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Synthetic schuetteite [trimercury(II) dioxide sulfate(VI)], Hg3(SO4)O2, has been prepared under hydro­thermal conditions starting from HgSO4 (520 K, 10 d) in demineralized water. The crystal structure comprises infinite two-dimensional cationic nets with an overall composition of [Hg3O2]2+, and disordered SO42- tetrahedra situated in the interstices of the nets.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801017561/om6059sup1.cif
Contains datablocks I, Hg3SO6

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801017561/om6059Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Hg-O) = 0.008 Å
  • Disorder in main residue
  • R factor = 0.021
  • wR factor = 0.051
  • Data-to-parameter ratio = 18.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

PLATON alerts of the form PLAT_7?? have been detected for an inorganic
structure. These tests are under development  for inorganics and
comments are welcomed. It is not necessary to supply a data
validation response form for these alerts at this time.


Red Alert Alert Level A:
DIFF_020 Alert A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards. DIFF_022 Alert A _diffrn_standards_decay_% is missing Percentage decrease in standards intensity. PLAT_701 Alert A Bond Calc 6.749(6), Rep 2.123(6), Dev. 771.00 Sigma HG1 -O1 1.555 5.555 PLAT_701 Alert A Bond Calc 6.60(2), Rep 2.473(19), Dev. 206.35 Sigma HG1 -O3B 1.555 6.565 PLAT_701 Alert A Bond Calc 6.42(2), Rep 2.750(18), Dev. 183.50 Sigma HG1 -O3A 1.555 6.565 PLAT_701 Alert A Bond Calc 5.92(2), Rep 2.836(17), Dev. 154.20 Sigma HG1 -O2A 1.555 6.565 PLAT_701 Alert A Bond Calc 4.362(7), Rep 2.070(7), Dev. 327.43 Sigma HG2 -O1 1.555 5.655 PLAT_701 Alert A Bond Calc 3.50(3), Rep 2.647(15), Dev. 28.43 Sigma HG2 -O2A 1.555 5.655 PLAT_701 Alert A Bond Calc 8.17(2), Rep 2.657(18), Dev. 275.65 Sigma HG2 -O3A 1.555 6.555 PLAT_701 Alert A Bond Calc 2.962(18), Rep 2.775(16), Dev. 10.39 Sigma HG2 -O2B 1.555 6.655 PLAT_701 Alert A Bond Calc 8.21(2), Rep 2.96(2), Dev. 262.50 Sigma HG2 -O3B 1.555 6.555 PLAT_701 Alert A Bond Calc 2.78(3), Rep 2.961(17), Dev. 6.03 Sigma HG2 -O2B 1.555 5.655 PLAT_701 Alert A Bond Calc 3.67(2), Rep 1.451(15), Dev. 110.95 Sigma S -O2B 1.555 6.555 PLAT_701 Alert A Bond Calc 5.73(2), Rep 1.461(19), Dev. 213.45 Sigma S -O3B 1.555 6.555 PLAT_701 Alert A Bond Calc 5.79(2), Rep 1.491(19), Dev. 214.95 Sigma S -O3A 1.555 6.555 PLAT_701 Alert A Bond Calc 4.11(2), Rep 1.523(16), Dev. 129.35 Sigma S -O2A 1.555 6.555 PLAT_701 Alert A Bond Calc 8.6348(9), Rep 3.3828(16), Dev. 5835.56 Sigma S -HG1 1.555 6.665 PLAT_701 Alert A Bond Calc 6.749(6), Rep 2.123(6), Dev. 771.00 Sigma O1 -HG1 1.555 5.555 PLAT_701 Alert A Bond Calc 7.202(18), Rep 2.836(17), Dev. 242.56 Sigma O2A -HG1 1.555 6.665 PLAT_701 Alert A Bond Calc 7.720(18), Rep 3.528(16), Dev. 232.89 Sigma O2B -HG1 1.555 6.665 PLAT_701 Alert A Bond Calc 8.764(19), Rep 2.750(18), Dev. 316.53 Sigma O3A -HG1 1.555 6.665 PLAT_701 Alert A Bond Calc 8.388(19), Rep 2.473(19), Dev. 311.32 Sigma O3B -HG1 1.555 6.665 PLAT_702 Alert A Angle Calc 108.0(2), Rep 169.72(6), Dev. 308.60 Sigma O1 -HG1 -O1 2.665 1.555 5.555 PLAT_702 Alert A Angle Calc 56.8(4), Rep 96.8(5), Dev. 100.00 Sigma O1 -HG1 -O2A 5.555 1.555 1.555 PLAT_702 Alert A Angle Calc 134.6(3), Rep 86.2(5), Dev. 161.33 Sigma O1 -HG1 -O3B 2.665 1.555 6.565 PLAT_702 Alert A Angle Calc 117.4(2), Rep 97.4(5), Dev. 100.00 Sigma O1 -HG1 -O3B 5.555 1.555 6.565 PLAT_702 Alert A Angle Calc 119.0(5), Rep 142.3(6), Dev. 46.60 Sigma O2A -HG1 -O3B 1.555 1.555 6.565 PLAT_702 Alert A Angle Calc 43.4(4), Rep 80.3(4), Dev. 92.25 Sigma O1 -HG1 -O2B 5.555 1.555 1.555 PLAT_702 Alert A Angle Calc 111.7(5), Rep 151.1(6), Dev. 78.80 Sigma O3B -HG1 -O2B 6.565 1.555 1.555 PLAT_702 Alert A Angle Calc 49.2(4), Rep 82.8(4), Dev. 84.00 Sigma O1 -HG1 -O3A 5.555 1.555 4.556 PLAT_702 Alert A Angle Calc 122.1(6), Rep 118.3(7), Dev. 6.33 Sigma O3B -HG1 -O3A 6.565 1.555 4.556 PLAT_702 Alert A Angle Calc 48.1(4), Rep 90.8(4), Dev. 106.75 Sigma O1 -HG1 -O3B 5.555 1.555 4.556 PLAT_702 Alert A Angle Calc 131.9(6), Rep 123.0(6), Dev. 14.83 Sigma O3B -HG1 -O3B 6.565 1.555 4.556 PLAT_702 Alert A Angle Calc 113.88(13), Rep 77.2(2), Dev. 282.15 Sigma O1 -HG1 -O1 5.555 1.555 1.555 PLAT_702 Alert A Angle Calc 48.6(2), Rep 72.6(5), Dev. 120.00 Sigma O3B -HG1 -O1 6.565 1.555 1.555 PLAT_702 Alert A Angle Calc 137.0(3), Rep 78.8(4), Dev. 194.00 Sigma O1 -HG1 -O3A 2.665 1.555 6.565 PLAT_702 Alert A Angle Calc 114.9(2), Rep 105.1(4), Dev. 49.00 Sigma O1 -HG1 -O3A 5.555 1.555 6.565 PLAT_702 Alert A Angle Calc 115.6(5), Rep 138.2(6), Dev. 45.20 Sigma O2A -HG1 -O3A 1.555 1.555 6.565 PLAT_702 Alert A Angle Calc 3.6(3), Rep 7.7(7), Dev. 13.67 Sigma O3B -HG1 -O3A 6.565 1.555 6.565 PLAT_702 Alert A Angle Calc 108.1(5), Rep 150.1(5), Dev. 84.00 Sigma O2B -HG1 -O3A 1.555 1.555 6.565 PLAT_702 Alert A Angle Calc 122.9(6), Rep 119.5(5), Dev. 5.67 Sigma O3A -HG1 -O3A 4.556 1.555 6.565 PLAT_702 Alert A Angle Calc 132.7(6), Rep 122.8(6), Dev. 16.50 Sigma O3B -HG1 -O3A 4.556 1.555 6.565 PLAT_702 Alert A Angle Calc 46.5(2), Rep 73.9(4), Dev. 137.00 Sigma O1 -HG1 -O3A 1.555 1.555 6.565 PLAT_702 Alert A Angle Calc 123.7(3), Rep 99.2(4), Dev. 81.67 Sigma O1 -HG1 -O2A 2.665 1.555 6.565 PLAT_702 Alert A Angle Calc 124.7(3), Rep 76.7(4), Dev. 160.00 Sigma O1 -HG1 -O2A 5.555 1.555 6.565 PLAT_702 Alert A Angle Calc 137.7(4), Rep 170.2(4), Dev. 81.25 Sigma O2A -HG1 -O2A 1.555 1.555 6.565 PLAT_702 Alert A Angle Calc 18.7(3), Rep 47.0(6), Dev. 94.33 Sigma O3B -HG1 -O2A 6.565 1.555 6.565 PLAT_702 Alert A Angle Calc 129.7(5), Rep 153.5(5), Dev. 47.60 Sigma O2B -HG1 -O2A 1.555 1.555 6.565 PLAT_702 Alert A Angle Calc 111.7(5), Rep 74.0(5), Dev. 75.40 Sigma O3A -HG1 -O2A 4.556 1.555 6.565 PLAT_702 Alert A Angle Calc 121.1(5), Rep 81.3(5), Dev. 79.60 Sigma O3B -HG1 -O2A 4.556 1.555 6.565 PLAT_702 Alert A Angle Calc 64.4(2), Rep 108.4(4), Dev. 220.00 Sigma O1 -HG1 -O2A 1.555 1.555 6.565 PLAT_702 Alert A Angle Calc 22.2(3), Rep 51.5(5), Dev. 97.67 Sigma O3A -HG1 -O2A 6.565 1.555 6.565 PLAT_702 Alert A Angle Calc 139.75(8), Rep 94.57(19), Dev. 564.75 Sigma O1 -HG1 -S 5.555 1.555 1.565 PLAT_702 Alert A Angle Calc 60.2(2), Rep 22.8(5), Dev. 187.00 Sigma O3B -HG1 -S 6.565 1.555 1.565 PLAT_702 Alert A Angle Calc 63.8(2), Rep 25.6(4), Dev. 191.00 Sigma O3A -HG1 -S 6.565 1.555 1.565 PLAT_702 Alert A Angle Calc 42.4(2), Rep 26.5(3), Dev. 79.50 Sigma O2A -HG1 -S 6.565 1.555 1.565 PLAT_702 Alert A Angle Calc 34.81(7), Rep 33.07(17), Dev. 24.86 Sigma O1 -HG1 -HG2 5.555 1.555 1.455 PLAT_702 Alert A Angle Calc 82.8(2), Rep 130.5(5), Dev. 238.50 Sigma O3B -HG1 -HG2 6.565 1.555 1.455 PLAT_702 Alert A Angle Calc 80.2(2), Rep 138.1(4), Dev. 289.50 Sigma O3A -HG1 -HG2 6.565 1.555 1.455 PLAT_702 Alert A Angle Calc 92.7(3), Rep 102.0(3), Dev. 31.00 Sigma O2A -HG1 -HG2 6.565 1.555 1.455 PLAT_702 Alert A Angle Calc 38.3(2), Rep 171.3(3), Dev. 665.00 Sigma O1 -HG2 -O1 5.655 1.555 2.655 PLAT_702 Alert A Angle Calc 46.4(3), Rep 84.4(4), Dev. 126.67 Sigma O1 -HG2 -O2A 5.655 1.555 5.655 PLAT_702 Alert A Angle Calc 71.1(4), Rep 97.2(4), Dev. 65.25 Sigma O1 -HG2 -O2A 2.655 1.555 5.655 PLAT_702 Alert A Angle Calc 52.1(6), Rep 97.2(4), Dev. 75.17 Sigma O1 -HG2 -O2A 5.655 1.555 2.655 PLAT_702 Alert A Angle Calc 70.6(6), Rep 159.0(7), Dev. 147.33 Sigma O2A -HG2 -O2A 5.655 1.555 2.655 PLAT_702 Alert A Angle Calc 117.5(2), Rep 90.5(4), Dev. 135.00 Sigma O1 -HG2 -O3A 5.655 1.555 6.555 PLAT_702 Alert A Angle Calc 80.3(3), Rep 81.6(4), Dev. 4.33 Sigma O1 -HG2 -O3A 2.655 1.555 6.555 PLAT_702 Alert A Angle Calc 140.2(3), Rep 76.4(6), Dev. 212.67 Sigma O2A -HG2 -O3A 5.655 1.555 6.555 PLAT_702 Alert A Angle Calc 134.3(6), Rep 124.4(5), Dev. 16.50 Sigma O2A -HG2 -O3A 2.655 1.555 6.555 PLAT_702 Alert A Angle Calc 100.0(4), Rep 81.6(4), Dev. 46.00 Sigma O1 -HG2 -O3A 5.655 1.555 1.555 PLAT_702 Alert A Angle Calc 143.3(5), Rep 124.4(5), Dev. 37.80 Sigma O2A -HG2 -O3A 5.655 1.555 1.555 PLAT_702 Alert A Angle Calc 61.1(5), Rep 50.3(8), Dev. 21.60 Sigma O3A -HG2 -O3A 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 90.7(4), Rep 75.8(3), Dev. 37.25 Sigma O1 -HG2 -O2B 5.655 1.555 1.655 PLAT_702 Alert A Angle Calc 44.9(5), Rep 69.0(5), Dev. 48.20 Sigma O2A -HG2 -O2B 5.655 1.555 1.655 PLAT_702 Alert A Angle Calc 134.6(4), Rep 143.7(5), Dev. 22.75 Sigma O3A -HG2 -O2B 6.555 1.555 1.655 PLAT_702 Alert A Angle Calc 116.5(5), Rep 112.8(3), Dev. 7.40 Sigma O1 -HG2 -O2B 5.655 1.555 6.655 PLAT_702 Alert A Angle Calc 103.2(5), Rep 75.8(3), Dev. 54.80 Sigma O1 -HG2 -O2B 2.655 1.555 6.655 PLAT_702 Alert A Angle Calc 79.9(5), Rep 91.0(5), Dev. 22.20 Sigma O2A -HG2 -O2B 5.655 1.555 6.655 PLAT_702 Alert A Angle Calc 145.3(7), Rep 69.0(5), Dev. 109.00 Sigma O2A -HG2 -O2B 2.655 1.555 6.655 PLAT_702 Alert A Angle Calc 80.3(5), Rep 152.5(5), Dev. 144.40 Sigma O3A -HG2 -O2B 6.555 1.555 6.655 PLAT_702 Alert A Angle Calc 136.3(6), Rep 143.7(5), Dev. 12.33 Sigma O3A -HG2 -O2B 1.555 1.555 6.655 PLAT_702 Alert A Angle Calc 54.7(6), Rep 41.4(6), Dev. 22.17 Sigma O2B -HG2 -O2B 1.655 1.555 6.655 PLAT_702 Alert A Angle Calc 119.8(2), Rep 97.0(4), Dev. 114.00 Sigma O1 -HG2 -O3B 5.655 1.555 6.555 PLAT_702 Alert A Angle Calc 83.0(3), Rep 75.0(4), Dev. 26.67 Sigma O1 -HG2 -O3B 2.655 1.555 6.555 PLAT_702 Alert A Angle Calc 143.3(3), Rep 78.9(5), Dev. 214.67 Sigma O2A -HG2 -O3B 5.655 1.555 6.555 PLAT_702 Alert A Angle Calc 133.4(6), Rep 121.4(5), Dev. 20.00 Sigma O2A -HG2 -O3B 2.655 1.555 6.555 PLAT_702 Alert A Angle Calc 3.1(3), Rep 6.8(6), Dev. 12.33 Sigma O3A -HG2 -O3B 6.555 1.555 6.555 PLAT_702 Alert A Angle Calc 59.1(5), Rep 50.2(3), Dev. 17.80 Sigma O3A -HG2 -O3B 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 135.1(4), Rep 147.6(5), Dev. 31.25 Sigma O2B -HG2 -O3B 1.655 1.555 6.555 PLAT_702 Alert A Angle Calc 81.3(5), Rep 147.5(5), Dev. 132.40 Sigma O2B -HG2 -O3B 6.655 1.555 6.555 PLAT_702 Alert A Angle Calc 106.2(4), Rep 75.0(4), Dev. 78.00 Sigma O1 -HG2 -O3B 5.655 1.555 1.555 PLAT_702 Alert A Angle Calc 148.0(5), Rep 121.4(5), Dev. 53.20 Sigma O2A -HG2 -O3B 5.655 1.555 1.555 PLAT_702 Alert A Angle Calc 60.9(4), Rep 50.2(3), Dev. 26.75 Sigma O3A -HG2 -O3B 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 132.2(6), Rep 147.6(5), Dev. 25.67 Sigma O2B -HG2 -O3B 6.655 1.555 1.555 PLAT_702 Alert A Angle Calc 58.6(4), Rep 51.2(7), Dev. 18.50 Sigma O3B -HG2 -O3B 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 49.5(4), Rep 80.4(3), Dev. 77.25 Sigma O1 -HG2 -O2B 5.655 1.555 5.655 PLAT_702 Alert A Angle Calc 75.9(5), Rep 103.2(3), Dev. 54.60 Sigma O1 -HG2 -O2B 2.655 1.555 5.655 PLAT_702 Alert A Angle Calc 4.9(5), Rep 14.4(4), Dev. 19.00 Sigma O2A -HG2 -O2B 5.655 1.555 5.655 PLAT_702 Alert A Angle Calc 69.1(7), Rep 145.3(5), Dev. 108.86 Sigma O2A -HG2 -O2B 2.655 1.555 5.655 PLAT_702 Alert A Angle Calc 144.5(4), Rep 90.3(5), Dev. 135.50 Sigma O3A -HG2 -O2B 6.555 1.555 5.655 PLAT_702 Alert A Angle Calc 143.8(6), Rep 136.3(5), Dev. 12.50 Sigma O3A -HG2 -O2B 1.555 1.555 5.655 PLAT_702 Alert A Angle Calc 41.3(6), Rep 54.7(6), Dev. 22.33 Sigma O2B -HG2 -O2B 1.655 1.555 5.655 PLAT_702 Alert A Angle Calc 147.5(4), Rep 93.1(5), Dev. 136.00 Sigma O3B -HG2 -O2B 6.555 1.555 5.655 PLAT_702 Alert A Angle Calc 147.6(5), Rep 132.1(5), Dev. 31.00 Sigma O3B -HG2 -O2B 1.555 1.555 5.655 PLAT_702 Alert A Angle Calc 43.9(5), Rep 103.2(3), Dev. 118.60 Sigma O1 -HG2 -O2B 5.655 1.555 2.655 PLAT_702 Alert A Angle Calc 56.1(5), Rep 145.3(5), Dev. 178.40 Sigma O2A -HG2 -O2B 5.655 1.555 2.655 PLAT_702 Alert A Angle Calc 145.1(5), Rep 136.3(5), Dev. 17.60 Sigma O3A -HG2 -O2B 6.555 1.555 2.655 PLAT_702 Alert A Angle Calc 132.5(7), Rep 54.7(6), Dev. 111.14 Sigma O2B -HG2 -O2B 6.655 1.555 2.655 PLAT_702 Alert A Angle Calc 145.0(5), Rep 132.1(5), Dev. 25.80 Sigma O3B -HG2 -O2B 6.555 1.555 2.655 PLAT_702 Alert A Angle Calc 54.7(6), Rep 132.6(6), Dev. 129.83 Sigma O2B -HG2 -O2B 5.655 1.555 2.655 PLAT_702 Alert A Angle Calc 36.0(8), Rep 85.1(13), Dev. 61.37 Sigma O2B -S -O2B 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 51.2(7), Rep 111.1(11), Dev. 85.57 Sigma O2B -S -O3B 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 15.4(5), Rep 110.9(9), Dev. 191.00 Sigma O2B -S -O3B 6.555 1.555 6.555 PLAT_702 Alert A Angle Calc 146.1(9), Rep 111.1(11), Dev. 38.89 Sigma O2B -S -O3B 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 161.4(8), Rep 121.8(16), Dev. 49.50 Sigma O3B -S -O3B 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 55.6(7), Rep 110.0(10), Dev. 77.71 Sigma O2B -S -O3A 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 19.8(5), Rep 128.3(9), Dev. 217.00 Sigma O2B -S -O3A 6.555 1.555 6.555 PLAT_702 Alert A Angle Calc 4.4(4), Rep 17.4(9), Dev. 32.50 Sigma O3B -S -O3A 6.555 1.555 6.555 PLAT_702 Alert A Angle Calc 165.6(8), Rep 108.6(9), Dev. 71.25 Sigma O3B -S -O3A 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 162.8(8), Rep 110.0(10), Dev. 66.00 Sigma O2B -S -O3A 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 174.8(8), Rep 108.6(9), Dev. 82.75 Sigma O3B -S -O3A 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 173.4(9), Rep 98.5(14), Dev. 83.22 Sigma O3A -S -O3A 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 55.6(8), Rep 113.7(11), Dev. 72.62 Sigma O2B -S -O2A 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 70.0(8), Rep 106.0(9), Dev. 45.00 Sigma O3B -S -O2A 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 74.0(7), Rep 96.5(10), Dev. 32.14 Sigma O3A -S -O2A 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 36.7(8), Rep 113.7(11), Dev. 96.25 Sigma O2B -S -O2A 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 9.3(5), Rep 29.9(8), Dev. 41.20 Sigma O2B -S -O2A 6.555 1.555 6.555 PLAT_702 Alert A Angle Calc 16.7(4), Rep 91.8(10), Dev. 187.75 Sigma O3B -S -O2A 6.555 1.555 6.555 PLAT_702 Alert A Angle Calc 147.2(9), Rep 106.0(9), Dev. 45.78 Sigma O3B -S -O2A 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 20.7(4), Rep 107.4(10), Dev. 216.75 Sigma O3A -S -O2A 6.555 1.555 6.555 PLAT_702 Alert A Angle Calc 164.5(8), Rep 96.5(10), Dev. 85.00 Sigma O3A -S -O2A 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 60.6(9), Rep 143.2(14), Dev. 91.78 Sigma O2A -S -O2A 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 132.4(3), Rep 137.5(7), Dev. 17.00 Sigma O2B -S -HG2 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 126.7(2), Rep 60.9(8), Dev. 329.00 Sigma O3B -S -HG2 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 124.1(2), Rep 49.3(7), Dev. 374.00 Sigma