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Single crystals of zinc mercury(II) arsenate(V) hydroxide, ZnHg(AsO4)(OH), were obtained under hydrothermal conditions and structurally characterized using X-ray diffraction. ZnHg(AsO4)(OH) crystallizes isotypically with the mineral descloizite, ZnPb(VO4)(OH). The structure is composed of linear chains of edge-sharing [Zn(OH)2O4] octahedra which are linked by vertices of AsO4 tetrahedra to form an open framework structure. In the channels of this arrangement, Hg atoms are situated, having two short bonds to one O atom of the AsO4 group and to the OH group. Additional stabilization of the structure is accomplished by weak hydrogen bonding.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (Zn-O) = 0.003 Å
- R factor = 0.018
- wR factor = 0.041
- Data-to-parameter ratio = 13.5
checkCIF/PLATON results
No syntax errors found
No errors found in this datablock
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, 2000); software used to prepare material for publication: SHELXL97.
Crystal data top
HgZn(AsO4)(OH) | F(000) = 736 |
Mr = 421.89 | Dx = 6.736 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 2675 reflections |
a = 7.6826 (7) Å | θ = 3.5–30.3° |
b = 6.2459 (6) Å | µ = 50.43 mm−1 |
c = 8.6691 (8) Å | T = 295 K |
V = 415.98 (7) Å3 | Parallelepiped, colourless |
Z = 4 | 0.08 × 0.08 × 0.05 mm |
Data collection top
Siemens SMART diffractometer | 677 independent reflections |
Radiation source: fine-focus sealed tube | 617 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
ω scans | θmax = 30.5°, θmin = 3.5° |
Absorption correction: numerical (HABITUS; Herrendorf, 1993-1997) | h = −10→10 |
Tmin = 0.088, Tmax = 0.209 | k = −8→8 |
4303 measured reflections | l = −12→11 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.018 | All H-atom parameters refined |
wR(F2) = 0.041 | w = 1/[σ2(Fo2) + (0.019P)2 + 0.725P] where P = (Fo2 + 2Fc2)/3 |
S = 1.12 | (Δ/σ)max < 0.001 |
677 reflections | Δρmax = 1.80 e Å−3 |
50 parameters | Δρmin = −1.13 e Å−3 |
1 restraint | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0111 (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 | x | y | z | Uiso*/Ueq | |
Hg | 0.39038 (3) | 0.2500 | 0.82965 (3) | 0.01511 (10) | |
As | 0.35298 (7) | 0.2500 | 0.18336 (6) | 0.00693 (13) | |
Zn | 0.0000 | 0.0000 | 0.0000 | 0.00928 (15) | |
O1 | 0.3664 (4) | 0.0245 (5) | 0.2887 (4) | 0.0122 (6) | |
