Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807058588/wm2157sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807058588/wm2157Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (P-O) = 0.002 Å
- Disorder in main residue
- R factor = 0.021
- wR factor = 0.045
- Data-to-parameter ratio = 22.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... -4 PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... -4 PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... -4 PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... m PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... m PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... m
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99 PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 7 Ang. PLAT301_ALERT_3_C Main Residue Disorder ......................... 11.00 Perc.
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 34.99 From the CIF: _reflns_number_total 1434 Count of symmetry unique reflns 812 Completeness (_total/calc) 176.60% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 622 Fraction of Friedel pairs measured 0.766 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3
0 ALERT level A = In general: serious problem 6 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For the previous powder study of the title compound, see Aatiq et al. (2006). The crystal structure of the mineral langbeinite was determined by Zemann & Zemann (1957). Other phosphates with langbeinite-type structure have been investigated by Norberg (2002), Ogorodnyk et al. (2006), Ogorodnyk, Zatovsky & Slobodyanik (2007), Ogorodnyk, Zatovsky, Baumer et al. (2007), and Orlova et al. (2003).
Crystals of (I) were obtained in the pseudo-quaternary system K2O—P2O5—SnO2—Fe2O3 using the high-temperature flux crystallization technique. A well ground mixture of 0.9 g SnO2 (6.0 mmol), 1,44 g Fe2O3 (9.0 mmol), 6,63 g KPO3 (56.2 mmol) and 1,03 g K4P2O7 (3.1 mmol) was placed into a platinum crucible, and was heated up to 1373 K. The melt was exposed during 6 h at this temperature to dissolve the metal oxides, and then was cooled down 1013 K at a rate 25 K/h. At the final stage of crystallization the melt was sustained under isothermal conditions for 1 h to gain equilibrium, and was then poured out onto a copper sheet for quenching. Yellow-brownish crystals with mostly tetrahedral shape were recovered from the remaining flux by leaching out with deionized water.
As suggested from the previous powder refinement (Aatiq et al., 2006), the Fe and Sn atoms are statistically distributed. Their coordinates and displacement ellipsoids were constrained. Three additional restraints were applied, viz. two for full occupancies of the Fe/Sn sites and one for the total charge of iron and tin (charge sum = 7.00). The highest peak in the final Fourier map is located 0.87 Å from atom P1, and the deepest hole is 1.05 Å from atom Sn1.
Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).
K2FeSn(PO4)3 | Dx = 3.664 Mg m−3 |
Mr = 537.65 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, P213 | Cell parameters from 5809 reflections |
Hall symbol: P 2ac 2ab 3 | θ = 2.9–35.0° |
a = 9.91473 (7) Å | µ = 5.47 mm−1 |
V = 974.64 (1) Å3 | T = 293 K |
Z = 4 | Tetrahedron, yellow brown |
F(000) = 1020 | 0.08 × 0.06 × 0.05 mm |
XCalibur-3 diffractometer | 1434 independent reflections |
Radiation source: fine focus sealed tube | 1338 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ϕ and ω scans | θmax = 35.0°, θmin = 2.9° |
Absorption correction: multi-scan (Blessing; 1995) | h = −13→16 |
Tmin = 0.669, Tmax = 0.772 | k = −15→15 |
5809 measured reflections | l = −15→16 |
Refinement on F2 | w = 1/[σ2(Fo2) + (0.0194P)2 + 0.5777P] where P = (Fo2 + 2Fc2)/3 |
Least-squares matrix: full | (Δ/σ)max < 0.001 |
R[F2 > 2σ(F2)] = 0.021 | Δρmax = 0.50 e Å−3 |
wR(F2) = 0.045 | Δρmin = −0.57 e Å−3 |
S = 1.1 | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1434 reflections | Extinction coefficient: 0.0058 (5) |
63 parameters | Absolute structure: Flack (1983), 621 Friedel Pairs |
3 restraints | Absolute structure parameter: −0.03 (2) |
K2FeSn(PO4)3 | Z = 4 |
Mr = 537.65 | Mo Kα radiation |
Cubic, P213 | µ = 5.47 mm−1 |
a = 9.91473 (7) Å | T = 293 K |
V = 974.64 (1) Å3 | 0.08 × 0.06 × 0.05 mm |
XCalibur-3 diffractometer | 1434 independent reflections |
Absorption correction: multi-scan (Blessing; 1995) | 1338 reflections with I > 2σ(I) |
Tmin = 0.669, Tmax = 0.772 | Rint = 0.035 |
5809 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 3 restraints |
wR(F2) = 0.045 | Δρmax = 0.50 e Å−3 |
S = 1.1 | Δρmin = −0.57 e Å−3 |
1434 reflections | Absolute structure: Flack (1983), 621 Friedel Pairs |
63 parameters | Absolute structure parameter: −0.03 (2) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
K1 | 0.70742 (8) | 0.70742 (8) | 0.70742 (8) | 0.0278 (3) | |
K2 | 0.93262 (6) | 0.93262 (6) | 0.93262 (6) | 0.0220 (2) | |
Fe1 | 0.14686 (2) | 0.14686 (2) | 0.14686 (2) | 0.00732 (8) | 0.4464 (11) |
Fe2 | 0.41421 (2) | 0.41421 (2) | 0.41421 (2) | 0.00737 (8) | 0.5538 (12) |
Sn1 | 0.14686 (2) | 0.14686 (2) | 0.14686 (2) | 0.00732 (8) | 0.5536 (11) |
Sn2 | 0.41421 (2) | 0.41421 (2) | 0.41421 (2) | 0.00737 (8) | 0.4462 (11) |
P1 | 0.46113 (6) | 0.22920 (6) | 0.12592 (6) | 0.00634 (10) | |
O1 | 0.31483 (18) | 0.2389 (2) | 0.0776 (2) | 0.0154 (4) | |
O2 | 0.5516 (2) | 0.2973 (2) | 0.0223 (2) | 0.0180 (4) | |
O3 | 0.5006 (2) | 0.08280 (19) | 0.1516 (2) | 0.0172 (3) | |
O4 | 0.4825 (2) | 0.3057 (2) | 0.2572 (2) | 0.0203 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
K1 | 0.0278 (3) | 0.0278 (3) | 0.0278 (3) | −0.0001 (3) | −0.0001 (3) | −0.0001 (3) |
