inorganic compounds
A high-precision structure of tetracobalt diniobium nonaoxide, Co4Nb2O9, is presented, based on X-ray single-crystal data. The space group and cation distribution previously obtained from powder data [Bertaut, Corliss, Forrat, Aleonard & Pauthenet (1961). J. Phys. Chem. Solids, 21, 234-251] are confirmed.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806012141/hb2026sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806012141/hb2026Isup2.hkl |
Computing details top
Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXTL-Plus (Sheldrick, 1998); program(s) used to refine structure: SHELXTL-Plus; molecular graphics: CaRIne Crystallography (Boudias & Monceau, 1998).
tetracobalt diniobium nonaoxide top
Crystal data top
Co4Nb2O9 | Dx = 5.728 Mg m−3 |
Mr = 565.54 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3c1 | Cell parameters from 34 reflections |
Hall symbol: -P 3 2"c | θ = 4.5–30.0° |
a = 5.1736 (3) Å | µ = 13.29 mm−1 |
c = 14.1457 (11) Å | T = 297 K |
V = 327.90 (4) Å3 | Block, violet |
Z = 2 | 0.12 × 0.07 × 0.05 mm |
F(000) = 524 |
Data collection top
Bruker P4 diffractometer | 262 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.076 |
Graphite monochromator | θmax = 30.0°, θmin = 2.9° |
ω scans | h = −7→7 |
Absorption correction: ψ scan (XSCANS; Siemens, 1996) | k = −7→7 |
Tmin = 0.272, Tmax = 0.510 | l = −19→19 |
1234 measured reflections | 2 standard reflections every 48 reflections |
328 independent reflections | intensity decay: 1.5% |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.031 | w = 1/[σ2(Fo2) + (0.0148P)2 + 2.3726P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.079 | (Δ/σ)max < 0.001 |
S = 1.28 | Δρmax = 0.95 e Å−3 |
328 reflections | Δρmin = −0.80 e Å−3 |
25 parameters | Extinction correction: SHELXTL-Plus, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0107 (11) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Nb1 | 0.0000 | 0.0000 | 0.14215 (4) | 0.0081 (3) | |
Co1 | 0.3333 | 0.6667 | 0.19304 (7) | 0.0103 (3) | |
Co2 | 0.3333 | 0.6667 | −0.01377 (8) | 0.0101 (3) | |
O1 | 0.0000 | 0.2876 (9) | 0.2500 | 0.0091 (9) | |
O2 | 0.0235 (7) | 0.6821 (7) | 0.0847 (2) | 0.0116 (7) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Nb1 | 0.0087 (3) | 0.0087 (3) | 0.0068 (3) | 0.00437 (15) | 0.000 | 0.000 |
