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The title compound, calcium dimanganese tetraoxide, CaMn2O4, was synthesized hydrothermally and is made up of edge-sharing Mn3+ distorted octahedral layers and eight-coordinate Ca2+ centered polyhedral layers.
Supporting information
Data collection: P3 Software (Siemens, 1989); cell refinement: P3 Software; data reduction: SHELXTL-Plus (Sheldrick, 1990); program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Calcium dimanganese(III) Oxide
top
Crystal data top
CaMn2O4 | F(000) = 408 |
Mr = 213.96 | Dx = 4.661 Mg m−3 |
Orthorhombic, Pbcm | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2c 2b | Cell parameters from 41 reflections |
a = 3.1546 (6) Å | θ = 7.5–17.5° |
b = 9.988 (2) Å | µ = 9.79 mm−1 |
c = 9.6769 (19) Å | T = 293 K |
V = 304.90 (10) Å3 | Hexagonal Rod, black |
Z = 4 | 0.82 × 0.38 × 0.34 mm |
Data collection top
Siemens R3m/V diffractometer | 701 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.043 |
Highly oriented graphite crystal monochromator | θmax = 35.1°, θmin = 4.1° |
ω/2–θ scans | h = −5→5 |
Absorption correction: analytical | k = −16→16 |
Tmin = 0.175, Tmax = 0.256 | l = −15→15 |
5238 measured reflections | 3 standard reflections every 97 reflections |
706 independent reflections | intensity decay: 6.2% |
Refinement top
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0218P)2 + 0.3104P] |
R[F2 > 2σ(F2)] = 0.022 | (Δ/σ)max = 0.011 |
wR(F2) = 0.052 | Δρmax = 0.56 e Å−3 |
S = 1.33 | Δρmin = −1.41 e Å−3 |
706 reflections | Extinction correction: SHELXTL (Sheldrick, 1998) |
42 parameters | Extinction coefficient: 0.161 (11) |
0 restraints | |
Special details top
Experimental. A linear correction was applied to the data to account for crystal
decomposition. |
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 >
σ(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 | |
Mn1 | 0.20400 (7) | 0.388233 (19) | 0.56852 (2) | 0.00466 (10) | |
Ca1 | 0.31754 (11) | 0.64882 (4) | 0.7500 | 0.00573 (13) | |
O1 | 0.8095 (5) | 0.81633 (14) | 0.7500 | 0.0064 (4) | |
O2 | 0.7994 (3) | 0.52716 (9) | 0.60794 (10) | 0.0060 (3) | |
O3 | 0.4077 (5) | 0.7500 | 0.5000 | 0.0067 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.00753 (14) | 0.00409 (12) | 0.00238 (12) | 0.00062 (5) | 0.00084 (5) | 0.00192 (5) |
Ca1 | 0.00586 (19) | 0.00543 (18) | 0.00588 (17) | 0.000 | 0.000 | −0.00007 (10) |
O1 | 0.0101 (7) | 0.0065 (6) | 0.0026 (5) | 0.000 | 0.000 | −0.0005 (4) |
O2 | 0.0084 (5) | 0.0060 (4) | 0.0037 (4) | 0.0005 (3) | 0.0010 (3) | 0.0018 (3) |
O3 | 0.0077 (6) | 0.0056 (6) | 0.0069 (5) | −0.0010 (4) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Mn1—O1i | 1.8978 (7) | Ca1—Ca1iii | 3.1546 (6) |
Mn1—O2ii | 1.9053 (10) | Ca1—Ca1vii | 3.1546 (6) |
Mn1—O2iii | 1.9236 (10) | Ca1—Mn1v | 3.1601 (6) |
Mn1—O3ii | 1.9612 (10) | O1—Mn1viii | 1.8978 (7) |
