Synthesis and structures of diaryloxystannylenes and -plumbylenes embedded in 1,3-diethers of thiacalix[4]arene

2020 ◽  
Vol 49 (35) ◽  
pp. 12234-12241
Author(s):  
Ryunosuke Kuriki ◽  
Takuya Kuwabara ◽  
Youichi Ishii
Keyword(s):  
Phenolic Oxygen ◽  
Oxygen Atoms

Monomeric stannylenes and plumbylenes embedded in 1,3-diethers of thiacalix[4]arene, whose structures are highly dependent on the substituents on the phenolic oxygen atoms, have been synthesized.

Structural Systematics of 2/4-Nitrophenoxide Complexes of Closed-Shell Metal Ions. VI 4-Nitrophenoxides of Group 2

1998 ◽  
Vol 51 (8) ◽  
pp. 775 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Raj Pal Sharma ◽  
Brian W. Skelton ◽  
Paloth Venugopalam ◽  
Allan H. White
Keyword(s):  
Metal Ions ◽  
Closed Shell ◽  
Water Molecules ◽  
One Dimensional ◽  
Phenolic Oxygen ◽  
C 23 ◽  
Structure Determinations ◽  
Group 2 ◽  
Coordinated Water ◽  
Oxygen Atoms

Room-temperature single-crystal X-ray structure determinations are recorded for 4-nitrophenolate (4-np-) salts of Group 2 metal ions, variously hydrated, M(4-np)2.xH2O, M = Mg, Ca, Sr, Ba. Mg(4-np)2.8H2 O is monoclinic, P21/c, a 12·402(3), b 6·673(7), c 11·833(6) Å, β 93·70(3)°, Z = 2; conventional R on |F| was 0·041 for No 1995 independent ‘observed’ (I > 3σ(I)) reflections. Ca(4-np)2.4H2O is monoclinic, P21/c, a 13·109(8), b 3·644(1), c 21·181(8) Å, β 125·55(3)°, Z= 2, R 0·050 for No 1371. Sr(4-np)2.8H2O is monoclinic, P21/n, a 7·934(1), b 10·658(1), c 23·602(2) Å, β 91·36(1)°, Z = 4, R 0·038 for No 2050. Ba(4-np)2.8H2O is monoclinic P21/c, a 15·990(8), b 6·337(3), c 25·634(8) Å, β 126·1(3)°, Z = 4, R 0·021 for No 3115. The magnesium salt is ionic with [Mg(OH2)6]2+ cations and interleaved anion stacks up b. The calcium salt is a one-dimensional polymer with ... Ca(µ-O)2Ca(µ-O)2Ca ... spine, the bridges being phenolic oxygen atoms.trans-Coordinated water molecules make up six-coordination about the calcium, the anion planes stacking at the b spacing. The strontium adduct is also a one-dimensional polymer with a similar spine, but with water molecule oxygen atoms bridging, the nine-coordinate strontium environment being made up by a chelating nitro group and three unidentate water molecules. Coordinated anions stacked up a are interleaved by free anions. The barium salt is simply [Ba(4-np)(OH2)8]+ (4-np-), the ligand anion (semi)chelated through the nitro pair of oxygen atoms, again with interleaving anion/ligand stacking.

The Crystal and Molecular Structure of Bis-[μ-2-(p-nitrophenyliminomethyl)phenolato-N,O]-bis(ethanol)bis(nitrato-O,O')dinickel(II), [Ni(slno)NO3(C2H5OH)]2, a Binuclear Ferromagnetic Salicylaldimine Derivative of Nickel Nitrate

1979 ◽  
Vol 32 (2) ◽  
pp. 331 ◽  
Author(s):  
RJ Butcher ◽  
E Sinn
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Nickel Atom ◽  
Nickel Nitrate ◽  
Distorted Octahedral Geometry ◽  
Tetrahedral Geometry ◽  
Imine Group ◽  
Phenolic Oxygen ◽  
Distorted Octahedral ◽  
Oxygen Atoms

