Structural Systematics of 2/4-Nitrophenoxide Complexes of Closed-Shell Metal Ions. III 2/4-Nitrophenoxides of Univalent Heavy Metals

1998 ◽  
Vol 51 (8) ◽  
pp. 735 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Raj Pal Sharma ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Room Temperature ◽  
Three Dimensional ◽  
Closed Shell ◽  
Two Dimensional ◽  
Nitrogen Base ◽  
Coinage Metal ◽  
Aromatic Carbon ◽  
X Ray ◽  
Dimensional Network ◽  
Oxygen Atoms

Room-temperature single-crystal X-ray studies are recorded for 2- and 4-nitrophenoxide salts of silver(I) and thallium(I), M(2-np) and Tl(4-np) (anhydrous), and Ag(4-np).H2O. Ag(2-np) is monoclinic, P21/c, a 9·012(4), b 5·743(5), c 12·594(5) Å, β 104·34(4)°, Z = 4; conventional R on |F| was 0·042 for No 1378 independent ‘observed’ (I > 3σ(I)) reflections. Tl(2-np) is monoclinic, C2/c, a 27·250(3), b 3·712(1), c 15·147(3) Å, β 114·41(1)°, Z = 8, R 0·025 for No 1346. Ag(4-np).H2O is monoclinic, P21/a, a 5·613(6), b 13·191(7), c 9·844(5) Å, β 92·50(6)°, Z = 4, R 0 ·033 for No 622. Tl(4-np) is tetragonal, I 41/a, a 18·037(8), c 8·979(8) Å, Z = 16, R 0·043 for No 924. An acid salt of the latter, Tl(4-np).(4-npH)3, triclinic, P-1, a 11·861(8), b 11·45(1), c 11· 423(1) Å, α 114·00(6), β 109·78(5), γ 96·87(7)°, Z = 2, R 0·042 for No 3814, is isomorphous with its rubidium analogue. These comprise a novel array of structures: although the structures of the silver(I) complexes are two-dimensional sheets with familiar head-tail connecting ligands, a strong silver-aromatic carbon interaction is found in Ag(2-np) (Ag–C 2·496(5) Å). Tl(2-np) and Tl(4-np) both present unusual forms related to the stair-polymer and cubane adducts found in 1 : 1 coinage metal(I)/halide-unidentate nitrogen base adducts; Tl(2-np) is a double-stranded stair-polymer array, with the phenoxide oxygen atoms incorporated in the stair and the nitro oxygen atoms linking successive thallium atoms. The structure of Tl(4-np) is based on a tetranuclear cubane motif of -4 symmetry, [Tl(O-phenoxide)]4, these being linked into a three-dimensional network by further Tl · · · O-nitro interactions from adjacent units. The structure of silver(I) picrate monohydrate, isomorphous with its sodium counterpart, is also recorded: monoclinic, C 2/m, a 12·818(7), b 20·208(8), c 3· 741(1) Å, β 88·25(3)°, Z = 4, R 0·047 for No 1042, void of any significant Ag · · · C contacts.

scholarly journals Synthesis, X-Ray Structure, and Characterization of a Complex Containing the Hexakis(urea)cobalt(II) Cation and Lattice Urea Molecules

2007 ◽  
Vol 2007 ◽  
pp. 1-7 ◽  
Author(s):  
Labrini Drakopoulou ◽  
Constantina Papatriantafyllopoulou ◽  
Aris Terzis ◽  
Spyros P. Perlepes ◽  
Evy Manessi-Zoupa ◽  
...  
Keyword(s):  
Room Temperature ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
X Ray ◽  
Lattice Constants ◽  
Dimensional Network ◽  
Different Types ◽  
Hydrogen Bonded

The 12: 1 reaction of urea (U) with CoI2in EtOH yielded the “clathrate-coordination” compound[CoU6]I2·4U (1). The complex crystallizes in the monoclinic space group P21/c. The lattice constants area= 9.844(4),b= 7.268(3),c= 24.12(1) Å, andβ=98.12(1)∘. The crystal structure determination demonstrates the existence of octahedral[CoU6]2+cations,I-counterions, and two different types (twoU1and twoU2) of hydrogen-bonded, lattice urea molecules. The[CoU6]2+cations and theU1lattice molecules form two-dimensional hydrogen-bonded layers which are parallel to theabplane. TheI-anions are placed above and below each layer, and are hydrogen bonded both toU1molecules and[CoU6]2+cations. EachU2molecule is connected to a[CoU6]2+cation through anN–H⋯Ohydrogen bond resulting in a three-dimensional network. Room temperature magnetic susceptibility and spectroscopic (solid-state UV/Vis, IR, Raman) data of1are discussed in terms of the nature of bonding and the known structure.