O3A -S -HG2 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 140.7(3), Rep 108.4(7), Dev. 107.67 Sigma O2A -S -HG2 6.555 1.555 1.555 PLAT_702 Alert A Angle Calc 47.0(8), Rep 83.5(6), Dev. 45.62 Sigma O2B -S -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 73.0(4), Rep 140.2(6), Dev. 168.00 Sigma O2B -S -HG1 6.555 1.555 6.665 PLAT_702 Alert A Angle Calc 86.8(3), Rep 108.8(7), Dev. 73.33 Sigma O3B -S -HG1 6.555 1.555 6.665 PLAT_702 Alert A Angle Calc 75.4(7), Rep 41.0(8), Dev. 49.14 Sigma O3B -S -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 90.5(2), Rep 91.4(6), Dev. 4.50 Sigma O3A -S -HG1 6.555 1.555 6.665 PLAT_702 Alert A Angle Calc 90.1(7), Rep 52.8(7), Dev. 53.29 Sigma O3A -S -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 18.0(8), Rep 56.3(7), Dev. 47.88 Sigma O2A -S -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 78.5(4), Rep 146.8(6), Dev. 170.75 Sigma O2A -S -HG1 6.555 1.555 6.665 PLAT_702 Alert A Angle Calc 93.26(3), Rep 63.56(6), Dev. 990.00 Sigma HG2 -S -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 104.2(4), Rep 83.5(6), Dev. 51.75 Sigma O2B -S -HG1 6.555 1.555 1.545 PLAT_702 Alert A Angle Calc 89.0(3), Rep 41.0(8), Dev. 160.00 Sigma O3B -S -HG1 6.555 1.555 1.545 PLAT_702 Alert A Angle Calc 84.5(3), Rep 52.8(7), Dev. 105.67 Sigma O3A -S -HG1 6.555 1.555 1.545 PLAT_702 Alert A Angle Calc 103.8(4), Rep 56.3(7), Dev. 118.75 Sigma O2A -S -HG1 6.555 1.555 1.545 PLAT_702 Alert A Angle Calc 146.73(6), Rep 127.13(13), Dev. 326.67 Sigma HG1 -S -HG1 6.665 1.555 1.545 PLAT_702 Alert A Angle Calc 47.6(3), Rep 42.5(7), Dev. 17.00 Sigma O2B -S -HG2 6.555 1.555 1.455 PLAT_702 Alert A Angle Calc 53.3(2), Rep 119.1(8), Dev. 329.00 Sigma O3B -S -HG2 6.555 1.555 1.455 PLAT_702 Alert A Angle Calc 55.9(2), Rep 130.7(7), Dev. 374.00 Sigma O3A -S -HG2 6.555 1.555 1.455 PLAT_702 Alert A Angle Calc 39.3(3), Rep 71.6(7), Dev. 107.67 Sigma O2A -S -HG2 6.555 1.555 1.455 PLAT_702 Alert A Angle Calc 86.74(3), Rep 116.44(6), Dev. 990.00 Sigma HG1 -S -HG2 6.665 1.555 1.455 PLAT_702 Alert A Angle Calc 66.14(15), Rep 112.9(2), Dev. 311.73 Sigma HG2 -O1 -HG1 3.664 1.555 5.555 PLAT_702 Alert A Angle Calc 171.9(2), Rep 113.8(3), Dev. 290.50 Sigma HG1 -O1 -HG1 3.564 1.555 5.555 PLAT_702 Alert A Angle Calc 65.93(11), Rep 102.8(2), Dev. 335.18 Sigma HG1 -O1 -HG1 5.555 1.555 1.555 PLAT_702 Alert A Angle Calc 130(2), Rep 151(2), Dev. 10.50 Sigma O2B -O2A -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 158.2(10), Rep 97.2(8), Dev. 61.00 Sigma S -O2A -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 51.1(3), Rep 83.5(5), Dev. 108.00 Sigma HG1 -O2A -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 57.8(3), Rep 101.3(6), Dev. 145.00 Sigma HG2 -O2A -HG1 3.664 1.555 6.665 PLAT_702 Alert A Angle Calc 113.7(4), Rep 142.1(5), Dev. 71.00 Sigma HG1 -O2A -HG2 6.665 1.555 1.455 PLAT_702 Alert A Angle Calc 109.1(3), Rep 106.6(5), Dev. 8.33 Sigma HG1 -O2A -HG1 6.665 1.555 3.554 PLAT_702 Alert A Angle Calc 110.2(4), Rep 58.1(3), Dev. 130.25 Sigma HG1 -O2A -HG2 6.665 1.555 1.555 PLAT_702 Alert A Angle Calc 46(2), Rep 23.0(17), Dev. 11.50 Sigma O2A -O2B -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 125.1(9), Rep 72.3(6), Dev. 58.67 Sigma S -O2B -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 39.3(3), Rep 69.1(4), Dev. 99.33 Sigma HG1 -O2B -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 113.5(5), Rep 143.7(5), Dev. 60.40 Sigma HG2 -O2B -HG1 1.455 1.555 6.665 PLAT_702 Alert A Angle Calc 49.3(3), Rep 81.1(4), Dev. 106.00 Sigma HG2 -O2B -HG1 3.664 1.555 6.665 PLAT_702 Alert A Angle Calc 106(2), Rep 143.6(18), Dev. 18.80 Sigma O2A -O2B -HG1 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 162.9(9), Rep 66.0(6), Dev. 107.67 Sigma S -O2B -HG1 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 64.9(4), Rep 138.1(6), Dev. 183.00 Sigma HG1 -O2B -HG1 1.555 1.555 6.555 PLAT_702 Alert A Angle Calc 62.6(4), Rep 58.4(3), Dev. 10.50 Sigma HG2 -O2B -HG1 1.455 1.555 6.555 PLAT_702 Alert A Angle Calc 57.2(3), Rep 124.6(5), Dev. 224.67 Sigma HG2 -O2B -HG1 3.664 1.555 6.555 PLAT_702 Alert A Angle Calc 65.0(2), Rep 137.5(4), Dev. 362.50 Sigma HG1 -O2B -HG1 6.665 1.555 6.555 PLAT_702 Alert A Angle Calc 144(2), Rep 105.8(18), Dev. 19.10 Sigma O2A -O2B -HG1 1.555 1.555 5.555 PLAT_702 Alert A Angle Calc 66.0(7), Rep 162.8(8), Dev. 138.29 Sigma S -O2B -HG1 1.555 1.555 5.555 PLAT_702 Alert A Angle Calc 138.1(7), Rep 64.9(3), Dev. 104.57 Sigma HG1 -O2B -HG1 1.555 1.555 5.555 PLAT_702 Alert A Angle Calc 58.5(3), Rep 62.6(3), Dev. 13.67 Sigma HG2 -O2B -HG1 1.455 1.555 5.555 PLAT_702 Alert A Angle Calc 124.7(5), Rep 57.3(3), Dev. 134.80 Sigma HG2 -O2B -HG1 3.664 1.555 5.555 PLAT_702 Alert A Angle Calc 168.3(5), Rep 119.2(4), Dev. 98.20 Sigma HG1 -O2B -HG1 6.665 1.555 5.555 PLAT_702 Alert A Angle Calc 32(4), Rep 48(5), Dev. 4.00 Sigma O3B -O3A -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 80.2(7), Rep 101.7(8), Dev. 30.71 Sigma S -O3A -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 104.5(4), Rep 91.3(6), Dev. 33.00 Sigma HG1 -O3A -HG1 4.556 1.555 6.665 PLAT_702 Alert A Angle Calc 96.7(4), Rep 82.4(6), Dev. 35.75 Sigma HG2 -O3A -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 142.1(5), Rep 151.0(6), Dev. 17.80 Sigma HG1 -O3A -HG2 6.665 1.555 2.545 PLAT_702 Alert A Angle Calc 132.4(4), Rep 138.0(6), Dev. 14.00 Sigma HG1 -O3A -HG1 6.665 1.555 1.545 PLAT_702 Alert A Angle Calc 154.0(5), Rep 130.7(6), Dev. 46.60 Sigma HG1 -O3A -HG1 6.665 1.555 2.655 PLAT_702 Alert A Angle Calc 36.61(18), Rep 57.5(3), Dev. 116.06 Sigma HG1 -O3A -HG1 6.665 1.555 1.555 PLAT_702 Alert A Angle Calc 146(4), Rep 124(5), Dev. 5.50 Sigma O3A -O3B -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 94.8(8), Rep 116.2(11), Dev. 26.75 Sigma S -O3B -HG1 1.555 1.555 6.665 PLAT_702 Alert A Angle Calc 113.7(5), Rep 97.2(6), Dev. 33.00 Sigma HG1 -O3B -HG1 6.665 1.555 4.556 PLAT_702 Alert A Angle Calc 101.8(4), Rep 81.4(6), Dev. 51.00 Sigma HG1 -O3B -HG2 6.665 1.555 1.555 PLAT_702 Alert A Angle Calc 38.9(2), Rep 66.2(4), Dev. 136.50 Sigma HG1 -O3B -HG1 6.665 1.555 1.555 PLAT_702 Alert A Angle Calc 150.2(5), Rep 159.2(7), Dev. 18.00 Sigma HG1 -O3B -HG2 6.665 1.555 2.545
Amber Alert Alert Level B:
PLAT_301 Alert B Main Residue Disorder ........................ 26.00 Perc. PLAT_702 Alert B Angle Calc 134.0(4), Rep 133.1(7), Dev. 2.25 Sigma HG1 -O3B -HG1 6.665 1.555 1.545
Yellow Alert Alert Level C:
PLAT_701 Alert C Bond Calc 4.05(2), Rep 4.026(16), Dev. 1.20 Sigma O2B -HG1 1.555 6.555 PLAT_701 Alert C Bond Calc 4.024(19), Rep 4.053(15), Dev. 1.53 Sigma O2B -HG1 1.555 5.555 General Notes
ABSTM_02 The ratio of expected to reported Tmax/Tmin(RR) is > 2.00 Tmin and Tmax reported: 0.030 0.458 Tmin and Tmax expected: 0.011 0.447 RR = 2.724 Please check that your absorption correction is appropriate. REFLT_03 From the CIF: _diffrn_reflns_theta_max 30.23 From the CIF: _reflns_number_total 845 Count of symmetry unique reflns 521 Completeness (_total/calc) 162.19% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 324 Fraction of Friedel pairs measured 0.622 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
196 Alert Level A = Potentially serious problem
2 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

