scholarly journals Reactions of Pentaphenylantimony and Penta-Para-Tolylanimony with Calixarene [4-t-BuC6H2OH(S-2)]4

2021 ◽  
Vol 13 (1) ◽  
pp. 47-57
Author(s):  
A.N. Efremov ◽  
◽  
V.V. Sharutin
Keyword(s):  
Hydrogen Bonds ◽  
Antimony Atom ◽  
Tetrahedral Coordination ◽  
X Ray Diffraction ◽  
Deprotonated Form ◽  
X Ray ◽  
Bond Lengths ◽  
Tert Butyl ◽  
Average Value ◽  
Intramolecular Hydrogen

Pentaphenylantimony and penta-para-tolylantimony react with calixarene [4-t-BuC6H2OH(S-2)]4 (СArH) by way of arene elimination and formation of the [Ph4Sb]+[СAr]- × TolH (1), [p-Tol4Sb]+[CAr]- × H2O (2) ionic products with a yield up to 96%. The compound has been identified by IR spectroscopy and X-ray diffraction analysis. According to the X-ray diffraction data, compounds 1 and 2 are ionic complexes with solvate molecules of toluene (1) and water (2). The cation has a tetrahedral coordination of the antimony atom with aryl ligands at the polyhedron vertices; the anion is represented by the deprotonated form of p-tert-butylthiacalix[4]arene. The three tert-butyl groups, the phenyl ring and solvated toluene in the structure of compound 1, and two tert-butyl fragments in the structure of compound 2 are disordered over two positions. The tetrahedral coordination of antimony atoms in the cations of compounds 1 and 2 is slightly distorted. The CSbC angles deviate from the theoretical value and vary within 106.0(4)−117.7(4)° (1), 105.75(15)−112.84(15)° (2). The average Sb–C bond lengths are 2.101(3) and 2.106(4) Å in structures 1 and 2, respectively. The [СAr]- anion is in the cone conformation, the upper rim of which is represented by the tert-butyl groups in the para-position, while the lower one is represented by hydroxy groups, one of which is deprotonated. The СAr–O– bond length (1.318(4) (1) and 1.326(4) (2) Å) is less than the average value of the СAr–OH bond lengths (1.338(4) (1) and 1.343(4) (2) Å), which indicates increasing multiplicity of the bond and localization of a negative charge on the oxygen atom. Intramolecular hydrogen bonds with the neiboring O atom are observed. The H∙∙∙O distances are 2.16, 1.69, 1.77 Å in 1 and 1.92, 1.79, 1.76 Å in 2. Dihedral angles between opposite phenoxide rings are 60.64° and 87.07° (1) and 83.85° and 80.42° (2), which indicates somewhat less symmetric anion in structure 1 than in structure 2. The formation of the crystal spatial structure is due to the formation of hydrogen bonds between ions with participation of oxygen and sulfur atoms, as well as СН∙∙∙π–interactions, while the ions form chains in the crystal of compound 1, and layers in the crystal of compound 2. Complete tables of atom coordinates, bond lengths and valence angles are deposited at the Cambridge Crystallographic Data Center (No. 1850118 (1); No. 2013220 (2); [email protected] or http://www.ccdc.cam.ac.uk/data_request/cif).

scholarly journals A novel сalcium trifluoroacetate structure

2021 ◽  
Vol 16 (4) ◽  
pp. 352-362
Author(s):  
A. A. Vasilyeva ◽  
T. Yu. Glazunova ◽  
D. S. Tereshchenko ◽  
E. Kh. Lermontova
Keyword(s):  
Thermal Decomposition ◽  
Hydrogen Bonds ◽  
Trifluoroacetic Acid ◽  
Calcium Fluoride ◽  
X Ray Diffraction ◽  
Absorption Bands ◽  
Intramolecular Hydrogen Bonds ◽  
X Ray ◽  
Cell Parameters ◽  
Intramolecular Hydrogen

