Manifestations of noncovalent interactions in the solid state. 3. X-ray crystal structures of [H4(cyclam)][FeCl5(OH2)](Cl)2 and [H4(cyclam)][CF3COO]4, two network hydrogen bonded solids

1993 ◽  
Vol 71 (4) ◽  
pp. 433-440 ◽  
Author(s):  
S. Subramanian ◽  
Michael J. Zaworotko
Keyword(s):  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Rational Design ◽  
Complex Anion ◽  
Noncovalent Interactions ◽  
Polar Space ◽  
Space Group ◽  
X Ray ◽  
Dark Orange ◽  
Interionic Hydrogen

FeCl2 or FeCl3 react with cyclam (cyclam = 1,4,8,11-tetraazacyclotetradecane) in an acidic medium (4 M HCl) to afford dark orange-red plates of [H4(cyclam)][FeCl5(OH2)](Cl)2 (1). 1 crystallizes in a polar space group (orthorhombic, Pc21b) with a = 10.7730(6), b = 13.3418(10), c = 14.4564(10) Å, V = 2077.84(24) Å3, and Dcalc = 1.68 g cm−3 for Z = 4. Final values of R = 0.031 and Rw = 0.034 were obtained for 1950 independent observed (I > 3σ(I)) reflections. Cyclam reacts with neat trifluoroacetic acid to afford a colourless salt, [H4(cyclam)][CF3COO]4 (2). 2 crystallizes in a centric space group (monoclinic, P21/c), with a = 8.7442(11), b = 10.5121(11), c = 15.2469(20) Å, β = 102.526(15)°, V = 1368.1(3) Å3, and Dcalc = 1.593 g cm−3 for Z = 2. Final values of R = 0.059 and Rw = 0.067 were obtained for 1336 independent observed (I > 3σ(I)) reflections. Extensive interionic hydrogen bonding between the cyclam cations, which adopt exodentate conformations, and anions results in network polymeric hydrogen bonding (1-D for 1, 2-D for 2). The networking in 1 is intrinsically polar because one chloride anion and the [FeCl5(OH2)]2− complex anion are involved in networking between the H4(cyclam)4+ cations. The implications of the crystal structures are discussed from the perspective of rational design of polar solids.

Tautomerism and hydrogen bonding in guaninium phosphite and guaninium phosphate salts

2007 ◽  
Vol 63 (3) ◽  
pp. 448-458 ◽  
Author(s):  
El-Eulmi Bendeif ◽  
Slimane Dahaoui ◽  
Nourredine Benali-Cherif ◽  
Claude Lecomte
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Data Sets ◽  
Hydrogen Bond Network ◽  
Space Group ◽  
X Ray ◽  
Bond Network ◽  
Phosphate Salts

The crystal structures of three similar guaninium salts, guaninium monohydrogenphosphite monohydrate, C5H6N5O+·H2O3P−·H2O, guaninium monohydrogenphosphite dihydrate, C5H6N5O+·H2O3P−·2H2O, and guaninium dihydrogenmonophosphate monohydrate, C5H6N5O+·H2O4P−·H2O, are described and compared. The crystal structures have been determined from accurate single-crystal X-ray data sets collected at 100 (2) K. The two phosphite salts are monoclinic, space group P21/c, with different packing and the monophosphate salt is also monoclinic, space group P21/n. An investigation of the hydrogen-bond network in these guaninium salts reveals the existence of two ketoamine tautomers, the N9H form and an N7H form.

Crystal structures of cefdinir, C14H13N5O5S2, and cefdinir sesquihydrate C14H13N5O5S2(H2O)1.5

2019 ◽  
Vol 34 (3) ◽  
pp. 267-278
Author(s):  
Austin M. Wheatley ◽  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Density Functional ◽  
Powder Diffraction Data ◽  
Powder Diffraction File ◽  
Space Group ◽  
X Ray ◽  
Additional Hydrogen

The crystal structures of cefdinir and cefdinir sesquihydrate have been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Cefdinir crystallizes in space group P21 (#4) with a = 5.35652(4), b = 19.85676(10), c = 7.57928(5) Å, β = 97.050(1) °, V = 800.061(6) Å3, and Z = 2. Cefdinir sesquihydrate crystallizes in space group C2 (#5) with a = 23.98775(20), b = 5.01646(3), c = 15.92016(12) Å, β = 109.4470(8) °, V = 1806.438(16) Å3, and Z = 4. The cefdinir molecules in the anhydrous crystal structure and sesquihydrate have very different conformations. The two conformations are similar in energy. The hydrogen bonding patterns are very different in the two structures, and the sesquihydrate is more stable than expected from the sum of the energies of cefdinir and cefdinir sesquihydrate, the result of additional hydrogen bonding. The powder patterns are included in the Powder Diffraction File™ as entries 00-066-1604 (cefdinir) and 00-066-1605 (cefdinir sesquihydrate).