K2 | 0.0220 (2) | 0.0220 (2) | 0.0220 (2) | −0.0026 (2) | −0.0026 (2) | −0.0026 (2) |
Fe1 | 0.00732 (8) | 0.00732 (8) | 0.00732 (8) | −0.00009 (7) | −0.00009 (7) | −0.00009 (7) |
Fe2 | 0.00737 (8) | 0.00737 (8) | 0.00737 (8) | −0.00050 (7) | −0.00050 (7) | −0.00050 (7) |
Sn1 | 0.00732 (8) | 0.00732 (8) | 0.00732 (8) | −0.00009 (7) | −0.00009 (7) | −0.00009 (7) |
Sn2 | 0.00737 (8) | 0.00737 (8) | 0.00737 (8) | −0.00050 (7) | −0.00050 (7) | −0.00050 (7) |
P1 | 0.0061 (2) | 0.0066 (2) | 0.0063 (2) | −0.00007 (18) | 0.00116 (17) | −0.00006 (17) |
O1 | 0.0068 (7) | 0.0201 (9) | 0.0194 (9) | −0.0031 (6) | −0.0024 (7) | 0.0086 (8) |
O2 | 0.0155 (9) | 0.0211 (10) | 0.0174 (9) | −0.0008 (7) | 0.0091 (7) | 0.0087 (8) |
O3 | 0.0220 (9) | 0.0078 (7) | 0.0219 (9) | 0.0063 (7) | 0.0031 (8) | 0.0032 (8) |
O4 | 0.0240 (11) | 0.0235 (11) | 0.0135 (9) | −0.0030 (8) | 0.0022 (8) | −0.0117 (8) |
K1—O1i | 2.852 (2) | Fe1—O1xiv | 2.0195 (19) |
K1—O1ii | 2.852 (2) | Fe1—K2xv | 3.6790 (12) |
K1—O1iii | 2.852 (2) | Fe1—K1xvi | 3.8453 (6) |
K1—O2iv | 3.013 (2) | Fe1—K1xvii | 3.8453 (6) |
K1—O2v | 3.013 (2) | Fe1—K1xviii | 3.8453 (6) |
K1—O2vi | 3.013 (2) | Fe2—O3i | 1.9830 (19) |
K1—O4iv | 3.117 (2) | Fe2—O3ii | 1.9830 (19) |
K1—O4v | 3.117 (2) | Fe2—O3iii | 1.9830 (19) |
K1—O4vi | 3.117 (2) | Fe2—O4 | 2.010 (2) |
K1—P1iv | 3.4419 (9) | Fe2—O4xiv | 2.010 (2) |
K1—P1v | 3.4419 (9) | Fe2—O4xiii | 2.010 (2) |
K1—P1vi | 3.4419 (9) | Fe2—K2xix | 3.7636 (4) |
K2—O3iv | 2.868 (2) | Fe2—K2xx | 3.7636 (4) |
K2—O3vi | 2.868 (2) | Fe2—K2xxi | 3.7636 (4) |
K2—O3v | 2.868 (2) | P1—O4 | 1.521 (2) |
K2—O2vii | 2.960 (2) | P1—O2 | 1.521 (2) |
K2—O2viii | 2.960 (2) | P1—O3 | 1.525 (2) |
K2—O2ix | 2.960 (2) | P1—O1 | 1.5306 (19) |
K2—O4iv | 3.053 (3) | O1—K1xvi | 2.852 (2) |
K2—O4v | 3.053 (3) | O2—Sn1xxii | 2.0032 (19) |
K2—O4vi | 3.053 (3) | O2—Fe1xxii | 2.0032 (19) |
K2—O4vii | 3.243 (2) | O2—K2xix | 2.960 (2) |
K2—O4viii | 3.243 (2) | O2—K1xxi | 3.013 (2) |
K2—O4ix | 3.243 (2) | O3—Sn2xvi | 1.9830 (19) |
Fe1—O2x | 2.0032 (19) | O3—Fe2xvi | 1.9830 (19) |
Fe1—O2xi | 2.0032 (19) | O3—K2xxi | 2.868 (2) |
Fe1—O2xii | 2.0032 (19) | O4—K2xxi | 3.053 (3) |
Fe1—O1xiii | 2.0195 (19) | O4—K1xxi | 3.117 (2) |
Fe1—O1 | 2.0195 (19) | O4—K2xix | 3.243 (2) |
O1i—K1—O1ii | 92.31 (7) | O3v—K2—O4viii | 86.13 (6) |
O1i—K1—O1iii | 92.31 (7) | O2vii—K2—O4viii | 88.43 (6) |
O1ii—K1—O1iii | 92.31 (7) | O2viii—K2—O4viii | 45.82 (5) |
O1i—K1—O2iv | 57.28 (5) | O2ix—K2—O4viii | 100.56 (6) |
O1ii—K1—O2iv | 81.42 (6) | O4iv—K2—O4viii | 137.22 (4) |
O1iii—K1—O2iv | 148.35 (7) | O4v—K2—O4viii | 54.34 (8) |
O1i—K1—O2v | 148.35 (7) | O4vi—K2—O4viii | 104.276 (11) |
O1ii—K1—O2v | 57.28 (5) | O4vii—K2—O4viii | 115.51 (3) |
O1iii—K1—O2v | 81.42 (6) | O3iv—K2—O4ix | 86.13 (6) |
O2iv—K1—O2v | 119.065 (15) | O3vi—K2—O4ix | 156.82 (6) |
