Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805033799/wm6103sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805033799/wm6103Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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.
Cs6Sb4Se9·0.5H2O | F(000) = 3380 |
Mr = 2004.11 | Dx = 4.537 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 17 reflections |
a = 10.409 (2) Å | θ = 5.0–13.1° |
b = 19.064 (4) Å | µ = 22.04 mm−1 |
c = 14.895 (3) Å | T = 293 K |
β = 94.39 (3)° | Block, red |
V = 2947.1 (10) Å3 | 0.14 × 0.11 × 0.10 mm |
Z = 4 |
Siemens P4 four-circle diffractometer | 1796 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.072 |
Graphite monochromator | θmax = 25.0°, θmin = 2.2° |
ω scans | h = 0→12 |
Absorption correction: ψ scan (XPREP in SHELXTL-Plus; Sheldrick, 1995) | k = 0→22 |
Tmin = 0.065, Tmax = 0.108 | l = −17→17 |
2733 measured reflections | 3 standard reflections every 97 reflections |
2563 independent reflections | intensity decay: 15% |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.067 | H-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 reflections | Δρmax = 1.54 e Å−3 |
89 parameters | Δρmin = −1.72 e Å−3 |
0 restraints |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cs1 | 0.31807 (14) | 0.20508 (7) | 0.89048 (9) | 0.0337 (4) | |
Cs2 | 0.5000 | 0.02479 (12) | 0.7500 | 0.0469 (6) | |
Cs3 | 0.15045 (15) | 0.34458 (8) | 0.59383 (11) | 0.0417 (4) | |
Cs4 | 0.0000 | −0.09570 (15) | 0.7500 | 0.0522 (7) | |
Sb1 | 0.11996 (13) | 0.11799 (7) | 0.65874 (9) | 0.0227 (3) | |
Sb2 | −0.14247 (14) | 0.04704 (7) | 0.47316 (9) | 0.0244 (4) | |
Se1 | 0.0151 (2) | 0.15548 (11) | 0.50002 (14) | 0.0253 (5) | |
Se2 | 0.0000 | 0.21143 (15) | 0.7500 | 0.0252 (7) | |
Se3 | −0.3104 (2) | 0.11586 (13) | 0.37927 (16) | 0.0381 (6) | |
Se4 | 0.3290 (2) | 0.18187 (14) | 0.64910 (16) | 0.0358 (6) | |
Se5 | 0.2113 (3) | 0.02934 (12) | 0.87011 (17) | 0.0427 (7) | |
O | 0.5000 | 0.0000 | 0.0000 | 0.09 (2)* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.0425 (9) | 0.0276 (8) | 0.0304 (8) | −0.0088 (7) | −0.0008 (7) | −0.0029 (6) |
Cs2 | 0.0330 (12) | 0.0309 (12) | 0.0786 (18) | 0.000 | 0.0149 (12) | 0.000 |
Cs3 | 0.0362 (9) | 0.0449 (9) | 0.0447 (9) | −0.0018 (8) | 0.0078 (7) | 0.0000 (8) |
Cs4 | 0.0432 (14) | 0.0845 (19) | 0.0292 (12) | 0.000 | 0.0056 (11) | 0.000 |
Sb1 | 0.0257 (8) | 0.0238 (7) | 0.0185 (7) | 0.0037 (7) | 0.0010 (6) | 0.0006 (6) |