Schuetteite is a naturally occurring supergene mercury mineral found as a weathering product of cinnabar, HgS (Bailey et al., 1959). In its synthetic form this basic mercury(II) sulfate has been described for the first time as `Turbithum (Turbethum) Minerale' by Paracelsus (Theophrast von Hohenheim; 1493–1541) and was applied as a laxative.

The crystal structure of Hg3(SO4)O2 was solved by Nagorsen et al. (1962). The authors reported the determined atomic coordinates to be provisional, because no absorption correction of the highly absorbing crystal (linear absorption coefficient µ ca 80 mm-1) had been applied to the measured intensity data. For a more detailed knowledge of the crystal chemistry of mercury–oxo compounds and an improvement of the structural data it seemed desirable to re-investigate the structure of schuetteite on the basis of modern intensity measurements and especially under consideration of an appropriate absorption correction. During this work the previously determined structure has in principle been confirmed. The most important result of the re-investigation is the information that the sulfate group is disordered which was not elaborated in the original study.

The structure consists of layers perpendicular to [001] (Fig. 1). The layers are composed of slightly corrugated hexagonal [Hg3O2]2+ nets with ¯d(Hg—O) = 2.092 Å and nearly linear (O—Hg—O) angles with a mean value of 170.5°. The Hg—O distances within the nets are considerably shorter than ¯d(Hg—O) = 2.712 Å to the O atoms of the disordered SO42- tetrahedra located inside the interstices of the nets and to SO42- groups of adjacent layers. The pronounced [2 + x] coordination with two short Hg—O bonds and an almost linear (O—Hg—O) angle is a frequently observed structure unit in the crystal chemistry of mercury(II)–oxo compounds (Aurivillius, 1965; Grdenić, 1965; Stålhandske, 1980; Müller-Buschbaum, 1995). The sulfate group is disordered around the twofold axis and is slightly distorted from the geometry of an ideal tetrahedron [¯d(S—O) = 1.482 Å, mean angle of 109.5°].

Experimental top

Single crystals of synthetic schuetteite were prepared by hydrothermal treatment of commercial HgSO4 (Merck, pA) in demineralized water (steel autoclave with teflon-lined tubes, filling degree 70%, 520 K, 10 d). The crystals obtained were canary yellow in colour and had an hexagonal plate-like habit with [001] as the main crystal face.

