Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401966X/wm6028sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680401966X/wm6028Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (P-O) = 0.004 Å
- R factor = 0.017
- wR factor = 0.041
- Data-to-parameter ratio = 15.1
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.88 PLAT430_ALERT_2_A Short Inter D...A Contact O1 .. O3 .. 2.47 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.33 Ratio PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.83 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.833 Tmax scaled 0.349 Tmin scaled 0.290 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 28.23 From the CIF: _reflns_number_total 936 Count of symmetry unique reflns 557 Completeness (_total/calc) 168.04% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 379 Fraction of Friedel pairs measured 0.680 Are heavy atom types Z>Si present yes
2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 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 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996-2001); software used to prepare material for publication: SHELXL97.
KSn4(PO4)3 | Dx = 3.962 Mg m−3 |
Mr = 798.77 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 4440 reflections |
Hall symbol: R 3 -2"c | θ = 2.9–28.2° |
a = 9.7342 (5) Å | µ = 8.10 mm−1 |
c = 24.4754 (14) Å | T = 293 K |
V = 2008.4 (3) Å3 | Trigonal prism, colourless |
Z = 6 | 0.16 × 0.13 × 0.13 mm |
F(000) = 2160 |
Bruker SMART Apex 2000 diffractometer | 936 independent reflections |
Radiation source: fine-focus sealed tube | 927 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
φ and ω scans | θmax = 28.2°, θmin = 2.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→12 |
Tmin = 0.290, Tmax = 0.349 | k = −11→12 |
4440 measured reflections | l = −32→31 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0167P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.001 |
wR(F2) = 0.041 | Δρmax = 0.94 e Å−3 |
S = 1.25 | Δρmin = −0.69 e Å−3 |
936 reflections | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
62 parameters | Extinction coefficient: 0.00092 (5) |
1 restraint | Absolute structure: Flack (1983), with 446 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.03 (3) |
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 | ||
Sn1 | 1.0000 | 1.0000 | 0.82700 (2) | 0.01923 (15) | |
Sn2 | 1.14901 (4) | 0.73914 (4) | 0.630155 (11) | 0.01765 (11) | |
P | 0.67206 (14) | 0.87550 (14) | 0.75941 (5) | 0.0119 (2) | |
O1 | 1.2176 (4) | 0.9535 (4) | 0.58913 (16) | 0.0249 (8) | |