Sb2 | 0.0276 (8) | 0.0202 (7) | 0.0256 (8) | 0.0034 (7) | 0.0043 (6) | −0.0029 (6) |
Se1 | 0.0269 (12) | 0.0273 (11) | 0.0211 (10) | −0.0015 (10) | −0.0026 (9) | 0.0051 (9) |
Se2 | 0.0296 (17) | 0.0210 (15) | 0.0260 (16) | 0.000 | 0.0094 (14) | 0.000 |
Se3 | 0.0317 (13) | 0.0391 (14) | 0.0410 (14) | 0.0078 (12) | −0.0128 (11) | −0.0056 (11) |
Se4 | 0.0213 (12) | 0.0562 (16) | 0.0302 (12) | 0.0001 (11) | 0.0033 (10) | 0.0071 (11) |
Se5 | 0.0624 (18) | 0.0257 (12) | 0.0439 (15) | −0.0046 (13) | 0.0302 (14) | −0.0074 (11) |
Cs1—Se5 | 3.535 (3) | Cs4—Se3vi | 3.905 (3) |
Cs1—Se4 | 3.633 (3) | Cs4—Se3xii | 3.905 (3) |
Cs1—Se1i | 3.664 (3) | Sb1—Se4 | 2.507 (3) |
Cs1—Se3i | 3.665 (3) | Sb1—Se2 | 2.615 (2) |
Cs1—Se2 | 3.7807 (19) | Sb1—Se1 | 2.626 (3) |
Cs1—Se4ii | 3.791 (3) | Sb2—Se5iii | 2.517 (3) |
Cs1—Se3iii | 3.834 (3) | Sb2—Se3 | 2.522 (3) |
Cs1—Se1iii | 4.055 (3) | Sb2—Se1 | 2.650 (3) |
Cs2—Se5ii | 3.614 (3) | Se1—Cs1xiii | 3.664 (3) |
Cs2—Se5 | 3.614 (3) | Se1—Cs3x | 3.850 (3) |
Cs2—Se4ii | 3.740 (3) | Se1—Cs4vi | 3.886 (2) |
Cs2—Se4 | 3.740 (3) | Se1—Cs1iii | 4.055 (3) |
Cs2—Oiv | 3.7536 (8) | Se2—Sb1iii | 2.615 (2) |
Cs2—Ov | 3.7536 (8) | Se2—Cs1iii | 3.7807 (19) |
Cs2—Se3vi | 3.769 (3) | Se2—Cs3iii | 3.855 (3) |
Cs2—Se3vii | 3.769 (3) | Se3—Cs1xiii | 3.665 (3) |
Cs3—Oviii | 3.5846 (17) | Se3—Cs3ix | 3.670 (3) |
Cs3—Se3ix | 3.670 (3) | Se3—Cs2vi | 3.769 (3) |
Cs3—Se4x | 3.676 (3) | Se3—Cs1iii | 3.834 (3) |
Cs3—Se4 | 3.677 (3) | Se3—Cs4vi | 3.905 (3) |
Cs3—Se5xi | 3.827 (3) | Se3—Cs3xiii | 4.307 (3) |
Cs3—Se1x | 3.850 (3) | Se4—Cs3x | 3.676 (3) |
Cs3—Se2 | 3.855 (3) | Se4—Cs1ii | 3.791 (3) |
Cs3—Se1 | 4.078 (3) | Se5—Sb2iii | 2.517 (3) |
Cs3—Se3i | 4.307 (3) | Se5—Cs3xiv | 3.827 (3) |
Cs4—Se5 | 3.622 (3) | O—Cs3xv | 3.5846 (17) |
Cs4—Se5iii | 3.622 (3) | O—Cs3xvi | 3.5846 (17) |
Cs4—Se1vi | 3.886 (2) | O—Cs2xvii | 3.7536 (8) |
Cs4—Se1xii | 3.886 (2) | O—Cs2xviii | 3.7536 (8) |
Se4—Sb1—Se2 | 98.62 (9) | Se5iii—Sb2—Se1 | 100.45 (9) |
Se4—Sb1—Se1 | 96.84 (9) | Se3—Sb2—Se1 | 94.16 (9) |
Se2—Sb1—Se1 | 95.76 (7) | Sb1—Se1—Sb2 | 97.67 (8) |
Se5iii—Sb2—Se3 | 110.46 (10) | Sb1—Se2—Sb1iii | 94.14 (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) −x−1/2, −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) x−1/2, −y+1/2, z−1/2; (xiv) −x+1/2, y−1/2, −z+3/2; (xv) x+1/2, −y+1/2, z−1/2; (xvi) −x+1/2, y−1/2, −z+1/2; (xvii) x, y, z−1; (xviii) −x+1, −y, −z+1. |