The synthesis, and molecular and crystal structure of diphenyl(2-oxidonaphthylmethyl-iminoacetato)tin(IV)

1996 ◽  
Vol 74 (11) ◽  
pp. 2041-2047 ◽  
Author(s):  
Frank. E. Smith ◽  
Lian Ee Khoo ◽  
Ngoh Khang Goh ◽  
Rosemary C. Hynes ◽  
George Eng
Keyword(s):  
Crystal Structure ◽  
Elemental Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Intermolecular Contacts ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

The new diorganotin complex ((C6H5)2Sn(OC10H6CH=NCH2COO)) was prepared and characterized by 1H NMR, IR, elemental analysis, and a single crystal X-ray diffraction study. The crystals are monoclinic, space group P21/a with a = 16.9167(9) Å, b = 19.1276(16) Å, c = 26.538(2) Å, β = 100.534(6)°, V = 8442.5(11) Å3, Z = 16, and Dcalc = 1.574 Mg m−3. The final discrepancy factors are RF = 0.030, and RW = 0.021 for 6524 significant reflections. The tin atom has a distorted trigonal bipyramidal coordination, with no short intermolecular contacts. The two axial Sn—O bonds of 2.12 Å and 2.09 Å and the equatorial Sn—N bond of 2.14 Å are among the shortest found in related complexes. Key words: diorganotin(IV), bicycloazastannoxide, trigonal bipyramidal, antitumour.

Darstellung und Kristallstruktur von Zinkazid · 4-Methylpyridin / Preparation and Crystal Structure of Zinc Azide · 4-Methylpyridine

1988 ◽  
Vol 43 (3) ◽  
pp. 253-256 ◽  
Author(s):  
Franz A. Mautner ◽  
Harald Krischner ◽  
Christoph Kratky
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Single Crystal ◽  
Zinc Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

Zinc azide · 4-methylpyridine (1) is formed by the reaction of zinc azide with the corresponding pyridine in aqueous solution. The crystal structure was determined by single crystal X-ray diffraction methods. The crystals of 1 are monoclinic, space group C2/c, Z = 4, a = 1085.5(2), b = 1692.7(11), c = 619.7(6) pm, β = 113.47(5)°. Each zinc atom is surrounded by five nitrogen atoms (four from azide groups and one from the pyridine adduct) in a distorted trigonal bipyramidal fashion. The ZnN5-polyhedra share common edges to form chains along the crystallographic c-axis.

Simple Synthesis, Characterization and Structure of Diorganotin(IV) Complexes Containing the N-(2-Salicylidene)-N'-benzoylhydrazone Ligand

2003 ◽  
Vol 58 (4) ◽  
pp. 336-344 ◽  
Author(s):  
Dilip Kumar Dey ◽  
Brajagopal Samanta ◽  
Antonin Lycka ◽  
Lutz Dahlenburg
Keyword(s):  
Schiff Base ◽  
Nitrogen Atom ◽  
Elemental Analysis ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

Two diorganotin(IV) complexes of general formula R2Sn[2-OC6H4CH=NDN=C(O)Ph] (R = Ph, 1; R = Me, 2) have been synthesized from the corresponding diorganotin(IV) dichloride and the Schiff base derived from salicylaldehyde and benzoyl hydrazide. The two compounds have been characterized by elemental analysis, IR and NMR (1H, 13C, 15N, 119Sn) spectra, and their structures have been confirmed by single crystal X-ray structure analysis. Crystals of complex 1 re triclinic, space group P1̄ , a = 11.1631(5), b = 13.462(2), c = 16.511(1) Å , α = 106.193(9), β = 106.379(8), γ = 94.932(8)°, Z = 4, R1 = 0.0461, wR2 = 0.0939 for 13194 unique reflections. Crystals of 2 are monoclinic, space group P21, a = 10.2073(5), b = 14.645(2), c = 10.411(3) Å, β = 92.572(9)°, Z = 4, R1 = 0.0395, wR2 = 0.0835 for 5050 unique reflections. The central tin atom of either complex adopts a distorted trigonal bipyramidal coordination with two ligand oxygen atoms in axial positions, the nitrogen atom of the ligand and two organic groups on tin occupying equatorial sites. The δ(119Sn) values for the complexes 1 and 2 are -329.2 and -150.3, respectively, thus indicating penta-coordinated tin centres.

