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1.
Venkatraman Junnotula Ujjal Sarkar Charles L. Barnes Praveen K. Thallapally Kent S. Gates 《Journal of chemical crystallography》2006,36(9):557-561
The compound 3-methyl 1,2,4-benzotriazine 1,4-dioxide (1) belongs to a new class of clinically promising, bioreductively-activated antitumor drugs. Reductive metabolism of these triazine di-N-oxides typically produces mixtures of mono-N-oxide analogues. As part of our efforts toward characterization of the in vitro metabolism of 1, we synthesized the 1-oxide (2) and 2-oxide (3) analogues and characterized these compounds using X-ray crystallography. Compounds 2 and 3 (C8H7N3O) crystallized in the monoclinic space group P21/c. Unit cell parameters for 2: a = 9.0466(7), b = 10.5959(8), c = 7.8981(6) ?, β = 98.4940(10), and z = 4. Unit cell parameters for 3: a = 5.7193(4), b = 9.3774(7), c = 13.8427(11) ?, β = 101.6370(10), and z = 4.Supplementary material X-ray crystallographic data reported in this paper is deposited with the Cambridge Crystallographic Data Center as supplementary publication numbers CCDC 294738 (compound 2) and CCDC 294739 (compound 3). Copies of available material can be obtained, free of charge, on application to the Director, CCDC, 12 Union Road, Cambridge CB21EZ, UK. 相似文献
2.
Saeid J. Behroozi Charles L. Barnes Kent S. Gates 《Journal of chemical crystallography》1998,28(9):689-691
The compound 3H-1,2-benzodithiol-3-one 1-oxide (2) has proven useful in modeling the reactivity of the novel antitumor antibiotic leinamycin (1). The crystal structure of this unusual sulfur heterocycle is reported here. The molecule crystallizes in the P-1 space group with cell parameters a = 7.168(4), b = 7.670(3), c = 7.922(3)Å, = 68.34(4), = 83.86(3), = 65.50(3),° and U = 367.8 Å3. 相似文献
3.
J. C. Morrow 《Journal of chemical crystallography》1974,4(4):243-252
The crystal and molecular structure of dichlorobis(pyridine-1-oxide) copper(II), C10H10N2O2Cl2Cu, has been determined from 3931 reflections measured on a Picker four-circle diffractometer, using the /2 scan technique and MoK radiation. The crystals are monoclinic, space groupP21/c,a = 6.900(4),b = 15.065(7),c = 12.065(5) Å, = 97.00(4) ° andZ = 4. The structure was solved by Fourier methods and refined by full-matrix least-squares. The final conventionalR-factor was 0.033. The compound is dimeric, and the units of the dimer are held together by oxygen bridges. The coordination polyhedron for Cu is a tetragonal pyramid, with two bridging oxygens and two chlorines in the basal plane. The apical position is occupied by oxygen in the non-bridging ligand. The Cu–Cu distance in the dimer is 3.306(1) Å. 相似文献
4.
The crystal and molecular structure oftrans-dichlorobis(oxazole)palladium-(II), Pd(C3H3ON)2Cl2, has been determined by single-crystal X-ray diffraction techniques using counter methods and has been refined by full-matrix least-squares procedures to a finalR index of 0.022. The complex crystallizes in the triclinic space groupP¯1 with unit cell dimensions ofa = 6.957(1),b = 7.506(1),c = 5.538(1) Å, = 109.22(1), = 91.37(1), and = 115.09(1) °, withZ = 1. The palladium(II) ion, located at an inversion center, is coordinated in a regular square-planar manner to two chloride ions at 2.293(1) Å and, at 2.016(2) Å, to the nitrogen atoms of two oxazole ligands. The planar oxazole rings are tilted 33 ° with respect to the PdN2Cl2 plane. Further verification of the presence of oxazole in the complex was obtained by high-resolution mass spectrometry. Crystals of Pd(C3H3ON)2Cl2 resulted irreproducibly from attempts to prepare single crystals of a previously reported dimeric palladium(II) disulfide complex by treating Pd(CH3CN)2Cl2 with a slight excess of diphenyl disulfide in benzene in the atmosphere. The source of the oxazole is not understood. 相似文献
5.
S. Ianelli G. Pelizzi F. Vitali G. Devoto M. Massacesi G. Ponticelli 《Journal of chemical crystallography》1985,15(4):351-358
The crystal structure of Pd(N-PropIm)2Cl2 has been determined from X-ray data collected by counter methods. The compound crystallizes in the monoclinic space groupP21/n with four molecules per unit cell, the dimensions of which area=14.554(5),b=8.204(2),c=14.860(3) Å,=115.63(2)°. Full-matrix least-squares refinement gave a final R value of 0.0263 for 1913 independent observed reflections. The Pd atom is four-coordinated and is surrounded in atrans square planar fashion by two N atoms of the imidazole groups and by two Cl ions. 相似文献
6.
