Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229619007794/yp3185sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229619007794/yp3185Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229619007794/yp3185sup3.pdf |
CCDC reference: 1919592
Data collection: APEX2 (Bruker, 2017); cell refinement: APEX2 (Bruker, 2017); data reduction: APEX2 (Bruker, 2017); program(s) used to solve structure: SHELXT2017 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2017 (Sheldrick, 2015b); molecular graphics: ?; software used to prepare material for publication: SHELXL2017 (Sheldrick, 2015b).
K3Eu5(PO4)6 | F(000) = 2616 |
Mr = 1446.92 | Dx = 4.786 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 17.4950 (11) Å | Cell parameters from 1295 reflections |
b = 6.9483 (4) Å | θ = 2.0–24.9° |
c = 18.1452 (12) Å | µ = 16.61 mm−1 |
β = 114.447 (1)° | T = 296 K |
V = 2008.0 (2) Å3 | Block, colorless |
Z = 4 | 0.20 × 0.15 × 0.15 mm |
Bruker APEXII CCD diffractometer | 2117 reflections with I > 2σ(I) |
Detector resolution: 83.33 pixels mm-1 | Rint = 0.031 |
ω scans | θmax = 28.3°, θmin = 2.5° |
Absorption correction: multi-scan SADABS (Bruker, 2017) | h = −19→23 |
Tmin = 0.085, Tmax = 0.413 | k = −9→7 |
6490 measured reflections | l = −23→23 |
2460 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.027P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.026 | (Δ/σ)max = 0.001 |
wR(F2) = 0.062 | Δρmax = 1.13 e Å−3 |
S = 1.01 | Δρmin = −1.47 e Å−3 |
2460 reflections | Extinction correction: SHELXL2017 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
174 parameters | Extinction coefficient: 0.00040 (2) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. A single crystal with dimensions of 0.20 × 0.15 × 0.15 mm was mounted on a glass fiber for SC-XRD experiments. A set of intensity data was collected using a Bruker SMART APEX2 CCD equipped with a graphite-monochromated Mo Kα radiation source (λ = 0.71073 Å) with a tube power of 50 kV and 20 mA. The frames were collected at ambient temperature with a scan width of 0.5 in ω and integrated with the Bruker SAINT software package using a narrow-frame integration algorithm (Bruker, 2017). The unit cells were determined and refined by least-squares upon the refinement of XYZ-centeroids of reflections above 2σ(I). The data were then scaled for absorption using the SADABS programme of APEX2 package. Intensities of all measured reflections were corrected for Lp and multi-scan crystal absorption effects. The crystal structures of title complexes were solved using SHELX2017 crystallographic computing system (Sheldrick, 2015). |
