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Acta Cryst. (2000). B56, 204-209
https://doi.org/10.1107/S0108768199014846
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Structure of the alums. I. On the sulfate group disorder in the α-alums

S. C. Nyburg, J. W. Steed, S. Aleksovska and V. M. Petruševski
The crystal structures at room (296 K) and low (173 K) temperature of several α-alums have been refined by single-crystal X-ray structure analysis. Many α-alums of known structure are disordered, the sulfate anions occupying one of two possible sites. All those studied here exhibited such disorder and the relative occupancies of the two sites are in excellent agreement with those obtained by Raman spectroscopy, where the ν1(SO4) mode is seen as a doublet owing to the presence of two different types of sulfate ion. No phase transitions were noted on cooling but there is less disorder.
Keywords: α-Alums; Sulfate; Disorder.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768199014846/na0101sup1.cif
Contains datablocks ou, ot, or, ol, ov, os, on, oq, global

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768199014846/na0101sup2.pdf
Supplementary material

Computing details top

For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

(ou) top
Crystal data top
H24AlKO20S2F(000) = 992
Mr = 474.39Dx = 1.763 Mg m−3
Cubic, Pa3Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2ab 3µ = 0.67 mm−1
a = 12.1350 (5) ÅT = 173 K
V = 1786.98 (13) Å30.6 × 0.5 × 0.5 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.009
Graphite monochromatorθmax = 26.0°, θmin = 3.8°
1087 measured reflectionsh = −10→10
584 independent reflectionsk = −14→14
571 reflections with I > 2σ(I)l = −10→10
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.022H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.063Calculated w = 1/[σ2(Fo2) + (0.0516P)2 + 0.6165P]
where P = (Fo2 + 2Fc2)/3
S = 0.90(Δ/σ)max = 0.001
584 reflectionsΔρmax = 0.21 e Å−3
68 parametersΔρmin = −0.33 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.069 (4)
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
xyzUiso*/UeqOcc. (<1)
S0.30610 (2)0.30610 (2)0.30610 (2)0.0150 (2)
Al10.00000.00000.00000.0130 (3)
O10.15173 (7)0.02080 (7)−0.01985 (8)0.0191 (3)
H120.1982 (17)0.0262 (18)0.034 (2)0.048 (5)*
H110.1750 (15)0.0365 (16)−0.0726 (17)0.034 (5)*
O20.04692 (9)0.13071 (8)0.30399 (7)0.0232 (3)
H220.0009 (18)0.1821 (16)0.2914 (17)0.042 (5)*
H210.104 (2)0.155 (2)0.3000 (16)0.044 (5)*
O30.23606 (11)0.23606 (11)0.23606 (11)0.0294 (6)0.787 (3)
O40.26302 (10)0.41979 (9)0.30624 (9)0.0240 (4)0.787 (3)
K0.50000.50000.50000.0271 (3)
O3A0.3746 (3)0.3746 (3)0.3746 (3)0.0226 (16)0.213 (3)
O4A0.2808 (3)0.2000 (3)0.3614 (3)0.0185 (13)0.213 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S0.0150 (2)0.0150 (2)0.0150 (2)0.00178 (9)0.00178 (9)0.00178 (9)
Al10.0130 (3)0.0130 (3)0.0130 (3)0.00010 (15)0.00010 (15)0.00010 (15)
O10.0150 (4)0.0231 (5)0.0190 (5)−0.0021 (3)0.0007 (4)0.0014 (3)
O20.0233 (5)0.0227 (5)0.0235 (5)0.0007 (4)−0.0022 (4)−0.0011 (3)
O30.0294 (6)0.0294 (6)0.0294 (6)−0.0038 (5)−0.0038 (5)−0.0038 (5)
O40.0299 (7)0.0194 (7)0.0226 (6)0.0088 (5)0.0074 (4)0.0044 (4)
K0.0271 (3)0.0271 (3)0.0271 (3)0.00815 (16)0.00815 (16)0.00815 (16)
O3A0.0226 (16)0.0226 (16)0.0226 (16)−0.0074 (14)−0.0074 (14)−0.0074 (14)
O4A0.019 (2)0.016 (2)0.020 (2)0.0019 (14)0.0039 (16)0.0091 (16)
Geometric parameters (Å, º) top
S—O3A1.440 (6)O2—H210.76 (3)
S—O31.472 (2)O3—O4Ai1.673 (4)
S—O41.4754 (11)O3—O4Aii1.673 (4)
S—O4i1.4754 (11)O3—O4A1.673 (4)
S—O4ii1.4754 (11)O4—O4Aii1.088 (4)
S—O4Ai1.484 (3)O4—O3A1.680 (3)
S—O4A1.484 (3)K—O3Avii2.635 (6)
S—O4Aii1.484 (3)K—O3A2.635 (6)
Al1—O1ii1.8740 (8)K—O2viii2.9151 (9)
Al1—O11.8740 (8)K—O2ix2.9151 (9)
Al1—O1iii1.8740 (8)K—O2x2.9151 (9)
Al1—O1iv1.8740 (8)K—O2xi2.9151 (9)
Al1—O1v1.8740 (8)K—O2xii2.9151 (9)
Al1—O1i1.8740 (8)K—O2xiii2.9151 (9)
O1—H120.87 (2)O3A—O4i1.680 (3)
O1—H110.73 (2)O3A—O4ii1.680 (3)
O2—Kvi2.9151 (9)O4A—O4i1.088 (4)
O2—H220.85 (2)
O3A—S—O3180.0 (4)S—O3—O4Aii55.87 (14)
O3A—S—O470.37 (5)O4Ai—O3—O4Aii91.6 (2)
O3—S—O4109.63 (5)S—O3—O4A55.87 (14)
O3A—S—O4i70.37 (5)O4Ai—O3—O4A91.6 (2)
O3—S—O4i109.63 (5)O4Aii—O3—O4A91.6 (2)
O4—S—O4i109.31 (5)O4Aii—O4—S68.85 (19)
O3A—S—O4ii70.37 (5)O4Aii—O4—O3A119.6 (3)
O3—S—O4ii109.63 (5)S—O4—O3A53.83 (17)
O4—S—O4ii109.31 (5)O3Avii—K—O3A180.0
O4i—S—O4ii109.31 (5)O3Avii—K—O2viii105.647 (18)
O3A—S—O4Ai111.06 (16)O3A—K—O2viii74.353 (18)
O3—S—O4Ai68.94 (16)O3Avii—K—O2ix74.354 (18)
O4—S—O4Ai110.75 (16)O3A—K—O2ix105.646 (18)
O4i—S—O4Ai137.55 (15)O2viii—K—O2ix66.990 (16)
O4ii—S—O4Ai43.13 (16)O3Avii—K—O2x105.646 (19)
O3A—S—O4A111.06 (16)O3A—K—O2x74.354 (18)
O3—S—O4A68.94 (16)O2viii—K—O2x113.010 (16)
O4—S—O4A137.55 (15)O2ix—K—O2x66.990 (16)
O4i—S—O4A43.13 (16)O3Avii—K—O2xi105.646 (18)
O4ii—S—O4A110.75 (16)O3A—K—O2xi74.354 (18)
O4Ai—S—O4A107.83 (17)O2viii—K—O2xi113.010 (16)
O3A—S—O4Aii111.06 (16)O2ix—K—O2xi180.0
O3—S—O4Aii68.94 (16)O2x—K—O2xi113.010 (15)
O4—S—O4Aii43.13 (16)O3Avii—K—O2xii74.353 (18)
O4i—S—O4Aii110.75 (16)O3A—K—O2xii105.647 (18)
O4ii—S—O4Aii137.55 (15)O2viii—K—O2xii180.0
O4Ai—S—O4Aii107.83 (17)O2ix—K—O2xii113.010 (16)
O4A—S—O4Aii107.83 (17)O2x—K—O2xii66.990 (16)
O1ii—Al1—O190.65 (4)O2xi—K—O2xii66.990 (16)
O1ii—Al1—O1iii89.35 (4)O3Avii—K—O2xiii74.353 (18)
O1—Al1—O1iii89.35 (4)O3A—K—O2xiii105.647 (18)
O1ii—Al1—O1iv89.35 (4)O2viii—K—O2xiii66.990 (16)
O1—Al1—O1iv180.0O2ix—K—O2xiii113.010 (15)
O1iii—Al1—O1iv90.65 (4)O2x—K—O2xiii180.0
O1ii—Al1—O1v180.0O2xi—K—O2xiii66.990 (16)
O1—Al1—O1v89.35 (4)O2xii—K—O2xiii113.010 (16)
O1iii—Al1—O1v90.65 (4)S—O3A—O4i55.80 (17)
O1iv—Al1—O1v90.65 (4)S—O3A—O4ii55.80 (17)
O1ii—Al1—O1i90.65 (4)O4i—O3A—O4ii91.5 (2)
O1—Al1—O1i90.65 (4)S—O3A—O455.80 (17)
O1iii—Al1—O1i180.0O4i—O3A—O491.5 (2)
O1iv—Al1—O1i89.35 (4)O4ii—O3A—O491.5 (2)
O1v—Al1—O1i89.35 (4)S—O3A—K180.0 (5)
Al1—O1—H12123.4 (14)O4i—O3A—K124.20 (17)
Al1—O1—H11122.1 (13)O4ii—O3A—K124.20 (17)
H12—O1—H11113 (2)O4—O3A—K124.20 (17)
Kvi—O2—H22114.7 (14)O4i—O4A—S68.02 (19)
Kvi—O2—H21116.3 (15)O4i—O4A—O3120.0 (3)
H22—O2—H21108 (2)S—O4A—O355.20 (13)
S—O3—O4Ai55.87 (14)
O3A—S—O3—O4Ai29 (100)O4Aii—S—O3A—K95 (100)
O4—S—O3—O4Ai105.41 (16)O4Aii—O4—O3A—S21.6 (2)
O4i—S—O3—O4Ai−134.59 (16)O4Aii—O4—O3A—O4i−24.1 (3)
O4ii—S—O3—O4Ai−14.59 (16)S—O4—O3A—O4i−45.77 (13)
O4A—S—O3—O4Ai−120.0O4Aii—O4—O3A—O4ii67.4 (3)
O4Aii—S—O3—O4Ai120.0S—O4—O3A—O4ii45.77 (13)
O3A—S—O3—O4Aii−91 (100)O4Aii—O4—O3A—K−158.4 (2)
O4—S—O3—O4Aii−14.59 (16)S—O4—O3A—K180.0
O4i—S—O3—O4Aii105.41 (16)O3Avii—K—O3A—S0 (100)
O4ii—S—O3—O4Aii−134.59 (16)O2viii—K—O3A—S−32 (100)
O4Ai—S—O3—O4Aii−120.0O2ix—K—O3A—S28 (100)
O4A—S—O3—O4Aii120.0O2x—K—O3A—S88 (100)
O3A—S—O3—O4A149 (100)O2xi—K—O3A—S−152 (100)
O4—S—O3—O4A−134.59 (16)O2xii—K—O3A—S148 (100)
O4i—S—O3—O4A−14.59 (16)O2xiii—K—O3A—S−92 (100)
O4ii—S—O3—O4A105.41 (16)O3Avii—K—O3A—O4i−135 (100)
O4Ai—S—O3—O4A120.0O2viii—K—O3A—O4i−42.59 (5)
O4Aii—S—O3—O4A−120.0O2ix—K—O3A—O4i17.41 (5)
O3A—S—O4—O4Aii−159.9 (2)O2x—K—O3A—O4i77.41 (5)
O3—S—O4—O4Aii20.1 (2)O2xi—K—O3A—O4i−162.59 (5)
O4i—S—O4—O4Aii−100.1 (2)O2xii—K—O3A—O4i137.41 (5)
O4ii—S—O4—O4Aii140.3 (2)O2xiii—K—O3A—O4i−102.59 (5)
O4Ai—S—O4—O4Aii94.3 (3)O3Avii—K—O3A—O4ii105 (100)
O4A—S—O4—O4Aii−59.8 (3)O2viii—K—O3A—O4ii−162.59 (5)
O3—S—O4—O3A180.0O2ix—K—O3A—O4ii−102.59 (5)
O4i—S—O4—O3A59.80 (6)O2x—K—O3A—O4ii−42.59 (5)
O4ii—S—O4—O3A−59.80 (6)O2xi—K—O3A—O4ii77.41 (5)
O4Ai—S—O4—O3A−105.84 (18)O2xii—K—O3A—O4ii17.41 (5)
O4A—S—O4—O3A100.1 (3)O2xiii—K—O3A—O4ii137.41 (5)
O4Aii—S—O4—O3A159.9 (2)O3Avii—K—O3A—O4−15 (100)
O3—S—O3A—O4i−163 (100)O2viii—K—O3A—O477.41 (5)
O4—S—O3A—O4i120.0O2ix—K—O3A—O4137.41 (5)
O4ii—S—O3A—O4i−120.0O2x—K—O3A—O4−162.59 (5)
O4Ai—S—O3A—O4i−134.59 (16)O2xi—K—O3A—O4−42.59 (5)
O4A—S—O3A—O4i−14.59 (16)O2xii—K—O3A—O4−102.59 (5)
O4Aii—S—O3A—O4i105.41 (16)O2xiii—K—O3A—O417.41 (5)
O3—S—O3A—O4ii−43 (100)O3A—S—O4A—O4i20.3 (2)
O4—S—O3A—O4ii−120.0O3—S—O4A—O4i−159.7 (2)
O4i—S—O3A—O4ii120.0O4—S—O4A—O4i−63.2 (3)
O4Ai—S—O3A—O4ii−14.59 (16)O4ii—S—O4A—O4i96.47 (19)
O4A—S—O3A—O4ii105.41 (16)O4Ai—S—O4A—O4i142.2 (3)
O4Aii—S—O3A—O4ii−134.59 (16)O4Aii—S—O4A—O4i−101.6 (3)
O3—S—O3A—O477 (100)O3A—S—O4A—O3180.0
O4i—S—O3A—O4−120.0O4—S—O4A—O396.5 (2)
O4ii—S—O3A—O4120.0O4i—S—O4A—O3159.7 (2)
O4Ai—S—O3A—O4105.41 (16)O4ii—S—O4A—O3−103.84 (10)
O4A—S—O3A—O4−134.59 (16)O4Ai—S—O4A—O3−58.10 (19)
O4Aii—S—O3A—O4−14.59 (16)O4Aii—S—O4A—O358.10 (19)
O3—S—O3A—K0 (100)S—O3—O4A—O4i21.8 (2)
O4—S—O3A—K109 (100)O4Ai—O3—O4A—O4i67.6 (2)
O4i—S—O3A—K−11 (100)O4Aii—O3—O4A—O4i−24.0 (3)
O4ii—S—O3A—K−131 (100)O4Ai—O3—O4A—S45.82 (11)
O4Ai—S—O3A—K−145 (100)O4Aii—O3—O4A—S−45.82 (11)
O4A—S—O3A—K−25 (100)
Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) −z, −x, −y; (iv) −x, −y, −z; (v) −y, −z, −x; (vi) y−1/2, −z+1/2, −x+1; (vii) −x+1, −y+1, −z+1; (viii) z, −x+1/2, y+1/2; (ix) x+1/2, −y+1/2, −z+1; (x) y+1/2, z, −x+1/2; (xi) −x+1/2, y+1/2, z; (xii) −z+1, x+1/2, −y+1/2; (xiii) −y+1/2, −z+1, x+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4xiv0.73 (2)1.89 (2)2.6071 (14)168.2 (18)
O1—H12···O2i0.87 (2)1.76 (2)2.6178 (12)172 (2)
O2—H21···O30.76 (3)2.03 (3)2.7536 (16)159 (2)
O2—H22···O4xv0.85 (2)1.92 (2)2.7529 (14)167 (2)
O1—H11···O4Axvi0.73 (2)2.19 (2)2.870 (4)156.9 (19)
O2—H22···O4Axvii0.85 (2)2.08 (2)2.897 (4)161.6 (19)
O2—H21···O4A0.76 (3)2.33 (3)3.041 (4)156 (2)
Symmetry codes: (i) z, x, y; (xiv) x, −y+1/2, z−1/2; (xv) y−1/2, z, −x+1/2; (xvi) y, −z+1/2, x−1/2; (xvii) z−1/2, x, −y+1/2.
