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The title compound, trimercury(II) bis[selenite(IV)] selenate(VI), contains three crystallographically inequivalent Hg
II cations with coordination numbers of eight (denoted Hg1 and Hg2) and five (denoted Hg3). The corresponding coordination polyhedra around the metal atoms might be described as intermediates between a square antiprism and a triangulated dodecahedron for both Hg1 and Hg2, and a strongly distorted truncated octahedron for Hg3.
[HgO
8/2] layers of edge-sharing [HgO
8] polyhedra propagate parallel to the
bc plane, and are connected
via Se
VIO
4 tetrahedra and [Hg3O
5] polyhedra along the
a axis, forming an arrangement with channels propagating parallel to the
b axis. The two independent Se
IVO
3 pyramids bridge the Hg atoms, and the non-bonding orbitals of the Se
IV ions protrude into the channels from opposite sides.
Supporting information
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 (Dowty, 1998); software used to prepare material for publication: SHELXL97.
Trimercury(II) {bis[selenite(IV)] selenate(VI)}]
top
Crystal data top
Hg3Se3O10 | F(000) = 844 |
Mr = 998.65 | Dx = 7.002 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.3979 (9) Å | Cell parameters from 981 reflections |
b = 5.3327 (6) Å | θ = 5.3–59.7° |
c = 11.1482 (12) Å | µ = 60.07 mm−1 |
β = 108.422 (2)° | T = 293 K |
V = 473.67 (9) Å3 | Fragment, colourless |
Z = 2 | 0.18 × 0.07 × 0.04 mm |
Data collection top
Siemens SMART CCD area-detector diffractometer | 2684 independent reflections |
Radiation source: fine-focus sealed tube | 2435 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.060 |
ω scans | θmax = 30.3°, θmin = 1.9° |
Absorption correction: numerical (HABITUS; Herrendorf, 1993-97) | h = −11→11 |
Tmin = 0.064, Tmax = 0.446 | k = −7→7 |
6813 measured reflections | l = −15→15 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.025P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.027 | (Δ/σ)max = 0.001 |
wR(F2) = 0.060 | Δρmax = 1.98 e Å−3 |
S = 1.02 | Δρmin = −1.51 e Å−3 |
2684 reflections | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
146 parameters | Extinction coefficient: 0.0090 (3) |
1 restraint | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.015 (11) |
Special details top
Experimental. 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. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Hg1 | 0.00338 (3) | 0.24647 (10) | 0.12945 (3) | 0.01513 (9) | |
Hg2 | 0.00612 (4) | 0.25889 (11) | 0.62586 (3) | 0.01722 (9) | |
Hg3 | 0.37438 (4) | 0.74340 (19) | 0.20835 (3) | 0.02385 (10) | |
Se1 | 0.26005 (9) | 0.2248 (3) | 0.96051 (7) | 0.01227 (17) | |
Se2 | 0.26538 (10) | 0.2866 (2) | 0.42224 (8) | 0.0120 (2) | |
Se3 | 0.64667 (9) | 0.2506 (4) | 0.28524 (7) | 0.01271 (15) | |
O1 | 0.1017 (8) | 0.1229 (12) | 0.8322 (6) | 0.0187 (14) | |
O2 | 0.1144 (9) | 0.4039 (12) | 0.4812 (7) | 0.0191 (14) | |
O3 | 0.1562 (8) | 0.0649 (12) | 0.3169 (6) | 0.0176 (14) | |