Syntheses, Structures and Photoluminescent Properties of the Two Novel Coordination Polymers [Cd(pydc)2(tu)]n and [Cd2(SO4)(nic)2(tu)1.5(H2O)2]n (pydc = Pyridine-2,3-dicarboxylate, nic = Nicotinate, tu = Thiourea)

2011 ◽  
Vol 66 (5) ◽  
pp. 459-464 ◽  
Author(s):  
Chao Xu ◽  
Sheng-Bo Liu ◽  
Taike Duan ◽  
Qun Chen ◽  
Qian-Feng Zhang
Keyword(s):  
Hydrogen Bonds ◽  
Coordination Polymers ◽  
Room Temperature ◽  
Three Dimensional ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
One Dimensional ◽  
X Ray ◽  
Dimensional Network

Two novel cadmium coordination polymers, [Cd(pydc)2(tu)]n (1) and [Cd2(SO4)(nic)2(tu)1.5 - (H2O)2]n (2) (pydc = pyridine-2,3-dicarboxylate, nic = nicotinate, tu = thiourea), have been synthesized under hydrothermal conditions and structurally characterized by X-ray diffraction analysis. 1 is a one-dimensional ladder coordination polymer in a two-dimensional network formed by hydrogen bonds. 2 consists of two kinds of Cd(II) centers in different coordination environments connected via nicotinate and sulfate to form a two-dimensional grid network integrated in a three-dimensional framework generated by hydrogen bonds. 2 shows intense fluorescent emission in the solid state at room temperature

Crystal and Molecular Structure of 3-Iodo-2-propynyl-N-butylcarbamate

1997 ◽  
Vol 52 (2) ◽  
pp. 256-258 ◽  
Author(s):  
Evgeni V. Avtomonov ◽  
Rainer Grüning ◽  
Jörg Lorberth
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Carbamate Group ◽  
Oxygen Atoms

Abstract The crystal structure of the title compound has been determined by X-ray diffraction methods. Due to the Lewis acidic character of the iodine substituent a “zig-zag” chain is formed via intermolecular interactions (2.933(4) A) between iodine and oxygen atoms of theocarbamate moiety. A three-dimensional network is formed through hydrogen-bridging (2.04 A) between NH-groups and the oxygen atoms of the neighbouring carbamate group of the next molecule.

Structural Systematics of 2/4-Nitrophenoxide Complexes of Closed-Shell Metal Ions. VII Acid Salts of the 4-Nitrophenoxides of Group 2

1998 ◽  
Vol 51 (8) ◽  
pp. 785 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Raj Pal Sharma ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Room Temperature ◽  
Calcium Salt ◽  
Three Dimensional ◽  
Closed Shell ◽  
The Other ◽  
X Ray ◽  
C 23 ◽  
Structure Determinations ◽  
Group 2 ◽  
Acid Salts

Room-temperature single-crystal X-ray structure determinations are recorded for a number of Group 2 4-nitrophenoxide acid salts, variously hydrated M(4-np)2.x(4-npH).yH2O. Ca(4-np)2.2(4-npH).8H2O is monoclinic, P 21/n, a 30·52(1), b 10·027(1), c 23·65(2) Å, β 116·3(5)°, Z = 8, conventional R on |F| being 0·058 for No 5092 independent ‘observed’ (I > 3s(I)) reflections. Sr(4-np)2.2(4-npH).8H2O, based on a subcell of the former, is monoclinic, P 21/c, a 15·576(5), b10·081(6), c 24·20(2) Å, β 117·99(5)° , Z = 4, R 0·054 for No 2908. Ba(4-np)2.2(4-npH).4H2O is orthorhombic, Fdd2, a 28·01(1), b 19·90(1), c 10·692(7)Å, Z = 8, R 0·028 for No 1967. The strontium array (and that of the calcium salt developed from it) may be represented as [(H2O)6Sr(4-npH.4-np)] (4-npH.4-np), a neutral ligand being unsymmetrically chelated to the strontium through the nitro group, with a quasi-parallel counter ion hydrogen-bonded to it by phenoxide confrontation. The other two 4-np residues make up a similar phenoxide-confronting pair (4-npH.4-np), the hydrogen being more intimately associated with one moiety. The barium salt is also an interesting array: the 10-coordinate barium lies on a crystallographic 2 axis, in an environment of two pairs of symmetry-related nitro-chelating ligand anions, and a pair of nitro-O coordinating neutral 4-npH ligands; the whole [(H2O)4Ba(4-np)2(4-npH)2] array may be envisaged as a single neutral (super)molecule. Hydrogen bonds between confronting phenoxides of the neutral 4-npH components of the parent and the 4-np- components of neighbouring molecules link the whole into a three-dimensional array.

