The Preparation of a Mixed-Ligand Cobalt(III) Complex of DPPZ and Ethylenediamine: Crystal Structures of [Co(en)2(DPPZ)] (ClO4)3.0·5H2O, [Co(en)2(bpy)]Br(ClO4)2 and [Co(en)2(phen)] Br3

1999 ◽  
Vol 52 (8) ◽  
pp. 817 ◽  
Author(s):  
Alison M. Funston ◽  
Robert W. Gable ◽  
W. David McFadyen ◽  
Peter A. Tregloan
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Mixed Ligand ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Triclinic Space Group ◽  
Space Group ◽  
Octahedral Environment

The complex [Co(en)2(DPPZ)] (ClO4)3 (3) has been synthesized, and the crystal structures of this complex and those of [Co(en)2(bpy)] Br(ClO4)2 (1) and [Co(en)2(phen)] Br3 (2) have been determined. Crystal data for (1): M 614 . 13, monoclinic, space group C2/c (No. 15), a 16 . 7834(16), b 16 . 308(3), c 8 . 3167(15) Å, β 104 . 932(11)°, V 2199 . 4(6) Å, F(000) 1240, Z 4, Dc 1 . 855 g cm−3, µ 2 . 895 cm−1 , Mo Kα (graphite monochromatized) radiation, γ 0 . 71073 Å, T 293(1) K. Crystal data for (2): M 599 . 07, triclinic, space group P1 (No. 2), a 7 . 7113(11), b 10 . 633(2), c 12 . 9884(18) Å, α 85 . 745(15), b 78 . 258(11), γ 74 . 967(16)°, V 1006 . 7(3) Å, F(000) 588, Z 2, Dc 1 . 976 g cm−3, µ6 . 819 cm−1 , MoKα (graphite monochromatized) radiation, γ 0 . 71073 Å, T 293(1) K. Crystal data for (3): M 773 . 44, monoclinic, space group P 21/c (No. 14), a 20 . 296(2), b 9 . 6197(11), c 15 . 725(2) Å, β 92 . 850(10)°, V 3066 . 4(6) Å, F(000) 1579, Z 4, Dc 1 . 675 g cm−3 , µ 0 . 898 cm−1 , MoKα(graphite monochromatized) radiation, γ 0 . 71073 Å, T 293(1) K. In all three complexes the cobalt is in the usual octahedral environment, with the cations being linked by hydrogen bonds between the amine hydrogens and the anions into extended structures.

The Synthesis and Crystal Structures of Two Cobalt(III) Complexes Containing the Ligand 1,4,8,11-Tetraazacyclotetradecane

2002 ◽  
Vol 55 (8) ◽  
pp. 535 ◽  
Author(s):  
A. M. Funston ◽  
W. D. McFadyen ◽  
P. A. Tregloan
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Triclinic Space Group ◽  
Space Group ◽  
Octahedral Environment ◽  
Related Complex

The new cobalt(III) complex [Co(cyclam)(NO3)2]NO3�HNO3 (2) has been synthesized. The crystal structure of this complex and the related complex [Co(cyclam)(NH3)2]Cl2BF4�2H2O (1) have been determined. Crystal data for (1): M 451.04, monoclinic, space group P21/c (No. 14), a 7.3927(10), b 13.3082(7), c 19.524(2) Å, β 97.625(14)�, V 1903.9(3) Å3, F(000) 936, Z 4, Dc 1.574 g cm–3, μ 1.225 cm–1, Mo Kα (graphite monochromatized) λ 0.71073 Å, T 293(1) K. Crystal data for (2): M 571.33, triclinic, space group P1–(No. 2),a 7.3988(14), b 8.5682(16), c�9.209(3) Å, α 89.02(2), β 76.64(3), γ 82.340(16)�, V 562.9(2) Å3, F(000) 296, Z 1, Dc 1.685 g cm–3, μ 0.854 cm–1, Mo Kα (graphite monochromatized) λ 0.71073 Å, T 293(1) K. In both complexes the complex crystallizes in the trans-III form with the cobalt in the usual octahedral environment.

