Crystal structure of fac-{5-[(hexylazaniumyl)methyl]-2-(pyridin-2-yl)phenyl-κ2
                  N,C
                  1}bis[2-(pyridin-2-yl)phenyl-κ2
                  N,C
                  1]iridium(III) chloride

The asymmetric unit of the title compound, fac-[Ir(C11H8N)2(C18H24N2)]Cl or fac-[Ir(ppy)2(Hppy-NC6)]Cl, contains two [Ir(ppy)2(ppy-NC6)](H+) cations, two Cl− anions and disordered solvent. In each complex molecule, the IrIII ion is coordinated by two C,N-bidentate 2-(pyridin-2-yl)phenyl ligands and one C,N-bidentate N-[4-(pyridin-2-yl)benzyl]hexan-1-aminium ligand, leading to a distorted fac-octahedral coordination environment. In the crystal, the molecules are linked by N—H...Cl, C—H...π and π–π interactions, forming a three-dimensional supramolecular structure. The hexyl group of one molecule is disordered over two orientations with a refined occupancy ratio of 0.412 (13):0.588 (13). The acetone and hexane solvent molecules were found to be highly disordered and their contribution to the scattering was masked using the solvent-masking routine smtbx.mask in OLEX2 [Rees et al. (2005). Acta Cryst. D61, 1299–1301]. These solvent molecules are not considered in the given chemical formula and other crystal data.

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Crystal structure of bis[cis-diaquabis(phenanthroline)cobalt(II)] bis(citrato)germanate(IV) dinitrate

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s205698902100846x ◽

2021 ◽

Vol 77 (9) ◽

Author(s):

Olha Buchko ◽

Viktoriya Dyakonenko ◽

Elena Martsinko ◽

Elena Chebanenko

Keyword(s):

Crystal Structure ◽

Solvent Molecule ◽

Crystal Data ◽

Chemical Formula ◽

Asymmetric Unit ◽

Acta Cryst ◽

Water Oxygen ◽

Solvent Molecules ◽

The Given ◽

Oxygen Atoms

The asymmetric unit of the title compound, [Co(C12H8N2)2(H2O)2]2[Ge(C6H5O7)2](NO3)2, features two complex [(C12H8N2)2(H2O)2Co]2+ cations, two NO3 − anions as well as one centrosymmetric [(C6H5O7)2Ge]2− anion. Two HCit ligands (Cit = citrate, C6H4O7) each coordinate via three different oxygen atoms (hydroxylate, α-carboxylate, β-carboxylate) to the Ge atom, forming a slightly distorted octahedron. The coordination polyhedron of the Co atom is also octahedral, formed by coordination of four nitrogen atoms from two phenanthroline molecules and two water oxygen atoms. In the crystal, the cations and anions are linked by hydrogen bonds and form layers parallel to the bc plane. The structure exhibits disorder of the NO3 − anion [disorder ratio 0.688 (9) to 0.312 (9)]. There are also highly disordered solvent molecules (presumably water and/or ethanol) in the crystal structure; explicit refinement of these molecules was not possible, and the content of the voids was instead taken into account using reverse Fourier transform methods [SQUEEZE procedure in PLATON; Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

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Construction of a supramolecule comprising [2,3,9,10,16,17,23,24-octakis(2,6-dimethylphenoxy)phthalocyaninato]zinc(II) and (5,10,15,20-tetraphenylporphyrinato)zinc(II)

IUCrData ◽

10.1107/s2414314618017418 ◽

2018 ◽

Vol 3 (12) ◽

Author(s):

Masatomo Makino ◽

Kazuhiko Matsubayashi ◽

Yukiko Kodama-Oda ◽

Naoto Imawaka ◽

Nobuhiro Mizuno ◽

...

Keyword(s):

