Crystal and molecular structure of Z- and E-1,2-dichloro-1,2-bis(2-chlorophenyl)ethylene. An X-ray and NMR study

1995 ◽  
Vol 73 (9) ◽  
pp. 1520-1525
Author(s):  
Luciano Antolini ◽  
Ugo Folli ◽  
Dario Iarossi ◽  
Adele Mucci ◽  
Silvia Sbardellati ◽  
...  
Keyword(s):  
Chemical Shifts ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Nmr Study ◽  
Phenyl Rings ◽  
A Cell ◽  
C Nmr

The crystal structures of the title compounds were determined by single crystal X-ray diffraction techniques. The molecule of the Z isomer, which crystallizes in the monoclinic space group C2/c with Z = 4 in a cell of dimensions a = 14.891 (2), b = 10.780(2), c = 8.769(1) Å, β = 97.47(2)°, V = 1395.7(7) Å3 has crystallographic twofold symmetry. The E form crystallizes in the orthorhombic space group Pbca with a = 11.730(1), b = 6.932(1), c = 16.841(1) Å, V = 1369.4(2) Å3 and Z = 4. Its molecules have crystallographically dictated [Formula: see text] symmetry. In both isomers the phenyl rings are roughly perpendicular to the average ethylene plane. The atoms characterizing this plane show significant deviations from planarity in the Z isomer. Marked bond-angle distortions at the ethene carbons of both structures are observed. The 1H and 13C NMR spectra of the compounds were measured and, particularly in the case of the 1H chemical shifts, fall into two quite separate spectral regions. At low temperature, two conformational isomers, those with different relative orientation of the C—Cl bonds of the phenyl rings, are observed in the spectrum of each compound. Keywords: chlorostilbenes, overcrowded molecules. X-ray structure, conformations, NMR spectroscopy.

Reaktionen von Mehrfachbindungssystemen mit dem 1.2.4-Trithia-3.5-diborolan-Ring -Eine strukturelle Richtigstellung / Reactions of Multiple-Bond-Systems with the 1,2,4-Trithia-3,5-diborolane Ring - A Structural Correction

1983 ◽  
Vol 38 (10) ◽  
pp. 1182-1191 ◽  
Author(s):  
Mathias Noltemeyer ◽  
George M. Sheldrick ◽  
Carl Habben ◽  
Anton Meller
Keyword(s):  
Ir Spectra ◽  
Multiple Bond ◽  
Monoclinic Space Group ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
C Nmr

The reaction of the 1,2,4-trithia-3,5-diborolane system with alkynes does not give 1,3,2-dithiaboroles, as suggested earlier [1, 2], but the previously unknown 1,2,3-dithiaboroles. With organic isocyanates and di-isopropylcarbodiimide, 1,2-dithia-3-bora-4-azacyclopentanones-( 5) and -thiones-(5), respectively, were isolated. The latter systems are isomers of the 5-methyl-1,4-dithia-2-aza-5-boracyclopentanones-(3) and -thiones-(3), which had been previously assumed as reaction products. The structures of 3-diethylamino-4,5- diphenyl -1,2,3 -dithiaborole - (4) (18), 3-(2,6-dimethylphenyl)-amino-4,5-diethyl-1,2,3-dithiaborole-( 4) (31) and 2-diphenylamino-1,3,2-dithiaborole-(4) (32) have been determined by X-ray diffraction. 18 is monoclinic, space group P21, a = 627.8(2), b = 1218.8(2), c = 1158.6(3) pm, β = 97.35(2)° and Z = 2. 31 is monoclinic, space group C2/c, a = 1475.9(5), b = 898.6(3), c = 2434.7(9) pm, β = 102.71(3)° and Z = 8. 32 is orthorhombic, space group Aba 2, a = 2557.3(8), b = 1748.5(5), c = 935.2(2) pm, Z = 12. 1H, 11B, 13C NMR, mass and IR spectra are also reported and discussed.