The Crystal Structures of 2-(3’-Hydroxypropyl)benzimidazolium Hexa- and Tetrachloroplatinate

2005 ◽  
Vol 60 (2) ◽  
pp. 164-168 ◽  
Author(s):  
A. Elmali ◽  
Y. Elerman ◽  
G. Eren ◽  
F. Gümüş ◽  
I. Svoboda
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Intermolecular Hydrogen Bonds ◽  
Triclinic Space Group ◽  
Space Group

2-(3’-Hydroxypropyl)benzimidazolium (Hhpb) hexa- and tetrachloroplatinate (C10H13N2O)2·[PtCl6] 1 and (C10H13N2O)2·[PtCl4] 2 were synthesized and their crystal structures determined. Compound 1 is monoclinic, space group P21/n, a = 8.800(1), b = 14.389(2), c = 10.264(2) Å, β = 98.540(10)°, V = 1285.3(3) Å3, Z = 2 and Dc = 1.959 g cm−3. Compound 2 is triclinic, space group P1̄, a=7.8480(10), b=9.0460(10), c=9.6980(10) Å ,α =65.420(10), β =68.810(10), γ = 76.770(1)°,V =581.26(4) Å3, Z =1 and Dc =1.969 g cm−3. In both compounds, the Pt atoms reside at a centre of inversion. Compounds 1 and 2 are comprised of 2-(3’-hydroxypropyl)benzimidazolium (Hhpb)+: (C10H12N2O)+ and [PtCl6]2− and [PtCl4]2− ions, respectively, linked by intermolecular hydrogen bonds N...Cl [range from 3.428(3) to 3.584(4) Å ], N···O [2.769(5) Å ] and O···Cl [3.338(4) and 3.321(3) Å ] for 1, and N···Cl [3.162(7) Å ], N···O [2.749(8) Å ] and O···Cl [3.289(6) Å ] for 2.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.

Strukturen der mehrkernigen nickelthiolato-komplexe [(μ-SMe)2(Ni(MeNHCS2))2] und cyclo-[(μ-SMe)2Ni]6 / Structures of Two Polynuclear Nickel-Thiolato-Complexes [(μ-SMe)2(Ni(MeNHCS2))2] and cyclo-[(μ-SMe)2Ni]6

1994 ◽  
Vol 49 (6) ◽  
pp. 770-772 ◽  
Author(s):  
Klaus Schulbert ◽  
Rainer Mattes
Keyword(s):  
Crystal Structures ◽  
Nickel Acetate ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Dithiocarbamic Acid ◽  
Coordination Spheres ◽  
Partial Degradation ◽  
Acid Esters

The reactions of N-substituted dithiocarbamic acid esters and nickel acetate yield, by partial degradation of the esters, the polynuclear nickel thiolato complexes cyclo-[(μ-SMe)2Ni]6, 1 and [(μ-SMe)2(Ni(MeNHCS2))2, 2. Their crystal structures have been determined. The Ni coordination spheres are comprised of four sulfur atoms in a planar arrangement. 1 is a second, highly symmetrical modification of the already known cyclic hexamer Ni6(SMe)12. In 2 two Ni(PhNHCS2) moieties are bridged to dimers by thiolato groups. Two of these dimers are connected to a tetramer by weak axial Ni-S interactions. Crystal data for 1: monoclinic, space group P21/n, a = 986.1(2), b = 1308.1(3), c = 1228.6(2) pm, β = 96.07(3)°, Z = 2, R = 0.072, Rw = 0.062, 3797 reflections. 2: orthorhombic, space group Pnma, a = 1790.0(4), b = 1806.7(4), c = 934.4(2) pm. Z = 4, R = 0.061, Rw = 0.051, 2079 reflections

79Br, 127I NQR of Diammoniumalkyl Halides and Piperazinium Halides. Crystal Structure of Piperazinium Dibromide Monohydrate and Piperazinium Monoiodide

1989 ◽  
Vol 44 (1) ◽  
pp. 41-55 ◽  
Author(s):  
Jutta Hartmann ◽  
Shi-Qi Dou ◽  
Alarich Weiss
Keyword(s):  
Crystal Structure ◽  
Phase Transitions ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Temperature Range