Refinement top

All crystals examined were systematically twinned. Under consideration of racemic twinning a twin ratio of ca 5:1 was determined for the measured crystal. During the last refinement cycles with Hg and S atoms refined anisotropically and O atoms isotropically, large displacement parameters for the O atoms of the sulfate group were observed [fractional coordinates and isotropic displacement parameters for this model: (O2) x = 0.178 (3), y = 0.155 (3), z = 0.2652 (16), Ueq = 0.074 Å2; (O3) x = 0.3948 (16), y = 0.1067 (19), z = 0.4325 (10), Ueq = 0.037 Å2]. This could not be explained by crystal chemical arguments or a possibly inappropriate absorption correction, since the latter is expected to be essentially correct (Rint before absorption correction = 0.34, Rint after correction = 0.06; no significant remaining electron density after convergence). Therefore, a split atom model with a disorder around the twofold axis was considered for the sulfate group with occupation factors constrained to 0.5 for the O atoms (the `free' occupation factors are close to this value) and the displacement parameters refined isotropically for O2A,B and O3A,B. The separation between the split O atoms is then 0.77 (2) (O2A—O2B) and 0.45 (2) Å (O3A—O3B). This model led to better R values and a better goodness-of-fit than the previous model without splitting of the sulfate O atoms.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS for Windows (Dowty, 1998); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. Part of an [Hg3O2]2+ net with disordered SO42- tetrahedra located inside the interstices in projection along [001] and displacement ellipsoids drawn at the 74% probability level. One orientation of the disordered sulfate group is given in white, the other in grey.
Trimercury(II) dioxide sulfate(VI) top
Crystal data top
Hg3SO4O2Dx = 8.450 Mg m3
Mr = 729.83Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3121Cell parameters from 2544 reflections
a = 7.0429 (5) Åθ = 6.7–59.8°
c = 10.0166 (7) ŵ = 80.41 mm1
V = 430.28 (5) Å3T = 293 K
Z = 3Trigonal plate, yellow
F(000) = 9120.10 × 0.06 × 0.01 mm
Data collection top
Siemens SMART
diffractometer
845 independent reflections
Radiation source: fine-focus sealed tube801 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.059
ω scansθmax = 30.2°, θmin = 3.3°
Absorption correction: numerical
The crystal shape was optimized by minimizing the internal R-value of selected reflections (I>20σ(I)) using the program HABITUS (Herrendorf, 1993-97). The habit so derived was used for the numerical absorption correction.
h = 99
Tmin = 0.030, Tmax = 0.458k = 99
4712 measured reflectionsl = 1214
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0266P)2 + 0.0858P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.021(Δ/σ)max < 0.001
wR(F2) = 0.051Δρmax = 1.96 e Å3
S = 1.04Δρmin = 1.81 e Å3
849 reflectionsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
45 parametersExtinction coefficient: 0.00086 (11)
0 restraintsAbsolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.16 (4)
Crystal data top
Hg3SO4O2Z = 3
Mr = 729.83Mo Kα radiation
Trigonal, P3121µ = 80.41 mm1
a = 7.0429 (5) ÅT = 293 K
c = 10.0166 (7) Å0.10 × 0.06 × 0.01 mm
V = 430.28 (5) Å3
Data collection top
Siemens SMART
diffractometer
845 independent reflections
Absorption correction: numerical
The crystal shape was optimized by minimizing the internal R-value of selected reflections (I>20σ(I)) using the program HABITUS (Herrendorf, 1993-97). The habit so derived was used for the numerical absorption correction.
801 reflections with I > 2σ(I)
Tmin = 0.030, Tmax = 0.458Rint = 0.059
4712 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0210 restraints
wR(F2) = 0.051Δρmax = 1.96 e Å3
S = 1.04Δρmin = 1.81 e Å3
849 reflectionsAbsolute structure: Flack (1983)
45 parametersAbsolute structure parameter: 0.16 (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)
Hg10.18904 (5)0.50427 (9)0.31516 (3)0.01543 (11)
Hg20.70266 (10)0.00000.33330.01503 (13)
S0.2231 (6)0.00000.33330.0180 (7)
O10.1553 (9)0.4840 (9)0.0490 (7)0.0169 (12)
O2A0.256 (3)0.202 (3)0.2578 (15)0.027 (2)*0.50
O2B0.133 (3)0.123 (3)0.2706 (16)0.027 (2)*0.50
O3A0.399 (3)0.076 (3)0.4362 (19)0.025 (2)*0.50
O3B0.391 (3)0.135 (3)0.431 (2)0.025 (2)*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Hg10.0116 (2)0.01295 (17)0.02007 (17)0.00489 (15)0.00111 (12)0.00063 (16)
Hg20.01365 (19)0.0100 (2)0.0202 (2)0.00502 (12)0.00068 (11)0.0014 (2)
