Single crystals of potassium dysprosium polyphosphate, KDy(PO3)4, were prepared by the flux method. The title compound crystallizes in structure type IV of KLn(PO3)4 (Ln = lanthanide) compounds. Two helical polyphosphate chains cross the unit cell along [101] with a repeat unit of eight tetrahedra, creating channels where the Dy and K atoms are situated. They have coordination numbers of 8 and 9, respectively.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (P-O)= 0.004 Å
- R factor = 0.027
- wR factor = 0.059
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
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No errors found in this datablock
Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.
potassium dysprosium polyphosphate
top
Crystal data top
KDy(PO3)4 | F(000) = 964 |
Mr = 517.48 | Dx = 3.562 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2751 reflections |
a = 10.2822 (4) Å | θ = 2.3–24.3° |
b = 8.9006 (3) Å | µ = 8.90 mm−1 |
c = 10.9848 (4) Å | T = 298 K |
β = 106.284 (2)° | Cubic, colourless |
V = 964.97 (6) Å3 | 0.14 × 0.14 × 0.14 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2270 independent reflections |
Radiation source: fine-focus sealed tube | 2054 reflections with I > 2σ(I) |
Detector resolution: 9 pixels mm-1 | Rint = 0.023 |
φ and ω scans | θmax = 27.9°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.288, Tmax = 0.291 | k = −11→10 |
3857 measured reflections | l = −14→14 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.027 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.059 | w = 1/[σ2(Fo2) + (0.0165P)2 + 4.0271P] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max < 0.001 |
2270 reflections | Δρmax = 1.98 e Å−3 |
163 parameters | Δρmin = −1.03 e Å−3 |
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 | |
Dy | 0.999226 (19) | 0.22606 (2) | 0.183461 (18) | 0.00897 (8) | |
K | 0.67724 (12) | −0.43184 (13) | −0.04142 (10) | 0.0224 (2) | |
P1 | 0.74585 (11) | −0.02656 (13) | 0.22082 (11) | 0.0095 (2) | |
P2 | 0.67400 (11) | 0.10862 (13) | −0.02360 (10) | 0.0094 (2) | |
P3 | 0.64637 (11) | −0.09119 (12) | −0.24255 (11) | 0.0094 (2) | |
P4 | 0.45889 (11) | −0.32647 (12) | −0.36526 (11) | 0.0094 (2) | |
O1 | 0.8317 (3) | −0.5948 (4) | 0.1977 (3) | 0.0134 (6) | |
O2 | 0.8528 (3) | 0.0846 (4) | 0.2822 (3) | 0.0134 (6) | |
O3 | 0.6379 (3) | 0.0460 (4) | 0.1001 (3) | 0.0123 (6) | |
O4 | 0.8123 (3) | −0.1580 (3) | 0.1575 (3) | 0.0116 (6) | |
O5 | 0.8151 (3) | 0.1651 (4) | 0.0166 (3) | 0.0155 (7) | |
O6 | 0.5656 (3) | 0.2116 (3) | −0.0947 (3) | 0.0124 (6) | |
O7 | 0.6694 (3) | −0.0471 (4) | −0.0979 (3) | 0.0148 (7) | |
O8 | 0.7352 (3) | −0.6772 (4) | −0.2436 (3) | 0.0150 (7) | |
O9 | 0.6007 (3) | 0.0416 (4) | −0.3248 (3) | 0.0152 (7) | |