Co1 | 0.0097 (4) | 0.0097 (4) | 0.0116 (5) | 0.0048 (2) | 0.000 | 0.000 |
Co2 | 0.0102 (4) | 0.0102 (4) | 0.0098 (5) | 0.0051 (2) | 0.000 | 0.000 |
O1 | 0.009 (2) | 0.0087 (14) | 0.0095 (19) | 0.0045 (10) | 0.0012 (15) | 0.0006 (8) |
O2 | 0.0103 (15) | 0.0104 (15) | 0.0135 (15) | 0.0049 (13) | −0.0005 (11) | −0.0024 (12) |
Geometric parameters (Å, º) top
Nb1—O2i | 1.892 (3) | Co1—O2iii | 2.247 (3) |
Nb1—O2ii | 1.892 (3) | Co2—O2vii | 2.083 (3) |
Nb1—O2iii | 1.892 (3) | Co2—O2viii | 2.083 (3) |
Nb1—O1 | 2.131 (3) | Co2—O2ix | 2.083 (3) |
Nb1—O1iv | 2.131 (3) | Co2—O2vi | 2.155 (3) |
Nb1—O1v | 2.131 (3) | Co2—O2 | 2.155 (3) |
Co1—O1vi | 2.022 (2) | Co2—O2iii | 2.155 (3) |
Co1—O1 | 2.022 (2) | O1—Co1x | 2.022 (2) |
Co1—O1iii | 2.022 (2) | O1—Nb1xi | 2.131 (3) |
Co1—O2 | 2.247 (3) | O2—Nb1xii | 1.892 (3) |
Co1—O2vi | 2.247 (3) | O2—Co2vii | 2.083 (3) |
O2i—Nb1—O2ii | 102.93 (11) | O2vi—Co1—O2iii | 78.64 (13) |
O2i—Nb1—O2iii | 102.93 (11) | O2vii—Co2—O2viii | 98.72 (12) |
O2ii—Nb1—O2iii | 102.93 (11) | O2vii—Co2—O2ix | 98.72 (12) |
O2i—Nb1—O1 | 91.50 (11) | O2viii—Co2—O2ix | 98.72 (12) |
O2ii—Nb1—O1 | 159.50 (13) | O2vii—Co2—O2vi | 168.48 (10) |
O2iii—Nb1—O1 | 87.65 (11) | O2viii—Co2—O2vi | 89.44 (12) |
O2i—Nb1—O1iv | 159.50 (13) | O2ix—Co2—O2vi | 87.97 (17) |
O2ii—Nb1—O1iv | 87.65 (11) | O2vii—Co2—O2 | 89.44 (12) |
O2iii—Nb1—O1iv | 91.50 (11) | O2viii—Co2—O2 | 87.97 (16) |
O1—Nb1—O1iv | 74.41 (13) | O2ix—Co2—O2 | 168.48 (10) |
O2i—Nb1—O1v | 87.65 (11) | O2vi—Co2—O2 | 82.70 (13) |
O2ii—Nb1—O1v | 91.50 (11) | O2vii—Co2—O2iii | 87.97 (16) |
O2iii—Nb1—O1v | 159.50 (13) | O2viii—Co2—O2iii | 168.48 (10) |
O1—Nb1—O1v | 74.41 (13) | O2ix—Co2—O2iii | 89.44 (12) |
O1iv—Nb1—O1v | 74.41 (13) | O2vi—Co2—O2iii | 82.70 (13) |
O1vi—Co1—O1 | 105.17 (5) | O2—Co2—O2iii | 82.70 (13) |
O1vi—Co1—O1iii | 105.17 (5) | Co1x—O1—Co1 | 114.1 (2) |
O1—Co1—O1iii | 105.17 (5) | Co1x—O1—Nb1 | 131.67 (5) |
O1vi—Co1—O2 | 81.47 (11) | Co1—O1—Nb1 | 95.40 (3) |
O1—Co1—O2 | 91.63 (10) | Co1x—O1—Nb1xi | 95.40 (3) |
O1iii—Co1—O2 | 159.21 (11) | Co1—O1—Nb1xi | 131.67 (5) |
O1vi—Co1—O2vi | 91.63 (10) | Nb1—O1—Nb1xi | 91.44 (17) |
O1—Co1—O2vi | 159.21 (11) | Nb1xii—O2—Co2vii | 123.06 (16) |