The synthesis and structural characterization of a series of pentacoordinate diorganotin(IV) N-arylidene-α-amino acid complexes

1992 ◽  
Vol 70 (4) ◽  
pp. 1114-1120 ◽  
Author(s):  
F. E. Smith ◽  
Rosemary C. Hynes ◽  
T. T. Ang ◽  
L. E. Khoo ◽  
G. Eng
Keyword(s):  
Molecular Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Intermolecular Contacts ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
C Nmr ◽  
Distorted Trigonal Bipyramidal

Eight new diorganotin complexes formulated as R2Sn(OArCR″=NCHR′COO) were prepared and characterized by 1H and 13 C NMR, IR, and elemental analysis. A single crystal X-ray diffraction study of the dibutyltin N-salicylidenevaline complex, Bu2Sn(OC6H4CH=NCH(i-Pr)COO), determines the molecular structure. The crystals are orthorhombic, space group P212121 with a = 9.187(2) Å, b = 10.003(2) Å, c = 23.482(4) Å, V = 2157.8(6) Å3, Z = 4, and Dc = 1.392 g cm−3. The final discrepancy factors are RF = 0.040, and Rw = 0.021 for 1131 significant reflections. The tin atom has a distorted trigonal bipyramidal coordination, with no short intermolecular contacts. The two axial Sn—O bonds of 2.078(10) and 2.151(8) Å and the equatorial Sn—N bond of 2.158(8) Å are among the shortest found in related complexes. The fact that the closest intermolecular Sn—O distance is 4.511(8) Å indicates a nonbridging carbonyl group.

scholarly journals Crystal structure refinement of magnesium zinc divanadate, MgZnV2O7, from powder X-ray diffraction data

2021 ◽  
Vol 77 (6) ◽  
pp. 588-591
Author(s):  
Stephanie J. Hong ◽  
Jun Li ◽  
Mas A. Subramanian
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Structure Refinement ◽  
Atomic Ratio ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Wyckoff Position ◽  
Distorted Trigonal Bipyramidal

The crystal structure of magnesium zinc divanadate, MgZnV2O7, was determined and refined from laboratory X-ray powder diffraction data. The title compound was synthesized by a solid-state reaction at 1023 K in air. The crystal structure is isotypic with Mn0.6Zn1.4V2O7 (C2/m; Z = 6) and is related to the crystal structure of thortveitite. The asymmetric unit contains two metal sites with statistically distributed magnesium and zinc atoms with the atomic ratio close to 1:1. One (Mg/Zn) metal site (M1) is located on Wyckoff position 8j and the other (M2) on 4h. Three V sites (all on 4i), and eight O (three 8j, four 4i, and one 2b) sites complete the asymmetric unit. The structure is an alternate stacking of V2O7 layers and (Mg/Zn) atom layers along [20\overline{1}]. It is distinct from other related structures in that each V2O7 layer consists of two groups: a V2O7 dimer and a V4O14 tetramer. Mixed-occupied M1 and M2 are coordinated by oxygen atoms in distorted trigonal bipyramidal and octahedral sites, respectively.

Synthesis and X-Ray Crystal Structure of Two Novel Ester Ferrocenophanes

2007 ◽  
Vol 62 (4) ◽  
pp. 605-609 ◽  
Author(s):  
Li Tao ◽  
Yang Bingqin ◽  
Gao Bo
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Elemental Analysis ◽  
3D Structure ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Carbonyl Chloride ◽  
Tof Ms

Two novel ester ferrocenophanes have been prepared by esterification of 1,1′-ferrocenedi(carbonyl chloride) with glycol and 1,4-butanediol, respectively. Both of them have been characterized by IR, elemental analysis, MALDI-TOF MS and 1H NMR spectroscopic methods, and their structures have been elucidated by X-ray diffraction. The intermolecular associations based on C-H···O hydrogen bonds have also been discussed. These molecules are assembled into chains, and the chains are further assembled into a 3D structure through several hydrogen bonds.