S0.0183 (10)0.0179 (19)0.0178 (15)0.0089 (9)0.0005 (7)0.0011 (14)
O10.009 (3)0.007 (2)0.028 (3)0.001 (3)0.001 (2)0.001 (2)
Geometric parameters (Å, º) top
Hg1—O1i2.105 (6)S—O3A1.491 (19)
Hg1—O1ii2.123 (6)S—O2A1.523 (16)
Hg1—O2A2.467 (16)S—O2Aix1.523 (16)
Hg1—O3Biii2.473 (19)S—Hg1xii3.3828 (16)
Hg1—O2B2.548 (15)S—Hg1xiii3.3828 (16)
Hg1—O3Aiv2.607 (19)S—Hg2vi3.665 (5)
Hg1—O3Biv2.64 (2)O1—Hg2xiv2.070 (7)
Hg1—O12.674 (7)O1—Hg1xv2.105 (6)
Hg1—O3Aiii2.750 (18)O1—Hg1ii2.123 (6)
Hg1—O2Aiii2.836 (17)O2A—O2B0.77 (2)
Hg1—Sv3.3828 (16)O2A—Hg2xiv2.647 (15)
Hg1—Hg2vi3.4950 (4)O2A—Hg1xii2.836 (17)
Hg2—O1vii2.070 (7)O2A—Hg2vi3.497 (18)
Hg2—O1viii2.070 (7)O2A—Hg1xvi4.068 (16)
Hg2—O2Avii2.647 (15)O2B—Hg2vi2.775 (16)
Hg2—O2Aviii2.647 (15)O2B—Hg2xiv2.961 (17)
Hg2—O3Aix2.657 (18)O2B—Hg1xii3.528 (16)
Hg2—O3A2.657 (18)O2B—Hg1ix4.026 (16)
Hg2—O2Bx2.775 (16)O2B—Hg1ii4.053 (15)
Hg2—O2Bxi2.775 (16)O3A—O3B0.45 (2)
Hg2—O3Bix2.96 (2)O3A—Hg1iv2.607 (19)
Hg2—O3B2.96 (2)O3A—Hg1xii2.750 (18)
Hg2—O2Bvii2.961 (17)O3A—Hg2xvii3.571 (19)
Hg2—O2Bviii2.961 (17)O3A—Hg1xiii3.729 (17)
S—O2B1.451 (15)O3A—Hg1viii3.801 (17)
S—O2Bix1.451 (15)O3B—Hg1xii2.473 (19)
S—O3Bix1.461 (19)O3B—Hg1iv2.64 (2)
S—O3B1.461 (19)O3B—Hg2xvii3.75 (2)
S—O3Aix1.491 (19)O3B—Hg1xiii4.094 (17)
O1i—Hg1—O1ii169.72 (6)O3Bix—S—Hg260.9 (8)
O1i—Hg1—O2A86.0 (5)O3B—S—Hg260.9 (8)
O1ii—Hg1—O2A96.8 (5)O3Aix—S—Hg249.3 (7)
O1i—Hg1—O3Biii86.2 (5)O3A—S—Hg249.3 (7)
O1ii—Hg1—O3Biii97.4 (5)O2A—S—Hg2108.4 (7)
O2A—Hg1—O3Biii142.3 (6)O2Aix—S—Hg2108.4 (7)
O1i—Hg1—O2B101.2 (4)O2B—S—Hg1xii83.5 (6)
O1ii—Hg1—O2B80.3 (4)O2Bix—S—Hg1xii140.2 (6)
O2A—Hg1—O2B17.5 (5)O3Bix—S—Hg1xii108.8 (7)
O3Biii—Hg1—O2B151.1 (6)O3B—S—Hg1xii41.0 (8)
O1i—Hg1—O3Aiv87.0 (4)O3Aix—S—Hg1xii91.4 (6)
O1ii—Hg1—O3Aiv82.8 (4)O3A—S—Hg1xii52.8 (7)
O2A—Hg1—O3Aiv98.1 (6)O2A—S—Hg1xii56.3 (7)
O3Biii—Hg1—O3Aiv118.3 (7)O2Aix—S—Hg1xii146.8 (6)
O2B—Hg1—O3Aiv90.2 (6)Hg2—S—Hg1xii63.56 (6)
O1i—Hg1—O3Biv79.2 (4)O2B—S—Hg1xiii140.2 (6)
O1ii—Hg1—O3Biv90.8 (4)O2Bix—S—Hg1xiii83.5 (6)
O2A—Hg1—O3Biv91.5 (6)O3Bix—S—Hg1xiii41.0 (8)
O3Biii—Hg1—O3Biv123.0 (6)O3B—S—Hg1xiii108.8 (7)
O2B—Hg1—O3Biv85.9 (6)O3Aix—S—Hg1xiii52.8 (7)
O3Aiv—Hg1—O3Biv9.8 (5)O3A—S—Hg1xiii91.4 (6)
O1i—Hg1—O1113.1 (2)O2A—S—Hg1xiii146.8 (6)
O1ii—Hg1—O177.2 (2)O2Aix—S—Hg1xiii56.3 (7)
O2A—Hg1—O176.8 (4)Hg2—S—Hg1xiii63.56 (6)
O3Biii—Hg1—O172.6 (5)Hg1xii—S—Hg1xiii127.13 (13)
O2B—Hg1—O178.8 (4)O2B—S—Hg2vi42.5 (7)
O3Aiv—Hg1—O1158.6 (4)O2Bix—S—Hg2vi42.5 (7)
O3Biv—Hg1—O1161.9 (5)O3Bix—S—Hg2vi119.1 (8)
O1i—Hg1—O3Aiii78.8 (4)O3B—S—Hg2vi119.1 (8)
O1ii—Hg1—O3Aiii105.1 (4)O3Aix—S—Hg2vi130.7 (7)
O2A—Hg1—O3Aiii138.2 (6)O3A—S—Hg2vi130.7 (7)
O3Biii—Hg1—O3Aiii7.7 (7)O2A—S—Hg2vi71.6 (7)
O2B—Hg1—O3Aiii150.1 (5)O2Aix—S—Hg2vi71.6 (7)
O3Aiv—Hg1—O3Aiii119.5 (5)Hg2—S—Hg2vi180.0
O3Biv—Hg1—O3Aiii122.8 (6)Hg1xii—S—Hg2vi116.44 (6)
O1—Hg1—O3Aiii73.9 (4)Hg1xiii—S—Hg2vi116.44 (6)
O1i—Hg1—O2Aiii99.2 (4)Hg2xiv—O1—Hg1xv117.0 (3)
O1ii—Hg1—O2Aiii76.7 (4)Hg2xiv—O1—Hg1ii112.9 (2)
O2A—Hg1—O2Aiii170.2 (4)Hg1xv—O1—Hg1ii113.8 (3)
O3Biii—Hg1—O2Aiii47.0 (6)Hg2xiv—O1—Hg1102.2 (3)
O2B—Hg1—O2Aiii153.5 (5)Hg1xv—O1—Hg1106.0 (2)
O3Aiv—Hg1—O2Aiii74.0 (5)Hg1ii—O1—Hg1102.8 (2)
O3Biv—Hg1—O2Aiii81.3 (5)O2B—O2A—S69.9 (17)
O1—Hg1—O2Aiii108.4 (4)O2B—O2A—Hg187.1 (18)
O3Aiii—Hg1—O2Aiii51.5 (5)S—O2A—Hg1133.2 (9)
O1i—Hg1—Sv85.0 (2)O2B—O2A—Hg2xiv107 (2)
O1ii—Hg1—Sv94.57 (19)S—O2A—Hg2xiv131.9 (9)
O2A—Hg1—Sv163.3 (4)Hg1—O2A—Hg2xiv93.0 (5)
O3Biii—Hg1—Sv22.8 (5)O2B—O2A—Hg1xii151 (2)
O2B—Hg1—Sv171.8 (4)S—O2A—Hg1xii97.2 (8)
O3Aiv—Hg1—Sv95.5 (4)Hg1—O2A—Hg1xii83.5 (5)
O3Biv—Hg1—Sv100.6 (5)Hg2xiv—O2A—Hg1xii101.3 (6)
O1—Hg1—Sv93.85 (14)O2B—O2A—Hg2vi17.9 (15)
O3Aiii—Hg1—Sv25.6 (4)S—O2A—Hg2vi84.0 (7)
O2Aiii—Hg1—Sv26.5 (3)Hg1—O2A—Hg2vi69.3 (4)
O1i—Hg1—Hg2vi142.53 (19)Hg2xiv—O2A—Hg2vi105.9 (5)
O1ii—Hg1—Hg2vi33.07 (17)Hg1xii—O2A—Hg2vi142.1 (5)
O2A—Hg1—Hg2vi69.4 (4)O2B—O2A—Hg1xvi95.0 (18)
O3Biii—Hg1—Hg2vi130.5 (5)S—O2A—Hg1xvi74.0 (6)
O2B—Hg1—Hg2vi51.8 (4)Hg1—O2A—Hg1xvi150.6 (6)
O3Aiv—Hg1—Hg2vi69.9 (4)Hg2xiv—O2A—Hg1xvi58.2 (3)
O3Biv—Hg1—Hg2vi73.9 (4)Hg1xii—O2A—Hg1xvi106.6 (5)
O1—Hg1—Hg2vi88.96 (10)Hg2vi—O2A—Hg1xvi110.0 (4)
O3Aiii—Hg1—Hg2vi138.1 (4)O2B—O2A—Hg2120.0 (18)
O2Aiii—Hg1—Hg2vi102.0 (3)S—O2A—Hg251.1 (6)
Sv—Hg1—Hg2vi125.01 (6)Hg1—O2A—Hg2139.7 (6)
O1vii—Hg2—O1viii171.3 (3)Hg2xiv—O2A—Hg2105.1 (5)
O1vii—Hg2—O2Avii84.4 (4)Hg1xii—O2A—Hg258.1 (3)
O1viii—Hg2—O2Avii97.2 (4)Hg2vi—O2A—Hg2135.1 (4)
O1vii—Hg2—O2Aviii97.2 (4)Hg1xvi—O2A—Hg262.4 (2)
O1viii—Hg2—O2Aviii84.4 (4)O2A—O2B—S80.3 (18)
O2Avii—Hg2—O2Aviii159.0 (7)O2A—O2B—Hg175.3 (17)
