Synthesis and characterization of organometallic hydro-tris-pyrazolylborate derivatives of scandium via alkane elimination

1997 ◽  
Vol 75 (6) ◽  
pp. 702-711 ◽  
Author(s):  
James Blackwell ◽  
Corinne Lehr ◽  
Yimin Sun ◽  
Warren E. Piers ◽  
Susan D. Pearce-Batchilder ◽  
...  
Keyword(s):  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
H Nmr ◽  
Alkyl Derivatives ◽  
Solid State Structures ◽  
Derivatives Of ◽  
Alkane Elimination

Reaction between the potassium salts of the hydro-tris-pyrazolylborate ligands TpMe'Me and TptBu'Me and the tris THF adduct of scandium trichloride lead to isolation of the scandium complexes (TpMe,Me)ScCl2(THF), 1a, and (TptBu,Me)ScCl2, 1b, in 65 and 49% yield, respectively. Subsequent reactions between 1a and 1b and alkyl lithium reagents RLi (R = Me, CH2SiMe3, and CH(SiMe3)2) gave the lithium salts of the Tp ligands as the major isolated products in all cases but one. The complex (TpMe,Me)Sc(CH2SiMe3)2(THF), 2a, could be obtained contaminated with at least 10% TpMe,MeLi via this methodology. A salt-free alkane elimination route to bis-trimethylsilylmethyl complexes 2a and the THF-free (TptBu,Me)Sc(CH2SiMe3)2, 2b, involving reaction between in situ generated Sc(CH2SiMe3)3(THF)2 and the protonated ligands, TpR,MeH, gave samples of the desired bis-alkyl derivatives in 67 and 87% yield, respectively. In solution, complexes 2a and 2b are both fluxional at room temperature. These dynamic processes were frozen out on the NMR time scale at lower temperatures and interpreted on the basis of the 1H NMR spectra obtained as well as information obtained from the solid state structures of both compounds, 2a: monoclinic, space group P21/c, a = 11.765(4) Ǻ, b = 14.8311(20) Ǻ, c = 20.891(5) Ǻ, β = 105.69(3)°, V = 3509.4(15) Ǻ3, Z = 4, R = 0.088, Rw = 0.082. 2b: triclinic, space group [Formula: see text], a = 11.9427(2) Ǻ, b = 20.3641(3) Ǻ, c = 26.5602(2) Ǻ, α = 112.192(1)°, β = 100.569(1)°, γ = 92.928(1)°, V = 5830.38(14) Ǻ3, Z = 6, R = 0.0500, Rw = 0.1137. Keywords: organoscandium complexes, hydro-tris-pyrazolylborate ligands, alkane elimination.

Supramoleküle aus Kronenethern und geminalen Sulfonen: Synthese von vier binären Komplexen und Kristallstruktur von (CH2CH2O)4·2H 2C(SO2C2H5)2/Supramolecules of Crown Ethers with Geminal Sulfones: Synthesis of Four Binary Complexes and Crystal Structure of (CH2CH2O )4·2H2C(SO2C2H5)2

1995 ◽  
Vol 50 (7) ◽  
pp. 1018-1024 ◽  
Author(s):  
Axel Michalides ◽  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Binary Complexes ◽  
Cyclic Polyethers ◽  
Adjacent Unit ◽  
Methylene Group

In a systematic search for supramolecular complexes involving all combinations of the cyclic polyethers 12-crown-4 (12C4), 15-crown-5 (15C 5), 18-crown-6 (18C 6) and dibenzo- 18-crown-6 (DB -18C6), and the geminal di- or trisulfones H2C(SO 2Me)2, H2C (SO2Et)2 and HC (SO2Me)3-n (SO2Et)n (n = 0 -3 ) , only the following four complexes could be isolated and unequivocally characterized by elemental analysis and 1H NMR spectroscopy: [(12C4){H2C (SO2Et)2}2] (3), [(18C6){H2C (S O2Me)2}] (4), [(DB -18C 6){H2C (SO2Et)2}] (5) and [(D B -18C 6)2{HC (SO2Me )(SO2Et)2}3] (6). The structure of 3 (triclinic, space group P1̄) consists of crystallographically centrosymmetric formula units, in which the disulfone molecules are bonded on each side of the ring by two C -H ··· O(crown) interactions originating from the central methylene group (H···O 213 pm) and from the methylene group of one EtSO2 moiety ( H ··· O 237 pm). Formula units related by translation are connected into parallel strands by a third type of reciprocal C -H ···O bond (H ···O 232 pm) between the second H atom of the central methylene group and a sulfonyl oxygen atom of the adjacent unit. The structure of 4 (monoclinic, space group C2/c) showed severe disorder of the crown ether and could not be refined satisfactorily. Compounds 5 and 6 crystallized as long and extremely thin fibres, indicative of linear-polymeric supramolecular structures; single crystals for X-ray crystallography were not available.