Abstract The 79Br and 127I NQR spectra were investigated for 1,2-diammoniumethane dibromide, -diiodide, 1,3-diammoniumpropane dibromide, -diiodide, piperazinium dibromide monohydrate, and piperazinium monoiodide in the temperature range 77 ≦ T/K ≦ 420. Phase transitions could be observed for the three iodides. The temperatures for the phase transitions are: 400 K and 404 K for 1,2-diammoniumethane diiodide, 366 K for 1,3-diammoniumpropane diiodide, and 196 K for piperazinium monoiodide.The crystal structures were determined for the piperazinium compounds. Piperazinium dibromide monohydrate crystallizes monoclinic, space group C2/c, with a= 1148.7 pm, 0 = 590.5 pm, c= 1501.6pm, β = 118.18°, and Z = 4. For piperazinium monoiodide the orthorhombic space group Pmn 21 was found with a = 958.1 pm, b = 776.9 pm, c = 989.3 pm, Z = 4. Hydrogen bonds N - H ... X with X = Br, I were compared with literature data.

Untersuchungen an Polyhalogeniden, XXXVI. Zur Kenntnis des Oktaiodid-Ions I82-: Darstellung und Kristallstruktur des [(Crypt-2.2.2)H2]l8, des [Ni(phen)3]I8 · 2CHCl3 und der Bis(N-alkylurotropinium) oktaiodide (UrR)2I8 mit R = Methyl und Ethyl / Studies on Polyhalides, XXXVI. On the Octaiodide Ion I82-: Preparation and Crystal Structure of [(Crypt-2.2.2)H2]I8, of [Ni(phen)3]I8-2CHCl3 and of the Bis(N-alkylurotropinium)octaiodides (UrR)2I8 with R = methyl and ethyl

1998 ◽  
Vol 53 (7) ◽  
pp. 641-652 ◽  
Author(s):  
Arista Gräfe-Kavoosian ◽  
Shida Nafepour ◽  
Klaus Nagel ◽  
Karl-Friedrich Tebbe
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Iodine Molecule ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group

Abstract The new compound [(Crypt-2.2.2)H2]I8 has been prepared by the reaction of [(Crypt-2.2.2)H2](I3)2 with iodine in methanol. It crystallizes in the orthorhombic space group Pbcn with a = 11.476 (2), b = 13.589 (2), c = 22.888 (2) Å and Z = 4. The crystal structure has been refined to RF = 0.031 for 1618 reflections. It may be described as a layerlike packing of octaiodide anions I82-and diprotonated 2.2.2-Crypt as cations. The non planar octaiodide anion is built up from two triiodide groups and a bridging iodine molecule.Tris(1, 10-phenanthroline)nickel(II) octaiodide bis(chloroform) crystallizes in the monoclinic space group P21/n with a = 11.683 (8), b = 21.717 (8), c = 20.752 (5) Å, β = 95.03 (5)° and Z = 4 formula units. The crystal structure has been refined to RF = 0.058 for 3894 reflections. The structure consists of two chloroform molecules, octahedrally coordinated complex cations [Ni(phen)3]2+ and nonplanar octaiodide anions I82- each composed of two asymmetric triiodide units I3- weakly associated with an elongated bridging iodine molecule I2.The already known structure of bis(N-methylurotropinium) octaiodide, (UrMe)2I8, has been verified and more accurate crystal data have been collected. The crystal structure has been refined to RF = 0.045 for 1908 reflections. The compound crystallizes in the monoclinic space group P21/c with a = 11.302 (2), b = 9.850 (2), c = 14.188 (2) Å , β = 92.59 (1)° and Z = 2. The anion has the shape of a stretched Z.The structure of bis(N-ethylurotropinium) octaiodide (UrEt)2I8 has been determined and a new configuration (I3-, I5-) for octaiodide ions between Z (I3- · I2 ·I3-) and a “broken” configuration (I3-, I5-) has been observed. The compound crystallizes in the triclinic space group P1̄ with a = 9.741 (3), b = 11.815 (3), c = 15.426 (3) Å, α = 91.80 (2), β = 107.14 (2), γ = 90.04 (2)° and Z = 2. The crystal structure has been refined to RF = 0.037 for 3657 reflections.

