A New Study of the Acid Rhodo Complex Salt [(NH3)5CrOHCr(NH3)5]Cl5.H2O Shows That the Crystals are Orthorhombic

1997 ◽  
Vol 53 (5) ◽  
pp. 795-802 ◽  
Author(s):  
P. Harris ◽  
H. Birkedal ◽  
S. Larsen ◽  
H. U. Güdel
Keyword(s):  
Hydrogen Bond ◽  
Magnetic Measurements ◽  
Structural Models ◽  
Complex Salt ◽  
Relative Orientation ◽  
Tetragonal Symmetry ◽  
Orthorhombic Space Group ◽  
Satisfactory Description ◽  
Space Groups ◽  
Chloride Monohydrate

Diffraction data recorded at low temperature with Mo K\alpha from two different crystals have been used in the refinement of the structure of the acid rhodo complex salt, \mu-hydroxo-bis[pentaamminechromium(III)] chloride monohydrate [(NH3)5CrOHCr(NH3)5]Cl5.H2O. Several structural models in two different tetragonal space groups have been investigated before a satisfactory description of the structure was obtained. The compound crystallizes in the orthorhombic space group P212121, with a= 16.155 (3), b = 16.154 (3), c = 14.750 (7) Å and Z = 8. The apparent tetragonal symmetry arises due to rotation twinning of the crystals. The diffraction pattern is further complicated by tetragonal pseudo-symmetry of the chromium sites, which means that reflections with l = 2n + 1 are systematically weak. The two independent dimeric cations are involved in slightly different hydrogen-bond patterns. This observation and the relative orientation of the dimers in the crystal is in accordance with spectral and magnetic measurements.

Supramolecular assembling using synthons with NH—CO(S)—CS—NH and NH—CO—CO—NH functionalities: crystal structures of (S,S)-N,N′-monothiooxalyldileucine methyl ester and its dithio analogue

2004 ◽  
Vol 60 (1) ◽  
pp. 90-96 ◽  
Author(s):  
Biserka Kojić-Prodić ◽  
Berislav Perić ◽  
Zoran Štefanić ◽  
Anton Meden ◽  
Janja Makarević ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonding ◽  
Methyl Ester ◽  
Crystal Structures ◽  
Hydrogen Bond Network ◽  
Asymmetric Unit ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Bond Network ◽  
Bonding Systems

To compare the structural properties of oxalamide and thiooxalamide groups in the formation of hydrogen bonds suitable for supramolecular assemblies a series of retropeptides was studied. Some of them, having oxalamide bridges, are gelators of organic solvents and water. However, retropeptides with oxygen replaced by the sp 2 sulfur have not exhibited such properties. The crystal structures of the two title compounds are homostructural, i.e. they have similar packing arrangements. The monothio compound crystallizes in the orthorhombic space group P212121 with two molecules in the asymmetric unit arranged in a hydrogen-bond network with an approximate 41 axis along the crystallographic b axis. However, the dithio and dioxo analogues crystallize in the tetragonal space group P41 with similar packing patterns and hydrogen-bonding systems arranged in agreement with a crystallographic 41 axis. Thus, these two analogues are isostructural having closely related hydrogen-bonding patterns in spite of the different size and polarity of oxygen and sulfur which serve as the proton acceptors.

scholarly journals Ice XIX: The second hydrogen-ordered polymorph related to ice VI

2020 ◽  
Author(s):  
Tobias Gasser ◽  
Alexander Thoeny ◽  
Andrew Fortes ◽  
Thomas Loerting
Keyword(s):  
High Resolution ◽  
Ambient Pressure ◽  
Structural Models ◽  
Neutron Powder Diffraction ◽  
Ex Situ ◽  
Water Molecules ◽  
Powder Diffraction Data ◽  
Space Groups ◽  
First Order ◽  
Neutron Powder Diffraction Data

Abstract We here report ex situ calorimetry and high-resolution neutron powder diffraction data of a novel ice polymorph produced at 1.8 GPa and recovered to ambient pressure at 80 K. Ice XIX, previously called ice β-XV by us, is shown to be partially hydrogen-ordered and crystallising in a √2 x √2 × 1 supercell with respect to the parent ice VI phase. Our powder data match two nearly degenerate structural models in space-groups \(P\stackrel{-}{4}\) and Pcc2, in which the water molecules are partially antiferroelectrically ordered. Key to the synthesis of deuterated ice XIX is the use of DCl as dopant and the use of a D2O/H2O mixture, where the small H2O fraction nucleates ice XIX. This provides the basis to study the first order-order transition known in ice physics, from ice XIX to its sibling ice XV at ambient pressure. It proceeds via a transition state, ice VI‡, which contains a disordered H-sublattice, whereas both ice XIX and ice XV are fully crystalline.

