The determination of crystal structure of chromium(II) phosphite dihydrate, CrHPO3 2 H2O

1987 ◽  
Vol 52 (7) ◽  
pp. 1742-1747 ◽  
Author(s):  
Jiří Brynda ◽  
Bohumil Kratochvíl ◽  
Ivana Císařová
Keyword(s):  
Crystal Structure ◽  
Heavy Atom ◽  
Cross Linking ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Interatomic Distances ◽  
Reliability Factor ◽  
Cell Parameters ◽  
Heavy Atom Method

The crystal structure of CrHPO3.2 H2O has been solved by the heavy atom method. The compound crystallizes in the orthorhombic space group P212121 with the unit cell parameters a = 679·25(8), b = 915·61(8), c = 752·2(1) pm, Z = 4. The structure was refined to the final reliability factor R = 0·043 for 1 040 observed reflexions (I > 1·96σ(I)). The structure consists of chains formed by CrO6 octahedra connected each other in vertices. The chains are interconnected by phosphite tetrahedra HPO3. Hydrogen bridges of water-phosphite tetrahedron and water-water types form space cross-linking of the whole structure. Bond distances Cr-O in the tetragonally distorted octahedron range from 201·2 to 304·9 pm. The interatomic distances P-O in phosphite tetrahedron are between 152·1 and 152·7 pm. The degree of the distorsion DISQ of HPO3 tetrahedron and CrO6 octahedron is discussed on the basis of known structures of phosphites and chromium(II) compounds.

Synthesis, vibrational spectra and single-crystal structure determination of lithium tricyanomethanide Li[C(CN)3]

2018 ◽  
Vol 73 (3-4) ◽  
pp. 225-229
Author(s):  
Olaf Reckeweg ◽  
Maurice Conrad ◽  
Armin Schulz ◽  
Francis J. DiSalvo ◽  
Thomas Schleid
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
Metathesis Reaction ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Cell Parameters ◽  
Related Compounds

AbstractThe long-elusive structure of lithium tricyanomethanide Li[C(CN)3] has been determined on the basis of material synthesized via a metathesis reaction of Ag[C(CN)3] with LiCl in water driven by AgCl precipitation and subsequently recrystallization from methanol. Li[C(CN)3] crystallizes in the non-centrosymmetric orthorhombic space groupIma2 with the unit-cell parametersa=751.06(4),b=1059.75(6) andc=563.27(3) pm adopting a unique structure with planar [C(CN)3]−anions exhibiting nearly ideal trigonal planarD3hsymmetry. The Li+cations are coordinated by five independent tricyanomethanide anions forming a distorted square pyramid with Li–N distances between 202 and 249 pm. The vibrational frequencies were also determined and along with other properties of Li[C(CN)3] compared with those of related compounds.

The Crystal Structure of S-Methyl 1-[Dicyclohexyl(thiophosphoryl)]-dithioformate: (c-C6H11)2P(S)C(S)Sme

1988 ◽  
Vol 41 (3) ◽  
pp. 405 ◽  
Author(s):  
BF Hoskins ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Mirror Plane ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Interatomic Distances ◽  
Full Matrix ◽  
Cell Parameters ◽  
Compound C

The crystal structure of the title compound, (c-C6H11)2P(S)C(S)SMe , has been determined and shows that the P(S)C(S)SC chromophore is situated on a crystallographic mirror plane with the cyclohexyl groups related to each other across this plane. Significant interatomic distances are: P=S 1.951(1), P-C 1.860(4), C=S 1.632(4) and C-S 1.700(4)Ǻ. A resonance scheme involving the delocalization of π-electrons over the CS2 moiety has been invoked to account for the observed C-S bond distances in the molecule. Crystals are orthorhombic, space group Pnma with unit cell parameters a 10.196(2), b 10.612(1) and c 15.370(3)Ǻ, and Z 4. The structure was solved by direct methods and refined by a full-matrix least-squares procedure to final R 0.045, Rw 0.047 for 1191 reflections with I ≥ 3.0σ(I).

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

scholarly journals The crystal and molecular structure of the bis(N,N,N′,N′-tetramethylethanediamine) adduct of I(Br)InInBr2, In2Br3I•2C6H16N2, an indium–indium bonded molecule

1984 ◽  
Vol 62 (3) ◽  
pp. 601-605 ◽  
Author(s):  
Masood A. Khan ◽  
Clovis Peppe ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Orthorhombic Space Group ◽  
Trigonal Bipyramidal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Distorted Trigonal Bipyramidal

The crystal structure of the title compound has been determined by the heavy atom method. The crystals are orthorhombic, space group Pbca, with unit cell dimensions a = 22.795(3) Å, b = 17.518(2) Å, c = 12.396(3) Å, Z = 8; R = 0.0409 for 1527 unique "observed" reflections. The structure is disordered, with each halogen site (X) occupied by 75% Br, 25% I. The molecule consists of two X2(tmen)In units (tmen = N,N,N′,N′-tetramethylethanediamine) with distorted trigonal bipyramidal geometry, joined by an In—In bond 2.775(2) Å in length.