Three polymorphs of 3-(3-phenyl-1H-1,2,4-triazol-5-yl)-2H-1-benzopyran-2-one formed from different solvents

2019 ◽  
Vol 75 (6) ◽  
pp. 822-832 ◽  
Author(s):  
Svitlana V. Shishkina ◽  
Irina S. Konovalova ◽  
Pavlo V. Trostianko ◽  
Anna O. Geleverya ◽  
Sergiy M. Kovalenko ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Pairwise Interaction ◽  
Structural Motif ◽  
Monoclinic Space Group ◽  
Interaction Energies ◽  
Orthorhombic Space Group ◽  
Structure Packing ◽  
Triclinic Space Group ◽  
Space Group ◽  
Polymorphic Modifications

The polymorphic study of 3-(3-phenyl-1H-1,2,4-triazol-5-yl)-2H-1-benzopyran-2-one, C17H11N3O2, was performed due to its potential biological activity and revealed three polymorphic modifications in the triclinic space group P\overline{1}, the monoclinic space group P21 and the orthorhombic space group Pbca. These polymorphs have a one-column layered type of crystal organization. The strongest interactions between the molecules of the studied structures is stacking between π-systems, while N—H...N and C—H...O hydrogen bonds link stacked columns forming layers as a secondary basic structural motif. C—H...π hydrogen bonds were observed between neighbouring layers and their role is the least significant in the formation of the crystal structure. Packing differences between the polymorphic modifications are minor and can be identified only using an analysis based on a comparison of the pairwise interaction energies.

Polysulfonylamine, CLXXXVIII [1]. Kristallstrukturen von drei Dimethylammonium-di(4-halogenbenzolsulfonyl)amiden (Halogen = Cl, Br, I) und von Dimethylammonium-di(4-methylbenzolsulfonyl)amid: Eine isotype Reihe mit strukturbestimmenden starken Wasserstoffbrücken und beiläufigen Halogenbrücken/ Polysulfonylamines, CLXXXVIII. Crystal Structures of Three Dimethylammonium Di(4-halobenzenesulfonyl)amides (Halogen = Cl, Br, I) and of Dimethylammonium Di(4-methylbenzenesulfonyl)amide: An Isotypical Series Featuring Strong Structure-determining Hydrogen Bonds and Incidental Halogen Bonds

2010 ◽  
Vol 65 (10) ◽  
pp. 1258-1266 ◽  
Author(s):  
Christoph Wölper ◽  
Alejandra Rodríguez-Gimeno ◽  
Matthias Freytag ◽  
Peter G. Jones ◽  
Armand Blaschette
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Causative Factor ◽  
Monoclinic Space Group ◽  
Halogen Bonds ◽  
Space Group ◽  
Dimethylammonium Chloride ◽  
Hydrogen Bonded

The four title compounds, Me2NH2+·(4-Cl/Br/I/Me-C6H4-SO2)2N-, were obtained by metathesis of dimethylammonium chloride with the corresponding silver di(arenesulfonyl)amides. The products crystallize isotypically in the monoclinic space group Cc (Z = 4, Z´ = 1). In each structure, the ionic entities associate into hydrogen-bonded chains, which propagate along the c axis of the crystals and consist of alternating cations and anions held together by charge-assisted N+-H· · ·N− and N+- H(· · ·O)2 hydrogen bonds. In the three structures containing 4-halobenzenesulfonyl groups, each hydrogen-bonded chain is linked to four neighboring chains by pairs of C-Cl/Br/I· · ·O halogen bonds, which at first sight seem to be the causative factor in the formation of catemeric head-to-tail arrays of anions propagating along the ab face diagonals. On suppressing these halogen bonds by means of halogen-methyl exchange, all essential features of the packing architecture, including the anion headto- tail arrays, are precisely maintained. It may be thus inferred that the halogen bonds occurring in the first three compounds are supportive incidentals, but do not play any structure-determining role.

