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

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.

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.

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.

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)].

Synthese und Kristallstruktur von Tribrommethyltriphenylphosphonium-bromid und Bis(tribrommethyltriphenylphosphonium)-tribroniid-bromid / Synthesis and Crystal Structure of Tribromomethyltriphenylphosphonium Bromide and Bis(tribromomethyltriphenylphosphonium) Tribromide Bromide

1995 ◽  
Vol 50 (2) ◽  
pp. 223-228 ◽  
Author(s):  
H. Vogt ◽  
C. Frauendorf ◽  
A. Fischer ◽  
P. G. Jones
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Red Light ◽  
Monoclinic Space Group ◽  
Reaction Conditions ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group

Tribromotriphenylphosphonium bromide 1 has been prepared by the reaction of triphenylphosphine with tetrabromomethane in dichloromethane. Colourless crystals were obtained by recrystallization from the same solvent. The light-sensitive crystals change colour to yellow. The crystals are triclinic, space group P1̄ , Z = 4, a = 1008.6(5), b = 1357.8(6), c = 1560.7(7) pm, α = 106.61(4), β = 91.80(4), γ = 93.88(4)°. In the solid state there are discrete monomeric (C6H5)3PCBr3+ cations and Br- anions. The cation has a slightly irregular tetrahedral geometry around the P atom. The crystals contain one molecule CH2C12 per four molecules (C6H5)3PCBr4.Bis(tribromomethyltriphenylphosphonium) tribromide bromide 2 can be obtained as a byproduct of the reaction of (C6H5)3P with CBr4 by variation of the reaction conditions. Red light-stable crystals are obtained by recrystallization from CH2C12. The crystals are monoclinic, space group C2/c, Z = 8, a = 2231.5(7), b = 1532.7(7), c = 1556.9(6) pm, β = 129.69(2)°. In the solid state bis(tribromomethyltriphenylphosphonium) tribromide bromide exists as discrete monomeric (C6H5)3PCBr3+ cations and Br- and Br3- anions. The Br anion and the central Br of Br3- anion lie on crystallographic twofold axes. The cation has also a slightly irregular tetrahedral geometry around the P atom, with a long P-CBr3 bond.

scholarly journals Synthesis and characterization of Ti(IV), Zr(IV) and Al(III) salen-based complexes

2021 ◽  
Vol 12 (2) ◽  
pp. 216-221
Author(s):  
Joana Hipolito ◽  
Luis Alves ◽  
Ana Martins
Keyword(s):  
Solid State ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Space Group ◽  
High Yields

New Ti(IV), Zr(IV) and Al(III) salen-based complexes of formulae [(L)TiCl2], 2, [(L)ZrCl2], 3, and [(L){Al(CH2CH(CH3)2)2}2], 4, where L = meso-(R,S)-diphenylethylene-salen, were synthesized in high yields. [(L){Al(CH2CH(CH3)2)2}2] is a bimetallic complex that results from the reaction of H2L with either 1 or 2 equivalent of Al(CH2CH(CH3)2)3. The solid-state molecular structures of compounds 2 and 4·(C7H8) were obtained by single-crystal X-ray diffraction. Crystal data for C44H54Cl2N2O2Ti, (2a): monoclinic, space group C2/c (no. 15), a = 27.384(1) Å, b = 12.1436(8) Å, c = 28.773(2) Å, β = 112.644(2)°, V = 8830.6(9) Å3, Z = 8, μ(MoKα) = 0.350 mm-1, Dcalc = 1.146 g/cm3, 26647 reflections measured (5.204° ≤ 2Θ ≤ 50.7°), 8072 unique (Rint = 0.0967, Rsigma = 0.1241) which were used in all calculations. The final R1 was 0.0640 (I > 2σ(I)) and wR2 was 0.1907 (all data). Crystal data for C62H72Cl2N2O2Ti (2b): monoclinic, space group P21/c (no. 14), a = 19.606(1) Å, b = 12.793(1) Å, c = 23.189(2) Å, β = 105.710(4)°, V = 5599.0(7) Å3, Z = 4, μ(MoKα) = 0.291 mm-1, Dcalc = 1.182 g/cm3, 37593 reflections measured (3.65° ≤ 2Θ ≤ 50.928°), 10304 unique (Rint = 0.0866, Rsigma = 0.1032) which were used in all calculations. The final R1 was 0.0593 (I > 2σ(I)) and wR2 was 0.1501 (all data). Crystal data for C67H97Al2N2O2 (4·(C7H8)): triclinic, space group P-1 (no. 2), a = 10.0619(9) Å, b = 16.612(2) Å, c = 21.308(2) Å, α = 67.193(5)°, β = 78.157(6)°, γ = 77.576(5)°, V = 3176.8(6) Å3, Z = 2, μ(MoKα) = 0.088 mm-1, Dcalc = 1.063 g/cm3, 42107 reflections measured (5.382° ≤ 2Θ ≤ 51.624°), 12111 unique (Rint = 0.0624, Rsigma = 0.0706) which were used in all calculations. The final R1 was 0.0568 (I > 2σ(I)) and wR2 was 0.1611 (all data). The solid-state molecular structure of [(L){Al(CH2CH(CH3)2)2}2] reveals that both metal centres display a slightly distorted tetrahedral geometry bridged by the salen ligand. Both [(L)TiCl2] and [(L)ZrCl2] complexes display octahedral geometry with trans-chlorido ligands.

