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Single crystals of digadolinium monooxy­gen diselenide, Gd2OSe2, have been obtained from a KBr flux. The compound is isostructural with the low-pressure form of Dy2OS2. All atoms lie on the mirror plane of Pnma. The Gd environments are a GdO3Se5 bicapped trigonal prism and a GdOSe5 distorted octahedron. The two coordination polyhedra pack by face-sharing and edge-sharing to form a [Gd8/4O4/4Sea8/8-Sei8/8] fragment, which is the main motif of the structure. These fragments lie in the ac plane and form infinite chains parallel to c through the sharing of Se atoms around atom Gd1. In the a direction, these chains stack through the sharing of an Se atom around atom Gd2, thereby delimiting large pentagonal cavities.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100003024/br1282sup1.cif
Contains datablocks Gd2OSe2, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100003024/br1282Isup2.hkl
Contains datablock I

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SMART (Bruker, 1999); data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL/PC (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL/PC.

(I) top
Crystal data top
Gd2OSe2Dx = 7.301 Mg m3
Mr = 488.42Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PnmaCell parameters from 2878 reflections
a = 16.050 (3) Åθ = 2.5–28.3°
b = 3.9375 (8) ŵ = 45.78 mm1
c = 7.0309 (14) ÅT = 153 K
V = 444.32 (15) Å3Rod, pale_yellow
Z = 40.24 × 0.02 × 0.02 mm
F(000) = 816
Data collection top
Bruker Smart 1000 CCD
diffractometer
623 independent reflections
Radiation source: standard-focus sealed tube580 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
ω scansθmax = 28.3°, θmin = 2.5°
Absorption correction: numerical
(face indexed; SHLEXTL/PC; Sheldrick, 1997b)
h = 2020
Tmin = 0.065, Tmax = 0.400k = 55
3870 measured reflectionsl = 99
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024 w = 1/[σ2(Fo2) + (0.04Fo2)2]
wR(F2) = 0.059(Δ/σ)max < 0.001
S = 1.10Δρmax = 2.96 e Å3
623 reflectionsΔρmin = 2.30 e Å3
32 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0017 (2)
Special details top

Experimental. Data collection covered more than a hemisphere of reciprocal space by a combination of three sets of 606 frames φ = 0°, 120°, and 240° with Δω = 0.3° and exposure times of 15 s. Crystal decay, which proved to be negligible, was monitored by repeating 50 initial frames at the end of the data collection.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Gd10.03937 (2)0.25000.69956 (6)0.00746 (16)
