Molecular Adducts of 2,6-Diaminopyridine with Nitro-Substituted Aromatic Carboxylic Acids and the Crystal Structure of the 1 : 1 Adduct of 2,6-Diaminopyridine with 2-Nitrobenzoic Acid

1999 ◽  
Vol 52 (1) ◽  
pp. 71 ◽  
Author(s):  
Graham Smith ◽  
Catherine E. Pascoe ◽  
Colin H. L. Kennard ◽  
Karl A. Byriel
Keyword(s):  
Crystal Structure ◽  
Proton Transfer ◽  
Carboxylic Acids ◽  
Monoclinic Space Group ◽  
Chain Polymer ◽  
Aromatic Carboxylic Acids ◽  
X Ray Crystallography ◽  
Nitrobenzoic Acid ◽  
A Cell ◽  
A Chain

The 1 : 1 adducts of 2,6-diaminopyridine (2,6-dap) with a series of nitro-substituted aromatic carboxylic acids have been prepared and the crystal structure of one of these, with 2-nitrobenzoic acid (2-nba), [(2,6-dap)+ (2-nba)-] has been determined by X-ray crystallography and refined to a residual R 0·034 for 655 observed reflections. Crystals are monoclinic, space group P 21/c, with four molecules in a cell of dimensions a 7·376(2), b 22·837(3), c 7·716(2) Å, β 90·01(2)°. The structure involves proton transfer with the resulting pyridinium proton and an amine proton combining with the carboxyl oxygens of the 2-nba molecule in a primary cyclic hydrogen-bonding association. Additional interactions, involving all the remaining amine protons of 2,6-dap with both carboxyl oxygens and one nitro oxygen of 2-nba, complete a chain polymer structure. All other members of this series have been confirmed by infrared spectroscopy as proton transfer adducts.

Molecular Cocrystals of Aromatic Carboxylic Acids with 1,1-Diethylurea: Synthesis and the Crystal Structures of a Series of Nitro-Substituted Analogues

2000 ◽  
Vol 53 (3) ◽  
pp. 203 ◽  
Author(s):  
Graham Smith ◽  
Michael G. Coyne ◽  
Jonathan M. White
Keyword(s):  
Hydrogen Bonding ◽  
Carboxylic Acids ◽  
Acid Group ◽  
X Ray Diffraction ◽  
Chain Polymer ◽  
Aromatic Carboxylic Acids ◽  
Nitrobenzoic Acid ◽  
Simple Chain ◽  
A Chain ◽  
Polymeric Structures

Molecular adducts of 1,1-diethylurea with the nitro-substituted aromatic carboxylic acids 2-nitrobenzoic acid, [(C7H5NO4)(C5H12N2O)] (1), 3-nitrobenzoic acid, [(C7H5NO4)(C5H12N2O)] (2), 4-nitrobenzoic acid, [(C7H5NO4)2(C5H12N2O)] (3), 3,5-dinitrobenzoic acid, [(C7H4N2O6)(C5H12N2O)] (4), 5-nitrosalicylic acid, [(C7H5NO5)(C5H12N2O)] (5) and 3,5-dinitrosalicylic acid, [(C7H4N2O7)(C5H12N2O)] (6), have been prepared and characterized by using infrared spectroscopy, and, in the case of four of these [(1), (4), (5) and (6)], by single-crystal X-ray diffraction methods. In all examples, primary cyclic hydrogen-bonding interactions are found between the amide group of the substituted urea and the carboxylic acid group of the acid, while further peripheral associations result predominantly in simple chain polymeric structures, and in one case [adduct (1)], a cyclic tetramer. The crystal structure of the parent 1,1-diethylurea has also been determined, revealing a cyclic hydrogen-bonded tetramer which forms into a chain polymer by weak hydrogen-bonding associations.

A New Supramolecular Synthon Using N-Methylaniline. The Crystal Structure of the 1 : 1 Adduct of N-Methylaniline with 5-Nitrofuran-2-carboxylic Acid

1998 ◽  
Vol 51 (9) ◽  
pp. 867 ◽  
Author(s):  
Daniel E. Lynch ◽  
Lisa C. Thomas ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Proton Transfer ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Supramolecular Synthon ◽  
X Ray ◽  
C 23 ◽  
A Cell

The crystal structure of the 1 : 1 adduct of N-methylaniline with 5-nitrofuran-2-carboxylic acid has been determined by single-crystal X-ray diffraction. Crystals are monoclinic, space group P21/c with Z 4 in a cell of dimensions a 8·467(5), b 6·106(2), c 23·95(1) Å, β 94·48(3)°. The molecules associate in a tetrameric, proton-transfer formation which has potential as a new supramolecular synthon.