Enclathrating Benzene in a Neutral Dicopper(II) Coordination Framework

2003 ◽  
Vol 56 (7) ◽  
pp. 671 ◽  
Author(s):  
Hong-Bo Liu ◽  
Shu-Yan Yu ◽  
Hui Huang ◽  
Zhong-Xing Zhang
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Aromatic Molecules ◽  
Coordination Framework

Two infinite complexes {[Cu2(O2CCH3)4](3-tpt)(CH3OH)2}∞ (1) and {[Cu2(O2CPh)4](3-tpt)(C6H6)1.5}∞ (2) were obtained by reactions of 2,4,6-tris(3′-pyridyl)-1,3,5-triazine (3-tpt) with Cu2(O2CCH3)4 and Cu2(O2CPh)4, respectively, which have been structurally established by single-crystal X-ray diffraction. Complex (1) consists of one-dimensional zig-zag chains in its solid state, which can encapsulate methanol molecules; complex (2) consists of one-dimensional helical chains in its solid state, providing large channels which can selectively enclathrate benzene molecules. (1) crystallizes in the monoclinic space group P21/c with a 8.2892(4), b 22.8479(8), c 16.9258(10) Å, β 99.1480(10)°, V 3164.8(3) Å3, and Z 4; (2) crystallizes in the triclinic space group P1 with a 10.7641(8), b 12.0908(8), c 18.9039(12) Å, α 82.514(3)°, β 85.268(2)°, γ 79.746(4)°, V 2395.9(3) Å3, and Z 2. The inclusion selectivity toward aromatic molecules was discussed.

Polysulfonylamine, LXV [1] Eine neue zentrosymmetrische Festkörper-Konformation von 18-Krone-6: Darstellung und Kristallstrukturen der monomeren Supramoleküle (CH2CH2O) 6 · 2 HN (SO2-2-Naphthyl)2 und (CH2CH2O) 6 · 2 iPrOH · 2 HN(SO2Ph)2 / Polysulfonylamines, LXV [1] A Novel Centrosymmetric Solid-State Conformation of 18-Crown-6: Synthesis and Crystal Structures of the Monomeric Supramolecules (CH2CH2O) 6 · 2 HN (SO2-2-Naphthyl)2 and (CH2CH2O) 6 · 2 iPrOH · 2 HN(SO2Ph)2

1995 ◽  
Vol 50 (6) ◽  
pp. 913-922 ◽  
Author(s):  
Dagmar Henschel ◽  
Martina Näveke ◽  
Thomas Hamann ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Solid State ◽  
Inversion Symmetry ◽  
Triclinic Space Group ◽  
Space Group ◽  
Ether Oxygen ◽  
O 175 ◽  
O 193 ◽  
Solid State Structures ◽  
Solid State Conformation ◽  
Oxygen Atoms

The complexes 18 C 6 · 2 HN (SO2-2 -Naphthyl)2 (2a) and 18 C 6 · 2 iPrOH · 2 HN (SO2Ph)2 (3e) were obtained by co-crystallization of 18-crown-6 (18 C 6) with the appropriate di(arenesulfonyl) amine from isopropanol solutions at temperatures ≥20 °C (for 2a) or at - 20 °C (for 3e). Both structures contain isolated formula units displaying crystallographic inversion symmetry. The conformation of the crown rings is characterized by the torsion angle sequence g+g+aag−g+ag+ag−g−aag+g−ag−a, unprecedented in solid-state structures of 18C 6 complexes. The six ether oxygen atoms and four out of twelve carbon atoms of the ring are coplanar within ± 7 pm. In 2a (triclinic, space group P 1̄) , the disulfonylamine molecules are linked to the oxygen atoms of the g±g∓g∓ units via N -H ··· O hydrogen bonds ( H ··· O 201 pm, N - H ··· O 161°). In 3e (triclinic, space group P 1̄ ) , each amine is N - H ··· O bonded to an isopropanol molecule (H ··· O 193 pm , N - H ··· O 175°) that is connected to a crown oxygen atom of the same conformational type as indicated above for 2a (H ··· O 198 pm, O - H ··· O 166°).

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.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.

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