scholarly journals Chemie polyfunktioneller Moleküle, 114 [1]. Synthese und Struktur eines ionischen und nichtionischen, cyclischen Carbaphosphazens und eines Cobalt(III)phosphazen-Komplexes / Chemistry of Polyfunctional Molecules, 114 [1]. Synthesis and Structure of an Ionic and Non Ionic Cyclic Carbaphosphazene and of a Cobalt(III)phosphazene Complex

1994 ◽  
Vol 49 (12) ◽  
pp. 1763-1773 ◽  
Author(s):  
Jochen Ellermann ◽  
Jörg Sutter ◽  
Falk A. Knoch ◽  
Matthias Moll ◽  
Walter Bauer
Keyword(s):  
Mass Spectra ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
H Nmr

Reaction of (1) in CH2Cl2 with benzimidazole yields . The salt [4]+BPh4- has been prepared in THF by metathesis of [4]+Cl- with NaBPh4. Deprotonation of the cationic ring in [4]+BPh4- was accomplished using 1,8-diazabicyclo[5.4.01,7]undec-7-ene and resulted in the six-membered carbacyclophosphazene (6). Treating 1 with 8 -hydroxyquinoline in CH2Cl2 yields the octahedral cis-complex = 8-oxyquinolinate group). The com pounds [4]+BPh4-, 6 and 7 are characterized by their IR, Raman, 31P{1H} NMR, 13C{1H} NMR, 1H NMR and mass spectra. Crystals suitable for X-ray structure analyses have been obtained for [4]+BPh4- and 7×0.5 CH2Cl2. The colourless plates of [4]+BPh4- crystallize in the triclinic space group P1̄, with the lattice constants a = 1172.7(3), b = 1326.2(3), c = 1806.1(6) pm; α = 100.79(2), β = 103.71(3), γ = 108.18(2)°. The black blocks of 7×0.5 CH2Cl2 crystallize in the monoclinic space group P 21/c with the lattice constants a = 1159.0(10), b = 2008.9(10), c = 2034.6(12) pm; β = 105.86(5)°.

Mono- and difunctional furan-based 1,2,3,5-dithiadiazolyl radicals; preparation and solid state structures of 2,5-[(S2N2C)OC4H2(CN2S2)] and 2,5-[(S2N2C)OC4H2(CN)]

1992 ◽  
Vol 70 (3) ◽  
pp. 919-925 ◽  
Author(s):  
A. Wallace Cordes ◽  
Charles M. Chamchoumis ◽  
Robin G. Hicks ◽  
Richard T. Oakley ◽  
Kelly M. Young ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
The Mean ◽  
Solid State Structures ◽  
Solid State Characterization

The preparation and solid state characterization of the bifunctional radical furan-2,5-bis(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN2S2)] and the related monofunctional radical 2-cyanofuran-5-(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN)] are described. The crystal structure of 2,5-[(S2N2C)OC4H2(CN2S2)] is orthorhombic, space group Pna21, and consists of interleaved arrays of dimers, for which the mean interannular [Formula: see text] contact is 3.137 Å. The crystal structure of the monofunctional radical 2,5-[(S2N2C)OC4H2(CN)] is monoclinic, space group P21/n, and consists of a ribbon-like network of dimers (mean interannular [Formula: see text] interconnected by close head-to-tail [Formula: see text] contacts. The dimer units form stacks parallel to z, with a mean interdimer [Formula: see text] separation of 3.956 Å. The similarities and differences between these two crystal structures and those of related benzene-substituted systems are discussed. Keywords: dithiadiazolyl radicals, furan-based diradicals, cyanofuran-based radicals, radical dimers, crystal structures.

