X-ray diffraction study of middlebackite [CuII2C2O4(OH)2, di-copper oxalate dihydroxide], using a mineral specimen from Mooloo Downs Station, Western Australia and chemically synthesized material

2019 ◽  
Vol 34 (4) ◽  
pp. 311-324
Author(s):  
B. H. O'Connor ◽  
R. M. Clarke ◽  
J. A. Kimpton ◽  
D. G. Allen
Keyword(s):  
Western Australia ◽  
A Priori ◽  
South Australia ◽  
Lattice Parameters ◽  
The Other ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Calculated Density ◽  
Copper Oxalate ◽  
X Ray

Additional crystallographic data are given for the recently reported mineral middlebackite, which has been described for discoveries at Iron Knob in South Australia and Passo di San Lugano near Trento, Italy. The material examined in the present study was from a third finding of the mineral, viz. from a quartz outcrop at Mooloo Downs Station in Western Australia within which it was co-located with the chemically- and structurally-related mineral moolooite, CuIIC2O4·nH2O, reported by Clarke and Williams (1986). In this study, the crystal structure was elucidated independently of the other studies using a combination of the a priori charge flipping and simulated annealing methods with synchrotron radiation diffraction (SRD) powder data. The principal crystal data for the Mooloo Downs material are: space group P21/c with lattice parameters a = 7.2659(18) Å, b = 5.7460(11) Å, c = 5.6806(11) Å, β = 104.588(3)°; Vc = 229.46(18) Å3; empirical formula CuII2C2O4(OH)2 with 2 formula units per unit cell; and calculated density = 3.605 g cm−3. The lattice parameters agree approximately with values given for the other studies, but not within the reported error estimates. The atom coordinates, interatomic distances, and angles for the Mooloo Downs material are compared with those from the other studies using single crystal data, with the values from all three studies agreeing approximately, but again not within the reported uncertainties. The crystal chemistry found for middlebackite received strong confirmation through the synthesis for the first time of di-copper oxalate di-hydroxide. Laboratory X-ray diffraction powder data for the synthetic form of the mineral from this study agree closely with the SRD data for the natural mineral.

Moolooite, a naturally occurring hydrated copper oxalate from Western Australia

1986 ◽  
Vol 50 (356) ◽  
pp. 295-298 ◽  
Author(s):  
R. M. Clarke ◽  
I. R. Williams
Keyword(s):  
Western Australia ◽  
Copper Ions ◽  
Orthorhombic Symmetry ◽  
X Ray Diffraction ◽  
Absorption Bands ◽  
Calculated Density ◽  
Copper Oxalate ◽  
Naturally Occurring ◽  
Diffraction Patterns ◽  
Bird Guano

AbstractMoolooite, a naturally occurring hydrated copper oxalate has been identified in a sulphide-bearing quartz outcrop 12 km east of Mooloo Downs station homestead (25° 01′ 30″ S., 116° 06′ 30″ E.), Western Australia. It has apparently formed by the interaction of solutions derived from bird guano and weathering copper sulphides. Partial microchemical analysis indicates a composition corresponding to CuC2O4 · 0.44H2O. The infra-red spectrum is similar to that of the artificial compound with diagnostic absorption bands at 3490, 2975, 2935, 1980, 1940, 1660, 1365,1320, 830, 510, 390, and 315 cm−1. Powder X-ray diffraction patterns indicate a disordered structure with orthorhombic symmetry; a 5.35, b 5.63, c 2.56 Å, Z = 1. The strongest lines of the powder pattern are [d Å, I, hkl]: 3.88, 100, (110); 2.50, 30, (120); 2.33, 18, (011); 2.31, 25,(101); 2.14, 20, (111); 1.938, 18, (220); 1.787, 25, (121); 1.753, 30, (211); 1.216, 15, (112). Unindexed very weak diffuse lines on some patterns can be indexed assuming a supercell with a′ = a, b′ = 2b, c′ = 2c indicating the presence of ordered crystallites.Moolooite occurs as micro-concretionary crusts and powder in cracks and solution cavities resulting from sulphide oxidation. It is found associated with opaline silica, gypsum, broehantite, antlerite, atacamite, whewellite, sampleite, and libethenite. It is turquoise-green in colour with similar streak, lustre dull to waxy, calculated density 3.43 g/cm3. Moolooite is composed of aggregates of generally sub-micrometre sized equidimensional crystallites with α ∼ 1.57 and γ ∼ 1.95.By analogy with artificial copper oxalate, moolooite is constructed from infinite ribbon-like elementary structural units consisting of alternating Cu2+ and (C2O4)2− ions. These units are arranged en echelon in layers which are stacked with displacements so that octahedral coordination of copper ions is completed by oxygen atoms in adjacent layers. The minimal role played by water in the structure and composition of moolooite distinguish it from other oxalate minerals. Because of the zeolitic character of the water a general formula CuC2O4 · nH2O (0 ⩽ n ⩽ 1) appears to be appropriate.

