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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806012141/hb2026sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806012141/hb2026Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 297 K
  • Mean [sigma](o-O) = 0.004 Å
  • R factor = 0.031
  • wR factor = 0.079
  • Data-to-parameter ratio = 13.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... 6 PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... m PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... m PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... m
Alert level C PLAT731_ALERT_1_C Bond Calc 2.022(5), Rep 2.022(2) ...... 2.50 su-Rat CO1 -O1 1.555 2.665
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

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
Co4Nb2O9Dx = 5.728 Mg m3
Mr = 565.54Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3c1Cell parameters from 34 reflections
Hall symbol: -P 3 2"cθ = 4.5–30.0°
a = 5.1736 (3) ŵ = 13.29 mm1
c = 14.1457 (11) ÅT = 297 K
V = 327.90 (4) Å3Block, violet
Z = 20.12 × 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 tubeRint = 0.076
Graphite monochromatorθmax = 30.0°, θmin = 2.9°
ω scansh = 77
Absorption correction: ψ scan
(XSCANS; Siemens, 1996)
k = 77
Tmin = 0.272, Tmax = 0.510l = 1919
1234 measured reflections2 standard reflections every 48 reflections
328 independent reflections intensity decay: 1.5%
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary 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 = 1.28Δρmax = 0.95 e Å3
328 reflectionsΔρmin = 0.80 e Å3
25 parametersExtinction correction: SHELXTL-Plus, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0107 (11)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nb10.00000.00000.14215 (4)0.0081 (3)
Co10.33330.66670.19304 (7)0.0103 (3)
Co20.33330.66670.01377 (8)0.0101 (3)
O10.00000.2876 (9)0.25000.0091 (9)
O20.0235 (7)0.6821 (7)0.0847 (2)0.0116 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0087 (3)0.0087 (3)0.0068 (3)0.00437 (15)0.0000.000
Co10.0097 (4)0.0097 (4)0.0116 (5)0.0048 (2)0.0000.000
Co20.0102 (4)0.0102 (4)0.0098 (5)0.0051 (2)0.0000.000
O10.009 (2)0.0087 (14)0.0095 (19)0.0045 (10)0.0012 (15)0.0006 (8)
O20.0103 (15)0.0104 (15)0.0135 (15)0.0049 (13)0.0005 (11)0.0024 (12)
Geometric parameters (Å, º) top
Nb1—O2i1.892 (3)Co1—O2iii2.247 (3)
Nb1—O2ii1.892 (3)Co2—O2vii2.083 (3)
Nb1—O2iii1.892 (3)Co2—O2viii2.083 (3)
Nb1—O12.131 (3)Co2—O2ix2.083 (3)
Nb1—O1iv2.131 (3)Co2—O2vi2.155 (3)
Nb1—O1v2.131 (3)Co2—O22.155 (3)
Co1—O1vi2.022 (2)Co2—O2iii2.155 (3)
Co1—O12.022 (2)O1—Co1x2.022 (2)
Co1—O1iii2.022 (2)O1—Nb1xi2.131 (3)
Co1—O22.247 (3)O2—Nb1xii1.892 (3)
Co1—O2vi2.247 (3)O2—Co2vii2.083 (3)
O2i—Nb1—O2ii102.93 (11)O2vi—Co1—O2iii78.64 (13)
O2i—Nb1—O2iii102.93 (11)O2vii—Co2—O2viii98.72 (12)
O2ii—Nb1—O2iii102.93 (11)O2vii—Co2—O2ix98.72 (12)