Kristallstrukturen der iodierten closo-Hexaborate trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P)2[B6H2I4] · 2 CH3CN und (CH2Py2)[B6HI5]/Crystal Structures of the Iodized closo-Hexaborates trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P )2[B6H2I4] · 2 CH3CN and (CH2Py2)[B6HI5]

1998 ◽  
Vol 53 (2) ◽  
pp. 206-210 ◽  
Author(s):  
D. Sonnak ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

Abstract X-ray structure determinations have been performed on single crystals of trans-(Ph4P)2-[B6H4I2] (1) (triclinic, space group P1̄, a = 9.9680(12), b = 10.9690(11), c = 11.0470(14) Å,α = 88.167(9), β = 80.466(12), γ = 68.839(11)°, Z = 1), mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2 (2)(triclinic, space group P1̄, a = 11.8694(11), b = 15.1699(13), c = 17.051(2) Å, α = 75.118(9), β = 71.953(10), γ = 69.331(8)°, Z = 2), trans-(Ph4P )2[B6H2I4] · 2 CH3CN (3) (monoclinic, space group P21/n, a = 14.9665(10), b = 7.6783(10), c = 23.385(3) Å, β = 95.78(9)°, Z = 2), and (CH2Py2)[B6HI5] (4) (orthorhombic, space group Pnma, a = 13.660(2), b = 11.8711(13), c = 13.839(2) Å, Z = 4). The B6 octahedra are compressed in the direction of the B-I bonds, resulting in shortened diagonal B ··· B distances with average values of the groups I-B ··· B-I = 2.37 and I-B ··· B-H = 2.43 Å as compared with H-B ··· B-H = 2.49 Å.

Synthese und Kristallstrukturen von N-[ω-(Dimethylammonio)alkyl]- N´,N´,N´´,N´´-tetramethylguanidinium-chlorid-tetraphenylboraten / Synthesis and Crystal Structures of N-[ω-(Dimethylammonio)alkyl]-N´,N´,N´´,N´´- tetramethylguanidinium Chloride Tetraphenylborates

2010 ◽  
Vol 65 (7) ◽  
pp. 907-916 ◽  
Author(s):  
Ioannis Tiritiris ◽  
Falk Lissner ◽  
Thomas Schleid ◽  
Willi Kantlehner
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Room Temperature ◽  
Chloride Ions ◽  
Monoclinic Space Group ◽  
Temperature Structure ◽  
Space Group ◽  
Temperature Modification

Dicationic N,N´,N´,N´´,N´´-pentasubstituted guanidinium dichlorides 4a, b are obtained from the chloroformamidinium salt 2 and diamines 3a, b. N-[2-(Dimethylammonio)ethyl]-N´,N´,N´´,N´´-tetramethylguanidinium chloride tetraphenylborate (5a) and N-[3-(dimethylammonio)propyl]-N´,N´,N´´,N´´-tetramethylguanidinium chloride tetraphenylborate (5b) were synthesized from 4a, b by anion metathesis with one equivalent of sodium tetraphenylborate. The thermal properties of the salts 5a, b were studied by means of DSC methods, and their crystal structures were determined by single-crystal X-ray diffraction analysis. For 5a a solid-solid phase transition is observed at −156 ◦C to a low-temperature structure. The room-temperature modification (α-5a) crystallizes in the centrosymmetric orthorhombic space group Pbca (a = 13.1844(4), b = 13.8007(4), c = 34.7537(11) A° ).The guanidinium ions are interconnected via chloride ions through bridging N-H· · ·Cl hydrogen bonds, providing isolated units. The tetraphenylborate ions show some dynamic disordering in the crystal structure. The low-temperature modification (β -5a) also crystallizes orthorhombically, but in the non-centrosymmetric space group Pna21 (a = 13.1099(4), b = 69.1810(11), c = 13.5847(5) A° ) and consists of four crystallographically independent cations and anions in the unit cell. Compared with the room-temperature structure, a similar N-H· · ·Cl hydrogen bond pattern is observed in the β -phase, but the tetraphenylborate ions are now completely ordered. 5b crystallizes in the monoclinic space group P21/c (a = 10.8010(3), b = 14.1502(5), c = 20.9867(9) A° , β = 94.322(1)◦). In the crystal structure the guanidinium ions are linked via chloride ions through N-H· · ·Cl hydrogen bonds, but in contrast to 5a two infinite strands are formed along the a axis with the tetraphenylborate ions interspersed between them for charge compensation.

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