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The title compound, Cs6Sb4Se9·0.5H2O, contains discrete [Sb4Se9]6- chain anions consisting of corner-linked SbSe3 pyramids. Mol­ecular C2 symmetry is observed for these nona­selenidoantimonate(III) anions, which exhibit bridging Sb-Se distances in the range 2.615 (2)-2.650 (3) Å and shorter terminal Sb-Se distances between 2.507 (3) and 2.522 (3) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805033799/wm6103sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805033799/wm6103Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](b-Se) = 0.003 Å
  • H-atom completeness 1%
  • Disorder in main residue
  • R factor = 0.067
  • wR factor = 0.135
  • Data-to-parameter ratio = 28.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc.
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:H1 Cs6 O0.5 Sb4 Se9 Atom count from the _atom_site data: Cs6 O0.5 Sb4 Se9 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum Cs6 H1 O0.5 Sb4 Se9 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff Cs 24.00 24.00 0.00 H 4.00 0.00 4.00 O 2.00 2.00 0.00 Sb 16.00 16.00 0.00 Se 36.00 36.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: R3m/V User's Guide (Siemens, 1989); cell refinement: R3m/V User's Guide; data reduction: XDISK (Siemens, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1995); software used to prepare material for publication: SHELXL97.

Hexacaesium nonaselenidotetraantimonate(III) hemihydrate top
Crystal data top
Cs6Sb4Se9·0.5H2OF(000) = 3380
Mr = 2004.11Dx = 4.537 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 17 reflections
a = 10.409 (2) Åθ = 5.0–13.1°
b = 19.064 (4) ŵ = 22.04 mm1
c = 14.895 (3) ÅT = 293 K
β = 94.39 (3)°Block, red
V = 2947.1 (10) Å30.14 × 0.11 × 0.10 mm
Z = 4
Data collection top
Siemens P4 four-circle
diffractometer
1796 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.072
Graphite monochromatorθmax = 25.0°, θmin = 2.2°
ω scansh = 012
Absorption correction: ψ scan
(XPREP in SHELXTL-Plus; Sheldrick, 1995)
k = 022
Tmin = 0.065, Tmax = 0.108l = 1717
2733 measured reflections3 standard reflections every 97 reflections
2563 independent reflections intensity decay: 15%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.067H-atom parameters not refined
wR(F2) = 0.135 w = 1/[σ2(Fo2) + (0.0473P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.18(Δ/σ)max < 0.001
2563 reflectionsΔρmax = 1.54 e Å3
89 parametersΔρmin = 1.72 e Å3
0 restraints
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)
Cs10.31807 (14)0.20508 (7)0.89048 (9)0.0337 (4)
Cs20.50000.02479 (12)0.75000.0469 (6)
Cs30.15045 (15)0.34458 (8)0.59383 (11)0.0417 (4)
Cs40.00000.09570 (15)0.75000.0522 (7)
Sb10.11996 (13)0.11799 (7)0.65874 (9)0.0227 (3)
Sb20.14247 (14)0.04704 (7)0.47316 (9)0.0244 (4)
