A two-dimensional copper(I) polymer containing both molecular rod and anionic bridges: synthesis and crystal structure of (µ-chloro)-(µ-pyrazine)copper(I)

1995 ◽  
Vol 73 (10) ◽  
pp. 1591-1595 ◽  
Author(s):  
J.M. Moreno ◽  
J. Suarez-Varela ◽  
E. Colacio ◽  
J.C. Avila-Rosón ◽  
M.A. Hidalgo ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Heavy Atom ◽  
Electronic Spectroscopy ◽  
Chloride Ions ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Tetrahedral Environment ◽  
Heavy Atom Method

The crystal structure of bright-red crystals of the bidimensional polynuclear diamagnetic (µ-chloro)(µ-pyrazine)copper(I) complex has been analyzed from X-ray diffraction data. The structure was solved by the heavy-atom method. Full-matrix least-squares refinement based on 673 reflections with F > 4σ(F) converged to a final R = 0.043 and Rw = 0.048. Crystals of this complex are monoclinic, space group P2/c, a = 3.814(1), b = 6.356(1) and c = 11.497(5) Å; β = 96.04(2)°, Z = 2. The structure consists of planes of copper(I) atoms linked by pyrazine and Cl− bridges, each Cu(I) being in a distorted tetrahedral environment formed by two chloride ions and two nitrogen atoms belonging to two pyrazine molecules, with bond distances of Cu—Cl = 2.349(1) and Cu—N = 2.038(4) Å. Vibrational and electronic spectroscopy of the title compound is also reported. Keywords: two-dimensional copper(I)–pyrazine complexes.

Synthesis and Crystal Structure Determination of Cyclosporin H

2000 ◽  
Vol 65 (8) ◽  
pp. 1317-1328 ◽  
Author(s):  
Alexandr Jegorov ◽  
Ladislav Cvak ◽  
Aleš Husek ◽  
Petr Šimek ◽  
Anna Heydová ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Amino Acids ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Acid Catalyzed ◽  
Products Of Reaction ◽  
Cyclosporin H

Acid-catalyzed degradation of cyclosporin A was studied in various solvents and products of reaction were monitored by HPLC. Identification of amino acids and their chirality were determined after hydrolysis and derivatization by GC-MS. Cyclosporin H was isolated as the principal product and its structure was determined by X-ray diffraction: Cyclosporin H- diethyl ether-water (1 : 0.5 : 1) crystallizes in the monoclinic space group I2 with a = 12.338(2) Å, b = 18.963(2) Å, c = 34.074(3) Å, β = 96.47(2)°, Z = 4, and V = 7 921.4(17) Å3.

Synthesis and Crystal Structure of a Fe(II,III) Complex with 2-(4΄-Chlorine-benzoyl)-benzoic acid and 3-(2-Pyridyl)pyrazole

2013 ◽  
Vol 634-638 ◽  
pp. 2592-2595
Author(s):  
Qing Wei Wang ◽  
Ting Feng Lu ◽  
Jia Guo ◽  
Xiu Mei Li
Keyword(s):  
Crystal Structure ◽  
Benzoic Acid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Organic Complex ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Elemental Analyses ◽  
Metal Organic Complex ◽  
Metal Organic

A new metal-organic complex FeII2FeIII2(cbba)4(L)6 (Hcbba = 2-(4΄-chlorine-benzoyl) benzoic acid, L = 3-(2-pyridyl)pyrazole) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, TG and IR spectroscopy. The compound crystallizes in monoclinic, space group Cc with a = 17.729(5), b = 15.919(5), c = 33.650(5) Å, β = 92.058(5)°, V = 9491(4) Å3, C104H68Cl4Fe4N18O12, Mr = 2126.96, Dc = 1.489 g/cm3, μ(MoKα) = 0.786 mm1, F(000) = 4344, Z = 4, the final R = 0.0559 and wR = 0.1122 for 12093 observed reflections (I > 2(I)).

Crystal and Molecular Structure of Dithiocyanato(triphenylarsine)mercury(II)

1975 ◽  
Vol 53 (22) ◽  
pp. 3383-3387 ◽  
Author(s):  
Joseph Hubert ◽  
André L. Beauchamp ◽  
Roland Rivest
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Coordination Number ◽  
Diffraction Data ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Heavy Atom Method

The crystal and molecular structure of dithiocyanato(triphenylarsine)mercury(II) has been determined from X-ray diffraction data. The crystals are monoclinic, space group P21/c, with a = 10.290(7), b = 21.199(23), c = 10.719(7) Å, β = 112.00(2)°, and Z = 4. The structure has been solved by the heavy-atom method and refined by block-diagonal least-squares calculations. The agreement factor R obtained for 2607 'observed' reflections is 0.030. The crystal consists of single molecules. The 'characteristic' coordination number of mercury is three, with two sulfur and one arsenic atoms at the apexes of a triangle. The nitrogen atoms of the thiocyanate groups are at 2.67 and 2.74 Å from the adjoining mercury atoms and therefore link the different molecules together.