O1vii—Hg2—O3Aix90.5 (4)S—O2B—Hg1132.1 (9)
O1viii—Hg2—O3Aix81.6 (4)O2A—O2B—Hg2vi157.3 (19)
O2Avii—Hg2—O3Aix76.4 (6)S—O2B—Hg2vi116.8 (9)
O2Aviii—Hg2—O3Aix124.4 (5)Hg1—O2B—Hg2vi82.0 (4)
O1vii—Hg2—O3A81.6 (4)O2A—O2B—Hg2xiv58.9 (17)
O1viii—Hg2—O3A90.5 (4)S—O2B—Hg2xiv116.5 (8)
O2Avii—Hg2—O3A124.4 (5)Hg1—O2B—Hg2xiv84.4 (4)
O2Aviii—Hg2—O3A76.4 (6)Hg2vi—O2B—Hg2xiv118.5 (5)
O3Aix—Hg2—O3A50.3 (8)O2A—O2B—Hg1xii23.0 (17)
O1vii—Hg2—O2Bx75.8 (3)S—O2B—Hg1xii72.3 (6)
O1viii—Hg2—O2Bx112.8 (3)Hg1—O2B—Hg1xii69.1 (4)
O2Avii—Hg2—O2Bx69.0 (5)Hg2vi—O2B—Hg1xii143.7 (5)
O2Aviii—Hg2—O2Bx91.0 (5)Hg2xiv—O2B—Hg1xii81.1 (4)
O3Aix—Hg2—O2Bx143.7 (5)O2A—O2B—Hg1ix143.6 (18)
O3A—Hg2—O2Bx152.5 (5)S—O2B—Hg1ix66.0 (6)
O1vii—Hg2—O2Bxi112.8 (3)Hg1—O2B—Hg1ix138.1 (6)
O1viii—Hg2—O2Bxi75.8 (3)Hg2vi—O2B—Hg1ix58.4 (3)
O2Avii—Hg2—O2Bxi91.0 (5)Hg2xiv—O2B—Hg1ix124.6 (5)
O2Aviii—Hg2—O2Bxi69.0 (5)Hg1xii—O2B—Hg1ix137.5 (4)
O3Aix—Hg2—O2Bxi152.5 (5)O2A—O2B—Hg1ii105.8 (18)
O3A—Hg2—O2Bxi143.7 (5)S—O2B—Hg1ii162.8 (8)
O2Bx—Hg2—O2Bxi41.4 (6)Hg1—O2B—Hg1ii64.9 (3)
O1vii—Hg2—O3Bix97.0 (4)Hg2vi—O2B—Hg1ii62.6 (3)
O1viii—Hg2—O3Bix75.0 (4)Hg2xiv—O2B—Hg1ii57.3 (3)
O2Avii—Hg2—O3Bix78.9 (5)Hg1xii—O2B—Hg1ii119.2 (4)
O2Aviii—Hg2—O3Bix121.4 (5)Hg1ix—O2B—Hg1ii103.3 (4)
O3Aix—Hg2—O3Bix6.8 (6)O3B—O3A—S78 (4)
O3A—Hg2—O3Bix50.2 (3)O3B—O3A—Hg1iv89 (4)
O2Bx—Hg2—O3Bix147.6 (5)S—O3A—Hg1iv145.9 (11)
O2Bxi—Hg2—O3Bix147.5 (5)O3B—O3A—Hg2129 (5)
O1vii—Hg2—O3B75.0 (4)S—O3A—Hg2105.6 (9)
O1viii—Hg2—O3B97.0 (4)Hg1iv—O3A—Hg2107.3 (7)
O2Avii—Hg2—O3B121.4 (5)O3B—O3A—Hg1xii48 (5)
O2Aviii—Hg2—O3B78.9 (5)S—O3A—Hg1xii101.7 (8)
O3Aix—Hg2—O3B50.2 (3)Hg1iv—O3A—Hg1xii91.3 (6)
O3A—Hg2—O3B6.8 (6)Hg2—O3A—Hg1xii82.4 (6)
O2Bx—Hg2—O3B147.5 (5)O3B—O3A—Hg2xvii110 (5)
O2Bxi—Hg2—O3B147.6 (5)S—O3A—Hg2xvii88.6 (8)
O3Bix—Hg2—O3B51.2 (7)Hg1iv—O3A—Hg2xvii66.8 (4)
O1vii—Hg2—O2Bvii80.4 (3)Hg2—O3A—Hg2xvii121.3 (5)
O1viii—Hg2—O2Bvii103.2 (3)Hg1xii—O3A—Hg2xvii151.0 (6)
O2Avii—Hg2—O2Bvii14.4 (4)O3B—O3A—Hg1xiii143 (5)
O2Aviii—Hg2—O2Bvii145.3 (5)S—O3A—Hg1xiii65.1 (6)
O3Aix—Hg2—O2Bvii90.3 (5)Hg1iv—O3A—Hg1xiii122.6 (6)
O3A—Hg2—O2Bvii136.3 (5)Hg2—O3A—Hg1xiii65.3 (3)
O2Bx—Hg2—O2Bvii54.7 (6)Hg1xii—O3A—Hg1xiii138.0 (6)
O2Bxi—Hg2—O2Bvii80.0 (3)Hg2xvii—O3A—Hg1xiii71.0 (3)
O3Bix—Hg2—O2Bvii93.1 (5)O3B—O3A—Hg1viii152 (5)
O3B—Hg2—O2Bvii132.1 (5)S—O3A—Hg1viii123.0 (8)
O1vii—Hg2—O2Bviii103.2 (3)Hg1iv—O3A—Hg1viii63.9 (4)
O1viii—Hg2—O2Bviii80.4 (3)Hg2—O3A—Hg1viii67.5 (3)
O2Avii—Hg2—O2Bviii145.3 (5)Hg1xii—O3A—Hg1viii130.7 (6)
O2Aviii—Hg2—O2Bviii14.4 (4)Hg2xvii—O3A—Hg1viii57.7 (3)
O3Aix—Hg2—O2Bviii136.3 (5)Hg1xiii—O3A—Hg1viii61.2 (2)
O3A—Hg2—O2Bviii90.3 (5)O3B—O3A—Hg116 (4)
O2Bx—Hg2—O2Bviii80.0 (3)S—O3A—Hg161.5 (6)
O2Bxi—Hg2—O2Bviii54.7 (6)Hg1iv—O3A—Hg1101.9 (5)
O3Bix—Hg2—O2Bviii132.1 (5)Hg2—O3A—Hg1130.4 (6)
O3B—Hg2—O2Bviii93.1 (5)Hg1xii—O3A—Hg157.5 (3)
O2Bvii—Hg2—O2Bviii132.6 (6)Hg2xvii—O3A—Hg1106.8 (4)
O2B—S—O2Bix85.1 (13)Hg1xiii—O3A—Hg1126.6 (5)
O2B—S—O3Bix111.1 (11)Hg1viii—O3A—Hg1161.5 (5)
O2Bix—S—O3Bix110.9 (9)O3A—O3B—S85 (4)
O2B—S—O3B110.9 (9)O3A—O3B—Hg1xii124 (5)
O2Bix—S—O3B111.1 (11)S—O3B—Hg1xii116.2 (11)
O3Bix—S—O3B121.8 (16)O3A—O3B—Hg1iv82 (4)
O2B—S—O3Aix110.0 (10)S—O3B—Hg1iv145.9 (12)
O2Bix—S—O3Aix128.3 (9)Hg1xii—O3B—Hg1iv97.2 (6)
O3Bix—S—O3Aix17.4 (9)O3A—O3B—Hg245 (5)
O3B—S—O3Aix108.6 (9)S—O3B—Hg293.5 (8)
O2B—S—O3A128.3 (9)Hg1xii—O3B—Hg281.4 (6)
O2Bix—S—O3A110.0 (10)Hg1iv—O3B—Hg298.5 (6)
O3Bix—S—O3A108.6 (9)O3A—O3B—Hg1162 (5)
O3B—S—O3A17.4 (9)S—O3B—Hg177.0 (8)
O3Aix—S—O3A98.5 (14)Hg1xii—O3B—Hg166.2 (4)
O2B—S—O2A29.9 (8)Hg1iv—O3B—Hg1113.1 (6)
O2Bix—S—O2A113.7 (11)Hg2—O3B—Hg1136.5 (7)
O3Bix—S—O2A106.0 (9)O3A—O3B—Hg2xvii64 (5)
O3B—S—O2A91.8 (10)S—O3B—Hg2xvii82.3 (8)
O3Aix—S—O2A96.5 (10)Hg1xii—O3B—Hg2xvii159.2 (7)
O3A—S—O2A107.4 (10)Hg1iv—O3B—Hg2xvii63.6 (4)
O2B—S—O2Aix113.7 (11)Hg2—O3B—Hg2xvii108.1 (5)
O2Bix—S—O2Aix29.9 (8)Hg1—O3B—Hg2xvii112.4 (5)
O3Bix—S—O2Aix91.8 (10)O3A—O3B—Hg1xiii34 (4)
O3B—S—O2Aix106.0 (9)S—O3B—Hg1xiii51.5 (6)
O3Aix—S—O2Aix107.4 (10)Hg1xii—O3B—Hg1xiii133.1 (7)
O3A—S—O2Aix96.5 (10)Hg1iv—O3B—Hg1xiii110.3 (5)
O2A—S—O2Aix143.2 (14)Hg2—O3B—Hg1xiii58.0 (3)
O2B—S—Hg2137.5 (7)Hg1—O3B—Hg1xiii128.5 (5)
O2Bix—S—Hg2137.5 (7)Hg2xvii—O3B—Hg1xiii65.3 (3)
Symmetry codes: (i) y+1, xy+1, z+1/3; (ii) xy, y, z+2/3; (iii) x, x+y+1, z+1/3; (iv) y, x, z+1; (v) x, y+1, z; (vi) x1, y, z; (vii) xy+1, y, z+2/3; (viii) y+1, xy, z+1/3; (ix) x, x+y, z+1/3; (x) x+1, y, z; (xi) x+1, x+y, z+1/3; (xii) x+1, x+y+1, z+1/3; (xiii) x, y1, z; (xiv) x+y+1, x+1, z1/3; (xv) x+y, x+1, z1/3; (xvi) x+y, x, z1/3; (xvii) y, xy1, z+1/3.