O2 | 0.8366 (3) | 1.0149 (4) | 0.77424 (14) | 0.0186 (7) | |
O3 | 1.1921 (4) | 0.8698 (4) | 0.70307 (13) | 0.0187 (7) | |
O4 | 0.6269 (5) | 0.7469 (4) | 0.80247 (15) | 0.0231 (8) | |
K | 1.0000 | 1.0000 | 0.67666 (9) | 0.0208 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.0222 (2) | 0.0222 (2) | 0.0133 (3) | 0.01110 (11) | 0.000 | 0.000 |
Sn2 | 0.01883 (18) | 0.01411 (18) | 0.02176 (17) | 0.00954 (15) | 0.00202 (12) | −0.00066 (13) |
P | 0.0103 (5) | 0.0113 (5) | 0.0135 (5) | 0.0049 (5) | 0.0034 (4) | 0.0018 (4) |
O1 | 0.0206 (17) | 0.0146 (18) | 0.024 (2) | −0.0030 (14) | −0.0038 (14) | 0.0044 (14) |
O2 | 0.0094 (16) | 0.0117 (15) | 0.0319 (19) | 0.0032 (13) | 0.0005 (14) | 0.0019 (14) |
O3 | 0.0204 (18) | 0.0150 (18) | 0.0163 (17) | 0.0055 (14) | −0.0028 (14) | 0.0021 (14) |
O4 | 0.034 (2) | 0.0142 (18) | 0.0155 (18) | 0.0082 (16) | 0.0065 (15) | 0.0032 (13) |
K | 0.0189 (6) | 0.0189 (6) | 0.0247 (10) | 0.0094 (3) | 0.000 | 0.000 |
Sn1—O2 | 2.110 (3) | O2—K | 2.913 (4) |
Sn1—O2i | 2.110 (3) | O3—Pi | 1.541 (3) |
Sn1—O2ii | 2.110 (3) | O3—K | 2.809 (4) |
Sn1—K | 3.680 (2) | O4—Sn2vii | 2.095 (4) |
Sn2—O4iii | 2.095 (4) | O4—Kv | 2.747 (4) |
Sn2—O1 | 2.101 (3) | K—O4iii | 2.747 (4) |
Sn2—O3 | 2.108 (4) | K—O4vi | 2.747 (4) |
Sn2—K | 3.6784 (9) | K—O4viii | 2.747 (4) |
P—O4 | 1.523 (4) | K—O3i | 2.809 (4) |
P—O1iv | 1.524 (4) | K—O3ii | 2.809 (4) |
P—O2 | 1.538 (3) | K—O2ii | 2.913 (4) |
P—O3ii | 1.541 (3) | K—O2i | 2.913 (4) |
P—K | 3.4485 (17) | K—O2 | 2.913 (4) |
P—Kv | 3.5383 (17) | K—O1ii | 3.200 (4) |
O1—Pvi | 1.524 (4) | K—O1i | 3.200 (4) |
O1—K | 3.200 (4) | K—O1 | 3.200 (4) |
O2—Sn1—O2i | 86.44 (13) | O4viii—K—O3i | 75.47 (10) |
O2—Sn1—O2ii | 86.44 (13) | O4iii—K—O3ii | 75.47 (10) |
O2i—Sn1—O2ii | 86.44 (13) | O4vi—K—O3ii | 168.69 (13) |
O2—Sn1—K | 52.26 (9) | O4viii—K—O3ii | 61.41 (11) |
O2i—Sn1—K | 52.26 (9) | O3i—K—O3ii | 114.87 (6) |
O2ii—Sn1—K | 52.26 (9) | O4iii—K—O3 | 61.41 (11) |
O4iii—Sn2—O1 | 88.16 (15) | O4vi—K—O3 | 75.47 (10) |
O4iii—Sn2—O3 | 84.92 (14) | O4viii—K—O3 | 168.69 (13) |
O1—Sn2—O3 | 86.39 (14) | O3i—K—O3 | 114.87 (6) |
O4iii—Sn2—K | 47.69 (10) | O3ii—K—O3 | 114.87 (6) |
O1—Sn2—K | 60.10 (11) | O4iii—K—O2ii | 130.42 (12) |
O3—Sn2—K | 49.46 (10) | O4vi—K—O2ii | 76.99 (12) |
O4—P—O1iv | 112.0 (2) | O4viii—K—O2ii | 118.17 (11) |
O4—P—O2 | 107.9 (2) | O3i—K—O2ii | 52.31 (9) |
O1iv—P—O2 | 110.5 (2) | O3ii—K—O2ii | 109.71 (12) |
O4—P—O3ii | 109.0 (2) | O3—K—O2ii | 73.04 (10) |
O1iv—P—O3ii | 107.3 (2) | O4iii—K—O2i | 76.99 (12) |