7.
8.
Crystals of the title compound, C17H16BrNO, are monoclinic, space groupP21/n, unit-cell parametersa = 14.48,b = 6.20,c = 16.72 Å, and = 97.35 °. Three-dimensional data were collected with CuK radiation using an automatic diffractometer. The structure was solved by the heavy-atom method and refined by block diagonal least squares to anR index of 0.088 for 2210 reflections. The main features obtained from our studies are (i) the C=O group is orientedanti to the benzene ring, in agreement with the nmr studies; (ii) the C(2) proton is equatorial while the methyl group at C(2) is in an axial position, also in agreement with nmr data. The bromobenzoyl ring and the benzene ring are at 64 ° to each other, while the carbonyl >C=O and the bromobenzoyl groupsBr are at 42 ° to each other. 相似文献
9.
Víctor Manríquez Marcelo Campos-Vallette Nelson Lara Nelson González-Tejeda Oscar Wittke Guillermo Díaz Sylvia Diez René Muñoz Lukas Kriskovic 《Journal of chemical crystallography》1996,26(1):15-22
The structures of [Cu(en)(H2O)2]SO4 (I), [Cu(en)2](NO3)2 (II) and [Cu(trien)I]I (III) have been determined by single crystal X-ray diffraction. ComplexI is monoclinic, space group C2/c, with unit cell parametera=7.232(1),b=11.725(2),c=9.768(1), =105.50(1)°, andZ=4. ComplexII is also monoclinic, space group P21/a, witha=7.978(2),b=9.982(4),c=8.218(3), =111.11(2)°, andZ=2. ComplexIII is orthorhombic, space group P212121, witha=8.098(1),b=11.902(1),c=13.682(2), andZ=4. The structures were solved by direct methods and refined by full-matrix least-squares to finalR values of 0.031, 0.043 and 0.036 for complexesI, II, andIII, respectively. ComplexesI andII show an octahedral coordination geometry. ComplexIII shows a square pyramidal coordination geometry. ComplexI forms infinite monodimensional chains where the SO
4
2–
ions acts as a bridge between two neighboringen molecules. The vibrational spectra of these complexes agree well with their crystal structures. Structure and stability of seven other related Cu(II) complexes of (trien), (dien)2, (en)2 and (en) are inferred in this study. 相似文献
10.
S. Rantsordas 《Journal of chemical crystallography》1991,21(2):139-143
The crystal and molecular structure of the title compound: C10H13OCl, determined by single-crystal X-ray diffraction is reported. Crystals are monoclinic, space group P21/a (No14),a=18.435(7),b=24.642(6),c=9.116(6)Å,=103.23(5)°,Z=16,D
x
=1.216 Mg m–3,F(000)=1568,V=4031(1)Å3. The structure was solved by direct methods and the finalR value is 8.5%. The four molecules in asymmetric unit are linked by hydrogen bonds and form an infinite chain parallel to the (bc) plane. Different chains are held together by van der Waals forces. 相似文献
11.
[C15H25N2O2
+·ClO
4
–
,M
r
=364.83, is monoclinic:P21,a=7.885(1),b=10.685(1),c=10.658(1) Å,=105.63(1)°,V
c
=864.8(2) Å3,Z=2,D
x
=1.39(1)g cm–3, (CuK)=1.54178 Å,(CuK)=21.4 cm–1,F(000)=388 e,T=292K,R=0.066 for 1205 unique reflections. The piperidine ringsA, B, C, andD have chair, chair, boat, and half-chair conformations, respectively. The quinolizidine system (ringsA/B) has atrans configuration. The cations are interconnected by a hydrogen bond O(N1)O(C15) of 2.552(10) Å into chains along [010]. Atoms C(12) and C(13) from ringD of the cation are disordered. Very high thermal parameters of the oxygen atoms of the perchlorate anion may indicate its orientational disorder. 相似文献
12.