Divalent Metal-Complexes of 2-Fluorophenoxyacetic Acid - the Crystal-Structures of 2-Fluorophenoxyacetic Acid, Tetraaquabis(2-Fluorophenoxyacetato)Zinc(II) Dihydrate and Aquabis(2-Fluorophenoxyacetato)Bis(Pyridine)Copper(II)

1986 ◽  
Vol 39 (11) ◽  
pp. 1823 ◽  
Author(s):  
CHL Kennard ◽  
EJ Oreilly ◽  
S Schiller ◽  
G Smith ◽  
AH White
Keyword(s):  
Metal Complexes ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyramidal Geometry ◽  
A Cell ◽  
Divalent Metal Complexes

The crystal structures of 2-fluorophenoxyacetic acid ( oflpaH ) and the metal complexes aquabis (2-fluorophenoxyacetato) bis (pyridine)copper(II) (1) and tetraaquabis (2-fluorophenoxyacetato)zinc(II) dihydrate (2) have been determined by X-ray diffraction and refined to residuals R 0.036, 0.041, 0.025 for 641, 863 and 1505 observed reflections respectively. The acid crystallizes in a monoclinic cell, space group P21/c with a 6.207(2), b 19.363(8), c 6.999(2) Ǻ, β 114.81(2)� and Z 4. The molecules form planar, centrosymmetric , hydrogen-bonded cyclic dimers [O...O, 2.618(4)Ǻ]. Complex (1) is orthorhombic, space group P2cb with two molecules in a cell of dimensions a 5.621 (2), b 17.218(7), c 13.288(6)Ǻ while (2) is monoclinic, space group P21/c, a 6.597(2), b 5.279(2), c 30.079(10) Ǻ, β 94.65(3)�; with Z 2. Complex (1) has square-pyramidal geometry with the basal plane containing two trans related carboxyl oxygens [Cu-O, 1.944(4)Ǻ] and two trans related pyridine nitrogens [Cu-N, 2.030(5)Ǻ]. A water molecule occupies the apex of the square pyramid [Cu-OW, 2.199(8)Ǻ]. Complex (2) has octahedral geometry with the MO6 octahedron containing two trans related carboxyl oxygens [Zn-O, 2.122(2)Ǻ] and four water oxygens [Zn-OW, 2.069(2), 2.085(2)Ǻ]. Preliminary X-ray data also confirm that the magnesium(II) and manganese(II) complexes of 2-fluorophenoxyacetic acid are isomorphous with (2) but different from the cobalt(II) derivative.

Kristallstrukturen, 195Pt-NMR-Verschiebungen, Schwingungsspektren und Normalkoordinatenanalysen von trans-Dihalogeno-bis(oxalato)platinaten(IV), trans-[PtX2(ox)2]2-, X = Cl, Br, I / Crystal Structure, 195Pt NMR Chemical Shifts, Vibrational Spectra, and Normal Coordinate Analyses of trans-Dihalogeno-bis(oxalato)platinates(IV), trans-[PtX2(ox)2]2-, X = Cl, Br, I

1998 ◽  
Vol 53 (1) ◽  
pp. 93-100 ◽  
Author(s):  
W. Preetz ◽  
J.-G. Uttecht
Keyword(s):  
Chemical Shifts ◽  
Normal Modes ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Orthorhombic Space Group ◽  
Valence Force ◽  
Space Group ◽  
X Ray ◽  
Modes Of Vibration

By reaction of (n-Bu4N)2[Pt(ox)2] with elemental halogens in dichloromethane the complexes trans-[PtX2(ox)2]2- (X = Cl, Br, I) are formed. The crystal structures of trans-(py2CH2)[PtCl2(ox)2] · C4H6O3 (1) (monoclinic, space group P21/n, a = 12.119(3), b = 14.926(2), c = 12.666(4) Å, β = 91.26(3)°, Z = 4), trans-(py2CH2)[PtBr2(ox)2] (2) (monoclinic, space group P21/n, a = 7.402(8), b = 16.997(3), c = 14.898(3) Å, β = 98.15(3)°, Z = 4) and trans-(py2CH2)[PtI2(ox)2] ·C3H7NO (3) (orthorhombic, space group Pnma, a = 10.380(9), b = 13.973(2), c = 17.440(4) Å, Z = 4) have been determined by single crystal X-ray diffraction analysis. Highly resolution IR and Raman spectra were measured at low temperature (10 K). Using the molecular parameters of the X-ray determinations normal coordinate analyses based on a modified valence force field have been performed and the normal modes of vibration are assigned. The valence force constants are fd(PtCl) = 2.19, fd(PtBr) = 1.68, fd(PtI) = 1.28 mdyn/Å and fd(PtO) ranges from 2.71 to 2.82 mdyn/Å. The observed 195Pt NMR shifts are δ(195Pt) = 6472.4 (X = Cl), 6027.1 (Br) and 5142.7 ppm (I).

