scholarly journals Crystal structures of 6-cyclopropyl-1,3-diphenylfulvene and 6-(2,3-dimethoxynaphthyl)-1,3-diphenylfulvene

2020 ◽  
Vol 76 (6) ◽  
pp. 896-899
Author(s):  
Loren C. Brown ◽  
Scott T. Iacono ◽  
Gary J. Balaich
Keyword(s):  
Crystal Structures ◽  
Asymmetric Unit ◽  
Ethanolic Solution ◽  
Bond Lengths

The title compounds, 6-cyclopropyl-1,3-diphenylfulvene, C21H18, [systematic name: 5-(cyclopropylmethylidene)-1,3-diphenylcyclopenta-1,3-diene], 1, and 6-(2,3-dimethoxynaphthyl)-1,3-diphenylfulvene, C30H24O2, {systematic name: 5-[(3,4-dimethoxynaphthalen-2-yl)methylidene]-1,3-diphenylcyclopenta-1,3-diene}, 2, were prepared from 1,3-diphenylcyclopentadiene, pyrrolidine, and the corresponding aldehydes in an ethanolic solution. Each structure crystallizes with one molecule per asymmetric unit and exhibits the alternating short and long bond lengths typical of fulvenes. A network of C—H...C ring interactions as well as C—H...O interactions is observed, resulting in the compact packing found in each structure.

Four (2,2′-bipyridyl)(ferrocenyl)boronium derivatives

2015 ◽  
Vol 71 (1) ◽  
pp. 26-31 ◽  
Author(s):  
Jan W. Bats ◽  
Kuangbiao Ma ◽  
Hans-Wolfram Lerner
Keyword(s):  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Tetrahedral Coordination ◽  
Asymmetric Unit ◽  
Bond Lengths ◽  
Distorted Tetrahedral Coordination

Crystal structures are reported for four (2,2′-bipyridyl)(ferrocenyl)boronium derivatives, namely (2,2′-bipyridyl)(ethenyl)(ferrocenyl)boronium hexafluoridophosphate, [Fe(C5H5)(C17H15BN2)]PF6, (Ib), (2,2′-bipyridyl)(tert-butylamino)(ferrocenyl)boronium bromide, [Fe(C5H5)(C19H22BN3)]Br, (IIa), (2,2′-bipyridyl)(ferrocenyl)(4-methoxyphenylamino)boronium hexafluoridophosphate acetonitrile hemisolvate, [Fe(C5H5)(C22H20BN3O)]PF6·0.5CH3CN, (IIIb), and 1,1′-bis[(2,2′-bipyridyl)(cyanomethyl)boronium]ferrocene bis(hexafluoridophosphate), [Fe(C17H14BN3)2](PF6)2, (IVb). The asymmetric unit of (IIIb) contains two independent cations with very similar conformations. The B atom has a distorted tetrahedral coordination in all four structures. The cyclopentadienyl rings of (Ib), (IIa) and (IIIb) are approximately eclipsed, while a bisecting conformation is found for (IVb). The N—H groups of (IIa) and (IIIb) are shielded by the ferrocenyl andtert-butyl or phenyl groups and are therefore not involved in hydrogen bonding. The B—N(amine) bond lengths are shortened by delocalization of π-electrons. In the cations with an amine substituent at boron, the B—N(bipyridyl) bonds are 0.035 (3) Å longer than in the cations with a methylene C atom bonded to boron. A similar lengthening of the B—N(bipyridyl) bonds is found in a survey of related cations with an oxy group attached to the B atom.

Biphenyl- and phenylnaphthalenyl-substituted 1H-imidazole-4,5-dicarbonitrile catalysts for the coupling reaction of nucleoside methyl phosphonamidites

2013 ◽  
Vol 69 (5) ◽  
pp. 529-533 ◽  
Author(s):  
Jan W. Bats ◽  
Peter Schell ◽  
Joachim W. Engels
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Phenyl Group ◽  
Coupling Reaction ◽  
Steric Repulsion ◽  
Asymmetric Unit ◽  
Bond Lengths ◽  
Imidazole Group ◽  
Independent Molecules ◽  
Substituted 1