scholarly journals Chiral crystallization of a zinc(II) complex

2021 ◽  
Vol 77 (5) ◽  
pp. 542-546
Author(s):  
Shabana Noor ◽  
Shintaro Suda ◽  
Tomoyuki Haraguchi ◽  
Fehmeeda Khatoon ◽  
Takashiro Akitsu
Keyword(s):  
Hydrogen Bond ◽  
Schiff Base ◽  
Complex Molecule ◽  
Solvent Molecule ◽  
Hirshfeld Surface ◽  
Supramolecular Interactions ◽  
Orthorhombic Space Group ◽  
Complex Molecules ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The compound, {6,6′-dimethoxy-2,2′-[(4-azaheptane-1,7-diyl)bis(nitrilomethanylidyne)]diphenolato}zinc(II) methanol monosolvate, [Zn(C22H27N3O4)]·CH3OH, at 298 K crystallizes in the orthorhombic space group Pna21. The Zn atom is coordinated by a pentadentate Schiff base ligand in a distorted trigonal–bipyramidal N3O2 geometry. The equatorial plane is formed by the two phenolic O and one amine N atom. The axial positions are occupied by two amine N atoms. The distorted bipyramidal geometry is also supported by the trigonality index (τ), which is found to be 0.85 for the molecule. In the crystal, methanol solvent molecule is connected to the complex molecule by an O—H...O hydrogen bond and the complex molecules are connected by weak supramolecular interactions, so achiral molecules generate a chiral crystal. The Hirshfeld surface analysis suggests that H...H contacts account for the largest percentage of all interactions.

scholarly journals Synthesis, Crystal Structure, Spectroscopic Properties, and Hirshfeld Surface Analysis of Diaqua [3,14-dimethyl-2,6,13,17 tetraazatricyclo(16.4.0.07,12)docosane]copper(II) Dibromide

Crystals ◽  
2019 ◽  
Vol 9 (7) ◽  
pp. 336 ◽  
Author(s):  
Jeon ◽  
Moncol ◽  
Mazúr ◽  
Valko ◽  
Choi
Keyword(s):  
Hydrogen Bonds ◽  
Surface Analysis ◽  
Macrocyclic Ligand ◽  
Complex Salt ◽  
Spectroscopic Properties ◽  
Hirshfeld Surface ◽  
Hirshfeld Surface Analysis ◽  
Axial Position ◽  
Tetragonal Symmetry ◽  
Water Molecules

A newly prepared Cu(II) complex salt, Cu(L1)(H2O)2Br2, where L1 is 3,14-dimethyl-2,6,13,17-tetraazatricyclo(16.4.0.07,12) docosane, is characterized by elemental and crystallographic analyses. The Cu(II) center is coordinated by four nitrogen atoms of macrocyclic ligand and the axial position by two water molecules. The macrocyclic ligand adopts an optimally stable trans-III conformation with normal Cu–N bond lengths of 2.018 (3) and 2.049 (3) Å and long axial Cu1–O1W length of 2.632 (3) Å due to the Jahn–Teller effect. The complex is stabilized by hydrogen bonds formed between the O atoms of water molecules and bromide anions. The bromide anion is connected to the neighboring complex cations and water molecules through N–H···Br and O–H···Br hydrogen bonds, respectively. The g-factors obtained from the electron spin resonance spectrum show the typical trend of g∥ > g⊥ > 2.0023, which is in a good accordance to the dx2-y2 ground state. It reveals a coordination sphere of tetragonal symmetry for the Cu(II) ion. The infrared and electronic absorption spectral properties of the complex are also discussed. Hirshfeld surface analysis represents that the H···H, H···Br/Br···H and H···O/O···H contacts are the major molecular interactions in the prepared complex.

scholarly journals Isomers and polymorphs of (E,E)-1,4-bis(nitrophenyl)-2,3-diaza-1,3-butadienes