Crystal Structure of Adeninium Trichloromercurate(II),

1975 ◽  
Vol 53 (15) ◽  
pp. 2345-2350 ◽  
Author(s):  
Monique Authier-Martin ◽  
André L. Beauchamp
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Title Compound ◽  
Heavy Atom ◽  
Chloride Ions ◽  
Water Molecules ◽  
Hydrogen Atoms ◽  
Space Group ◽  
Heavy Atom Method

The title compound belongs to space group P21/c with a = 23.99(1), b = 4.245(2), c = 25.98(1) Å, β = 117.58(7)°, and Z = 8. The structure was solved by the heavy-atom method and refined by block-diagonal least squares on 2589 independent observed reflections. All non-hydrogen atoms were refined anisotropically and some of the hydrogen atoms were located but their parameters were not refined. The final values of R and Rw were 0.042 and 0.047, respectively.The two nonequivalent mercury atoms have very similar environments. Two short Hg—Cl bonds (2.34–2.38 Å) at ∼ 165° define a quasi-molecular HgCl2 unit. Overall octahedral coordination is completed with two chloride ions at 2.76–2.84 Å and two chlorine atoms at 3.19–3.26 Å on neighboring HgCl2 quasi-molecules. HgCl6 octahedra share edges to form twofold ribbons in the b direction. This pattern of octahedra is identical with the onereported for β-NH4HgCl3. The cations are pairs of N(1)-protonated adenine molecules linked by two N(10)—H(10)… N(7) hydrogen bonds and stacked in the b direction. Water molecules act as acceptors in moderately strong hydrogen bonds with acidic protons H(1) and H(9) of adeninium ions. Other generally weaker hydrogen bonds exist between the various parts of the structure.

Synthese und Kristallstruktur von [Hg2(p-SC6H4NO2)]NO3 / Synthesis and Crystal Structure of [Hg2(p-SC6H4NO2)]NO3

1990 ◽  
Vol 45 (8) ◽  
pp. 1193-1196 ◽  
Author(s):  
Klaus Brodersen ◽  
Axel Knörr
Keyword(s):  
Crystal Structure ◽  
Chain Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Nitrate Ions ◽  
R Value ◽  
A Chain

[Hg2(p-SC6H4NO2)]NO3 is formed by the reaction of p-nitrothiophenol with dimercury(I)-dinitrate in methanol. It crystallizes in the monoclinic space group P21/n with a = 1175.5(9) pm, b = 1079.8(8) pm, c = 876.2(8) pm, β = 110.74(4)° and Z = 4. The crystal structure has been determined by X-ray diffraction and refined to an R-value of 0.052. The results show that the compound exists as a chain structure of [—®S(C6H4NO2)— Hg— Hg—]n with nitrate ions connecting the chains.

Synthesis and Crystal Structure of a Caesium Hydrogen Benzoylcyanoximate Complex with 18-Crown-6: Cs(18-Crown-6){H(L)2}

1997 ◽  
Vol 52 (8) ◽  
pp. 901-905 ◽  
Author(s):  
Vera V Ponomareva ◽  
Victor V Skopenko ◽  
Konstantin V Domasevitch ◽  
Joachim Sieler ◽  
Thomas Gelbrich
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Crown Ether ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
The Mean ◽  
Cyano Groups ◽  
Oxygen Atoms

Abstract The caesium hydrogen benzoylcyanoximate (L-) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [monoclinic, space group P21/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Å, β = 90.13(1)°, V = 3434.3(9) Å, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of Cs(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}-, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O - - - O ca. 2.456(5)Å]. The caesium atom deviates by 1.492(3) Å from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical “sunrise coordination” [Cs-O (ether) 3.040(9)-3.312(7) Å]. The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (Cs-O ca. 3.040(9), 3.312(7) Å; Cs-N ca. 3.469(5), 3.679(6) Å). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism.

