Colourless single crystals of Na3YCl6, crystallizing in the cryolite structure type and isotypic with Na3GdCl6-II and Na3MCl6 (M = Sc, Dy-Lu), were prepared from a flux of YCl3, NaCN and NaN3; the trivalent yttrium is octahedrally coordinated by chlorine atoms with an average Y-Cl distance of 2.62 Å. The Y atom and one Na atom lie on centres of symmetry.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Y-Cl) = 0.001 Å
- R factor = 0.027
- wR factor = 0.059
- Data-to-parameter ratio = 25.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Y
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 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
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXTL.
trisodium yttrium(III) hexachloride
top
Crystal data top
Na3YCl6 | F(000) = 348 |
Mr = 370.58 | Dx = 2.439 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 6796 reflections |
a = 6.8558 (9) Å | θ = 3.5–28.3° |
b = 7.255 (1) Å | µ = 7.42 mm−1 |
c = 10.1444 (13) Å | T = 293 K |
β = 90.869 (3)° | Block, colorless |
V = 504.51 (12) Å3 | 0.13 × 0.09 × 0.04 mm |
Z = 2 | |
Data collection top
Bruker AXS APEX CCD diffractometer | 1258 independent reflections |
Radiation source: fine-focus sealed tube | 1055 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
ω scans | θmax = 28.3°, θmin = 3.5° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.498, Tmax = 0.743 | k = −9→9 |
6796 measured reflections | l = −13→13 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: isomorphous structure methods |
R[F2 > 2σ(F2)] = 0.027 | w = 1/[σ2(Fo2) + (0.0259P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.059 | (Δ/σ)max < 0.001 |
S = 1.02 | Δρmax = 0.39 e Å−3 |
1258 reflections | Δρmin = −0.38 e Å−3 |
49 parameters | |
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 | |
Y | 0.0000 | 0.5000 | 0.0000 | 0.02038 (11) | |
Cl1 | 0.13788 (11) | 0.56484 (11) | 0.23953 (7) | 0.03117 (18) | |
Cl2 | 0.16846 (11) | 0.80526 (11) | −0.07710 (9) | 0.0391 (2) | |
Cl3 | 0.31504 (11) | 0.32048 (11) | −0.06380 (8) | 0.0389 (2) | |
Na1 | 0.5226 (2) | 0.4251 (2) | 0.24215 (16) | 0.0514 (4) | |
Na2 | 0.5000 | 0.0000 | 0.0000 | 0.0354 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y | 0.02109 (19) | 0.02026 (19) | 0.01983 (18) | −0.00047 (15) | 0.00127 (13) | −0.00124 (16) |
Cl1 | 0.0353 (4) | 0.0362 (4) | 0.0219 (4) | 0.0031 (3) | −0.0041 (3) | −0.0036 (3) |
Cl2 | 0.0371 (4) | 0.0297 (4) | 0.0501 (5) | −0.0122 (3) | −0.0072 (4) | 0.0122 (3) |
Cl3 | 0.0339 (4) | 0.0358 (4) | 0.0472 (5) | 0.0147 (3) | 0.0114 (3) | 0.0092 (4) |