Strukturuntersuchungen an Diaryldichalkogeniden: Die Molekülstrukturen von [2,4,6-(CF3)3C6H2S]2,[2,4,6-Me3C6H2Te]2 und [2-Me2N-4,6-(CF3)2C6H2Te]2 / Structural Investigations of Diaryl Dichalcogenides: The Molecular Structures of [2,4,6-(CF3)3C6H2S]2, [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2

1992 ◽  
Vol 47 (3) ◽  
pp. 305-309 ◽  
Author(s):  
Anja Edelmann ◽  
Sally Brooker ◽  
Norbert Bertel ◽  
Mathias Noltemeyer ◽  
Herbert W. Roesky ◽  
...  
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Structural Investigations ◽  
Space Group ◽  
X Ray

Abstract The Molecular Structures of [2,4,6-(CF3)3C6H2S]2 (1) [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2 (3) have been determined by X-ray diffraction. Crystal data: 1: orthorhombic, space group P212121, Z = 4, a = 822.3(2), b = 1029.2(2), c = 2526.6(5) pm (2343 observed independent reflexions, R = 0.042); 2: orthorhombic, space group Iba 2, Z = 8, a = 1546.5(2), b = 1578.4(2), c = 1483.9(1) pm (2051 observed independent reflexions, R = 0.030); 3: monoclinic, space group P 21/c, Z = 4, a = 1118.7(1), b = 1536.5(2), c = 1492.6(2) pm, β = 98.97(1)° (3033 observed independent reflexions, R = 0.025).

The Crystal and Molecular Structures of Two Modifications of cis-Dichloro-mer-tris-(dimethylphenylphosphine)hydridoiridium(III)

1988 ◽  
Vol 41 (3) ◽  
pp. 283 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Heavy Atom ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Ligand ◽  
Ligand Bond

The structures of two crystalline modifications of mer -(Pme2Ph)3H-cis-Cl2IrIII, (1), have been determined from single-crystal X-ray diffraction data. Modification (A) is monoclinic, space group P21/c with a 12.635(1), b 30.605(3), c 14.992(2)Ǻ, β 110.01(2)° and Z = 8. Modification (B) is orthorhombic, space group Pbca with a 27.646(3), b 11.366(1), c 17.252(2)Ǻ and Z = 8. The structures were solved by conventional heavy atom techniques and refined by full-matrix least- squares analyses to conventional R values of 0.037 [(A), 8845 independent reflections] and 0.028 [(B), 5291 independent reflections]. Important bond lengths [Ǻ] are Ir -P(trans to Cl ) 2.249(1) av. (A) and 2.234(1) (B), Ir -P(trans to PMe2Ph) 2.339(2) av. (A) and 2.344(1), 2.352(1) (B), Ir-Cl (trans to H) 2.492(2), 2.518(2) (A) and 2.503(1) (B) and Ir-Cl (trans to PMe2Ph)2.452(2) av. (A) and 2.449(1)(B). Differences in chemically equivalent metal- ligand bond lengths emphasize the importance of non-bonded contacts in determining those lengths.

