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).

scholarly journals Multianvil High-Pressure/High-Temperature Synthesis and Characterization of multiferroic HP-Co3TeO6

2021 ◽  
Author(s):  
Gunter Heymann ◽  
Elisabeth Selb ◽  
Toni Buttlar ◽  
Oliver Janka ◽  
Martina Tribus ◽  
...  
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Type Structure ◽  
Synthesis And Characterization ◽  
Temperature Synthesis ◽  
Space Group ◽  
Crystal System ◽  
High Temperature Synthesis ◽  
High Pressure High Temperature

By high-pressure/high-temperature multianvil synthesis a new high-pressure (HP) phase of Co3TeO6 was obtained. The compound crystallizes in the acentric trigonal crystal system of the Ni3TeO6-type structure with space group R3...

Kristallstrukturen der iodierten closo-Hexaborate trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P)2[B6H2I4] · 2 CH3CN und (CH2Py2)[B6HI5]/Crystal Structures of the Iodized closo-Hexaborates trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P )2[B6H2I4] · 2 CH3CN and (CH2Py2)[B6HI5]

1998 ◽  
Vol 53 (2) ◽  
pp. 206-210 ◽  
Author(s):  
D. Sonnak ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

Abstract X-ray structure determinations have been performed on single crystals of trans-(Ph4P)2-[B6H4I2] (1) (triclinic, space group P1̄, a = 9.9680(12), b = 10.9690(11), c = 11.0470(14) Å,α = 88.167(9), β = 80.466(12), γ = 68.839(11)°, Z = 1), mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2 (2)(triclinic, space group P1̄, a = 11.8694(11), b = 15.1699(13), c = 17.051(2) Å, α = 75.118(9), β = 71.953(10), γ = 69.331(8)°, Z = 2), trans-(Ph4P )2[B6H2I4] · 2 CH3CN (3) (monoclinic, space group P21/n, a = 14.9665(10), b = 7.6783(10), c = 23.385(3) Å, β = 95.78(9)°, Z = 2), and (CH2Py2)[B6HI5] (4) (orthorhombic, space group Pnma, a = 13.660(2), b = 11.8711(13), c = 13.839(2) Å, Z = 4). The B6 octahedra are compressed in the direction of the B-I bonds, resulting in shortened diagonal B ··· B distances with average values of the groups I-B ··· B-I = 2.37 and I-B ··· B-H = 2.43 Å as compared with H-B ··· B-H = 2.49 Å.

Isoselenocyanatoborate -Kristallstrukturen von (n-Bu4N)[BH(NCSe)3] und (Ph4P)[B3H7(NCSe)] / Isoselenocyanatoborates -Crystal Structures of (n-Bu4N)[BH(NCSe)3] and (Ph4P)[B3H7(NCSe)]

1998 ◽  
Vol 53 (3) ◽  
pp. 271-274 ◽  
Author(s):  
B. Steuer ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Elemental Selenium ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Average Bond

Abstract The treatment of [B6H6]2- with an excess of (SCN)2 in dichloromethane in the presence of solid KOH gives the hexaisoselenocyanatodiborate anion [B2(NCSe)6]2- as an intermediate (δ(11B) = -10.3 ppm), from which [BH(NCSe)3]- and elemental selenium are formed. The X-ray structure determinations on single crystals of (n-Bu4N)2[BH(NCSe)3] (1) (triclinic, space group Pi with a = 8.512(2), b = 10.885(3), c = 14.895(4) Å, α = 79.52(2), β = 74.86(2), γ = 86.768(2)°, Z = 2) and (Ph4P)[B3H7(NCSe)] (2) (monoclinic, space group C2, a = 7.686(5), b = 10.366(3), c = 17.533(3) A, β = 108.89°, Z = 4) show that the selenocyanate groups are coordinated exclusively via the N atoms with average bond lengths of B-N = 1.52, C-N = 1.15, C-Se = 1.75 A and angles N-C-Se = 179°, B-N-C = 168.7 - 176.8°. The N-B-N angles of 1 range from 107.5 to 109.5°.

