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The crystal structure of hexagonal ErMnO3, erbium manganese trioxide, has been determined at room temperature. It is isomorphous with YMnO3. Although we observed inversion twinning, similar to YMnO3, the twin fractions do not have a 1:1 ratio, and the crystals are expected to show net ferroelectricity.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Mn-O) = 0.005 Å
- R factor = 0.034
- wR factor = 0.079
- Data-to-parameter ratio = 23.0
checkCIF results
No syntax errors found
Alert Level A:
PLAT_213 Alert A Atom O1 has ADP max/min Ratio ........... 9.90
| Author response: ...
Both the Ueq and the refined anisotropic displacement patterns of O1 are in
line with the values refined for the other atoms. Especially, if we take the
standard deviations into account the differences between the a.d.p.'s is almos
negligible. However using isotropic atomic displacement for all oxygen
positions, yields a very similar model. All atomic positions stay equal within
the error of the refinement.
|
Alert Level B:
PLAT_111 Alert B ADDSYM detects (pseudo) centre of symmetry ... 100 Perc Fit
PLAT_111 Alert B ADDSYM detects (pseudo) centre of symmetry ... 100 Perc Fit
Alert Level C:
DIFMN_02 Alert C The minimum difference density is < -0.1*ZMAX*0.75
_refine_diff_density_min given = -6.400
Test value = -5.100
DIFMN_03 Alert C The minimum difference density is < -0.1*ZMAX*0.75
The relevant atom site should be identified.
General Notes
REFLT_03
From the CIF: _diffrn_reflns_theta_max 38.49
From the CIF: _reflns_number_total 759
Count of symmetry unique reflns 411
Completeness (_total/calc) 184.67%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 348
Fraction of Friedel pairs measured 0.847
Are heavy atom types Z>Si present yes
Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
1 Alert Level A = Potentially serious problem
2 Alert Level B = Potential problem
2 Alert Level C = Please check
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: XPREP (Bruker, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP (Farrugia, 2000); software used to prepare material for publication: PLATON (Spek, 2001).
Erbium Manganese Oxide
top
Crystal data top
ErMnO3 | Dx = 7.286 Mg m−3 |
Mr = 270.20 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63cm | Cell parameters from 3929 reflections |
Hall symbol: P 6c -2 | θ = 3.5–38.4° |
a = 6.1121 (5) Å | µ = 38.68 mm−1 |
c = 11.4200 (14) Å | T = 293 K |
V = 369.47 (6) Å3 | Triangular platelet, black |
Z = 6 | 0.11 × 0.10 × 0.08 mm |
F(000) = 702 | |
Data collection top
Bruker SMART Apex diffractometer | 759 independent reflections |