Self Assembly ◽

Solvent Molecule ◽

Phenyl Group ◽

Van Der Waals Interactions ◽

Crystal Data ◽

Chemical Formula ◽

Asymmetric Unit ◽

Acta Cryst ◽

Solvent Molecules ◽

The Given

The supramolecular features in the title compound, [2,3,9,10,16,17,23,24-octakis(2,6-dimethylphenoxy)phthalocyaninato]zinc(II) bis[(5,10,15,20-tetraphenylporphyrinato)zinc(II)] chloroform tetrasolvate, [Zn(C96H80N8O8)][Zn(C44H28N4)]2·4CHCl3 or [Zn(Pc)][Zn(TPP)]2·4CHCl3, result from a self-assembly of one molecule of [2,3,9,10,16,17,23,24-octakis(2,6-dimethylphenoxy)phthalocyaninato]zinc(II) (ZnPc) and two molecules of (5,10,15,20-tetraphenylporphyrinato)zinc(II) (ZnTPP). One half ZnPc, one ZnTPP and two chloroform molecules define the asymmetric unit, with the zinc(II) cation of ZnPc situated on an inversion centre. In the supramolecule, the central ZnPc moiety is sandwiched between two ZnTPPs moieties in a co-facial conformation with a π-conjugated system, leading to a nearly H-type aggregate with a distance of 3.4967 (5) Å between adjacent zinc sites. The ZnTPP units are slightly glided away to form a partial ecliptic arrangement. Each phenyl group of the TPP ligand is anchored above the N atom of the isoindole linker of the Pc ligand through weak C—H...N hydrogen bonds and is held into the crevice between the two dimethylphenoxy groups of phthalocyanine via van der Waals interactions. In the crystal, chloroform solvent molecules are situated between the supramolecules. There is another solvent-accessible void of 341 (2) Å3. The contribution of disordered solvent molecules situated in this void was removed from the diffraction data using SQUEEZE in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not consider this unknown solvent molecule(s).

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Crystal structure of triaqua(2,6-dimethylpyrazine-κN4)bis(thiocyanato-κN)manganese(II) 2,5-dimethylpyrazine disolvate

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989015020769 ◽

2015 ◽

Vol 71 (12) ◽

pp. m223-m224 ◽

Cited By ~ 2

Author(s):

Stefan Suckert ◽

Susanne Wöhlert ◽

Inke Jess ◽

Christian Näther

Keyword(s):

Crystal Structure ◽

Rotation Axis ◽

Complex Molecule ◽

Three Dimensional ◽

Water Molecules ◽

Asymmetric Unit ◽

Acta Cryst ◽

Dimensional Network ◽

Entire Complex ◽

Solvent Molecules

In the crystal structure of the title complex, [Mn(NCS)2(C6H8N2)(H2O)3]·2C6H8N2, the MnIIcation is coordinated by two terminallyN-bonded thiocyanate anions, three water molecules and one 2,6-dimethylpyrazine ligand within a slightly distorted N3O3octahedral geometry; the entire complex molecule is generated by the application of a twofold rotation axis. The asymmetric unit also contains an uncoordinating 2,5-dimethylpyrazine ligand in a general position. Obviously, the coordination to the 2,6-dimethylpyrazine ligand is preferred because coordination to the 2,5-dimethylpyrazine is hindered due to the bulky methyl group proximate to the N atom. The discrete complexes are linked by water-O—H...N(2,6-dimethylpyzazine/2,5-dimethylpyzazine) hydrogen bonding, forming a three-dimensional network. In the crystal, molecules are arranged in a way that cavities are formed in which unspecified, disordered solvent molecules reside. These were modelled employing the SQUEEZE routine inPLATON[Spek (2015).Acta Cryst. C71, 9–18]. The composition of the unit cell does not take into account the presence of the unspecified solvent.

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The crystal structure of bis{3,5-difluoro-2-[4-(2,4,6-trimethylphenyl)pyridin-2-yl]phenyl}(picolinato)iridium(III) and its 4-tert-butylpyridin-2-yl analogue

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989018012409 ◽

2018 ◽

Vol 74 (10) ◽

pp. 1467-1470 ◽

Cited By ~ 2

Author(s):

Robert D. Sanner ◽

Victor G. Young

Keyword(s):

Crystal Structure ◽

Pyridine Ring ◽

Solvent Molecule ◽

Quantum Yields ◽

Dihedral Angles ◽

Crystal Data ◽

Chemical Formula ◽

Acta Cryst ◽

Solvent Molecules ◽

The Given

The crystal structures of bis{3,5-difluoro-2-[4-(2,4,6-trimethylphenyl)pyridin-2-yl]phenyl-κ2 N,C 1}(picolinato-κ2 N,O)iridium(III), [Ir(C20H16F2N)2(C6H4NO2)], 1, and bis[2-(4-tert-butylpyridin-2-yl)-3,5-difluorophenyl-κ2 N,C 1](picolinato-κ2 N,O)iridium(III), [Ir(C15H14F2N)2(C6H4NO2)], 2, are presented herein. These phosphorescent cyclometallated iridium(III) compounds have been structurally investigated in order to better understand the nature of their blue-shifted emssions while maintaining high quantum yields. Compound 1 exhibits substantial twisting of the mesitylene rings out of the plane of the attached pyridine ring, with dihedral angles of 67.0 (1) and 78.7 (1)° between the best mean planes. For both compounds, the contribution of disordered solvent molecule(s) was removed using the SQUEEZE [Spek (2015). Acta Cryst. C71, 9–18] routine in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. These solvent molecules are not considered in the given chemical formula and other crystal data.