x | y | z | Uiso*/Ueq | ||
K1 | −0.07658 (9) | 0.09710 (19) | −0.07467 (8) | 0.0177 (3) | |
K2 | 0.000000 | −0.1711 (3) | 0.250000 | 0.0477 (8) | |
Eu1 | 0.000000 | 0.36450 (5) | 0.250000 | 0.00466 (10) | |
Eu2 | 0.14403 (2) | 0.58607 (4) | 0.48109 (2) | 0.00453 (9) | |
Eu3 | 0.22012 (2) | 0.12515 (4) | 0.29233 (2) | 0.00454 (9) | |
P1 | 0.20791 (9) | 0.61898 (19) | 0.34185 (8) | 0.0042 (3) | |
P2 | 0.13583 (9) | 0.08484 (19) | 0.41326 (8) | 0.0041 (3) | |
P3 | 0.07312 (8) | 0.4036 (2) | 0.11707 (7) | 0.0039 (3) | |
O1 | 0.1227 (2) | 0.2509 (6) | 0.4603 (2) | 0.0095 (8) | |
O2 | 0.0975 (2) | −0.1012 (5) | 0.4269 (2) | 0.0099 (8) | |
O3 | 0.0928 (2) | 0.1276 (5) | 0.3200 (2) | 0.0064 (8) | |
O4 | 0.2286 (2) | 0.0676 (5) | 0.4260 (2) | 0.0068 (8) | |
O5 | 0.2554 (2) | 0.4596 (5) | 0.3180 (2) | 0.0080 (8) | |
O6 | 0.1207 (2) | 0.5480 (5) | 0.3297 (2) | 0.0068 (8) | |
O7 | 0.2538 (2) | 0.6711 (5) | 0.4307 (2) | 0.0066 (8) | |
O8 | 0.1999 (2) | 0.7859 (5) | 0.2837 (2) | 0.0082 (8) | |
O9 | 0.0997 (2) | 0.2527 (6) | 0.1859 (2) | 0.0087 (8) | |
O10 | 0.0048 (2) | 0.5229 (5) | 0.1291 (2) | 0.0072 (8) | |
O11 | 0.1462 (2) | 0.5361 (5) | 0.1234 (2) | 0.0091 (8) | |
O12 | 0.0475 (2) | 0.3043 (5) | 0.0357 (2) | 0.0070 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
K1 | 0.0158 (7) | 0.0120 (7) | 0.0187 (7) | 0.0032 (5) | 0.0007 (5) | −0.0042 (5) |
K2 | 0.0331 (14) | 0.0055 (11) | 0.0623 (17) | 0.000 | −0.0225 (12) | 0.000 |
Eu1 | 0.00403 (19) | 0.00320 (19) | 0.00728 (19) | 0.000 | 0.00288 (15) | 0.000 |
Eu2 | 0.00473 (15) | 0.00307 (15) | 0.00693 (15) | 0.00021 (10) | 0.00355 (11) | 0.00003 (9) |
Eu3 | 0.00474 (15) | 0.00313 (15) | 0.00682 (15) | 0.00011 (10) | 0.00344 (11) | 0.00051 (9) |
P1 | 0.0052 (7) | 0.0028 (7) | 0.0067 (7) | −0.0015 (5) | 0.0047 (6) | −0.0005 (5) |
P2 | 0.0045 (7) | 0.0026 (7) | 0.0068 (6) | 0.0009 (5) | 0.0040 (5) | 0.0015 (5) |
P3 | 0.0023 (7) | 0.0053 (7) | 0.0048 (7) | 0.0005 (5) | 0.0021 (6) | 0.0001 (5) |
O1 | 0.011 (2) | 0.005 (2) | 0.012 (2) | 0.0020 (16) | 0.0049 (16) | −0.0043 (15) |
O2 | 0.008 (2) | 0.003 (2) | 0.019 (2) | −0.0006 (15) | 0.0063 (17) | 0.0021 (15) |
O3 | 0.0067 (19) | 0.0059 (19) | 0.0057 (18) | −0.0013 (15) | 0.0018 (15) | 0.0003 (14) |
O4 | 0.0074 (19) | 0.0041 (19) | 0.011 (2) | −0.0011 (15) | 0.0054 (16) | 0.0011 (15) |
O5 | 0.011 (2) | 0.005 (2) | 0.010 (2) | −0.0002 (16) | 0.0077 (16) | 0.0011 (15) |