scholarly journals Münzmetall-Lanthanid-Chalkogenide: II. Kupfer(I)-Lanthanid(III)- Sulfide der Zusammensetzung CuMS2 (M = Dy – Lu) im orthorhombischen B-Typ / Coinage Metal Lanthanide Chalcogenides: II. Copper(I) Lanthanide(III) Sulfides of the Composition CuMS2 (M = Dy – Lu) with the Orthorhombic B-Type Structure

2007 ◽  
Vol 62 (1) ◽  
pp. 15-22 ◽  
Author(s):  
Sabine Strobel ◽  
Thomas Schleid
Keyword(s):  
Three Dimensional ◽  
Charge Compensation ◽  
Molar Ratio ◽  
Single Crystal Diffraction ◽  
Coinage Metal ◽  
X Ray ◽  
Dimensional Network ◽  
Elemental Copper ◽  
Lanthanide Metal ◽  
Type Crystal

Single crystals of the ternary copper(I) lanthanide(III) sulfides with the composition CuMS2 (M = Dy - Lu) are formed within seven days at 750 °C by oxidation of elemental copper and lanthanide metal with sulfur (molar ratio: 1 : 1 : 2, evacuated silica tubes) in equimolar quantities of CsCl, CsBr or CsI as fluxing agents. The CuYS2-type crystal structures (orthorhombic, Pnma, Z = 4; e. g. CuDyS2: a = 1342.51(9), b = 397.96(3), c = 627.43(5) pm and CuLuS2: a = 1315.06(9), b = 391.04(3), c = 624.18(5) pm) exhibit chains of cis edge-linked [CuS4]7− tetrahedra with the composition 1∞{[Cu(S1)3/3(S2)1/1]3−} which run parallel to [010] and show hexagonal rod packing. Charge compensation and three-dimensional interconnection of these anionic strands occur via octahedrally coordinated M3+ cations surrounded by six S2− anions. These [MS6]9− octahedra share vertices and edges to form a three-dimensional network 3∞{[M(S1)3/3(S2)3/3]−} with the ramsdellite-type topology of γ-MnO2. The metal sulfur distances within the [MS6] polyhedra are very similar (M-S: 263 - 279 pm), whereas those within the [CuS4] units cover the ranges 227 - 230 (Cu-S2) and 231 - 233 (Cu-S1) as well as 250 - 252 pm (Cu-S1′, 2×). The present work is the first comprehensive X-ray single crystal diffraction study of the complete isotypic B-type series CuMS2 (M = Dy - Lu).

Poly[[μ-(1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonato)]sodium]: a powder X-ray diffraction study

2013 ◽  
Vol 69 (8) ◽  
pp. 815-818 ◽  
Author(s):  
Mwaffak Rukiah ◽  
Thaer Assaad
Keyword(s):  
Hydrogen Bonding ◽  
Rietveld Method ◽  
Three Dimensional ◽  
Coordination Geometry ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