(ot) top
Crystal data top
H24AlKO20S2F(000) = 992
Mr = 474.39Dx = 1.751 Mg m−3
Cubic, Pa3Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2ab 3µ = 0.67 mm−1
a = 12.1640 (5) ÅT = 296 K
V = 1799.82 (13) Å30.6 × 0.6 × 0.5 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.009
Graphite monochromatorθmax = 26.0°, θmin = 3.4°
1101 measured reflectionsh = −15→14
592 independent reflectionsk = −10→10
558 reflections with I > 2σ(I)l = −10→10
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.073Calculated w = 1/[σ2(Fo2) + (0.053P)2 + 0.7284P]
where P = (Fo2 + 2Fc2)/3
S = 0.92(Δ/σ)max < 0.001
592 reflectionsΔρmax = 0.24 e Å−3
68 parametersΔρmin = −0.29 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.064 (4)
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
xyzUiso*/UeqOcc. (<1)
S0.30764 (3)0.30764 (3)0.30764 (3)0.0265 (3)
Al10.00000.00000.00000.0208 (3)
O10.15176 (8)0.01980 (9)−0.01855 (10)0.0308 (3)
H120.198 (2)0.025 (2)0.038 (2)0.061 (6)*
H110.1752 (17)0.0350 (18)−0.0683 (19)0.044 (6)*
O20.04633 (12)0.13357 (10)0.30258 (9)0.0417 (4)
H220.008 (2)0.184 (2)0.290 (2)0.060 (7)*
H210.104 (3)0.160 (2)0.299 (2)0.077 (9)*
O30.23898 (16)0.23898 (16)0.23898 (16)0.0633 (12)0.697 (5)
O40.2648 (2)0.42078 (16)0.30973 (15)0.0479 (8)0.697 (5)
K10.50000.50000.50000.0492 (3)
O3A0.3749 (4)0.3749 (4)0.3749 (4)0.082 (3)0.303 (5)
O4A0.2853 (4)0.2042 (4)0.3643 (5)0.0501 (18)0.303 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S0.0265 (3)0.0265 (3)0.0265 (3)0.00369 (12)0.00369 (12)0.00369 (12)
Al10.0208 (3)0.0208 (3)0.0208 (3)−0.00036 (18)−0.00036 (18)−0.00036 (18)
O10.0237 (5)0.0385 (6)0.0303 (6)−0.0046 (4)0.0013 (4)0.0013 (4)
O20.0443 (8)0.0396 (7)0.0413 (7)0.0008 (6)−0.0050 (5)−0.0052 (5)
O30.0633 (12)0.0633 (12)0.0633 (12)−0.0121 (9)−0.0121 (9)−0.0121 (9)
O40.0620 (15)0.0378 (11)0.0440 (10)0.0213 (10)0.0212 (9)0.0115 (7)
K10.0492 (3)0.0492 (3)0.0492 (3)0.0104 (2)0.0104 (2)0.0104 (2)
O3A0.082 (3)0.082 (3)0.082 (3)−0.028 (2)−0.028 (2)−0.028 (2)
O4A0.048 (2)0.037 (3)0.066 (4)0.0116 (19)0.023 (2)0.027 (3)
Geometric parameters (Å, º) top
S—O3A1.418 (8)O2—H210.77 (3)
S—O31.447 (3)O3—O4Ai1.679 (6)
S—O4Ai1.460 (4)O3—O4Aii1.679 (6)
S—O4A1.460 (4)O3—O4A1.679 (6)
S—O4Aii1.460 (4)O4—O4Aii1.051 (6)
S—O4ii1.4717 (17)O4—O3A1.654 (5)
S—O41.4717 (17)K1—O3A2.635 (8)
S—O4i1.4717 (17)K1—O3Avii2.635 (8)
Al1—O1iii1.8753 (10)K1—O2viii2.9536 (12)
Al1—O1i1.8753 (10)K1—O2ix2.9536 (12)
Al1—O11.8753 (10)K1—O2x2.9536 (12)
Al1—O1ii1.8753 (10)K1—O2xi2.9537 (12)
Al1—O1iv1.8753 (10)K1—O2xii2.9537 (12)
Al1—O1v1.8753 (10)K1—O2xiii2.9537 (12)
O1—H120.89 (3)O3A—O4ii1.654 (5)
O1—H110.69 (2)O3A—O4i1.654 (5)
O2—K1vi2.9536 (12)O4A—O4i1.051 (6)
O2—H220.78 (3)
O3A—S—O3180.0 (5)S—O3—O4Aii55.1 (2)
O3A—S—O4Ai109.4 (3)O4Ai—O3—O4Aii90.5 (3)
O3—S—O4Ai70.6 (3)S—O3—O4A55.1 (2)
O3A—S—O4A109.4 (3)O4Ai—O3—O4A90.5 (3)
O3—S—O4A70.6 (3)O4Aii—O3—O4A90.5 (3)
O4Ai—S—O4A109.5 (3)O4Aii—O4—S68.4 (2)
O3A—S—O4Aii109.4 (3)O4Aii—O4—O3A118.9 (3)
O3—S—O4Aii70.6 (3)S—O4—O3A53.6 (2)
O4Ai—S—O4Aii109.5 (3)O3A—K1—O3Avii180.0
O4A—S—O4Aii109.5 (3)O3A—K1—O2viii74.81 (3)
O3A—S—O4ii69.78 (12)O3Avii—K1—O2viii105.19 (3)
O3—S—O4ii110.22 (12)O3A—K1—O2ix74.81 (3)
O4Ai—S—O4ii42.0 (2)O3Avii—K1—O2ix105.19 (3)
O4A—S—O4ii110.86 (18)O2viii—K1—O2ix113.39 (2)
O4Aii—S—O4ii137.04 (18)O3A—K1—O2x105.19 (3)
O3A—S—O469.78 (12)O3Avii—K1—O2x74.81 (3)
O3—S—O4110.22 (12)O2viii—K1—O2x180.0
O4Ai—S—O4110.86 (18)O2ix—K1—O2x66.61 (2)
O4A—S—O4137.04 (18)O3A—K1—O2xi105.19 (3)
O4Aii—S—O442.0 (2)O3Avii—K1—O2xi74.81 (3)
O4ii—S—O4108.71 (12)O2viii—K1—O2xi66.61 (2)
O3A—S—O4i69.78 (12)O2ix—K1—O2xi66.61 (2)
O3—S—O4i110.22 (12)O2x—K1—O2xi113.39 (2)
O4Ai—S—O4i137.04 (18)O3A—K1—O2xii105.19 (3)
O4A—S—O4i42.0 (2)O3Avii—K1—O2xii74.81 (3)
O4Aii—S—O4i110.86 (18)O2viii—K1—O2xii66.61 (2)
O4ii—S—O4i108.71 (12)O2ix—K1—O2xii180.0
O4—S—O4i108.71 (12)O2x—K1—O2xii113.39 (2)
O1iii—Al1—O1i89.57 (5)O2xi—K1—O2xii113.39 (2)
O1iii—Al1—O189.57 (5)O3A—K1—O2xiii74.81 (3)
O1i—Al1—O190.43 (5)O3Avii—K1—O2xiii105.19 (3)
O1iii—Al1—O1ii180.0O2viii—K1—O2xiii113.39 (2)
O1i—Al1—O1ii90.43 (5)O2ix—K1—O2xiii113.39 (2)
O1—Al1—O1ii90.43 (5)O2x—K1—O2xiii66.61 (2)
O1iii—Al1—O1iv90.43 (5)O2xi—K1—O2xiii180.0
O1i—Al1—O1iv180.0O2xii—K1—O2xiii66.61 (2)
O1—Al1—O1iv89.57 (5)S—O3A—O4ii56.6 (2)
O1ii—Al1—O1iv89.57 (5)S—O3A—O456.6 (2)
O1iii—Al1—O1v90.43 (5)O4ii—O3A—O492.7 (3)
O1i—Al1—O1v89.57 (5)S—O3A—O4i56.6 (2)
O1—Al1—O1v180.0O4ii—O3A—O4i92.7 (3)
O1ii—Al1—O1v89.57 (5)O4—O3A—O4i92.7 (3)
O1iv—Al1—O1v90.43 (5)S—O3A—K1180.0 (7)
Al1—O1—H12122.2 (15)O4ii—O3A—K1123.4 (2)
Al1—O1—H11123.0 (16)O4—O3A—K1123.4 (2)
H12—O1—H11114 (2)O4i—O3A—K1123.4 (2)
K1vi—O2—H22118.2 (19)O4i—O4A—S69.6 (3)
K1vi—O2—H21117 (2)O4i—O4A—O3120.8 (3)
H22—O2—H21101 (3)S—O4A—O354.35 (18)
S—O3—O4Ai55.1 (2)
O3A—S—O3—O4Ai−150 (100)O4i—S—O3A—K1104 (100)
O4A—S—O3—O4Ai−120.0O4Aii—O4—O3A—S21.5 (3)
O4Aii—S—O3—O4Ai120.0O4Aii—O4—O3A—O4ii67.9 (3)
O4ii—S—O3—O4Ai−14.19 (18)S—O4—O3A—O4ii46.39 (18)
O4—S—O3—O4Ai105.81 (18)O4Aii—O4—O3A—O4i−24.9 (4)
O4i—S—O3—O4Ai−134.19 (18)S—O4—O3A—O4i−46.39 (18)
O3A—S—O3—O4Aii90 (100)O4Aii—O4—O3A—K1−158.5 (3)
O4Ai—S—O3—O4Aii−120.0S—O4—O3A—K1180.000 (1)
O4A—S—O3—O4Aii120.0O3Avii—K1—O3A—S0 (100)
O4ii—S—O3—O4Aii−134.19 (18)O2viii—K1—O3A—S93 (100)
O4—S—O3—O4Aii−14.19 (18)O2ix—K1—O3A—S−27 (100)
O4i—S—O3—O4Aii105.81 (18)O2x—K1—O3A—S−87 (100)
O3A—S—O3—O4A−30 (100)O2xi—K1—O3A—S33 (100)
O4Ai—S—O3—O4A120.0O2xii—K1—O3A—S153 (100)
O4Aii—S—O3—O4A−120.0O2xiii—K1—O3A—S−147 (100)
O4ii—S—O3—O4A105.81 (18)O3Avii—K1—O3A—O4ii74 (100)
O4—S—O3—O4A−134.19 (18)O2viii—K1—O3A—O4ii76.64 (8)
O4i—S—O3—O4A−14.19 (18)O2ix—K1—O3A—O4ii−43.36 (8)
O3A—S—O4—O4Aii−159.8 (3)O2x—K1—O3A—O4ii−103.36 (8)
O3—S—O4—O4Aii20.2 (3)O2xi—K1—O3A—O4ii16.64 (8)
O4Ai—S—O4—O4Aii96.4 (4)O2xii—K1—O3A—O4ii136.64 (8)
O4A—S—O4—O4Aii−62.6 (4)O2xiii—K1—O3A—O4ii−163.36 (8)
O4ii—S—O4—O4Aii141.1 (3)O3Avii—K1—O3A—O4−46 (100)
O4i—S—O4—O4Aii−100.7 (3)O2viii—K1—O3A—O4−43.36 (8)
O3—S—O4—O3A180.000 (1)O2ix—K1—O3A—O4−163.36 (8)
O4Ai—S—O4—O3A−103.8 (3)O2x—K1—O3A—O4136.64 (8)
O4A—S—O4—O3A97.2 (5)O2xi—K1—O3A—O4−103.36 (8)
O4Aii—S—O4—O3A159.8 (3)O2xii—K1—O3A—O416.64 (8)
O4ii—S—O4—O3A−59.10 (14)O2xiii—K1—O3A—O476.64 (8)
O4i—S—O4—O3A59.10 (14)O3Avii—K1—O3A—O4i−166 (100)
O3—S—O3A—O4ii136 (100)O2viii—K1—O3A—O4i−163.36 (8)
O4Ai—S—O3A—O4ii−14.19 (18)O2ix—K1—O3A—O4i76.64 (8)
O4A—S—O3A—O4ii105.81 (18)O2x—K1—O3A—O4i16.64 (8)
O4Aii—S—O3A—O4ii−134.19 (18)O2xi—K1—O3A—O4i136.64 (8)
O4—S—O3A—O4ii−120.0O2xii—K1—O3A—O4i−103.36 (8)
O4i—S—O3A—O4ii120.0O2xiii—K1—O3A—O4i−43.36 (8)
O3—S—O3A—O4−104 (100)O3A—S—O4A—O4i20.1 (3)
O4Ai—S—O3A—O4105.81 (18)O3—S—O4A—O4i−159.9 (3)
O4A—S—O3A—O4−134.19 (18)O4Ai—S—O4A—O4i140.0 (4)
O4Aii—S—O3A—O4−14.19 (18)O4Aii—S—O4A—O4i−99.8 (5)
O4ii—S—O3A—O4120.0O4ii—S—O4A—O4i95.2 (3)
O4i—S—O3A—O4−120.0O4—S—O4A—O4i−60.7 (5)
O3—S—O3A—O4i16 (100)O3A—S—O4A—O3180.0
O4Ai—S—O3A—O4i−134.19 (18)O4Ai—S—O4A—O3−60.1 (3)
O4A—S—O3A—O4i−14.19 (18)O4Aii—S—O4A—O360.1 (3)
O4Aii—S—O3A—O4i105.81 (18)O4ii—S—O4A—O3−104.94 (19)
O4ii—S—O3A—O4i−120.0O4—S—O4A—O399.2 (4)
O4—S—O3A—O4i120.0O4i—S—O4A—O3159.9 (3)
O3—S—O3A—K10 (100)S—O3—O4A—O4i22.0 (3)
O4Ai—S—O3A—K1−30 (100)O4Ai—O3—O4A—O4i67.3 (3)
O4A—S—O3A—K190 (100)O4Aii—O3—O4A—O4i−23.2 (4)
O4Aii—S—O3A—K1−150 (100)O4Ai—O3—O4A—S45.24 (15)
O4ii—S—O3A—K1−16 (100)O4Aii—O3—O4A—S−45.24 (15)
O4—S—O3A—K1−136 (100)
Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) −y, −z, −x; (iv) −z, −x, −y; (v) −x, −y, −z; (vi) y−1/2, −z+1/2, −x+1; (vii) −x+1, −y+1, −z+1; (viii) −x+1/2, y+1/2, z; (ix) y+1/2, z, −x+1/2; (x) x+1/2, −y+1/2, −z+1; (xi) −z+1, x+1/2, −y+1/2; (xii) −y+1/2, −z+1, x+1/2; (xiii) z, −x+1/2, y+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4xiv0.69 (2)1.92 (2)2.603 (2)169 (2)
O1—H12···O2i0.89 (3)1.74 (3)2.6257 (16)170 (2)
O2—H21···O30.77 (3)2.04 (3)2.781 (2)161 (3)
O2—H22···O4xv0.78 (3)1.98 (3)2.756 (2)171 (3)
O1—H11···O4Axvi0.69 (2)2.19 (2)2.844 (5)157 (2)
O2—H22···O4Axvii0.78 (3)2.15 (3)2.884 (5)158 (2)
O2—H21···O4A0.77 (3)2.40 (3)3.123 (6)155 (3)
O1—H11···O4Axviii0.69 (2)3.06 (2)3.169 (4)92.6 (19)
Symmetry codes: (i) z, x, y; (xiv) x, −y+1/2, z−1/2; (xv) y−1/2, z, −x+1/2; (xvi) y, −z+1/2, x−1/2; (xvii) z−1/2, x, −y+1/2; (xviii) −x+1/2, −y, z−1/2.