The Crystal Structure of KIO3.HIO3

1971 ◽  
Vol 49 (3) ◽  
pp. 468-476 ◽  
Author(s):  
Lilian Y. Y. Chan ◽  
F. W. B. Einstein
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
R Factor ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Potassium Hydrogen ◽  
A Cell ◽  
Least Squares Techniques

The crystal structure of potassium hydrogen di-iodate (bi-iodate) KIO3.HIO3 was determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.0 % for the 1392 observed reflexions. The salt crystallizes in the monoclinic space group P21/c with eight formula units in a cell of dimension a = 7.028(1) Å, b = 8.203(1) Å, c = 21.841(3) Å, β = 98.03(1)°.The iodate units are all basically pyramidal; weak interionic I—O contacts complete a very distorted octahedral environment around three iodine atoms. There is a capped octahedral (7-coordinate) environment around the remaining iodine atom. The I—O bonds are in the range 1.75–1.82 Å and the I—OH bonds are 1.91 and 1.95 Å, variations in length can be correlated with differences in the degree of involvement in (a) hydrogen bonding and (b) interaction with adjacent iodine atoms.

Preparation and Crystal Structure of Silver(I) Anthranilate

1999 ◽  
Vol 52 (4) ◽  
pp. 325 ◽  
Author(s):  
Graham Smith ◽  
Colin H. L. Kennard ◽  
Karl A. Byriel
Keyword(s):  
Major Constituent ◽  
Monoclinic Space Group ◽  
Zigzag Chain ◽  
Aminobenzoic Acid ◽  
X Ray Diffraction ◽  
Amine Nitrogen ◽  
Chain Polymer ◽  
X Ray ◽  
A Cell ◽  
Planar Angle

Silver(I) anthranilate, [Ag2(C7H6NO2)2]n, was isolated as the major constituent in the attempted preparation of the adduct of anthranilic acid (2-aminobenzoic acid) with silver(I) p-toluenesulfonate and its structure has been determined by using single-crystal X-ray diffraction. Crystals of the complex are monoclinic, space group P 21/n, with two dimers in a cell of dimensions a 5·3516(8), b 4·9746(2), c 25·386(5) Å, β 91· 547(8)°. The complex repeating unit comprises a distorted centrosymmetric biscarboxylato(-O,O′)-bridged dimer [Ag−O, 2·223, 2·409(4) Å; Ag---Ag 2·9128(9) Å] but has, in addition, a third bond to an adjacent amine nitrogen [Ag−N, 2·301(5) Å], which extends the structure into a zigzag chain polymer. The stereochemistry about each Ag centre is distorted trigonal planar [angle range, 89·9−142·9(2)°]. Relatively short inter-dimer Ag---Ag separations [2·989(1) Å] are also present.

The crystal structure of Bis[2-(pyridin-2-ylamino)-4-(pyridin-2-yl)thiazole]iron(II) Bis(tetrafluoroborate) trihydrate

1984 ◽  
Vol 37 (2) ◽  
pp. 443 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin ◽  
AD Rae
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Octahedral Structure ◽  
Space Group ◽  
X Ray ◽  
Disordered Structure ◽  
Distorted Octahedral ◽  
A Cell

The crystal structure of an iron(II) complex of 2-(pyridin-2-ylamino)-4-(pyridin-2-yl)tliazoe (paptH) has been determined by single-crystal X-ray diffractometry. [Fe(paptH)2] [BF4]2.3H2O is monoclinic, space group P21/c, with Z = 4 in a cell of dimensions a 8.968(6), b 9.038(4), c 41.15(2)�, β 94.81(2)�. The disordered structure was refined to a residual R 0.0826 for 2549 observed reflections. The ligands and anions are orientationally disordered, and the waters of crystallization are positionally disordered. Comprehensive constrained refinement, with 220 parameters for 139 atom positions, produced reliable geometry. The complex cation has a distorted octahedral structure of meridional configuration with both paptH ligands functioning as tridentates.