The crystal and molecular structure of the complex bis-[μ-2-(p-nitrophenyliminomethyl)phenolato- N,O]-bis(ethanol)bis(nitrato-O,O')dinickel(11) and its magnetic properties are reported. Crystal data: space group PI, Z 1, a 8.882(2), b 9.332(3), c 12.533(4) �, α 94.40(2),B 109.99(2), γ 111.61(2)�, U 883 �3, R 2.8%, Rw 3.3% for 2154 reflections. The compound is prepared from the reaction of bis(N-p-nitrophenylsalicylaldimine)nickel(II) with nickel nitrate in hot triethoxymethane, and on cooling the solution deposited pale green transparent crystals. The structure contains neutral dimeric units with bridging through the phenolic oxygen atoms and has distorted octahedral geometry about each crystallographically identical nickel atom. The six donor atoms are made up of two oxygen atoms from the bidentate nitrate, oxygen from ethanol, nitrogen from the imine group and two bridging phenolic oxygen atoms. The Ni2O2 group is strictly planar possessing a crystallographic centre of symmetry. The angles subtended at the bridging oxygen atoms indicate a tetrahedral geometry and it is demonstrated that this is important in explaining the ferromagnetic intradimer interaction. The presence of hydrogen bonding between the ethanol hydrogen and the nitrate group of an adjacent molecule appears to be an important stabilizing factor in determining the structure and provides a possible pathway for the antiferromagnetic interdimer exchange interaction.

The structure of ferroverdin II. Rhombohedral ferroverdin crystals

1973 ◽  
Vol 184 (1075) ◽  
pp. 137-148 ◽  
Keyword(s):  
Carbon Tetrachloride ◽  
Sodium Ion ◽  
Double Layers ◽  
Sodium Ions ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
Data Space ◽  
Phenolic Oxygen ◽  
Disordered Carbon ◽  
Oxygen Atoms

Ferroverdin, a green iron containing natural product, crystallizes in rhombohedral crystals which have the following composition Crystal data: Space group R 3̄ c ; a = 16.06; c = 88.78; ρ calc = 1.446 for, as asymmetric unit, Fe/3.Na/3.C 15 H 10 NO 4 .CCl 4 .CH 3 OH, M , 480. R = 16% on Weissenberg photographic data, eye estimated intensities. The iron nitrosophenyl complexes are linked together by sodium ions in double layers; each sodium ion contacts three carboxy oxygen atoms and three methanol oxygen atoms and the methanoloxygen atoms are hydrogen bonded to the phenolic oxygen atoms. The layers are stacked to enclose large cavities in each of which are sited six, partly disordered, carbon tetrachloride molecules.

A dinuclear molybdenum(VI) complex with a triaminoguanidine ligand: synthesis and structure of [Mo2O4(OH2)(DMF)(HtBu6L)]·3DMF ([H6tBu6L]Cl=tris(3,5-di-tert-butyl-2-hydroxybenzylidene)-triaminoguanidinium chloride)

2018 ◽  
Vol 73 (5) ◽  
pp. 323-327
Author(s):  
Si-Meng Wu ◽  
Xin Chen ◽  
Zhifeng Xin ◽  
Ai-Quan Jia ◽  
Qian-Feng Zhang
Keyword(s):  
Azomethine Nitrogen ◽  
Tert Butyl ◽  
Coordination Sites ◽  
Phenolic Oxygen ◽  
Ligand Synthesis ◽  
Solvent Molecules ◽  
Oxygen Atoms

AbstractInteraction of (NH4)6Mo7O24·4H2O with tris-(3,5-di-tert-butyl-2-hydroxy-benzylidene)triaminoguanidinium chloride [H6tBu6L]Cl in DMF-H2O resulted in isolation of a neutral dinuclear Mo(VI) complex [Mo2O4(OH2)(DMF)(HtBu6L)]·3DMF. The C3-symmetric-type ligand HtBu6L is coordinated to two cis-{MoO2}2+ moieties via phenolic-oxygen, guanidine nitrogen and azomethine nitrogen atoms, and the remaining sixth coordination sites of the molybdenum centers are occupied by the oxygen atoms from the solvent molecules.