Synthesis and Characterization of Bromo- and Bromochloroplumbates(II). Crystal Structures of [Ph4E]2[Pb3Br8] (E = P, As) and [Ph4P][PbBrCl2] • CH3CN

2000 ◽  
Vol 55 (5) ◽  
pp. 377-382 ◽  
Author(s):  
Thomas M. Klapötke ◽  
Burkhard Krumm ◽  
Kurt Polbom ◽  
Claudia M. Rienäcker
Keyword(s):  
Crystal Structures ◽  
Lattice Parameters ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group

[Ph4P]2[Pb3Br8] and [Ph4As]2[Pb3Br8] crystallize both in the monoclinic space group P 21/n. The lattice parameters of [Ph4P]2[Pb3Br8] are a = 14.637(7), b = 8.151(3), c = 23.388(8) Å, β = 106.02(3)°, Z = 2 and of [Ph4As]2[Pb3Br8] are a = 14.697(7), b = 8.219(3), c = 23.527(8) Å, β = 106.27(3)°, Z = 2. The lattice parameters of [Ph4P][PbBrCl2]·CH3CN, which crystallizes in the triclinic space group (P 1̅), are a = 9.435(3), b = 10.2577(14), c = 14.055(2) Å, α = 88.320(11)°, β = 84.82(2)°, γ = 84.19(2)°, Z = 2. 207Pb NMR shifts of halogenoplumbates in solution are reported.

scholarly journals High-Pressure, High-Temperature Synthesis and Characterization of Polar and Magnetic LuCrWO6

2020 ◽  
Vol 59 (6) ◽  
pp. 3579-3584
Author(s):  
Sun Woo Kim ◽  
Xiaoyan Tan ◽  
Corey E. Frank ◽  
Zheng Deng ◽  
Huaiyu Wang ◽  
...  
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Synthesis And Characterization ◽  
Temperature Synthesis ◽  
High Temperature Synthesis ◽  
High Pressure High Temperature

The Crystal Structures of 2-(3’-Hydroxypropyl)benzimidazolium Hexa- and Tetrachloroplatinate

2005 ◽  
Vol 60 (2) ◽  
pp. 164-168 ◽  
Author(s):  
A. Elmali ◽  
Y. Elerman ◽  
G. Eren ◽  
F. Gümüş ◽  
I. Svoboda
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Intermolecular Hydrogen Bonds ◽  
Triclinic Space Group ◽  
Space Group

2-(3’-Hydroxypropyl)benzimidazolium (Hhpb) hexa- and tetrachloroplatinate (C10H13N2O)2·[PtCl6] 1 and (C10H13N2O)2·[PtCl4] 2 were synthesized and their crystal structures determined. Compound 1 is monoclinic, space group P21/n, a = 8.800(1), b = 14.389(2), c = 10.264(2) Å, β = 98.540(10)°, V = 1285.3(3) Å3, Z = 2 and Dc = 1.959 g cm−3. Compound 2 is triclinic, space group P1̄, a=7.8480(10), b=9.0460(10), c=9.6980(10) Å ,α =65.420(10), β =68.810(10), γ = 76.770(1)°,V =581.26(4) Å3, Z =1 and Dc =1.969 g cm−3. In both compounds, the Pt atoms reside at a centre of inversion. Compounds 1 and 2 are comprised of 2-(3’-hydroxypropyl)benzimidazolium (Hhpb)+: (C10H12N2O)+ and [PtCl6]2− and [PtCl4]2− ions, respectively, linked by intermolecular hydrogen bonds N...Cl [range from 3.428(3) to 3.584(4) Å ], N···O [2.769(5) Å ] and O···Cl [3.338(4) and 3.321(3) Å ] for 1, and N···Cl [3.162(7) Å ], N···O [2.749(8) Å ] and O···Cl [3.289(6) Å ] for 2.

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.

