Darstellung, Schwingungsspektren und Normalkoordinatenanalyse der 10B-und 11B-Isotopomeren von [B2(NCS)6]2- sowie Kristallstruktur von (Ph3P=N=PPh3)2[B2(NCS)6] / Preparation, Vibrational Spectra and Normal Coordinate Analysis of the 10B and 11B Isotopomers of [B2(NCS)6]2- and Crystal Structure of (Ph3P=N=PPh3)2[B2(NCS)6]

1996 ◽  
Vol 51 (4) ◽  
pp. 551-556 ◽  
Author(s):  
W. Preetz ◽  
B. Steuer
Keyword(s):  
Crystal Structure ◽  
Normal Coordinate Analysis ◽  
Force Constants ◽  
Potential Energy Distribution ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
X Ray ◽  
Fractionated Crystallization ◽  
Good Agreement

Abstract By reaction of [B6H6]2- with a solution of (SCN)2 in dichloromethane in the presence of solid KOH the hexaisothiocyanatodiborate anion [B2(NCS)6]2- is formed and can be isolated by fractionated crystallization. The crystal structure of (PNP)2[B2(NCS)6] has been determined by single crystal X-ray diffraction analysis; triclinic space group P1̄ with a=12,282(5), b=12,416(5), c=14,155(5)Å, a=68,36(5), β=70,59(5), γ=80,93(5)°.The [B2(NCS)6]2- anion reveals a staggered conformation with nearly local D3d symmetry and a B-B bond length of 1,73(2) Å. Using the crystallographic data a normal coordinate analysis has been performed. With a set of 12 force constants (e.g. fd(BB)=3,62, fd(BN)=4,21 mdyn/Å) a good agreement between observed and calculated frequencies for the 10B and 11B isotopomers has been achieved. The potential energy distribution on the force constants reveals strong vibrational couplings within the B2N6 framework.

Darstellung, Schwingungsspektren und Normalkoordinationsanalyse der D- und 13C-Isotopomeren des Methylpentahydro-closo-hexaborats [B6H5(CH3)]2- sowie Kristallstruktur von [P(C6H5)4][B6H6(CH3)] / Preparation, Vibrational Spectra and Normal Coordinate Analysis of the D and 13C Isotopomeres of the Methylpentahydro-closo-hexaborate [B6H5(CH3)]2- and the Crystal Structure of [P(C6H5)4][B6H6(CH3)]

1995 ◽  
Vol 50 (4) ◽  
pp. 623-629 ◽  
Author(s):  
J. Baurmeister ◽  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Normal Coordinate Analysis ◽  
Force Constants ◽  
Potential Energy Distribution ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Stretching Vibration ◽  
Ir And Raman ◽  
Good Agreement

The crystal structure of [P(C6H5)4][B6H6(CH3)] has been determined by single crystal X-ray diffraction analysis; triclinic space group P 1̄ with a = 7.408(2), b = 11.887(3), c = 14.4486(9) Å , α = 80.013(12), β = 79.421(10), γ = 88.85(2)°. The additional H atom could be refined with B - H distances between 1.21 and 1.31 Å above one of the facettes of the B6 octahedron adjacent to the methyl group. The IR and Raman spectra of the ueprotonated Cs salts of the six isotopomers [B6H5(CH3)]2-, [B6H5(CD3)]2-, [B6H5(13CH3)]2-, [B6D5(CH3)]2-, [B6D5(CD3)]2- and [B6D5(13CH3)]2- exhibit characteristic shifts of their vibration bands. Using the crystallographic data a normal coordinate analysis has been performed, based on a general valence force field. With a set of 14 force constants (e.g. fd(BB ) = 1.80, fd(BC ) = 3.70, fd(BH ) = 3.17, fd(CH ) = 4.62 mdyn/Å) good agreement between observed and calculated frequencies o f all D and 13C isotopically labeled derivatives has been achieved. The potential energy distribution on the force constants reveals strong vibrational couplings of the boron cage with the substituents. The B - C stretching vibration o f the CH3 group is observed in the region 1142-1153 cm-1, for the CD3 substituent at higher frequencies of 1168-1179 cm-1.