Synthesis and structural characterization of donor-stabilized disubstituted diphenyldithiophosphates of nickel(II)

2014 ◽  
Vol 70 (4) ◽  
pp. 761-767 ◽  
Author(s):  
Sandeep Kumar ◽  
Ruchi Khajuria ◽  
Amanpreet Kaur Jassal ◽  
Geeta Hundal ◽  
Maninder S. Hundal ◽  
...  
Keyword(s):  
Single Crystal ◽  
Chelate Ring ◽  
Donor Ligands ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Donor-stabilized addition complexes of nickel(II) with disubstituted diphenyldithiophosphates, [{(ArO)2PS2}2NiL2] {Ar = 2,4-(CH3)2C6H3[(1), (5)], 2,5-(CH3)2C6H3[(2), (6)], 3,4-(CH3)2C6H3[(3), (7)] and 3,5-(CH3)2C6H3[(4), (8)];L= C5H5N [(1)–(4)] and C7H9N [(5)–(8)]}, were successfully isolated and characterized by elemental analysis, magnetic moment, IR spectroscopy and single-crystal X-ray analysis. Compound (4) crystallizes in the monoclinic space groupP21/nwhereas compounds (7) and (8) crystallize in the triclinic space group P\bar 1. The single-crystal X-ray diffraction analysis of (4), (7) and (8) reveals a six-coordinated octahedral geometry for the NiS4N2chromophore. Two diphenyldithiophosphate ions act as bidentate ligands with their S atoms coordinated to the Ni centre. Each of them forms a four-membered chelate ring in the equatorial plane. The N atoms from two donor ligands are axially coordinated to the Ni atom.

Structure and conformation of the N-β-propionic acids of cyclohexan[b]indole and cyclooctan[b]indole

1986 ◽  
Vol 64 (9) ◽  
pp. 1829-1835 ◽  
Author(s):  
Carmen Esteban-Calderon ◽  
Martín Martinez-Ripoll ◽  
Severino García-Blanco ◽  
Fernando Temprano ◽  
José Gonzalo Rodriguez
Keyword(s):  
Propionic Acid ◽  
Monoclinic Space Group ◽  
Trans Conformation ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
H Nmr ◽  
Ray Methods

The structures of cyclohexan[b]indole N-β-propionic acid (1) and cyclooctan[b]indole N-β-propionic acid (2) have been determined by X-ray methods. The conformational populations of their N-β-propionic chains have been determined in solution by 1H nmr analyses. Crystals of 1 are triclinic, space group [Formula: see text] with a = 12.3562(4), b = 11.0727(3), c = 10.2050(4) Å, α = 108.519(3), β = 83.941(3), γ = 104.826(3)°, and Z = 4. Crystals of 2 are monoclinic, space group P21/c, with a = 5.636(1), b = 18.937(3), c = 13.976(4) Å, β = 98.84(3)°, and Z = 4. In both structures, the molecules are linked forming dimers through centrosymmetric H bonds. In solution the trans conformation of the chain is the preferred one in both compounds and increases with dilution until a constant value is reached.

Bis(trifluormethyl)disulfan und -trisulfan: Molekülgeometrie im festen Zustand [1] / Bis(trifluoromethyl)disulfane and Trisulfane: Molecular Geometry in the Solid State [1]

1997 ◽  
Vol 52 (1) ◽  
pp. 69-71 ◽  
Author(s):  
Christian Meyer ◽  
Dietrich Mootz ◽  
Birgit Bäck ◽  
Rolf Minkwitz
Keyword(s):  
Solid State ◽  
Electron Diffraction ◽  
Molecular Geometry ◽  
Monoclinic Space Group ◽  
Trans Conformation ◽  
Gaseous State ◽  
Triclinic Space Group ◽  
Space Group ◽  
Solid State Structures ◽  
State 1

The solid-state structures of the low-melting compounds bis(trifluoromethyl)disulfane (CF3SSCF3, triclinic, space group P 1̄, Z = 2) and bis(trifluoromethyl)trisulfane (CF3SSSCF3, monoclinic, space group C2/c, Z = 4) have been determined on single crystals with MoK α radiation at -160°C. The trisulfane has trans conformation. The geometry of both molecules agrees well with results of electron diffraction on the gaseous state. A comparison is made also with the crystal structures of the related molecules CF3TeTeCF3 and CF3OOOCF3

