Buy article online - an online subscription or single-article purchase is required to access this article.
The crystal structure of commensurately modulated Pr2SbO2 was solved in the orthorhombic superspace group Immm(0β0)000, q = 3/4b*, a = 13.5790 (15), b = 3.9818 (18), c = 4.0041 (18) Å (T = 40 K) from a crystal twinned by reticular pseudomerohedry applying the twin law (1 0 0, 0 0 1, 0 −1 0), corresponding to a rotation by 90° along the reciprocal a axis. The formation of Zintl-type Sb2−–Sb2− dumbbells in Pr23+Sb2−O22− is considered to be accountable for its semiconducting properties, as observed previously. The space group for the three-dimensional commensurate supercell a = 13.5790 (15), b = 15.9272 (18), c = 4.0041 (18) Å (T = 40 K) is Pmnm.
Supporting information
B-IncStrDB references: 8292Ebau5x; 8312EnSPI5; 8332EyvURZ; 8352EqCIs1
Crystal data top
Pr2SbO2 | Z = 2 |
Mr = 435.6 (1) | F(000) = 370 |
Orthorhombic, Immm(0β0)000† | Dx = 6.679 (1) Mg m−3 |
q = 0.750000b* | Mo Kα radiation, λ = 0.71069 Å |
a = 13.579 Å | µ = 28.16 (1) mm−1 |
b = 3.9818 Å | T = 40 K |
c = 4.0041 Å | × × mm |
V = 216.50 Å3 | |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, x3, −x4; (3) −x1, x2, −x3, x4; (4) x1, −x2, −x3, −x4; (5) −x1, −x2, −x3, −x4; (6) x1, x2, −x3, x4; (7) x1, −x2, x3, −x4; (8) −x1, x2, x3, x4; (9) x1+1/2, x2+1/2, x3+1/2, x4; (10) −x1+1/2, −x2+1/2, x3+1/2, −x4; (11) −x1+1/2, x2+1/2, −x3+1/2, x4; (12) x1+1/2, −x2+1/2, −x3+1/2, −x4; (13) −x1+1/2, −x2+1/2, −x3+1/2, −x4; (14) x1+1/2, x2+1/2, −x3+1/2, x4; (15) x1+1/2, −x2+1/2, x3+1/2, −x4; (16) −x1+1/2, x2+1/2, x3+1/2, x4.
|
Data collection top
Radiation source: X-ray tube | θmax = 54.8°, θmin = 2.0° |
26960 measured reflections | h = 0→30 |
2999 independent reflections | k = 0→9 |
2561 reflections with I > 3σ(I) | l = 0→8 |
Rint = 0.035 | |
Refinement top
Refinement on F | 96 parameters |
R[F2 > 2σ(F2)] = 0.060 | 0 restraints |
wR(F2) = 0.129 | 0 constraints |
S = 2.31 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
2999 reflections | (Δ/σ)max = 0.002 |
Crystal data top
Pr2SbO2 | V = 216.50 Å3 |
Mr = 435.6 (1) | Z = 2 |
Orthorhombic, Immm(0β0)000† | Mo Kα radiation |
q = 0.750000b* | µ = 28.16 (1) mm−1 |
a = 13.579 Å | T = 40 K |
b = 3.9818 Å | × × mm |
c = 4.0041 Å | |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, x3, −x4; (3) −x1, x2, −x3, x4; (4) x1, −x2, −x3, −x4; (5) −x1, −x2, −x3, −x4; (6) x1, x2, −x3, x4; (7) x1, −x2, x3, −x4; (8) −x1, x2, x3, x4; (9) x1+1/2, x2+1/2, x3+1/2, x4; (10) −x1+1/2, −x2+1/2, x3+1/2, −x4; (11) −x1+1/2, x2+1/2, −x3+1/2, x4; (12) x1+1/2, −x2+1/2, −x3+1/2, −x4; (13) −x1+1/2, −x2+1/2, −x3+1/2, −x4; (14) x1+1/2, x2+1/2, −x3+1/2, x4; (15) x1+1/2, −x2+1/2, x3+1/2, −x4; (16) −x1+1/2, x2+1/2, x3+1/2, x4.