scholarly journals Crystal Structures of Two Macrocyclic Bischalcones Possessing 26-Membered Rings

2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Rina Mondal ◽  
Nayim Sepay ◽  
Debajyoti Ghoshal ◽  
Asok K. Mallik
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Crystal Structures ◽  
Membered Ring ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonding Interactions

Single crystal X-ray diffraction of two macrocyclic bischalcones, namely, (2E,25E)-11,17,33,37-tetraoxapentacyclo[36.4.0.05,10.018,23.027,32]dotetraconta-1(42),2,5,7,9,18,20,22,25,27,29,31,38,40-tetradecaene-4,24-dione(1) and (2E,24E)-11,16,32,37-tetraoxapentacyclo[36.4.0.05,10.017,22.026,31]dotetraconta-1(42),2,5,7,9,17,19,21,24,26,28,30,38,40-tetradecaene-4,23-dione(2), each containing a 26-membered ring, has been studied. Compound 1 belongs to the monoclinic system, space group C2/c with a = 34.3615(9) Å, b = 12.7995(3) Å, c = 14.6231(3) Å, β = 96.912(2)°,  V = 6,384.6(3) Å3, and Z = 8. Compound 2 is triclinic, space group P-1 with a = 10.066(2) Å, b = 10.670(3) Å, c = 16.590(3) Å, α = 85.95(2), β = 89.244(14), γ = 62.211(13), V = 1572.0(6) Å3, and Z = 2. Intermolecular C–H⋯O hydrogen bonding interactions are present in both compounds.

Novel hydrogen bonding in crystalline tetra-n-butylammonium salts of catechol halides

1985 ◽  
Vol 63 (8) ◽  
pp. 2119-2122 ◽  
Author(s):  
Masood A. Khan ◽  
Archibald W. McCulloch ◽  
A. Gavin McInnes
Keyword(s):  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Halide Anions ◽  
Cell Dimensions

The crystal structures of [N(n-C4H9)4] [catechol … Cl] (1) and [N(n-C4H9)4] [catechol … Br] (2) have been determined by X-ray analysis which showed that the two structures are isomorphous, with the orthorhombic space group Pbca, Z = 8. The cell dimensions and final R-values are: (1) a = 15.323(2), b = 16.166(2), c = 19.713(2) Å, R = 0.048 for 1361 observed reflections; (2) a = 15.432(1), b = 16.244(2), c = 19.824(1) Å, R = 0.041 for 1958 observed reflections. The crystal structures consist of discrete tetra-n-butylammonium cations and catechol halide anions. Catechol forms two strong hydrogen bonds to a single halide ion giving a pattern of hydrogen bonding unique for such systems.

The absolute configuration of Λ-[Co(sen)] [(R,R)(+)tart] C1.6H2O and of Δ-[Co(sen)] [(R,R)(+)tart] C1.4. 5H2O (sen is 5-Methyl-5-(4-amino-2-azabutyl)-3,7-diazanonane-1,9-diamine): A comment on the mode of chiral resolutions by (R,R)(+)Tartrate on the antipodal cations of cobalt(III) salts

1984 ◽  
Vol 37 (11) ◽  
pp. 2365 ◽  
Author(s):  
I Bernal ◽  
JD Korp ◽  
II Creaser
Keyword(s):  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Absolute Configuration ◽  
Close Contact ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Local Block ◽  
Do So ◽  
Close Contacts

The X-ray crystal structures of the Λ and ∆ diastereoisomeric pair of [Co(sen)] [(R,R)(+)tart] ClnH2O (sen is 5-methyl-5-(4-amino-2-azabutyl)-3,7-diazanonane-1,9-diamine, tart is tartrate) have been determined. Crystals of the less soluble Λ isomer, (Λ-(1); n = 6), are othorhombic, space group P212121, with a 10.817(8), b 13.626(8), c 17.724(6) �, while those of the non-preferred Λ isomer, (Λ-(1); n = 4.5), are monoclinic, space group P21, with a 9,469(8), b 12.116(9), c 12.132(7) �, β 95.94(6)�. Both structures were solved by the Patterson method, and refined to R 3.8% (Λ-(1)) and 10.8% (Λ-(1)). In ∆-(1) the waters of hydration are partly disordered in the unit cell. Both crystal structures exhibit extensive hydrogen bonding; however, the mode of contact between the cation and the tartrate dianion in the two compounds is slightly different. In Λ-(1) the three amino hydrogens involved each have only one close contact to a tartrate oxygen, whereas in ∆-(1) each hydrogen has two close contacts. The mode of chiral resolution thus seems to depend on the strength of the hydrogen bonding found in this 'local block', and not simply on its ability to form such a block, since both enantiomers do so.