Crystal data for ternary compounds of the system Cu–As2Se3

1987 ◽  
Vol 20 (4) ◽  
pp. 323-323
Author(s):  
C. A. Majid ◽  
M. A. Hussain
Keyword(s):  
Diffraction Data ◽  
Lattice Parameters ◽  
Structural Studies ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Ternary Compounds

Structural studies of polycrystalline CuAsSe2, Cu3AsSe4 and Cu3AsSe3 are reported. These were found to be cubic with space group Pm{\bar 3}m and lattice parameters as follows: (1) CuAsSe2: a = 5.513(4) Å, V = 167.47(1) Å3, Z = 2; Dm = 5.56(6), Dx = 5.88 g cm−3. (2) Cu3AsSe4: a = 5.530(5) Å; V = 169.11(2) Å3; Z = 1; Dm = 5.51(5), Dx = 5.75 g cm−3. (3) Cu3AsSe3: a = 5.758(9) Å, V = 190.87(3) Å3, Z = 1, Dm = 5.03(9), Dx = 4.45 g cm−3. X-ray diffraction data using a Rigaku DMAX-IIIA diffractometer and Cu Kα radiation.

Lattice parameters and spontaneous strain in AX 2 polytypes: CdI2, PbI2 SnS2 and SnSe2

1989 ◽  
Vol 22 (6) ◽  
pp. 622-623 ◽  
Author(s):  
B. Pałosz ◽  
E. Salje
Keyword(s):  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Basal Plane ◽  
Lattice Parameter ◽  
Structural Transformations ◽  
Lattice Parameters ◽  
The Other ◽  
X Ray Diffraction ◽  
Spontaneous Strain ◽  
X Ray

Structural transformations between polytypes of a given material are expected to lead to lattice relaxations. Powder X-ray diffraction of basic AX 2 polytypes of CdI2, PbI2, SnS2 and SnSe2 showed these relaxations for the repetition unit along the stacking axis, conventionally the c axis. No variation of the lattice parameters were detected in the basal plane (001), except for CdI2 where small variations occur also for the a lattice parameter. The tensor of the spontaneous strain has its maximum component e 3 ≲ 12 × 10−4 for SnS2. The powder diffraction pattern and lattice parameters of the phases of CdI2 (2H, 12R, 4H), PbI2 (2H, 12R), SnS2 (2H, 18R, 4H) and SnSe2 (2H, 18R) are given. JCPDS Diffraction File Nos. are: 40-1468 for CdI2-12H; 40–1469 for CdI2-2H; 40-1466 for SnS2-18R, 40–1467 for SnS2-2H; 40–1465 for SnSe2-18R. The other polytypes studied in this paper have data in earlier sets of the PDF.

