We describe here the case of twinning by reticular (pseudo)merohedry in case of natural zippeite crystal from Cap Garonne, France. The twin is by two-fold rotation in [100] and it is a first document of this type of twinning in zippeite-related minerals and compounds. Zippeite crystals from Cap Garonne mine, France, were studied by single-crystal X-ray diffraction [a=8.7243(4), b=13.9337(7), c=8.8741(4) Å, β=104.243(5) and V=1045.59(9) Å3, Z=2, in C2/m]; refinement taking into account of the twinning resulted in R=2.81% for 1596 reflections with [I>3σ(I)] and refined twin fraction 0.7773(9):0.2227(9).
A new superstructure of the mineral camerolaite, CuAl(OH)(HO)[Sb(OH)](SO), has been refined in space group P\bar 1 with unit-cell parameters a = 7.7660 (16), b = 8.759 (4), c = 11.306 (2) Å, α = 108.67 (4), β = 83.41 (3), γ = 126.64 (2)°, V = 581.6 (3) Å and Z = 1, with R = 0.0951 (all data). This is the first refined example of a cyanotrichite-group mineral in which long-range order of interlayer anions produces a superstructure along b, although diffuse scattering has previously been reported that corresponds to short-range order. Though the structure shares with other members of the cyanotrichite group a structural unit in which ribbons of edge-sharing Cu and Al octahedra form layers || (001), the superstructure arises from regular alternation of [SO] and [Sb(OH)] polyhedra along rods that lie between the layers, and phase coupling between rods that maximizes the distance between [SO] groups of adjacent rods along a and c directions. This arrangement suggests an alternative nearly orthogonal choice of unit cell in F\bar 1 with parameters a = 12.473 (26), b = 8.759 (4), c = 21.476 (7) Å, α = 85.94 (4), β = 95.91 (5), γ = 92.34 (9)°, which is recommended for comparing this structural variety of camerolaite with other members of the group.
Natural orthorhombic sulfur (α-S8), grown on galena crystals from Cap Garonne, Mine du Pradet, France, were studied by single crystal X-ray diffraction at 150 K: Fddd, a=1036.75(5), b=1273.54(7), c=2437.85(13) pm, wR=0.0380, 1433 F2 values (all data) and 37 variables. Refinements of the occupancy parameters along with EDX data indicate pure sulfur.
Natural lead dioxide samples (β modification) from Cap Garonne, Mine du Pradet, France and Mount Trevasco, Italy were studied by single crystal X-ray and electron diffraction, clearly manifesting the rutile-type structure. A needle from the Mount Trevasco sample was investigated on a single crystal diffractometer: P42/mnm, a = 495.81(10), c = 338.66(7) pm, wR = 0.0513, 117 F2 values (all data) and nine variables (293 K data). An additional data set at T = 90 K gave no hint for structural distortions.
Abstract. The new mineral gobelinite, ideally CoCu4(SO4)2(OH)6⚫6H2O, is a new member of the ktenasite group and the Co analogue of ktenasite, ZnCu4(SO4)2(OH)6⚫6H2O. It occurs at Cap Garonne (CG), Var, France (type locality), and Eisenzecher Zug (EZ), Siegerland, North Rhine-Westphalia, Germany (cotype locality). The mineral forms pale green, bluish green or greyish green, blocky to thin, lath-like crystals. They are transparent and non-fluorescent, with a vitreous, sometimes also pearly, lustre and a white streak having a pale-green cast. Mohs hardness is about 2.5. The crystals are brittle with an irregular fracture; no cleavage was observed. D(meas.) is 2.95(2) and D(calc.) is 2.907 g cm−3 (for empirical formula, CG). Common associates are brochantite and various other hydrated metal sulfates. Electron-microprobe analyses of the CG material yielded (wt. %) CuO 42.45, CoO 6.58, NiO 3.37, ZnO 3.14, SO3 22.12, and H2O 22.62 (calculated on structural grounds), and total = 100.30 wt. %, giving the empirical formula (based on 20 O atoms) (Co0.63Ni0.32Zn0.28Cu3.83)Σ5.06S1.98O20H18.00. The simplified formula is (Co,Ni)(Cu,Zn)4(SO4)2(OH)6⚫6H2O, and the endmember formula is CoCu4(SO4)2(OH)6⚫6H2O. Scanning electron microscopy–energy dispersive X-ray spectroscopy (SEM–EDS) analyses of the (Zn-free) EZ material gave the simplified average formula (Co0.92Ni0.21Mg0.01Cu3.79)Σ4.93(SO4)2.08(OH)6⚫6H2O. Optically, gobelinite (CG) is biaxial negative, with α=1.576(2), β=1.617(2) and γ=1.630(2); 2Vmeas=58(4)∘ and 2Vcalc=57.5∘. Dispersion is weak, r>v; orientation is X=β, Y=γ and Z≈α, with strong pleochroism X equaling colourless, Y equaling green and Z equaling pale green. The mineral is monoclinic, space group P21∕c, with a=5.599(1), b=6.084(1), c=23.676(5) Å, β=95.22(3)∘ and V=803.2(3) Å3 (at 100 K; CG) and a=5.611(1), b=6.103(1), c=23.808(5) Å, β=95.18(3)∘ and V=811.9(3) Å3 (at 298 K; EZ), respectively (Z=2). The eight strongest measured powder X-ray diffraction lines (d in Å (I) hkl (CG material)) are 11.870 (100) 002, 5.924 (40) 004, 4.883 (10) 102, 4.825 (15) 013, 3.946 (15) 006, 2.956 (15) 008, 2.663 (20) 202 and 2.561 (15) 1‾23. Single-crystal structure determinations gave R1=0.0310 (CG) and 0.0280 (EZ). The atomic arrangement is based on brucite-like sheets formed from edge-sharing, Jahn–Teller-distorted (4+2 coordination) CuO6 octahedra. These sheets are decorated on both sides with SO4 tetrahedra and linked via hydrogen bonds to interstitial, fairly regular Co(H2O)6 octahedra. The name alludes to the Old French word gobelin, equivalent to the German word kobold, from which the designation of the element cobalt was derived.
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