O1i—K1—O2vi | 81.42 (6) | O3v—K2—O4ix | 56.20 (5) |
O1ii—K1—O2vi | 148.35 (7) | O2vii—K2—O4ix | 100.56 (6) |
O1iii—K1—O2vi | 57.28 (5) | O2viii—K2—O4ix | 88.43 (6) |
O2iv—K1—O2vi | 119.065 (15) | O2ix—K2—O4ix | 45.82 (5) |
O2v—K1—O2vi | 119.065 (15) | O4iv—K2—O4ix | 54.34 (8) |
O1i—K1—O4iv | 103.75 (6) | O4v—K2—O4ix | 104.276 (11) |
O1ii—K1—O4iv | 82.12 (6) | O4vi—K2—O4ix | 137.22 (4) |
O1iii—K1—O4iv | 163.15 (6) | O4vii—K2—O4ix | 115.51 (3) |
O2iv—K1—O4iv | 46.64 (6) | O4viii—K2—O4ix | 115.51 (3) |
O2v—K1—O4iv | 82.20 (6) | O2x—Fe1—O2xi | 88.12 (9) |
O2vi—K1—O4iv | 129.53 (7) | O2x—Fe1—O2xii | 88.12 (9) |
O1i—K1—O4v | 163.15 (6) | O2xi—Fe1—O2xii | 88.12 (9) |
O1ii—K1—O4v | 103.75 (6) | O2x—Fe1—O1xiii | 88.81 (8) |
O1iii—K1—O4v | 82.12 (6) | O2xi—Fe1—O1xiii | 176.13 (9) |
O2iv—K1—O4v | 129.53 (7) | O2xii—Fe1—O1xiii | 89.43 (9) |
O2v—K1—O4v | 46.64 (6) | O2x—Fe1—O1 | 89.43 (9) |
O2vi—K1—O4v | 82.20 (6) | O2xi—Fe1—O1 | 88.81 (8) |
O4iv—K1—O4v | 83.78 (7) | O2xii—Fe1—O1 | 176.13 (9) |
O1i—K1—O4vi | 82.12 (6) | O1xiii—Fe1—O1 | 93.51 (9) |
O1ii—K1—O4vi | 163.15 (6) | O2x—Fe1—O1xiv | 176.13 (9) |
O1iii—K1—O4vi | 103.75 (6) | O2xi—Fe1—O1xiv | 89.43 (9) |
O2iv—K1—O4vi | 82.20 (6) | O2xii—Fe1—O1xiv | 88.81 (8) |
O2v—K1—O4vi | 129.53 (7) | O1xiii—Fe1—O1xiv | 93.51 (9) |
O2vi—K1—O4vi | 46.64 (6) | O1—Fe1—O1xiv | 93.51 (9) |
O4iv—K1—O4vi | 83.78 (7) | O3i—Fe2—O3ii | 93.35 (9) |
O4v—K1—O4vi | 83.78 (7) | O3i—Fe2—O3iii | 93.35 (9) |
O3iv—K2—O3vi | 100.64 (6) | O3ii—Fe2—O3iii | 93.35 (9) |
O3iv—K2—O3v | 100.64 (6) | O3i—Fe2—O4 | 172.59 (9) |
O3vi—K2—O3v | 100.64 (6) | O3ii—Fe2—O4 | 93.04 (9) |
O3iv—K2—O2vii | 95.91 (6) | O3iii—Fe2—O4 | 82.53 (9) |
O3vi—K2—O2vii | 100.74 (6) | O3i—Fe2—O4xiv | 93.04 (9) |
O3v—K2—O2vii | 149.93 (6) | O3ii—Fe2—O4xiv | 82.53 (9) |
O3iv—K2—O2viii | 149.93 (6) | O3iii—Fe2—O4xiv | 172.59 (9) |
O3vi—K2—O2viii | 95.91 (6) | O4—Fe2—O4xiv | 91.52 (9) |
O3v—K2—O2viii | 100.74 (6) | O3i—Fe2—O4xiii | 82.53 (9) |
O2vii—K2—O2viii | 56.14 (6) | O3ii—Fe2—O4xiii | 172.59 (9) |
O3iv—K2—O2ix | 100.74 (6) | O3iii—Fe2—O4xiii | 93.04 (9) |
O3vi—K2—O2ix | 149.93 (6) | O4—Fe2—O4xiii | 91.52 (9) |
O3v—K2—O2ix | 95.91 (6) | O4xiv—Fe2—O4xiii | 91.52 (9) |
O2vii—K2—O2ix | 56.14 (6) | O4—P1—O2 | 105.93 (13) |
O2viii—K2—O2ix | 56.14 (6) | O4—P1—O3 | 107.23 (13) |
O3iv—K2—O4iv | 48.81 (5) | O2—P1—O3 | 112.54 (12) |
O3vi—K2—O4iv | 114.59 (7) | O4—P1—O1 | 111.60 (13) |
O3v—K2—O4iv | 52.71 (6) | O2—P1—O1 | 108.63 (12) |
O2vii—K2—O4iv | 132.57 (6) | O3—P1—O1 | 110.83 (12) |
O2viii—K2—O4iv | 141.48 (6) | P1—O1—Fe1 | 130.29 (12) |
O2ix—K2—O4iv | 95.42 (6) | P1—O1—K1xvi | 112.12 (11) |
O3iv—K2—O4v | 114.59 (7) | Fe1—O1—K1xvi | 102.92 (7) |
O3vi—K2—O4v | 52.71 (6) | P1—O2—Sn1xxii | 165.01 (15) |
O3v—K2—O4v | 48.81 (5) | P1—O2—Fe1xxii | 165.01 (15) |
O2vii—K2—O4v | 141.48 (6) | P1—O2—K2xix | 93.70 (9) |
