Bi3ScMo2O12, tribismuth(III) scandium molybdate(VI), has a framework structure derived from that of scheelite. It is nearly isotypic with Bi3FeMo2O12; while in the latter the FeIII atom is tetrahedrally coordinated by O atoms, the Sc atom in the title compound has a distorted octahedral coordination, and is substituted by Bi to a very minor extent (ca 4%). The change in coordination is achieved predominantly by shifts of two O atoms. The average Sc-O and Mo-O bond lengths are 2.162 and 1.775 Å, respectively. The environments of the two eight-coordinated Bi sites are very similar to those in Bi3FeMo2O12. All atoms are on general positions except Sc and one Bi (both of which have site symmetry 2).
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Mo-O) = 0.003 Å
- R factor = 0.022
- wR factor = 0.052
- Data-to-parameter ratio = 21.3
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
ABSMU_01 Alert C The ratio of given/expected absorption coefficient lies
outside the range 0.99 <> 1.01
Calculated value of mu = 55.621
Value of mu given = 54.940
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: COLLECT (Nonius, 2002); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO (Otwinowski & Minor, 1997)and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Shape Software, 1999) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
tribismuth(III) scandium molybdate(VI)
top
Crystal data top
Bi3.04Sc0.96Mo2O12 | F(000) = 1800 |
Mr = 1055.78 | Dx = 6.912 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1881 reflections |
a = 16.996 (3) Å | θ = 2.0–32.6° |
b = 11.601 (2) Å | µ = 54.94 mm−1 |
c = 5.319 (1) Å | T = 293 K |
β = 104.67 (3)° | Irregular fragment, yellow |
V = 1014.6 (3) Å3 | 0.06 × 0.05 × 0.05 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 1833 independent reflections |
Radiation source: fine-focus sealed tube | 1777 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
ψ and ω scans | θmax = 32.6°, θmin = 3.5° |
Absorption correction: multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997) | h = −25→25 |
Tmin = 0.052, Tmax = 0.064 | k = −17→17 |
3569 measured reflections | l = −8→7 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.022 | w = 1/[σ2(Fo2) + (0.025P)2 + 7.1P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.052 | (Δ/σ)max = 0.001 |
S = 1.14 | Δρmax = 3.57 e Å−3 |
1833 reflections | Δρmin = −3.08 e Å−3 |
86 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.00384 (9) |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
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 | Occ. (<1) |
Bi1 | 0.154483 (9) | 0.881574 (12) | 0.42921 (3) | 0.00517 (7) | |
Bi2 | 0.0000 | 0.662245 (17) | 0.2500 | 0.00605 (7) | |
Sc | 0.0000 | 0.09325 (10) | 0.2500 | 0.0063 (3) | 0.9589 (17) |
Bi3 | 0.0000 | 0.09325 (10) | 0.2500 | 0.0063 (3) | 0.0411 (17) |