O10 | 0.5221 (3) | −0.2052 (3) | −0.2567 (3) | 0.0134 (6) | |
O11 | 0.4368 (3) | −0.2579 (4) | −0.4918 (3) | 0.0148 (7) | |
O12 | 0.5367 (3) | −0.4672 (3) | −0.3314 (3) | 0.0154 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Dy | 0.00845 (12) | 0.00866 (12) | 0.00974 (12) | −0.00045 (7) | 0.00244 (8) | −0.00073 (7) |
K | 0.0277 (6) | 0.0246 (6) | 0.0139 (5) | −0.0036 (5) | 0.0045 (4) | 0.0008 (4) |
P1 | 0.0087 (5) | 0.0098 (5) | 0.0108 (5) | −0.0003 (4) | 0.0040 (4) | 0.0002 (4) |
P2 | 0.0086 (5) | 0.0105 (5) | 0.0084 (5) | −0.0001 (4) | 0.0011 (4) | −0.0005 (4) |
P3 | 0.0087 (5) | 0.0092 (5) | 0.0097 (5) | −0.0002 (4) | 0.0017 (4) | −0.0011 (4) |
P4 | 0.0086 (5) | 0.0081 (5) | 0.0114 (5) | −0.0006 (4) | 0.0029 (4) | −0.0008 (4) |
O1 | 0.0110 (15) | 0.0158 (16) | 0.0154 (16) | 0.0041 (12) | 0.0070 (13) | 0.0007 (13) |
O2 | 0.0115 (15) | 0.0150 (16) | 0.0141 (16) | −0.0027 (12) | 0.0044 (13) | −0.0020 (12) |
O3 | 0.0083 (15) | 0.0153 (16) | 0.0136 (16) | 0.0012 (12) | 0.0038 (12) | 0.0029 (13) |
O4 | 0.0094 (14) | 0.0092 (15) | 0.0172 (16) | 0.0006 (12) | 0.0053 (12) | −0.0026 (12) |
O5 | 0.0120 (16) | 0.0222 (17) | 0.0120 (16) | −0.0026 (13) | 0.0030 (13) | −0.0031 (13) |
O6 | 0.0114 (15) | 0.0135 (16) | 0.0131 (16) | 0.0043 (12) | 0.0050 (12) | 0.0008 (12) |
O7 | 0.0201 (17) | 0.0120 (15) | 0.0106 (15) | 0.0015 (13) | 0.0014 (13) | −0.0025 (12) |
O8 | 0.0101 (15) | 0.0164 (16) | 0.0177 (16) | −0.0011 (13) | 0.0025 (13) | 0.0039 (13) |
O9 | 0.0176 (17) | 0.0109 (15) | 0.0172 (17) | 0.0014 (13) | 0.0053 (14) | 0.0003 (13) |
O10 | 0.0133 (16) | 0.0124 (16) | 0.0144 (16) | −0.0041 (12) | 0.0036 (13) | −0.0032 (13) |
O11 | 0.0130 (16) | 0.0204 (17) | 0.0122 (16) | 0.0011 (13) | 0.0054 (13) | 0.0013 (13) |
O12 | 0.0127 (16) | 0.0100 (15) | 0.0253 (18) | −0.0001 (13) | 0.0083 (14) | 0.0025 (13) |
Geometric parameters (Å, º) top
Dy—O5 | 2.301 (3) | P2—O5 | 1.481 (3) |
Dy—O9i | 2.329 (3) | P2—O6 | 1.485 (3) |
Dy—O12ii | 2.349 (3) | P2—O7 | 1.603 (3) |
Dy—O8ii | 2.372 (3) | P2—O3 | 1.605 (3) |
Dy—O11iii | 2.380 (3) | P3—O8iii | 1.482 (3) |
Dy—O1iv | 2.384 (3) | P3—O9 | 1.482 (3) |
Dy—O6i | 2.404 (3) | P3—O7 | 1.588 (3) |
Dy—O2 | 2.438 (3) | P3—O10 | 1.605 (3) |
Dy—Kii | 4.0298 (11) | P3—Kiii | 3.6532 (16) |
Dy—Kv | 4.4459 (11) | P4—O11 | 1.476 (3) |
K—O2vi | 2.953 (3) | P4—O12 | 1.477 (3) |
K—O1 | 3.031 (3) | P4—O4x | 1.601 (3) |
K—O9vii | 3.052 (3) | P4—O10 | 1.605 (3) |
K—O11ii | 3.075 (3) | P4—Kx | 3.7781 (16) |
K—O12 | 3.123 (4) | O1—P1vi | 1.485 (3) |
K—O10 | 3.177 (3) | O1—Dyviii | 2.384 (3) |
K—O8 | 3.287 (4) | O2—Kix | 2.953 (3) |
K—O4 | 3.308 (3) | O4—P4ii | 1.601 (3) |
K—O6viii | 3.370 (3) | O6—Dyxi | 2.404 (3) |
K—P1vi | 3.4895 (16) | O6—Kiv | 3.370 (3) |