Bildung eines Kupfer-Nitratokomplexes aus einem Azidokomplex und Ozon. Die Kristallstruktur von (PPh4)2[CuCl(NO3)3] · CH2Cl2/ Formation of a Copper Nitrato Complex from an Azido Complex. Crystal Structure of (PPh4)2[CuCl(NO3)3] · CH2Cl2

1992 ◽  
Vol 47 (1) ◽  
pp. 31-34 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Alfred D. Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Coordination Number ◽  
The Other ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Complex Crystal Structure ◽  
Monodentate Ligands ◽  
Complex Crystal

(PPh4)2[CuCl(NO3)3] · CH2Cl2 is formed when ozone reacts with (PPh4)2[Cu2(N3)6] in dichloromethane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1113(1), b = 1156(1), c = 1965(2) pm , α = 101.02(1), β = 93.74(1), γ = 104.05(2)° at 130 K, space group P1̄, Z = 2, R = 0.057 for 3951 observed reflexions. The structure contains CH2Cl2 molecules and PPh4+ and [CuCl(NO3)3]2- ions, with copper having coordination number 5. One nitrate ligand acts as a bidentate chelating unit, and the other two as monodentate ligands.

Twinning and incommensurate modulation in baumoite, Ba0.5[(UO2)3O8Mo2(OH)3](H2O)~3, the first natural Ba uranyl molybdate

2019 ◽  
Vol 83 (4) ◽  
pp. 507-514
Author(s):  
Peter Elliott ◽  
Jakub Plášil ◽  
Václav Petříček ◽  
Jiří Čejka ◽  
Luca Bindi
Keyword(s):  
South Australia ◽  
New Mineral ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Calculated Density ◽  
X Ray ◽  
Cell Parameters ◽  
Orange Yellow ◽  
Incommensurate Modulation ◽  
Mohs Hardness

ABSTRACTBaumoite, Ba0.5[(UO2)3O8Mo2(OH)3](H2O)~3, is a new mineral found near Radium Hill, South Australia, where it occurs in a granite matrix associated with baryte, metatorbernite, phurcalite and kaolinite. Baumoite forms thin crusts of yellow to orange–yellow tabular to prismatic crystals. The mineral is translucent with a vitreous lustre and pale yellow streak. Crystals are brittle, the fracture is uneven and show one excellent cleavage. The Mohs hardness is ~2½. The calculated density is 4.61 g/cm3. Optically, baumoite crystals are biaxial (–), with α = 1.716(4), β = 1.761(4), γ = 1.767(4) (white light); and 2Vcalc= 42.2°. Electron microprobe analyses gave the empirical formula Ba0.87Ca0.03Al0.04U2.97Mo2.02P0.03O22H11.99, based on 22 O atoms per formula unit. The eight strongest lines in the powder X-ray diffraction pattern are [dobsÅ (I) (hkl)]: 9.175(39)(12${\bar 1}$), 7.450(100)(020), 3.554(20)(221), 3.365(31)(004, 202), 3.255(31)(123, 30${\bar 2}$), 3.209(28)(12${\bar 4}$), 3.067(33)(30${\bar 3}$, 222, 32${\bar 2}$) and 2.977(20)(142). Single-crystal X-ray studies (R1= 5.85% for 1892 main reflections) indicate that baumoite is monoclinic, superspace groupX2/m(a0g)0swithX= (0,½,0,½), with unit-cell parameters:a= 9.8337(3),b= 15.0436(5),c= 14.2055(6) Å, β = 108.978(3)°,V= 1987.25(13) Å3andZ= 4. The crystal structure is twinned and incommensurately modulated and is based upon sheets of U6+and Mo6+polyhedra of unique topology. Four independent cationic sites partially occupied by Ba atoms are located between the sheets, together with H2O molecules.