Molecular Cocrystals of Carboxylic Acids. XXXII The Crystal Structures of the Adducts of 2-Aminobenzothiazole with 3,5-Dinitrobenzoic Acid (Adduct Hydrate) and 3-Aminobenzoic Acid, and 2-Amino-2-thiazoline with 2-Aminobenzoic Acid

1998 ◽  
Vol 51 (7) ◽  
pp. 587 ◽  
Author(s):  
Daniel E. Lynch ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Optical Properties ◽  
Proton Transfer ◽  
Crystal Structures ◽  
Carboxylic Acids ◽  
Second Order ◽  
Aminobenzoic Acid ◽  
Aromatic Carboxylic Acids ◽  
X Ray ◽  
Linear Optical Properties ◽  
Acid Adduct

Two adducts of 2-aminobenzothiazole and one of 2-amino-2-thiazoline with aromatic carboxylic acids have been synthesized and their X-ray crystal structures determined. These are 2-aminobenzothiazole with 3,5-dinitrobenzoic acid (the 1 : 1 adduct hydrate) (1), and 3-aminobenzoic acid (1 : 1) (2), and 2-amino-2-thiazoline with 2-aminobenzoic acid (1 : 1) (3). Compound (1) is a non-centrosymmetric proton-transfer complex and gave a signal of 0·30 relative to urea when tested for second-order non-linear optical properties. Compound (3) is also a proton-transfer complex but (2) is not.

The Crystal Structure of Acifluorfen {5-[2-Chloro-4-(trifluoromethyl)-phenoxy]-2-nitrobenzoic Acid}

1987 ◽  
Vol 40 (6) ◽  
pp. 1131 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
T Hari
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Phenyl Ring ◽  
Acid Group ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Carboxylic Acid Group ◽  
X Ray ◽  
Nitrobenzoic Acid ◽  
Cell Dimensions

The crystal structure of the herbicide acifluorfen (5-[(2-chloro-4-trifluoromethyl)]phenoxy-2- nitrobenzoic acid] has been determined by X-ray diffraction and refined to a residual of 0.051for 1124 observed reflections. Crystals are monoclinic, space group C2/c with cell dimensions a 26.848(7), b 8 .O29(2), c 19 .Ol4(6) �, ,R l34.72(2)� and Z 8. The molecules form centrosymmetric hydrogen-bonded cyclic dimers [O---0, 2.637(7) �] with the carboxylic acid group and the phenoxy group synclinally related to the first phenyl ring while the nitro substituent isessentially coplanar with the ring.

The preparation and X-ray crystal structure of Te(N3)3SbF6 containing the triazidotellurium(IV) cation, Te(N3)3+

1989 ◽  
Vol 67 (11) ◽  
pp. 1687-1692 ◽  
Author(s):  
James P. Johnson ◽  
Gregory K. MacLean ◽  
Jack Passmore ◽  
Peter S. White
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Angles ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Average Bond

The crystal structure of Te(N3)3SbF6 containing the first binary tellurium–nitrogen cation, triazidotellurium(IV) (Te(N3)3+), has been determined by X-ray crystallography. Single crystals of Te(N3)3SbF6 are monoclinic, space group P21/c with a = 9.201(6), b = 8.445(4), c = 13.582(7) Å, β = 100.36(5)°, Z = 4, final R1 = 0.036 for 1286 observed reflections. The structure consists of discrete Te(N3)3+ cations and distorted octahedral SbF6− anions, with some cation–anion interactions. The average Te—Nα—Nβ—Nγ bond distances in Te(N3)3+ are Te—Nα, 1.994(7); Nα—Nβ, 1.237(11); and Nβ—Nγ, 1.116(12) Å. The average bond angles about the Te, Nα, and Nβ atoms are 94.1(3)°, 116.5(6)°, and 173.7(9)°. Structural correlations with other TeX3+ species have yielded an estimate of the electronegativity of the N3− group to be 3.1 ± 0.1. Keywords: tetratellurium (2+) cation, triazidotellurium(IV) cation, electronegativity, azide.

The Crystal Structure of Bis(2-chlorophenyl) Disulfide

1989 ◽  
Vol 42 (8) ◽  
pp. 1403 ◽  
Author(s):  
TCW Mak ◽  
WH Yip ◽  
WH Chan ◽  
G Smith ◽  
CHL Kennard
Keyword(s):  
Crystal Structure ◽  
Disulfide Bond ◽  
Torsion Angle ◽  
Monoclinic Space Group ◽  
Space Group ◽  
A Cell

The crystal structure of bis(2-chlorophenyl) disulfide has been determined and refined to a residual of 0.035 for 1573 observed reflections. Crystals are monoclinic, space group P21/a with Z 4 in a cell of dimensions a 7.724(1), b 22.360(7), c 7.917(2) � , β 114. 75�. The two chlorophenyl rings are synclinally related with a torsion angle of -85.0 � down the disulfide bond vector.

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