K—P3vii | 3.6532 (16) | O8—P3vii | 1.482 (3) |
K—P3 | 3.7123 (16) | O8—Dyx | 2.372 (3) |
P1—O1ix | 1.485 (3) | O9—Dyxi | 2.329 (3) |
P1—O2 | 1.492 (3) | O9—Kiii | 3.052 (3) |
P1—O3 | 1.607 (3) | O11—Dyvii | 2.380 (3) |
P1—O4 | 1.608 (3) | O11—Kx | 3.075 (3) |
P1—Kix | 3.4895 (16) | O12—Dyx | 2.349 (3) |
| | | |
O5—Dy—O9i | 117.12 (12) | O12—K—P3vii | 58.02 (6) |
O5—Dy—O12ii | 80.08 (12) | O10—K—P3vii | 90.00 (7) |
O9i—Dy—O12ii | 141.63 (11) | O8—K—P3vii | 23.91 (6) |
O5—Dy—O8ii | 139.57 (11) | O4—K—P3vii | 121.48 (6) |
O9i—Dy—O8ii | 75.47 (11) | O6viii—K—P3vii | 74.25 (6) |
O12ii—Dy—O8ii | 70.83 (11) | P1vi—K—P3vii | 123.26 (4) |
O5—Dy—O11iii | 71.30 (11) | O2vi—K—P3 | 121.26 (7) |
O9i—Dy—O11iii | 70.99 (11) | O1—K—P3 | 147.49 (7) |
O12ii—Dy—O11iii | 84.60 (11) | O9vii—K—P3 | 74.17 (7) |
O8ii—Dy—O11iii | 78.42 (11) | O11ii—K—P3 | 65.30 (7) |
O5—Dy—O1iv | 76.20 (11) | O12—K—P3 | 62.45 (6) |
O9i—Dy—O1iv | 75.44 (11) | O10—K—P3 | 25.45 (6) |
O12ii—Dy—O1iv | 142.74 (11) | O8—K—P3 | 98.16 (6) |
O8ii—Dy—O1iv | 142.17 (11) | O4—K—P3 | 75.02 (6) |
O11iii—Dy—O1iv | 113.70 (11) | O6viii—K—P3 | 134.23 (6) |
O5—Dy—O6i | 142.95 (11) | P1vi—K—P3 | 139.05 (4) |
O9i—Dy—O6i | 80.31 (11) | P3vii—K—P3 | 84.59 (3) |
O12ii—Dy—O6i | 106.95 (11) | O1ix—P1—O2 | 116.82 (19) |
O8ii—Dy—O6i | 74.19 (11) | O1ix—P1—O3 | 107.38 (18) |
O11iii—Dy—O6i | 144.36 (11) | O2—P1—O3 | 110.93 (18) |
O1iv—Dy—O6i | 77.53 (11) | O1ix—P1—O4 | 109.14 (18) |
O5—Dy—O2 | 76.09 (11) | O2—P1—O4 | 109.19 (17) |
O9i—Dy—O2 | 144.59 (11) | O3—P1—O4 | 102.39 (17) |
O12ii—Dy—O2 | 70.01 (11) | O1ix—P1—Kix | 59.92 (13) |
O8ii—Dy—O2 | 117.12 (11) | O2—P1—Kix | 56.92 (13) |
O11iii—Dy—O2 | 141.54 (11) | O3—P1—Kix | 130.12 (13) |
O1iv—Dy—O2 | 76.62 (11) | O4—P1—Kix | 127.48 (13) |
O6i—Dy—O2 | 72.75 (10) | O5—P2—O6 | 118.39 (19) |
O5—Dy—Kii | 122.93 (9) | O5—P2—O7 | 109.40 (19) |
O9i—Dy—Kii | 119.47 (8) | O6—P2—O7 | 110.81 (18) |
O12ii—Dy—Kii | 50.66 (8) | O5—P2—O3 | 107.76 (18) |
O8ii—Dy—Kii | 54.64 (8) | O6—P2—O3 | 110.00 (17) |
O11iii—Dy—Kii | 121.49 (8) | O7—P2—O3 | 98.64 (17) |
O1iv—Dy—Kii | 124.75 (8) | O8iii—P3—O9 | 118.61 (19) |
O6i—Dy—Kii | 56.61 (8) | O8iii—P3—O7 | 109.49 (18) |
O2—Dy—Kii | 62.48 (8) | O9—P3—O7 | 110.23 (18) |
O5—Dy—Kv | 110.32 (8) | O8iii—P3—O10 | 108.56 (18) |
O9i—Dy—Kv | 39.94 (8) | O9—P3—O10 | 109.72 (18) |
O12ii—Dy—Kv | 103.07 (8) | O7—P3—O10 | 98.31 (18) |
O8ii—Dy—Kv | 53.05 (8) | O8iii—P3—Kiii | 64.03 (14) |
O11iii—Dy—Kv | 40.97 (8) | O9—P3—Kiii | 54.87 (13) |
O1iv—Dy—Kv | 111.90 (8) | O7—P3—Kiii | 126.29 (13) |
O6i—Dy—Kv | 103.48 (7) | O10—P3—Kiii | 135.18 (13) |
O2—Dy—Kv | 170.07 (8) | O8iii—P3—K | 72.74 (14) |
Kii—Dy—Kv | 107.679 (15) | O9—P3—K | 166.87 (14) |
O2vi—K—O1 | 50.14 (8) | O7—P3—K | 69.05 (12) |