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Crystal structure of an unknown tetrahydrofuran solvate of tetrakis(μ3-cyanato-κ3N:N:N)tetrakis[(triphenylphosphane-κP)silver(I)]

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989015017636 ◽

2015 ◽

Vol 71 (10) ◽

pp. 1262-1265

Author(s):

Peter Frenzel ◽

Dieter Schaarschmidt ◽

Alexander Jakob ◽

Heinrich Lang

Keyword(s):

Crystal Structure ◽

Three Dimensional ◽

Acta Cryst ◽

Compound C ◽

Hydrogen Bonding Interactions ◽

Dimensional Network ◽

Solvent Molecules ◽

Set Up ◽

The Given ◽

Triphenylphosphine Ligand

In the title compound, [{[(C6H5)3P]Ag}4{NCO}4], a distorted Ag4N4-heterocubane core is set up by four AgIions being coordinated by the N atoms of the cyanato anions in aμ3-bridging mode. In addition, a triphenylphosphine ligand is datively bonded to each of the AgIions. Intramolecular Ag...Ag distances as short as 3.133 (9) Å suggest the presence of argentophilic (d10...d10) interactions. Five moderate-to-weak C—H...O hydrogen-bonding interactions are observed in the crystal structure, spanning a three-dimensional network. A region of electron density was treated with the SQUEEZE procedure inPLATON[Spek (2015).Acta Cryst.C71, 9–18] following unsuccessful attempts to model it as being part of disordered tetrahydrofuran solvent molecules. The given chemical formula and other crystal data do not take into account these solvent molecules.

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Crystal structure of (20S)-21-[4-(2-hydroxypropan-2-yl)-1H-1,2,3-triazol-4-yl]-20-(4-methylpentyl)-5-pregnen-3β-ol with an unknown solvate

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989018003286 ◽

2018 ◽

Vol 74 (4) ◽

pp. 465-468

Author(s):

Hugo Santalla ◽

Saray Argibay

Keyword(s):

Crystal Structure ◽

Solvent Molecule ◽

Hydroxyl Group ◽

Crystal Data ◽

Chemical Formula ◽

Isopropyl Group ◽

Terminal Position ◽

Acta Cryst ◽

The Given ◽

Tertiary Hydroxyl

In the title cholesterol analogue, [systematic name: (3S,8S,9S,10R,13S,14S,17R)-17-{(S)-1-[4-(2-hydroxypropan-2-yl)-1H-1,2,3-triazol-1-yl]-6-methylheptan-2-yl}-10,13-dimethyl-2,3,4,7,8,9,10,11,12,13,14,15,16,17-tetradecahydro-1H-cyclopenta[a]phenanthren-3-ol] C32H53N3O2, a new chain, including an intermediate triazole and a tertiary hydroxyl group in the terminal position, has been added at position 20 inducing a change in its stereochemistry. In the crystal, molecules are linked by O—H...O and O—H...N hydrogen bonds, forming layers lying parallel to (-201) and enclosing R 4 4(36) ring motifs. The isopropyl group is disordered about two positions with a refined occupancy ratio of 0.763 (5):0.237 (5). A region of disordered electron density was corrected for using the SQUEEZE routine in PLATON (Spek (2015). Acta Cryst. C71, 9–18). The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

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Tetracarbonyl[N-(diphenylphosphanyl-κP)-N,N′-diisopropyl-P-phenylphosphorus diamide-κP]molybdenum(0) with an unknown solvent

IUCrData ◽

10.1107/s2414314618008465 ◽

2018 ◽

Vol 3 (6) ◽

Cited By ~ 3

Author(s):

Martha Höhne ◽

Marc Gongoll ◽

Anke Spannenberg ◽

Bernd H. Müller ◽

Normen Peulecke ◽

...

Keyword(s):

Solvent Molecule ◽

Coordination Geometry ◽

Crystal Data ◽

Chemical Formula ◽

Acta Cryst ◽

Carbonyl Ligands ◽

Distorted Octahedral Coordination Geometry ◽

Distorted Octahedral ◽

Solvent Molecules ◽

The Given

The title complex, [Mo(C24H30N2P2)(CO)4], contains a molybdenum centre bearing a P,P′-cis-chelating Ph2PN( i Pr)P(Ph)NH( i Pr) and four carbonyl ligands in a distorted octahedral coordination geometry. This results in a nearly planar four-membered metallacycle. In the crystal, molecules are linked by N—H...O and C—H...O hydrogen bonds to form layers parallel to the ac plane. For the final refinement, the contributions of disordered solvent molecules were removed from the diffraction data with SQUEEZE in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

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Crystal structure of bis{1-[(E)-(2-methoxyphenyl)diazenyl]naphthalen-2-olato-κ3O,N2,O′}copper(II) containing an unknown solvate

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989015019817 ◽

2015 ◽

Vol 71 (11) ◽

pp. m207-m208 ◽

Cited By ~ 3

Author(s):