Objectives. The study was devoted to considering the features of the synthesis and crystal structure of calcium trifluoroacetate Ca2(CF3COO)4·8CF3COOH and investigating the products of its thermal behavior.Methods. The compositions of the proposed structural form were characterized by various physicochemical methods (X-ray diffraction, IR spectroscopy), and the products of thermal decomposition were determined under dynamic vacuum conditions.Results. The reaction between calcium carbonate and 99% trifluoroacetic acid yielded a new structural type of calcium trifluoroacetate Ca2(CF3COO)4·8CF3COOH (I) in the form of colorless prismatic crystals unstable air. X-ray diffraction results confirmed the composition I: space group P21, with unit cell parameters: a = 10.0193(5) Å, b = 15.2612(7) Å, c = 16.3342(8) Å, β = 106.106(2)°, V = 2399.6(2) Å3, Z = 2. The structure is molecular, constructed from Ca2(CF3COO)4·8CF3COOH dimers. The end molecules of the trifluoroacetic acid were involved in the formation of intramolecular hydrogen bonds with oxygen atoms of the bidentate bridging anions CF3COO−. There were strongly pronouncedsymmetric and asymmetric absorption bands of COO and CF3-groups in the IR spectrum of the resulting compound in the range of 1200–1800 cm−1. The definite peak of the oscillation of the OH-group at 3683 cm−1 corresponds to the trifluoroacetic acid molecules present in the structure. The broadpeak of the valence oscillations in the range of 3300–3500 cm−1 is caused by the presence of intramolecular hydrogen bonds. Decomposition began at 250°C and 10−2 mm Hg with calcium fluoride CaF2 as the final decomposition product.Conclusions. We obtained a previously undescribed calcium–trifluoroacetic acid complex whose composition can be represented by Ca2(CF3COO)4·8CF3COOH. The crystal island structure is a dimeric molecule where the calcium atoms are bound into dimers by four trifluoroacetate groups. The complex was deposited in the Cambridge Structural Data Bank with a deposit number CCDC 2081186. Although the compound has a molecular structure, thermal decomposition leads to the formation of calcium fluoride characterized by a small particle size, which may further determine its applications.

Crystal structure of low-cristobalite-type Al0.5Ga0.5PO4: A combined Rietveld refinement of neutron and X-ray diffraction data

2005 ◽  
Vol 20 (3) ◽  
pp. 207-211 ◽  
Author(s):  
S. N. Achary ◽  
A. K. Tyagi ◽  
S. K. Kulshreshtha ◽  
O. D. Jayakumar ◽  
P. S. R. Krishna ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Crystal Structure Analysis ◽  
Tetrahedral Coordination ◽  
X Ray Diffraction ◽  
Rietveld Refinements ◽  
X Ray ◽  
Cell Parameters ◽  
Bond Lengths

The low-cristobalite-type modification of Al0.5Ga0.5PO4 is prepared by annealing the amorphous precipitate of stoichiometric phosphate at 1300 °C. The phase purity of the sample is ascertained by powder X-ray diffraction. The crystal structure is refined by Rietveld refinements of the neutron and X-ray diffraction data of the polycrystalline powder. This compound crystallizes in an orthorhombic lattice with unit cell parameters, a=7.0295(8), b=7.0132(8), and c=6.9187(4) Å, V=341.08(6) Å3, Z=4 (Space group C 2221, No. 20). The crystal structure analysis reveals the random distribution of the Al3+ and Ga3+ having tetrahedral coordination with typical M–O (M=Al3+:Ga3+) bond lengths as 1.74 Å. Similarly, the P5+ have tetrahedral coordination with typical P–O bond lengths 1.52–1.54 Å. The Mo4 and PO4 tetraheda are linked by common corners forming a three-dimensional framework lattice. The details of the crystal structure are presented in this paper.

