Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100015597/na0110sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100015597/na0110sup2.fcf |
Data collection: STOE IPDS Software; cell refinement: STOE IPDS Software; data reduction: STOE IPDS Software; program(s) used to solve structure: coordinates from model; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
MoO4Tl2 | F(000) = 944 |
Mr = 568.68 | Dx = 6.931 Mg m−3 |
Monoclinic, C2 | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: C 2y | Cell parameters from 1132 reflections |
a = 10.565 (3) Å | θ = 2.5–25.9° |
b = 6.4178 (13) Å | µ = 61.16 mm−1 |
c = 8.039 (2) Å | T = 293 K |
β = 91.05 (4)° | Hexagonal prismatic, yellow |
V = 545.0 (3) Å3 | 0.09 × 0.08 × 0.003 mm |
Z = 4 |
STOE IPDS diffractometer | 644 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.057 |
Graphite monochromator | θmax = 25.9°, θmin = 2.5° |
Absorption correction: gaussian ? | h = −12→12 |
Tmin = 0.050, Tmax = 0.796 | k = −7→7 |
2138 measured reflections | l = −9→9 |
1006 independent reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Calculated w = 1/[σ2(Fo2) + (0.P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.029 | (Δ/σ)max = 0.001 |
wR(F2) = 0.039 | Δρmax = 0.96 e Å−3 |
S = 0.71 | Δρmin = −0.93 e Å−3 |
1006 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
66 parameters | Extinction coefficient: 0.00092 (4) |
0 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: model | Absolute structure parameter: 0.159 (16) |
MoO4Tl2 | V = 545.0 (3) Å3 |
Mr = 568.68 | Z = 4 |
Monoclinic, C2 | Mo Kα radiation |
a = 10.565 (3) Å | µ = 61.16 mm−1 |
b = 6.4178 (13) Å | T = 293 K |
c = 8.039 (2) Å | 0.09 × 0.08 × 0.003 mm |
β = 91.05 (4)° |
STOE IPDS diffractometer | 1006 independent reflections |
Absorption correction: gaussian ? | 644 reflections with I > 2σ(I) |
Tmin = 0.050, Tmax = 0.796 | Rint = 0.057 |
2138 measured reflections |
R[F2 > 2σ(F2)] = 0.029 | 0 restraints |
wR(F2) = 0.039 | Δρmax = 0.96 e Å−3 |
S = 0.71 | Δρmin = −0.93 e Å−3 |
1006 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
66 parameters | Absolute structure parameter: 0.159 (16) |
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. |
x | y | z | Uiso*/Ueq | ||
Tl1 | 0.0000 | 0.0000 | 0.0000 | 0.0300 (5) | |
Tl2 | 0.0000 | 0.0506 (3) | 0.5000 | 0.0309 (5) | |
Tl3 | 0.33358 (12) | 0.0071 (4) | 0.17767 (15) | 0.0377 (5) | |
Mo1 | 0.6623 (2) | 0.0257 (5) | 0.3081 (2) | 0.0172 (6) | |
O1 | 0.6911 (15) | −0.0510 (19) | 0.5099 (15) | 0.051 (4) | |
O2 | 0.5627 (17) | 0.2330 (18) | 0.2873 (18) | 0.048 (5) | |
O3 | 0.8026 (14) | 0.080 (2) | 0.2167 (18) | 0.051 (4) | |
O4 | 0.5837 (17) | −0.1848 (19) | 0.2007 (18) | 0.047 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Tl1 | 0.0328 (9) | 0.0296 (13) | 0.0278 (8) | 0.000 | 0.0034 (7) | 0.000 |
Tl2 | 0.0428 (10) | 0.0265 (11) | 0.0235 (9) | 0.000 | 0.0004 (8) | 0.000 |