Crystal structures are reported for three substituted 1H-imidazole-4,5-dicarbonitrile compounds used as catalysts for the coupling reaction of nucleoside methyl phosphonamidites, namely 2-(3′,5′-dimethylbiphenyl-2-yl)-1H-imidazole-4,5-dicarbonitrile, C19H14N4, (I), 2-(2′,4′,6′-trimethylbiphenyl-2-yl)-1H-imidazole-4,5-dicarbonitrile, C20H16N4, (II), and 2-[8-(3,5-dimethylphenyl)naphthalen-1-yl]-1H-imidazole-4,5-dicarbonitrile, C23H16N4, (III). The asymmetric unit of (I) contains two independent molecules with similar conformations. There is steric repulsion between the imidazole group and the terminal phenyl group in all three compounds, resulting in the nonplanarity of the molecules. The naphthalene group of (III) shows significant deviation from planarity. The C—N bond lengths in the imidazole rings range from 1.325 (2) to 1.377 (2) Å. The molecules are connected into zigzag chains by intermolecular N—H...Nimidazole[for (I)] or N—H...·Ncyano[for (II) and (III)] hydrogen bonds.

The first crystal structures of six- and seven-membered tellurium- and nitrogen-containing (Te—N) heterocycles: 2H-1,4-benzotellurazin-3(4H)-one and 2,3-dihydro-1,5-benzotellurazepin-4(5H)-one

2016 ◽  
Vol 72 (1) ◽  
pp. 1-5 ◽  
Author(s):  
Joshua P. Myers ◽  
Frank R. Fronczek ◽  
Thomas Junk
Keyword(s):  
Hydrogen Bonding ◽  
Crystal Structures ◽  
Boat Conformation ◽  
Asymmetric Unit ◽  
Bond Lengths ◽  
Independent Molecules ◽  
Twist Boat ◽  
Good Agreement

There is a paucity of data concerning the structures of six- and seven-membered tellurium- and nitrogen-containing (Te—N) heterocycles. The title compounds, C8H7NOTe, (I), and C9H9NOTe, (II), represent the first structurally characterized members of their respective classes. Both crystallize with two independent molecules in the asymmetric unit. When compared to their sulfur analogs, they exhibit slightly greater deviations from planarity to accommodate the larger chalcogenide atom, with (II) adopting a pronounced twist-boat conformation. The C—Te—C angles of 85.49 (15) and 85.89 (15)° for the two independent molecules of (I) were found to be somewhat smaller than those of 97.4 (2) and 97.77 (19)° for the two independent molecules of (II). The C—Te bond lengths [2.109 (4)–2.158 (5) Å] are in good agreement with those predicted by the covalent radii. Intermolecular N—H...O hydrogen bonding in (I) forms centrosymmetricR22(8) dimers, while that in (II) forms chains. In addition, intermolecular Te...O contacts [3.159 (3)–3.200 (3) Å] exist in (I).

Structural characteristics of dibromoborylated benzene derivatives

2012 ◽  
Vol 68 (6) ◽  
pp. o226-o230 ◽  
Author(s):  
Sebastian Popp ◽  
Kai Ruth ◽  
Hans-Wolfram Lerner ◽  
Michael Bolte
Keyword(s):  
Crystal Structures ◽  
Aromatic Ring ◽  
Structural Characteristics ◽  
Geometric Parameters ◽  
Mirror Plane ◽  
Methyl Groups ◽  
Benzene Derivatives ◽  
Asymmetric Unit ◽  
Bond Lengths ◽  
Structural Database

The crystal structures of five dibromobenzene derivatives, namely dibromoborylbenzene, C6H5BBr2, (I), 1-dibromoboryl-4-(trimethylsilyl)benzene, C9H13BBr2Si, (II), 4-bromo-1-(dibromoboryl)benzene, C6H4BBr3, (III), dibromo(dimethylamino)(phenyl)borane, C8H12BBr2N, (IV), and dibromo(dimethylsulfanyl)[4-(trimethylsilyl)phenyl]borane, C11H19BBr2SSi, (V), have been determined. Compounds (I)–(IV) crystallize with one molecule in the asymmetric unit, but the molecule of (V) is located on a crystallographic mirror plane, implying twofold disorder of the central aromatic ring, the S atom and one of the methyl groups bonded to the S atom. In (I), (II) and (III), the B atom is three-coordinated, and in (IV) and (V) it is four-coordinated. The geometric parameters of the –BBr2group in these five structures agree well with those of comparable structures retrieved from the Cambridge Structural Database. The C—B and B—Br bond lengths in the molecules with a three-coordinated B atom are significantly shorter than those in the molecules with a four-coordinated B atom. In the compounds with a three-coordinated B atom, the –BBr2group tends to be coplanar with the aromatic ring to which it is attached.