Crystal and Molecular Structures of the Functional Lithium Cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph, Me

2000 ◽  
Vol 55 (11) ◽  
pp. 1005-1010 ◽  
Author(s):  
Ulrich Jürgen Bildmann ◽  
Martin Winkler ◽  
Gerhard Müller Fachbereich
Keyword(s):  
Solid State ◽  
Functional Group ◽  
Molecular Structures ◽  
The Other ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal and molecular structures of the phosphinomethyl-substituted lithium cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph (1), Me (2) (tmeda = N,N,N',N'-tetramethylethylenediamine) were determined as their tmeda adducts on the basis of low temperature single crystal X-ray diffraction. (Crystal data: 1: monoclinic, space group P21/n, a = 8.511(5), b = 11.936(2), c = 24.20(1) Å, β = 90.02(3)°, Z = 4.2: monoclinic, space group P21/n, a = 10.887(2), b = 13.326(2), c = 13.131(2) Å, β= 92.872(6)°, Z = 4). In both compounds lithium has a slightly distorted 17 coordination to the cyclopentadienide (Cp) ring. There are no interactions between lithium and the phosphine donors in the solid state as the phosphinomethyl substituents are oriented to the other side of the Cp ring for steric reasons. The isopropene-substituted lithium cyclopentadienide, which is formed as a by-product in the synthesis of phosphinomethyl cyclopentadienides containing a CMe2 bridge, was also structurally characterized as its tmeda adduct [Li(tmeda)][H2C=CMeC5H4] (3). (Crystal data: monoclinic, P21/c, a = 8.00(2), b = 16.701(2), c = 11.942(6) Å, β= 112.68(7)°, Z = 4). As in 1 and 2, lithium is η5 -coordinated to the Cp ring, and there is no interaction of the functional group (isopropene) with lithium.

Electron density and electrostatic properties of two peptide molecules: tyrosyl-glycyl-glycine monohydrate and glycyl-aspartic acid dihydrate

2000 ◽  
Vol 56 (4) ◽  
pp. 728-737 ◽  
Author(s):  
Virginie Pichon-Pesme ◽  
Hassane Lachekar ◽  
Mohamed Souhassou ◽  
Claude Lecomte
Keyword(s):  
High Resolution ◽  
Electron Density ◽  
Diffraction Data ◽  
Experimental Studies ◽  
Lattice Parameters ◽  
Crystal Data ◽  
Topological Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electrostatic Properties

The electron density and electrostatic properties of Tyr-Gly-Gly and Gly-Asp molecules have been determined from high-resolution X-ray diffraction data at 123 K. Topological properties of the charge distribution are discussed and compared with those derived from other experimental studies on peptide molecules, and the characteristics of the (3,−1) critical points of the C=O, C—N, C—C bonds are analysed. Crystal data for Tyr-Gly-Gly: C13H17N3O5·H2O, Mr = 313, orthorhombic, P212121, Z = 4, T = 123 ± 2 K; lattice parameters: a = 7.984 (2), b = 9.535 (3), c = 18.352 (5) Å, V = 1397.1 (6) Å3, Dx = 1.49 g cm−3, μ = 1.2 cm−1 for λMo = 0.7107 Å. Crystal data for Gly-Asp: C6H10N2O5·2H2O, Mr = 212, orthorhombic, P212121, Z = 4, T = 123 ± 2 K; lattice parameters: a = 9.659 (1), b = 9.672 (1), c = 10.739 (1) Å, V = 1003.3 (4) Å3, Dx = 1.40 g cm−3, μ = 1.3 cm−1 for λMo = 0.7107 Å.

Middlebackite, a new Cu oxalate mineral from Iron Monarch, South Australia: Description and crystal structure

2018 ◽  
Vol 83 (03) ◽  
pp. 427-433 ◽  
Author(s):  
Peter Elliott
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
South Australia ◽  
Monoclinic Space Group ◽  
Formula Unit ◽  
X Ray Diffraction ◽  
Calculated Density ◽  
X Ray ◽  
Perfect Cleavage ◽  
Mohs Hardness