O2vi—K—O9vii | 139.73 (9) | O10—P3—K | 58.28 (12) |
O1—K—O9vii | 95.70 (9) | Kiii—P3—K | 136.76 (4) |
O2vi—K—O11ii | 97.02 (9) | O11—P4—O12 | 121.2 (2) |
O1—K—O11ii | 83.77 (9) | O11—P4—O4x | 106.24 (18) |
O9vii—K—O11ii | 53.02 (9) | O12—P4—O4x | 110.76 (18) |
O2vi—K—O12 | 147.67 (9) | O11—P4—O10 | 110.16 (19) |
O1—K—O12 | 144.67 (9) | O12—P4—O10 | 107.81 (19) |
O9vii—K—O12 | 72.29 (9) | O4x—P4—O10 | 98.32 (17) |
O11ii—K—O12 | 111.50 (9) | O11—P4—K | 152.72 (14) |
O2vi—K—O10 | 121.34 (9) | O12—P4—K | 53.98 (14) |
O1—K—O10 | 168.76 (9) | O4x—P4—K | 99.74 (12) |
O9vii—K—O10 | 88.74 (9) | O10—P4—K | 56.91 (12) |
O11ii—K—O10 | 90.74 (9) | O11—P4—Kx | 51.13 (13) |
O12—K—O10 | 46.57 (8) | O12—P4—Kx | 158.19 (14) |
O2vi—K—O8 | 140.58 (9) | O4x—P4—Kx | 60.85 (11) |
O1—K—O8 | 96.74 (9) | O10—P4—Kx | 93.65 (13) |
O9vii—K—O8 | 47.24 (8) | K—P4—Kx | 143.72 (4) |
O11ii—K—O8 | 99.89 (9) | P1vi—O1—Dyviii | 146.39 (19) |
O12—K—O8 | 50.46 (8) | P1vi—O1—K | 94.99 (14) |
O10—K—O8 | 93.85 (8) | Dyviii—O1—K | 118.42 (12) |
O2vi—K—O4 | 57.63 (8) | P1—O2—Dy | 127.61 (18) |
O1—K—O4 | 76.07 (9) | P1—O2—Kix | 98.03 (15) |
O9vii—K—O4 | 98.22 (8) | Dy—O2—Kix | 134.36 (12) |
O11ii—K—O4 | 45.22 (8) | P2—O3—P1 | 124.6 (2) |
O12—K—O4 | 137.45 (9) | P4ii—O4—P1 | 131.5 (2) |
O10—K—O4 | 93.11 (8) | P4ii—O4—K | 94.15 (13) |
O8—K—O4 | 144.49 (8) | P1—O4—K | 132.15 (15) |
O2vi—K—O6viii | 95.25 (9) | P2—O5—Dy | 146.8 (2) |
O1—K—O6viii | 76.71 (8) | P2—O6—Dyxi | 129.32 (18) |
O9vii—K—O6viii | 96.20 (9) | P2—O6—Kiv | 108.71 (15) |
O11ii—K—O6viii | 141.68 (9) | Dyxi—O6—Kiv | 86.84 (9) |
O12—K—O6viii | 71.94 (8) | P3—O7—P2 | 134.3 (2) |
O10—K—O6viii | 113.15 (8) | P3vii—O8—Dyx | 148.5 (2) |
O8—K—O6viii | 51.27 (8) | P3vii—O8—K | 92.06 (15) |
O4—K—O6viii | 150.24 (8) | Dyx—O8—K | 89.30 (10) |
O2vi—K—P1vi | 25.05 (6) | P3—O9—Dyxi | 138.9 (2) |
O1—K—P1vi | 25.09 (6) | P3—O9—Kiii | 101.73 (16) |
O9vii—K—P1vi | 118.61 (7) | Dyxi—O9—Kiii | 110.72 (12) |
O11ii—K—P1vi | 90.80 (7) | P4—O10—P3 | 130.0 (2) |
O12—K—P1vi | 156.08 (7) | P4—O10—K | 98.06 (14) |
O10—K—P1vi | 146.01 (7) | P3—O10—K | 96.27 (14) |
O8—K—P1vi | 119.26 (7) | P4—O11—Dyvii | 143.2 (2) |
O4—K—P1vi | 64.97 (6) | P4—O11—Kx | 106.91 (16) |
O6viii—K—P1vi | 85.28 (6) | Dyvii—O11—Kx | 108.53 (12) |
O2vi—K—P3vii | 148.31 (7) | P4—O12—Dyx | 139.62 (19) |
O1—K—P3vii | 98.17 (7) | P4—O12—K | 103.54 (16) |
O9vii—K—P3vii | 23.40 (6) | Dyx—O12—K | 93.77 (11) |
O11ii—K—P3vii | 76.35 (7) | | |
Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) x+1/2, −y−1/2, z+1/2; (iii) −x+3/2, y+1/2, −z−1/2; (iv) x, y+1, z; (v) −x+2, −y, −z; (vi) −x+3/2, y−1/2, −z+1/2; (vii) −x+3/2, y−1/2, −z−1/2; (viii) x, y−1, z; (ix) −x+3/2, y+1/2, −z+1/2; (x) x−1/2, −y−1/2, z−1/2; (xi) x−1/2, −y+1/2, z−1/2. |