Holmium chloride oxoselenate(IV), HoClSeO₃

In the title compound, HoClSeO₃, the Ho³⁺ ion is coordinated by three monodentate SeO₃^2- ions, one chelating selenite group, and two chloride ligands. The [HoO₅Cl₂] polyhedra are pentagonal bipyramids which are connected to form a three-dimensional network via edges and vertices. The SeO₃^2- ion shows the typical pyramidal shape due to the lone electron pair of the selenium atom.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](Se-O) = 0.004 Å
• R factor = 0.023
• wR factor = 0.053
• Data-to-parameter ratio = 19.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

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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, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

(I)

Crystal data

ClHoO3Se	Dx = 4.966 Mg m^−3
Mr = 327.34	Melting point: not measured K
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -p_2ac_2n	Cell parameters from 2000 reflections
a = 7.2093 (15) Å	θ = 3.0–28.0°
b = 6.9259 (10) Å	µ = 26.85 mm^−1
c = 8.7689 (15) Å	T = 293 K
V = 437.84 (13) Å^3	Column, yellow
Z = 4	0.15 × 0.13 × 0.12 mm
F(000) = 568

Data collection

IPDS I diffractometer	688 independent reflections
Radiation source: fine-focus sealed tube	626 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.061
Detector resolution: not measured pixels mm^-1	θmax = 30.0°, θmin = 3.7°
w? f? oscillation scans	h = −10→10
Absorption correction: numerical crystal shape optimization (X-SHAPE; Stoe & Cie, 1999)	k = −9→9
Tmin = 0.023, Tmax = 0.039	l = −12→12
4891 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.023	w = 1/[σ^2(Fo^2) + (0.0338P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.053	(Δ/σ)max < 0.001
S = 1.04	Δρmax = 1.21 e Å^−3
688 reflections	Δρmin = −1.79 e Å^−3
35 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0412 (15)

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
Ho	0.10634 (4)	0.2500	0.03988 (3)	0.01370 (14)
Se	0.71023 (8)	0.2500	0.86659 (7)	0.01506 (16)
Cl	0.4421 (3)	0.2500	0.18300 (19)	0.0271 (4)
O1	0.8575 (5)	0.0729 (5)	0.9313 (4)	0.0207 (6)
O2	0.7532 (8)	0.2500	0.6802 (6)	0.0238 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ho	0.01865 (18)	0.00919 (18)	0.01326 (17)	0.000	−0.00076 (9)	0.000
Se	0.0176 (3)	0.0119 (3)	0.0156 (3)	0.000	−0.0018 (2)	0.000
Cl	0.0239 (7)	0.0365 (10)	0.0207 (7)	0.000	−0.0066 (6)	0.000
O1	0.0249 (15)	0.0120 (15)	0.0252 (14)	−0.0002 (13)	−0.0068 (13)	0.0028 (13)
O2	0.028 (2)	0.026 (3)	0.018 (2)	0.000	−0.0015 (18)	0.000

Geometric parameters (Å, º)

Ho—O2^i	2.201 (5)	Ho—Ho^vii	3.8513 (5)
Ho—O1^ii	2.266 (3)	Se—O2	1.664 (5)
Ho—O1^iii	2.266 (3)	Se—O1^viii	1.718 (3)
Ho—O1^iv	2.373 (4)	Se—O1	1.718 (3)
Ho—O1^v	2.373 (4)	Se—Ho^ix	3.2348 (9)
Ho—Cl^i	2.7033 (17)	Cl—Ho^x	2.7033 (17)
Ho—Cl	2.7264 (18)	O1—Ho^ii	2.266 (3)
Ho—Se^iv	3.2348 (9)	O1—Ho^ix	2.373 (4)
Ho—Ho^vi	3.8513 (5)	O2—Ho^x	2.201 (5)
O2^i—Ho—O1^ii	92.42 (10)	O2^i—Ho—Ho^vi	91.85 (6)
O2^i—Ho—O1^iii	92.42 (10)	O1^ii—Ho—Ho^vi	34.77 (9)
O1^ii—Ho—O1^iii	161.56 (18)	O1^iii—Ho—Ho^vi	162.48 (9)
O2^i—Ho—O1^iv	90.69 (15)	O1^iv—Ho—Ho^vi	33.00 (8)
O1^ii—Ho—O1^iv	67.76 (14)	O1^v—Ho—Ho^vi	95.21 (8)
O1^iii—Ho—O1^iv	129.94 (10)	Cl^i—Ho—Ho^vi	89.36 (2)
O2^i—Ho—O1^v	90.69 (15)	Cl—Ho—Ho^vi	115.915 (9)
O1^ii—Ho—O1^v	129.94 (10)	Se^iv—Ho—Ho^vi	64.101 (9)
O1^iii—Ho—O1^v	67.76 (14)	O2^i—Ho—Ho^vii	91.85 (6)
O1^iv—Ho—O1^v	62.24 (16)	O1^ii—Ho—Ho^vii	162.48 (9)
O2^i—Ho—Cl^i	177.24 (15)	O1^iii—Ho—Ho^vii	34.77 (9)
O1^ii—Ho—Cl^i	87.16 (9)	O1^iv—Ho—Ho^vii	95.21 (8)
O1^iii—Ho—Cl^i	87.16 (10)	O1^v—Ho—Ho^vii	33.00 (8)
O1^iv—Ho—Cl^i	91.68 (10)	Cl^i—Ho—Ho^vii	89.36 (2)
O1^v—Ho—Cl^i	91.68 (10)	Cl—Ho—Ho^vii	115.915 (9)
O2^i—Ho—Cl	88.66 (15)	Se^iv—Ho—Ho^vii	64.101 (9)
O1^ii—Ho—Cl	81.17 (9)	Ho^vi—Ho—Ho^vii	128.099 (17)
O1^iii—Ho—Cl	81.17 (9)	O2—Se—O1^viii	102.11 (19)
O1^iv—Ho—Cl	148.87 (8)	O2—Se—O1	102.11 (18)
O1^v—Ho—Cl	148.87 (8)	O1^viii—Se—O1	91.1 (2)
Cl^i—Ho—Cl	88.58 (3)	O2—Se—Ho^ix	107.3 (2)
O2^i—Ho—Se^iv	90.73 (14)	O1^viii—Se—Ho^ix	45.53 (12)
O1^ii—Ho—Se^iv	98.86 (9)	O1—Se—Ho^ix	45.53 (12)
O1^iii—Ho—Se^iv	98.86 (9)	Ho^x—Cl—Ho	143.39 (8)
O1^iv—Ho—Se^iv	31.12 (8)	Se—O1—Ho^ii	144.3 (2)
O1^v—Ho—Se^iv	31.12 (8)	Se—O1—Ho^ix	103.35 (16)
Cl^i—Ho—Se^iv	92.04 (4)	Ho^ii—O1—Ho^ix	112.24 (14)
Cl—Ho—Se^iv	179.39 (4)	Se—O2—Ho^x	140.5 (3)

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