Na1 | 0.0449 (8) | 0.0363 (8) | 0.0730 (11) | −0.0064 (6) | 0.0033 (7) | 0.0028 (7) |
Na2 | 0.0354 (9) | 0.0300 (9) | 0.0405 (10) | 0.0037 (8) | −0.0053 (8) | −0.0034 (8) |
Geometric parameters (Å, º) top
Y—Cl3i | 2.6120 (8) | Na1—Cl3vi | 2.8247 (17) |
Y—Cl3 | 2.6120 (8) | Na1—Cl1vii | 2.8433 (16) |
Y—Cl2i | 2.6226 (8) | Na1—Cl2viii | 2.8517 (17) |
Y—Cl2 | 2.6226 (8) | Na1—Cl2vi | 3.1923 (18) |
Y—Cl1i | 2.6362 (8) | Na1—Cl3ix | 3.3091 (18) |
Y—Cl1 | 2.6362 (8) | Na1—Na2 | 3.9446 (16) |
Y—Na1ii | 4.0487 (16) | Na1—Yvii | 4.0487 (16) |
Y—Na1iii | 4.0487 (16) | Na1—Na2x | 4.1940 (15) |
Cl1—Na1 | 2.8254 (16) | Na2—Cl3xi | 2.7218 (8) |
Cl1—Na1iii | 2.8433 (16) | Na2—Cl2xii | 2.7786 (8) |
Cl1—Na2iii | 2.8588 (8) | Na2—Cl2vi | 2.7786 (8) |
Cl2—Na2iv | 2.7786 (8) | Na2—Cl1xiii | 2.8588 (8) |
Cl2—Na1v | 2.8517 (17) | Na2—Cl1vii | 2.8588 (8) |
Cl2—Na1vi | 3.1923 (18) | Na2—Na1xi | 3.9446 (16) |
Cl3—Na2 | 2.7218 (8) | Na2—Na1ii | 4.1940 (15) |
Cl3—Na1vi | 2.8247 (17) | Na2—Na1xiv | 4.1940 (15) |
Cl3—Na1ii | 3.3091 (18) | | |
| | | |
Cl3i—Y—Cl3 | 180.0 | Cl2viii—Na1—Na2 | 161.23 (5) |
Cl3i—Y—Cl2i | 88.72 (3) | Cl2vi—Na1—Na2 | 44.28 (2) |
Cl3—Y—Cl2i | 91.28 (3) | Cl3ix—Na1—Na2 | 88.11 (4) |
Cl3i—Y—Cl2 | 91.28 (3) | Cl3vi—Na1—Yvii | 158.57 (5) |
Cl3—Y—Cl2 | 88.72 (3) | Cl1—Na1—Yvii | 103.56 (4) |
Cl2i—Y—Cl2 | 180.0 | Cl1vii—Na1—Yvii | 40.42 (2) |
Cl3i—Y—Cl1i | 91.78 (3) | Cl2viii—Na1—Yvii | 97.10 (5) |
Cl3—Y—Cl1i | 88.22 (3) | Cl2vi—Na1—Yvii | 88.40 (4) |
Cl2i—Y—Cl1i | 88.33 (3) | Cl3ix—Na1—Yvii | 40.02 (2) |
Cl2—Y—Cl1i | 91.67 (3) | Na2—Na1—Yvii | 78.76 (3) |
Cl3i—Y—Cl1 | 88.22 (3) | Cl3vi—Na1—Na2x | 90.20 (4) |
Cl3—Y—Cl1 | 91.78 (3) | Cl1—Na1—Na2x | 132.77 (5) |
Cl2i—Y—Cl1 | 91.67 (3) | Cl1vii—Na1—Na2x | 112.17 (4) |
Cl2—Y—Cl1 | 88.33 (3) | Cl2viii—Na1—Na2x | 41.19 (2) |
Cl1i—Y—Cl1 | 180.0 | Cl2vi—Na1—Na2x | 82.95 (3) |
Cl3i—Y—Na1ii | 125.44 (3) | Cl3ix—Na1—Na2x | 40.42 (2) |
Cl3—Y—Na1ii | 54.56 (3) | Na2—Na1—Na2x | 120.83 (4) |
Cl2i—Y—Na1ii | 64.58 (3) | Yvii—Na1—Na2x | 74.51 (3) |
Cl2—Y—Na1ii | 115.42 (3) | Cl3—Na2—Cl3xi | 180.00 (3) |
Cl1i—Y—Na1ii | 44.38 (3) | Cl3—Na2—Cl2xii | 89.50 (3) |
Cl1—Y—Na1ii | 135.62 (3) | Cl3xi—Na2—Cl2xii | 90.50 (3) |
Cl3i—Y—Na1iii | 54.56 (3) | Cl3—Na2—Cl2vi | 90.50 (3) |
Cl3—Y—Na1iii | 125.44 (3) | Cl3xi—Na2—Cl2vi | 89.50 (3) |
Cl2i—Y—Na1iii | 115.42 (3) | Cl2xii—Na2—Cl2vi | 180.00 (3) |
Cl2—Y—Na1iii | 64.58 (3) | Cl3—Na2—Cl1xiii | 94.60 (2) |
Cl1i—Y—Na1iii | 135.62 (3) | Cl3xi—Na2—Cl1xiii | 85.40 (2) |
Cl1—Y—Na1iii | 44.38 (3) | Cl2xii—Na2—Cl1xiii | 86.37 (2) |