2006 ◽  
Vol 62 (4) ◽  
pp. 666-675 ◽  
Author(s):  
Christopher Glidewell ◽  
John N. Low ◽  
Janet M. S. Skakle ◽  
James L. Wardell
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Stacking Interactions ◽  
Space Group ◽  
Stacking Interaction ◽  
Space Groups ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
Polymorphic Forms

The structures of five of the possible six isomers of (E,E)-1,4-bis(nitrophenyl)-2,3-diaza-1,3-butadiene are reported, including two polymorphs of one of the isomers. (E,E)-1,4-Bis(2-nitrophenyl)-2,3-diaza-1,3-butadiene, C14H10N4O4 (I), crystallizes in two polymorphic forms (Ia) and (Ib) in which the molecules lie across centres of inversion in space groups P21/n and P21/c, respectively: the molecules in (Ia) and (Ib) are linked into chains by aromatic π...π stacking interactions and C—H...π(arene) hydrogen bonds, respectively. Molecules of (E,E)-1-(2-nitrophenyl)-4-(3-nitrophenyl)-2,3-diaza-1,3-butadiene (II) are linked into sheets by two independent C—H...O hydrogen bonds. The molecules of (E,E)-1,4-bis(3-nitrophenyl)-2,3-diaza-1,3-butadiene (III) lie across inversion centres in the space group P21/n, and a combination of a C—H...O hydrogen bond and a π...π stacking interaction links the molecules into sheets. A total of four independent C—H...O hydrogen bonds link the molecules of (E,E)-1-(3-nitrophenyl)-4-(4-nitrophenyl)-2,3-diaza-1,3-butadiene (IV) into sheets. In (E,E)-1,4-bis(4-nitrophenyl)-2,3-diaza-1,3-butadiene (V) the molecules, which lie across centres of inversion in the space group P21/n, are linked by just two independent C—H...O hydrogen bonds into a three-dimensional framework.

Relative configuration, absolute configuration and absolute structure of three isomeric 8-benzyl-2-[(4-bromophenyl)(hydroxy)methyl]-8-azabicyclo[3.2.1]octan-3-ones

2013 ◽  
Vol 69 (3) ◽  
pp. 303-306 ◽  
Author(s):  
Krzysztof Brzezinski ◽  
Ryszard Lazny ◽  
Aneta Nodzewska ◽  
Katarzyna Sidorowicz
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Crystal Structures ◽  
Absolute Configuration ◽  
Compound I ◽  
Relative Configuration ◽  
Enantiomerically Pure ◽  
Space Groups ◽  
Intramolecular Hydrogen ◽  
Absolute Structure

The title compounds, C21H22BrNO2, are isomeric 8-benzyl-2-[(4-bromophenyl)(hydroxy)methyl]-8-azabicyclo[3.2.1]octan-3-ones. Compound (I), the (±)-exo,syn-(1RS,2SR,5SR,9SR) isomer, crystallizes in the hexagonal space groupR\overline{3}, while compounds (II) [the (+)-exo,anti-(1R,2S,5S,9R) isomer] and (III) [the (±)-exo,anti-(1RS,2SR,5SR,9RS) isomer] crystallize in the orthorhombic space groupsP212121andPna21, respectively. The absolute configuration was determined for enantiomerically pure (II). For the noncentrosymmetric crystal of (III), its absolute structure was established. In the crystal structures of (I) and (II), an intramolecular hydrogen bond is formed between the hydroxy group and the heterocyclic N atom. In the crystal structure of racemic (III), hydrogen-bonded chains of molecules are formedviaintermolecular O—H...O interactions. Additionally, face-to-edge π–π interactions are present in the crystal structures of (I) and (II). In all three structures, the piperidinone rings adopt chair conformations and theN-benzyl substituents occupy the equatorial positions.

Single-crystal neutron diffraction of urea-phosphoric acid: evidence for H-atom migration in a short hydrogen bond between 150 K and 350 K

2001 ◽  
Vol 216 (6) ◽  
Author(s):  
C. C. Wilson ◽  
K. Shankland ◽  
N. Shankland
Keyword(s):  
Hydrogen Bond ◽  
Neutron Diffraction ◽  
Phosphoric Acid ◽  
Single Crystal ◽  
Diffraction Data ◽  
Neutron Diffraction Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Short Hydrogen Bond ◽  
Atom Migration