Gd20.16208 (3)0.25000.25860 (6)0.00901 (16)
Se10.31982 (5)0.25000.05159 (12)0.0088 (2)
Se20.40054 (4)0.25000.50993 (12)0.0082 (2)
O10.0314 (3)0.25000.3705 (9)0.0071 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.0081 (2)0.0060 (2)0.0083 (2)0.0000.00025 (14)0.000
Gd20.0093 (2)0.0074 (2)0.0104 (3)0.0000.00097 (14)0.000
Se10.0087 (4)0.0079 (4)0.0098 (4)0.0000.0005 (3)0.000
Se20.0105 (4)0.0061 (4)0.0079 (4)0.0000.0008 (3)0.000
O10.003 (2)0.008 (3)0.010 (3)0.0000.003 (2)0.000
Geometric parameters (Å, º) top
Gd1—O12.317 (6)Gd2—Se12.9203 (10)
Gd1—O1i2.326 (3)Gd2—Gd1i3.7968 (7)
Gd1—O1ii2.326 (3)Gd2—Gd1ii3.7968 (7)
Gd1—Se2iii3.0228 (10)Gd2—Gd2viii3.9375 (8)
Gd1—Se2iv3.0932 (8)Gd2—Gd2ix3.9375 (8)
Gd1—Se2v3.0932 (8)Se1—Gd2vi2.8642 (8)
Gd1—Se1iv3.1726 (8)Se1—Gd2vii2.8642 (8)
Gd1—Se1v3.1726 (8)Se1—Gd1vii3.1726 (8)
Gd1—Gd1i3.6535 (8)Se1—Gd1vi3.1726 (8)
Gd1—Gd1ii3.6535 (8)Se2—Gd2iv2.8183 (7)
Gd1—Gd23.6729 (8)Se2—Gd2v2.8183 (7)
Gd1—Gd2i3.7968 (7)Se2—Gd1x3.0228 (10)
Gd2—O12.240 (5)Se2—Gd1vi3.0932 (8)
Gd2—Se2vi2.8183 (7)Se2—Gd1vii3.0932 (8)
Gd2—Se2vii2.8183 (7)O1—Gd1i2.326 (3)
Gd2—Se1iv2.8642 (8)O1—Gd1ii2.326 (3)
Gd2—Se1v2.8642 (8)
O1—Gd1—O1i76.20 (17)Se2vii—Gd2—Se1v164.26 (3)
O1—Gd1—O1ii76.20 (17)Se1iv—Gd2—Se1v86.84 (3)
O1i—Gd1—O1ii115.7 (2)O1—Gd2—Se1170.67 (15)
O1—Gd1—Se2iii129.35 (12)Se2vi—Gd2—Se190.00 (2)
O1i—Gd1—Se2iii77.47 (14)Se2vii—Gd2—Se190.00 (2)
O1ii—Gd1—Se2iii77.47 (14)Se1iv—Gd2—Se1105.695 (17)
O1—Gd1—Se2iv136.19 (5)Se1v—Gd2—Se1105.695 (17)
O1i—Gd1—Se2iv147.19 (15)O1—Gd2—Gd137.01 (15)
O1ii—Gd1—Se2iv76.29 (13)Se2vi—Gd2—Gd1109.42 (2)
Se2iii—Gd1—Se2iv75.71 (2)Se2vii—Gd2—Gd1109.42 (2)
O1—Gd1—Se2v136.19 (5)Se1iv—Gd2—Gd156.448 (18)
O1i—Gd1—Se2v76.29 (13)Se1v—Gd2—Gd156.448 (18)
O1ii—Gd1—Se2v147.19 (15)Se1—Gd2—Gd1152.32 (2)
Se2iii—Gd1—Se2v75.71 (2)O1—Gd2—Gd1i34.46 (6)
Se2iv—Gd1—Se2v79.06 (3)Se2vi—Gd2—Gd1i51.844 (18)
O1—Gd1—Se1iv73.25 (9)Se2vii—Gd2—Gd1i96.12 (2)
O1i—Gd1—Se1iv143.49 (14)Se1iv—Gd2—Gd1i112.77 (2)
O1ii—Gd1—Se1iv75.71 (11)Se1v—Gd2—Gd1i70.989 (19)
Se2iii—Gd1—Se1iv138.303 (16)Se1—Gd2—Gd1i140.973 (16)
Se2iv—Gd1—Se1iv67.31 (2)Gd1—Gd2—Gd1i58.535 (13)
Se2v—Gd1—Se1iv113.84 (2)O1—Gd2—Gd1ii34.46 (6)
O1—Gd1—Se1v73.25 (9)Se2vi—Gd2—Gd1ii96.12 (2)
O1i—Gd1—Se1v75.71 (11)Se2vii—Gd2—Gd1ii51.844 (18)
O1ii—Gd1—Se1v143.49 (14)Se1iv—Gd2—Gd1ii70.989 (19)
Se2iii—Gd1—Se1v138.303 (16)Se1v—Gd2—Gd1ii112.77 (2)
Se2iv—Gd1—Se1v113.84 (2)Se1—Gd2—Gd1ii140.974 (16)
Se2v—Gd1—Se1v67.31 (2)Gd1—Gd2—Gd1ii58.535 (13)
Se1iv—Gd1—Se1v76.71 (2)Gd1i—Gd2—Gd1ii62.466 (17)