The Constituents of Marine Sponges. IX New Norditerpenoids from Aplysilla pallida

1997 ◽  
Vol 50 (9) ◽  
pp. 903 ◽  
Author(s):  
Trevor W. Hambley ◽  
Walter C. Taylor ◽  
Stephen Toth
Keyword(s):  
Crystal Structures ◽  
Spectroscopic Studies ◽  
Marine Sponges ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

Four novel norditerpenoids were isolated from a new encrusting sponge, conveniently labelled Aplysilla pallida. The structures of aplypallidenone (1), aplypallidoxone (2), aplypallidione (3) and aplypallidioxone (4) were elucidated by spectroscopic studies and the crystal structures of aplypallidenone and aplypallidoxone have been determined by X-ray diffraction methods. The structure of (1) was refined to a residual of 0·040 for 1665 independent observed reflections and the structure of (2) was refined to a residual of 0·031 for 1699 independent observed reflections. The crystals of (1) are orthorhombic, space group P212121, a 7·728(2), b 10·838(4), c 24·880(5) Å, Z 4. Those of (2) are monoclinic, space group C 2, a 23·927(7), b 6·674(2), c 14·033(3) Å, Z 4.

Molecular Motions in (CH3)3XCl, X = Sn and Pb. NMR Investigations and Crystal Structure Study of (CH3)3PbCl and CH3SnBr3

1991 ◽  
Vol 46 (4) ◽  
pp. 337-343 ◽  
Author(s):  
Da Zhang ◽  
Shi-Qi Dou ◽  
Alarich Weiss
Keyword(s):  
Molecular Motion ◽  
Structure Study ◽  
Methyl Groups ◽  
Monoclinic Space Group ◽  
Molecular Motions ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Group D

Abstract The molecular motion in (CH3)3XCl, X = Sn and Pb has been investigated by measurement of the second moment M2(1H) as function of temperature in the range 95 < T,/K<345. The methyl groups in both compounds rotate freely over the whole temperature range studied. In (CH3)3SnCl the C'3-rotation of (CH3)3Sn-group about the Sn CI axis sets in above 273 K. To explain the NMR and INS results, the crystal structures of (CH3)3PbCl and CH3SnBr3 were determined by single X-ray diffraction. (CH3)3PbCl crystallizes in a monoclinic space group C32-C2, a = 1276.7(3) pm, b = 982.3(3) pm, c = 547.0(2) pm, ß = 91.12(1)°; Z = 4, R = 0.035. CH3SnBr3 crystallizes in an orthorhombic space group D162h-Pnma, a = 643.0(3) pm, b= 1005.3(4) pm, c= 1148.0(4) pm; Z = 4, R =0.057

Structural Systematics of Metal Acetylide Complexes. II. X-Ray Studies of Some Nickel σ-Acetylide Complexes

1998 ◽  
Vol 51 (3) ◽  
pp. 219 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Trans Influence

The structures of Ni(C≡CR)(PPh3)(η-C5H5) (R = Ph (1), C6H4-4-NO2 (2), 4-C6H4C6H4-4′-NO2 (3), (E)-4-C6H4CH=CHC6H4-4′-NO2 (4), 4-C6H4C≡CC6H4-4′-NO2 (5), 4-C6H4N=CHC6H4-4′-NO2 (6)) have been determined by single-crystal X-ray diffraction studies, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a 10·094(2), b13·429(3), c 18·835(5) Å,α 103·24(2), β 91·50(2), γ 90·10(2)°, Z 4, 5844 unique reflections (595 parameters), converging at R 0·033 and Rw 0·024. For (2), crystals are orthorhombic, space group Pna21, with a 16·799(2), b 8·681(2), c 17·485(2) Å, Z 4, 1774 unique reflections (325 parameters), converging at R 0·031 and Rw 0·029. For (3), crystals are monoclinic, space group P 21/c, with a 11·140(3), b 18·282(4), c 15·296(2) Å, β 105·18(2)°, Z 4, 3132 unique reflections (397 parameters), converging at R 0·039 and Rw 0·024. For (4), crystals are monoclinic, space group P 21/n, with a 12·929(7), b 16·953(8), c 15·601(7) Å, β 112·55(3), Z 4, 3023 unique reflections (397 parameters), converging at R 0·039 and Rw 0·025. For (5), crystals are monoclinic, space group P 21/n, with a 12·710(5), b 16·882(3), c 15·693(4) Å, β 111·37(3)°, Z 4, 3216 unique reflections (397 parameters), converging at R 0·035 and Rw 0·030. For (6), crystals are monoclinic, space group P 21/n, with a 12·594(1), b 16·936(2), c 15·611(1) Å, β 112·476(5)°, Z 4, 3564 unique reflections (397 parameters), converging at R 0·038 and Rw 0·041. For structurally characterized 18-electron (cyclopentadienyl)nickel(II) acetylide complexes, statistically insignificant decreases in the average Ni-C(1) distance and trans influence and an increase in the average C(1)-C(2) parameter are observed on introduction of an acceptor substituent at the alkynyl ligand.

