Preparation of Some Pyrrole-3,4-dicarboxylic Acid Derivatives and the Crystal Structure of 2-Methylpyrrolo[3,4-c]pyrrole-1,3(2H,5H)-dione

1991 ◽  
Vol 44 (2) ◽  
pp. 323 ◽  
Author(s):  
DP Arnold ◽  
LJ Nitschinsk ◽  
CHL Kennard ◽  
G Smith
Keyword(s):  
Crystal Structure ◽  
Dicarboxylic Acid ◽  
Substituent Effects ◽  
Ring System ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fused Ring ◽  
A Cell ◽  
Fused Ring System

A series of pyrrole-3,4-dicarboxylic acid derivatives has been prepared, and the crystal structure of one, 2-methylpyrrolo[3,4-c]pyrrole-1,3(2H,5H)- dione, has been determined by X-ray diffraction and refined to a residual R 0.049 for 1415 observed reflections. Crystals are monoclinic, space group P21/c, with Z= 8 in a cell of dimensions a 14.775(3), b 7.0692(5), c 15.151(3)Ǻ, β 118.82(8)�. Strain in the planar fused ring system is evident from the widening of the external interring angles to 143°, and from the unusual substituent effects in the 13C n.m.r. spectra.

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.

Synthesis and Crystal Structure of 9,9-Dipropionitrilefluorene

2013 ◽  
Vol 787 ◽  
pp. 208-210 ◽  
Author(s):  
Yuan Fang Hu
Keyword(s):  
Addition Reaction ◽  
High Yield ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
H Nmr ◽  
Fused Ring ◽  
Nucleophilic Addition Reaction ◽  
Fused Ring System

A compound of 9,9-dipropionitrilefluorene (C19H16N2,Mr=272.34) was synthesized via nucleophilic addition reaction under microwave irradiation (500 w) within short reaction time (8 min), giving high yield of product (87%). Its structure was determined IR,1H NMR, MS, elemental analysis and X-ray diffraction. The crystal belongs to monoclinic, space group P2(1)/c witha= 21.8358(16),b= 8.9457(7),c= 15.9895(12) Å, β = 105.078(2)o, V= 3015.8(4) Å3,Z=8,Dc= 1.200 g/cm3,μ=0.071 mm-1,F(000)=1152,R=0.0629 andwR= 0.0881 for 3155 observed reflection with I>2σ (I). X-ray analysis reveals that the three fused rings of the fluorene system are almost coplanar and the two propionitrile groups are completely perpendicular to the fused-ring system, the molecular is symmetrical.

Crystal structure of 9-Oxofluorene-4-carboxylic acid

1981 ◽  
Vol 34 (5) ◽  
pp. 1143 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
GF Katekar
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
A Cell

The crystal structure of 9-oxofluorene-4-carboxylic acid has been determined by direct methods using three-dimensional X-ray diffraction data, and refined to R0·068 for 1323 'observed' reflections. Crystals are monoclinic, space group P21/c with 24 in a cell of dimensions a 3·843(3), b 7·986(5), c 3269(2) �, β 96·64(4)�. The molecules form centrosymmetric hydrogen-bonded cyclic dimers [O···O 2·642(3) �] with the plane of the carboxylic acid making an angle of 26·5� with that of the 9-oxofluorene group. Stacks of molecules form down the a axis with 3.843 �. separation.

The Preparation and Crystal Structure of Ammonium Bis[citrato(3-)]cuprate(II)

1991 ◽  
Vol 44 (10) ◽  
pp. 1495 ◽  
Author(s):  
RC Bott ◽  
DS Sagatys ◽  
DE Lynch ◽  
G Smith ◽  
CHL Kennard ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Citric Acid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Teller Distortion ◽  
Space Group ◽  
X Ray ◽  
Jahn Teller ◽  
A Cell ◽  
Jahn Teller Distortion

The copper(II) complex with citric acid (NH4)4 [Cu(C6H5O7)2] has been prepared, and its structure determined by X-ray diffraction, giving a residual R 0.035 for 1208 observed reflections. Crystals are monoclinic, space group P21/c with Z 2 in a cell of dimensions a 8.755(3), b 13.185(4), c 9.364(2)Ǻ, β 113.73(2)°. The complex is a centrosymmetric six-coordinate monomer which is isomorphous with ammonium zinc(II) citrate. However, the Cu-O(hydroxyl) bonds [2.341(3)Ǻ] show Jahn-Teller distortion relative to the Cu-O(carboxyl) bonds [1.969(3) and 1.977(3)Ǻ].

Zur Struktur des Cycloheptatrienid-tricarbonyl-eisen(0)-Anions, [C7H7Fe(CO)3]– / The Structure of the Cyeloheptatrienide Triearbonyl Iron(O) Anion, [C7H7Fe(CO)3]-

1978 ◽  
Vol 33 (3) ◽  
pp. 261-264 ◽  
Author(s):  
Erich Sepp ◽  
Albert Pürzer ◽  
Gerhard Thiele ◽  
Helmut Behrens
Keyword(s):  
Crystal Structure ◽  
Ring System ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants

Abstract The crystal structure of the [C7H7Fe(CO)3]- anion stabilized with the [(C6H5)4As]+ cation has been determinated by X-ray diffraction. The crystals are monoclinic, space group P21/n. The unit cell with lattice constants a = 1607.9 pm, b = 1386.8 pm, c = 1249.1 pm and β - 91.52° includes four formula units. The Fe(CO)3 group is bonded to the allyl anion part of the C7H7 ring system, while the diene part is unco-ordinated.