AbstractMiddlebackite is a new supergene mineral formed in the upper levels of the Iron Monarch quarry, South Australia. It occurs as aggregates of blue, prismatic crystals up to 0.3 mm across comprising individual crystals up to 0.05 mm in length associated with atacamite and mottramite. Crystals are translucent with a vitreous lustre and have a pale blue streak. Middlebackite is brittle with one perfect cleavage and uneven fracture. Mohs hardness is ~2. The calculated density is 3.64 g cm–3. Crystals are biaxial (+) with α = 1.663(4), β = 1.748(4) and γ = 1.861(4) (measured in white light). The calculated 2V is 86.7°. Pleochroism isX= colourless,Y= very pale blue andZ= dark sky blue;Z>Y>X. The empirical formula unit, based on six oxygen atoms per formula unit is Cu2.00(C2O4)Cl0.02(OH)1.98. Middlebackite is monoclinic, space groupP21/c witha= 7.2597(15),b= 5.7145(11),c= 5.6624(11) Å, β = 104.20(3)°,V= 227.73(8) Å3andZ= 2. The five strongest lines in the powder X-ray diffraction pattern are [d(Å), (I), (hkl)]: 7.070 (16) (100), 3.739 (100) (11$\bar{1}$), 2.860 (18) (020), 2.481 (12) (12$\bar{1}$) and 2.350 (9) (300). The crystal structure was refined from synchrotron single-crystal X-ray diffraction data toR1= 0.0341 for 596 observed reflections withF0> 4σ(F0). The structure is based on sheets of edge- and corner-sharing octahedra parallel to thebcplane. Sheets link in theadirection via oxalate anions.

The Electron Effect of Aromatic Group: Control Conformation of 2-Aromatic Cyclododecanone Derivatives

2020 ◽  
Vol 24 (10) ◽  
pp. 1139-1147
Author(s):  
Yang Mingyan ◽  
Wang Daoquan ◽  
Wang Mingan
Keyword(s):  
1H Nmr ◽  
13C Nmr ◽  
Nmr Spectra ◽  
Coupling Constants ◽  
The Other ◽  
Repulsive Interaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electron Effect ◽  
Group Control

2-Phenylcyclododecanone and 2-cyclohexylcyclododecanone derivatives were synthesized and characterized by 1H NMR, 13C NMR, HR-ESI-MS and X-ray diffraction. Their preferred conformations were analyzed by the coupling constants in the 1H NMR spectra and X-ray diffraction, which showed the skeleton ring of these derivatives containing [3333]-2-one conformation, and the phenyl groups were located at the side-exo position of [3333]-2-one conformation due to the strong π-π repulsive interaction between the π- electron of benzene ring and π-electron of carbonyl group. The cyclohexyl groups were located at the corner-syn or the side-exo position of [3333]-2-one conformation depending on the hindrance of the other substituted groups. The π-π electron effect played a crucial role in efficiently controlling the preferred conformation of 2-aromatic cyclododecanone and the other 2-aromatic macrocyclic derivatives with the similar preferred square and rectangular conformations.

Single-crystal investigation of Ce5AgxGe4−x (x = 0.1−1.08) with Sm5Ge4 type

2020 ◽  
Vol 75 (8) ◽  
pp. 765-768
Author(s):  
Bohdana Belan ◽  
Dorota Kowalska ◽  
Mariya Dzevenko ◽  
Mykola Manyako ◽  
Roman Gladyshevskii
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Binary Compound ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

AbstractThe crystal structure of the phase Ce5AgxGe4−x (x = 0.1−1.08) has been determined using single-crystal X-ray diffraction data for Ce5Ag0.1Ge3.9. This phase is isotypic with Sm5Ge4: space group Pnma (No. 62), Pearson code oP36, Z = 4, a = 7.9632(2), b = 15.2693(5), c = 8.0803(2) Å; R1 = 0.0261, wR2 = 0.0460, 1428 F2 values and 48 variables. The two crystallographic positions 8d and 4c show Ge/Ag mixing, leading to a slight increase in the lattice parameters as compared to those of the pure binary compound Ce5Ge4.

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