Darstellung, Kristallstruktur, Schwingungsspektren und Normalkoordinatenanalyse von [Os(acac)3]/ Synthesis, Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of [Os(acac)3]

1998 ◽  
Vol 53 (2) ◽  
pp. 232-238 ◽  
Author(s):  
K. Dallmann ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Normal Modes ◽  
Normal Coordinate Analysis ◽  
Force Constants ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
X Ray ◽  
Modes Of Vibration ◽  
Ir And Raman ◽  
Good Agreement

Abstract In the reaction of K2[OsCl6] with boiling water/acetylacetone (1:1) a mixture of different chloro-acetylacetonato complexes is formed, from which [Os(acac)3] can be isolated by column chromatography with dichloromethane on silica gel. The crystal structure of [Os(acac)3] (mo­noclinic, space group P21/c,a = 13.968(5), b = 7.517(5), c = 16.455(5) Å ,β = 98.939(5)°, Z = 4) has been determined by single crystal X-ray diffraction analysis. High resolution IR and Raman spectra were measured at low temperature (10K). Based on the molecular parameters of the X-ray structure determination a normal coordinate analysis has been performed and the normal modes of vibration have been assigned. With a set of 32 force constants, taking into account the intraligand vibrations, a good agreement between observed and calculated frequencies has been achieved. The valence force constants are fd(OsO) = 3.19 and fd(OC) = 6.74 mdyn/Å.

Darstellung, Schwingungsspektren und Normalkoordinatenanalyse von (n-Bu4N)2[Pt(SCN)n(ox)], n = 2, 4, sowie Kristallstruktur von [(C5H5N)2CH2][Pt(SCN)4(ox)] / Synthesis, Vibrational Spectra and Normal Coordinate Analysis of (n-Bu4N)2[Pt(SCN)n(ox)], n = 2, 4, and Crystal Structure of [(C5H5N)2CH2][Pt(SCN)4(ox)]

2002 ◽  
Vol 57 (9) ◽  
pp. 1036-1042 ◽  
Author(s):  
J.-G. Uttecht ◽  
C. Nöther ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Vibrational Spectra ◽  
Normal Coordinate Analysis ◽  
Normal Coordinate ◽  
Photochemical Reduction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Trans Influence ◽  
Ir And Raman ◽  
Good Agreement

On exposure of trans-(n-Bu4N)2[Pt(SCN)2(ox)2] to photochemical reduction (n-Bu4N)2- [Pt(SCN)2(ox)] (1) is formed. Further treatment with (SCN)2 yields (n-Bu4N)2- [Pt(SCN)4(ox)] (2). The X-ray structure determination on a single crystal was performed of [(C5H5N)2CH2][Pt(SCN)4 (ox)] (triclinic, space group P1̅, a = 9.823(1), b = 14.850(1), c = 15.799(1) Å , α= 74.304(9), β= 86.268(9), γ= 87.455(9)°, Z = 4). Based on the molecular parameters of the X-ray determination the IR and Raman spectra have been assigned by normal coordinate analysis. The valence force constants of the symmetric axis S-Pt-S and of the asymmetrically coordinated S'-Pt-O* axes are fd(PtS) = 1.71, fd(PtS') = 1.92 (1), fd(PtS') = 2.02 (2) and fd(PtO•) = 2.45 (1) and 2.24 (2) mdyn/Å. Taking into account increments of the trans influence a good agreement between observed and calculated frequencies is achieved. The NMR shifts are δ(195Pt) = 1967.7 (1) and 2930.8 ppm (2)

Darstellung, Kristallstruktur, Schwingungsspektren und Normalkoordinatenanalyse von trans-[OsO2(N2H2C2O2)2]2- / Synthesis, Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of trans-[OsO2(N2H2C202)2]2-

1998 ◽  
Vol 53 (11) ◽  
pp. 1338-1342 ◽  
Author(s):  
A. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Vibrational Spectra ◽  
Room Temperature ◽  
Normal Coordinate Analysis ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir And Raman

The treatment of K2[OsO2(OH)4] with oxamide in aqueous solution yields [OsO2(N2H2C2O2)2]2-. The crystal structure of trans-(Ph4P)2[ OsO2(N2H2C2O2)2]·CH2Cl2 (triclinic, space group P1̅, a = 10.447(1), b = 14.102(4), c = 16.962(2) Å, a = 90.037(1), β = 90.633(7), γ = 98.812(2)°, Z = 2) has been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra were measured at room temperature. Based on the molecular parameters of the X-ray determination a normal coordinate analysis has been performed and the vibrations are assigned. The valence force constants are fd(Os=O) = 6.7, fd(Os-N) = 2.4, fd(C-N) = 4.9, fd(C=0) = 11.15 and fd(C-C) = 4.7 mdyn/Å.