O6 | 0.0066 (19) | 0.0042 (19) | 0.012 (2) | 0.0003 (15) | 0.0060 (16) | 0.0009 (15) |
O7 | 0.0064 (19) | 0.0065 (19) | 0.0079 (18) | 0.0010 (15) | 0.0038 (15) | −0.0021 (15) |
O8 | 0.010 (2) | 0.004 (2) | 0.012 (2) | −0.0007 (16) | 0.0070 (16) | 0.0014 (15) |
O9 | 0.009 (2) | 0.008 (2) | 0.011 (2) | 0.0036 (16) | 0.0063 (16) | 0.0031 (15) |
O10 | 0.0051 (19) | 0.010 (2) | 0.010 (2) | 0.0011 (15) | 0.0064 (15) | −0.0008 (15) |
O11 | 0.0058 (19) | 0.010 (2) | 0.012 (2) | −0.0043 (16) | 0.0039 (16) | −0.0008 (16) |
O12 | 0.008 (2) | 0.0048 (19) | 0.0100 (19) | 0.0014 (15) | 0.0055 (15) | 0.0006 (15) |
K1—O12 | 2.683 (4) | Eu2—O2viii | 2.385 (4) |
K1—O1i | 2.736 (4) | Eu2—O12ix | 2.409 (3) |
K1—O5ii | 2.801 (4) | Eu2—O4x | 2.416 (4) |
K1—O11iii | 2.806 (4) | Eu2—O7xi | 2.497 (4) |
K1—O12iv | 2.871 (4) | Eu2—O7 | 2.515 (3) |
K1—O2v | 3.034 (4) | Eu2—O10i | 2.581 (4) |
K1—O9iv | 3.077 (4) | Eu2—O6 | 2.618 (3) |
K1—O2i | 3.168 (4) | Eu2—O11ix | 2.703 (4) |
K1—O10iii | 3.248 (4) | Eu3—O11xii | 2.287 (4) |
K2—O3 | 2.617 (4) | Eu3—O9 | 2.363 (4) |
K2—O3i | 2.617 (4) | Eu3—O8vii | 2.379 (4) |
K2—O6vi | 2.798 (4) | Eu3—O5 | 2.400 (4) |
K2—O6vii | 2.798 (4) | Eu3—O4 | 2.402 (3) |
K2—O2i | 2.986 (4) | Eu3—O3 | 2.478 (4) |
K2—O2 | 2.986 (4) | Eu3—O5xii | 2.495 (3) |
K2—O10vii | 3.080 (4) | Eu3—O8xii | 2.590 (3) |
K2—O10vi | 3.080 (4) | P1—O7 | 1.518 (4) |
K2—O8vi | 3.305 (4) | P1—O6 | 1.531 (4) |
K2—O8vii | 3.305 (4) | P1—O8 | 1.535 (4) |
Eu1—O3 | 2.291 (4) | P1—O5 | 1.550 (4) |
Eu1—O3i | 2.291 (4) | P2—O1 | 1.508 (4) |
Eu1—O6 | 2.376 (4) | P2—O2 | 1.523 (4) |
Eu1—O6i | 2.376 (4) | P2—O4 | 1.547 (4) |
Eu1—O10i | 2.486 (4) | P2—O3 | 1.570 (4) |
Eu1—O10 | 2.486 (4) | P3—O12 | 1.519 (4) |
Eu1—O9i | 2.585 (3) | P3—O11 | 1.541 (4) |
Eu1—O9 | 2.585 (3) | P3—O10 | 1.543 (4) |
Eu2—O1 | 2.364 (4) | P3—O9 | 1.548 (4) |
O7—P1—O6 | 106.7 (2) | O1—P2—O3 | 110.3 (2) |
O7—P1—O8 | 114.1 (2) | O2—P2—O3 | 106.8 (2) |
O6—P1—O8 | 110.0 (2) | O4—P2—O3 | 100.5 (2) |
O7—P1—O5 | 111.0 (2) | O12—P3—O11 | 104.2 (2) |
O6—P1—O5 | 110.4 (2) | O12—P3—O10 | 116.6 (2) |
O8—P1—O5 | 104.8 (2) | O11—P3—O10 | 109.6 (2) |
O1—P2—O2 | 112.2 (2) | O12—P3—O9 | 110.2 (2) |
O1—P2—O4 | 111.8 (2) | O11—P3—O9 | 112.4 (2) |
O2—P2—O4 | 114.5 (2) | O10—P3—O9 | 104.0 (2) |
Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x, −y+1, −z; (iv) −x, −y, −z; (v) x, −y, z−1/2; (vi) −x, y−1, −z+1/2; (vii) x, y−1, z; (viii) x, y+1, z; (ix) x, −y+1, z+1/2; (x) −x+1/2, −y+1/2, −z+1; (xi) −x+1/2, −y+3/2, −z+1; (xii) −x+1/2, y−1/2, −z+1/2. |