Crystal structure and solution studies of the product of the reaction of β-mercaptoethanol with vanadate

1999 ◽  
Vol 77 (12) ◽  
pp. 2088-2094 ◽  
Author(s):  
Sudeep Bhattacharyya ◽  
Raymond J Batchelor ◽  
Frederick WB Einstein ◽  
Alan S Tracey
Keyword(s):  
Crystal Structure ◽  
Mixed Solvent ◽  
Axial Position ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Solution Studies ◽  
Alkaline Conditions

Reaction of β-mercaptoethanol with vanadate under slightly alkaline conditions provided a crystalline complex that was characterized by X-ray diffraction and FTIR spectroscopy. The complex was dimeric in structure with a central [VO]2 core and a pentacoordinate, crudely trigonal bipyramidal arrangement about each vanadium atom with a sulphur occupying a pseudo-axial position. A single 51V NMR signal was observed for this complex when dissolved in water, chloroform or acetonitrile. A large influence of acetonitrile on the vanadium chemical shift suggested the possibility of reaction with acetonitrile. FTIR showed the presence of two complexes in acetonitrile solution but only one in chloroform or water. Mixed solvent studies were carried out in an effort to further characterize the solution complexes. Crystal structure of [{VO2(OC2H4S)}2][NEt4]2: monoclinic, space group P21/n,. a = 8.3451(17), b = 16.954(4), c = 10. 2064(25) Å; β = 101. 271(18)°; V = 1416.2 Å3; Z = 2; RF = 0.048 for 1355 data (Io 2..5σ (Io) and 147 variables.Key words: mercaptoethanol, vanadate, vanadium NMR, X-ray diffraction, FTIR, thiolate.

scholarly journals A New 3D Coordination Polymer of Bismuth with Nicotinic AcidN-Oxide

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Farzin Marandi ◽  
Ingo Pantenburg ◽  
Gerd Meyer
Keyword(s):  
Crystal Structure ◽  
Thermal Stability ◽  
Coordination Polymer ◽  
Three Dimensional ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Thermal Stability Of

The new three-dimensional coordination polymer {[Bi(NNO)2(NO3)]·1.5H2O}n(1, NNO−= nicotinateN-oxide) was synthesized and characterized by elemental analysis, IR and1H-NMR spectroscopy, as well as single-crystal X-ray diffraction analysis.1crystallizes in the monoclinic space group C2/c. The crystal structure consists of a rectangular-shaped grid constructed with NNO linkers. Cavities of a diameter of 7.9–8.3 Å2are filled with disordered water molecules. The thermal stability of the compound was evaluated by thermogravimetric analysis.

Synthesis and Crystal Structure of (1E,2E)-1,2-Di (-3-Nitrobenzylidene) Hydrazine under Micromave Irradiation

2013 ◽  
Vol 787 ◽  
pp. 205-207
Author(s):  
Hong Yan Zhou
Keyword(s):  
Crystal Structure ◽  
Microwave Irradiation ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
H Nmr ◽  
The Stability ◽  
High Yields

A compound of (1E,2E)-1,2-di (-3-nitrobenzylidene) hydrazine was synthesized under microwave irradiation (500 w), giving high yields of products (93%). Its structure was determined IR, 1H NMR, MS, elemental analysis and X-ray diffraction. The crystal of the compound is Monoclinic, space group P2(1)/n with a = 6.9611(18), b = 7.823(2), c = 12.999(3) Å, α = 90, β = 105.215(4), γ = 90o, V= 683.1(3) Å3, Z=4, Dc=1.450g/cm3,μ=0.110 mm-1, F(000)=308, R=0.0401 and wR = 0.1131 for 1273 observed reflection with I>2σ (I). π-π stacking interactions contribute to the stability of the structure.