Douglas X. West Christine A. Brown Jerry P. Jasinski John M. Jasinski Rick M. Heathwaite David G. Fortier Richard J. Staples Ray J. Butcher 《Journal of chemical crystallography》1998,28(12):853-860
Structures of the following compounds have been solved: tris(2-thio-6-picoline N-oxide)cobalt(III), [Co(6MOS)3], orthorhombic, Pca21, a = 17.871(3), b = 14.061(2), c = 15.964(2) Å, V = 4011(1) Å3, Z = 8, and = 1.193 mm–1; bis (2-thio-6-picoline N-oxide)nickel(II), [Ni(6MOS)2], orthorhombic, Pbca, a = 15.602(8), b = 13.606(4), c = 13.348(8) Å, V = 2833(4) Å3, Z = 8, and = 1.655 mm–1; bis(2-thio-6-picoline N-oxide)copper(II), [Cu(6MOS)2], orthorhombic, Pbca, a = 13.914(5), b = 12.984(5), c = 15.663(6) Å, V = 2830(2) Å3, Z = 8, and = 1.836 mm–1; and bis(2-thio-6-picoline N-oxide)zinc(II), [Zn(6MOS)2], triclinic, P – 1, a = 7.9737(8), b = 11.7786(9), c = 7.9206(8) Å, = 104.502(7), = 104.495(8), = 93.445(8)°, V = 691.3(1) Å3, Z = 2, and = 2.106 mm–1. The steric effect of the methyl group in the six-position of the N-oxide ring is considered in comparing these structures to complexes of 2-thiopyridine N-oxide. 相似文献
13.
A. Mukhopadhyay P. K. Maiti M. K. Das S. K. Talapatra 《Journal of chemical crystallography》1993,23(6):465-468
The crystal structure of the title compound, C7H10N3B, has been determined by X-ray diffraction using CuK radiation. The crystals are monoclinic,P21/c witha=6.941(2),b=15.961(3),c=7.739(2) Å,=90.5(2)° andZ=4. The structure was solved by direct methods, and refined by full matrix least squares to a finalR-value of 056 with 833 observed reflections. The molecule is in the elongated form, but is not planar; the torsion angle C(2)-N(1)-B-C(8) is 82.9(4)°. The bond distances N(1)-B=1.587(5) Å; B-C(8)=1.586(6) Å; C(8)N(3)=1.134(5) Å. The B-C-N moiety is slightly [176.9(4)°] nonlinear. The molecules are linked by weak hydrogen bonds N(2)-H(1N)N(3), N(2)-N(3)=3.055(5) Å and N(2)-H(2N)N(3), N(2)-N(3)=3.165 Å. 相似文献
14.
Yu. M. Chumakov V. I. Tsapkov I. G. Filippova G. Bocelli A. P. Gulea 《Crystallography Reports》2008,53(4):619-625
The crystal structures of {4-bromo-2-[(2-hydroxyethylimino)-methyl]phenolo}aquacopper(II) nitrate hemihydrate (I), chloro-{4-bromo-2-[(2-hydroxyethylimino)-methyl]phenolo}copper hemihydrate (II), and chloro-{4-bromo-2-[(2-hydroxyethylimino)-methyl]phenolo}aquanickel (III) are determined using X-ray diffraction. Crystals of compound I are formed by cationic complexes, nitrate ions, and solvate water molecules. In the cation, the copper atom coordinates the singly deprotonated molecule of tridentate azomethine and the water molecule. The copper complexes are joined into centrosymmetric dimers by the O w -H···O hydrogen bonds. The crystal structure of compound II is composed of binuclear copper complexes and solvate water molecules. The copper atom coordinates the O,N,O ligand molecule and the chlorine ion, which fulfills a bridging function. The coordination polyhedron of the metal atom is a distorted tetragonal bipyramid in which the vertex is occupied by the chlorine atom of the neighboring complex in the dimer. Compound III is a centrosymmetric dimer complex. The coordination polyhedra of two nickel atoms related via the inversion center are distorted octahedra shared by the edge. 相似文献
15.
T. Głowiak W. Sawka-Dobrowolska B. Jeżowska-Trzebiatowska A. Antonow 《Journal of chemical crystallography》1980,10(1-2):1-10
The crystal and molecular structure of bis(aminomethylphosphonate)-copper(II), C2H10N2O6P2Cu, has been determined from MoK diffractometer data. The compound crystallizes in the monoclinic space groupP21/n witha =7.571(2),b = 4.943(1),c = 11.212(3) Å, = 105.84(2) °, andZ = 2. The structure was solved by the heavy-atom technique and refined by full-matrix least-squares methods toR = 0.041, using 1084 reflections for which ¦F
o¦ > 3.92 (¦F
o¦). In this complex, the Cu atom is square-planar coordinated by four O atoms from four phosphonic groups, and not by the amino group. The Cu-O bond lengths are 1.928(3) and 1.937(3) Å, and the phosphonic groups bridge adjacent Cu atoms in polymeric chains. The infrared spectrum of this complex is reported. 相似文献
16.