(or) top
Crystal data top
H24AlO20S2TlF(000) = 1240
Mr = 639.66Dx = 2.336 Mg m−3
Cubic, Pa3Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2ab 3µ = 9.25 mm−1
a = 12.2070 (5) ÅT = 173 K
V = 1818.98 (13) Å30.2 × 0.2 × 0.2 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.023
Graphite monochromatorθmax = 26.0°, θmin = 3.7°
1108 measured reflectionsh = −15→14
596 independent reflectionsk = −10→10
560 reflections with I > 2σ(I)l = −10→10
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.060Calculated w = 1/[σ2(Fo2) + (0.0132P)2 + 2.1175P]
where P = (Fo2 + 2Fc2)/3
S = 1.30(Δ/σ)max = 0.317
596 reflectionsΔρmax = 0.76 e Å−3
68 parametersΔρmin = −0.61 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0065 (5)
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
xyzUiso*/UeqOcc. (<1)
Tl10.50000.50000.50000.0314 (2)
S0.31104 (6)0.31104 (6)0.31104 (6)0.0135 (3)
Al10.00000.00000.00000.0101 (5)
O10.1526 (2)0.01481 (19)−0.0146 (2)0.0159 (5)
H120.194 (4)0.024 (3)0.042 (4)0.037 (12)*
H110.174 (4)0.034 (4)−0.068 (4)0.033 (12)*
O20.0469 (2)0.13812 (19)0.29852 (19)0.0220 (5)
H220.005 (3)0.183 (4)0.293 (4)0.041 (14)*
H210.115 (4)0.159 (3)0.296 (4)0.045 (13)*
O30.2420 (2)0.2420 (2)0.2420 (2)0.0328 (15)0.940 (7)
O40.2666 (2)0.42301 (19)0.31399 (19)0.0261 (8)0.940 (7)
O3A0.377 (3)0.377 (3)0.377 (3)0.05 (3)0.060 (7)
O4A0.282 (3)0.201 (2)0.368 (2)0.010 (10)0.060 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tl10.0314 (2)0.0314 (2)0.0314 (2)0.00870 (8)0.00870 (8)0.00870 (8)
S0.0135 (3)0.0135 (3)0.0135 (3)0.0025 (3)0.0025 (3)0.0025 (3)
Al10.0101 (5)0.0101 (5)0.0101 (5)−0.0001 (4)−0.0001 (4)−0.0001 (4)
O10.0121 (11)0.0213 (12)0.0142 (11)−0.0027 (9)0.0009 (9)0.0018 (8)
O20.0235 (13)0.0201 (11)0.0225 (11)0.0033 (10)−0.0039 (9)−0.0012 (9)
O30.0328 (15)0.0328 (15)0.0328 (15)−0.0061 (11)−0.0061 (11)−0.0061 (11)
O40.0372 (16)0.0198 (14)0.0213 (12)0.0164 (13)0.0112 (11)0.0057 (10)
O3A0.05 (3)0.05 (3)0.05 (3)−0.03 (2)−0.03 (2)−0.03 (2)
O4A0.019 (17)0.000 (16)0.010 (16)0.008 (12)0.010 (13)0.016 (13)
Geometric parameters (Å, º) top
Tl1—O3A2.61 (6)Al1—O1v1.880 (3)
Tl1—O3Ai2.61 (6)Al1—O1viii1.880 (3)
Tl1—O2ii3.036 (2)Al1—O11.880 (3)
Tl1—O2iii3.036 (2)O1—H120.86 (5)
S—O3A1.39 (6)O1—H110.74 (5)
S—O31.459 (5)O2—H220.75 (5)
S—O4iv1.471 (2)O2—H210.87 (5)
S—O41.471 (2)O3—O4A1.68 (3)
S—O4v1.471 (2)O3—O4Aiv1.68 (3)
S—O4A1.55 (3)O3—O4Av1.68 (3)
S—O4Aiv1.55 (2)O4—O4Av1.11 (4)
S—O4Av1.55 (3)O4—O3A1.65 (4)
Al1—O1vi1.880 (3)O3A—O4iv1.65 (4)
Al1—O1iv1.880 (3)O3A—O4v1.65 (4)
Al1—O1vii1.880 (3)O4A—O4iv1.11 (3)
O3A—Tl1—O3Ai180.000 (3)O1iv—Al1—O1v90.43 (10)
O3A—Tl1—O2ii104.83 (5)O1vii—Al1—O1v180.0
O3Ai—Tl1—O2ii75.17 (5)O1vi—Al1—O1viii90.43 (10)
O3A—Tl1—O2iii75.17 (5)O1iv—Al1—O1viii89.57 (10)
O3Ai—Tl1—O2iii104.83 (5)O1vii—Al1—O1viii90.43 (10)
O2ii—Tl1—O2iii66.31 (4)O1v—Al1—O1viii89.57 (10)
O3A—S—O3180 (4)O1vi—Al1—O189.57 (10)
O3A—S—O4iv70.28 (12)O1iv—Al1—O190.43 (10)
O3—S—O4iv109.72 (12)O1vii—Al1—O189.57 (10)
O3A—S—O470.28 (12)O1v—Al1—O190.43 (10)
O3—S—O4109.72 (12)O1viii—Al1—O1180.0
O4iv—S—O4109.22 (12)Al1—O1—H12122 (3)
O3A—S—O4v70.28 (12)Al1—O1—H11118 (3)
O3—S—O4v109.72 (12)H12—O1—H11117 (5)
O4iv—S—O4v109.22 (12)H22—O2—H21115 (4)
O4—S—O4v109.22 (12)S—O3—O4A58.4 (11)
O3A—S—O4A111.9 (13)S—O3—O4Aiv58.4 (11)
O3—S—O4A68.1 (13)O4A—O3—O4Aiv95.0 (15)
O4iv—S—O4A43.2 (13)S—O3—O4Av58.4 (11)
O4—S—O4A135.2 (10)O4A—O3—O4Av95.0 (15)
O4v—S—O4A113.4 (11)O4Aiv—O3—O4Av95.0 (15)
O3A—S—O4Aiv111.9 (13)O4Av—O4—S72.0 (12)
O3—S—O4Aiv68.1 (13)O4Av—O4—O3A122 (2)
O4iv—S—O4Aiv135.2 (10)S—O4—O3A52.5 (19)
O4—S—O4Aiv113.4 (11)S—O3A—O4iv57.2 (19)
O4v—S—O4Aiv43.2 (13)S—O3A—O4v57.2 (19)
O4A—S—O4Aiv107.0 (14)O4iv—O3A—O4v93 (3)
O3A—S—O4Av111.9 (13)S—O3A—O457.2 (19)
O3—S—O4Av68.1 (13)O4iv—O3A—O493 (3)
O4iv—S—O4Av113.4 (11)O4v—O3A—O493 (3)
O4—S—O4Av43.2 (13)S—O3A—Tl1180 (6)
O4v—S—O4Av135.2 (10)O4iv—O3A—Tl1122.8 (19)
O4A—S—O4Av107.0 (14)O4v—O3A—Tl1122.8 (19)
O4Aiv—S—O4Av107.0 (14)O4—O3A—Tl1122.8 (19)
O1vi—Al1—O1iv180.0O4iv—O4A—S64.9 (14)
O1vi—Al1—O1vii90.43 (10)O4iv—O4A—O3116.4 (18)
O1iv—Al1—O1vii89.57 (10)S—O4A—O353.5 (8)
O1vi—Al1—O1v89.57 (10)
O3A—S—O3—O4A91 (100)O4Aiv—S—O3A—O4108.1 (11)
O4iv—S—O3—O4A−11.9 (11)O4Av—S—O3A—O4−11.9 (11)
O4—S—O3—O4A−131.9 (11)O3—S—O3A—Tl1−179 (100)
O4v—S—O3—O4A108.1 (11)O4iv—S—O3A—Tl1−76 (100)
O4Aiv—S—O3—O4A120.000 (3)O4—S—O3A—Tl144 (52)
O4Av—S—O3—O4A−120.000 (3)O4v—S—O3A—Tl1164 (100)
O3A—S—O3—O4Aiv−29 (59)O4A—S—O3A—Tl1−88 (100)
O4iv—S—O3—O4Aiv−131.9 (11)O4Aiv—S—O3A—Tl1152 (100)
O4—S—O3—O4Aiv108.1 (11)O4Av—S—O3A—Tl132 (52)
O4v—S—O3—O4Aiv−11.9 (11)O4Av—O4—O3A—S18.4 (18)
O4A—S—O3—O4Aiv−120.0O4Av—O4—O3A—O4iv−28 (3)
O4Av—S—O3—O4Aiv120.0S—O4—O3A—O4iv−46.8 (15)
O3A—S—O3—O4Av−149 (100)O4Av—O4—O3A—O4v65 (2)
O4iv—S—O3—O4Av108.1 (11)S—O4—O3A—O4v46.8 (15)
O4—S—O3—O4Av−11.9 (11)O4Av—O4—O3A—Tl1−161.6 (18)
O4v—S—O3—O4Av−131.9 (11)S—O4—O3A—Tl1180.000 (8)
O4A—S—O3—O4Av120.000 (3)O3Ai—Tl1—O3A—S0 (100)
O4Aiv—S—O3—O4Av−120.000 (4)O2ii—Tl1—O3A—S92 (100)
O3A—S—O4—O4Av−163.7 (16)O2iii—Tl1—O3A—S152 (100)
O3—S—O4—O4Av16.3 (16)O3Ai—Tl1—O3A—O4iv163 (100)
O4iv—S—O4—O4Av−104.0 (16)O2ii—Tl1—O3A—O4iv15.77 (10)
O4v—S—O4—O4Av136.6 (16)O2iii—Tl1—O3A—O4iv75.77 (10)
O4A—S—O4—O4Av−62.1 (19)O3Ai—Tl1—O3A—O4v43 (100)
O4Aiv—S—O4—O4Av90 (2)O2ii—Tl1—O3A—O4v−104.23 (10)
O3—S—O4—O3A180.000 (9)O2iii—Tl1—O3A—O4v−44.23 (10)
O4iv—S—O4—O3A59.70 (15)O3Ai—Tl1—O3A—O4−77 (100)
O4v—S—O4—O3A−59.70 (15)O2ii—Tl1—O3A—O4135.77 (10)
O4A—S—O4—O3A101.6 (19)O2iii—Tl1—O3A—O4−164.23 (11)
O4Aiv—S—O4—O3A−106.0 (14)O3A—S—O4A—O4iv16.5 (15)
O4Av—S—O4—O3A163.7 (16)O3—S—O4A—O4iv−163.5 (15)
O3—S—O3A—O4iv−103 (100)O4—S—O4A—O4iv−67 (2)
O4—S—O3A—O4iv120.0O4v—S—O4A—O4iv93.7 (12)
O4v—S—O3A—O4iv−120.000 (3)O4Aiv—S—O4A—O4iv139.4 (19)
O4A—S—O3A—O4iv−11.9 (11)O4Av—S—O4A—O4iv−106 (2)
O4Aiv—S—O3A—O4iv−131.9 (11)O3A—S—O4A—O3180.000 (3)
O4Av—S—O3A—O4iv108.1 (11)O4iv—S—O4A—O3163.5 (15)
O3—S—O3A—O4v17 (41)O4—S—O4A—O396.4 (14)
O4iv—S—O3A—O4v120.000 (3)O4v—S—O4A—O3−102.9 (7)
O4—S—O3A—O4v−120.000 (2)O4Aiv—S—O4A—O3−57.2 (15)
O4A—S—O3A—O4v108.1 (11)O4Av—S—O4A—O357.2 (15)
O4Aiv—S—O3A—O4v−11.9 (11)S—O3—O4A—O4iv16.7 (16)
O4Av—S—O3A—O4v−131.9 (11)O4Aiv—O3—O4A—O4iv64.5 (14)
O3—S—O3A—O4137 (100)O4Av—O3—O4A—O4iv−31 (2)
O4iv—S—O3A—O4−120.000 (3)O4Aiv—O3—O4A—S47.7 (9)
O4v—S—O3A—O4120.000 (4)O4Av—O3—O4A—S−47.7 (9)
O4A—S—O3A—O4−131.9 (11)
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1/2, −y+1/2, −z+1; (iii) y+1/2, z, −x+1/2; (iv) z, x, y; (v) y, z, x; (vi) −z, −x, −y; (vii) −y, −z, −x; (viii) −x, −y, −z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4ix0.74 (5)1.90 (5)2.625 (3)165 (5)
O1—H12···O2iv0.86 (5)1.76 (5)2.608 (3)169 (5)
O2—H21···O30.87 (5)1.97 (5)2.786 (4)157 (4)
O2—H22···O4x0.75 (5)2.03 (5)2.743 (3)161 (5)
O1—H11···O4Axi0.74 (5)2.21 (6)2.93 (3)162 (5)
O2—H22···O4Axii0.75 (5)2.08 (6)2.81 (3)167 (5)
O2—H21···O4A0.87 (5)2.29 (7)3.09 (3)155 (4)
Symmetry codes: (iv) z, x, y; (ix) x, −y+1/2, z−1/2; (x) y−1/2, z, −x+1/2; (xi) y, −z+1/2, x−1/2; (xii) z−1/2, x, −y+1/2.