Reaktionen von Zintl-Phasen mit Trimethylphosphinkomplexen Strukturen mit ebenem Vierring Co2X2 (X = S, Se, Te) / Reactions of Zintl-Phases with Trimethylphosphine Complexes Structures Containing Planar Metallocycles Co2X2 (X = S. Se. Te)

1988 ◽  
Vol 43 (7) ◽  
pp. 830-838 ◽  
Author(s):  
Hans-Friedrich Klein ◽  
Michael Gaß ◽  
Udo Koch ◽  
Brigitte Eisenmann ◽  
Herbert Schäfer
Keyword(s):  
Phosphine Ligands ◽  
Molecular Structures ◽  
High Yield ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Zintl Phases ◽  
Triclinic Space Group ◽  
Space Group ◽  
Cobalt Compounds ◽  
Derivatives Of

Low-valent trimethylphosphine cobalt compounds are oxidized by tellurium, selenium, or sulfur to give the title compounds. Several high-yield syntheses are described. The crystal and molecular structures of (Me3P)3CoX3Co(PMe3)3 (1: X = Te. 2: X = Se. 3: X = S) have been determined by single crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic space group P21/n; a = 933.8(6) pm. b = 1488.3(6) pm. c = 1257.9(6) pm. β = 92.82(6)°. Z = 2. Complex 2 crystallizes in the triclinic space group P1, a = 1785.6(7) pm. b = 1599.7(7) pm. c = 928.9(5) pm. α = 87.8(1)°. β = 85.2(1)°. γ = 73.3(1)°. Z = 3. Complex 3 crystallizes in the monoclinic space group P21/c; a = 952.6(5) pm. b = 1868.7(8) pm. c - 1893.1(8) pm. β = 90.19(6)°. Z = 4. All three structures contain centrosymmetric molecules with planar Co2X2 rings. In solution dissociation of phosphine ligands occurs followed by slow decomposition to produce [(Me3P)2Co(PMe2)]2 among other products. 1 reacts with carbon monoxide to afford a ditelluride [(Me3P)2(CO)2Co]2Te2. but no corresponding derivatives of 2 or 3 were obtained.

Darstellung und spektroskopische Charakterisierung von Methylnitro-closo-hexaboraten sowie Kristallstrukturen von cis-(Ph4As)2[B6H4(CH3)(NO2)],fac-(Ph4As)2[B6H3(CH3)(NO2)2] · CH3CN und mer-(Ph4P)2[B6H3(CH3)(NO2)C2] / Synthesis and Spectroscopic Characterization of Methylnitro-closo-hexaborates and Crystal Structures of cis -(Ph4As)2[B6H4(CH3)(NO2)],fac-(Ph4As)2[B6H3(CH3)(NO2)2] · CH3CN and mer-(Ph4P)2[B6H3(CH3)(NO2)C2]

1999 ◽  
Vol 54 (3) ◽  
pp. 349-356 ◽  
Author(s):  
C. Drewes ◽  
W. Preetz
Keyword(s):  
Nmr Spectra ◽  
Spectroscopic Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cis And Trans

By electrochemical oxidation of (n-Bu4N)[B6H6(CH3)] in the presence of nitrite ions and of the base DBU in dichloromethane solution cis- and trans-[B6H4(CH3)(NO2)]2- , fac- [B6H3(CH3)(NO2)2]2- and mer-[B6H3(CH3)(NO2)c2]2- are formed. X-ray diffraction analyses have been performed on single crystals of cis-(Ph4As)2[B6H4(CH3O)(NO2)] (1) (monoclinic, space group P21/a, a = 20.063(2), b = 10.858(1), c =21.384(2) Å, β = 105.818(9)°, Z = 4), fac-(Ph4As)2[B6H3(CH3)(NO2)2] ·CH3CN (2) (triclinic, space group P1̄, a = 10.333(3), b = 10.695(3), c = 22.833(6) Å, α = 93.91(3), β = 96.79(3), γ = 104.56(2)°, Z = 2), and mer-(Ph4P)2[B6H3(CH3)(NO2)c2] (3) (triclinic, space group P1̄, a - 10.100(1), b = 10.402(3), c = 22.923(3) Å, α = 96.328(18), β = 89.928(12), γ = 107.963(16)°, Z = 2). The 11B NMR spectra and the vibrational spectra of the methylnitro compounds are discussed and compared with those of the monomethyl- and mononitro-closo-hexaborates.