The structure of ferroverdin I. Monoclinic ferroverdin crystals

1973 ◽  
Vol 184 (1075) ◽  
pp. 121-135 ◽  
Keyword(s):  
Double Bond ◽  
Iron Atom ◽  
Sodium Ion ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
Double Bond Character ◽  
X Ray ◽  
Phenolic Oxygen ◽  
Bond Character ◽  
Oxygen Atoms

X-ray crystallographic measurements on monoclinic crystals show that ferroverdin should be formulated The iron atom is attached to three nitrosophenylligands, cis to each other, through the phenolic oxygen and nitrogen atoms. The sodium ion is surrounded by three phenolic oxygen atoms associated with one iron atom, two oxygen atoms from two other ferroverdin molecules and one from solvent acetone. The crystal data are: space group, C2/ c ; a = 38.88 Å (1Å = 0.1 nm), b = 13.60 Å, c = 18.44 Å, β = 96° 41'; density 1.43 g/cm 3 ; M , asymmetric unit, 1042; M , calculated for Fe.Na.C 45 H 30 N 3 O 12 .2 (CH 3 ) 2 CO 1000. R = 11% on diffractometer data. The distance Fe—N, average 1.83 Å, is short suggesting some double bond character.

Amine and Imine Nitrogen Atoms of a New Schiff Base Type Ligand Simultaneously Coordinated to a Dinuclear Mn2O2 Core

2003 ◽  
Vol 58 (11) ◽  
pp. 1087-1090 ◽  
Author(s):  
Won K. Seoka ◽  
Konstantin Karaghiosoff ◽  
Thomas M. Klapötkeb ◽  
Peter Mayer
Keyword(s):  
Schiff Base ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Coordination Environment ◽  
Space Group ◽  
Imine Nitrogen ◽  
Phenolic Oxygen ◽  
Centrosymmetric Structure ◽  
Oxygen Atoms

Abstract The dinuclear Mn(IV) complex [Mn(C-X-salpn)(μ-O)]2·Me2CO (H2salpn=N,N’-bis(salicylidene)- 1,3-diaminopropane and X = CH2C(=O)CH3) crystallizes in the monoclinic space group C2/c with a = 27.388(6), b = 10.388(2), c = 19.797(4) Å , β = 133.11(3)°, V = 4111(1) Å3 and Z = 4. It contains a new Schiff base type ligand, which is related to salpn by the addition of acetone to one of the two C=N moieties. Main feature of the centrosymmetric structure is a planar Mn2O2 four-membered ring. The coordination environment of the manganese atoms is roughly octahedral comprising two phenolic oxygen atoms as well as two amine and two imine nitrogen atoms of the ligand. The Mn···Mn distance is 2.740(8) Å and the Mn-O-Mn bridging angle amounts to 97.2(1)°.

Structural Studies of the Alkali Metal Picrates

1995 ◽  
Vol 48 (7) ◽  
pp. 1311 ◽  
Author(s):  
JM Harrowfield ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Alkali Metal ◽  
Sodium Salt ◽  
The Other ◽  
Two Dimensional ◽  
Phenolic Oxygen ◽  
Metal Atoms ◽  
Group Oxygen ◽  
The One ◽  
Potassium Picrate ◽  
Oxygen Atoms

A comparative series of room-temperature, single-crystal X-ray studies of the alkali metal (and ammonium) picrate structures is presented, all being in some sense revisitations of earlier work of various vintages, except for that of the sodium salt. Lithium picrate monohydrate is triclinic, Pī, a 10.710(6), b 7.186(1), c 7.112(1) Ǻ, α 65.89(1), β 71.90(3), γ 84.45(2)°, Z = 2 f.u.; conventional R on |F| was 0.053 for No = 1792 'observed' (I > 3σ(I)) reflections. Sodium picrate monohydrate is monoclinic, C 2/m, a 13.074(6), b 20.080(6), c 3.690(3) Ǻ, β 90.67(3)°, Z = 4 f.u.; R was 0.056 for No 519. Potassium picrate (anhydrous) is orthorhombic, Ibca , a 13.316(3), b 19.107(5), c 7.138(2) Ǻ, Z = 8 f.u ., R 0.036 for No 1308; the ammonium salt is isomorphous, a 13.474(4), b 19.790(7), c 7.131 (4) Ǻ, R 0.040 for No 981. Rubidium picrate (anhydrous) is monoclinic, P 21/c, a 10.604(1), b 4.556(3), c 19.183(2) Ǻ, β 101.41(1)°, Z = 4 f.u ., R 0.039 for No 1878; the caesium salt is isomorphous, a 10.810(1), b 4.700(1), c 19.400(3) Ǻ, β 101.43(1)°, R 0.027 for No 2177. The lithium salt is binuclear, the phenolic oxygen atoms bridging the five-coordinate lithium atoms, while the sodium salt is a two-dimensional polymer parallel to the ab plane, the picrates cross-linking one-dimensional arrays of sodium atoms of two types, one eight-coordinate and linked by bridging phenolic oxygen atoms, and the other six-coordinate and linked by water molecules. The potassium and ammonium salts are also two-dimensional polymers parallel to the ab planes, linked in the second dimension by pairs of picrates opposed in polarity and linking the eight-coordinate potassium atoms by phenolic oxygen atoms on the one hand, and the 4-nitro group oxygen atoms on the other. The rubidium and caesium salts are two-dimensional polymers in the ac plane, eight-coordinate metal atoms being linked by a complex web of picrate groups; unlike the other compounds, they do not contain bridging phenolic oxygen atoms.