Radiation source: fine focus sealed Siemens Mo tube | 569 reflections with F > 4σ(F) |
Parallel mounted graphite monochromator | Rint = 0.068 |
Detector resolution: 4096x4096 62x62(binned 512) pixels mm-1 | θmax = 38.5°, θmin = 3.6° |
area detector scans | h = −6→10 |
Absorption correction: gaussian (XPREP, Bruker, 2000) | k = −10→8 |
Tmin = 0.019, Tmax = 0.083 | l = −18→19 |
7178 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: none |
R[F2 > 2σ(F2)] = 0.034 | w = 1/[σ2(Fo2) + (0.0457P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.079 | (Δ/σ)max < 0.001 |
S = 1.03 | Δρmax = 3.8 (9) e Å−3 |
759 reflections | Δρmin = −6.4 (9) e Å−3 |
33 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.0223 (11) |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All e.s.d.'s are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
2σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R-factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Er1 | 0.00000 | 0.00000 | −0.22783 (9) | 0.0084 (2) | |
Er2 | 0.33333 | 0.66667 | 0.22951 (2) | 0.0089 (1) | |
Mn1 | 0.00000 | 0.3396 (3) | −0.00248 (17) | 0.0090 (3) | |
O1 | 0.00000 | 0.3593 (12) | −0.1645 (7) | 0.012 (2) | |
O2 | 0.00000 | 0.3113 (14) | 0.1620 (7) | 0.012 (2) | |
O3 | 0.00000 | 0.00000 | −0.025 (3) | 0.010 (3) | |
O4 | 0.33333 | 0.66667 | 0.0161 (13) | 0.011 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Er1 | 0.0093 (3) | 0.0093 (3) | 0.0067 (3) | 0.0047 (2) | 0.0000 | 0.0000 |
Er2 | 0.0090 (2) | 0.0090 (2) | 0.0088 (2) | 0.0045 (1) | 0.0000 | 0.0000 |
Mn1 | 0.0122 (8) | 0.0105 (5) | 0.0048 (3) | 0.0061 (4) | 0.0000 | 0.0015 (4) |
O1 | 0.030 (5) | 0.008 (2) | 0.004 (3) | 0.015 (3) | 0.0000 | −0.001 (2) |
O2 | 0.018 (5) | 0.012 (3) | 0.008 (3) | 0.009 (2) | 0.0000 | 0.001 (2) |
O3 | 0.010 (4) | 0.010 (4) | 0.009 (7) | 0.005 (2) | 0.0000 | 0.0000 |
O4 | 0.013 (4) | 0.013 (4) | 0.008 (4) | 0.0066 (19) | 0.0000 | 0.0000 |
Geometric parameters (Å, º) top
Er2—O4 | 2.437 (15) | Er1—O1viii | 2.312 (7) |
Er2—O2 | 2.244 (7) | Er1—O2ix | 2.281 (7) |
Er2—O1i | 2.306 (5) | Er1—O1x | 2.312 (7) |
Er2—O2ii | 2.244 (9) | Er1—O2xi | 2.281 (8) |
Er2—O1iii | 2.306 (5) | Er1—O3vii | 3.39 (3) |
Er2—O2iv | 2.244 (5) | Mn1—O3 | 2.092 (4) |
Er2—O4v | 3.273 (15) | Mn1—O4 | 2.030 (2) |
Er2—O1vi | 2.306 (7) | Mn1—O1 | 1.854 (8) |
Er1—O3 | 2.32 (3) | Mn1—O2 | 1.886 (8) |
Er1—O1 | 2.312 (6) | Mn1—O4xii | 2.0296 (18) |
Er1—O2vii | 2.281 (8) | | |
| | | |
O4—Er2—O2 | 69.9 (2) | O1viii—Er1—O2xi | 164.8 (3) |
O4—Er2—O1i | 121.66 (17) | O1x—Er1—O2ix | 77.08 (19) |
O4—Er2—O2ii | 69.9 (2) | O2ix—Er1—O2xi | 92.5 (3) |