Structure and hydrogen bonding in 2,4-dihydroxybenzoic acid at 90, 100, 110 and 150 K; a theoretical and single-crystal X-ray diffraction study

2007 ◽  
Vol 63 (2) ◽  
pp. 303-308 ◽  
Author(s):  
Andrew Parkin ◽  
Martin Adam ◽  
Richard I. Cooper ◽  
Derek S. Middlemiss ◽  
Chick C. Wilson
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Hydrogen Bonds ◽  
X Ray Diffraction ◽  
Dihydroxybenzoic Acid ◽  
X Ray ◽  
Hydrogen Bond System ◽  
Proton Disorder ◽  
Intramolecular Hydrogen ◽  
Carboxylic Acid Dimer

A new polymorph of 2,4-dihydroxybenzoic acid is reported. The structure was characterized by multiple-temperature X-ray diffraction and solid-state DFT computations. The material shows a geometric pattern of hydrogen bonding consistent with cooperativity between the intermolecular carboxylic acid dimer and intramolecular hydrogen bonds. The presence of proton disorder within this hydrogen-bond system, which would support such a cooperative model, was not fully ruled out by the initial X-ray studies. However, solid-state calculations on the three possible end-point tautomers indicate that the dominant crystallographically observed configuration is substantially lower in energy than the other tautomers (by at least 9 kJ mol−1), indicating that no disorder should be expected. It is therefore concluded that no disorder is observed either in the intra- or intermolecular hydrogen bonds of the title compound and that the cooperativity between the hydrogen bonds is not present within the temperature range studied.

The crystal structure of C.I. Pigment Red 2, 1′-(2,5-dichlorophenyl)azo-2′hydroxy-3′-phenylamidonaphthalene

1977 ◽  
Vol 146 (4-6) ◽  
Author(s):  
A. Whitaker
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Parameters ◽  
Intramolecular Hydrogen

AbstractThe crystal and molecular structure of C.I. Pigment Red 2, l′-(2,5-dichlorophenyl)azo-2′-hydroxy-3′-phenylamidonaphthalene has been determined by x-ray diffraction techniques. It crystallizes in the monoclinic system with cell parametersThe hydrogen atoms have been found and included but not refined. The final residual is 15.3%. The molecule is probably in the form of the hydrazone tautomer. The intramolecular hydrogen bonds keep most of the molecule approximately planar while it appears that the remainder is held in the same plane due to steric hinderence between the molecules. The molecules are packed in columns with alternate molecules antiparallel and are linked by van der Waals forces.

scholarly journals (3-Ammonio-2,2-dimethyl-propyl)carbamate Dihydrate

Molbank ◽  
10.3390/m1015 ◽  
2018 ◽  
Vol 2018 (3) ◽  
pp. M1015
Author(s):  
Jaqueline Heimgert ◽  
Dennis Neumann ◽  
Guido Reiss
Keyword(s):  
Hydrogen Bond ◽  
Raman Spectroscopy ◽  
Acetic Acid ◽  
Hydrogen Bonds ◽  
Chain Structure ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Title Molecule ◽  
Intramolecular Hydrogen

(3-Ammonio-2,2-dimethylpropyl)carbamate dihydrate was synthesised. The title compound was characterised by single crystal X-ray diffraction and IR-/Raman-spectroscopy. It has been demonstrated that a mixture of dilute acetic acid and 2,2-dimethyl-1,3-diaminopropane is able to capture CO2 spontaneously from the atmosphere. An intramolecular hydrogen bond stabilises the conformation of the ylide-type title molecule. Intermolecular hydrogen bonds between all moieties connect them to a strand-type chain structure.