Steric Modification of Metal-Phosphorus Bond Lengths: the Preparation, Characterization and CrystalStructures of mer-trans-(PPri3)2(Pme2Ph)-Cl-cis-H2IrIII(1) and mer-trans-(PPri3)2(PMe2Ph)H3IrIII

1995 ◽  
Vol 48 (6) ◽  
pp. 1183 ◽  
Author(s):  
EJ Ditzel ◽  
GB Robertson
Keyword(s):  
Chloride Content ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Steric Crowding ◽  
Unit Increase

The syntheses and subsequent characterization of the complexes mer -trans-(PPri3)2(Pme2Ph)-Cl-cis-H2IrIII(1) and mer-trans-(PPri3)2(PMe2Ph)H3IrIII (2) by n.m.r. and by low temperature (153�5 K) X-ray diffraction analyses are reported. Crystals of (1) are monoclinic, space group P21/c with a 19.277(2), b 9.020(1), c 17.657(2) Ǻ, β 101.40(1)° and Z 4. Crystals of (2) are orthorhombic, space group P212121, with a 19.373(3), b 18.724(2), c 8.113(1) Ǻ and Z 4. Full-matrix least-squares analyses converged with R = 0.027 and wR = 0.031 for (1) (3243 reflections), and R = 0.030 and wR = 0.038 for (2) (2892 reflections). Consistent with previous observation, the unit increase in chloride content (in place of hydride) in (1) is accompanied by a global lengthening of 0.036 Ǻ (av.) in the Ir -P bond lengths cf. those in (2). Also, because of increased steric crowding (two PPri3 ligands in place of two Pme2Ph), the Ir-PMe2Ph bond in (1) is 0.019(2) Ǻ longer than the chemically equivalent bond in mer-(PMe2Ph)3Cl-cis-H2IrIII. In previously reported complexes in this series metrically similar increases in Ir-PMe2Ph distances result from the replacement of just one Pme2Ph ligand by PPri3.

Crystal structures of two lactones of the bicyclo[2,2,2]octane series

1982 ◽  
Vol 35 (2) ◽  
pp. 457 ◽  
Author(s):  
RM Carman ◽  
SS Smith ◽  
CHL Kennard ◽  
G Smith ◽  
AH White ◽  
...  
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Three Dimensional ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
A Cell

The crystal structures of two γ-lactones of the bicyclo[2,2,2]octane series, endo-3-carboxy-exo-5- iodobicyclo[2,2,2]octane-2,6-carbolactone (2; R = CO2H) and exo-3-methoxycarbonyl-endo-5-acetoxybicyclo[2,2,2] octane-2,6-carbolactone (7b), have been determined by direct methods from three-dimensional X-ray data and refined by least-squares to final residuals of 0.033 (2; R = CO2H) and 0.036 (7b) for 1918 and 630 'observed' reflections respectively. Crystals for (2; R = CO2H) are monoclinic, space group P21/c with Z 8 in a cell of dimensions a 7.192(2), b 23.785(8), c 13.199(5) �, β 105.35(2)�, while (7b) crystallizes in the orthorhombic space group P212121 with Z 4 in a cell of dimensions a 13.347(7), b 11.839(7), c 8.227(11) �.

Sign in / Sign up

Export Citation Format

Share Document