The title two-dimensional coordination polymer, [Na(C2H8NO6P2)]n, was characterized using powder X-ray diffraction data and its structure refined using the Rietveld method. The asymmetric unit contains one Na+cation and one (1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonate) anion. The central Na+cation exhibits distorted octahedral coordination geometry involving two deprotonated O atoms, two hydroxy O atoms and two double-bonded O atoms of the bisphosphonate anion. Pairs of sodium-centred octahedra share edges and the pairs are in turn connected to each other by the biphosphonate anion to form a two-dimensional network parallel to the (001) plane. The polymeric layers are connected by strong O—H...O hydrogen bonding between the hydroxy group and one of the free O atoms of the bisphosphonate anion to generate a three-dimensional network. Further stabilization of the crystal structure is achived by N—H...O and O—H...O hydrogen bonding.<!?tpb=18.7pt>

Structural Systematics of 2/4-Nitrophenoxide Complexes of Closed-Shell Metal Ions. I 2-Nitrophenoxides of Group 1

1998 ◽  
Vol 51 (8) ◽  
pp. 707 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Raj Pal Sharma ◽  
Todd M. Shand ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Room Temperature ◽  
Closed Shell ◽  
Aromatic Rings ◽  
X Ray ◽  
Metal Atoms ◽  
Metal Derivatives ◽  
Derivatives Of ◽  
Fourth Coordination ◽  
Group 1 ◽  
Oxygen Atoms

Room-temperature, single-crystal X-ray studies are recorded for the variously hydrated Group 1 metal derivatives of 2-nitrophenol (2-npH = C6H5NO3). A provisional determination is reported for Li(2-np).½H2O, set as monoclinic, P21/c, a 3·535(3), b 15·06(1), c 24·42(2) Å, β 91·7(1)°, Z = 8, conventional R on F currently 0·18 for No 875 ‘observed’ (I > 3σ(I)) reflections. Na(2-np).H2O is monoclinic, C2/c, a 34 ·23(2), b 3·624(4), c 35·48(2) Å, β 91·24(4)°, Z = 24, R 0·060 for No 1371. Rb(2-np).½ H2O is monoclinic, C2/c (isomorphous with the previously determined potassium analogue), a 25·269(9), b 5·381(5), c 12·010(3) Å, β 105·35(3)°, Z = 8, R 0·046 for No 1380. Cs(2-np).½H2O is monoclinic, P21/n, a 7·648(3), b 26·19(1), c 8·713(6) Å, β 111·75(2)°, Z = 8, R 0·061 for No 2347. All compounds except the lithium derivative are two-dimensional polymeric sheets in which the aromatic rings project to either side of a core of metal atoms coordinated by a web of 2-nitrophenoxide oxygen atoms in various bridging functionalities. The lithium compound is a novel ‘stair’ polymer with two crystallographically independent lithium atoms at successive independent Li–O crossbars, the oxygen atoms of which are phenoxide-Oof each of the two independent ligands. The lithium atoms are alternately four- and five-coordinate, the fourth coordination site of the first being occupied by the water molecule oxygen atom, while the fourth and fifth sites of the second are occupied by the cis-2-nitro oxygen atoms of the two ligands

Tetrabutylammonium Salts of 2-Nitropropane, Cyclopentadiene and 9-Ethylfluorene: Crystal Structures and Use in Anionic Polymerization

1995 ◽  
Vol 50 (3) ◽  
pp. 415-422 ◽  
Author(s):  
Manfred T. Reetz ◽  
Stephan Hütte ◽  
Richard Goddard
Keyword(s):  
Anionic Polymerization ◽  
Room Temperature ◽  
Ion Pairs ◽  
Three Dimensional ◽  
Star Polymers ◽  
X Ray ◽  
Dimensional Network ◽  
Acidic Compounds ◽  
Cyclopentadienyl Anion ◽  
Special Case

Reaction of the CH-acidic compounds 2-nitropropane, cyclopentadiene and 9-ethylfluorene with HON (nBu)4 affords the corresponding tetrabutylammonium salts in crystalline form, which have been characterized by X -ray structure analysis. The nitrostabilized salt is not a “naked ” anion (real carbanion). Rather, the α-methylene entities of the N+(nBu)4 cations form relatively strong hydrogen bonds with the O -atom s of the nitronateanion, forming dimers in a three-dimensional network. In solution dimers in the form of supramolecular ion pairs exist. In contrast, the cyclopentadienyl anion appears to be a real carbanion, since anion and cation do not interact with one another via H -bonding. The structure of the N+(nBu)4 salt of the 9-ethylfluorenyl anion is a special case in that closer contacts between cation and anion occur, which may be indicative of unusual [CH ··· C]- bonding. All three salts function as initiators in the metal-free anionic polymerization of acrylates and methacrylates at room temperature. In the case of tetrabutylammoniumcyclopentadienide, star polymers are formed.

