Redetermination of mercury(II) hydro­xide chlorate(V)

Hg(OH)ClO₃ is built up from infinite zigzag [Hg(OH)_2/2]⁺ chains along [001] and [ClO₃]⁻ ions. These chains are connected via weak Hg—O interactions to O atoms of the [ClO₃]⁻ ions, leading to layers parallel to (010). O—H...O hydrogen bonds are present between these layers.

Key indicators

• Single-crystal X-ray study
• T = 170 K
• Mean [sigma](Cl-O) = 0.005 Å
• R factor = 0.020
• wR factor = 0.043
• Data-to-parameter ratio = 16.0

checkCIF/PLATON results

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Computing details

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.

mercury(II) hydroxide chlorate(V)

Crystal data

Hg(OH)ClO3	F(000) = 520
Mr = 301.05	Dx = 5.253 Mg m^−3
Orthorhombic, Pbcm	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2c 2b	Cell parameters from 2000 reflections
a = 4.6375 (6) Å	θ = 1.8–29.6°
b = 11.4064 (19) Å	µ = 40.99 mm^−1
c = 7.1965 (11) Å	T = 170 K
V = 380.67 (10) Å^3	Rod-shaped, colourless
Z = 4	0.13 × 0.07 × 0.02 mm

Data collection

IPDS-II diffractometer	592 independent reflections
Radiation source: fine-focus sealed tube	457 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.100
ω oscillation scans	θmax = 30.0°, θmin = 3.6°
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1999)	h = −6→6
Tmin = 0.012, Tmax = 0.116	k = −16→16
9295 measured reflections	l = −10→10

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.020	All H-atom parameters refined
wR(F^2) = 0.043	w = 1/[σ^2(Fo^2) + (0.0208P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.97	(Δ/σ)max = 0.006
592 reflections	Δρmax = 2.03 e Å^−3
37 parameters	Δρmin = −1.21 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0265 (9)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Hg1	0.56532 (4)	0.2500	0.0000	0.01323 (12)
O1	0.5736 (8)	0.1638 (4)	0.2500	0.0135 (10)
Cl1	0.9968 (4)	0.43891 (14)	0.2500	0.0136 (3)
O11	0.6740 (10)	0.4461 (5)	0.2500	0.0204 (9)
O12	0.0692 (6)	0.3682 (4)	0.0831 (5)	0.0227 (8)
H1	0.464 (17)	0.097 (7)	0.2500	0.010 (19)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Hg1	0.01271 (15)	0.01731 (16)	0.00967 (16)	0.000	0.000	−0.00004 (9)
O1	0.018 (2)	0.014 (2)	0.0084 (18)	−0.0037 (16)	0.000	0.000
Cl1	0.0110 (5)	0.0151 (6)	0.0146 (5)	−0.0024 (7)	0.000	0.000
O11	0.0143 (19)	0.020 (2)	0.027 (2)	0.005 (2)	0.000	0.000
O12	0.0163 (17)	0.0294 (19)	0.0224 (18)	0.0029 (13)	0.0011 (11)	−0.0096 (17)

Geometric parameters (Å, º)

Hg1—O1^i	2.051 (2)	Cl1—O12^iii	1.486 (4)
Hg1—O1	2.051 (2)	Cl1—O12^iv	1.486 (4)
O1—Hg1^ii	2.051 (2)	Cl1—O11	1.499 (5)
O1—H1	0.92 (8)	O12—Cl1^v	1.486 (4)
O1^i—Hg1—O1	177.9 (2)	O12^iii—Cl1—O12^iv	107.9 (3)
Hg1^ii—O1—Hg1	122.6 (2)	O12^iii—Cl1—O11	104.81 (18)
Hg1^ii—O1—H1	112.8 (15)	O12^iv—Cl1—O11	104.81 (18)
Hg1—O1—H1	112.8 (15)

Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, y, −z+1/2; (iii) x+1, y, z; (iv) x+1, y, −z+1/2; (v) x−1, y, z.