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalyse von cis-[ReCl4X2]2-, X = NCS, NCSe / Crystal Structures, Vibrational Spectra and Normal Coordinate Analysis of cis-[ReCl4X2]2-, X = NCS, NCSe

1998 ◽  
Vol 53 (11) ◽  
pp. 1329-1334 ◽  
Author(s):  
L. Homolya ◽  
S. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Normal Coordinate Analysis ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Valence Force ◽  
Space Group ◽  
X Ray ◽  
Valence Force Field ◽  
Ir And Raman

The crystal structures of cis-(n-Bu4N)2[ReCl4(NCS)2] (triclinic, space group P1̅, a = 11,245( 1), b = 20.174(3), c = 21.320(8) Å, a =109.06(2), β = 96.46(2), γ = 98.22(5)°, Z = 4) and cis-(Ph4P)2[ReCl4(NCSe)2]·2CH2Cl2 (triclinic, space group P1̅, a = 10.341(2), b = 13.436(3), c = 19.616(4) Å, α = 92.70(2), β = 92.02(2), γ = 89.99( 1)°, Z= 2) have been determined by single crystal X-ray diffraction analysis. Both ambidentate ligands NCS and NCSe are bonded via the N atom. Using the molecular parameters of the X-ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis based on a modified valence force field. The valence force constants fd(ReN) are 1,78(NCS) and 1,79(NCSe) mdyn/ Å.

Darstellung, Schwingungsspektren und Normalkoordinatenanalyse von bindungsisomeren Halogenoselenocyanatorhenaten(IV) sowie Kristallstrukturen von mer-(Ph4P)2[ReCl3(NCSe)2cis (SeCN)] und mer-(n-Bu4N)2[ReCl3I(NCSe)2cis] / Synthesis, Vibrational Spectra and Normal Coordinate Analysis of Linkage Isomeric Halogenoselenocyanatorhenates(IV) and Crystal Structures of mer-(Ph4P)2[ReCl3(NCSe)2cis (SeCN)] and mer-(n-Bu4N)2[ReCl3I(NCSe)2cis]

1999 ◽  
Vol 54 (10) ◽  
pp. 1222-1228 ◽  
Author(s):  
S. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Exchange Chromatography ◽  
Normal Coordinate Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By treatment of fac-[ReCl3I3]2- with (SeCN)2 indichloromethane fac-[ReCl3(NCSe)3]2- (1), mer-[ReCl3(NCSe)2cis (SeCN)]2- (2) and mer-[ReCl3I(NCSe)2cis]2- (3) are formed which have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of mer-(Ph-P)2[ReCl3(NCSe)2cis(SeCN)] (triclinic, space group Pl̅, a = 16.099(1), b = 16.729(3), c =21.026(2) Å, α = 70.194(10), ß = 73.958(10), γ = 83.929(10)°, Z = 4) and mer-(n-Bu4N)2[ReCl3|(NCSe)2cis] (monoclinic, space group P21/c, a = 11.838(1), b = 12.796(2), c = 30.767(2) Å, ß = 97.419(6)°, Z = 4) have been determined by single crystal X-ray diffraction analysis. Based on the molecular parameters of the X-ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis. The valence force constants are fd(ReN) = 1.79 (1), 1.71 (2), 1.71 (3) and fd(ReSe) = 1.15 (2) mdyn/Å.

Kristallstrukturen von [P(C6H5)4]2[B6Cl6](CH3CN)2 und [P(C6H5)4]2[B6Br6](CH3CN)2 sowie Schwingungsspektren und Normalkoordinatenanalyse der isotopomeren closo-Hexahalogenohexaborate [11Bn10B6-nX6]2-, Χ = Cl, Br; n = 0-6 / Crystal Structures of [P(C6H5)4]2[B6Cl6](CH3CN)2 and [P(C6H5)4]2[B6Br6](CH3CN)2, Vibrational Spectra and Normal Coordinate Analysis of Isotopomeric closo-Hexahalogenohexaborates [11Bn10B6-nX6]2-, X = Cl, Br; n = 0-6

1991 ◽  
Vol 46 (6) ◽  
pp. 800-808 ◽  
Author(s):  
J. Thesing ◽  
J. Baurmeister ◽  
W. Preetz ◽  
D. Thiery ◽  
H. G. von Schnering
Keyword(s):  
Crystal Structures ◽  
Molecular Data ◽  
Force Constants ◽  
Geometric Isomers ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Vibrational Coupling ◽  
Triclinic Space Group ◽  
Bond Lengths ◽  
Good Agreement

