P 2 1 / c emulating orthorhombic Pbca symmetry (β = 90.0445 (9)°]. The two molecules are related by pseudo-glide symmetry, broken by modulation of each one catecholate and dimethyl sulfoxide (DMSO) ligand. Twinning by pseudomerohedry was observed [twin ratio 0.5499 (7):0.4401 (7)]. Complex 3 was obtained by heating of diprotonated titanium tris-catecholate precursor 2 H in DMSO, by formal displacement of a catechol molecule by two DMSO molecules. Complex 3 is just the second heteroleptic, mono-nuclear, neutral bis-catecholate complex with TiO 6 metal coordination, the only other one being its bis-DMF analogue 6 . The two molecules of 3 exhibit a distorted octahedral geometry. The geometry and distortions from ideal symmetry of 3 are discussed and compared to 6 and to cationic tris-catecholate titanium complexes. 

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4. Crystal structure of [Ni(OH ₂ ) ₆ ]Cl ₂ ·(18-crown-6) ₂ ·2H ₂ O

   https://doi.org/10.1107/S2056989024010041  

   Brannon, Jacob P; Liang, Kevin; Stieber, S_Chantal E (November 2024, Acta Crystallographica Section E Crystallographic Communications)

   The crystal structure of the title compound, hexaaquanickel(II) dichloride–1,4,7,10,13,16-hexaoxacyclooctadecane–water (1/2/2), [Ni(H₂O)₆]Cl₂·2C₁₂H₂₄O₆·2H₂O, is reported. The asymmetric unit contains half of the Ni(OH₂)₆moiety with a formula of C₁₂H₃₂ClNi_0.50O₁₀at 105 K and triclinic (P1) symmetry. The [Ni(OH₂)₆]²⁺cation has close to ideal octahedral geometry with O—Ni—O bond angles that are within 3° of idealized values. The supramolecular structure includes hydrogen bonding between the water ligands, 18-crown-6 molecules, Cl⁻anions, and co-crystallized water solvent. Two crown ether molecules flank the [Ni(OH₂)₆]²⁺molecule at the axial positions in a sandwich-like structure. The relatively symmetric hydrogen-bonding network is enabled by small Cl⁻counter-ions and likely influences the more idealized octahedral geometry of [Ni(OH₂)₆]²⁺. 

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5. Crystal structures of trans -acetyldicarbonyl(η ⁵ -cyclopentadienyl)(1,3,5-triaza-7-phosphaadamantane)molybdenum(II) and trans -acetyldicarbonyl(η ⁵ -cyclopentadienyl)(3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane)molybdenum(II)

   https://doi.org/10.1107/S2056989020003679  

   Anstey, Mitchell R.; Bost, John L.; Grumman, Anna S.; Kennedy, Nicholas D.; Whited, Matthew T. (April 2020, Acta Crystallographica Section E Crystallographic Communications)

   null (Ed.)

   The title compounds, [Mo(C 5 H 5 )(COCH 3 )(C 6 H 12 N 3 P)(CO) 2 ], (1), and [Mo(C 5 H 5 )(COCH 3 )(C 9 H 16 N 3 O 2 P)(C 6 H 5 ) 2 ))(CO) 2 ], (2), have been prepared by phosphine-induced migratory insertion from [Mo(C 5 H 5 )(CO) 3 (CH 3 )]. The molecular structures of these complexes are quite similar, exhibiting a four-legged piano-stool geometry with trans -disposed carbonyl ligands. The extended structures of complexes (1) and (2) differ substantially. For complex (1), the molybdenum acetyl unit plays a dominant role in the organization of the extended structure, joining the molecules into centrosymmetrical dimers through C—H...O interactions with a cyclopentadienyl ligand of a neighboring molecule, and these dimers are linked into layers parallel to (100) by C—H...O interactions between the molybdenum acetyl and the cyclopentadienyl ligand of another neighbor. The extended structure of (2) is dominated by C—H...O interactions involving the carbonyl groups of the acetamide groups of the DAPTA ligand, which join the molecules into centrosymmetrical dimers and link them into chains along [010]. Additional C—H...O interactions between the molybdenum acetyl oxygen atom and an acetamide methyl group join the chains into layers parallel to (101). 

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