O2viii—K2—O4v | 95.42 (6) | Sn1xxii—O2—K2xix | 93.67 (8) |
O2ix—K2—O4v | 132.57 (6) | Fe1xxii—O2—K2xix | 93.67 (8) |
O4iv—K2—O4v | 85.96 (7) | P1—O2—K1xxi | 92.83 (10) |
O3iv—K2—O4vi | 52.71 (6) | Sn1xxii—O2—K1xxi | 98.07 (8) |
O3vi—K2—O4vi | 48.81 (5) | Fe1xxii—O2—K1xxi | 98.07 (8) |
O3v—K2—O4vi | 114.59 (7) | K2xix—O2—K1xxi | 103.77 (7) |
O2vii—K2—O4vi | 95.42 (6) | P1—O3—Sn2xvi | 148.98 (14) |
O2viii—K2—O4vi | 132.57 (6) | P1—O3—Fe2xvi | 148.98 (14) |
O2ix—K2—O4vi | 141.48 (6) | P1—O3—K2xxi | 105.79 (11) |
O4iv—K2—O4vi | 85.96 (7) | Sn2xvi—O3—K2xxi | 100.16 (8) |
O4v—K2—O4vi | 85.96 (7) | Fe2xvi—O3—K2xxi | 100.16 (8) |
O3iv—K2—O4vii | 56.20 (5) | P1—O4—Fe2 | 151.99 (15) |
O3vi—K2—O4vii | 86.13 (6) | P1—O4—K2xxi | 98.04 (10) |
O3v—K2—O4vii | 156.82 (6) | Fe2—O4—K2xxi | 93.77 (8) |
O2vii—K2—O4vii | 45.82 (5) | P1—O4—K1xxi | 88.91 (9) |
O2viii—K2—O4vii | 100.56 (6) | Fe2—O4—K1xxi | 118.50 (9) |
O2ix—K2—O4vii | 88.43 (6) | K2xxi—O4—K1xxi | 77.63 (6) |
O4iv—K2—O4vii | 104.276 (11) | P1—O4—K2xix | 83.19 (10) |
O4v—K2—O4vii | 137.22 (4) | Fe2—O4—K2xix | 88.28 (8) |
O4vi—K2—O4vii | 54.34 (8) | K2xxi—O4—K2xix | 172.75 (8) |
O3iv—K2—O4viii | 156.82 (6) | K1xxi—O4—K2xix | 95.28 (7) |
O3vi—K2—O4viii | 56.20 (5) |
Symmetry codes: (i) −z+1/2, −x+1, y+1/2; (ii) −x+1, y+1/2, −z+1/2; (iii) y+1/2, −z+1/2, −x+1; (iv) z+1/2, −x+3/2, −y+1; (v) −x+3/2, −y+1, z+1/2; (vi) −y+1, z+1/2, −x+3/2; (vii) −z+1, x+1/2, −y+3/2; (viii) −y+3/2, −z+1, x+1/2; (ix) x+1/2, −y+3/2, −z+1; (x) −y+1/2, −z, x−1/2; (xi) x−1/2, −y+1/2, −z; (xii) −z, x−1/2, −y+1/2; (xiii) y, z, x; (xiv) z, x, y; (xv) x−1, y−1, z−1; (xvi) −x+1, y−1/2, −z+1/2; (xvii) x−1/2, −y+1/2, −z+1; (xviii) −x+1/2, −y+1, z−1/2; (xix) x−1/2, −y+3/2, −z+1; (xx) −x+1, y−1/2, −z+3/2; (xxi) −x+3/2, −y+1, z−1/2; (xxii) x+1/2, −y+1/2, −z. |
Experimental details
Crystal data | |
Chemical formula | K2FeSn(PO4)3 |
Mr | 537.65 |
Crystal system, space group | Cubic, P213 |
Temperature (K) | 293 |
a (Å) | 9.91473 (7) |
V (Å3) | 974.64 (1) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.47 |
Crystal size (mm) | 0.08 × 0.06 × 0.05 |
Data collection | |
Diffractometer | XCalibur-3 diffractometer |
Absorption correction | Multi-scan (Blessing; 1995) |
Tmin, Tmax | 0.669, 0.772 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5809, 1434, 1338 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.807 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.045, 1.1 |
No. of reflections | 1434 |
No. of parameters | 63 |
No. of restraints | 3 |
Δρmax, Δρmin (e Å−3) | 0.50, −0.57 |
Absolute structure | Flack (1983), 621 Friedel Pairs |
Absolute structure parameter | −0.03 (2) |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2005), CrysAlis CCD, CrysAlis RED (Oxford Diffraction, 2005), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2006), WinGX publication routines (Farrugia, 1999).