The crystal structures of (TPP)2[B6Cl6](CH3CN)2 and (TPP)2[B6Br6](CH3CN)2 were determined from single crystal X-ray diffraction analyses at 147 K. They are triclinic, space group P1̅, and contain nearly regular octahedral anions with bond lengths d(B-B) 1.716, d(B-Cl) 1.818 for [B6Cl6]2- and d̅(B-B) 1.684, d̅(B-Br) 1.993 Å for [B6Br6]2-. Using these molecular data, normal coordinate analyses for the ten isotopomers [11Bn10B6-nX6]2-, n = 0-6, X = Cl, Br, including the pairs of geometric isomers for n = 2, 3, 4 have been performed, based on a general valence force field. With a set of 8 force constants for Cs2[B6Br6] (e.g. fd(BB) = 1.39, fd(BBr) = 3.18 mdyn/Å) and 10 for Cs2[B6Cl16] (e. g. fd(BB) = 1.30, fd(BCl) = 4.01 mdyn/Å) the calculated frequencies are in good agreement with observed IR (10 K) and Raman bands (80 K) in natural abundance as well as for 11B- and 10B-enriched derivatives. For the series [B6X6]2-, X = Cl, Br, I the correlation of decreasing bond lengths d(B-B) and increasing force constants fd(BB) along with vibrational coupling between the B6 cage and the substituent sphere is discussed.

Schwingungsspektren und Normalkoordinatenanalysen der Dioxoosmate( VI) trans-[OsO2(CN)4]2-, trans-[OsO2(CN)2(0H )]22- und trans-[OsO2(CN)2(OCH3)]22 sowie Kristallstruktur von trans-(Ph3PNPPh3)2[OsO2(CN)2(OCH3)]2 / Vibrational Spectra and Normal Coordinate Analysis of the Dioxoosmates(VI) trans-[OsO2(CN)4]2-, trans-[OsO2 (CN)2(OH)]22- and trans-[OsO2(CN)2(OCH3]22- , and Crystal Structure of trans-(Ph3PNPPh3)2[OsO2(CN)2(OCH3)]2

1999 ◽  
Vol 54 (9) ◽  
pp. 1109-1115
Author(s):  
A. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Vibrational Spectra ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir And Raman

The crystal structure of trans-(Ph3PNPPh3)2[OsO2(CN)2(OCH3)]2 (triclinic, space group P1̄, a = 11.816(2), b = 13.480(3), c = 13.610(5) Å, α = 83.46(2), ß = 77.09(2), γ = 71.06(2)°, Z = 1) has been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra of the (n-Bu4N)-salts of trans-[OsO2(CN)4]2- (1), trans-[OsO2(CN)2(OH)]22- (2) and trans-[OsO2(CN)2(OCH3)]22- (3) were measured at room temperature. Based on the molecular parameters of the X-ray determination normal coordinate analyses have been performed and the vibrations are assigned. The valence force constants of 1 are fd(Os=O) = 6.5, fd(Os-C) = 2.62 and fd(C≡N ) = 16.85 mdyn/A, of 2 and 3 are fd(Os=O) = 6.7, fd(Os-C) = 2.55 and fd(C≡N ) = 16.95 mdyn/Å. fd(Os-O) ranges from 2.0 - 2.2 and for the methoxy bridge is fd(C-O) = 4.00 mdyn/Å

Two-dimensional lanthanide(III) coordination polymers: solvothermal synthesis, crystal structure, and stability

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Runmei Ding ◽  
Zixin He ◽  
Meilin Wang ◽  
Danian Tian ◽  
Peipei Cen
Keyword(s):  
Crystal Structure ◽  
Coordination Polymers ◽  
Solvothermal Synthesis ◽  
Analysis Data ◽  
Water Stability ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Solvothermal Conditions

AbstractBased on 2-(4-pyridyl)-terephthalate (H2pta) and oxalate ligands, two new lanthanide-containing coordination polymers (CPs), [Tb(pta)(C2O4)0.5(H2O)2)]·2H2O (1) and [Sm(pta)(C2O4)0.5(H2O)2)]·2H2O (2), have been synthesized under solvothermal conditions. The structures of both 1 and 2 have been determined by single-crystal X-ray diffraction. Infrared, elemental analysis, powder X-ray diffraction and thermogravimetric analysis data are also presented. The crystals of 1 and 2 exhibit isostructural layer-like networks, crystallizing in the triclinic space group P$‾{1}$. The layers are further stabilized and associated into 3D architectures through hydrogen bonding. Remarkably, the CPs 1 and 2 exhibit excellent water stability and remarkable thermostability with thermal decomposition temperatures of more than 420 °C.