Synthesis, Spectroscopic Studies, and Crystal Structure of Diethylchlorotin Dimethylphosphinate Et2ClSnO2PMe2

1998 ◽  
Vol 53 (7) ◽  
pp. 699-703 ◽  
Author(s):  
Abdel-Fattah Shihada ◽  
Frank Weller
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Studies ◽  
Chain Structure ◽  
Polymeric Chain ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Axis Of Symmetry ◽  
Ir Bands ◽  
Distorted Trigonal Bipyramidal

Abstract Diethylchlorotin dimethylphosphinate has been synthesized by treating (Et2ClSn)2O with HO2PMe2 in toluene. Single crystal X-ray analysis shows that O2PMe2 groups behave as bidentate bridge ligands between Et2ClSn units leading to a polymeric chain structure in which the tin atoms exhibit a distorted trigonal bipyramidal geometry with the oxygen atoms in the axial positions. The Sn-Cl bond lies on a C2 axis of symmetry in the (C2v) OCClSnCO unit. Et2ClSnO2PMe2 crystallizes in the monoclinic space group C2/c (a = 877.9 (2), b = 1907.8 (4), c = 695.5 (1) pm, β= 106.72 (2)°, Z = 4 and R = 0.043). The characteristic IR bands of Et2ClSnO2PMe2 are assigned and the mass spectrum is reported and discussed.

scholarly journals Synthesis and Structure Features of Tetraphenylantimony 2,3-Difluoro- and 2,3,4,5,6-Pentafluorobenzoate

2020 ◽  
Vol 12 (4) ◽  
pp. 51-62
Author(s):  
A. Efremov ◽  
Keyword(s):  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Cambridge Crystallographic Data Center ◽  
Redistribution Reaction ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
Distorted Trigonal Bipyramidal

Tetraphenylantimony 2,3-difluorobenzoate (1) and tetraphenylantimony 2,3,4,5,6-pentafluorobenzoate (2) was obtained by the interaction of pentaphenylantimony with 2,3-difluorobenzoic and 2,3,4,5,6-pentafluorobenzoic acids in benzene with a yield of up to 98 %. The compounds were also synthesized by the ligand redistribution reaction between pentaphenylantimony and triphenylantimony dicarboxylates. The compounds have been identified by IR spectroscopy and X-ray diffraction analysis. According to the X-ray diffraction data, the antimony atoms in compounds 1 and 2 have a distorted trigonal-bipyramidal coordination with the oxygen atom in axial positions. X-ray diffraction analysis was performed on a D8 QUEST diffractometer (Bruker). The crystallographic parameters of the unit cell of the compounds: 1 space group Р1 ̅, а = 9.857(5), b = 10.154(7), c = 14.362(11) Å, α = 83.74(4)°, β = 82.59(3), γ = 68.34(2)°, V = 1321.9(16) Å3, ρcalc = 1.475 g/cm3, Z = 2; 2 space group Р21/с, а = 16.186(9), b = 8.771(6), c = 20.413(13) Å, α = 90.00°, β = 113.073(17), γ = 90.00°, V = 2666(3) Å3, ρcalc = 1.597 g/cm3, Z = 4. The OSbO axial angles are slightly different and amount to 177.90(5)º in 1 and 179.00(5)º in 2. The sums of the CSbC equatorial angles are 356.89(9)º (1), 355.85(7)º (2). The Sb–Ceq distances in compounds 1 and 2 are 2.116(2), 2.119(2), 2.118(2) and 2.1073(17), 2.1158(18), 2.1152(19) Å respectively, which are significantly shorter than the Sb–Сax bond lengths (2.169(2) and 2.1617(19) Å). The organization of molecules in the crystals of compounds is due to hydrogen bonds and CHπ-interactions of the aryl and carboxyl ligands. The main difference between structures 1 and 2 is the different Sb–O bond lengths (2.2864(18) and 2.3168(18) Å), which is due to an increase in the electronegativity of the carboxyl ligand in 2, caused by the presence of five electronegative fluorine atoms in the benzoate substituent. Complete tables of atom coordinates, bond lengths and valence angles are deposited at the Cambridge Crystallographic Data Center (No. 1980908 (1); 1977189 (2); [email protected]; http://www.ccdc.cam.ac.uk/data_request/cif).

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