Hydrogen-bond directionality and symmetry in [C(O)NH](N)2P(O)-based structures: a comparison between X-ray crystallography data and neutron-normalized values, and evaluation of reliability

2021 ◽  
Vol 77 (3) ◽  
Author(s):  
Maryam Taherzadeh ◽  
Mehrdad Pourayoubi ◽  
Banafsheh Vahdani Alviri ◽  
Samad Shoghpour Bayraq ◽  
Maral Ariani ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Maximum Percentage ◽  
Bond Lengths ◽  
X Ray Crystallography ◽  
Percentage Difference ◽  
Structural Database

For [C(O)NH](N)2P(O)-based structures, the magnitude of the differences in the N—H...O, H...O=P and H...O=C angles has been evaluated when the N—H bond lengths, determined by X-ray diffraction, were compared to the neutron normalized values and the maximum percentage difference was obtained, i.e. about 3% for the angle even if the N—H bond lengths have a difference of about 30% (0.7 Å for the X-ray and 1.03 Å for the neutron-normalized value). The symmetries of the crystals are discussed with respect to the symmetry of the molecules, as well as to the symmetry of hydrogen-bonded motifs, and the role of the most directional hydrogen bond in raising the probability of obtaining centrosymmetric crystal structures is investigated. The work was performed by considering nine new X-ray crystal structures and 204 analogous structures retrieved from the Cambridge Structural Database.

scholarly journals M + M 3+ 2As(HAsO4)6 (M + M 3+ = TlGa, CsGa, CsAl): three new metal arsenates containing AsO6 octahedra

2018 ◽  
Vol 74 (8) ◽  
pp. 1163-1167 ◽  
Author(s):  
Karolina Schwendtner ◽  
Uwe Kolitsch
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
New Compounds ◽  
Metal Arsenates

The crystal structures of hydrothermally synthesized (T = 493 K, 7 d) thallium(I) digallium arsenic(V) hexakis[hydrogenarsenate(V)], TlGa2As(HAsO4)6, caesium digallium arsenic(V) hexakis[hydrogenarsenate(V)], CsGa2As(HAsO4)6, and caesium dialuminium arsenic(V) hexakis[hydrogenarsenate(V)], CsAl2As(HAsO4)6, were solved by single-crystal X-ray diffraction. The three compounds are isotypic and adopt the structure type of RbAl2As(HAsO4)6 (R\overline{3}c), which itself represents a modification of the RbFe(HPO4)2 structure type and consists of a tetrahedral–octahedral framework in which the slightly disordered M + cations are located in channels. The three new compounds contain AsO6 octahedra assuming the topological role of M 3+O6 octahedra. The As—O bond lengths are among the shortest As—O bond lengths known so far in AsO6 octahedra.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIX. Crystal Structure Determinations of Tetrakis(trimethylphosphine)copper(I) Halides and Tetrakis(triphenylphosphine)-copper(I) and -silver(I) Hexafluorophosphates

1990 ◽  
Vol 43 (10) ◽  
pp. 1697 ◽  
Author(s):  
GA Bowmaker ◽  
PC Healy ◽  
LM Engelhardt ◽  
JD Kildea ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Bond Lengths ◽  
Cu Complex ◽  
Structure Determinations

The crystal structures of [Cu(Pme3)4]X (X = Cl , Br, I) and of [M(PPh3)4] [PF6] (M = Cu, Ag) have been determined by single-crystal X-ray diffraction methods at 295 K. The former compounds contain nearly tetrahedral [Cu(PMe3)4]+ ions on sites of m symmetry with mean Cu-P bond lengths of 2.270, 2.271 and 2.278 Ǻ for X = Cl , Br and I respectively. The latter compounds contain [M(PPh3)4]+ ions on sites of 3 symmetry. In the M =Ag complex the coordination environment is close to tetrahedral, but in the M =Cu complex the length of the axial Cu-P bond [2.465(2)Ǻ] is significantly shorter than that of the off-axis bonds [2.566(2)Ǻ]. Possible reasons for this are discussed.