The reaction of CuBr2 with benzimidazole and HBr in aqueous solution leads to the formation of Cu(C7H6N2)2Br2 as dark-brown, stable monoclinic crystals. Space groupP21/c witha=13.794(5),b=7.875(2),c=14.510(6) Å;=105.82(5)°;V
c
=1516(5) Å3;D
x
=2.010(3) Mg m–3. The structure was refined by a full-matrix least-squares procedure to giveR=R
w
=0.045 for 1932 intensities above 3(I). The copper (II) ions are four coordinates in the form of a distorted flattened tetrahedron CuN2Br2, with the bond lengths Cu-Br(1)=2.402(1), Cu-Br(2)=2.446(1), Cu-N(1)=1.976(7), and Cu-N(11)=1.946(7) Å. The flattened angles are Br-Cu-Br=139.0(1) and N-Cu-N=154.6(3)°. The geometry of intermolecular and intramolecular hydrogen bonds is discussed. 相似文献
17.
Colin Hester Russell G. Baughman Harvest Collier 《Journal of chemical crystallography》1996,26(10):695-699
The reaction between cadmium(II) chloride and 2,2'-bi-1H-imidazole (H2biim) in an acidic solution affords [Cd(H3biim)2Cl4] (H3biim=2-(2-1H-imidazolyl)-1H-imidazolium) in 63% yield. The compound crystallizes in the triclinic space groupP1, wherea=8.072(2),b=8.100(2),c=8.593(2) Å, =75.89(2), =62.94(2), =63.29(1)°,V=446.4(2) Å3, andZ=1. The central Cd atom exhibits an octahedral geometry composed of a Cl4N2 core. The Cd-N bond distance is 2.392(2) Å. Cd–Cl distances are 2.5919(9) and 2.671(1) Å. 相似文献
18.
R. Mrozek Z. Rza¸czyńska M. Sikorska-Iwan T. Głowiak 《Journal of chemical crystallography》1999,29(7):803-808
Two polymeric complexes of glicyne with manganese(II) have been prepared and characterized by means of spectroscopic and x-ray analyses. The first complex of the formula [Mn(Gly)Cl2(H2O)2] crystallizes in the monoclinic space group P21/n with a = 6.519(2), b = 15.981(3), c = 7.893(2) Å, and = 97.18(3)°. The Mn atoms are in distorted octahedral environments with all ligands in cis positions. The adjacent manganese(II) ions are linked in polymeric chains via carboxylate groups. The second complex [Mn(Gly)2Cl2] crystallizes in the triclinic space group P
with a = 4.968(2), b = 6.582(2), c = 7.925(3) Å, = 106.17(3), = 92.86(3), and = 107.21(3)°. The octahedral-coordinated manganese(II) ion is situated on a crystallographic center of symmetry and is bound to four carboxylate oxygen atoms from different glicyne molecules and two chloride ions. 相似文献
19.
P. T. Beurskens J. A. Cras Th. W. Hummelink J. H. Noordik 《Journal of chemical crystallography》1971,1(3):253-257
The crystal and molecular structure of bis(N,N-diethyldithiocarbamato)palladium(II), Pd(S2CN(C2H5)2)2, has been determined by a three-dimensional X-ray analysis. The compound crystallizes in the tetragonal space groupP42/n with unit cell dimensionsa = 16·439(8) Å andc = 6·247(3) Å. The crystals are isomorphous with bis(N,N-diethyldithiocarbamato)platinum(II). Intensities were obtained with an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·038 for 600 non-zero observed reflections. The palladium is in planar coordination with four sulphur atoms, the two non-equivalent Pd-S bond lengths being 2·317(3) and 2·315(3) Å.The authors are grateful to Mr J. G. M. van Rens for providing the crystals and measuring the unit cell dimensions, to Professor J.J. Steggerda for his continuous interest and to Mr W.P.J.H. Bosman, Mr J.M.M. Smits and Mr J.A.B.C. Wolf for valuable assistance. 相似文献
20.
The imidazolinone herbicide imazapyr, 2-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)nicotinic acid (H2imz) interacts with Cu(II) leading to [Cu(Himz)2(H2O)2] which crystallizes in the space group Pbca, with a = 12.5370(3) Å, b = 19.8500(5) Å, c = 22.7720(9) Å, and Z = 8. The Cu(II) atom is octahedrally surrounded by four nitrogen atoms of two Himz– anions and two water molecules. Each Himz– acts as a chelating ligand by means of N pyridine and N lactam atoms leading to five-membered chelate rings. The Cu
N distances vary from 1.948(4) to 2.299(5) Å while the Cu
O are 2.114(5) and 2.256(6) Å. The imidazol N-H are involved in short intramolecular hydrogen bonds with the carboxylate groups. The structure is stabilized by an intermolecular hydrogen-bonded network involving the water molecules and the carboxylate groups. 相似文献