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalysen von trans-[PtX2(acac)2], X = CI, Br, I, SCN / Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of trans-[PtX2(acac)2], X = Cl, Br, I, SCN

1996 ◽  
Vol 51 (10) ◽  
pp. 1400-1406 ◽  
Author(s):  
D. Rickert ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Normal Modes ◽  
Force Constants ◽  
Monoclinic Space Group ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Valence Force ◽  
Space Group ◽  
X Ray ◽  
Modes Of Vibration

The crystal structures of trans-[PtCl2(acac)2](monoclinic, space group P21/c, a - 7.616(5), b = 12.759(5), c = 7.892(5) Å, β = 118.459(5)°, Z = 2), trans-[PtBr2(acac)2] (triclinic, space group P1̅, a = 7.502(5), b = 7.665(5), c = 8.155(5) Å, α = 114~508(5), β = 94.537(5), γ = 117.669(5)°. Z = 1) and trans-[Pt(SCN)2(acac)2] (triclinic, space group P1̅ , a = 7.9095(10), b = 7.9393( 10), c = 7.9631 Å, a = 114.051 (10), β = 100.955(10), γ = 100.573(10)°, Z = 1) have been determined by single crystal X-ray diffraction analysis. The crystal structure of trans- [Ptl2(acac)2] is known from the literature. To enhance the spectroscopic resolution, the IR and Raman spectra of the four complexes have been measured at low temperature (10 K). Using the X-ray data, normal coordinate analyses based on a modified valence force field have been performed and the normal modes of vibration for the octahedral skeleton [PtX2O4] have been assigned. With a set of 19 or 23 force constants taking into account the inner-ligand vibrations a good agreement between observed and calculated frequencies has been achieved. The valence force constants are e.g.fd (PtCl) = 2.16, fd (PtBr) = 1.45, fd (PtI) = 1.01, fd (PtS) = 1.80 mdyn/Å, and fd (PtO) ranges from 1.89 to 1.91 mdyn/Å.

Structural Studies of Complexes of Tridentate Terimine Systems. Crystal Structure of Bis(2,2′:6′,2′′-terpyridine)ruthenium(II) Perchlorate Hydrate, Bis(2,2′:6′,2′′-terpyridine)- osmium(II) Perchlorate Hemihydrate and Bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)amine)iron(II) Tetrafluoroborate Dihydrate

1998 ◽  
Vol 51 (12) ◽  
pp. 1131 ◽  
Author(s):  
Donald C. Craig ◽  
Marcia L. Scudder ◽  
Wendy-Anne McHale ◽  
Harold A. Goodwin
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Metal Ion ◽  
Chelate Ring ◽  
Monoclinic Space Group ◽  
Structural Studies ◽  
Triclinic Space Group ◽  
Space Group ◽  
Membered Chelate Ring ◽  
Group I

The crystal structures of bis(2,2′:6′,2″-terpyridine)ruthenium(II) perchlorate hydrate, bis(2,2′:6′,2″- terpyridine)osmium(II) perchlorate hemihydrate and bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)- amine)iron(II) tetrafluoroborate dihydrate are described. In the terpyridine complexes the ruthenium-nitrogen distances and the corresponding osmium-nitrogen distances are not significantly different. In both complexes the ligand geometry and the metal ion environment show the distortions usual for bis(terpyridine) systems. Distortions are less marked in the bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)amine)iron(II) cation in which each tridentate unit forms one five-membered and one six-membered chelate ring. [Ru(trpy)2] [ClO4]2.(H2O)1.1: tetragonal, space group I 41/a, a, b 12·527(2), c 40·202(11) Å, Z 8. [Os(trpy)2] [ClO4]2.(H2O)0·5: monoclinic, space group P 21/n, a 8·842(3), b 8·861(1), c 39·22(2) Å, β93·89(2)°, Z 4. [Fe(phpyam)2] [BF4]2.(H2O)2: triclinic, space group P -1, a 12·43(1), b 12·45(1), c 13·35(1) Å, α 62·70(10), β 78·55(8), γ 72·46(9)°, Z 2.

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