Experimental details

Crystal data
Chemical formulaHg3SO4O2
Mr729.83
Crystal system, space groupTrigonal, P3121
Temperature (K)293
a, c (Å)7.0429 (5), 10.0166 (7)
V3)430.28 (5)
Z3
Radiation typeMo Kα
µ (mm1)80.41
Crystal size (mm)0.10 × 0.06 × 0.01
Data collection
DiffractometerSiemens SMART
diffractometer
Absorption correctionNumerical
The crystal shape was optimized by minimizing the internal R-value of selected reflections (I>20σ(I)) using the program HABITUS (Herrendorf, 1993-97). The habit so derived was used for the numerical absorption correction.
Tmin, Tmax0.030, 0.458
No. of measured, independent and
observed [I > 2σ(I)] reflections
4712, 845, 801
Rint0.059
(sin θ/λ)max1)0.708
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.021, 0.051, 1.04
No. of reflections849
No. of parameters45
Δρmax, Δρmin (e Å3)1.96, 1.81
Absolute structureFlack (1983)
Absolute structure parameter0.16 (4)

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ATOMS for Windows (Dowty, 1998), SHELXL97.

Selected geometric parameters (Å, º) top
Hg1—O1i2.105 (6)Hg2—O2Avi2.647 (15)
Hg1—O1ii2.123 (6)Hg2—O3Avii2.657 (18)
Hg1—O2A2.467 (16)Hg2—O3A2.657 (18)
Hg1—O3Biii2.473 (19)Hg2—O2Bviii2.775 (16)
Hg1—O2B2.548 (15)Hg2—O2Bix2.775 (16)
Hg1—O3Aiv2.607 (19)Hg2—O3Bvii2.96 (2)
Hg1—O3Biv2.64 (2)Hg2—O3B2.96 (2)
Hg1—O12.674 (7)Hg2—O2Bv2.961 (17)
Hg1—O3Aiii2.750 (18)Hg2—O2Bvi2.961 (17)
Hg1—O2Aiii2.836 (17)S—O2B1.451 (15)
Hg2—O1v2.070 (7)S—O3B1.461 (19)
Hg2—O1vi2.070 (7)S—O3Avii1.491 (19)
Hg2—O2Av2.647 (15)S—O2Avii1.523 (16)
O1i—Hg1—O1ii169.72 (6)O3B—S—O3Avii108.6 (9)
O1v—Hg2—O1vi171.3 (3)O2Bvii—S—O2A113.7 (11)
O2Bvii—S—O3B111.1 (11)O3Bvii—S—O2A106.0 (9)
O2B—S—O3Avii110.0 (10)O3A—S—O2A107.4 (10)
Symmetry codes: (i) y+1, xy+1, z+1/3; (ii) xy, y, z+2/3; (iii) x, x+y+1, z+1/3; (iv) y, x, z+1; (v) xy+1, y, z+2/3; (vi) y+1, xy, z+1/3; (vii) x, x+y, z+1/3; (viii) x+1, y, z; (ix) x+1, x+y, z+1/3.
 

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