Studies on tellurium-carbon bonded compounds. II. The crystal structure of [Heptane-3,5-dionato(2 - )]tellurium(II) ('1,1′-Dimethylacetylacetone tellurium(II)')

1977 ◽  
Vol 30 (3) ◽  
pp. 487 ◽  
Author(s):  
JC Dewan ◽  
J Silver
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Heavy Atom ◽  
Chair Conformation ◽  
Heterocyclic Ring ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
Heavy Atom Method

The structure of the title compound has been determined by the heavy- atom method from 973 reflections, measured with a diffractometer, and refined by full-matrix least-squares methods to R 0.030. Crystals are monoclinic, space group P21, a = 8.69(1), b = 4.86(1), c = 10.14(2) Ǻ, β = 98.7(1)�, Z = 2. In the discrete molecules of the complex a tellurium(II) atom is bonded to one bivalent heptane-3,5-dione ligand through the α-carbon atoms [Te-C 2.184(6), 2.206(7) Ǻ; C-Te-C 89.7(3)�], forming a heterocyclic ring of chair conformation with the methyl substituents both in equatorial positions. The molecules are arranged in a zig-zag polymeric manner about the 21 axes at x = 0 and z = 0. All hydrogen atoms have been located.

scholarly journals Synthesis and Crystal Structure ofN-Dichloroacetyl-3,4-dihydro-3-methyl-6-chloro-2H-1,4-benzoxazine

2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Shuang Gao ◽  
Hai-Tao Qu ◽  
Fei Ye ◽  
Ying Fu
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Compound C

A new compound,N-dichloroacetyl-3,4-dihydro-3-methyl-6-chloro-2H-1,4-benzoxazine, was synthesized and characterized. The crystal structure of the title compound (C11H10Cl3NO2,Mr=294.55) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space groupP21/c, witha=6.7619(14),b=24.866(5),c=9.737(3) Å,α=90.00,β=130.982(18),γ=90.00°,V=1235.9(5) Å3,Z=4,Dx=1.583 Mg/cm3,λ(Mo  Ka)=0.71073 Å,F(000)=600,μ=0.729 mm−1,R=0.0476, andwR=0.1274for 2217 reflections withI>2σ(I).

Ab initio determination and Rietveld refinement of the crystal structure of Ni0.50TiO(PO4)

1999 ◽  
Vol 14 (1) ◽  
pp. 10-15 ◽  
Author(s):  
P. Gravereau ◽  
J. P. Chaminade ◽  
B. Manoun ◽  
S. Krimi ◽  
A. El Jazouli
Keyword(s):  
Crystal Structure ◽  
Ab Initio ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Heavy Atom ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Heavy Atom Method

The structure of the oxyphosphate Ni0.50TiO(PO4) has been determined ab initio from conventional X-ray powder diffraction data by the “heavy atom” method. The cell is monoclinic (space group P21/c, Z=4) with a=7.3830(5) Å, b=7.3226(5) Å, c=7.3444(5) Å, and β=120.233(6)°. Refinement of 46 parameters by the Rietveld method, using 645 reflexions, leads to cRwp=0.152, cRp=0.120, and RB=0.043. The structure of Ni0.50TiO(PO4) can be described as a TiOPO4 framework constituted by chains of tilted corner-sharing TiO6 octahedra running parallel to the c axis, crosslinked by phosphate tetrahedra and in which one-half of octahedral cavities created are occupied by Ni atoms. Ti atoms are displaced from the center of octahedra units in alternating long (2.231) and short (1.703 Å) Ti–O bonds along chains.

scholarly journals Synthesis and crystal structure of dichlorido(1,10-phenanthroline-κ2N,N′)gold(III) hexafluoridophosphate

2017 ◽  
Vol 73 (7) ◽  
pp. 1048-1051 ◽  
Author(s):  
Raphael Enoque Ferraz de Paiva ◽  
Douglas Hideki Nakahata ◽  
Pedro Paulo Corbi
Keyword(s):  
Crystal Structure ◽  
Crystal Packing ◽  
Chloride Ions ◽  
Mass Spectrometric ◽  
Spectrometric Analysis ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Square Planar ◽  
Phenanthroline Ligand

A gold(III) salt of composition [AuCl2(C12H8N2)]PF6was prepared and characterized by elemental and mass spectrometric analysis (ESI(+)–QTOF–MS),1H nuclear magnetic resonance measurements and by single-crystal X-ray diffraction. The square-planar coordination sphere of AuIIIcomprises the bidentate 1,10-phenanthroline ligand and two chloride ions, with the AuIIIion only slightly shifted from the least-squares plane of the ligating atoms (r.m.s. = 0.018 Å). In contrast to two other previously reported AuIII-phenantroline structures that are stabilized by interactions involving the chlorido ligands, the packing of the title compound does not present these features. Instead, the hexafluoridophosphate counter-ion gives rise to anion...π interactions that are a crucial factor for the crystal packing.

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