Se10.0151 (2)0.15548 (11)0.50002 (14)0.0253 (5)
Se20.00000.21143 (15)0.75000.0252 (7)
Se30.3104 (2)0.11586 (13)0.37927 (16)0.0381 (6)
Se40.3290 (2)0.18187 (14)0.64910 (16)0.0358 (6)
Se50.2113 (3)0.02934 (12)0.87011 (17)0.0427 (7)
O0.50000.00000.00000.09 (2)*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs10.0425 (9)0.0276 (8)0.0304 (8)0.0088 (7)0.0008 (7)0.0029 (6)
Cs20.0330 (12)0.0309 (12)0.0786 (18)0.0000.0149 (12)0.000
Cs30.0362 (9)0.0449 (9)0.0447 (9)0.0018 (8)0.0078 (7)0.0000 (8)
Cs40.0432 (14)0.0845 (19)0.0292 (12)0.0000.0056 (11)0.000
Sb10.0257 (8)0.0238 (7)0.0185 (7)0.0037 (7)0.0010 (6)0.0006 (6)
Sb20.0276 (8)0.0202 (7)0.0256 (8)0.0034 (7)0.0043 (6)0.0029 (6)
Se10.0269 (12)0.0273 (11)0.0211 (10)0.0015 (10)0.0026 (9)0.0051 (9)
Se20.0296 (17)0.0210 (15)0.0260 (16)0.0000.0094 (14)0.000
Se30.0317 (13)0.0391 (14)0.0410 (14)0.0078 (12)0.0128 (11)0.0056 (11)
Se40.0213 (12)0.0562 (16)0.0302 (12)0.0001 (11)0.0033 (10)0.0071 (11)
Se50.0624 (18)0.0257 (12)0.0439 (15)0.0046 (13)0.0302 (14)0.0074 (11)
Geometric parameters (Å, º) top
Cs1—Se53.535 (3)Cs4—Se3vi3.905 (3)
Cs1—Se43.633 (3)Cs4—Se3xii3.905 (3)
Cs1—Se1i3.664 (3)Sb1—Se42.507 (3)
Cs1—Se3i3.665 (3)Sb1—Se22.615 (2)
Cs1—Se23.7807 (19)Sb1—Se12.626 (3)
Cs1—Se4ii3.791 (3)Sb2—Se5iii2.517 (3)
Cs1—Se3iii3.834 (3)Sb2—Se32.522 (3)
Cs1—Se1iii4.055 (3)Sb2—Se12.650 (3)
Cs2—Se5ii3.614 (3)Se1—Cs1xiii3.664 (3)
Cs2—Se53.614 (3)Se1—Cs3x3.850 (3)
Cs2—Se4ii3.740 (3)Se1—Cs4vi3.886 (2)
Cs2—Se43.740 (3)Se1—Cs1iii4.055 (3)
Cs2—Oiv3.7536 (8)Se2—Sb1iii2.615 (2)
Cs2—Ov3.7536 (8)Se2—Cs1iii3.7807 (19)
Cs2—Se3vi3.769 (3)Se2—Cs3iii3.855 (3)
Cs2—Se3vii3.769 (3)Se3—Cs1xiii3.665 (3)
Cs3—Oviii3.5846 (17)Se3—Cs3ix3.670 (3)
Cs3—Se3ix3.670 (3)Se3—Cs2vi3.769 (3)
Cs3—Se4x3.676 (3)Se3—Cs1iii3.834 (3)
Cs3—Se43.677 (3)Se3—Cs4vi3.905 (3)
Cs3—Se5xi3.827 (3)Se3—Cs3xiii4.307 (3)
Cs3—Se1x3.850 (3)Se4—Cs3x3.676 (3)
Cs3—Se23.855 (3)Se4—Cs1ii3.791 (3)
Cs3—Se14.078 (3)Se5—Sb2iii2.517 (3)
Cs3—Se3i4.307 (3)Se5—Cs3xiv3.827 (3)
Cs4—Se53.622 (3)O—Cs3xv3.5846 (17)
Cs4—Se5iii3.622 (3)O—Cs3xvi3.5846 (17)
Cs4—Se1vi3.886 (2)O—Cs2xvii3.7536 (8)
Cs4—Se1xii3.886 (2)O—Cs2xviii3.7536 (8)
Se4—Sb1—Se298.62 (9)Se5iii—Sb2—Se1100.45 (9)
Se4—Sb1—Se196.84 (9)Se3—Sb2—Se194.16 (9)
Se2—Sb1—Se195.76 (7)Sb1—Se1—Sb297.67 (8)
Se5iii—Sb2—Se3110.46 (10)Sb1—Se2—Sb1iii94.14 (11)
Symmetry codes: (i) x+1/2, y+1/2, z+1/2; (ii) x+1, y, z+3/2; (iii) x, y, z+3/2; (iv) x+1, y, z+1/2; (v) x, y, z+1; (vi) x, y, z+1; (vii) x+1, y, z+1/2; (viii) x+1/2, y+1/2, z+1/2; (ix) x1/2, y+1/2, z+1; (x) x+1/2, y+1/2, z+1; (xi) x+1/2, y+1/2, z+3/2; (xii) x, y, z+1/2; (xiii) x1/2, y+1/2, z1/2; (xiv) x+1/2, y1/2, z+3/2; (xv) x+1/2, y+1/2, z1/2; (xvi) x+1/2, y1/2, z+1/2; (xvii) x, y, z1; (xviii) x+1, y, z+1.
 

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