Article

1998 ◽  
Vol 76 (3) ◽  
pp. 301-306
Author(s):  
Sengen Sun ◽  
James F Britten ◽  
Christopher N Cow ◽  
Chérif F Matta ◽  
Paul HM Harrison
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
The Other ◽  
Methyl Groups ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Form Part ◽  
Two Sides ◽  
Opposite Helicity

The crystal structure of 3,4,7,8-tetramethylglycoluril (5) was determined by X-ray diffraction. The structure reveals a hydrogen-bonding motif in the crystal lattice that differs from that present in related glycolurils. The two sides of each molecule form part of two independent, but parallel, infinite helical chains. These chains are formed by the NH donor and C==O acceptor on one side of a glycoluril molecule, forming H-bonds to two different molecules at adjacent positions within the helix. On the other side of the same molecule, a similar motif generates another helix of opposite helicity to the first. The molecule has a crystallographic plane of symmetry through the two bridgehead carbon atoms and the two bridgehead methyl groups, which are syn-periplanar. Thus, 5 is similar to 3,4-dimethylglycoluril (3), but differs from some glycolurils, where there is a significant dihedral angle between the two bridgehead-to-bridgehead substituent bonds. Bond lengths and angles in 5 resemble those reported for 3, but bond lengths around the bridgehead positions are slightly lengthened relative to 3.Key words: glycoluril, 1,2,5,8-tetramethyl-2,6,7,8-tetraazabicyclo[3.3.0]octane-3,7-dione, X-ray diffraction, crystal structure, hydrogen-bond array.

Adamantane derivatives of sulfonamide molecular crystals: structure, sublimation thermodynamic characteristics, molecular packing, and hydrogen bond networks

CrystEngComm ◽  
2015 ◽  
Vol 17 (4) ◽  
pp. 753-763 ◽  
Author(s):  
German L. Perlovich ◽  
Alex M. Ryzhakov ◽  
Valery V. Tkachev ◽  
Alexey N. Proshin
Keyword(s):  
Hydrogen Bond ◽  
Crystal Structures ◽  
Molecular Crystals ◽  
Thermodynamic Characteristics ◽  
Molecular Packing ◽  
Adamantane Derivatives ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bond Networks ◽  
Derivatives Of

The crystal structures of six adamantane derivatives of sulfonamides have been determined by X-ray diffraction and their sublimation and fusion processes have been studied.

scholarly journals Disordered sodium alkoxides from powder data: crystal structures of sodium ethoxide, propoxide, butoxide and pentoxide, and some of their solvates

2021 ◽  
Vol 77 (1) ◽  
pp. 68-82
Author(s):  
Maurice Beske ◽  
Stephanie Cronje ◽  
Martin U. Schmidt ◽  
Lukas Tapmeyer
Keyword(s):  
Hydrogen Bond ◽  
Crystal Structures ◽  
Sodium Ethoxide ◽  
Amyl Alcohol ◽  
X Ray Diffraction ◽  
Oh Groups ◽  
Space Group ◽  
X Ray ◽  
Alkyl Groups ◽  
Hydrogen Bond Networks

The crystal structures of sodium ethoxide (sodium ethanolate, NaOEt), sodium n-propoxide (sodium n-propanolate, NaO n Pr), sodium n-butoxide (sodium n-butanolate, NaO n Bu) and sodium n-pentoxide (sodium n-amylate, NaO n Am) were determined from powder X-ray diffraction data. NaOEt crystallizes in space group P 421 m, with Z = 2, and the other alkoxides crystallize in P4/nmm, with Z = 2. To resolve space-group ambiguities, a Bärnighausen tree was set up, and Rietveld refinements were performed with different models. In all structures, the Na and O atoms form a quadratic net, with the alkyl groups pointing outwards on both sides (anti-PbO type). The alkyl groups are disordered. The disorder becomes even more pronounced with increasing chain length. Recrystallization from the corresponding alcohols yielded four sodium alkoxide solvates: sodium ethoxide ethanol disolvate (NaOEt·2EtOH), sodium n-propoxide n-propanol disolvate (NaO n Pr·2 n PrOH), sodium isopropoxide isopropanol pentasolvate (NaO i Pr·5 i PrOH) and sodium tert-amylate tert-amyl alcohol monosolvate (NaO t Am· t AmOH, t Am = 2-methyl-2-butyl). Their crystal structures were determined by single-crystal X-ray diffraction. All these solvates form chain structures consisting of Na+, –O− and –OH groups, encased by alkyl groups. The hydrogen-bond networks diverge widely among the solvate structures. The hydrogen-bond topology of the i PrOH network in NaO i Pr·5 i PrOH shows branched hydrogen bonds and differs considerably from the networks in pure crystalline i PrOH.