O2i—Nb1—O191.50 (11)O2viii—Co2—O2ix98.72 (12)
O2ii—Nb1—O1159.50 (13)O2vii—Co2—O2vi168.48 (10)
O2iii—Nb1—O187.65 (11)O2viii—Co2—O2vi89.44 (12)
O2i—Nb1—O1iv159.50 (13)O2ix—Co2—O2vi87.97 (17)
O2ii—Nb1—O1iv87.65 (11)O2vii—Co2—O289.44 (12)
O2iii—Nb1—O1iv91.50 (11)O2viii—Co2—O287.97 (16)
O1—Nb1—O1iv74.41 (13)O2ix—Co2—O2168.48 (10)
O2i—Nb1—O1v87.65 (11)O2vi—Co2—O282.70 (13)
O2ii—Nb1—O1v91.50 (11)O2vii—Co2—O2iii87.97 (16)
O2iii—Nb1—O1v159.50 (13)O2viii—Co2—O2iii168.48 (10)
O1—Nb1—O1v74.41 (13)O2ix—Co2—O2iii89.44 (12)
O1iv—Nb1—O1v74.41 (13)O2vi—Co2—O2iii82.70 (13)
O1vi—Co1—O1105.17 (5)O2—Co2—O2iii82.70 (13)
O1vi—Co1—O1iii105.17 (5)Co1x—O1—Co1114.1 (2)
O1—Co1—O1iii105.17 (5)Co1x—O1—Nb1131.67 (5)
O1vi—Co1—O281.47 (11)Co1—O1—Nb195.40 (3)
O1—Co1—O291.63 (10)Co1x—O1—Nb1xi95.40 (3)
O1iii—Co1—O2159.21 (11)Co1—O1—Nb1xi131.67 (5)
O1vi—Co1—O2vi91.63 (10)Nb1—O1—Nb1xi91.44 (17)
O1—Co1—O2vi159.21 (11)Nb1xii—O2—Co2vii123.06 (16)
O1iii—Co1—O2vi81.47 (11)Nb1xii—O2—Co2132.99 (17)
O2—Co1—O2vi78.64 (13)Co2vii—O2—Co290.56 (12)
O1vi—Co1—O2iii159.21 (11)Nb1xii—O2—Co195.47 (13)
O1—Co1—O2iii81.47 (11)Co2vii—O2—Co1129.54 (15)
O1iii—Co1—O2iii91.63 (9)Co2—O2—Co183.25 (12)
O2—Co1—O2iii78.64 (13)
O1vi—Co1—O1—Co1x18.27 (8)O2vii—Co2—O2—Nb1xii139.0 (3)
O2—Co1—O1—Co1x63.33 (8)O2viii—Co2—O2—Nb1xii40.3 (2)
O2vi—Co1—O1—Co1x124.6 (3)O2ix—Co2—O2—Nb1xii85.6 (8)
O2iii—Co1—O1—Co1x141.58 (9)O2vi—Co2—O2—Nb1xii49.4 (3)
O1vi—Co1—O1—Nb1159.01 (15)O2iii—Co2—O2—Nb1xii132.96 (18)
O1iii—Co1—O1—Nb190.22 (9)O2vii—Co2—O2—Co2vii0.0
O2—Co1—O1—Nb177.41 (11)O2viii—Co2—O2—Co2vii98.75 (12)
O2vi—Co1—O1—Nb116.1 (3)O2ix—Co2—O2—Co2vii135.4 (6)
O2iii—Co1—O1—Nb10.85 (10)O2vi—Co2—O2—Co2vii171.55 (13)
O1vi—Co1—O1—Nb1xi104.22 (12)O2iii—Co2—O2—Co2vii88.03 (17)
O1iii—Co1—O1—Nb1xi6.55 (19)O2vii—Co2—O2—Co1129.79 (14)
O2—Co1—O1—Nb1xi174.2 (2)O2viii—Co2—O2—Co1131.46 (11)
O2vi—Co1—O1—Nb1xi112.9 (2)O2ix—Co2—O2—Co15.6 (7)
O2iii—Co1—O1—Nb1xi95.9 (2)O1vi—Co1—O2—Nb1xii0.95 (12)
O2i—Nb1—O1—Co1x27.5 (2)O1—Co1—O2—Nb1xii106.05 (14)
O2ii—Nb1—O1—Co1x107.7 (3)O1iii—Co1—O2—Nb1xii109.6 (3)
O2iii—Nb1—O1—Co1x130.4 (2)O2vi—Co1—O2—Nb1xii92.46 (19)
O1iv—Nb1—O1—Co1x137.42 (16)O2iii—Co1—O2—Nb1xii172.99 (15)
O1v—Nb1—O1—Co1x59.7 (2)O1vi—Co1—O2—Co2vii141.2 (2)
O2i—Nb1—O1—Co1101.88 (12)O1—Co1—O2—Co2vii36.1 (2)
O2ii—Nb1—O1—Co1123.0 (3)O1iii—Co1—O2—Co2vii108.3 (3)
O2iii—Nb1—O1—Co11.00 (12)O2vi—Co1—O2—Co2vii125.39 (15)
O1iv—Nb1—O1—Co193.21 (11)O2iii—Co1—O2—Co2vii44.9 (2)
O2i—Nb1—O1—Nb1xi126.02 (10)O1vi—Co1—O2—Co2133.68 (10)
O2ii—Nb1—O1—Nb1xi9.1 (3)O1—Co1—O2—Co2121.22 (12)
O2iii—Nb1—O1—Nb1xi131.10 (10)O1iii—Co1—O2—Co223.2 (3)
Symmetry codes: (i) x+y1, x, z; (ii) x, y1, z; (iii) y+1, xy+1, z; (iv) x+y, x, z; (v) y, xy, z; (vi) x+y, x+1, z; (vii) x, y+1, z; (viii) xy+1, x+1, z; (ix) y, x+y, z; (x) y1, x, z+1/2; (xi) y, x, z+1/2; (xii) x, y+1, z.
 

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