Hydrogen bonding in hydroxypyridium salts

2018 ◽  
Vol 233 (7) ◽  
pp. 501-506
Author(s):  
Andrei V. Mironov ◽  
Victor A. Tafeenko ◽  
Dmitrii Yu. Grebenkin ◽  
Alexander E. Oblezov
Keyword(s):  
Hydrogen Bonding ◽  
Oxygen Atom ◽  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Nitrate Anion ◽  
Single Crystal Diffraction ◽  
Space Group ◽  
X Ray ◽  
Unit Cells

Abstract The crystal structures of 6-methyl-2-ethyl-3-hydroxypyridiniun nitrate (C8H12NO)NO3 (I) and fumarate (C8H12NO)2C4H2O4 (II) were solved and refined from X-ray single crystal diffraction data (CuKα, (I) a=4.6477(2), b=14.5906(9), c=14.5551(8) Å, β=99.100(4)°, space group P21/c, Z=4, Rp/Rwp=0.033/0.047; (II) a=8.8293(3), b=13.4268(5), c=8.3893(3) Å, β=96.303(3)°, space group P21/c, Z=2, Rp/Rwp= 0.034/0.049). Both structures are built of infinite chains along ac diagonal of the unit cells formed by hydrogen bonding between the hydroxypyridium cation and the corresponding anion. Each fumarate anion is linked to four hydroxypyridium cations while nitrate anion is connected with two hydroxypyridium cations only leaving one oxygen atom in the nitrogen group isolated.

scholarly journals Über Verbindungen subvalenter Hauptgruppenmetallkationen mit Dithiolaten, 4. Mitteilung [1] Die Kristallstrukturen der Verbindungen Pb[S(CN)C=C(CN)S] und (AsPh4)2{Pb[S(CN)C=C(CN)S]2} / Compounds of Subvalent Main Group Metal Cations with Dithiolates, Part 4 [1] Crystal Structures of Pb[S(CN)C=C(CN)S] and (AsPh4)2{Pb[S(CN)C=C(CN)S]2}

1989 ◽  
Vol 44 (12) ◽  
pp. 1531-1537 ◽  
Author(s):  
Hans-Ulrich Hummel ◽  
Hermann Meske
Keyword(s):  
Crystal Structures ◽  
Complex Anion ◽  
Lone Pair ◽  
Equatorial Position ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Main Group Metal ◽  
Distorted Trigonal Bipyramid

The crystal structures of Pb[S(CN)C=C(CN)S] and (AsPh4)2{Pb[S(CN)C=C(CN)S]2} have been determined by X-ray diffraction. PbS2C4N2, crystallizes in the non-centrosymmetric space group P21 with a = 7.292(3), b = 7.420(3), c = 5.789(2) Å, β = 95.47(5)° and Ζ = 2. The lead atom is coordinated by three S atoms of dithioligands. The coordination sphere around Pb includes a stereochemically active lone-pair and is described as a distorted tetrahedron. (AsPh4)2[Pb(S2C4N2)2] crystallizes in the triclinic space group P1 with a = 17.205(3), b = 13.342(3), c = 12.059(2) Å, α = 106.15(7), β = 102.92(6), γ = 79.50(3)° and Z = 2. In the complex anion {Pb[S(CN)C=C(CN)S]2}2- the Pb-atom is located at a centre of a distorted trigonal bipyramid with a stereochemically active lone-pair in an equatorial position.

scholarly journals The crystal structures and mechanical properties of the uranyl carbonate minerals roubaultite, fontanite, sharpite, widenmannite, grimselite and čejkaite

2020 ◽  
Vol 7 (21) ◽  
pp. 4197-4221 ◽  
Author(s):  
Francisco Colmenero ◽  
Jakub Plášil ◽  
Jiří Sejkora
Keyword(s):  
Mechanical Properties ◽  
Hydrogen Bonding ◽  
Diffraction Pattern ◽  
Crystal Structures ◽  
First Principles ◽  
X Ray Diffraction ◽  
Carbonate Minerals ◽  
X Ray ◽  
Uranyl Carbonate

The structure, hydrogen bonding, X-ray diffraction pattern and mechanical properties of six important uranyl carbonate minerals, roubaultite, fontanite, sharpite, widenmannite, grimselite and čejkaite, are determined using first principles methods.

Distorted chiolite crystal structures of α-Na5M3F14 (M=Cr,Fe,Ga) studied by X-ray powder diffraction

2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Refinements ◽  
Space Group ◽  
X Ray ◽  
Precise Characterization

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.

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.

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