(ol) top
Crystal data top
H24AlO20S2TlF(000) = 1240
Mr = 639.66Dx = 2.322 Mg m−3
Cubic, Pa3Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2ab 3µ = 9.20 mm−1
a = 12.2305 (5) ÅT = 296 K
V = 1829.50 (13) Å30.2 × 0.2 × 0.2 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.026
Graphite monochromatorθmax = 26.0°, θmin = 3.7°
1115 measured reflectionsh = −15→15
599 independent reflectionsk = −10→10
513 reflections with I > 2σ(I)l = −10→10
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.069Calculated w = 1/[σ2(Fo2) + (0.0369P)2 + 0.9092P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
599 reflectionsΔρmax = 0.46 e Å−3
62 parametersΔρmin = −0.62 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0330 (14)
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
xyzUiso*/UeqOcc. (<1)
Tl10.50000.50000.50000.0519 (3)
S0.31138 (5)0.31138 (5)0.31138 (5)0.0259 (3)
Al10.00000.00000.00000.0196 (5)
O10.1521 (2)0.01508 (19)−0.0144 (2)0.0284 (5)
H120.192 (4)0.018 (3)0.038 (4)0.040 (11)*
H110.176 (3)0.028 (3)−0.066 (3)0.037 (11)*
O20.04606 (18)0.13994 (17)0.29729 (16)0.0405 (6)
H220.00440.19190.29580.12 (3)*
H210.11400.17320.29300.104 (18)*
O30.2434 (2)0.2434 (2)0.2434 (2)0.065 (3)0.843 (13)
O40.2676 (4)0.4232 (3)0.3157 (2)0.0465 (13)0.843 (13)
O3A0.3779 (14)0.3779 (14)0.3779 (14)0.13 (2)0.157 (13)
O4A0.2918 (18)0.2065 (19)0.368 (2)0.064 (10)0.157 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tl10.0519 (3)0.0519 (3)0.0519 (3)0.00830 (8)0.00830 (8)0.00830 (8)
S0.0259 (3)0.0259 (3)0.0259 (3)0.0037 (3)0.0037 (3)0.0037 (3)
Al10.0196 (5)0.0196 (5)0.0196 (5)−0.0002 (3)−0.0002 (3)−0.0002 (3)
O10.0226 (11)0.0355 (12)0.0271 (12)−0.0034 (8)0.0007 (9)0.0021 (8)
O20.0457 (12)0.0351 (11)0.0408 (12)0.0025 (10)−0.0076 (10)−0.0060 (9)
O30.065 (3)0.065 (3)0.065 (3)−0.0166 (15)−0.0166 (15)−0.0166 (15)
O40.064 (3)0.0342 (18)0.0417 (15)0.0240 (18)0.0205 (15)0.0103 (12)
O3A0.13 (2)0.13 (2)0.13 (2)−0.052 (13)−0.052 (13)−0.052 (13)
O4A0.067 (13)0.044 (12)0.082 (18)0.026 (10)0.052 (12)0.040 (13)
Geometric parameters (Å, º) top
Tl1—O3Ai2.59 (3)Al1—O1vii1.877 (3)
Tl1—O3A2.59 (3)Al1—O1viii1.877 (3)
Tl1—O2ii3.065 (2)Al1—O1iv1.877 (3)
Tl1—O2iii3.065 (2)O1—H120.81 (5)
S—O3A1.41 (3)O1—H110.72 (4)
S—O31.439 (5)O2—H220.8146
S—O4iv1.470 (2)O2—H210.9271
S—O41.470 (2)O3—O4Av1.70 (3)
S—O4v1.470 (2)O3—O4A1.70 (3)
S—O4A1.480 (14)O3—O4Aiv1.70 (3)
S—O4Av1.480 (14)O4—O4Av1.04 (3)
S—O4Aiv1.480 (14)O4—O3A1.645 (17)
Al1—O1v1.877 (3)O3A—O4iv1.645 (17)
Al1—O11.877 (3)O3A—O4v1.645 (17)
Al1—O1vi1.877 (3)O4A—O4iv1.04 (3)
O3Ai—Tl1—O3A180.000 (1)O1—Al1—O1vii180.0
O3Ai—Tl1—O2ii75.48 (4)O1vi—Al1—O1vii90.30 (10)
O3A—Tl1—O2ii104.52 (4)O1v—Al1—O1viii180.0
O3Ai—Tl1—O2iii104.52 (4)O1—Al1—O1viii89.70 (10)
O3A—Tl1—O2iii75.48 (4)O1vi—Al1—O1viii90.30 (10)
O2ii—Tl1—O2iii66.07 (3)O1vii—Al1—O1viii90.30 (10)
O3A—S—O3180.0 (17)O1v—Al1—O1iv90.30 (10)
O3A—S—O4iv69.66 (19)O1—Al1—O1iv90.30 (10)
O3—S—O4iv110.3 (2)O1vi—Al1—O1iv180.0
O3A—S—O469.66 (19)O1vii—Al1—O1iv89.70 (10)
O3—S—O4110.3 (2)O1viii—Al1—O1iv89.70 (10)
O4iv—S—O4108.6 (2)Al1—O1—H12122 (3)
O3A—S—O4v69.7 (2)Al1—O1—H11121 (3)
O3—S—O4v110.34 (19)H12—O1—H11116 (5)
O4iv—S—O4v108.6 (2)H22—O2—H21102.6
O4—S—O4v108.6 (2)S—O3—O4Av55.5 (10)
O3A—S—O4A108.7 (15)S—O3—O4A55.5 (10)
O3—S—O4A71.3 (15)O4Av—O3—O4A91.0 (14)
O4iv—S—O4A41.5 (13)S—O3—O4Aiv55.5 (10)
O4—S—O4A136.9 (7)O4Av—O3—O4Aiv91.0 (14)
O4v—S—O4A110.7 (6)O4A—O3—O4Aiv91.0 (14)
O3A—S—O4Av108.7 (15)O4Av—O4—S69.8 (8)
O3—S—O4Av71.3 (15)O4Av—O4—O3A120.0 (11)
O4iv—S—O4Av110.7 (6)S—O4—O3A53.4 (9)
O4—S—O4Av41.5 (13)S—O3A—O4iv56.9 (9)
O4v—S—O4Av136.9 (7)S—O3A—O456.9 (9)
O4A—S—O4Av110.2 (15)O4iv—O3A—O493.0 (12)
O3A—S—O4Aiv108.7 (15)S—O3A—O4v56.9 (9)
O3—S—O4Aiv71.3 (15)O4iv—O3A—O4v93.0 (12)
O4iv—S—O4Aiv136.9 (7)O4—O3A—O4v93.0 (12)
O4—S—O4Aiv110.7 (6)S—O3A—Tl1180 (3)
O4v—S—O4Aiv41.5 (13)O4iv—O3A—Tl1123.1 (9)
O4A—S—O4Aiv110.2 (15)O4—O3A—Tl1123.1 (9)
O4Av—S—O4Aiv110.2 (15)O4v—O3A—Tl1123.1 (9)
O1v—Al1—O190.30 (10)O4iv—O4A—S68.8 (12)
O1v—Al1—O1vi89.70 (10)O4iv—O4A—O3118.9 (11)
O1—Al1—O1vi89.70 (10)S—O4A—O353.3 (7)
O1v—Al1—O1vii89.70 (10)
O3A—S—O3—O4Av27 (100)O4Av—S—O3A—O4v−134.2 (6)
O4iv—S—O3—O4Av105.8 (6)O4Aiv—S—O3A—O4v−14.2 (6)
O4—S—O3—O4Av−14.2 (6)O3—S—O3A—Tl10 (100)
O4v—S—O3—O4Av−134.2 (6)O4iv—S—O3A—Tl185 (100)
O4A—S—O3—O4Av120.000 (4)O4—S—O3A—Tl1−155 (100)
O4Aiv—S—O3—O4Av−120.000 (3)O4v—S—O3A—Tl1−35 (100)
O3A—S—O3—O4A−93 (100)O4A—S—O3A—Tl170 (100)
O4iv—S—O3—O4A−14.2 (6)O4Av—S—O3A—Tl1−170 (100)
O4—S—O3—O4A−134.2 (6)O4Aiv—S—O3A—Tl1−50 (100)
O4v—S—O3—O4A105.8 (6)O4Av—O4—O3A—S22.3 (12)
O4Av—S—O3—O4A−120.000 (3)O4Av—O4—O3A—O4iv−24.3 (14)
O4Aiv—S—O3—O4A120.000 (3)S—O4—O3A—O4iv−46.6 (7)
O3A—S—O3—O4Aiv147 (100)O4Av—O4—O3A—O4v68.9 (13)
O4iv—S—O3—O4Aiv−134.2 (6)S—O4—O3A—O4v46.6 (7)
O4—S—O3—O4Aiv105.8 (6)O4Av—O4—O3A—Tl1−157.7 (12)
O4v—S—O3—O4Aiv−14.2 (6)S—O4—O3A—Tl1180.000 (4)
O4A—S—O3—O4Aiv−120.0O3Ai—Tl1—O3A—S0 (100)
O4Av—S—O3—O4Aiv120.0O2ii—Tl1—O3A—S−69 (100)
O3A—S—O4—O4Av−159.5 (10)O2iii—Tl1—O3A—S−9 (100)
O3—S—O4—O4Av20.5 (10)O3Ai—Tl1—O3A—O4iv171 (80)
O4iv—S—O4—O4Av−100.5 (10)O2ii—Tl1—O3A—O4iv15.25 (15)
O4v—S—O4—O4Av141.6 (11)O2iii—Tl1—O3A—O4iv75.25 (15)
O4A—S—O4—O4Av−63.5 (19)O3Ai—Tl1—O3A—O4−69 (80)
O4Aiv—S—O4—O4Av97 (2)O2ii—Tl1—O3A—O4135.25 (15)
O3—S—O4—O3A180.000 (4)O2iii—Tl1—O3A—O4−164.75 (15)
O4iv—S—O4—O3A58.9 (2)O3Ai—Tl1—O3A—O4v51 (80)
O4v—S—O4—O3A−58.9 (2)O2ii—Tl1—O3A—O4v−104.75 (15)
O4A—S—O4—O3A96 (2)O2iii—Tl1—O3A—O4v−44.75 (15)
O4Av—S—O4—O3A159.5 (10)O3A—S—O4A—O4iv20.3 (9)
O4Aiv—S—O4—O3A−103.1 (16)O3—S—O4A—O4iv−159.7 (9)
O3—S—O3A—O4iv79 (100)O4—S—O4A—O4iv−60 (2)
O4—S—O3A—O4iv120.0O4v—S—O4A—O4iv95.0 (8)
O4v—S—O3A—O4iv−120.000 (2)O4Av—S—O4A—O4iv−99 (2)
O4A—S—O3A—O4iv−14.2 (6)O4Aiv—S—O4A—O4iv139.4 (17)
O4Av—S—O3A—O4iv105.8 (6)O3A—S—O4A—O3180.000 (3)
O4Aiv—S—O3A—O4iv−134.2 (6)O4iv—S—O4A—O3159.7 (9)
O3—S—O3A—O4−41 (100)O4—S—O4A—O3100.1 (18)
O4iv—S—O3A—O4−120.000 (1)O4v—S—O4A—O3−105.3 (7)
O4v—S—O3A—O4120.000 (2)O4Av—S—O4A—O360.9 (19)
O4A—S—O3A—O4−134.2 (6)O4Aiv—S—O4A—O3−60.9 (19)
O4Av—S—O3A—O4−14.2 (6)S—O3—O4A—O4iv21.7 (11)
O4Aiv—S—O3A—O4105.8 (6)O4Av—O3—O4A—O4iv−23.9 (16)
O3—S—O3A—O4v−161 (100)O4Aiv—O3—O4A—O4iv67.2 (9)
O4iv—S—O3A—O4v120.000 (1)O4Av—O3—O4A—S−45.5 (7)
O4—S—O3A—O4v−120.000 (1)O4Aiv—O3—O4A—S45.5 (7)
O4A—S—O3A—O4v105.8 (6)
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1/2, −y+1/2, −z+1; (iii) y+1/2, z, −x+1/2; (iv) z, x, y; (v) y, z, x; (vi) −z, −x, −y; (vii) −x, −y, −z; (viii) −y, −z, −x.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4ix0.72 (4)1.92 (4)2.623 (4)167 (4)
O1—H12···O2iv0.81 (5)1.82 (5)2.620 (3)168 (4)
O2—H21···O30.931.902.804 (4)165
O2—H22···O4x0.811.972.740 (3)158
O1—H11···O4Axi0.72 (4)2.18 (5)2.84 (3)155 (4)
O2—H22···O4Axii0.812.062.858 (17)165
O2—H21···O4A0.932.403.23 (3)150
Symmetry codes: (iv) z, x, y; (ix) x, −y+1/2, z−1/2; (x) y−1/2, z, −x+1/2; (xi) y, −z+1/2, x−1/2; (xii) z−1/2, x, −y+1/2.