O1iii—Co1—O2vi | 81.47 (11) | Nb1xii—O2—Co2 | 132.99 (17) |
O2—Co1—O2vi | 78.64 (13) | Co2vii—O2—Co2 | 90.56 (12) |
O1vi—Co1—O2iii | 159.21 (11) | Nb1xii—O2—Co1 | 95.47 (13) |
O1—Co1—O2iii | 81.47 (11) | Co2vii—O2—Co1 | 129.54 (15) |
O1iii—Co1—O2iii | 91.63 (9) | Co2—O2—Co1 | 83.25 (12) |
O2—Co1—O2iii | 78.64 (13) | ||
O1vi—Co1—O1—Co1x | 18.27 (8) | O2vii—Co2—O2—Nb1xii | −139.0 (3) |
O2—Co1—O1—Co1x | −63.33 (8) | O2viii—Co2—O2—Nb1xii | −40.3 (2) |
O2vi—Co1—O1—Co1x | −124.6 (3) | O2ix—Co2—O2—Nb1xii | 85.6 (8) |
O2iii—Co1—O1—Co1x | −141.58 (9) | O2vi—Co2—O2—Nb1xii | 49.4 (3) |
O1vi—Co1—O1—Nb1 | 159.01 (15) | O2iii—Co2—O2—Nb1xii | 132.96 (18) |
O1iii—Co1—O1—Nb1 | −90.22 (9) | O2vii—Co2—O2—Co2vii | 0.0 |
O2—Co1—O1—Nb1 | 77.41 (11) | O2viii—Co2—O2—Co2vii | 98.75 (12) |
O2vi—Co1—O1—Nb1 | 16.1 (3) | O2ix—Co2—O2—Co2vii | −135.4 (6) |
O2iii—Co1—O1—Nb1 | −0.85 (10) | O2vi—Co2—O2—Co2vii | −171.55 (13) |
O1vi—Co1—O1—Nb1xi | −104.22 (12) | O2iii—Co2—O2—Co2vii | −88.03 (17) |
O1iii—Co1—O1—Nb1xi | 6.55 (19) | O2vii—Co2—O2—Co1 | 129.79 (14) |
O2—Co1—O1—Nb1xi | 174.2 (2) | O2viii—Co2—O2—Co1 | −131.46 (11) |
O2vi—Co1—O1—Nb1xi | 112.9 (2) | O2ix—Co2—O2—Co1 | −5.6 (7) |
O2iii—Co1—O1—Nb1xi | 95.9 (2) | O1vi—Co1—O2—Nb1xii | 0.95 (12) |
O2i—Nb1—O1—Co1x | 27.5 (2) | O1—Co1—O2—Nb1xii | 106.05 (14) |
O2ii—Nb1—O1—Co1x | −107.7 (3) | O1iii—Co1—O2—Nb1xii | −109.6 (3) |
O2iii—Nb1—O1—Co1x | 130.4 (2) | O2vi—Co1—O2—Nb1xii | −92.46 (19) |
O1iv—Nb1—O1—Co1x | −137.42 (16) | O2iii—Co1—O2—Nb1xii | −172.99 (15) |
O1v—Nb1—O1—Co1x | −59.7 (2) | O1vi—Co1—O2—Co2vii | −141.2 (2) |
O2i—Nb1—O1—Co1 | −101.88 (12) | O1—Co1—O2—Co2vii | −36.1 (2) |
O2ii—Nb1—O1—Co1 | 123.0 (3) | O1iii—Co1—O2—Co2vii | 108.3 (3) |
O2iii—Nb1—O1—Co1 | 1.00 (12) | O2vi—Co1—O2—Co2vii | 125.39 (15) |
O1iv—Nb1—O1—Co1 | 93.21 (11) | O2iii—Co1—O2—Co2vii | 44.9 (2) |
O2i—Nb1—O1—Nb1xi | 126.02 (10) | O1vi—Co1—O2—Co2 | 133.68 (10) |
O2ii—Nb1—O1—Nb1xi | −9.1 (3) | O1—Co1—O2—Co2 | −121.22 (12) |
O2iii—Nb1—O1—Nb1xi | −131.10 (10) | O1iii—Co1—O2—Co2 | 23.2 (3) |
Symmetry codes: (i) −x+y−1, −x, z; (ii) x, y−1, z; (iii) −y+1, x−y+1, z; (iv) −x+y, −x, z; (v) −y, x−y, z; (vi) −x+y, −x+1, z; (vii) −x, −y+1, −z; (viii) x−y+1, x+1, −z; (ix) y, −x+y, −z; (x) y−1, x, −z+1/2; (xi) y, x, −z+1/2; (xii) x, y+1, z. |