scholarly journals Fogoite-(Y), Na3Ca2Y2Ti(Si2O7)2OF3, a Group I TS-block mineral from the Lagoa do Fogo, the Fogo volcano, São Miguel Island, the Azores: Description and crystal structure

2017 ◽  
Vol 81 (2) ◽  
pp. 369-381 ◽  
Author(s):  
F. Cámara ◽  
E. Sokolova ◽  
Y. A. Abdu ◽  
F. C. Hawthorne ◽  
T. Charrier ◽  
...  
Keyword(s):  
Crystal Structure ◽  
New Mineral ◽  
X Ray Diffraction ◽  
Titanium Silicate ◽  
Triclinic Space Group ◽  
X Ray ◽  
Group I ◽  
Mohs Hardness ◽  
Fogo Volcano ◽  
The Ideal

AbstractFogoite-(Y), Na3Ca2Y2Ti(Si2O7)2OF3, is a new mineral from the Lagoa do Fogo, São Miguel Island, the Azores. It occurs in cavities as highly elongated (on [001]) prisms, up to 2000 μm long and 50 μm× 50 μm in cross-section, associated with sanidine, astrophyllite, fluornatropyrochlore, ferrokentbrooksite, quartz and ferro-katophorite. Crystals are generally transparent and colourless, with vitreous lustre, occasionally creamy white. Fogoite-(Y) has a white streak, splintery fracture and very good {100} cleavage. Mohs hardness is ∼5. Dcalc. = 3.523 g/cm3. It is biaxial (+) with refractive indices (λ = 590 nm) α = 1.686(2), β = 1.690(2), γ = 1.702(5); 2Vmeas. = 57(1)° and 2Vcalc. = 60°. It is nonpleochroic. Fogoite-(Y) is triclinic, space group P1, a = 9.575(6), b = 5.685(4), c = 7.279(5) Å, α = 89.985(6), β = 100.933(4), γ = 101.300(5)°, V = 381.2 (7) Å3. The six strongest reflections in the powder X-ray diffraction data [d (Å), I, (hkl)] are: 2.954, 100, (1̄1̄2, 3̄10); 3.069, 42, (300, 01̄2); 2.486, 24, (310, 21̄2); 3.960, 23, (1̄1̄1, 2̄10); 2.626, 21, (2̄20); 1.820, 20, (1̄04). Electron microprobe analysis gave the following empirical formula calculated on 18 (O + F) (Na2.74Mn0.15)∑2.89Ca2[Y1.21(La0.01Ce0.03Nd0.03Sm0.02Gd0.08Dy0.08Er0.05Yb0.04Lu0.01)∑0.35Mn0.16Zr0.11Na0.09Fe0.072+Ca0.01]∑2(Ti0.76Nb0.23Ta0.01)∑1(Si4.03O14)O1.12F2.88, Z = 1. The crystal structure was refined on a twinnedcrystal to R1 = 2.81% on the basis of 2157 unique reflections (Fo > 4σFo) and is a framework of TS (Titanium Silicate) blocks, which consist of HOH sheets (H – heteropolyhedral, O – octahedral) parallel to (100). In the O sheet, the the [6]MO(1) site is occupied mainly by Ti, <MO(1)–ϕ> = 1.980 Å, and the [6]MO(2) and [6]MO(3) sites are occupied by Na and Na plus minor Mn, <MO(2)–ϕ>= 2.490 Å and <MO(3)–ϕ> = 2.378 Å. In the H sheet, the two [4]Si sites are occupied by Si, with <Si–O> = 1.623 Å; the [6]MH site is occupied by Y and rare-earth elements (Y > REE), with minor Mn, Zr, Na, Fe2+ and Ca, <MH–ϕ> = 2.271 Å and the [6]AP site is occupied by Ca, <AP–ϕ> = 2.416 Å. The MH and AP octahedra and Si2O7 groups constitute the H sheet. The ideal compositions of the O and two H sheets are Na3Ti(OF)F2 and Y2Ca2(Si2O7)2 apfu. Fogoite-(Y) is isostructural with götzenite and hainite. The mineral is named after the type locality, the Fogo volcano in the Azores.

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