(ov) top
Crystal data top
H24CrKO20S2F(000) = 1036
Mr = 499.41Dx = 1.821 Mg m−3
Cubic, Pa3Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2ab 3µ = 1.18 mm−1
a = 12.2133 (5) ÅT = 173 K
V = 1821.79 (13) Å30.8 × 0.8 × 0.8 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.010
Graphite monochromatorθmax = 26.0°, θmin = 3.7°
1112 measured reflectionsh = −15→15
597 independent reflectionsk = −10→10
591 reflections with I > 2σ(I)l = −10→10
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.044H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.133Calculated w = 1/[σ2(Fo2) + (0.0922P)2 + 1.5879P]
where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max < 0.001
597 reflectionsΔρmax = 1.25 e Å−3
68 parametersΔρmin = −1.90 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.015 (5)
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
xyzUiso*/UeqOcc. (<1)
Cr10.00000.00000.00000.0111 (5)
K0.50000.50000.50000.0562 (8)
S0.30918 (5)0.30918 (5)0.30918 (5)0.0150 (5)
O10.15926 (16)0.01347 (15)−0.0155 (2)0.0189 (5)
H120.200 (3)0.017 (2)0.042 (3)0.016 (7)*
H110.181 (3)0.026 (2)−0.062 (3)0.012 (8)*
O20.0473 (2)0.13690 (18)0.30445 (16)0.0255 (6)
H220.006 (4)0.178 (4)0.287 (4)0.046 (13)*
H210.087 (3)0.160 (3)0.292 (3)0.016 (10)*
O30.2403 (2)0.2403 (2)0.2403 (2)0.0400 (14)0.913 (7)
O40.2660 (2)0.42175 (18)0.31071 (17)0.0303 (9)0.913 (7)
O3A0.3782 (13)0.3782 (13)0.3782 (13)0.032 (10)0.087 (7)
O4A0.2856 (15)0.2030 (13)0.3612 (15)0.014 (7)0.087 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0111 (5)0.0111 (5)0.0111 (5)−0.00047 (15)−0.00047 (15)−0.00047 (15)
K0.0562 (8)0.0562 (8)0.0562 (8)0.0097 (6)0.0097 (6)0.0097 (6)
S0.0150 (5)0.0150 (5)0.0150 (5)0.00256 (19)0.00256 (19)0.00256 (19)
O10.0135 (9)0.0256 (10)0.0177 (11)−0.0036 (7)0.0018 (8)0.0019 (7)
O20.0247 (13)0.0248 (11)0.0270 (11)0.0001 (10)−0.0038 (9)−0.0031 (7)
O30.0400 (14)0.0400 (14)0.0400 (14)−0.0060 (10)−0.0060 (10)−0.0060 (10)
O40.0398 (16)0.0238 (14)0.0271 (12)0.0150 (11)0.0118 (9)0.0076 (8)
O3A0.032 (10)0.032 (10)0.032 (10)−0.022 (7)−0.022 (7)−0.022 (7)
O4A0.015 (9)0.003 (9)0.023 (12)0.010 (6)0.024 (8)0.023 (8)
Geometric parameters (Å, º) top
Cr1—O11.961 (2)S—O41.472 (2)
Cr1—O1i1.961 (2)S—O4Ai1.472 (13)
Cr1—O1ii1.961 (2)S—O4A1.472 (13)
Cr1—O1iii1.961 (2)S—O4Aii1.472 (13)
Cr1—O1iv1.961 (2)O1—H120.87 (4)
Cr1—O1v1.961 (2)O1—H110.65 (4)
K—O3Avi2.58 (3)O2—Kxiii2.972 (2)
K—O3A2.58 (3)O2—H220.74 (6)
K—O2vii2.972 (2)O2—H210.59 (4)
K—O2viii2.972 (2)O3—O4Ai1.642 (18)
K—O2ix2.972 (2)O3—O4A1.642 (18)
K—O2x2.972 (2)O3—O4Aii1.642 (18)
K—O2xi2.972 (2)O4—O4Aii1.11 (2)
K—O2xii2.972 (2)O4—O3A1.685 (16)
S—O31.458 (5)O3A—O4i1.685 (16)
S—O3A1.46 (3)O3A—O4ii1.685 (16)
S—O4i1.472 (2)O4A—O4i1.11 (2)
S—O4ii1.472 (2)
O1—Cr1—O1i91.17 (9)O3A—S—O470.13 (11)
O1—Cr1—O1ii91.17 (9)O4i—S—O4109.07 (11)
O1i—Cr1—O1ii91.17 (9)O4ii—S—O4109.07 (11)
O1—Cr1—O1iii88.83 (9)O3—S—O4Ai68.1 (9)
O1i—Cr1—O1iii180.0O3A—S—O4Ai111.9 (9)
O1ii—Cr1—O1iii88.83 (9)O4i—S—O4Ai138.3 (6)
O1—Cr1—O1iv88.83 (9)O4ii—S—O4Ai44.3 (8)
O1i—Cr1—O1iv88.83 (9)O4—S—O4Ai110.4 (6)
O1ii—Cr1—O1iv180.0O3—S—O4A68.1 (9)
O1iii—Cr1—O1iv91.17 (9)O3A—S—O4A111.9 (9)
O1—Cr1—O1v180.0O4i—S—O4A44.3 (8)
O1i—Cr1—O1v88.83 (9)O4ii—S—O4A110.4 (6)
O1ii—Cr1—O1v88.83 (9)O4—S—O4A138.3 (6)
O1iii—Cr1—O1v91.17 (9)O4Ai—S—O4A107.0 (9)
O1iv—Cr1—O1v91.17 (9)O3—S—O4Aii68.1 (9)
O3Avi—K—O3A180.000 (1)O3A—S—O4Aii111.9 (9)
O3Avi—K—O2vii104.56 (4)O4i—S—O4Aii110.4 (6)
O3A—K—O2vii75.44 (4)O4ii—S—O4Aii138.3 (6)
O3Avi—K—O2viii75.44 (4)O4—S—O4Aii44.3 (8)
O3A—K—O2viii104.56 (4)O4Ai—S—O4Aii107.0 (9)
O2vii—K—O2viii66.10 (3)O4A—S—O4Aii107.0 (10)
O3Avi—K—O2ix75.44 (4)Cr1—O1—H12120 (2)
O3A—K—O2ix104.56 (4)Cr1—O1—H11121 (3)
O2vii—K—O2ix66.10 (3)H12—O1—H11118 (4)
O2viii—K—O2ix113.90 (4)Kxiii—O2—H22118 (4)
O3Avi—K—O2x104.56 (4)Kxiii—O2—H21131 (4)
O3A—K—O2x75.44 (4)H22—O2—H2199 (5)
O2vii—K—O2x113.90 (3)S—O3—O4Ai56.4 (7)
O2viii—K—O2x66.10 (3)S—O3—O4A56.4 (7)
O2ix—K—O2x180.0O4Ai—O3—O4A92.3 (9)
O3Avi—K—O2xi104.56 (4)S—O3—O4Aii56.4 (7)
O3A—K—O2xi75.44 (4)O4Ai—O3—O4Aii92.3 (9)
O2vii—K—O2xi113.90 (4)O4A—O3—O4Aii92.3 (9)
O2viii—K—O2xi180.0O4Aii—O4—S67.8 (7)
O2ix—K—O2xi66.10 (3)O4Aii—O4—O3A119.3 (10)
O2x—K—O2xi113.90 (4)S—O4—O3A54.6 (8)
O3Avi—K—O2xii75.44 (4)S—O3A—O4i55.3 (8)
O3A—K—O2xii104.56 (4)S—O3A—O4ii55.3 (8)
O2vii—K—O2xii180.0O4i—O3A—O4ii90.7 (11)
O2viii—K—O2xii113.90 (3)S—O3A—O455.3 (8)
O2ix—K—O2xii113.90 (3)O4i—O3A—O490.7 (11)
O2x—K—O2xii66.10 (3)O4ii—O3A—O490.7 (11)
O2xi—K—O2xii66.10 (3)S—O3A—K180 (2)
O3—S—O3A180.0 (15)O4i—O3A—K124.7 (8)
O3—S—O4i109.87 (11)O4ii—O3A—K124.7 (8)
O3A—S—O4i70.13 (11)O4—O3A—K124.7 (8)
O3—S—O4ii109.87 (11)O4i—O4A—S67.8 (9)
O3A—S—O4ii70.13 (11)O4i—O4A—O3120.0 (10)
O4i—S—O4ii109.07 (11)S—O4A—O355.5 (5)
O3—S—O4109.87 (11)
O3A—S—O3—O4Ai179 (100)O4Aii—S—O3A—K96 (100)
O4i—S—O3—O4Ai−135.3 (7)O4Aii—O4—O3A—S21.8 (10)
O4ii—S—O3—O4Ai−15.3 (7)O4Aii—O4—O3A—O4i−23.6 (12)
O4—S—O3—O4Ai104.7 (7)S—O4—O3A—O4i−45.4 (6)
O4A—S—O3—O4Ai−120.0O4Aii—O4—O3A—O4ii67.2 (11)
O4Aii—S—O3—O4Ai120.0S—O4—O3A—O4ii45.4 (5)
O3A—S—O3—O4A−61 (100)O4Aii—O4—O3A—K−158.2 (10)
O4i—S—O3—O4A−15.3 (7)S—O4—O3A—K180.000 (4)
O4ii—S—O3—O4A104.7 (7)O3Avi—K—O3A—S0 (100)
O4—S—O3—O4A−135.3 (7)O2vii—K—O3A—S86 (100)
O4Ai—S—O3—O4A120.000 (2)O2viii—K—O3A—S146 (100)
O4Aii—S—O3—O4A−120.000 (2)O2ix—K—O3A—S26 (100)
O3A—S—O3—O4Aii59 (100)O2x—K—O3A—S−154 (100)
O4i—S—O3—O4Aii104.7 (7)O2xi—K—O3A—S−34 (100)
O4ii—S—O3—O4Aii−135.3 (7)O2xii—K—O3A—S−94 (100)
O4—S—O3—O4Aii−15.3 (7)O3Avi—K—O3A—O4i−106 (100)
O4Ai—S—O3—O4Aii−120.000 (2)O2vii—K—O3A—O4i77.40 (10)
O4A—S—O3—O4Aii120.000 (2)O2viii—K—O3A—O4i137.40 (10)
O3—S—O4—O4Aii20.5 (9)O2ix—K—O3A—O4i17.40 (10)
O3A—S—O4—O4Aii−159.5 (9)O2x—K—O3A—O4i−162.60 (10)
O4i—S—O4—O4Aii−100.0 (10)O2xi—K—O3A—O4i−42.60 (10)
O4ii—S—O4—O4Aii141.0 (9)O2xii—K—O3A—O4i−102.60 (10)
O4Ai—S—O4—O4Aii93.7 (15)O3Avi—K—O3A—O4ii134 (100)
O4A—S—O4—O4Aii−58.6 (11)O2vii—K—O3A—O4ii−42.60 (10)
O3—S—O4—O3A180.000 (4)O2viii—K—O3A—O4ii17.40 (10)
O4i—S—O4—O3A59.51 (13)O2ix—K—O3A—O4ii−102.60 (10)
O4ii—S—O4—O3A−59.51 (13)O2x—K—O3A—O4ii77.40 (10)
O4Ai—S—O4—O3A−106.7 (9)O2xi—K—O3A—O4ii−162.60 (10)
O4A—S—O4—O3A100.9 (13)O2xii—K—O3A—O4ii137.40 (10)
O4Aii—S—O4—O3A159.5 (9)O3Avi—K—O3A—O414 (100)
O3—S—O3A—O4i46 (100)O2vii—K—O3A—O4−162.60 (10)
O4ii—S—O3A—O4i−120.000 (1)O2viii—K—O3A—O4−102.60 (10)
O4—S—O3A—O4i120.0O2ix—K—O3A—O4137.40 (10)
O4Ai—S—O3A—O4i−135.3 (7)O2x—K—O3A—O4−42.60 (10)
O4A—S—O3A—O4i−15.3 (7)O2xi—K—O3A—O477.40 (10)
O4Aii—S—O3A—O4i104.7 (7)O2xii—K—O3A—O417.40 (10)
O3—S—O3A—O4ii166 (100)O3—S—O4A—O4i−159.2 (9)
O4i—S—O3A—O4ii120.000 (1)O3A—S—O4A—O4i20.8 (9)
O4—S—O3A—O4ii−120.0O4ii—S—O4A—O4i96.8 (7)
O4Ai—S—O3A—O4ii−15.3 (7)O4—S—O4A—O4i−63.5 (15)
O4A—S—O3A—O4ii104.7 (7)O4Ai—S—O4A—O4i143.6 (11)
O4Aii—S—O3A—O4ii−135.3 (7)O4Aii—S—O4A—O4i−102.1 (16)
O3—S—O3A—O4−74 (100)O3A—S—O4A—O3180.000 (2)
O4i—S—O3A—O4−120.000 (1)O4i—S—O4A—O3159.2 (9)
O4ii—S—O3A—O4120.000 (2)O4ii—S—O4A—O3−104.0 (4)
O4Ai—S—O3A—O4104.7 (7)O4—S—O4A—O395.7 (10)
O4A—S—O3A—O4−135.3 (7)O4Ai—S—O4A—O3−57.2 (10)
O4Aii—S—O3A—O4−15.3 (7)O4Aii—S—O4A—O357.2 (10)
O3—S—O3A—K0 (100)S—O3—O4A—O4i22.3 (10)
O4i—S—O3A—K−9 (100)O4Ai—O3—O4A—O4i68.5 (8)
O4ii—S—O3A—K−129 (100)O4Aii—O3—O4A—O4i−23.9 (13)
O4—S—O3A—K111 (100)O4Ai—O3—O4A—S46.2 (5)
O4Ai—S—O3A—K−144 (100)O4Aii—O3—O4A—S−46.2 (5)
O4A—S—O3A—K−24 (100)
Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) −z, −x, −y; (iv) −y, −z, −x; (v) −x, −y, −z; (vi) −x+1, −y+1, −z+1; (vii) y+1/2, z, −x+1/2; (viii) −z+1, x+1/2, −y+1/2; (ix) x+1/2, −y+1/2, −z+1; (x) −x+1/2, y+1/2, z; (xi) z, −x+1/2, y+1/2; (xii) −y+1/2, −z+1, x+1/2; (xiii) y−1/2, −z+1/2, −x+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4xiv0.65 (4)1.97 (4)2.614 (3)170 (4)
O1—H12···O2i0.87 (4)1.76 (4)2.603 (3)164 (3)
O2—H21···O30.59 (4)2.20 (4)2.786 (4)177 (5)
O2—H22···O4xv0.74 (6)2.03 (6)2.757 (3)168 (5)
O1—H11···O4Axvi0.65 (4)2.33 (4)2.92 (2)153 (3)
O2—H22···O4Axvii0.74 (6)2.21 (6)2.910 (15)159 (5)
O2—H21···O4A0.59 (4)2.62 (4)3.10 (2)141 (4)
Symmetry codes: (i) z, x, y; (xiv) x, −y+1/2, z−1/2; (xv) y−1/2, z, −x+1/2; (xvi) y, −z+1/2, x−1/2; (xvii) z−1/2, x, −y+1/2.