Notizen: Synthesis and Crystal Structure of the Hydrogen Bonded Complex of Tri-paratoluidylphosphazenyl Oxide with Ethyl Alcohol

1976 ◽  
Vol 31 (9) ◽  
pp. 1295-1296 ◽  
Author(s):  
T. Stanley Cameron ◽  
M. Gerard Magee ◽  
Samuel Mclean
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Oxygen Atom ◽  
Ethyl Alcohol ◽  
Title Compound ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Bond Lengths ◽  
X Ray Crystallography ◽  
Phosphoryl Oxygen

The title compound was synthesised and its structure determined by X-ray crystallography. The structure contains a hydrogen bond between the OH group of the alcohol and the phosphoryl oxygen atom. The P–N bond lengths are significantly different and the differences can be attributed to varying ρπ—dπ interactions along the bonds.

Molecular reorientation in a dehydration process of an organic polar salt of 2,4-diaminotoluene/L(+)-tartaric acid

2017 ◽  
Vol 32 (1) ◽  
pp. 15-22
Author(s):  
Weicai Ju ◽  
Simin Qiu ◽  
Yaqiu Tao ◽  
Xiaodong Shen ◽  
Zhigang Pan
Keyword(s):  
Crystal Structures ◽  
Tartaric Acid ◽  
Variable Temperature ◽  
Ethanol Dehydration ◽  
X Ray Diffraction ◽  
Molecular Reorientation ◽  
X Ray ◽  
Hydrate Crystal ◽  
Dehydration Behavior

An organic polar hydrate was obtained through cocrystallization of 2,4-diaminotoluene (2,4-DAT) and L(+)-tartaric acid (TA) from ethanol. Dehydration behavior of the obtained hydrate was investigated using variable temperature powder X-ray diffraction (PXRD) and thermal analysis. Proton transfer from L(+)-TA to 2,4-DAT in both hydrate and dehydrated form was revealed via Fourier transform infrared spectroscopy. The crystal structures of both forms were determined using PXRD techniques. The similarities and differences between two crystal structures were analyzed and the role of water in the hydrate crystal structure was demonstrated.

Reaction products of ammonium pertechnetate(VII) with triphenylphosphine and crystal structures of mer-Tc(PPh3)2Cl3(DMF) •2PPh3 and NH2(CH3)2+DMAH+ [TcCl6]2−•PPh3O

1991 ◽  
Vol 69 (3) ◽  
pp. 397-403 ◽  
Author(s):  
Fernande D. Rochon ◽  
Robert Melanson ◽  
Pi-Chang Kong
Keyword(s):  
Key Words ◽  
Crystal Structures ◽  
Bond Distance ◽  
Acetone Solution ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Group A