|
Data collection top
26960 measured reflections | 2561 reflections with I > 3σ(I) |
2999 independent reflections | Rint = 0.035 |
Refinement top
R[F2 > 2σ(F2)] = 0.060 | 2999 reflections |
wR(F2) = 0.129 | 96 parameters |
S = 2.31 | 0 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Pr1 | 0.16224 (5) | 0.5 | 0 | 0.00470 (16) | |
Sb1 | 0.5 | 0.5 | 0.0326 (13) | 0.0532 (12) | 0.5 |
O1 | 0.2510 (3) | 0 | 0 | 0.0066 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pr1 | 0.00645 (16) | 0.0040 (3) | 0.0037 (3) | 0 | 0 | 0 |
Sb1 | 0.0098 (10) | 0.0701 (14) | 0.080 (3) | 0 | 0 | 0 |
O1 | 0.0114 (14) | 0.007 (2) | 0.0019 (19) | 0 | 0 | 0 |
Bond lengths (Å) top | Average | Minimum | Maximum |
Pr1—Pr1i | 3.6959 (12) | 3.6725 (11) | 3.7304 (11) |
Pr1—Pr1ii | 3.6959 (12) | 3.6725 (11) | 3.7304 (11) |
Pr1—Pr1iii | 3.6959 (12) | 3.6758 (12) | 3.7160 (12) |
Pr1—Pr1iv | 3.6959 (12) | 3.6758 (12) | 3.7160 (12) |
Pr1—Sb1i | 3.487 (3) | 3.345 (3) | 3.780 (3) |
Pr1—Sb1ii | 3.635 (3) | 3.386 (3) | 3.857 (3) |
Pr1—Sb1iii | 3.571 (3) | 3.365 (3) | 3.937 (3) |
Pr1—Sb1v | 3.634 (3) | 3.382 (3) | 3.859 (3) |
Pr1—Sb1vi | 3.486 (3) | 3.343 (3) | 3.782 (3) |
Pr1—Sb1vii | 3.571 (3) | 3.365 (3) | 3.934 (3) |
Pr1—O1 | 2.329 (4) | 2.322 (4) | 2.338 (4) |
Pr1—O1viii | 2.329 (4) | 2.313 (4) | 2.339 (3) |
Pr1—O1i | 2.323 (3) | 2.318 (3) | 2.327 (2) |
Pr1—O1ii | 2.323 (3) | 2.318 (3) | 2.327 (2) |
Sb1—Sb1ix | 3.9838 (2) | 2.90260 (14) | 4.43280 (11) |
Sb1—Sb1viii | 3.9838 (2) | 2.90260 (14) | 4.43280 (11) |
Sb1—Sb1x | 3.9917 (5) | 2.9036 (2) | 4.4536 (7) |
Sb1—Sb1xi | 0.264 (8) | 0.039 (7) | 0.501 (8) |
Sb1—Sb1xii | 3.9917 (5) | 2.9036 (2) | 4.4536 (7) |
Symmetry codes: (i) −x1, −x2, −x3−1, −x4; (ii) −x1, −x2, −x3, −x4; (iii) −x1, −x2+1, −x3−1, −x4; (iv) −x1, −x2+1, −x3, −x4; (v) x1−1, x2, −x3−1, x4; (vi) x1−1, x2, −x3, x4; (vii) x1−1, x2+1, −x3, x4; (viii) x1, x2+1, x3, x4; (ix) x1, x2−1, x3, x4; (x) −x1+1, −x2−1, x3, −x4; (xi) −x1+1, −x2, x3, −x4; (xii) −x1+1, −x2+1, x3, −x4. |
Experimental details
Crystal data |
Chemical formula | Pr2SbO2 |
Mr | 435.6 (1) |
Crystal system, space group | Orthorhombic, Immm(0β0)000† |
Temperature (K) | 40 |
Wave vectors | q = 0.750000b* |
a, b, c (Å) | 13.579, 3.9818, 4.0041 |
V (Å3) | 216.50 |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 28.16 (1) |
Crystal size (mm) | × × |
|
Data collection |
Diffractometer | ? |
Absorption correction | ? |
No. of measured, independent and observed [I > 3σ(I)] reflections | 26960, 2999, 2561 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 1.150 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.060, 0.129, 2.31 |
No. of reflections | 2999 |
No. of parameters | 96 |
Δρmax, Δρmin (e Å−3) | ?, ? |
Subscribe to Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.