(os) top
Crystal data top
H24CrKO20S2F(000) = 1036
Mr = 499.41Dx = 1.813 Mg m−3
Cubic, Pa3Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2ab 3µ = 1.17 mm−1
a = 12.2305 (5) ÅT = 296 K
V = 1829.50 (13) Å30.8 × 0.8 × 0.8 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.014
Graphite monochromatorθmax = 26.0°, θmin = 3.7°
1114 measured reflectionsh = −15→15
597 independent reflectionsk = −10→10
574 reflections with I > 2σ(I)l = −10→10
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.046H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.135Calculated w = 1/[σ2(Fo2) + (0.0961P)2 + 1.0171P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.002
597 reflectionsΔρmax = 1.06 e Å−3
68 parametersΔρmin = −1.53 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.021 (6)
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
xyzUiso*/UeqOcc. (<1)
Cr10.00000.00000.00000.0194 (5)
K10.50000.50000.50000.0767 (10)
S0.31011 (5)0.31011 (5)0.31011 (5)0.0267 (5)
O10.15869 (17)0.01364 (17)−0.0145 (2)0.0310 (6)
H120.200 (3)0.022 (3)0.040 (3)0.038 (9)*
H110.178 (3)0.030 (2)−0.056 (3)0.020 (9)*
O20.0470 (2)0.13945 (18)0.30272 (16)0.0430 (7)
H220.014 (7)0.193 (7)0.312 (6)0.12 (3)*
H210.105 (6)0.164 (5)0.301 (5)0.091 (18)*
O30.2420 (3)0.2420 (3)0.2420 (3)0.066 (3)0.766 (15)
O40.2682 (5)0.4227 (3)0.3128 (2)0.0484 (15)0.766 (15)
O3A0.3751 (10)0.3751 (10)0.3751 (10)0.136 (15)0.234 (15)
O4A0.2921 (13)0.2100 (15)0.3690 (19)0.072 (8)0.234 (15)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0194 (5)0.0194 (5)0.0194 (5)−0.00070 (15)−0.00070 (15)−0.00070 (15)
K10.0767 (10)0.0767 (10)0.0767 (10)0.0088 (6)0.0088 (6)0.0088 (6)
S0.0267 (5)0.0267 (5)0.0267 (5)0.0035 (2)0.0035 (2)0.0035 (2)
O10.0223 (10)0.0415 (12)0.0293 (12)−0.0049 (7)0.0017 (8)0.0019 (8)
O20.0456 (14)0.0402 (12)0.0433 (12)0.0019 (9)−0.0060 (9)−0.0064 (8)
O30.066 (3)0.066 (3)0.066 (3)−0.0151 (15)−0.0151 (15)−0.0151 (15)
O40.067 (3)0.0356 (18)0.0422 (17)0.0213 (19)0.0214 (15)0.0106 (11)
O3A0.136 (15)0.136 (15)0.136 (15)−0.057 (9)−0.057 (9)−0.057 (9)
O4A0.071 (8)0.049 (9)0.096 (16)0.030 (7)0.048 (9)0.054 (10)
Geometric parameters (Å, º) top
Cr1—O11.956 (2)S—O4Aii1.437 (10)
Cr1—O1i1.956 (2)S—O4ii1.470 (3)
Cr1—O1ii1.956 (2)S—O4i1.470 (3)
Cr1—O1iii1.956 (2)S—O41.470 (3)
Cr1—O1iv1.956 (2)O1—H120.85 (4)
Cr1—O1v1.956 (2)O1—H110.60 (4)
K1—O3A2.65 (2)O2—K1xiii3.010 (2)
K1—O3Avi2.65 (2)O2—H220.78 (8)
K1—O2vii3.010 (2)O2—H210.77 (8)
K1—O2viii3.010 (2)O3—O4A1.71 (2)
K1—O2ix3.010 (2)O3—O4Aii1.71 (2)
K1—O2x3.010 (2)O3—O4Ai1.71 (2)
K1—O2xi3.010 (2)O4—O4Aii1.00 (3)
K1—O2xii3.010 (2)O4—O3A1.621 (12)
S—O3A1.38 (2)O3A—O4i1.621 (12)
S—O31.442 (6)O3A—O4ii1.621 (12)
S—O4A1.437 (10)O4A—O4i1.00 (3)
S—O4Ai1.437 (9)
O1—Cr1—O1i90.76 (9)O3—S—O4Aii73.1 (12)
O1—Cr1—O1ii90.76 (9)O4A—S—O4Aii111.9 (11)
O1i—Cr1—O1ii90.76 (9)O4Ai—S—O4Aii111.9 (11)
O1—Cr1—O1iii89.24 (9)O3A—S—O4ii69.3 (2)
O1i—Cr1—O1iii180.0O3—S—O4ii110.7 (2)
O1ii—Cr1—O1iii89.24 (9)O4A—S—O4ii109.7 (5)
O1—Cr1—O1iv89.24 (9)O4Ai—S—O4ii40.3 (10)
O1i—Cr1—O1iv89.24 (9)O4Aii—S—O4ii137.2 (6)
O1ii—Cr1—O1iv180.0O3A—S—O4i69.3 (2)
O1iii—Cr1—O1iv90.76 (9)O3—S—O4i110.7 (2)
O1—Cr1—O1v180.0O4A—S—O4i40.3 (10)
O1i—Cr1—O1v89.24 (9)O4Ai—S—O4i137.2 (6)
O1ii—Cr1—O1v89.24 (9)O4Aii—S—O4i109.7 (5)
O1iii—Cr1—O1v90.76 (9)O4ii—S—O4i108.2 (2)
O1iv—Cr1—O1v90.76 (9)O3A—S—O469.3 (2)
O3A—K1—O3Avi180.0O3—S—O4110.7 (2)
O3A—K1—O2vii104.24 (5)O4A—S—O4137.2 (5)
O3Avi—K1—O2vii75.76 (5)O4Ai—S—O4109.7 (5)
O3A—K1—O2viii75.76 (5)O4Aii—S—O440.3 (10)
O3Avi—K1—O2viii104.24 (5)O4ii—S—O4108.2 (2)
O2vii—K1—O2viii65.84 (4)O4i—S—O4108.2 (2)
O3A—K1—O2ix75.76 (5)Cr1—O1—H12122 (2)
O3Avi—K1—O2ix104.24 (5)Cr1—O1—H11121 (3)
O2vii—K1—O2ix180.0H12—O1—H11113 (4)
O2viii—K1—O2ix114.16 (4)K1xiii—O2—H22105 (6)
O3A—K1—O2x75.76 (5)K1xiii—O2—H21115 (4)
O3Avi—K1—O2x104.24 (5)H22—O2—H2199 (7)
O2vii—K1—O2x65.84 (4)S—O3—O4A53.3 (8)
O2viii—K1—O2x114.16 (4)S—O3—O4Aii53.3 (8)
O2ix—K1—O2x114.16 (4)O4A—O3—O4Aii88.0 (11)
O3A—K1—O2xi104.24 (5)S—O3—O4Ai53.3 (8)
O3Avi—K1—O2xi75.76 (5)O4A—O3—O4Ai88.0 (11)
O2vii—K1—O2xi114.16 (4)O4Aii—O3—O4Ai88.0 (11)
O2viii—K1—O2xi180.0O4Aii—O4—S68.1 (6)
O2ix—K1—O2xi65.84 (4)O4Aii—O4—O3A117.2 (9)
O2x—K1—O2xi65.84 (4)S—O4—O3A52.6 (6)
O3A—K1—O2xii104.24 (5)S—O3A—O4i58.0 (6)
O3Avi—K1—O2xii75.76 (5)S—O3A—O4ii58.0 (6)
O2vii—K1—O2xii114.16 (4)O4i—O3A—O4ii94.5 (9)
O2viii—K1—O2xii65.84 (4)S—O3A—O458.0 (6)
O2ix—K1—O2xii65.84 (4)O4i—O3A—O494.5 (9)
O2x—K1—O2xii180.0O4ii—O3A—O494.5 (9)
O2xi—K1—O2xii114.16 (4)S—O3A—K1180.0 (18)
O3A—S—O3180.0 (12)O4i—O3A—K1122.0 (6)
O3A—S—O4A106.9 (12)O4ii—O3A—K1122.0 (6)
O3—S—O4A73.1 (12)O4—O3A—K1122.0 (6)
O3A—S—O4Ai106.9 (12)O4i—O4A—S71.6 (9)
O3—S—O4Ai73.1 (12)O4i—O4A—O3121.5 (8)
O4A—S—O4Ai111.9 (11)S—O4A—O353.6 (5)
O3A—S—O4Aii106.9 (12)
O3A—S—O3—O4A−93 (100)O4—S—O3A—K1−138 (100)
O4Ai—S—O3—O4A120.000 (3)O4Aii—O4—O3A—S23.2 (9)
O4Aii—S—O3—O4A−120.000 (2)O4Aii—O4—O3A—O4i−24.3 (10)
O4ii—S—O3—O4A105.2 (5)S—O4—O3A—O4i−47.5 (5)
O4i—S—O3—O4A−14.8 (5)O4Aii—O4—O3A—O4ii70.7 (10)
O4—S—O3—O4A−134.8 (5)S—O4—O3A—O4ii47.5 (5)
O3A—S—O3—O4Aii27 (100)O4Aii—O4—O3A—K1−156.8 (9)
O4A—S—O3—O4Aii120.000 (3)S—O4—O3A—K1180.000 (3)
O4Ai—S—O3—O4Aii−120.000 (3)O3Avi—K1—O3A—S0 (100)
O4ii—S—O3—O4Aii−134.8 (5)O2vii—K1—O3A—S−85 (100)
O4i—S—O3—O4Aii105.2 (5)O2viii—K1—O3A—S−25 (100)
O4—S—O3—O4Aii−14.8 (5)O2ix—K1—O3A—S95 (100)
O3A—S—O3—O4Ai147 (100)O2x—K1—O3A—S−145 (100)
O4A—S—O3—O4Ai−120.0O2xi—K1—O3A—S155 (100)
O4Aii—S—O3—O4Ai120.0O2xii—K1—O3A—S35 (100)
O4ii—S—O3—O4Ai−14.8 (5)O3Avi—K1—O3A—O4i−136 (100)
O4i—S—O3—O4Ai−134.8 (5)O2vii—K1—O3A—O4i17.27 (17)
O4—S—O3—O4Ai105.2 (5)O2viii—K1—O3A—O4i77.27 (17)
O3A—S—O4—O4Aii−157.8 (8)O2ix—K1—O3A—O4i−162.73 (17)
O3—S—O4—O4Aii22.2 (8)O2x—K1—O3A—O4i−42.73 (17)
O4A—S—O4—O4Aii−64.9 (15)O2xi—K1—O3A—O4i−102.73 (17)
O4Ai—S—O4—O4Aii101.0 (18)O2xii—K1—O3A—O4i137.27 (17)
O4ii—S—O4—O4Aii143.6 (9)O3Avi—K1—O3A—O4ii104 (100)
O4i—S—O4—O4Aii−99.3 (8)O2vii—K1—O3A—O4ii−102.73 (17)
O3—S—O4—O3A180.000 (3)O2viii—K1—O3A—O4ii−42.73 (17)
O4A—S—O4—O3A92.9 (19)O2ix—K1—O3A—O4ii77.27 (17)
O4Ai—S—O4—O3A−101.2 (13)O2x—K1—O3A—O4ii−162.73 (17)
O4Aii—S—O4—O3A157.8 (8)O2xi—K1—O3A—O4ii137.27 (17)
O4ii—S—O4—O3A−58.6 (3)O2xii—K1—O3A—O4ii17.27 (17)
O4i—S—O4—O3A58.6 (3)O3Avi—K1—O3A—O4−16 (100)
O3—S—O3A—O4i78 (100)O2vii—K1—O3A—O4137.27 (17)
O4A—S—O3A—O4i−14.8 (5)O2viii—K1—O3A—O4−162.73 (17)
O4Ai—S—O3A—O4i−134.8 (5)O2ix—K1—O3A—O4−42.73 (17)
O4Aii—S—O3A—O4i105.2 (5)O2x—K1—O3A—O477.27 (17)
O4ii—S—O3A—O4i−120.000 (1)O2xi—K1—O3A—O417.27 (17)
O4—S—O3A—O4i120.0O2xii—K1—O3A—O4−102.73 (17)
O3—S—O3A—O4ii−162 (100)O3A—S—O4A—O4i21.7 (7)
O4A—S—O3A—O4ii105.2 (5)O3—S—O4A—O4i−158.3 (7)
O4Ai—S—O3A—O4ii−14.8 (5)O4Ai—S—O4A—O4i138.4 (14)
O4Aii—S—O3A—O4ii−134.8 (5)O4Aii—S—O4A—O4i−95 (2)
O4i—S—O3A—O4ii120.0O4ii—S—O4A—O4i95.2 (7)
O4—S—O3A—O4ii−120.0O4—S—O4A—O4i−55.9 (19)
O3—S—O3A—O4−42 (100)O3A—S—O4A—O3180.000 (2)
O4A—S—O3A—O4−134.8 (5)O4Ai—S—O4A—O3−63.3 (16)
O4Ai—S—O3A—O4105.2 (5)O4Aii—S—O4A—O363.3 (16)
O4Aii—S—O3A—O4−14.8 (5)O4ii—S—O4A—O3−106.4 (6)
O4ii—S—O3A—O4120.000 (1)O4i—S—O4A—O3158.3 (7)
O4i—S—O3A—O4−120.000 (1)O4—S—O4A—O3102.4 (15)
O3—S—O3A—K1−180 (100)S—O3—O4A—O4i24.3 (9)
O4A—S—O3A—K188 (100)O4Aii—O3—O4A—O4i−19.8 (13)
O4Ai—S—O3A—K1−32 (100)O4Ai—O3—O4A—O4i68.3 (7)
O4Aii—S—O3A—K1−152 (100)O4Aii—O3—O4A—S−44.0 (5)
O4ii—S—O3A—K1−18 (100)O4Ai—O3—O4A—S44.0 (5)
O4i—S—O3A—K1102 (100)
Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) −z, −x, −y; (iv) −y, −z, −x; (v) −x, −y, −z; (vi) −x+1, −y+1, −z+1; (vii) x+1/2, −y+1/2, −z+1; (viii) y+1/2, z, −x+1/2; (ix) −x+1/2, y+1/2, z; (x) z, −x+1/2, y+1/2; (xi) −y+1/2, −z+1, x+1/2; (xii) −z+1, x+1/2, −y+1/2; (xiii) y−1/2, −z+1/2, −x+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4xiv0.60 (4)2.03 (4)2.619 (4)171 (4)
O1—H12···O2i0.85 (4)1.77 (4)2.611 (3)171 (4)
O2—H21···O30.77 (8)2.06 (8)2.795 (4)160 (6)
O2—H22···O4xv0.78 (8)2.09 (8)2.750 (4)143 (7)
O1—H11···O4Axvi0.60 (4)2.27 (4)2.84 (2)162 (4)
O2—H22···O4Axvii0.78 (8)2.16 (8)2.872 (13)152 (7)
O2—H21···O4A0.77 (8)2.50 (8)3.22 (2)157 (6)
Symmetry codes: (i) z, x, y; (xiv) x, −y+1/2, z−1/2; (xv) y−1/2, z, −x+1/2; (xvi) y, −z+1/2, x−1/2; (xvii) z−1/2, x, −y+1/2.