Formamidinium Salts of Low Valent Metal Halide Anions MX3 – (M = Ge, Sn) and M2X62– (M = Ga, In)

2004 ◽  
Vol 59 (11-12) ◽  
pp. 1524-1531 ◽  
Author(s):  
Xin Tian ◽  
Tania Pape ◽  
Norbert W. Mitzel
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Crystal Structures ◽  
Raman Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Metal ◽  
Weak Hydrogen Bonds ◽  
Low Valent

Tetramethylformamidinium trichlorogermanite, [CH(NMe2)2][GeCl3], tetramethylformamidinium trichlorostannite, [CH(NMe2)2][SnCl3], bis-(tetramethylformamidinium hexaiododigallate, [CH(NMe2)2]2[Ga2I6] and bis-(tetramethylformamidinium hexachlorodiindate, [CH(NMe2)2]2[In2Cl6] have been prepared by the reactions between tetramethylformamidinium chloride, [CH(NMe2)2]Cl, and the corresponding low valent halides GeCl2 (as dioxane adduct), SnCl2, “GaI” and InCl. Their crystal structures have been determined by single crystal X-ray diffraction. [CH(NMe2)2][GeCl3] aggregates in a centrosymmetric dimeric structure, in which two trigonal pyramidal GeCl3 units are connected together by two weak Ge···Cl bonds and each Ge atom is bonded to one cation by a weak Ge···N contact. Two sets of weak hydrogen bonds C-H···Cl are observed with bond lengths of 2.87(2) Å and 2.85(2) Å . In [CH(NMe2)2][SnCl3], the SnCl3 − units adopts a (3+3) coordination with three normal Sn-Cl bonds and three weak Sn···Cl contacts. [CH(NMe2)2]2[Ga2I6] and [CH(NMe2)2]2[In2Cl6] contain metal-metal bonded anions with distorted staggered ethane-like conformations. The metal-metal bond lengths are 2.423(1) Å (Ga-Ga) and 2.719(1) Å (In-In). Their Raman spectra contain intense bands at 118.7 cm−1(Ga-Ga) and 174.7 cm−1(In-In) associated with metal-metal stretching modes.

Structural studies of organoboron compounds. LV. N,N′-Di-tert-butyl-N,N′- dihydroxypropane-1,3-diamine(O-B)ethoxydiphenylborane and N1,N2-di-tert-butyl-N1,N2-dihydroxy-1-phenylpropane-1,3-diamine(N2-O-B)hydroxydiphenylborane

1992 ◽  
Vol 70 (7) ◽  
pp. 2033-2039 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Gottfried Lubkowitz ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Hydrogen Bonds ◽  
Least Squares ◽  
Direct Methods ◽  
Structural Studies ◽  
Open Chain ◽  
Organoboron Compounds ◽  
Full Matrix ◽  
Bond Lengths ◽  
Tert Butyl ◽  
Intramolecular Hydrogen

The 1,3-propanediamine derivatives N,N′-di-tert-butyl-N,N′-dihydroxy-1,3-propanediamine and N,N′-di-tert-butyl-N,N′-dihydroxy-1-phenyl-1,3-propanediamine have been prepared and reacted with oxybis(diphenylborane) to yield, respectively, the crystalline organoboron compounds N,N′-di-tert-butyl-N,N′-dihydroxypropane-1,3-diamine(O-B)-ethoxydiphenylborane, 5a, and N1,N2-di-tert-butyl-N1,N2-dihydroxy-1-phenylpropane-1,3-diamine(N2-O-B)-hydroxydiphenylborane, 5b. Crystals of 5a are monoclinic, C2/c, a = 35.402(1), b = 9.212(2), c = 18.101(2) Å, β = 116.688(3)°, Z = 8, ρc = 1.079 g cm−3, and crystals of 5b are monoclinic, P21/c, a = 12.899(4), b = 12.571(4), c = 17.412(3) Å, β = 90.02(2)°, Z = 4, ρc = 1.121 g cm−3. The structures were solved by direct methods and were refined by full-matrix least-squares procedures to final R values of 0.047 and 0.041 for 2492 and 3334 reflections with I ≥ 3σ(I), respectively. Compounds 5a and 5b are open-chain hydroxylamine adducts of diphenylborinic acid and ethyl diphenylborinate, respectively. Both of these compounds are stabilized by a system of three intramolecular hydrogen bonds [Formula: see text]. Bond lengths involving the tetrahedrally coordinated boron atoms are: (C)O—B = 1.457(3), (N)O—B = 1.558(3), and C—B = 1.613(4) and 1.615(4) Å for 5a; (H)O—B = 1.475(3), (N)O—B = 1.562(2), and C—B = 1.618(3) and 1.619(3) Å for 5b.