O4—Er2—O1iii | 121.66 (18) | O1x—Er1—O2xi | 77.1 (3) |
O4—Er2—O2iv | 69.9 (2) | O3—Mn1—O4 | 119.49 (7) |
O4—Er2—O1vi | 121.66 (19) | O3—Mn1—O1 | 86.7 (9) |
O1i—Er2—O2 | 168.4 (3) | O3—Mn1—O2 | 91.8 (10) |
O2—Er2—O2ii | 108.8 (2) | O3—Mn1—O4xii | 119.49 (9) |
O1iii—Er2—O2 | 76.7 (2) | O4—Mn1—O1 | 94.2 (5) |
O2—Er2—O2iv | 108.8 (2) | O4—Mn1—O2 | 86.6 (5) |
O1vi—Er2—O2 | 77.9 (3) | O4—Mn1—O4xii | 120.76 (13) |
O1i—Er2—O2ii | 77.9 (3) | O1—Mn1—O2 | 178.5 (3) |
O1i—Er2—O1iii | 95.0 (3) | O4xii—Mn1—O1 | 94.2 (4) |
O1i—Er2—O2iv | 76.7 (2) | O4xii—Mn1—O2 | 86.6 (4) |
O1i—Er2—O1vi | 95.0 (2) | Er1—O3—Mn1 | 97.1 (9) |
O1iii—Er2—O2ii | 168.4 (3) | Er1—O3—Mn1viii | 97.1 (9) |
O2ii—Er2—O2iv | 108.8 (3) | Er1—O3—Mn1x | 97.1 (9) |
O1vi—Er2—O2ii | 76.7 (3) | Mn1—O3—Mn1viii | 118.5 (4) |
O1iii—Er2—O2iv | 77.9 (3) | Mn1—O3—Mn1x | 118.5 (4) |
O1iii—Er2—O1vi | 95.0 (3) | Mn1viii—O3—Mn1x | 118.5 (4) |
O1vi—Er2—O2iv | 168.4 (3) | Er2—O4—Mn1 | 96.0 (4) |
O3—Er1—O1 | 71.8 (2) | Er2—O4—Mn1iv | 96.0 (4) |
O3—Er1—O2vii | 123.5 (2) | Mn1—O4—Mn1ii | 118.92 (16) |
O3—Er1—O1viii | 71.8 (2) | Mn1—O4—Mn1iv | 118.92 (16) |
O3—Er1—O2ix | 123.47 (19) | Mn1ii—O4—Mn1iv | 118.92 (16) |
O3—Er1—O1x | 71.8 (2) | Er1—O1—Mn1 | 104.5 (3) |
O3—Er1—O2xi | 123.5 (2) | Er2vii—O1—Er1 | 101.0 (3) |
O1—Er1—O2vii | 77.08 (18) | Er2xiii—O1—Er1 | 101.0 (2) |
O1—Er1—O1viii | 110.7 (2) | Er2vii—O1—Mn1 | 123.2 (2) |
O1—Er1—O2ix | 164.8 (3) | Er2xiii—O1—Mn1 | 123.2 (3) |
O1—Er1—O1x | 110.69 (16) | Er2vii—O1—Er2xiii | 99.8 (3) |
O1—Er1—O2xi | 77.1 (3) | Er2—O2—Mn1 | 107.2 (3) |
O1viii—Er1—O2vii | 77.1 (2) | Er2—O2—Er1xiv | 103.8 (3) |
O2vii—Er1—O2ix | 92.5 (2) | Er2—O2—Er2xii | 103.6 (3) |
O1x—Er1—O2vii | 164.8 (3) | Er1xiv—O2—Mn1 | 128.7 (4) |
O2vii—Er1—O2xi | 92.5 (3) | Er2xii—O2—Mn1 | 107.2 (2) |
O1viii—Er1—O2ix | 77.1 (3) | Er2xii—O2—Er1xiv | 103.8 (3) |
O1viii—Er1—O1x | 110.7 (2) | | |
| | | |
O2—Er2—O4—Mn1 | 4.11 (14) | O3—Mn1—O4—Er2 | −94.7 (11) |
O4—Er2—O2—Mn1 | −4.61 (16) | O1—Mn1—O4—Er2 | 176.74 (15) |
O1—Er1—O3—Mn1 | 0.00 (14) | O2—Mn1—O4—Er2 | −4.61 (16) |
O3—Er1—O1—Mn1 | 0.00 (14) | O3—Mn1—O1—Er1 | 0.02 (15) |
O4—Mn1—O3—Er1 | −92.9 (7) | O4—Mn1—O1—Er1 | 119.35 (16) |
O1—Mn1—O3—Er1 | −0.02 (13) | O3—Mn1—O2—Er2 | 124.64 (18) |
O2—Mn1—O3—Er1 | −180.00 (18) | O4—Mn1—O2—Er2 | 5.21 (18) |
Symmetry codes: (i) x−y+1, x+1, z+1/2; (ii) −y+1, x−y+1, z; (iii) −x, −y+1, z+1/2; (iv) −x+y, −x+1, z; (v) −x+y, y, z+1/2; (vi) y, −x+y, z+1/2; (vii) x−y, x, z−1/2; (viii) −y, x−y, z; (ix) −x, −y, z−1/2; (x) −x+y, −x, z; (xi) y, −x+y, z−1/2; (xii) y−1, x, z; (xiii) −x+y, y, z−1/2; (xiv) x−y, x, z+1/2. |
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