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Crystals of calcium potassium cyclo-triphosphate, CaKP3O9, have been synthesized from a melt and structurally characterized using single-crystal X-ray diffraction. The compound is isostructural with the mineral benitoite (BaTiSi3O9).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804000303/wm6003sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804000303/wm6003Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](P-O) = 0.001 Å
  • R factor = 0.024
  • wR factor = 0.056
  • Data-to-parameter ratio = 22.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
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 34.94 From the CIF: _reflns_number_total 639 Count of symmetry unique reflns 357 Completeness (_total/calc) 178.99% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 282 Fraction of Friedel pairs measured 0.790 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: Collect (Nonius B.V., 1999); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2000); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) and local procedures.

Calcium potassium cyclo-triphosphate top
Crystal data top
CaK(P3O9)Dx = 2.520 Mg m3
Mr = 316.10Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6c2Cell parameters from 455 reflections
Hall symbol: P -6c 2θ = 2.9–33.1°
a = 6.8090 (3) ŵ = 1.85 mm1
c = 10.3760 (9) ÅT = 293 K
V = 416.61 (4) Å3Fragment, colourless
Z = 20.19 × 0.12 × 0.05 mm
F(000) = 312
Data collection top
Nonius KappaCCD
diffractometer
639 independent reflections
Radiation source: fine-focus sealed tube, KappaCCD628 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.077
φ and ω scansθmax = 34.9°, θmin = 3.5°
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
h = 1010
Tmin = 0.794, Tmax = 0.914k = 1010
25323 measured reflectionsl = 1616
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.019P)2 + 0.3146P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.024(Δ/σ)max < 0.001
wR(F2) = 0.056Δρmax = 0.44 e Å3
S = 1.18Δρmin = 0.40 e Å3
639 reflectionsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
28 parametersExtinction coefficient: 0.130 (6)
0 restraintsAbsolute structure: Flack (1983), 282 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (7)
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
xyzUiso*/Ueq
Ca0.333330.666671.00000.01396 (15)
K0.666670.333331.00000.0233 (2)
P0.73221 (9)0.96188 (9)0.75000.01192 (13)
O10.8054 (3)0.7734 (3)0.75000.0220 (3)
O20.6141 (2)0.9486 (2)0.87205 (11)0.0239 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca0.0153 (2)0.0153 (2)0.0113 (3)0.00765 (10)0.0000.000
K0.0220 (3)0.0220 (3)0.0260 (4)0.01100 (13)0.0000.000
P0.0098 (2)0.0124 (3)0.0140 (2)0.00589 (19)0.0000.000
O10.0127 (7)0.0127 (7)0.0410 (10)0.0067 (7)0.0000.000
O20.0284 (7)0.0230 (6)0.0208 (6)0.0131 (5)0.0106 (5)0.0034 (5)
Geometric parameters (Å, º) top
Ca—O2i2.3309 (12)K—O2vii2.7955 (14)
Ca—O2ii2.3309 (12)K—O2viii2.7955 (14)
Ca—O2iii2.3309 (13)K—O2ix2.7956 (14)
Ca—O2iv2.3309 (12)P—O11.592 (2)
Ca—O22.3309 (13)P—O1x1.5950 (18)
Ca—O2v2.3309 (13)P—O21.4785 (12)
K—O2iv2.7955 (14)P—O2xi1.4785 (12)
K—O2v2.7955 (14)O1—Pviii1.5951 (18)
K—O2vi2.7955 (14)
O2i—Ca—O2ii89.47 (8)O2—P—O1x107.89 (7)
O2i—Ca—O2iii88.99 (7)O2xi—P—O1x107.89 (7)
O2ii—Ca—O2iii90.77 (5)O2—P—O2xi117.87 (13)
O2i—Ca—O2iv90.77 (5)P—O1—Pviii136.40 (13)
O2ii—Ca—O2iv179.66 (8)O2iii—Ca—O2179.66 (8)
O2iii—Ca—O2iv89.47 (8)O2iv—Ca—O290.77 (5)
O2i—Ca—O290.77 (5)O2i—Ca—O2v179.66 (8)
O2ii—Ca—O288.99 (7)O2ii—Ca—O2v90.77 (5)
O2iii—Ca—O2179.66 (8)O2iii—Ca—O2v90.77 (5)
O2iv—Ca—O290.77 (5)O2iv—Ca—O2v88.99 (7)
O2i—Ca—O2v179.66 (8)O2—Ca—O2v89.47 (8)
O2ii—Ca—O2v90.77 (5)O2iv—K—O2v71.52 (5)
O2iii—Ca—O2v90.77 (5)O2iv—K—O2vi91.04 (7)
O2iv—Ca—O2v88.99 (7)O2v—K—O2vi99.31 (3)
O2—Ca—O2v89.47 (8)O2iv—K—O2vii99.31 (3)
O2iv—K—O2v71.52 (5)O2v—K—O2vii167.27 (6)
O2iv—K—O2vi91.04 (7)O2vi—K—O2vii71.52 (5)
O2v—K—O2vi99.31 (3)O2iv—K—O2viii99.31 (3)
O2iv—K—O2vii99.31 (3)O2v—K—O2viii91.04 (7)
O2v—K—O2vii167.27 (6)O2vi—K—O2viii167.27 (6)
O2vi—K—O2vii71.52 (5)O2vii—K—O2viii99.31 (3)
O2iv—K—O2viii99.31 (3)O2iv—K—O2ix167.27 (6)
O2v—K—O2viii91.04 (7)O2v—K—O2ix99.31 (3)
O2vi—K—O2viii167.27 (6)O2vi—K—O2ix99.31 (3)
O2vii—K—O2viii99.31 (3)O2vii—K—O2ix91.04 (6)
O2iv—K—O2ix167.27 (6)O2viii—K—O2ix71.52 (5)
O2v—K—O2ix99.31 (3)O1—P—O1x103.60 (13)
O2vi—K—O2ix99.31 (3)O2—P—O1109.31 (7)
O2vii—K—O2ix91.04 (6)O2xi—P—O1109.31 (7)
O2viii—K—O2ix71.52 (5)O2—P—O1x107.89 (7)
O1—P—O1x103.60 (13)O2xi—P—O1x107.89 (7)
O2—P—O1109.31 (7)O2—P—O2xi117.87 (13)
O2xi—P—O1109.31 (7)P—O1—Pviii136.40 (13)
Symmetry codes: (i) y+1, xy+1, z; (ii) x+y, y, z+2; (iii) y+1, x+1, z+2; (iv) x+y, x+1, z; (v) x, xy+1, z+2; (vi) x+y, y1, z+2; (vii) x, y1, z; (viii) y+2, xy+1, z; (ix) y+2, x+1, z+2; (x) x+y+1, x+2, z; (xi) x, y, z+3/2.
 

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