(on) top
Crystal data top
H24GaO20RbS2F(000) = 1136
Mr = 563.50Dx = 2.027 Mg m−3
Cubic, Pa3Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2ab 3µ = 4.43 mm−1
a = 12.2679 (5) ÅT = 296 K
V = 1846.34 (13) Å30.2 × 0.2 × 0.2 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.055
Graphite monochromatorθmax = 26.0°, θmin = 3.7°
1130 measured reflectionsh = −10→10
608 independent reflectionsk = −15→15
505 reflections with I > 2σ(I)l = −10→10
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.042H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.102Calculated w = 1/[σ2(Fo2) + (0.046P)2 + 0.9565P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
608 reflectionsΔρmax = 0.50 e Å−3
68 parametersΔρmin = −0.54 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0101 (14)
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
xyzUiso*/UeqOcc. (<1)
Ga0.00000.00000.00000.0253 (4)
Rb0.50000.50000.50000.0514 (4)
S0.31299 (6)0.31299 (6)0.31299 (6)0.0305 (4)
O30.2453 (2)0.2453 (2)0.2453 (2)0.066 (3)0.892 (15)
O10.1577 (2)0.0107 (2)−0.0125 (2)0.0349 (6)
O40.2701 (5)0.4245 (3)0.3178 (3)0.0507 (14)0.892 (15)
O20.0479 (3)0.1425 (2)0.2988 (2)0.0451 (7)
O4A0.292 (3)0.211 (3)0.369 (5)0.068 (18)0.108 (15)
O3A0.380 (3)0.380 (3)0.380 (3)0.18 (5)0.108 (15)
H120.203 (4)0.025 (3)0.048 (4)0.059 (12)*
H110.181 (4)0.029 (4)−0.061 (4)0.062 (15)*
H220.013 (4)0.191 (5)0.285 (5)0.072 (17)*
H210.102 (6)0.165 (5)0.299 (5)0.09 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ga0.0253 (4)0.0253 (4)0.0253 (4)−0.00039 (16)−0.00039 (16)−0.00039 (16)
Rb0.0514 (4)0.0514 (4)0.0514 (4)0.0108 (2)0.0108 (2)0.0108 (2)
S0.0305 (4)0.0305 (4)0.0305 (4)0.0037 (3)0.0037 (3)0.0037 (3)
O30.066 (3)0.066 (3)0.066 (3)−0.0149 (16)−0.0149 (16)−0.0149 (16)
O10.0286 (12)0.0445 (15)0.0317 (13)−0.0035 (9)0.0008 (10)0.0030 (10)
O40.064 (3)0.0422 (19)0.0458 (17)0.0213 (19)0.0185 (17)0.0088 (14)
O20.0486 (16)0.0402 (14)0.0465 (14)0.0025 (13)−0.0053 (12)−0.0041 (11)
O4A0.057 (18)0.038 (18)0.11 (4)0.014 (14)0.06 (2)0.04 (2)
O3A0.18 (5)0.18 (5)0.18 (5)−0.07 (3)−0.07 (3)−0.07 (3)
Geometric parameters (Å, º) top
Ga—O1i1.945 (3)S—O4ii1.466 (3)
Ga—O1ii1.945 (3)S—O4Aii1.45 (2)
Ga—O1iii1.945 (3)S—O4Av1.45 (2)
Ga—O1iv1.945 (3)S—O4A1.45 (2)
Ga—O11.945 (3)S—O3A1.43 (6)
Ga—O1v1.945 (3)O3—O4A1.68 (6)
Rb—O3A2.54 (6)O3—O4Aii1.68 (6)
Rb—O3Avi2.54 (6)O3—O4Av1.68 (6)
Rb—O2vii3.081 (3)O1—H120.94 (5)
Rb—O2viii3.081 (3)O1—H110.69 (5)
Rb—O2ix3.081 (3)O4—O4Av1.04 (6)
Rb—O2x3.081 (3)O4—O3A1.65 (3)
Rb—O2xi3.081 (3)O2—Rbxiii3.081 (3)
Rb—O2xii3.081 (3)O2—H220.75 (6)
Rb—S3.9736 (13)O2—H210.72 (8)
Rb—Svi3.9736 (13)O4A—O4ii1.04 (6)
S—O31.439 (5)O3A—O4v1.65 (3)
S—O4v1.466 (3)O3A—O4ii1.65 (3)
S—O41.466 (3)
O1i—Ga—O1ii180.0O4v—S—O4108.1 (2)
O1i—Ga—O1iii90.95 (11)O3—S—O4ii110.8 (2)
O1ii—Ga—O1iii89.05 (11)O4v—S—O4ii108.1 (2)
O1i—Ga—O1iv90.95 (11)O4—S—O4ii108.1 (2)
O1ii—Ga—O1iv89.05 (11)O3—S—O4Aii71 (3)
O1iii—Ga—O1iv90.95 (11)O4v—S—O4Aii42 (3)
O1i—Ga—O189.05 (11)O4—S—O4Aii111.7 (10)
O1ii—Ga—O190.95 (11)O4ii—S—O4Aii136.1 (13)
O1iii—Ga—O189.05 (11)O3—S—O4Av71 (3)
O1iv—Ga—O1180.0O4v—S—O4Av136.1 (13)
O1i—Ga—O1v89.05 (11)O4—S—O4Av42 (3)
O1ii—Ga—O1v90.95 (11)O4ii—S—O4Av111.7 (10)
O1iii—Ga—O1v180.0O4Aii—S—O4Av110 (3)
O1iv—Ga—O1v89.05 (11)O3—S—O4A71 (3)
O1—Ga—O1v90.95 (11)O4v—S—O4A111.7 (10)
O3A—Rb—O3Avi180.000 (2)O4—S—O4A136.1 (13)
O3A—Rb—O2vii75.82 (6)O4ii—S—O4A42 (3)
O3Avi—Rb—O2vii104.18 (6)O4Aii—S—O4A110 (3)
O3A—Rb—O2viii104.18 (6)O4Av—S—O4A110 (3)
O3Avi—Rb—O2viii75.82 (6)O3—S—O3A180 (3)
O2vii—Rb—O2viii65.79 (4)O4v—S—O3A69.2 (2)
O3A—Rb—O2ix104.18 (6)O4—S—O3A69.2 (2)
O3Avi—Rb—O2ix75.82 (6)O4ii—S—O3A69.2 (2)
O2vii—Rb—O2ix65.79 (4)O4Aii—S—O3A109 (3)
O2viii—Rb—O2ix114.21 (5)O4Av—S—O3A109 (3)
O3A—Rb—O2x75.82 (6)O4A—S—O3A109 (3)
O3Avi—Rb—O2x104.18 (6)O3—S—Rb180.0 (3)
O2vii—Rb—O2x114.21 (4)O4v—S—Rb69.2 (2)
O2viii—Rb—O2x65.79 (4)O4—S—Rb69.2 (2)
O2ix—Rb—O2x180.0O4ii—S—Rb69.2 (2)
O3A—Rb—O2xi104.18 (6)O4Aii—S—Rb109 (3)
O3Avi—Rb—O2xi75.82 (6)O4Av—S—Rb109 (3)
O2vii—Rb—O2xi180.0O4A—S—Rb109 (3)
O2viii—Rb—O2xi114.21 (5)O3A—S—Rb0 (3)
O2ix—Rb—O2xi114.21 (4)S—O3—O4A54.6 (16)
O2x—Rb—O2xi65.79 (4)S—O3—O4Aii54.6 (16)
O3A—Rb—O2xii75.82 (6)O4A—O3—O4Aii90 (2)
O3Avi—Rb—O2xii104.18 (6)S—O3—O4Av54.6 (16)
O2vii—Rb—O2xii114.21 (5)O4A—O3—O4Av90 (2)
O2viii—Rb—O2xii180.0O4Aii—O3—O4Av90 (2)
O2ix—Rb—O2xii65.79 (4)Ga—O1—H12122 (3)
O2x—Rb—O2xii114.21 (5)Ga—O1—H11120 (4)
O2xi—Rb—O2xii65.79 (4)H12—O1—H11111 (5)
O3A—Rb—S0.0 (19)O4Av—O4—S68.2 (15)
O3Avi—Rb—S180.0 (19)O4Av—O4—O3A120 (2)
O2vii—Rb—S75.82 (6)S—O4—O3A54.4 (17)
O2viii—Rb—S104.18 (6)Rbxiii—O2—H22121 (4)
O2ix—Rb—S104.18 (6)Rbxiii—O2—H21113 (5)
O2x—Rb—S75.82 (6)H22—O2—H21103 (6)
O2xi—Rb—S104.18 (6)O4ii—O4A—S70.2 (19)
O2xii—Rb—S75.82 (6)O4ii—O4A—O3121.5 (17)
O3A—Rb—Svi180.0 (19)S—O4A—O354.1 (14)
O3Avi—Rb—Svi0.0 (19)S—O3A—O4v56.3 (17)
O2vii—Rb—Svi104.18 (6)S—O3A—O456.3 (17)
O2viii—Rb—Svi75.82 (6)O4v—O3A—O492 (2)
O2ix—Rb—Svi75.82 (6)S—O3A—O4ii56.3 (17)
O2x—Rb—Svi104.18 (6)O4v—O3A—O4ii92 (2)
O2xi—Rb—Svi75.82 (6)O4—O3A—O4ii92 (2)
O2xii—Rb—Svi104.18 (6)S—O3A—Rb180 (5)
S—Rb—Svi180.0O4v—O3A—Rb123.7 (17)
O3—S—O4v110.8 (2)O4—O3A—Rb123.7 (17)
O3—S—O4110.8 (2)O4ii—O3A—Rb123.7 (17)
O3A—Rb—S—O30 (100)Rb—S—O4—O4Av−160.9 (16)
O3Avi—Rb—S—O30 (100)O3—S—O4—O3A180.000 (7)
O2vii—Rb—S—O383 (100)O4v—S—O4—O3A−58.4 (3)
O2viii—Rb—S—O323 (100)O4ii—S—O4—O3A58.4 (3)
O2ix—Rb—S—O3143 (100)O4Aii—S—O4—O3A−103 (3)
O2x—Rb—S—O3−37 (100)O4Av—S—O4—O3A160.9 (16)
O2xi—Rb—S—O3−97 (100)O4A—S—O4—O3A96 (4)
O2xii—Rb—S—O3−157 (100)Rb—S—O4—O3A0.000 (8)
Svi—Rb—S—O30 (36)O3—S—O4A—O4ii−161.2 (14)
O3A—Rb—S—O4v165 (100)O4v—S—O4A—O4ii93.3 (14)
O3Avi—Rb—S—O4v−133 (100)O4—S—O4A—O4ii−60 (4)
O2vii—Rb—S—O4v76.01 (17)O4Aii—S—O4A—O4ii138 (3)
O2viii—Rb—S—O4v16.01 (17)O4Av—S—O4A—O4ii−100 (4)
O2ix—Rb—S—O4v136.01 (17)O3A—S—O4A—O4ii18.8 (14)
O2x—Rb—S—O4v−43.99 (17)Rb—S—O4A—O4ii18.8 (14)
O2xi—Rb—S—O4v−103.99 (17)O4v—S—O4A—O3−105.6 (12)
O2xii—Rb—S—O4v−163.99 (17)O4—S—O4A—O3101 (3)
Svi—Rb—S—O4v−48 (100)O4ii—S—O4A—O3161.2 (14)
O3A—Rb—S—O445 (100)O4Aii—S—O4A—O3−61 (3)
O3Avi—Rb—S—O4107 (100)O4Av—S—O4A—O361 (3)
O2vii—Rb—S—O4−43.99 (17)O3A—S—O4A—O3180.000 (4)
O2viii—Rb—S—O4−103.99 (17)Rb—S—O4A—O3180.000 (5)
O2ix—Rb—S—O416.01 (17)S—O3—O4A—O4ii20.9 (16)
O2x—Rb—S—O4−163.99 (17)O4Aii—O3—O4A—O4ii65.8 (14)
O2xi—Rb—S—O4136.01 (17)O4Av—O3—O4A—O4ii−24 (2)
O2xii—Rb—S—O476.01 (17)O4Aii—O3—O4A—S44.9 (11)
Svi—Rb—S—O4−168 (100)O4Av—O3—O4A—S−44.9 (11)
O3A—Rb—S—O4ii−75 (100)O3—S—O3A—O4v−162 (100)
O3Avi—Rb—S—O4ii−13 (100)O4—S—O3A—O4v−120.000 (2)
O2vii—Rb—S—O4ii−163.99 (17)O4ii—S—O3A—O4v120.000 (3)
O2viii—Rb—S—O4ii136.01 (17)O4Aii—S—O3A—O4v−13.3 (11)
O2ix—Rb—S—O4ii−103.99 (17)O4Av—S—O3A—O4v−133.3 (11)
O2x—Rb—S—O4ii76.01 (17)O4A—S—O3A—O4v106.7 (11)
O2xi—Rb—S—O4ii16.01 (17)Rb—S—O3A—O4v15 (100)
O2xii—Rb—S—O4ii−43.99 (17)O3—S—O3A—O4−42 (100)
Svi—Rb—S—O4ii72 (100)O4v—S—O3A—O4120.000 (4)
O3A—Rb—S—O4Aii152 (100)O4ii—S—O3A—O4−120.000 (3)
O3Avi—Rb—S—O4Aii−146 (100)O4Aii—S—O3A—O4106.7 (11)
O2vii—Rb—S—O4Aii62.8 (11)O4Av—S—O3A—O4−13.3 (11)
O2viii—Rb—S—O4Aii2.8 (11)O4A—S—O3A—O4−133.3 (11)
O2ix—Rb—S—O4Aii122.8 (11)Rb—S—O3A—O4135 (100)
O2x—Rb—S—O4Aii−57.2 (11)O3—S—O3A—O4ii78 (100)
O2xi—Rb—S—O4Aii−117.2 (11)O4v—S—O3A—O4ii−120.000 (3)
O2xii—Rb—S—O4Aii−177.2 (11)O4—S—O3A—O4ii120.0
Svi—Rb—S—O4Aii−61 (100)O4Aii—S—O3A—O4ii−133.3 (11)
O3A—Rb—S—O4Av32 (100)O4Av—S—O3A—O4ii106.7 (11)
O3Avi—Rb—S—O4Av94 (100)O4A—S—O3A—O4ii−13.3 (11)
O2vii—Rb—S—O4Av−57.2 (11)Rb—S—O3A—O4ii−105 (100)
O2viii—Rb—S—O4Av−117.2 (11)O3—S—O3A—Rb0 (100)
O2ix—Rb—S—O4Av2.8 (11)O4v—S—O3A—Rb−15 (100)
O2x—Rb—S—O4Av−177.2 (11)O4—S—O3A—Rb−135 (100)
O2xi—Rb—S—O4Av122.8 (11)O4ii—S—O3A—Rb105 (100)
O2xii—Rb—S—O4Av62.8 (11)O4Aii—S—O3A—Rb−28 (100)
Svi—Rb—S—O4Av179 (100)O4Av—S—O3A—Rb−148 (100)
O3A—Rb—S—O4A−88 (100)O4A—S—O3A—Rb92 (100)
O3Avi—Rb—S—O4A−26 (100)O4Av—O4—O3A—S20.5 (19)
O2vii—Rb—S—O4A−177.2 (11)O4Av—O4—O3A—O4v67 (2)
O2viii—Rb—S—O4A122.8 (11)S—O4—O3A—O4v46.2 (13)
O2ix—Rb—S—O4A−117.2 (11)O4Av—O4—O3A—O4ii−26 (2)
O2x—Rb—S—O4A62.8 (11)S—O4—O3A—O4ii−46.2 (13)
O2xi—Rb—S—O4A2.8 (11)O4Av—O4—O3A—Rb−159.5 (19)
O2xii—Rb—S—O4A−57.2 (11)S—O4—O3A—Rb180.000 (7)
Svi—Rb—S—O4A59 (100)O3Avi—Rb—O3A—S0 (100)
O3Avi—Rb—S—O3A0 (100)O2vii—Rb—O3A—S91 (100)
O2vii—Rb—S—O3A−89 (100)O2viii—Rb—O3A—S31 (100)
O2viii—Rb—S—O3A−149 (100)O2ix—Rb—O3A—S151 (100)
O2ix—Rb—S—O3A−29 (100)O2x—Rb—O3A—S−29 (100)
O2x—Rb—S—O3A151 (100)O2xi—Rb—O3A—S−89 (100)
O2xi—Rb—S—O3A91 (100)O2xii—Rb—O3A—S−149 (100)
O2xii—Rb—S—O3A31 (100)Svi—Rb—O3A—S0 (100)
Svi—Rb—S—O3A0 (84)O3Avi—Rb—O3A—O4v−138 (95)
O4v—S—O3—O4A106.7 (11)O2vii—Rb—O3A—O4v76.01 (17)
O4—S—O3—O4A−133.3 (11)O2viii—Rb—O3A—O4v16.01 (17)
O4ii—S—O3—O4A−13.3 (11)O2ix—Rb—O3A—O4v136.01 (17)
O4Aii—S—O3—O4A120.000 (5)O2x—Rb—O3A—O4v−43.99 (17)
O4Av—S—O3—O4A−120.000 (6)O2xi—Rb—O3A—O4v−103.99 (17)
O3A—S—O3—O4A−91 (100)O2xii—Rb—O3A—O4v−163.99 (17)
Rb—S—O3—O4A100 (100)S—Rb—O3A—O4v−15 (100)
O4v—S—O3—O4Aii−13.3 (11)Svi—Rb—O3A—O4v−90 (100)
O4—S—O3—O4Aii106.7 (11)O3Avi—Rb—O3A—O4102 (95)
O4ii—S—O3—O4Aii−133.3 (11)O2vii—Rb—O3A—O4−43.99 (17)
O4Av—S—O3—O4Aii120.0O2viii—Rb—O3A—O4−103.99 (17)
O4A—S—O3—O4Aii−120.0O2ix—Rb—O3A—O416.01 (17)
O3A—S—O3—O4Aii149 (100)O2x—Rb—O3A—O4−163.99 (17)
Rb—S—O3—O4Aii−20 (100)O2xi—Rb—O3A—O4136.01 (17)
O4v—S—O3—O4Av−133.3 (11)O2xii—Rb—O3A—O476.01 (17)
O4—S—O3—O4Av−13.3 (11)S—Rb—O3A—O4−135 (100)
O4ii—S—O3—O4Av106.7 (11)Svi—Rb—O3A—O4150 (100)
O4Aii—S—O3—O4Av−120.000 (7)O3Avi—Rb—O3A—O4ii−18 (95)
O4A—S—O3—O4Av120.000 (7)O2vii—Rb—O3A—O4ii−163.99 (16)
O3A—S—O3—O4Av29 (100)O2viii—Rb—O3A—O4ii136.01 (16)
Rb—S—O3—O4Av−140 (100)O2ix—Rb—O3A—O4ii−103.99 (16)
O3—S—O4—O4Av19.1 (16)O2x—Rb—O3A—O4ii76.01 (17)
O4v—S—O4—O4Av140.7 (16)O2xi—Rb—O3A—O4ii16.01 (16)
O4ii—S—O4—O4Av−102.5 (15)O2xii—Rb—O3A—O4ii−43.99 (16)
O4Aii—S—O4—O4Av96 (4)S—Rb—O3A—O4ii105 (100)
O4A—S—O4—O4Av−65 (3)Svi—Rb—O3A—O4ii30 (100)
O3A—S—O4—O4Av−160.9 (16)
Symmetry codes: (i) −z, −x, −y; (ii) z, x, y; (iii) −y, −z, −x; (iv) −x, −y, −z; (v) y, z, x; (vi) −x+1, −y+1, −z+1; (vii) −x+1/2, y+1/2, z; (viii) −z+1, x+1/2, −y+1/2; (ix) −y+1/2, −z+1, x+1/2; (x) y+1/2, z, −x+1/2; (xi) x+1/2, −y+1/2, −z+1; (xii) z, −x+1/2, y+1/2; (xiii) y−1/2, −z+1/2, −x+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4xiv0.69 (5)1.93 (6)2.621 (4)170 (5)
O1—H12···O2ii0.94 (5)1.68 (5)2.612 (4)171 (4)
O2—H21···O30.72 (8)2.12 (7)2.808 (5)160 (7)
O2—H22···O4xv0.75 (6)2.01 (7)2.763 (4)173 (6)
O1—H11···O4Axvi0.69 (5)2.22 (8)2.89 (5)160 (5)
O2—H22···O4Axvii0.75 (6)2.15 (7)2.86 (3)157 (6)
O2—H21···O4A0.72 (8)2.56 (10)3.23 (5)159 (7)
Symmetry codes: (ii) z, x, y; (xiv) x, −y+1/2, z−1/2; (xv) y−1/2, z, −x+1/2; (xvi) y, −z+1/2, x−1/2; (xvii) z−1/2, x, −y+1/2.