Kupfer(I)-chlorid-Addukte von Phosphoraniminen Die Kristallstrukturen von Ph 3 PNPh * CuCl und von 2,3-Bis(triphenylphosphoranylidenamino)maIeinsäure-N-methylimid- Kupfer(I)-chlorid / Copper(I) Chloride Adducts of Phosphoranimines The Crystal Structures of Ph3 PNPh·CuCl and of 2,3-Bis(triphenylphosphoranylideneamino)maleic Acid N-Methylimide Copper(I) Chloride

1988 ◽  
Vol 43 (1) ◽  
pp. 5-11 ◽  
Author(s):  
Andrea Maurer ◽  
Dieter Fenske ◽  
Johannes Beck ◽  
Joachim Strähle ◽  
Eberhard Böhm ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Crystal Structures ◽  
Maleic Acid ◽  
Bond Angle ◽  
Asymmetric Unit ◽  
Space Group ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Independent Molecules

Abstract The title compounds Ph3PNPh · CuCl (1) and (Ph3P)2 N2 C4O2 (NMe) CuCl (2) have been prepared by the reactions of CuCl with the corresponding phosphoranimines Ph3PNPh and 2.3-bis(triphenylphosphoranylideneamino)maleic acid N-methylimide, respectively. Both com-plexes were characterized by their IR spectra as well as by crystal structure determinations. Ph3PNPh · CuCl (1): space group P1, Z = 4, 3639 independent observed reflexions, R = 0.038. Lattice dimensions (18 °C): a = 1047.6; b = 1251.5; c = 1755 pm; α = 103.43°; β = 97.24°; γ = 101.30°. The compound forms monomeric molecules; the asymmetric unit contains two crystallo-graphically independent molecules. The CuCl molecule is bonded via the N atom of the phos-phoranimine. Bond lengths: Cu-N = 189 pm; Cu-CI = 209 pm; bond angle N - Cu - CI = 177°. (Ph3P)2N2C4O2(NMe) · CuCl (2): space group Pbca, Z = 8, 5611 independent, observed reflexions, R = 0.069. Lattice dimensions (25 °C): a = 1224.3; b = 1962.5: c = 2994.0 pm. The compound forms monomeric molecules with the CuCl molecule bonded via one of the N atoms of the phosphoranimine groups. Bond lengths: Cu - N = 194 pm; Cu-CI = 212 pm; bond angle N-Cu -CI -175°.

scholarly journals Crystal structures of three (trichloromethyl)(carbamoyl)disulfanes

2015 ◽  
Vol 71 (10) ◽  
pp. 1169-1173 ◽  
Author(s):  
Barbara L. Goldenberg ◽  
Victor G. Young Jr ◽  
George Barany
Keyword(s):  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Crystal Packing ◽  
Molecular Structures ◽  
Protecting Groups ◽  
Asymmetric Unit ◽  
Bond Lengths ◽  
Independent Molecules ◽  
Related Compounds

The present paper reports crystallographic studies on three related compounds that were of interest as precursors for synthetic and mechanistic work in organosulfur chemistry, as well as to model nitrogen-protecting groups: (N-methylcarbamoyl)(trichloromethyl)disulfane, C3H4Cl3NOS2, (1), (N-benzylcarbamoyl)(trichloromethyl)disulfane, C9H8Cl3NOS2, (2), and (N-methyl-N-phenylcarbamoyl)(trichloromethyl)disulfane, C9H8Cl3NOS2, (3). Their molecular structures, with similar bond lengths and angles for the CCl3SS(C=O)N moieties, are confirmed. Compounds (1) and (3) both crystallized with two independent molecules in the asymmetric unit. Classical hydrogen bonding, as well as chlorine-dense regions, are evident in the crystal packing for (1) and (2). In the crystal of (1), molecules are linkedviaN—H...O hydrogen bonds forming chains along [110], which are linked by short Cl...Cl and S...O contacts forming sheets parallel to (001). In the crystal of (2), molecules are linkedviaN—H...O hydrogen bonds forming chains along [001], which in turn are linked by pairs of short O...Cl contacts forming ribbons along thec-axis direction. In the crystal of (3), there are no classical hydrogen bonds present and the chlorine-dense regions observed in (1) and (2) are lacking.