Souheyla Chetioui ◽

Noudjoud Hamdouni ◽

Djamil-Azzeddine Rouag ◽

Salah Eddine Bouaoud ◽

Hocine Merazig

Keyword(s):

Crystal Structure ◽

Hydrogen Bonds ◽

Electron Density ◽

Title Complex ◽

Unit Cell ◽

Asymmetric Unit ◽

Acta Cryst ◽

Coordination Environment ◽

Independent Molecules ◽

Solvent Molecules

The title complex, [Cu(C17H13N2O2)2], crystallizes with two independent molecules in the asymmetric unit. Each CuIIatom has a distorted ocahedral coordination environment defined by two N atoms and four O atoms from two tridentate 1-[(E)-(2-methoxyphenyl)diazenyl]naphthalen-2-olate ligands. In the crystal, the two molecules are linkedviaweak C—H...O hydrogen bonds which in turn stack parallel to [010]. A region of disordered electron density, most probably disordered methanol solvent molecules, was corrected for using the SQUEEZE routine inPLATON[Spek (2015).Acta Cryst.C71, 9–18]. Their formula mass and unit-cell characteristics were not taken into account during refinement.

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(E)-4-[4-(Dimethylamino)styryl]-1-methylpyridin-1-ium tetrakis[(Z)-4,4,4-trifluoro-3-oxo-1-(thiophen-2-yl)but-1-en-1-olato]gadolinate(III) with an unknown amount of water as solvate

IUCrData ◽

10.1107/s2414314616017272 ◽

2016 ◽

Vol 1 (11) ◽

Author(s):

Da-Jun Wu ◽

Bin Fang

Keyword(s):

Complex Anion ◽

Water Molecules ◽

Crystal Data ◽

Chemical Formula ◽

Acta Cryst ◽

Data Set ◽

Benzene Rings ◽

Solvent Molecules ◽

The Given ◽

Complex Anions

In the complex anion of the title salt, (C16H19N2)[Gd(C8H4F3S)4], the GaIIIcation isO,O′-chelated by four anionic 4,4,4-trifluoro-3-oxo-1-(thiophen-2-yl)but-1-en-1-olate ligands in a distorted square-antiprismatic geometry; the 4-[4-(dimethylamino)styryl]-1-methylpyridin-1-ium cation is nearly planar, with a dihedral angle of 9.6 (5)° between the planes of the pyridine and benzene rings. In the crystal, the cations are linked with the complex anionsviaweak C—H...F and C—H...π interactions. Two of the four independent thiophene rings are disordered over two sites; occupancies were refined to 0.662 (10):0.338 (10). The solvent water molecules are highly disordered in a solvent-accessible void of 54 (3) Å3; the diffuse electron densities were removed from the data set using SQUEEZE [Spek (2015).Acta Cryst. C71, 9–16]. These solvent molecules are not considered in the given chemical formula and other crystal data.

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Crystal structure of [1,3-bis(2,4,6-trimethylphenyl)imidazolidin-2-ylidene]dichlorido{2-[1-(dimethylamino)ethyl]benzylidene}ruthenium including an unknown solvate

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989019001725 ◽

2019 ◽

Vol 75 (3) ◽

pp. 342-345 ◽

Cited By ~ 1

Author(s):

Kirill B. Polyanskii ◽

Kseniia A. Alekseeva ◽

Pavel A. Kumandin ◽

Zeliha Atioğlu ◽

Mehmet Akkurt ◽

...

Keyword(s):

Crystal Structure ◽

Chelate Ring ◽

Ruthenium Catalysts ◽

Stacking Interactions ◽

Crystal Data ◽

Acta Cryst ◽

Trigonal Bipyramidal ◽

Solvent Molecules ◽

New Generation ◽

The Given

The title compound, [RuCl2(C21H26N2)(C11H15N)], is an example of a new generation ofN,N-dialkyl metallocomplex ruthenium catalysts with an N→Ru coordination bond as part of a six-membered chelate ring. The Ru atom has an Addison τ parameter of 0.234, which indicates a geometry intermediate between square-based pyramidal and trigonal–bipyramidal. The complex shows the usualtransarrangement of the two chloride ligands, with Ru—Cl bond lengths of 2.3397 (8) and 2.3476 (8) Å, and a Cl—Ru— Cl angle of 157.47 (3)°. The crystal structure features C—H...Cl, C—H...π and π–π stacking interactions. The solvent molecules were found to be highly disordered and their contribution to the scattering was removed with the SQUEEZE procedure inPLATON[Spek (2015).Acta Cryst.C71, 9–18], which indicated a solvent cavity of volume 1096 Å3containing approximately 419 electrons. These solvent molecules are not considered in the given chemical formula and other crystal data.

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