Mo | 0.16858 (2) | 0.37156 (3) | 0.42735 (7) | 0.00543 (8) | |
O1 | 0.08237 (17) | 0.0238 (3) | 0.5871 (6) | 0.0061 (5) | |
O2 | 0.05005 (19) | 0.2055 (3) | 0.0279 (6) | 0.0084 (6) | |
O3 | 0.2165 (2) | 0.2877 (3) | 0.2330 (6) | 0.0111 (6) | |
O4 | 0.11628 (19) | 0.2825 (3) | 0.6196 (6) | 0.0093 (6) | |
O5 | 0.0948 (2) | 0.4556 (3) | 0.2225 (7) | 0.0144 (6) | |
O6 | 0.2466 (2) | 0.4544 (3) | 0.6306 (6) | 0.0122 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Bi1 | 0.00429 (10) | 0.00643 (9) | 0.00466 (10) | 0.00036 (4) | 0.00089 (7) | 0.00099 (4) |
Bi2 | 0.00514 (11) | 0.00476 (11) | 0.00849 (11) | 0.000 | 0.00216 (8) | 0.000 |
Sc | 0.0037 (5) | 0.0133 (5) | 0.0022 (5) | 0.000 | 0.0010 (3) | 0.000 |
Bi3 | 0.0037 (5) | 0.0133 (5) | 0.0022 (5) | 0.000 | 0.0010 (3) | 0.000 |
Mo | 0.00468 (17) | 0.00784 (16) | 0.00425 (19) | −0.00094 (12) | 0.00201 (14) | −0.00038 (11) |
O1 | 0.0044 (13) | 0.0079 (12) | 0.0055 (12) | 0.0000 (10) | 0.0005 (10) | −0.0011 (10) |
O2 | 0.0065 (13) | 0.0082 (13) | 0.0115 (14) | 0.0041 (10) | 0.0038 (11) | 0.0030 (11) |
O3 | 0.0098 (14) | 0.0120 (14) | 0.0129 (15) | −0.0007 (12) | 0.0055 (12) | −0.0027 (11) |
O4 | 0.0096 (14) | 0.0096 (13) | 0.0110 (14) | 0.0011 (11) | 0.0069 (12) | 0.0031 (11) |
O5 | 0.0158 (16) | 0.0144 (15) | 0.0124 (14) | 0.0028 (13) | 0.0027 (12) | 0.0014 (12) |
O6 | 0.0142 (15) | 0.0115 (14) | 0.0095 (14) | −0.0050 (12) | 0.0006 (12) | −0.0008 (11) |
Geometric parameters (Å, º) top
Bi1—O1i | 2.211 (3) | Bi2—O5vii | 2.955 (4) |
Bi1—O2ii | 2.218 (3) | Bi2—O5ii | 2.955 (4) |
Bi1—O1iii | 2.335 (3) | Sc—O2ix | 2.079 (3) |
Bi1—O4i | 2.492 (3) | Sc—O2 | 2.079 (3) |
Bi1—O3ii | 2.591 (3) | Sc—O1ix | 2.134 (3) |
Bi1—O6iv | 2.612 (3) | Sc—O1 | 2.134 (3) |
Bi1—O6v | 2.651 (3) | Sc—O1x | 2.274 (3) |
Bi1—O3vi | 2.775 (3) | Sc—O1xi | 2.274 (3) |
Bi2—O2ii | 2.151 (3) | Sc—O4 | 3.259 (3) |
Bi2—O2vii | 2.151 (3) | Sc—O4ix | 3.259 (3) |
Bi2—O4i | 2.344 (3) | Mo—O5 | 1.737 (3) |
Bi2—O4viii | 2.344 (3) | Mo—O3 | 1.762 (3) |
Bi2—O5ix | 2.913 (4) | Mo—O6 | 1.767 (3) |
Bi2—O5 | 2.913 (4) | Mo—O4 | 1.834 (3) |
| | | |
O2ix—Sc—O2 | 102.43 (18) | O2—Sc—O1xi | 77.16 (11) |
O2ix—Sc—O1ix | 115.98 (11) | O1ix—Sc—O1xi | 77.91 (12) |
O2—Sc—O1ix | 92.01 (12) | O1—Sc—O1xi | 76.02 (8) |
O2ix—Sc—O1 | 92.01 (12) | O1x—Sc—O1xi | 106.66 (16) |
O2—Sc—O1 | 115.98 (11) | O5—Mo—O3 | 108.03 (16) |
O1ix—Sc—O1 | 135.63 (17) | O5—Mo—O6 | 112.91 (16) |
O2ix—Sc—O1x | 77.16 (11) | O3—Mo—O6 | 105.82 (16) |
O2—Sc—O1x | 166.06 (11) | O5—Mo—O4 | 106.92 (16) |
O1ix—Sc—O1x | 76.02 (8) | O3—Mo—O4 | 112.13 (14) |
O1—Sc—O1x | 77.91 (12) | O6—Mo—O4 | 111.08 (15) |
O2ix—Sc—O1xi | 166.06 (11) | | |
Symmetry codes: (i) x, −y+1, z−1/2; (ii) x, −y+1, z+1/2; (iii) x, y+1, z; (iv) −x+1/2, −y+3/2, −z+1; (v) −x+1/2, y+1/2, −z+3/2; (vi) −x+1/2, y+1/2, −z+1/2; (vii) −x, −y+1, −z; (viii) −x, −y+1, −z+1; (ix) −x, y, −z+1/2; (x) −x, −y, −z+1; (xi) x, −y, z−1/2. |