Determination of the Crystal Structure and Redefinition of Tsugaruite, Pb28As15S50Cl, the First Lead-Arsenic Chloro-Sulfosalt

2020 ◽  
Author(s):  
Cristian Biagioni ◽  
Luca Bindi ◽  
Koichi Momma ◽  
Ritsuro Miyawaki ◽  
Yoshitaka Matsushita ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Atomic Ratio ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Specific Position ◽  
Actual Classification ◽  
Aomori Prefecture

Abstract Tsugaruite was originally defined as a lead-arsenic sulfosalt from the Yunosawa mine, Aomori Prefecture, Japan. Until recently its crystal structure remained unsolved and its actual classification in the sulfosalt realm was unknown. Here the refinement of the crystal structure of tsugaruite using single-crystal X-ray diffraction data is reported. The mineral is orthorhombic, space group P2nn, with unit-cell parameters a = 8.0774(10), b = 15.1772(16), c = 38.129(4) Å, V = 4674.3(9) Å3, in agreement with previous studies. The solution of the crystal structure of this mineral revealed Cl occupying a specific position. Chlorine was thus sought and found using the electron microprobe; the average of six spot analyses gave (in wt.%): Pb 68.04, As 12.83, S 18.29, Cl 0.63, total 99.80. The empirical formula, calculated on the basis of Pb + As = 43 atoms per formula unit, is Pb28.26As14.74S49.08Cl1.52. Tsugaruite is an N = 4 plesiotypic derivative of the homologous series of Pb-Sb chloro-sulfosalts having the general formula Pb(2+2N)(Sb,Pb)(2+2N)S(2+2N)(S,Cl)(4+2N)ClN. It has a Cl/(Cl + S) atomic ratio close to that of other known Pb-Sb chloro-sulfosalts (pillaite, pellouxite) and slightly higher than that of dadsonite.

scholarly journals The crystal structure of alstonite, BaCa(CO3)2: an extraordinary example of ‘hidden’ complex twinning in large single crystals

2020 ◽  
Vol 84 (5) ◽  
pp. 699-704
Author(s):  
Luca Bindi ◽  
Andrew C. Roberts ◽  
Cristian Biagioni
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Unit Cell ◽  
Crystal Structure Determination ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
Structure Determinations

AbstractAlstonite, BaCa(CO3)2, is a mineral described almost two centuries ago. It is widespread in Nature and forms magnificent cm-sized crystals. Notwithstanding, its crystal structure was still unknown. Here, we report the crystal-structure determination of the mineral and discuss it in relationship to other polymorphs of BaCa(CO3)2. Alstonite is trigonal, space group P31m, with unit-cell parameters a = 17.4360(6), c = 6.1295(2) Å, V = 1613.80(9) Å3 and Z = 12. The crystal structure was solved and refined to R1 = 0.0727 on the basis of 4515 reflections with Fo > 4σ(Fo) and 195 refined parameters. Alstonite is formed by the alternation, along c, of Ba-dominant and Ca-dominant layers, separated by CO3 groups parallel to {0001}. The main take-home message is to show that not all structure determinations of minerals/compounds can be solved routinely. Some crystals, even large ones displaying excellent diffraction quality, can be twinned in complex ways, thus making their study a crystallographic challenge.

Crystal structure determination of non-stoichiometric Ca4−xRuO6−x (x = 1.17) from X-ray powder diffraction data

2016 ◽  
Vol 31 (1) ◽  
pp. 59-62
Author(s):  
Martin Etter ◽  
Maximilian J. Krautloher ◽  
Nakheon Sung ◽  
Joel Bertinshaw ◽  
Bumjoon Kim ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Flux Growth ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Growth Method ◽  
Calcium Ruthenate

A new non-stoichiometric calcium ruthenate [Ca4−xRuO6−x with x = 1.17(1)] was synthesized by the flux growth method and characterized by the X-ray powder diffraction. The crystal structure is isostructural to the K4CdCl6 type with space group R$\bar 3$c. Unit-cell parameters are a = 9.2881(1), c = 11.1634(2) Å, V = 834.03(3) Å3, and Z = 6.