O2—P—O3ii | 110.17 (18) | O4vi—K—O2i | 118.17 (11) |
O2—Sn1—O2i | 86.44 (13) | O4viii—K—O2i | 130.42 (12) |
O2—Sn1—O2ii | 86.44 (13) | O3i—K—O2i | 109.71 (12) |
O2i—Sn1—O2ii | 86.44 (13) | O3ii—K—O2i | 73.04 (10) |
O2—Sn1—K | 52.26 (9) | O3—K—O2i | 52.31 (9) |
O2i—Sn1—K | 52.26 (9) | O2ii—K—O2i | 59.47 (11) |
O2ii—Sn1—K | 52.26 (9) | O4iii—K—O2 | 118.17 (11) |
O4iii—Sn2—O1 | 88.16 (15) | O4vi—K—O2 | 130.42 (12) |
O4iii—Sn2—O3 | 84.92 (14) | O4viii—K—O2 | 76.99 (12) |
O1—Sn2—O3 | 86.39 (14) | O3i—K—O2 | 73.04 (10) |
O4iii—Sn2—K | 47.69 (10) | O3ii—K—O2 | 52.31 (9) |
O1—Sn2—K | 60.10 (11) | O3—K—O2 | 109.71 (12) |
O3—Sn2—K | 49.46 (10) | O2ii—K—O2 | 59.47 (11) |
O4—P—O1iv | 112.0 (2) | O2i—K—O2 | 59.47 (11) |
O4—P—O2 | 107.9 (2) | O4iii—K—O1ii | 49.55 (11) |
O1iv—P—O2 | 110.5 (2) | O4vi—K—O1ii | 116.40 (15) |
O4—P—O3ii | 109.0 (2) | O4viii—K—O1ii | 58.20 (11) |
O1iv—P—O3ii | 107.3 (2) | O3i—K—O1ii | 131.13 (10) |
O2—P—O3ii | 110.17 (18) | O3ii—K—O1ii | 56.84 (10) |
O4—P—K | 122.08 (15) | O3—K—O1ii | 110.56 (10) |
O1iv—P—K | 125.84 (16) | O2ii—K—O1ii | 166.53 (11) |
O2—P—K | 57.04 (13) | O2i—K—O1ii | 111.73 (10) |
O3ii—P—K | 53.15 (14) | O2—K—O1ii | 107.68 (9) |
O4—P—Kv | 47.40 (16) | O4iii—K—O1 | 58.20 (11) |
O1iv—P—Kv | 64.74 (15) | O4vi—K—O1 | 49.55 (10) |
O2—P—Kv | 129.06 (14) | O4viii—K—O1 | 116.40 (15) |
O3ii—P—Kv | 119.72 (15) | O3i—K—O1 | 110.56 (10) |
K—P—Kv | 167.36 (4) | O3ii—K—O1 | 131.13 (10) |
Pvi—O1—Sn2 | 140.7 (2) | O3—K—O1 | 56.84 (10) |
Pvi—O1—K | 89.74 (16) | O2ii—K—O1 | 111.73 (10) |
Sn2—O1—K | 85.21 (12) | O2i—K—O1 | 107.68 (9) |
P—O2—Sn1 | 124.9 (2) | O2—K—O1 | 166.53 (10) |
P—O2—K | 96.67 (15) | O1ii—K—O1 | 80.08 (11) |
Sn1—O2—K | 92.80 (11) | O4iii—K—O1i | 116.40 (15) |
Pi—O3—Sn2 | 124.6 (2) | O4vi—K—O1i | 58.20 (11) |
Pi—O3—K | 100.82 (17) | O4viii—K—O1i | 49.55 (11) |
Sn2—O3—K | 95.78 (13) | O3i—K—O1i | 56.84 (10) |
P—O4—Sn2vii | 131.1 (2) | O3ii—K—O1i | 110.56 (10) |
P—O4—Kv | 108.5 (2) | O3—K—O1i | 131.13 (10) |
Sn2vii—O4—Kv | 97.98 (13) | O2ii—K—O1i | 107.68 (9) |
O4iii—K—O4vi | 107.53 (11) | O2i—K—O1i | 166.53 (10) |
O4iii—K—O4viii | 107.53 (11) | O2—K—O1i | 111.73 (10) |
O4vi—K—O4viii | 107.53 (11) | O1ii—K—O1i | 80.08 (11) |
O4iii—K—O3i | 168.69 (13) | O1—K—O1i | 80.08 (11) |
O4vi—K—O3i | 61.41 (11) |
Symmetry codes: (i) −y+2, x−y+1, z; (ii) −x+y+1, −x+2, z; (iii) −y+5/3, −x+4/3, z−1/6; (iv) x−2/3, x−y+2/3, z+1/6; (v) −x+y+1/3, y−1/3, z+1/6; (vi) x+2/3, x−y+4/3, z−1/6; (vii) −y+4/3, −x+5/3, z+1/6; (viii) −x+y+2/3, y+1/3, z−1/6. |
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