AbstractThe structure of urea-phosphoric acid has been refined using single-crystal neutron diffraction data collected at seven temperatures in the range 150 K to 350 K. The structure is orthorhombic, space group

scholarly journals 3-(4-Bromophenyl)cyclopent-2-en-1-one

2014 ◽  
Vol 70 (6) ◽  
pp. o692-o693
Author(s):  
Endrit Shurdha ◽  
Kelsey Dees ◽  
Hannah A. Miller ◽  
Scott T. Iacono ◽  
Gary J. Balaich
Keyword(s):  
Hydrogen Bond ◽  
Dihedral Angle ◽  
Title Compound ◽  
Crystal Packing ◽  
Relative Orientation ◽  
Weak Hydrogen Bond ◽  
Torsion Angles ◽  
Face To Face ◽  
Compound C ◽  
Side Face

In the title compound, C11H9BrO, the cyclopentenone ring is almost planar with an r.m.s. deviation of 0.0097 Å. The largest inter-ring torsion angles [2.4 (3), 1.3 (3) and 3.53 (2)°] reveal only a very small twist between the rings, and suggest that the two rings are conjugated. The molecule is slightly bowed, as shown by the small dihedral angle between the rings [5.3 (1)°]. The crystal packing pattern consists of parallel sheets that stack parallel to theacplane. Each sheet consists of molecules that pack side-to-side with the same relative orientation of phenyl and cyclopentenone rings along thea- andc-axis directions. Slipped side-to-side, face-to-face and edge-to-face interactions exist between pairs of sheets with edge-to-edge and edge-to-face O...H—C(sp2) weak hydrogen-bond contacts. A relatively short edge-to-face contact (2.77 Å) also exists between pairs of sheets.

scholarly journals Two orthorhombic polymorphs of hydromorphone

2016 ◽  
Vol 72 (5) ◽  
pp. 730-733
Author(s):  
Jaroslaw Mazurek ◽  
Marcel Hoffmann ◽  
Ana Fernandez Casares ◽  
D. Phillip Cox ◽  
Mathew D. Minardi ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Cyclic Ether ◽  
Hydroxyl Group ◽  
Analgesic Drug ◽  
Orthorhombic Space Group ◽  
Methyl Amine ◽  
Polymorphic Forms ◽  
Crystalline Forms ◽  
Crystallization From Solution

Conditions to obtain two polymorphic forms by crystallization from solution were determined for the analgesic drug hydromorphone [C17H19NO3; systematic name: (4R,4aR,7aR,12bS)-9-hydroxy-3-methyl-1,2,4,4a,5,6,7a,13-octahydro-4,12-methanobenzofuro[3,2-e]isoquinolin-7-one]. These two crystalline forms, designated as I and II, belong to theP212121orthorhombic space group. In both polymorphs, the hydromorphone molecules adopt very similar conformations with some small differences observed only in theN-methyl amine part of the molecule. The crystal structures of both polymorphs feature chains of molecules connected by hydrogen bonds; however, in form I this interaction occurs between the hydroxyl group and the tertiary amine N atom whereas in form II the hydroxyl group acts as a donor of a hydrogen bond to the O atom from the cyclic ether part.

scholarly journals (Acetamide-κO){2,2′,2′′-boranetriyltris[6-tert-butyl-4-methylpyridazine-3(2H)-thione]-κ4 B,S,S′,S′′}copper(I) trifluoromethanesulfonate chloroform disolvate

IUCrData ◽  
2018 ◽  
Vol 3 (1) ◽  
Author(s):  
Stefan Holler ◽  
Ferdinand Belaj ◽  
Nadia C. Mösch-Zanetti
Keyword(s):  
Hydrogen Bond ◽  
Equatorial Plane ◽  
Complex Salt ◽  
Amide Group ◽  
Trigonal Bipyramid ◽  
Tert Butyl ◽  
Bifurcated Hydrogen Bond ◽  
Scorpionate Ligand

In the title solvated complex salt, [Cu(C27H39BN6S3)(C2H5NO)](CF3O3S)·2CHCl3, the CuI atom is coordinated by the three S atoms of the pyridazine-3-thione rings in the equatorial plane [Cu—S = 2.3072 (4)–2.3280 (4) Å] and the B atom of the scorpionate ligand and the O atom of an acetamide ligand as the apices of a trigonal bipyramid [Cu—B = 2.0456 (16) Å and Cu—O = 1.9957 (11) Å]. The amide group of the latter ligand is involved in a bifurcated hydrogen bond to the trifluoromethanesulfonate anion.

Sign in / Sign up

Export Citation Format

Share Document