O4 | 0.1604 (9) | 0.4619 (11) | 0.0134 (7) | 0.0159 (14) | |
O5 | 0.2287 (9) | 0.0004 (13) | 0.0601 (7) | 0.0242 (17) | |
O6 | 0.2451 (10) | 0.5265 (14) | 0.3179 (8) | 0.0293 (18) | |
O7 | 0.5236 (8) | 0.0632 (12) | 0.3330 (6) | 0.0197 (14) | |
O8 | 0.5272 (9) | 0.4256 (13) | 0.1660 (6) | 0.0214 (14) | |
O9 | 0.7470 (9) | 0.4314 (13) | 0.4004 (7) | 0.0238 (15) | |
O10 | 0.7704 (9) | 0.0820 (12) | 0.2280 (6) | 0.0227 (15) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Hg1 | 0.01823 (15) | 0.01396 (19) | 0.01333 (14) | 0.0008 (2) | 0.00517 (11) | 0.0000 (2) |
Hg2 | 0.02466 (17) | 0.01580 (19) | 0.01375 (14) | −0.0026 (2) | 0.00971 (12) | −0.00090 (18) |
Hg3 | 0.02511 (18) | 0.01728 (17) | 0.02787 (18) | 0.0001 (3) | 0.00653 (13) | 0.0091 (2) |
Se1 | 0.0129 (3) | 0.0120 (4) | 0.0121 (3) | −0.0011 (4) | 0.0044 (3) | −0.0010 (4) |
Se2 | 0.0118 (4) | 0.0130 (5) | 0.0108 (3) | −0.0005 (3) | 0.0032 (3) | 0.0002 (3) |
Se3 | 0.0115 (3) | 0.0140 (4) | 0.0127 (3) | −0.0004 (6) | 0.0039 (3) | −0.0023 (4) |
O1 | 0.023 (3) | 0.020 (3) | 0.010 (3) | −0.009 (3) | 0.003 (3) | −0.001 (2) |
O2 | 0.021 (4) | 0.022 (3) | 0.019 (3) | 0.009 (3) | 0.015 (3) | 0.007 (3) |
O3 | 0.019 (3) | 0.017 (3) | 0.014 (3) | −0.004 (3) | 0.002 (3) | −0.004 (3) |
O4 | 0.023 (4) | 0.011 (3) | 0.019 (4) | 0.008 (3) | 0.014 (3) | 0.002 (2) |
O5 | 0.021 (4) | 0.022 (4) | 0.024 (4) | 0.004 (3) | −0.001 (3) | 0.007 (3) |
O6 | 0.030 (4) | 0.024 (3) | 0.041 (5) | 0.004 (3) | 0.022 (4) | 0.019 (3) |
O7 | 0.021 (3) | 0.021 (3) | 0.022 (4) | −0.004 (3) | 0.012 (3) | 0.002 (3) |
O8 | 0.019 (4) | 0.028 (4) | 0.016 (3) | 0.004 (3) | 0.004 (3) | 0.007 (3) |
O9 | 0.026 (4) | 0.021 (3) | 0.023 (4) | −0.007 (3) | 0.005 (3) | −0.011 (3) |
O10 | 0.027 (4) | 0.022 (3) | 0.023 (4) | 0.001 (3) | 0.014 (3) | −0.010 (3) |
Geometric parameters (Å, º) top
Hg1—O1i | 2.287 (6) | Se2—O6 | 1.702 (7) |
Hg1—O3 | 2.293 (7) | Se2—O3 | 1.714 (6) |
Hg1—O4ii | 2.312 (7) | Se2—O2 | 1.719 (6) |
Hg1—O4 | 2.411 (7) | Se3—O9 | 1.613 (7) |
Hg1—O5 | 2.612 (8) | Se3—O7 | 1.643 (6) |
Hg1—O10iii | 2.677 (7) | Se3—O10 | 1.647 (6) |
Hg1—O5iv | 2.738 (8) | Se3—O8 | 1.674 (7) |
Hg1—O6 | 2.840 (9) | O1—Hg1vi | 2.287 (6) |
Hg1—Se1v | 3.2821 (8) | O1—Hg1i | 3.501 (6) |
Hg1—Se2 | 3.3169 (9) | O1—Hg1xi | 3.718 (6) |
Hg2—O2 | 2.226 (6) | O1—Hg3vi | 3.931 (7) |
Hg2—O2vi | 2.295 (7) | O2—Hg2i | 2.295 (7) |
Hg2—O1 | 2.301 (6) | O2—Hg2vi | 3.676 (7) |
Hg2—O3i | 2.340 (6) | O3—Hg2vi | 2.340 (6) |
Hg2—O10vii | 2.686 (7) | O3—Hg3xii | 3.027 (6) |
Hg2—O6vi | 2.686 (8) | O3—Hg2i | 4.063 (7) |
Hg2—O9viii | 2.796 (7) | O4—Se1v | 1.720 (6) |
Hg2—O9iii | 2.906 (8) | O4—Hg1iv | 2.312 (7) |
Hg2—Se2vi | 3.3252 (15) | O5—Se1v | 1.709 (7) |
Hg2—Se2i | 3.5542 (15) | O5—Hg3xii | 2.197 (7) |
Hg3—O5ix | 2.197 (7) | O5—Hg1ii | 2.738 (8) |
Hg3—O6 | 2.201 (7) | O6—Hg2i | 2.686 (7) |
Hg3—O8 | 2.263 (7) | O7—Hg3xii | 2.304 (7) |
Hg3—O7ix | 2.304 (7) | O7—Hg2viii | 4.159 (7) |
Hg3—O4 | 2.782 (7) | O8—Hg3xii | 3.935 (7) |