Silver and Thallium Ion Complexation with Allyloxycalix[4]arenes

1999 ◽  
Vol 52 (3) ◽  
pp. 227 ◽  
Author(s):  
Daniel Couton ◽  
Mauro Mocerino ◽  
Chris Rapley ◽  
Chitoshi Kitamura ◽  
Akio Yoneda ◽  
...  
Keyword(s):  
Solvent Extraction ◽  
Functional Groups ◽  
Cation Binding ◽  
Cone Conformation ◽  
Conformational Rigidity ◽  
Phenolic Oxygen ◽  
Ion Complexation ◽  
Oxygen Atoms

A series of six calix[4]arene derivatives bearing allyl groups and/or benzyl groups functionalized at the phenolic oxygen atoms were synthesized and their cation-binding abilities for silver(I) and thallium(I) ions were evaluated through solvent extraction experiments. The results showed that both silver(I) and thallium(I) picrates were readily extracted by the tetrasubstituted p-t-butylcalixarene derivatives, while no extraction of sodium or potassium picrates was observed. The high extractability of thallium(I) picrate by these ligands was independent of the functional groups present, but the extraction of silver picrate seemed to be dependent on the conformational rigidity of the calixarene; those locked into the cone conformation showed the highest extractability for silver picrate.

Crystal Structure and Magnetic Properties of a Linear Trinuclear Ni(II) Complex

2001 ◽  
Vol 56 (1) ◽  
pp. 43-48 ◽  
Author(s):  
E. Kavlakoglu ◽  
A. Eimali ◽  
Y. Elerman ◽  
R. Werner ◽  
I. Svoboda ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Exchange Interactions ◽  
Trinuclear Complex ◽  
Antiferromagnetic Coupling ◽  
Temperature Dependent ◽  
Nickel Ion ◽  
Phenolic Oxygen ◽  
Characteristic Maximum ◽  
L 13 ◽  
Oxygen Atoms

Abstract Linear Trinuclear Nickel(II) Complex, Super-Exchange Interactions, Antiferromagnetic Coupling [Ni3(C2H32(CH3O)2L2] [L = 13-bis(5-chlorosalicylideneamino)propan-2-ol dianion, (C2H3O2)- = acetate, (CH3OH) = methanol] was synthesized and its crystal structure was determined. It crystallizes in the monoclinic spaceeroup P21 /n with a = 12.694(2), b = 13.281 (4), c = 15.420(3) Å, β = 111.25(2)°, V = 2422.9(9) Å3 ,Z = 2 . The molecule is a "linear" trinuclear complex with nearly octahedral coordination of each nickel ion. Adjacent nickel(II) ions are bridged by the phenolic oxygen atoms of the ligands and the oxygen atoms of the acetato ligands. The coordination sphere of the terminal nickel(II) ions is completed by the oxygen atom of the methanol. Adjacent nickel(II) centers are separated by 3.043(1) Å and weakly antiferromagnetically coupled (J1 = -3 .4 cm-1). The terminal nickel(II) centers are separated by 6.086(1) Å and very weakly antiferromagnetically coupled (J2 = -0 .3 cm-1) which follows from temperature-dependent magnetic susceptibility measurements in the temperature range 4.5 to 318 K. The magnetic moment rises from 2.99 μB at 4.5 K to 5.42 μB at 318 K. In the X(T) curve no characteristic maximum was observed.

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