O1—Gd1—Gd1i38.19 (6)O1—Gd2—Gd2viii90.0
O1i—Gd1—Gd1i38.02 (15)Se2vi—Gd2—Gd2viii134.312 (15)
O1ii—Gd1—Gd1i97.15 (13)Se2vii—Gd2—Gd2viii45.688 (15)
Se2iii—Gd1—Gd1i105.31 (2)Se1iv—Gd2—Gd2viii46.578 (15)
Se2iv—Gd1—Gd1i173.069 (15)Se1v—Gd2—Gd2viii133.421 (15)
Se2v—Gd1—Gd1i107.863 (17)Se1—Gd2—Gd2viii90.0
Se1iv—Gd1—Gd1i109.20 (3)Gd1—Gd2—Gd2viii90.0
Se1v—Gd1—Gd1i70.13 (2)Gd1i—Gd2—Gd2viii121.233 (8)
O1—Gd1—Gd1ii38.19 (6)Gd1ii—Gd2—Gd2viii58.767 (8)
O1i—Gd1—Gd1ii97.15 (13)O1—Gd2—Gd2ix90.0
O1ii—Gd1—Gd1ii38.02 (15)Se2vi—Gd2—Gd2ix45.688 (15)
Se2iii—Gd1—Gd1ii105.31 (2)Se2vii—Gd2—Gd2ix134.312 (15)
Se2iv—Gd1—Gd1ii107.863 (17)Se1iv—Gd2—Gd2ix133.422 (15)
Se2v—Gd1—Gd1ii173.069 (15)Se1v—Gd2—Gd2ix46.578 (15)
Se1iv—Gd1—Gd1ii70.13 (2)Se1—Gd2—Gd2ix90.0
Se1v—Gd1—Gd1ii109.20 (3)Gd1—Gd2—Gd2ix90.0
Gd1i—Gd1—Gd1ii65.213 (19)Gd1i—Gd2—Gd2ix58.767 (8)
O1—Gd1—Gd235.59 (12)Gd1ii—Gd2—Gd2ix121.233 (8)
O1i—Gd1—Gd294.76 (14)Gd2viii—Gd2—Gd2ix180.0
O1ii—Gd1—Gd294.76 (14)Gd2vi—Se1—Gd2vii86.84 (3)
Se2iii—Gd1—Gd2164.93 (2)Gd2vi—Se1—Gd2116.51 (2)
Se2iv—Gd1—Gd2115.36 (2)Gd2vii—Se1—Gd2116.51 (2)
Se2v—Gd1—Gd2115.36 (2)Gd2vi—Se1—Gd1vii126.17 (3)
Se1iv—Gd1—Gd248.797 (16)Gd2vii—Se1—Gd1vii74.755 (18)
Se1v—Gd1—Gd248.797 (16)Gd2—Se1—Gd1vii117.01 (3)
Gd1i—Gd1—Gd262.428 (17)Gd2vi—Se1—Gd1vi74.755 (18)
Gd1ii—Gd1—Gd262.428 (17)Gd2vii—Se1—Gd1vi126.17 (3)
O1—Gd1—Gd2i91.74 (10)Gd2—Se1—Gd1vi117.01 (3)
O1i—Gd1—Gd2i33.02 (12)Gd1vii—Se1—Gd1vi76.71 (2)
O1ii—Gd1—Gd2i92.26 (10)Gd2iv—Se2—Gd2v88.62 (3)
Se2iii—Gd1—Gd2i47.150 (15)Gd2iv—Se2—Gd1x81.01 (2)
Se2iv—Gd1—Gd2i122.74 (2)Gd2v—Se2—Gd1x81.01 (2)
Se2v—Gd1—Gd2i83.155 (17)Gd2iv—Se2—Gd1vi173.44 (3)
Se1iv—Gd1—Gd2i162.50 (2)Gd2v—Se2—Gd1vi95.982 (17)
Se1v—Gd1—Gd2i108.072 (18)Gd1x—Se2—Gd1vi104.29 (2)
Gd1i—Gd1—Gd2i59.037 (13)Gd2iv—Se2—Gd1vii95.982 (17)
Gd1ii—Gd1—Gd2i92.541 (17)Gd2v—Se2—Gd1vii173.44 (3)
Gd2—Gd1—Gd2i121.465 (13)Gd1x—Se2—Gd1vii104.29 (2)
O1—Gd2—Se2vi83.34 (11)Gd1vi—Se2—Gd1vii79.06 (3)
O1—Gd2—Se2vii83.34 (11)Gd2—O1—Gd1107.4 (2)
Se2vi—Gd2—Se2vii88.62 (3)Gd2—O1—Gd1i112.51 (15)
O1—Gd2—Se1iv80.93 (11)Gd1—O1—Gd1i103.80 (17)
Se2vi—Gd2—Se1iv164.26 (3)Gd2—O1—Gd1ii112.51 (15)
Se2vii—Gd2—Se1iv90.12 (2)Gd1—O1—Gd1ii103.80 (17)
O1—Gd2—Se1v80.93 (11)Gd1i—O1—Gd1ii115.7 (2)
Se2vi—Gd2—Se1v90.12 (2)
Symmetry codes: (i) x, y, z+1; (ii) x, y+1, z+1; (iii) x1/2, y, z+3/2; (iv) x+1/2, y+1, z+1/2; (v) x+1/2, y, z+1/2; (vi) x+1/2, y, z1/2; (vii) x+1/2, y+1, z1/2; (viii) x, y+1, z; (ix) x, y1, z; (x) x+1/2, y, z+3/2.
 

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