Tl3 | 0.0369 (6) | 0.0490 (11) | 0.0272 (7) | 0.0030 (7) | −0.0023 (5) | 0.0007 (9) |
Mo1 | 0.0197 (11) | 0.0161 (17) | 0.0157 (12) | 0.0017 (10) | 0.0008 (10) | 0.0026 (14) |
O1 | 0.090 (13) | 0.049 (7) | 0.014 (7) | 0.007 (8) | −0.011 (8) | −0.004 (6) |
O2 | 0.068 (13) | 0.044 (7) | 0.032 (10) | 0.040 (7) | −0.019 (9) | −0.021 (6) |
O3 | 0.037 (10) | 0.069 (8) | 0.049 (10) | −0.015 (7) | 0.015 (8) | −0.010 (7) |
O4 | 0.065 (13) | 0.049 (9) | 0.029 (11) | −0.016 (8) | 0.022 (10) | 0.000 (6) |
Tl1—O4i | 2.725 (12) | Mo1—O2 | 1.702 (13) |
Tl1—O4ii | 2.725 (12) | Mo1—O3 | 1.702 (14) |
Tl1—O3iii | 2.789 (14) | Mo1—O1 | 1.717 (12) |
Tl1—O3iv | 2.789 (14) | Mo1—O4 | 1.798 (13) |
Tl1—Tl3 | 3.7784 (18) | O1—Tl3viii | 2.557 (13) |
Tl1—Tl3v | 3.7784 (18) | O2—Tl2ix | 2.749 (12) |
Tl2—O2vi | 2.749 (12) | O3—Tl3ix | 2.781 (13) |
Tl2—O2vii | 2.749 (12) | O3—Tl1x | 2.789 (14) |
Tl3—O1viii | 2.557 (13) | O4—Tl1xi | 2.725 (12) |
Tl3—O3vi | 2.781 (13) | ||
O4i—Tl1—O4ii | 84.1 (7) | O1viii—Tl3—O3vi | 74.4 (4) |
O4i—Tl1—O3iii | 89.7 (4) | O1viii—Tl3—Tl1 | 105.0 (4) |
O4ii—Tl1—O3iii | 74.5 (4) | O3vi—Tl3—Tl1 | 85.4 (3) |
O4i—Tl1—O3iv | 74.5 (4) | O2—Mo1—O3 | 109.9 (8) |
O4ii—Tl1—O3iv | 89.7 (4) | O2—Mo1—O1 | 114.5 (7) |
O3iii—Tl1—O3iv | 158.9 (5) | O3—Mo1—O1 | 109.0 (7) |
O4i—Tl1—Tl3 | 58.5 (4) | O2—Mo1—O4 | 105.1 (7) |
O4ii—Tl1—Tl3 | 120.3 (4) | O3—Mo1—O4 | 110.1 (7) |
O3iii—Tl1—Tl3 | 62.0 (3) | O1—Mo1—O4 | 108.1 (7) |
O3iv—Tl1—Tl3 | 117.7 (3) | Mo1—O1—Tl3viii | 150.1 (7) |
O4i—Tl1—Tl3v | 120.3 (4) | Mo1—O2—Tl2ix | 132.4 (7) |
O4ii—Tl1—Tl3v | 58.5 (4) | Mo1—O3—Tl3ix | 110.7 (6) |
O3iii—Tl1—Tl3v | 117.7 (3) | Mo1—O3—Tl1x | 154.1 (7) |
O3iv—Tl1—Tl3v | 62.0 (3) | Tl3ix—O3—Tl1x | 91.1 (4) |
Tl3—Tl1—Tl3v | 178.63 (7) | Mo1—O4—Tl1xi | 169.8 (8) |
O2vi—Tl2—O2vii | 84.3 (7) |
Symmetry codes: (i) x−1/2, y+1/2, z; (ii) −x+1/2, y+1/2, −z; (iii) −x+1, y, −z; (iv) x−1, y, z; (v) −x, y, −z; (vi) x−1/2, y−1/2, z; (vii) −x+1/2, y−1/2, −z+1; (viii) −x+1, y, −z+1; (ix) x+1/2, y+1/2, z; (x) x+1, y, z; (xi) x+1/2, y−1/2, z. |
Experimental details
Crystal data | |
Chemical formula | MoO4Tl2 |
Mr | 568.68 |
Crystal system, space group | Monoclinic, C2 |
Temperature (K) | 293 |
a, b, c (Å) | 10.565 (3), 6.4178 (13), 8.039 (2) |
β (°) | 91.05 (4) |
V (Å3) | 545.0 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 61.16 |
Crystal size (mm) | 0.09 × 0.08 × 0.003 |
Data collection | |
Diffractometer | STOE IPDS diffractometer |
Absorption correction | Gaussian |
Tmin, Tmax | 0.050, 0.796 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2138, 1006, 644 |
Rint | 0.057 |
(sin θ/λ)max (Å−1) | 0.615 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.039, 0.71 |
No. of reflections | 1006 |
No. of parameters | 66 |
Δρmax, Δρmin (e Å−3) | 0.96, −0.93 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0.159 (16) |
Computer programs: STOE IPDS Software, coordinates from model, SHELXL97 (Sheldrick, 1997).