(oq) top
Crystal data top
H24GaO20S2TlF(000) = 1312
Mr = 682.40Dx = 2.474 Mg m−3
Cubic, Pa3Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2ab 3µ = 10.57 mm−1
a = 12.2368 (5) ÅT = 296 K
V = 1832.33 (13) Å30.2 × 0.2 × 0.1 mm
Z = 4
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.021
Graphite monochromatorθmax = 26.0°, θmin = 3.7°
1118 measured reflectionsh = −10→10
601 independent reflectionsk = −15→15
498 reflections with I > 2σ(I)l = −10→10
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.064Calculated w = 1/[σ2(Fo2) + (0.0249P)2 + 1.5522P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.006
601 reflectionsΔρmax = 0.67 e Å−3
68 parametersΔρmin = −0.41 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0130 (6)
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
xyzUiso*/UeqOcc. (<1)
Tl10.50000.50000.50000.0513 (3)
S0.31303 (5)0.31303 (5)0.31303 (5)0.0268 (3)
Ga10.00000.00000.00000.0199 (3)
O10.1579 (2)0.0104 (2)−0.0124 (2)0.0311 (6)
H120.193 (3)0.022 (3)0.033 (3)0.040 (12)*
H110.177 (3)0.026 (3)−0.056 (3)0.035 (13)*
O20.0486 (3)0.1433 (2)0.2987 (2)0.0422 (6)
H220.014 (3)0.180 (3)0.289 (3)0.032 (12)*
H210.123 (6)0.168 (4)0.301 (5)0.109 (17)*
O30.2453 (2)0.2453 (2)0.2453 (2)0.070 (4)0.830 (17)
O40.2700 (5)0.4249 (3)0.3178 (3)0.0478 (15)0.830 (17)
O3A0.3772 (15)0.3772 (15)0.3772 (15)0.19 (3)0.170 (17)
O4A0.295 (2)0.212 (2)0.372 (3)0.079 (13)0.170 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tl10.0513 (3)0.0513 (3)0.0513 (3)0.00574 (9)0.00574 (9)0.00574 (9)
S0.0268 (3)0.0268 (3)0.0268 (3)0.0037 (3)0.0037 (3)0.0037 (3)
Ga10.0199 (3)0.0199 (3)0.0199 (3)−0.00036 (14)−0.00036 (14)−0.00036 (14)
O10.0235 (12)0.0425 (15)0.0274 (14)−0.0055 (9)−0.0001 (10)0.0017 (10)
O20.0459 (15)0.0360 (12)0.0448 (13)0.0049 (12)−0.0089 (11)−0.0047 (11)
O30.070 (4)0.070 (4)0.070 (4)−0.0208 (17)−0.0208 (17)−0.0208 (17)
O40.064 (3)0.0355 (19)0.0433 (17)0.024 (2)0.0229 (17)0.0111 (14)
O3A0.19 (3)0.19 (3)0.19 (3)−0.086 (19)−0.086 (19)−0.086 (19)
O4A0.080 (15)0.057 (15)0.10 (2)0.038 (12)0.064 (15)0.062 (16)
Geometric parameters (Å, º) top
Tl1—O3Ai2.60 (3)Ga1—O1vii1.942 (3)
Tl1—O3A2.60 (3)Ga1—O1v1.942 (3)
Tl1—O2ii3.081 (3)Ga1—O1viii1.942 (3)
Tl1—O2iii3.081 (3)O1—H120.72 (4)
S—O4Aiv1.453 (15)O1—H110.61 (4)
S—O4Av1.453 (15)O2—H220.63 (4)
S—O4A1.453 (15)O2—H210.96 (8)
S—O31.435 (5)O3—O4Aiv1.72 (4)
S—O4v1.468 (3)O3—O4Av1.72 (4)
S—O41.468 (3)O3—O4A1.72 (4)
S—O4iv1.468 (3)O4—O4Av1.00 (5)
S—O3A1.36 (3)O4—O3A1.610 (18)
Ga1—O1vi1.942 (3)O3A—O4v1.610 (17)
Ga1—O1iv1.942 (3)O3A—O4iv1.610 (17)
Ga1—O11.942 (3)O4A—O4iv1.00 (5)
O3Ai—Tl1—O3A180.000 (1)O1iv—Ga1—O1vii180.0
O3Ai—Tl1—O2ii75.85 (5)O1—Ga1—O1vii89.01 (11)
O3A—Tl1—O2ii104.15 (5)O1vi—Ga1—O1v180.0
O3Ai—Tl1—O2iii104.15 (5)O1iv—Ga1—O1v90.99 (11)
O3A—Tl1—O2iii75.85 (5)O1—Ga1—O1v90.99 (11)
O2ii—Tl1—O2iii65.77 (4)O1vii—Ga1—O1v89.01 (11)
O4Aiv—S—O4Av111.9 (18)O1vi—Ga1—O1viii90.99 (11)
O4Aiv—S—O4A111.9 (18)O1iv—Ga1—O1viii89.01 (11)
O4Av—S—O4A111.9 (19)O1—Ga1—O1viii180.0
O4Aiv—S—O373 (2)O1vii—Ga1—O1viii90.99 (11)
O4Av—S—O373 (2)O1v—Ga1—O1viii89.01 (11)
O4A—S—O373 (2)Ga1—O1—H12123 (3)
O4Aiv—S—O4v40.0 (19)Ga1—O1—H11118 (4)
O4Av—S—O4v136.3 (9)H12—O1—H11113 (5)
O4A—S—O4v110.6 (8)H22—O2—H21115 (5)
O3—S—O4v110.7 (2)S—O3—O4Aiv53.9 (13)
O4Aiv—S—O4110.6 (8)S—O3—O4Av53.9 (13)
O4Av—S—O440.0 (19)O4Aiv—O3—O4Av88.9 (19)
O4A—S—O4136.3 (9)S—O3—O4A53.9 (13)
O3—S—O4110.7 (2)O4Aiv—O3—O4A88.9 (19)
O4v—S—O4108.2 (2)O4Av—O3—O4A88.9 (19)
O4Aiv—S—O4iv136.3 (9)O4Av—O4—S69.2 (9)
O4Av—S—O4iv110.6 (8)O4Av—O4—O3A118.2 (13)
O4A—S—O4iv40.0 (18)S—O4—O3A52.2 (10)
O3—S—O4iv110.7 (2)S—O3A—O4v58.5 (10)
O4v—S—O4iv108.2 (2)S—O3A—O458.5 (10)
O4—S—O4iv108.2 (2)O4v—O3A—O495.2 (13)
O4Aiv—S—O3A107 (2)S—O3A—O4iv58.5 (10)
O4Av—S—O3A107 (2)O4v—O3A—O4iv95.2 (13)
O4A—S—O3A107 (2)O4—O3A—O4iv95.2 (13)
O3—S—O3A180.0 (19)S—O3A—Tl1180 (3)
O4v—S—O3A69.3 (2)O4v—O3A—Tl1121.5 (10)
O4—S—O3A69.3 (2)O4—O3A—Tl1121.5 (10)
O4iv—S—O3A69.3 (2)O4iv—O3A—Tl1121.5 (10)
O1vi—Ga1—O1iv89.01 (11)O4iv—O4A—S70.8 (16)
O1vi—Ga1—O189.01 (11)O4iv—O4A—O3120.6 (12)
O1iv—Ga1—O190.99 (11)S—O4A—O353.0 (9)
O1vi—Ga1—O1vii90.99 (11)
O4Av—S—O3—O4Aiv120.0O4v—S—O3A—O4iv−120.000 (2)
O4A—S—O3—O4Aiv−120.0O4—S—O3A—O4iv120.0
O4v—S—O3—O4Aiv−13.8 (8)O4Aiv—S—O3A—Tl1−147 (100)
O4—S—O3—O4Aiv106.2 (8)O4Av—S—O3A—Tl193 (100)
O4iv—S—O3—O4Aiv−133.8 (8)O4A—S—O3A—Tl1−27 (100)
O3A—S—O3—O4Aiv−2 (100)O3—S—O3A—Tl10 (100)
O4Aiv—S—O3—O4Av−120.000 (5)O4v—S—O3A—Tl1−133 (100)
O4A—S—O3—O4Av120.000 (5)O4—S—O3A—Tl1107 (100)
O4v—S—O3—O4Av−133.8 (8)O4iv—S—O3A—Tl1−13 (100)
O4—S—O3—O4Av−13.8 (8)O4Av—O4—O3A—S22.1 (14)
O4iv—S—O3—O4Av106.2 (8)O4Av—O4—O3A—O4v70.0 (16)
O3A—S—O3—O4Av−122 (100)S—O4—O3A—O4v47.9 (8)
O4Aiv—S—O3—O4A120.000 (4)O4Av—O4—O3A—O4iv−25.8 (17)
O4Av—S—O3—O4A−120.000 (4)S—O4—O3A—O4iv−47.9 (8)
O4v—S—O3—O4A106.2 (7)O4Av—O4—O3A—Tl1−157.9 (14)
O4—S—O3—O4A−133.8 (7)S—O4—O3A—Tl1180.000 (4)
O4iv—S—O3—O4A−13.8 (7)O3Ai—Tl1—O3A—S0 (100)
O3A—S—O3—O4A118 (100)O2ii—Tl1—O3A—S29 (100)
O4Aiv—S—O4—O4Av100 (3)O2iii—Tl1—O3A—S89 (100)
O4A—S—O4—O4Av−66 (2)O3Ai—Tl1—O3A—O4v−154 (100)
O3—S—O4—O4Av20.8 (13)O2ii—Tl1—O3A—O4v−103.78 (19)
O4v—S—O4—O4Av142.3 (13)O2iii—Tl1—O3A—O4v−43.78 (19)
O4iv—S—O4—O4Av−100.7 (12)O3Ai—Tl1—O3A—O486 (100)
O3A—S—O4—O4Av−159.2 (13)O2ii—Tl1—O3A—O4136.22 (19)
O4Aiv—S—O4—O3A−101 (2)O2iii—Tl1—O3A—O4−163.78 (19)
O4Av—S—O4—O3A159.2 (13)O3Ai—Tl1—O3A—O4iv−34 (100)
O4A—S—O4—O3A93 (3)O2ii—Tl1—O3A—O4iv16.22 (19)
O3—S—O4—O3A180.000 (4)O2iii—Tl1—O3A—O4iv76.22 (19)
O4v—S—O4—O3A−58.5 (3)O4Aiv—S—O4A—O4iv137 (2)
O4iv—S—O4—O3A58.5 (3)O4Av—S—O4A—O4iv−96 (3)
O4Aiv—S—O3A—O4v−13.8 (8)O3—S—O4A—O4iv−159.7 (11)
O4Av—S—O3A—O4v−133.8 (8)O4v—S—O4A—O4iv94.0 (11)
O4A—S—O3A—O4v106.2 (8)O4—S—O4A—O4iv−57 (3)
O3—S—O3A—O4v−12 (100)O3A—S—O4A—O4iv20.3 (11)
O4—S—O3A—O4v−120.000 (1)O4Aiv—S—O4A—O3−63 (3)
O4iv—S—O3A—O4v120.000 (1)O4Av—S—O4A—O363 (3)
O4Aiv—S—O3A—O4106.2 (7)O4v—S—O4A—O3−106.3 (9)
O4Av—S—O3A—O4−13.8 (7)O4—S—O4A—O3103 (2)
O4A—S—O3A—O4−133.8 (7)O4iv—S—O4A—O3159.7 (11)
O3—S—O3A—O4108 (100)O3A—S—O4A—O3180.000 (3)
O4v—S—O3A—O4120.000 (2)S—O3—O4A—O4iv22.4 (13)
O4iv—S—O3A—O4−120.000 (1)O4Aiv—O3—O4A—O4iv66.8 (10)
O4Aiv—S—O3A—O4iv−133.8 (8)O4Av—O3—O4A—O4iv−22 (2)
O4Av—S—O3A—O4iv106.2 (8)O4Aiv—O3—O4A—S44.4 (9)
O4A—S—O3A—O4iv−13.8 (8)O4Av—O3—O4A—S−44.4 (9)
O3—S—O3A—O4iv−132 (100)
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1/2, −y+1/2, −z+1; (iii) y+1/2, z, −x+1/2; (iv) z, x, y; (v) y, z, x; (vi) −y, −z, −x; (vii) −z, −x, −y; (viii) −x, −y, −z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4ix0.61 (4)2.01 (4)2.613 (4)168 (5)
O1—H12···O2iv0.72 (4)1.89 (4)2.611 (4)174 (4)
O2—H21···O30.96 (8)1.89 (7)2.789 (4)153 (6)
O2—H22···O4x0.63 (4)2.13 (4)2.749 (4)167 (4)
O1—H11···O4Axi0.61 (4)2.25 (6)2.83 (3)162 (5)
O2—H22···O4Axii0.63 (4)2.23 (4)2.85 (2)167 (5)
O2—H21···O4A0.96 (8)2.34 (10)3.26 (4)159 (5)
Symmetry codes: (iv) z, x, y; (ix) x, −y+1/2, z−1/2; (x) y−1/2, z, −x+1/2; (xi) y, −z+1/2, x−1/2; (xii) z−1/2, x, −y+1/2.
 

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