Na1ii—Y—Na1iii | 180.00 (4) | Cl2vi—Na2—Cl1xiii | 93.63 (2) |
Y—Cl1—Na1 | 105.44 (4) | Cl3—Na2—Cl1vii | 85.40 (2) |
Y—Cl1—Na1iii | 95.20 (4) | Cl3xi—Na2—Cl1vii | 94.60 (2) |
Na1—Cl1—Na1iii | 133.73 (5) | Cl2xii—Na2—Cl1vii | 93.63 (2) |
Y—Cl1—Na2iii | 134.72 (3) | Cl2vi—Na2—Cl1vii | 86.37 (2) |
Na1—Cl1—Na2iii | 104.71 (4) | Cl1xiii—Na2—Cl1vii | 180.00 (3) |
Na1iii—Cl1—Na2iii | 87.54 (4) | Cl3—Na2—Na1xi | 120.41 (3) |
Y—Cl2—Na2iv | 135.03 (3) | Cl3xi—Na2—Na1xi | 59.59 (3) |
Y—Cl2—Na1v | 128.26 (4) | Cl2xii—Na2—Na1xi | 53.34 (3) |
Na2iv—Cl2—Na1v | 96.29 (4) | Cl2vi—Na2—Na1xi | 126.66 (3) |
Y—Cl2—Na1vi | 90.74 (4) | Cl1xiii—Na2—Na1xi | 46.07 (3) |
Na2iv—Cl2—Na1vi | 82.38 (3) | Cl1vii—Na2—Na1xi | 133.93 (3) |
Na1v—Cl2—Na1vi | 104.53 (3) | Cl3—Na2—Na1 | 59.59 (3) |
Y—Cl3—Na2 | 138.68 (3) | Cl3xi—Na2—Na1 | 120.41 (3) |
Y—Cl3—Na1vi | 99.69 (4) | Cl2xii—Na2—Na1 | 126.66 (3) |
Na2—Cl3—Na1vi | 121.58 (4) | Cl2vi—Na2—Na1 | 53.34 (3) |
Y—Cl3—Na1ii | 85.42 (3) | Cl1xiii—Na2—Na1 | 133.93 (3) |
Na2—Cl3—Na1ii | 87.55 (3) | Cl1vii—Na2—Na1 | 46.07 (3) |
Na1vi—Cl3—Na1ii | 102.23 (3) | Na1xi—Na2—Na1 | 180.00 (4) |
Cl3vi—Na1—Cl1 | 97.84 (5) | Cl3—Na2—Na1ii | 52.03 (3) |
Cl3vi—Na1—Cl1vii | 143.05 (7) | Cl3xi—Na2—Na1ii | 127.97 (3) |
Cl1—Na1—Cl1vii | 88.18 (4) | Cl2xii—Na2—Na1ii | 42.52 (3) |
Cl3vi—Na1—Cl2viii | 79.98 (5) | Cl2vi—Na2—Na1ii | 137.48 (3) |
Cl1—Na1—Cl2viii | 94.49 (5) | Cl1xiii—Na2—Na1ii | 73.18 (3) |
Cl1vii—Na1—Cl2viii | 136.12 (6) | Cl1vii—Na2—Na1ii | 106.82 (3) |
Cl3vi—Na1—Cl2vi | 74.64 (4) | Na1xi—Na2—Na1ii | 71.94 (2) |
Cl1—Na1—Cl2vi | 144.06 (6) | Na1—Na2—Na1ii | 108.06 (2) |
Cl1vii—Na1—Cl2vi | 79.24 (4) | Cl3—Na2—Na1xiv | 127.97 (3) |
Cl2viii—Na1—Cl2vi | 117.87 (5) | Cl3xi—Na2—Na1xiv | 52.03 (3) |
Cl3vi—Na1—Cl3ix | 119.46 (5) | Cl2xii—Na2—Na1xiv | 137.48 (3) |
Cl1—Na1—Cl3ix | 139.10 (6) | Cl2vi—Na2—Na1xiv | 42.52 (3) |
Cl1vii—Na1—Cl3ix | 72.40 (4) | Cl1xiii—Na2—Na1xiv | 106.82 (3) |
Cl2viii—Na1—Cl3ix | 77.50 (4) | Cl1vii—Na2—Na1xiv | 73.18 (3) |
Cl2vi—Na1—Cl3ix | 68.24 (4) | Na1xi—Na2—Na1xiv | 108.06 (2) |
Cl3vi—Na1—Na2 | 97.13 (5) | Na1—Na2—Na1xiv | 71.94 (2) |
Cl1—Na1—Na2 | 104.29 (4) | Na1ii—Na2—Na1xiv | 180.00 (5) |
Cl1vii—Na1—Na2 | 46.39 (3) | | |
Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, y+1, z; (v) x−1/2, −y+3/2, z−1/2; (vi) −x+1, −y+1, −z; (vii) −x+1/2, y−1/2, −z+1/2; (viii) x+1/2, −y+3/2, z+1/2; (ix) x+1/2, −y+1/2, z+1/2; (x) −x+3/2, y+1/2, −z+1/2; (xi) −x+1, −y, −z; (xii) x, y−1, z; (xiii) x+1/2, −y+1/2, z−1/2; (xiv) −x+3/2, y−1/2, −z+1/2. |