O2 | 0.0141 (5) | 0.2500 | 0.4532 (5) | 0.0142 (8) | |
O3 | 0.1682 (5) | 0.2500 | 0.0768 (5) | 0.0108 (8) | |
O4 | 0.3611 (5) | 0.2500 | 0.5879 (5) | 0.0086 (8) | |
H | 0.264 (7) | 0.2500 | 0.556 (11) | 0.03 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Hg | 0.01543 (14) | 0.02212 (16) | 0.00777 (13) | 0.000 | 0.00061 (8) | 0.000 |
As | 0.0074 (2) | 0.0072 (3) | 0.0062 (3) | 0.000 | −0.00175 (18) | 0.000 |
Zn | 0.0113 (3) | 0.0077 (3) | 0.0088 (3) | 0.0007 (2) | −0.0005 (2) | 0.0004 (2) |
O1 | 0.0148 (13) | 0.0109 (14) | 0.0109 (13) | 0.0000 (11) | −0.0029 (11) | 0.0016 (11) |
O2 | 0.0105 (19) | 0.023 (2) | 0.0097 (18) | 0.000 | −0.0032 (16) | 0.000 |
O3 | 0.0082 (17) | 0.0072 (19) | 0.017 (2) | 0.000 | −0.0059 (15) | 0.000 |
O4 | 0.0033 (16) | 0.012 (2) | 0.011 (2) | 0.000 | 0.0030 (14) | 0.000 |
Geometric parameters (Å, º) top
Hg—O4 | 2.108 (4) | Zn—Znxv | 3.1229 (3) |
Hg—O2i | 2.109 (5) | Zn—Znxvi | 3.1229 (3) |
Hg—O1ii | 2.638 (3) | Zn—Hgxi | 3.3636 (3) |
Hg—O1iii | 2.638 (3) | Zn—Hgxiii | 3.3637 (3) |
Hg—O1iv | 2.736 (3) | Zn—Hgix | 3.6897 (3) |
Hg—O1v | 2.736 (3) | Zn—Hgxvii | 3.6897 (3) |
Hg—O3vi | 2.740 (4) | O1—Znii | 2.105 (3) |
Hg—Asvi | 3.0799 (7) | O1—Hgxi | 2.638 (3) |
As—O1vii | 1.682 (3) | O1—Hgv | 2.736 (3) |
As—O1 | 1.682 (3) | O2—Asxiii | 1.713 (4) |
As—O3 | 1.694 (4) | O2—Hgxviii | 2.109 (5) |
As—O2viii | 1.713 (4) | O2—Hgxi | 3.3820 (17) |
As—Hgix | 3.0799 (7) | O2—Hgxii | 3.3820 (17) |
As—Hgx | 3.6950 (4) | O3—Znxvi | 2.133 (3) |
As—Hgv | 3.6950 (4) | O3—Hgix | 2.740 (4) |
As—Hgxi | 3.8544 (4) | O3—Hgxii | 3.842 (3) |
As—Hgxii | 3.8544 (4) | O3—Hgxi | 3.842 (3) |
Zn—O4xiii | 2.039 (2) | O3—Hgxiii | 4.120 (4) |
Zn—O4xi | 2.039 (2) | O4—Znxix | 2.039 (2) |
Zn—O1xiii | 2.105 (3) | O4—Znii | 2.039 (2) |
Zn—O1xi | 2.105 (3) | O4—Hgxviii | 3.686 (4) |
Zn—O3 | 2.133 (3) | O4—Hgi | 4.129 (4) |
Zn—O3xiv | 2.133 (3) | | |
| | | |
O4—Hg—O2i | 159.35 (16) | As—O1—Hgxi | 124.87 (15) |
O4—Hg—O1ii | 77.67 (11) | Znii—O1—Hgxi | 101.56 (12) |
O2i—Hg—O1ii | 117.20 (10) | As—O1—Hgv | 111.27 (14) |
O4—Hg—O1iii | 77.67 (11) | Znii—O1—Hgv | 86.99 (10) |
O2i—Hg—O1iii | 117.20 (10) | Hgxi—O1—Hgv | 98.85 (10) |
O1ii—Hg—O1iii | 81.10 (14) | Asxiii—O2—Hgxviii | 106.9 (2) |
O4—Hg—O1iv | 72.54 (10) | Asxiii—O2—Hgxi | 86.45 (9) |
O2i—Hg—O1iv | 91.55 (11) | Hgxviii—O2—Hgxi | 112.36 (7) |
O1ii—Hg—O1iv | 150.21 (3) | Asxiii—O2—Hgxii | 86.45 (9) |
O1iii—Hg—O1iv | 93.03 (9) | Hgxviii—O2—Hgxii | 112.36 (7) |