Ni(C2(COO)2)(H2O)4 · 2 H2O und Ni(C2(COO)2)(H2O)2: zwei Koordinationspolymere mit dem Acetylendicarboxylat-Dianion / Ni(C2(COO)2)(H2O)4 · 2 H2O and Ni(C2 (COO)2)(H2O)2: Two Co-ordination Polymers of the Acetylenedicarboxylate Dianion

2002 ◽  
Vol 57 (12) ◽  
pp. 1375-1381 ◽  
Author(s):  
Frauke Hohn ◽  
Heinrich Billetter ◽  
Ingo Pantenburg ◽  
Uwe Ruschewitz
Keyword(s):  
Room Temperature ◽  
Three Dimensional ◽  
Water Molecules ◽  
State Structure ◽  
Slow Evaporation ◽  
Thermoanalytical Investigations ◽  
Dimensional Network ◽  
Carboxylate Anions ◽  
Acetylenedicarboxylic Acid ◽  
Oxygen Atoms

From a solution of Ni(CH3COO)2 ∙ 4 H2O and acetylenedicarboxylic acid in deionized water single crystals of Ni(C2(COO)2)(H2O)4 ∙ 2 H2O(P21/a, Z = 2, isotypic to Co(C2(COO)2)(H2O)4 ∙ 2 H2O) were obtained by slow evaporation of the solvent. In the solid state structure nickel is octahedrally surrounded by four water molecules and two oxygen atoms of the carboxylate anions. These octahedra are connected to chains by the dicarboxylates. Heating the hexahydrate to 100 °C in a stream of argon leads to Ni(C2(COO)2)(H2O)2 (C2/c, Z = 4, isotypic to Mn[C2(COO)2] ∙ 2 H2O). Here, the NiO6 octahedron is built by two water molecules and four oxygen atoms of the dicarboxylate ligands, which connect the Ni octahedra to a three-dimensional network. Thermoanalytical investigations show another mass loss at about 200 °C, which leads to non-crystalline products. Finally, at about 400 °C NiO is formed. Measurements of the magnetic susceptibilities result in the expected behaviour for Ni2+ in an octahedral co-ordination (3A2 ground state). The effective magnetic moment at room temperature is μeff = 3.20 μB.

Synthese, Kristallstruktur und Eigenschaften von 1,1,3,3,3-Pentaamino-1-oxo- 1λ5 ,3λ5-diphosphaz-2-en, (NH2)2(O)P-N=P(NH2)3 / Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaamino-1-oxo-1λ5, 3λ5-diphosphaz-2-ene, (NH2)2(O)P-N=P(NH2)3

1996 ◽  
Vol 51 (8) ◽  
pp. 1079-1083 ◽  
Author(s):  
N. Stock ◽  
W. Schnick
Keyword(s):  
Crystal Structure ◽  
Thermal Properties ◽  
Room Temperature ◽  
Three Dimensional ◽  
Intermolecular Hydrogen Bonding ◽  
Structure And Properties ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Dimensional Network ◽  
Ray Methods

Coarse crystalline (NH2)2(O)P-N=P(NH2)3 is obtained from a NH3 saturated CH2Cl2 suspension of (NH2)2(O)P-N=P(NH2)3 NH4Cl at room temperature. (NH2)2(O)P-N=P(NH2)3·NH4Cl is synthesized by slow addition of Cl2(O)P-N=PCl3 to a solution of NH3 in CH2Cl2 at -78 °C. Excess NH4Cl is removed by treatment with HNEt2 followed by extraction with CH2Cl2. The crystal structure of (NH2)2(O)P-N=P(NH2)3 has been determined by single crystal X-ray methods (P21/c; a = 1462.8(3), b = 944.8(2), c = 1026.9(2) pm, β = 110.69(3)°; Z = 8). In the unit cell there are two crystallographically unique molecules. They form a three dimensional network by intermolecular hydrogen bonding interactions (N-H···N ≥ 313 pm. N-H···O ≥ 293 pm). The investigation of the thermal properties shows decomposition with evolution of NH3 above 80 °C.

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