CuIIand ZnIIβ-diketonate coordination polymers based on pyrimidin-2-amine, pyrazine and 1,2-bis(4-pyridyl)ethane

2016 ◽  
Vol 72 (6) ◽  
pp. 828-835 ◽  
Author(s):  
Franc Perdih
Keyword(s):  
Single Crystal ◽  
Coordination Polymers ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Metal Centers ◽  
Space Group ◽  
Π Interactions ◽  
Nitrogen Ligands ◽  
Polymeric Chains ◽  
Solid State Structures

Copper(II) and zinc(II) bis(4,4,4-trifluoro-1-phenylbutane-1,3-dionato) compounds with pyrimidin-2-amine (pyr2a), pyrazine (pyz) and 1,2-bis(4-pyridyl)ethane (dpet) were prepared and solid-state structures of coordination polymers [M(tfpb)2(pyr2a)]∞[M= Cu (1), Zn (2); tfpb = 4,4,4-trifluoro-1-phenylbutane-1,3-dionate], [M(tfpb)2(pyz)]∞[M= Cu (3), Zn (4a, 4b)] and [Cu(tfpb)2(dpet)]∞(5), respectively, were determined by single-crystal X-ray analysis. The coordination of metal centers in all compounds is octahedral with nitrogen ligands occupying the axial positions. Compound (1) crystallizes in the triclinic space group P\bar 1, whereas (2) crystallizes in the monoclinic space groupP2/n. Differences are due to the different orientation of adjacentM(tfpb)2units, whereas the orientation of pyrimidin-2-amine is the same in both compounds. Polymeric chains in (1) and (2) contain intramolecular N—H...O hydrogen bonding between amino and carbonyl groups. Room-temperature structures (3) and (4a) are isomorphous adopting the monoclinic space groupC2/m; however, on cooling crystals (4a) to 150 K a single-crystal-to-single-crystal transformation to (4b) possessing the triclinic space group P\bar 1 was observed. Compound (5) crystallizes in the triclinic space group P\bar 1 and contains a parallel aggregation of chains in contrast to the known structure of the non-fluorinated benzoylacetonato ligand, where chains aggregate in a perpendicular fashion. In the compounds studied intramolecular C—H...O and/or C—H...F interactions are present. The neighboring chains are linked by π...π interactions and in some compounds also by C—H...π interactions [(1), (4b), (5)].

scholarly journals Syntheses and crystal structures of the manganese hydroxide halides Mn5(OH)6Cl4, Mn5(OH)7I3, and Mn7(OH)10I4

2020 ◽  
Vol 235 (8-9) ◽  
pp. 375-389
Author(s):  
Viktoria Falkowski ◽  
Alexander Zeugner ◽  
Stefan Seidel ◽  
Rainer Pöttgen ◽  
Klaus Wurst ◽  
...  
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Temperature Synthesis ◽  
Triclinic Space Group ◽  
Manganese Hydroxide ◽  
Space Group ◽  
High Temperature Synthesis ◽  
High Pressure High Temperature

AbstractSingle-crystals of the new manganese hydroxide halides Mn5(OH)6Cl4, Mn5(OH)7I3, and Mn7(OH)10I4 were obtained by means of high-pressure/high-temperature synthesis in a Walker-type multianvil apparatus. The chloride crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters (single-crystal data) a = 592.55(8), b = 1699.7(2), c = 597.33(8) pm, and β = 112.58(1)°. The iodides crystallize in the triclinic space group P$\bar{1}$ (no. 2) with a = 653.16(2), b = 905.98(3), c = 1242.98(4) pm, α = 114.21(1)°, β = 99.91(1)°, and γ = 94.37(1)° for Mn5(OH)7I3 and a = 656.90(3), b = 906.59(4), c = 909.32(4) pm, α = 119.29(1)°, β = 97.99(1)°, and γ = 95.03(1)° for Mn7(OH)10I4. The crystal structures consist of edge-sharing Mn(OH)6–nXn (X = Cl, I; n = 1, 2, 3) octahedra arranged in stacked sheets. Adjacent layers are connected by hydrogen bonds of type O–H···X, confirmed by further characterization of single-crystals by IR-spectroscopy. The crystal chemical relationship with the aristotype Mg(OH)2 (brucite) is discussed on the basis of Bärnighausen trees (group–subgroup relations).

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