O4—Hg—O1v | 72.54 (10) | Hgxi—O2—Hgxii | 134.85 (14) |
O2i—Hg—O1v | 91.55 (11) | As—O3—Zn | 132.68 (8) |
O1ii—Hg—O1v | 93.03 (9) | As—O3—Znxvi | 132.68 (8) |
O1iii—Hg—O1v | 150.21 (3) | Zn—O3—Znxvi | 94.09 (16) |
O1iv—Hg—O1v | 77.62 (13) | As—O3—Hgix | 84.51 (17) |
O4—Hg—O3vi | 135.33 (13) | Zn—O3—Hgix | 97.65 (14) |
O2i—Hg—O3vi | 65.33 (13) | Znxvi—O3—Hgix | 97.65 (14) |
O1ii—Hg—O3vi | 68.85 (9) | As—O3—Hgxii | 77.71 (10) |
O1iii—Hg—O3vi | 68.85 (9) | Zn—O3—Hgxii | 134.60 (16) |
O1iv—Hg—O3vi | 135.97 (7) | Znxvi—O3—Hgxii | 60.80 (6) |
O1v—Hg—O3vi | 135.97 (8) | Hgix—O3—Hgxii | 121.28 (7) |
O1vii—As—O1 | 113.7 (2) | As—O3—Hgxi | 77.71 (10) |
O1vii—As—O3 | 110.33 (12) | Zn—O3—Hgxi | 60.80 (6) |
O1—As—O3 | 110.33 (12) | Znxvi—O3—Hgxi | 134.60 (16) |
O1vii—As—O2viii | 109.34 (13) | Hgix—O3—Hgxi | 121.28 (7) |
O1—As—O2viii | 109.34 (13) | Hgxii—O3—Hgxi | 108.76 (11) |
O3—As—O2viii | 103.2 (2) | As—O3—Hgxiii | 154.2 (2) |
O4xiii—Zn—O4xi | 180.0 (3) | Zn—O3—Hgxiii | 54.49 (9) |
O4xiii—Zn—O1xiii | 90.80 (15) | Znxvi—O3—Hgxiii | 54.49 (9) |
O4xi—Zn—O1xiii | 89.20 (15) | Hgix—O3—Hgxiii | 69.74 (9) |
O4xiii—Zn—O1xi | 89.20 (15) | Hgxii—O3—Hgxiii | 115.30 (6) |
O4xi—Zn—O1xi | 90.80 (15) | Hgxi—O3—Hgxiii | 115.30 (6) |
O1xiii—Zn—O1xi | 180.00 (14) | Znxix—O4—Znii | 99.95 (17) |
O4xiii—Zn—O3 | 82.71 (11) | Znxix—O4—Hg | 108.39 (14) |
O4xi—Zn—O3 | 97.29 (11) | Znii—O4—Hg | 108.39 (14) |
O1xiii—Zn—O3 | 88.31 (14) | Znxix—O4—Hgxviii | 125.87 (10) |
O1xi—Zn—O3 | 91.69 (14) | Znii—O4—Hgxviii | 125.87 (10) |
O4xiii—Zn—O3xiv | 97.29 (11) | Hg—O4—Hgxviii | 84.95 (12) |
O4xi—Zn—O3xiv | 82.71 (11) | Znxix—O4—Hgi | 63.20 (10) |
O1xiii—Zn—O3xiv | 91.69 (14) | Znii—O4—Hgi | 63.20 (10) |
O1xi—Zn—O3xiv | 88.31 (14) | Hg—O4—Hgi | 73.90 (11) |
O3—Zn—O3xiv | 180.0 (2) | Hgxviii—O4—Hgi | 158.84 (12) |
As—O1—Znii | 124.29 (17) | | |
Symmetry codes: (i) x+1/2, y, −z+3/2; (ii) −x+1/2, −y, z+1/2; (iii) −x+1/2, y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+1; (v) −x+1, −y, −z+1; (vi) x, y, z+1; (vii) x, −y+1/2, z; (viii) x+1/2, y, −z+1/2; (ix) x, y, z−1; (x) −x+1, −y+1, −z+1; (xi) −x+1/2, −y, z−1/2; (xii) −x+1/2, −y+1, z−1/2; (xiii) x−1/2, y, −z+1/2; (xiv) −x, −y, −z; (xv) −x, y−1/2, −z; (xvi) −x, y+1/2, −z; (xvii) −x, −y, −z+1; (xviii) x−1/2, y, −z+3/2; (xix) x+1/2, −y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H···O2 | 0.80 (5) | 2.12 (5) | 2.910 (6) | 175 (10) |
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