Hydrogen Bonding in Acid Li-, Ni-, Tetrabutylammonium, and Ammonium Salts of Benzene-1,2,4,5-tetracarboxylic Acid (Pyromellitic Acid)

1992 ◽  
Vol 47 (8) ◽  
pp. 1141-1153 ◽  
Author(s):  
Sven M. Jessen ◽  
Horst Küppers ◽  
Dean C. Luehrs
Keyword(s):  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Ammonium Salts ◽  
Tetracarboxylic Acid ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
Pyromellitic Acid ◽  
X Ray ◽  
Carboxylic Groups ◽  
Intramolecular Hydrogen

Four acid salts of pyromellitic acid (benzene-1,2,4,5-tetracarboxylic acid) have been synthesized and studied by X-ray diffraction and IR spectroscopy. (1) Dilithium dihydrogen pyromellitate pentahydrate, Li2[C6H2(COO)4H2]· 5H2O; monoclinic, P21/m, a = 6.214(2), b = 19.647(7), c = 6.592(2)Å, β = 115.90(2)°, Ζ = 2, R = 0.068, Rw = 0.067. (2) Hexaaquanickel dihydrogen pyromellitate, [Ni(H2O)6][C6H2(COO)4H2]; monoclinic, P2/m, a = 6.528(1), b = 9.927(2), c = 6.472(1)Å, β = 115.57(1)°, Z = 1, R = 0.044, Rw = 0.039. (3) Tetrabutylammonium trihydrogen pyromellitate, [(C4H9)4N][C6H2(COO)4H3]; monoclinic, P21/c, a = 9.719(4), b = 18.823(8), c = 15.795(5)Å, β = 107.42(3)°, Z = 4, R = 0.059, Rw = 0.039. (4) Diammonium dihydrogen pyromellitate, [NH4]2[C6H2(COO)4H2]; monoclinic, P21/c, a = 4.7665(6), b = 11.681(3), c = 10.149(2)Å, ß = 102.19(2)°, Z = 2, R = 0.045, Rw = 0.039. Compounds 1, 2, and 3 show very short intramolecular hydrogen bonds between adjacent carboxylic groups (O ••• O distances 2.384(6), 2.386(5), 2.387(3)Å, respectively). Compound 4 forms intermolecular hydrogen bonds (O ··· O distance 2.642(2) A). The different hydrogen bonding modes are also evident in the IR spectra.

scholarly journals A trigonal coordination of Au(I) phosphane complexes stabilized by O–H⋯X (X = Cl–, Br–, I–) interactions

2021 ◽  
Author(s):  
Petra Gründlinger ◽  
Cezarina Cela Mardare ◽  
Thorsten Wagner ◽  
Uwe Monkowius
Keyword(s):  
Hydrogen Bonding ◽  
Carboxylic Acid ◽  
Hydrogen Bonds ◽  
Intramolecular Hydrogen Bonding ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Standard Linear ◽  
Intramolecular Hydrogen ◽  
Linear Coordination

AbstractIn this work, we show that intramolecular hydrogen bonding can be used to stabilize tri-coordinated phosphane-gold(I) complexes. Two molecular structures of 2-(diphenylphosphino)benzoic acid (L) coordinated to a gold(I) atom were determined by single-crystal X-ray diffraction. The linear L–Au–Br shows a standard linear coordination and dimerizes via hydrogen bonds of the carboxylic acid. Upon addition of two additional phosphane ligands the complex [L3Au]X is formed which is stabilized by three intramolecular –C(O)O–H…X hydrogen bonds as proven by the X-ray structure of the respective chlorido-complex. X-ray powder diffractograms suggest the same structure also for X– = Br– and I–. Graphic abstract

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