Mn1—O2 | 2.3661 (11) | O1—Mn1ix | 1.8978 (7) |
Mn1—O3iv | 2.4637 (12) | O1—Ca1vii | 2.3169 (15) |
Ca1—O1 | 2.2819 (15) | O2—Mn1ii | 1.9053 (10) |
Ca1—O1iii | 2.3169 (15) | O2—Mn1vii | 1.9236 (10) |
Ca1—O2 | 2.3825 (10) | O2—Ca1vii | 2.4573 (11) |
Ca1—O2v | 2.3825 (10) | O3—Mn1ix | 1.9612 (10) |
Ca1—O2iii | 2.4573 (11) | O3—Mn1ii | 1.9612 (10) |
Ca1—O2vi | 2.4573 (11) | O3—Mn1iv | 2.4637 (12) |
Ca1—O3v | 2.6372 (5) | O3—Mn1x | 2.4637 (12) |
Ca1—O3 | 2.6372 (5) | O3—Ca1xi | 2.6372 (5) |
| | | |
O1i—Mn1—O2ii | 175.61 (5) | O1iii—Ca1—O3 | 78.34 (3) |
O1i—Mn1—O2iii | 94.28 (5) | O2—Ca1—O3 | 66.25 (3) |
O2ii—Mn1—O2iii | 81.61 (5) | O2v—Ca1—O3 | 130.99 (4) |
O1i—Mn1—O3ii | 93.47 (4) | O2iii—Ca1—O3 | 75.41 (3) |
O2ii—Mn1—O3ii | 90.73 (3) | O2vi—Ca1—O3 | 140.75 (4) |
O2iii—Mn1—O3ii | 171.62 (4) | O3v—Ca1—O3 | 133.08 (3) |
O1i—Mn1—O2 | 95.19 (5) | Mn1viii—O1—Mn1ix | 135.45 (8) |
O2ii—Mn1—O2 | 83.62 (4) | Mn1viii—O1—Ca1 | 105.20 (4) |
O2iii—Mn1—O2 | 94.11 (4) | Mn1ix—O1—Ca1 | 105.20 (4) |
O3ii—Mn1—O2 | 88.37 (4) | Mn1viii—O1—Ca1vii | 106.78 (4) |
O1i—Mn1—O3iv | 91.11 (4) | Mn1ix—O1—Ca1vii | 106.78 (4) |
O2ii—Mn1—O3iv | 90.17 (3) | Ca1—O1—Ca1vii | 86.62 (5) |
O2iii—Mn1—O3iv | 86.44 (4) | Mn1ii—O2—Mn1vii | 98.39 (5) |
O3ii—Mn1—O3iv | 90.21 (2) | Mn1ii—O2—Mn1 | 96.38 (4) |
O2—Mn1—O3iv | 173.61 (3) | Mn1vii—O2—Mn1 | 94.11 (4) |
O1—Ca1—O1iii | 86.62 (5) | Mn1ii—O2—Ca1 | 106.70 (4) |
O1—Ca1—O2 | 86.56 (4) | Mn1vii—O2—Ca1 | 154.91 (5) |
O1iii—Ca1—O2 | 144.06 (3) | Mn1—O2—Ca1 | 83.44 (4) |
O1—Ca1—O2v | 86.56 (4) | Mn1ii—O2—Ca1vii | 106.61 (4) |
O1iii—Ca1—O2v | 144.06 (3) | Mn1vii—O2—Ca1vii | 91.50 (4) |
O2—Ca1—O2v | 70.48 (5) | Mn1—O2—Ca1vii | 155.26 (5) |
O1—Ca1—O2iii | 144.58 (3) | Ca1—O2—Ca1vii | 81.34 (3) |
O1iii—Ca1—O2iii | 84.08 (4) | Mn1ix—O3—Mn1ii | 102.70 (7) |
O2—Ca1—O2iii | 81.34 (3) | Mn1ix—O3—Mn1iv | 167.09 (6) |
O2v—Ca1—O2iii | 119.67 (5) | Mn1ii—O3—Mn1iv | 90.21 (2) |
O1—Ca1—O2vi | 144.58 (3) | Mn1ix—O3—Mn1x | 90.21 (2) |
O1iii—Ca1—O2vi | 84.08 (4) | Mn1ii—O3—Mn1x | 167.09 (6) |
O2—Ca1—O2vi | 119.67 (5) | Mn1iv—O3—Mn1x | 76.88 (5) |
O2v—Ca1—O2vi | 81.34 (3) | Mn1ix—O3—Ca1xi | 96.19 (2) |
O2iii—Ca1—O2vi | 68.03 (5) | Mn1ii—O3—Ca1xi | 91.55 (2) |
O1—Ca1—O3v | 69.25 (3) | Mn1iv—O3—Ca1xi | 83.30 (3) |
O1iii—Ca1—O3v | 78.34 (3) | Mn1x—O3—Ca1xi | 87.00 (3) |
O2—Ca1—O3v | 130.99 (4) | Mn1ix—O3—Ca1 | 91.55 (2) |
O2v—Ca1—O3v | 66.25 (3) | Mn1ii—O3—Ca1 | 96.19 (2) |
O2iii—Ca1—O3v | 140.75 (4) | Mn1iv—O3—Ca1 | 87.00 (3) |
O2vi—Ca1—O3v | 75.41 (3) | Mn1x—O3—Ca1 | 83.30 (3) |
O1—Ca1—O3 | 69.25 (3) | | |
Symmetry codes: (i) −x+1, y−1/2, −z+3/2; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) −x, −y+1, −z+1; (v) x, y, −z+3/2; (vi) x−1, y, −z+3/2; (vii) x+1, y, z; (viii) −x+1, y+1/2, −z+3/2; (ix) −x+1, y+1/2, z; (x) −x, y+1/2, z; (xi) x, −y+3/2, z−1/2. |
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