35CI NQR and Structural Studies of N-(2,6-Dichlorophenyl)-Amides, 2,6-Cl2C6H3-NHCO-R (R = H or CH3-y Xy and X = CH3 or CI; y = 0,1, 2 or 3)

2000 ◽  
Vol 55 (9-10) ◽  
pp. 791-800 ◽  
Author(s):  
B. Thimme Gowda ◽  
Helmut Paulus ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Crystal Symmetry ◽  
Side Chain ◽  
Structural Studies ◽  
Asymmetric Unit ◽  
Space Group ◽  
Lattice Constants ◽  
Bond Lengths ◽  
Crystal Type

The effect of side chain substitution on the 35CI NQR and crystal structure of amides of the type N-(2,6-dichlorophenyl)-amides, 2,6-Cl2C6H3-NHCO-R (R = H or CH3_yXy where X = CH3 or CI and y = 0, 1, 2 or 3), has been studied by measuring the 35C1 NQR spectra and determining the crystal structures of the compounds N-(2,6-dichlorophenyl)-formamide, 2,6-Cl2C6H3- NHCO-H (DCPFA); N-(2,6-dichlorophenyl)-2-methylacetamide(propionamide), 2,6-Cl2C6H3- NHCO-CH2CH3 (DCPMA); N-(2,6-dichlorophenyl)-2,2-dimethylacetamide(isobutyramide), 2,6- Cl2C6H3-NHCO-CH(CH3 ) 2 (DCPDMA) and N-(2,6-dichlorophenyl)-2,2,2-trimethylacetamide (neopentylamide), 2,6-Cl2C6H3-NHCO-C(CH3)3 (DCPTMA), and by analysing the present data along with the 35CI NQR spectra and / or crystal structures of the compounds, 2,6-dichloroaniline, 2,6-Cl2C6H3-NH2 (DCA), N-(2,6-dichlorophenyl)-acetamide, 2,6-Cl2C6H3--NHCO-CH3 (DCPA), N-(2,6-dichlorophenyl)-2-chloroacetamide, 2,6-Cl2C6H3-NHCO-CH2Cl (DCPCA), N- (2,6-dichlorophenyl)-2,2-dichloroacetamide, 2,6-Cl2C6H3-NHCO-CHCl2 (DCPDCA) and N- (2,6-dichlorophenyl)-2,2,2-trichloroacetamide, 2,6-Cl2C6H3-NHCO-CCl3 (DCPTCA). The crystal type, space group, formula units and lattice constants in A of the new structures are;DCPFA: orthorhombic, Pbca, Z = 8, a = 8.593(3), b = 12.728(4), c = 14.376(4); DCPMA: orthorhombic, P212121, Z = 4, a = 4.774(2), b = 10.961(5), c = 19.562(8); DCPDMA: monoclinic, P21/c, Z = 4, a = 9.901(4), b = 13.785(5), c = 9.060(3), ß = 103.58(2)° and DCPTMA: monoclinic, P21/n, Z = 8, a = 16.047(5), b = 9.882(3), c = 16.270(5) ß = 102.12(1)°. The compound, DCPTMA shows two molecules in its asymmetric unit. This is in agreement with the multiple lines observed in the 35CI NQR spectra of the compound. The conversion of DCA (monoclinic) into it's various acid amides DCPFA, DCPA, DCPMA, DCPDMA, DCPTMA, DCPCA and DCPTCA affects it's crystal symmetry. The replacement of the side chain CH3 in DCPA by the H atom or substitution of either a CH3 group or a CI atom for one of the H atoms in the side chain CH3 or replacement of the two ring CI atoms by the H atoms changes it's crystal symmetry from monoclinic to orthorhombic, while the substitution of 2 or all the 3 H atoms in the CH3 group of DCPA by 2 or 3 CH3 groups or CI atoms restores it's crystal symmetry back to the monoclinic type. The bond lengths and bond angles are normal except for some deviations.