The reaction of NH4TcO4 with PPh3 in DMF solution in the presence of HCl produces mer-Tciii(PPh3)2Cl3(DMF)•2PPh3 (1). When the reaction is done in acidic DMA, the yellow product isolated was identified as NH2(CH3)2+DMAH+ [TcCl6]2−•PPh3O (2). The dimethylammonium cation was produced from the reaction of the solvent (DMA) with aqueous HCl. The reaction of NH4TcO4 with PPh3 in acidic acetone solution produces yellow (PPh3H)2[TcCl6] (≈15% yield) and some orange crystals (≈65% yield) identified by X-ray diffraction as [Ph3P-C(CH3)2-CH2-CO-CH3]+ [Tc(PPh3)Cl5]−. The cation was produced from the reaction of acetone used as solvent with HCl and PPh3. The crystals of 1 are monoclinic with P21/m space group, a = 11.393(4), b = 24.993(11), c = 12.398(4) Å, β = 106.98(3)°, Z = 2. The structure was refined to R = 0.072 and wR = 0.058. The Tc—O bond distance is 2.115(12) Å while the Tc—P bond lengths are 2.496(5) and 2.499(5) Å and the Tc—Cl are 2.399(5) and 2.342(3) Å. The C atoms of the DMF ligand are disordered. The crystals of 2 are triclinic, [Formula: see text] space group with a = 8.627(5), b = 13.308(7), c = 14.401(9) Å, α = 97.62(5), β = 91.31(5), γ = 106.42(5)°, and Z = 2. The structure was refined to R = 0.060 and wR = 0.076. The proton on DMAH+ is hydrogen bonded to the oxygen of PPh3O with a distance [Formula: see text] Key words: technetium, DMF, triphenylphosphine, dimethylacetamide.

scholarly journals Chloroantimonate(III), IV. Darstellung und Kristallstruktur von 2,2′-Bipyridinium-pentachloroantimonat (C10H8N2H2)SbCl5 und der metastabilen Modifikation von 4,4′ -Bipyridinium-pentachloroantimonat (C10H8N2H2)SbCl5 / Chloroantimonates(III), IV. Preparation and Crystal Structures of 2,2′-Bipyridinium Pentachloroantimonate (C10H8N2H2)SbCl5 and of the Metastable Modification of 4,4′-Bipyridinium Pentachloroantimonate (C10H8N2H2)SbCl5

1983 ◽  
Vol 38 (12) ◽  
pp. 1615-1621 ◽  
Author(s):  
Annegret Lipka
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Crystal Structures ◽  
Bond Order ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Intermolecular Contacts

2,2′-Bipyridinium pentachloroantimonate (III) and the metastable modification of 4,4′-bipyridinium pentachloroantimonate(III) were synthezised and investigated by single crystal X-ray diffraction analysis. The structures consist of 2,2′-bipyridinium and 4,4′-bipyridinium cations, respectively, and of pentachloroantimonate anions. With regard to bonding and short intermolecular contacts the coordination of the Sb atoms is distorted octahedral in both structures. Bond lengths of equivalent Sb-Cl bonds differ strongly within the structure of the 2,2′-bipyridinium salt (239.9 pm to 312.1 pm) and are not distinguishable from short intermolecular contacts (305.4 pm and 321.8 pm). In the structure of the 4,4′-bipyridinium salt, bond distances vary only from 240.9 pm to 267.8 pm and are clearly below intermolecular contacts at 318.2 pm. In spite of the different distances the total bond order for each Sb atom is 3. In the structure of the 2,2′-bipyridinium salt the anions build tetramers, whereas in the structure of the 4,4′-bipyridinium salt the anions form chains

scholarly journals The synthesis of a pyridine-N-oxide isophthalamide rotaxane utilizing supplementary amide hydrogen bond interactions

2016 ◽  
Vol 14 (33) ◽  
pp. 7972-7981 ◽  
Author(s):  
Nicholas H. Evans ◽  
Charles E. Gell ◽  
Michael J. G. Peach
Keyword(s):  
Hydrogen Bond ◽  
Nmr Spectroscopy ◽  
Computational Modelling ◽  
Amide Hydrogen ◽  
X Ray ◽  
X Ray Crystallography ◽  
Hydrogen Bond Interactions

A pyridine-N-oxide containing rotaxane has been prepared in 32% yield. The role of macrocycle structure in successful pseudo-rotaxane formation has been rationalised by a combination of NMR spectroscopy, X-ray crystallography and computational modelling.

Sign in / Sign up

Export Citation Format

Share Document