Darstellung, 11B-, 13C-, 29Si-NMR- und Schwingungsspektren von Trimethylsilylmethyl-hexahydro-closo-hexaborat, [B6H6(CH2Si(CH3)3)]- sowie Kristallstruktur von [P(C6H5)4][B6H6(CH2Si(CH3)3)] / Preparation, 11B, 13C, 29Si NMR and Vibrational Spectra of Trimethylsilylmethyl-hexahydro-clo-hexaborate, [B6H6(CH2Si(CH 3)3)]-and the Crystal Structure of [P(C6H5)4] [B6H6(CH2Si(CH3)3)]

1995 ◽  
Vol 50 (7) ◽  
pp. 1025-1029 ◽  
Author(s):  
J. Baurmeister ◽  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
29Si Nmr ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
Quadrupole Coupling ◽  
Stretching Vibration ◽  
Ir And Raman ◽  
C Nmr

By reaction of [N(C4H9 )4]2 [B6H6] with iodomethyl-trimethylsilane in acetonitrile a solution with trimethylsilylm ethyl-closo-hexaborate(1-)anions, [B6H6 (CH2Si(CH3)3)]-, is formed. The crystal structure of [P(C6H5 )4][B6H6(CH2Si(CH3)3)] has been determined by single crystal X-ray diffraction analysis; monoclinic, space group P21/n with a = 16.140(2), b = 11.646(8), c = 16.731(3) Å, β 109.664(11)°. The 11B NMR spectrum reveals features of a mono hetero substituted octahedral B6 cage. The 13C NMR spectrum exhibits a quartet at +0.18 ppm with 1J(C,H) = 118 Hz for the three methyl groups and a weak multiplet at -0.65 ppm for the methylene bridge due to quadrupole coupling with the boron atoms. In the 29Si NMR spectrum a decet at +2.25 ppm with 2J(C,H ) = 6.9 Hz is observed. The B -C stretching vibration is observed at 1155 cm-1 in the IR and Raman spectrum.

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

The Influence of the Axial Ligands of a Series of Platinum(IV) Anti-Cancer Complexes on Their Reduction to Platinum(II) and Reaction With DNA

1995 ◽  
Vol 48 (4) ◽  
pp. 793 ◽  
Author(s):  
LT Ellis ◽  
HM Er ◽  
TW Hambley
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reduction Potentials ◽  
Axial Ligands ◽  
Carboxylate Anions ◽  
Anti Cancer ◽  
Molecular Modelling Studies ◽  
Modelling Studies

The electrochemical reduction and DNA binding have been studied for a series of platinum(IV) complexes with Cl-, OH-, and carboxylate anions as the axial ligands ; [Pt(en)Cl4], [Pt(en)Cl2(OH)2], and [Pt(en)Cl2(OC(O)R)2], R = CH3, CH2CH3, CH2CH2CH3. Cathodic reduction potentials vary by more than 650 mV with the tetrachloro complex reduced most readily and the dihydroxo least readily. The binding of the complexes correlates with the reduction potentials with the more readily reduced complexes binding more readily to DNA. The influence of the reducing agent glutathione on platinum binding to DNA was found to depend on whether it was added before or after Pt/DNA incubation. The results are consistent with octahedral platinum(IV) binding monofunctionally to DNA, and molecular modelling studies have been used to confirm that this is sterically feasible. The crystal structure of [Pt(en)Cl2(OC(O)CH3)2] has been determined by X-ray diffraction methods and refined to R = 0.028 (977 F). The crystals are monoclinic, space group C2/c, a 15.569(6), b 8.104(1), c 13.188(1) Ǻ, β 136.38(2)°.

Darstellung von Mononitropentahydrohexaborat(2-) und Kristallstruktur von M2[B6H5(NO2)], M = K, Cs / Preparation of Mononitropentahydrohexaborate(2—) and Crystal Structure of M2[B6H5(NO2)], M = K, Cs

1993 ◽  
Vol 48 (12) ◽  
pp. 1727-1731 ◽  
Author(s):  
A. Franken ◽  
W. Preetz ◽  
M. Rath ◽  
K.-F. Hesse
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and the base DBU in dichloromethane solution mononitropentahydrohexaborate [B6H5(NO2)]2- ions are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of the K and Cs salt were determined from single crystal X-ray diffraction analyses. K2[B6H5(NO2)] is monoclinic, space group P21/m with a = 5.953(1), b = 8.059(4), c = 8.906(1) Å, β = 109.553(9)°; Cs2[B6H5(NO2)] is monoclinic, space group P21/a with a = 9.438(6), b = 9.644(7), c = 11.138(9) Å, β = 101.44(9)°. The B6 octahedron is compressed in the direction of the B—NO2 bond by about 5%, with bond lengths between 1.67 and 1.77 A.

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.

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