Synthesis and Crystal Structures of Three Carboxylate- Bridged Tetranuclear Copper(II) - Lanthanide(III) Complexes of Ph3P+CH2CH2CO2−

1999 ◽  
Vol 52 (10) ◽  
pp. 983 ◽  
Author(s):  
Yang-Yi Yang ◽  
Seik Weng Ng ◽  
Xiao-Ming Chen
Keyword(s):  
Oxygen Atom ◽  
Crystal Structures ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
Space Group ◽  
Bond Angles ◽  
Bond Lengths ◽  
Metal Atoms ◽  
Apical Site

Three tetranuclear copper(II)–lanthanide(III) complexes of triphenylphosphoniopropionate (Ph3P+CH2CH2CO2−,tppp), namely [Cu2Ln2(tppp)8(H2O)8](ClO4)10·2H 2 O [Ln = EuIII, NdIII or CeIII], were synthesized and characterized by crystallography. The EuIII complex crystallizes in the triclinic space group P1 – with a 16.249(7), b 17.185(11), c 17.807(11) Å, α 69.750(10), β 89.230(10), γ 84.070(10)˚, V 4639(5) Å3, Z 1. In the crystal structures, four tppp ligands bridge a pair of CuII and tetraaquo-EuIII atoms (Cu···Eu 3.527(2) Å) through their µ2-carboxylato ends to form a dinuclear subunit; two of these subunits are additionally linked by one of the CuII -bonded carboxylato oxygen ends, across a centre of inversion, to furnish a dimeric tetranuclear [Cu(tppp)4 Eu(H2O)4]2 species (Cu···Cu 3.323(2) Å). This CuII -bonded oxygen atom occupies the apical site of the square-pyramidal coordination environment of the CuII atom. The EuIII atom is eight-coordinated in a square-antiprismatic geometry. The NdIII and CeIII complexes are isomorphous to the EuIII complex, and only minor differences in bond lengths and bond angles involving the metal atoms are noted.

Studies in aryltin chemistry. Part 6. Crystal and molecular structures of tetra(p-methylsulphonylphenyl)tin(IV) and tetra(p-methylsulphinylphenyl)tin(IV) monohydrate

1990 ◽  
Vol 68 (8) ◽  
pp. 1277-1282 ◽  
Author(s):  
Ivor Wharf ◽  
Michel G. Simard ◽  
Henry Lamparski
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Direct Method ◽  
Molecular Structures ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Molecular Symmetry ◽  
Asymmetric Unit ◽  
Full Matrix ◽  
Space Group

Tetrakis(p-methylsulphonylphenyl)tin(IV) and tetrakis(p-methylsulphinylphenyl)tin(IV) n-hydrate have been prepared and their spectra (ir 1350–400 cm−1; nmr, 1H, 13C, 119Sn) and X-ray crystal structures are reported. The first compound is monoclinic, space group C2/c, Z = 4, with a = 21.589(6), b = 6.207(3), c = 22.861(11) Å, β = 93.80(3)° (22 °C); the structure was solved by the direct method and refined by full-matrix least squares calculations to R = 0.043 for 2755 observed reflections. It has 2 molecular symmetry with the methyl group and one oxygen atom completely disordered in both CH3S(O2) groups in the asymmetric unit. The second compound is tetragonal, space group P42/n, Z = 2, with a = b = 15.408(6), c = 6.379(2) Å (−100 °C); the structure was solved by the Patterson method and refined by full-matrix least squares calculations to R = 0.060 for 1209 observed reflections. It has [Formula: see text] molecular symmetry with the whole asymmetric unit disordered. Water molecules occupy positions on parallel 42 axes but molecular packing requirements prevent all sites having 100% occupancy giving n ~ 1 for the hydrate. Keywords: Tetra-aryltins, crystal structures, sulphone, sulphoxide, hydrogen-bonding.

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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