Crystal structure and topological affinities of magbasite, KBaFe3+Mg7Si8O22(OH)2F6: a trellis structure related to amphibole and carpholite

2014 ◽  
Vol 78 (1) ◽  
pp. 29-45 ◽  
Author(s):  
M. D. Welch ◽  
R. H. Mitchell ◽  
A. R. Kampf ◽  
A. R. Chakhmouradian ◽  
D. Smith ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Carbonatite Complex ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
Structural Relations ◽  
Final Agreement

AbstractThe crystal structure of magbasite from the Eldor carbonatite complex, Quebec, Canada, has been determined and indicates that the currently accepted formula should be revised to KBaFe3+Mg7Si8O22(OH)2F6. Magbasite is orthorhombic, space group Cmme (Cmma), with unit-cell parameters a 18.9506(3) Å, b 22.5045(3) Å, c 5.2780(1) Å, V 2250.93(6) Å3 (Z = 4). The structure has been solved and refined to final agreement indices R1 = 0.026, wR2 = 0.052, GooF = 1.116 for a total of 2379 unique reflections, and is a new kind of trellis motif related to amphibole and carpholite topologies. An amphibole-like I-beam ‖(100) of edge-sharing octahedrally-coordinated M(1,2,3) sites, which are filled by Mg, is sandwiched between double-chains of SiO4 tetrahedra ‖c. This I-beam is connected to side-ribbons ‖(010) of edge-sharing (Mg,Fe2+)O4(OH,F)2 and Fe3+O4(OH)2 octahedra to form a tunnelled box or trellis structure very like that of carpholite, for which the I-beams are pyroxene-like. K occupies a tunnel site analogous to the A site of amphibole. Ba occupies a cavity site at the corners where the I-beam and side-ribbon meet, and corresponds to the A site of carpholite. The structural relations between magbasite and carpholite are discussed.

Weissite from Gambatesa mine, Val Graveglia, Liguria, Italy: occurrence, composition and determination of the crystal structure

2013 ◽  
Vol 77 (4) ◽  
pp. 475-483 ◽  
Author(s):  
L. Bindi ◽  
C. Carbone ◽  
D. Belmonte ◽  
R. Cabella ◽  
R. Bracco
Keyword(s):  
Crystal Structure ◽  
Vickers Hardness ◽  
Crystal Chemical ◽  
Chemical Formula ◽  
Unit Cell Parameters ◽  
Cell Parameters ◽  
Black Streak ◽  
Pure Metals ◽  
Complex Crystal

AbstractWeissite, Cu2–xTe (x ≈ 0.21), a very rare copper telluride, occurs in a sample from the Gambatesa mine, Val Graveglia, Liguria, Italy, where it occurs as purplish black anhedral grains up to 0.1 mm in length and shows a black streak. No cleavage is observed and the Vickers hardness (VHN100) is 142 kg/mm2. Weissite is dark bluish black, weakly pleochroic, and moderately anisotropic in bluish tints. Reflectance percentages in air for Rmin and Rmax are 37.0, 38.4 (471.1 nm), 33.2, 34.2 (548.3 nm), 31.2, 32.1 (586.6 nm), and 28.6, 31.0 (652.3 nm), respectively.Weissite is trigonal and belongs to the space group P3m1 with the following unit-cell parameters: a = 8.3124(7) Å, c = 21.546(1) Å, V = 1289.3(2) Å3, and Z = 24. Electron microprobe analyses gave the chemical formula (Cu1.62Ag0.04Au0.04Fe0.04Sb0.04)Σ=1.78(Te0.96S0.02Se0.02). The crystal structure has been solved and refined to R = 1.95%. It consists of Cu and Te polyhedra forming complex crystal-chemical environments as is typical of many intermetallic compounds. The exceedingly short bond distances observed among the metals are discussed in relation to other copper tellurides and pure metals.

The crystal structure of Cu2GeSe3 and the structure-types of the I2-IV-VI3 family of semiconducting compounds

2021 ◽  
Vol 77 (1) ◽  
pp. 158-167
Author(s):  
Analio Dugarte-Dugarte ◽  
Nahum Ramírez Pineda ◽  
Luis Nieves ◽  
José Antonio Henao ◽  
Graciela Díaz de Delgado ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Initial Report ◽  
Space Group ◽  
Cell Parameters ◽  
Semiconducting Compounds ◽  
Bond Valence Model

Almost 50 years after the initial report, the crystal structure of Cu2GeSe3, a I2-IV-VI3 semiconductor, has been revised using modern single-crystal X-ray diffraction data. The structure of this material can be properly described in the monoclinic space group Cc (No. 9) with unit-cell parameters a = 6.7703 (4) Å, b = 11.8624 (5) Å, c = 6.7705 (4) Å, β = 108.512 (6)°, V = 515.62 (5) Å3, Z = 4, rather than in the orthorhombic space group Imm2 (No. 44) with unit-cell parameters a = 11.860 (3), b = 3.960 (1), c = 5.485 (2) Å, V = 257.61 Å3, Z = 2, as originally proposed [Parthé & Garín (1971). Monatsh. Chem. 102, 1197–1208]. Contrary to what was observed in the orthorhombic structure, the distortions of the tetrahedra in the monoclinic structure are consistent with the distortions expected from considerations derived from the bond valence model. A brief revision of the structures reported for the I2-IV-VI3 family of semiconducting compounds (I: Cu, Ag; IV: Si, Ge, Sn; and VI: S, Se, Te) is also presented.

Sign in / Sign up

Export Citation Format

Share Document