K1—O1i | 2.852 (2) | Fe1—O1v | 2.0195 (19) |
K1—O2ii | 3.013 (2) | Fe2—O3i | 1.9830 (19) |
K1—O4ii | 3.117 (2) | Fe2—O4 | 2.010 (2) |
K2—O3ii | 2.868 (2) | P1—O4 | 1.521 (2) |
K2—O2iii | 2.960 (2) | P1—O2 | 1.521 (2) |
K2—O4ii | 3.053 (3) | P1—O3 | 1.525 (2) |
K2—O4iii | 3.243 (2) | P1—O1 | 1.5306 (19) |
Fe1—O2iv | 2.0032 (19) |
Symmetry codes: (i) −z+1/2, −x+1, y+1/2; (ii) z+1/2, −x+3/2, −y+1; (iii) −z+1, x+1/2, −y+3/2; (iv) −y+1/2, −z, x−1/2; (v) y, z, x. |
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Langbeinite-type frameworks [M2(PO4)3]∞ can be composed from various types of tetravalent and bi- or trivalent metal pairs. For example, the structures of K2M0.5Ti1.5(PO4)3 (M = Ni, Co, Mn) (Ogorodnyk et al., 2006; 2007a), K2MTi(PO4)3 (M = Y, Yb, Er) (Norberg, 2002), K2FeZr(PO4)3 (Orlova et al., 2003) and K2LuZr(PO4)3 (Ogorodnyk et al., 2007b) have been investigated in the past years. Among other langbeinite-related compounds, the structures of only two tin(IV)-containing phosphates, viz. K2MSn(PO4)3 (M = Fe, Yb) refined from X-ray powder data, were previously reported (Aatiq et al., 2006). Herein we report the single-crystal growth and re-investigation of K2FeSn(PO4)3 (I), a structure that is isotypic with the mineral langbeinite, K2Mg2(SO4)3 (Zemann, & Zemann, 1957).
Sn and Fe atoms are statistically distributed over two octahedrally coordinated positions with an insignificant priority of the M1 site occupation by Sn and of the M2 site by Fe. The {Sn(Fe)1-Sn(Fe)2-K1—K2} sequence runs along [111] (Fig. 1). K1 atoms are coordinated by 9 O atoms, while K2 atoms are surrounded by 12 O atoms (Fig. 2), with K—O bond lengths ranging from 2.852 (2) to 3.243 (2) Å.
Comparing the results from the single-crystal study with the results of the previous powder study, the following points are noteable. The distribution of two type of metals (Fe and Sn) over two octahedrally coordinated positions are close to those reported earlier, but the accuracy of single-crystal refinement is more precise. The values of corresponding Fe/Sn—O bond lengths insignificantly differs from one another in each type of octahedron in the present structure model, while the values found by Rietveld refinement differs a lot. Actually, the new results of the single-crystal refinement suggest a lower degree of distortion of the [(Fe,Sn)O6] polyhedra. Moreover, in contrast to the results of the powder refinement with each of the K+ cations in 9-fold coordination, we assume that K1 is 9-coordinate, while K2 is 12-coordinate, which agrees with the most of earlier discussed structures of langbeinite-related phosphates.