Hg3—O3ix | 3.027 (6) | O9—Hg2vii | 2.796 (7) |
Hg3—Se3 | 3.4103 (15) | O9—Hg2xiii | 2.906 (8) |
Hg3—Se3ix | 3.4700 (14) | O10—Hg1xiii | 2.677 (7) |
Hg3—Se1x | 3.6702 (12) | O10—Hg2viii | 2.686 (7) |
Se1—O1 | 1.705 (6) | O10—Hg3xii | 3.729 (7) |
Se1—O5xi | 1.709 (7) | O10—Hg2vii | 4.156 (7) |
Se1—O4xi | 1.720 (6) | | |
| | | |
O1i—Hg1—O3 | 109.8 (2) | O1—Hg2—O9viii | 82.6 (2) |
O1i—Hg1—O4ii | 121.6 (2) | O3i—Hg2—O9viii | 168.3 (2) |
O3—Hg1—O4ii | 113.0 (2) | O10vii—Hg2—O9viii | 93.7 (2) |
O1i—Hg1—O4 | 89.5 (2) | O6vi—Hg2—O9viii | 113.5 (2) |
O3—Hg1—O4 | 116.6 (2) | O2—Hg2—O9iii | 68.2 (2) |
O4ii—Hg1—O4 | 104.50 (16) | O2vi—Hg2—O9iii | 74.0 (2) |
O1i—Hg1—O5 | 148.7 (2) | O1—Hg2—O9iii | 153.4 (2) |
O3—Hg1—O5 | 79.0 (2) | O3i—Hg2—O9iii | 70.9 (2) |
O4ii—Hg1—O5 | 78.2 (3) | O10vii—Hg2—O9iii | 120.7 (2) |
O4—Hg1—O5 | 60.69 (19) | O6vi—Hg2—O9iii | 85.4 (2) |
O1i—Hg1—O10iii | 80.5 (2) | O9viii—Hg2—O9iii | 118.99 (15) |
O3—Hg1—O10iii | 76.0 (2) | O5ix—Hg3—O6 | 119.3 (3) |
O4ii—Hg1—O10iii | 73.4 (2) | O5ix—Hg3—O8 | 121.9 (3) |
O4—Hg1—O10iii | 166.2 (2) | O6—Hg3—O8 | 97.7 (3) |
O5—Hg1—O10iii | 130.4 (2) | O5ix—Hg3—O7ix | 93.4 (3) |
O1i—Hg1—O5iv | 59.2 (2) | O6—Hg3—O7ix | 108.9 (3) |
O3—Hg1—O5iv | 165.8 (2) | O8—Hg3—O7ix | 116.4 (2) |
O4ii—Hg1—O5iv | 70.7 (2) | O5ix—Hg3—O4 | 71.3 (2) |
O4—Hg1—O5iv | 74.1 (3) | O6—Hg3—O4 | 80.8 (3) |
O5—Hg1—O5iv | 115.18 (14) | O8—Hg3—O4 | 72.7 (2) |
O10iii—Hg1—O5iv | 92.6 (2) | O7ix—Hg3—O4 | 164.7 (2) |
O1i—Hg1—O6 | 68.2 (2) | O5ix—Hg3—O3ix | 71.6 (2) |
O3—Hg1—O6 | 59.0 (2) | O6—Hg3—O3ix | 67.0 (2) |
O4ii—Hg1—O6 | 170.0 (2) | O8—Hg3—O3ix | 164.1 (2) |
O4—Hg1—O6 | 76.2 (2) | O7ix—Hg3—O3ix | 67.8 (2) |
O5—Hg1—O6 | 93.9 (2) | O4—Hg3—O3ix | 107.15 (18) |
O10iii—Hg1—O6 | 108.2 (2) | O5ix—Hg3—O9 | 155.5 (2) |
O5iv—Hg1—O6 | 118.6 (2) | O6—Hg3—O9 | 85.2 (2) |
O2—Hg2—O2vi | 97.12 (17) | O8—Hg3—O9 | 48.2 (2) |
O2—Hg2—O1 | 137.8 (2) | O7ix—Hg3—O9 | 77.2 (2) |
O2vi—Hg2—O1 | 102.5 (2) | O4—Hg3—O9 | 116.21 (17) |
O2—Hg2—O3i | 111.2 (2) | O3ix—Hg3—O9 | 123.18 (16) |
O2vi—Hg2—O3i | 121.2 (2) | O1—Se1—O5xi | 94.7 (3) |
O1—Hg2—O3i | 89.8 (2) | O1—Se1—O4xi | 100.8 (3) |
O2—Hg2—O10vii | 81.3 (2) | O5xi—Se1—O4xi | 95.8 (3) |
O2vi—Hg2—O10vii | 162.4 (2) | O6—Se2—O3 | 97.7 (4) |
O1—Hg2—O10vii | 68.9 (2) | O6—Se2—O2 | 93.5 (3) |
O3i—Hg2—O10vii | 75.1 (2) | O3—Se2—O2 | 102.3 (3) |
O2—Hg2—O6vi | 149.4 (3) | O9—Se3—O7 | 109.2 (3) |
O2vi—Hg2—O6vi | 59.4 (2) | O9—Se3—O10 | 113.6 (4) |
O1—Hg2—O6vi | 70.9 (2) | O7—Se3—O10 | 109.4 (4) |
O3i—Hg2—O6vi | 71.9 (2) | O9—Se3—O8 | 109.3 (4) |
O10vii—Hg2—O6vi | 127.2 (2) | O7—Se3—O8 | 108.4 (3) |
O2—Hg2—O9viii | 69.8 (2) | O10—Se3—O8 | 106.9 (3) |
O2vi—Hg2—O9viii | 69.5 (2) | | |
Symmetry codes: (i) −x, y+1/2, −z+1; (ii) −x, y−1/2, −z; (iii) x−1, y, z; (iv) −x, y+1/2, −z; (v) x, y, z−1; (vi) −x, y−1/2, −z+1; (vii) −x+1, y+1/2, −z+1; (viii) −x+1, y−1/2, −z+1; (ix) x, y+1, z; (x) x, y+1, z−1; (xi) x, y, z+1; (xii) x, y−1, z; (xiii) x+1, y, z. |
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