Crystals of the title compound, CsCd(P3O9), were grown from a melt. The structure is isotypic with CsCdP3O9. The three-dimensional framework is built up from [CaO6] octahedra linked together via corner-sharing to cyclic [P3O9]3− anions. The Cs cations are situated in large cavities in the [CaP3O9]∞− anion framework. Except for one P and three O atoms, all other atoms (one Cs, one Ca, one P and three O atoms) are located on mirror planes.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (P-O) = 0.002 Å
- R factor = 0.020
- wR factor = 0.041
- Data-to-parameter ratio = 20.3
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: Ca1 Cs1 O9 P3
Atom count from _chemical_formula_moiety:
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
4 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
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
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, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).
Caesium calcium
cyclo-triphosphate
top
Crystal data top
CsCa(P3O9) | F(000) = 768 |
Mr = 409.9 | Dx = 2.863 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 13085 reflections |
a = 9.8287 (2) Å | θ = 2.6–30.0° |
b = 7.5642 (1) Å | µ = 4.96 mm−1 |
c = 12.7905 (2) Å | T = 293 K |
V = 950.93 (3) Å3 | Prism, colourless |
Z = 4 | 0.05 × 0.04 × 0.03 mm |
Data collection top
Oxford Xcalibur-3 CCD area-detector diffractometer | 1482 independent reflections |
Radiation source: fine-focus sealed tube | 1278 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
φ and ω scans | θmax = 30°, θmin = 2.6° |
Absorption correction: multi-scan (Blessing, 1995) | h = −13→13 |
Tmin = 0.790, Tmax = 0.865 | k = −10→10 |
13085 measured reflections | l = −17→17 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.020 | w = 1/[σ2(Fo2) + (0.0198P)2 + 0.1458P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.041 | (Δ/σ)max = 0.001 |
S = 1.13 | Δρmax = 0.70 e Å−3 |
1482 reflections | Δρmin = −0.52 e Å−3 |
73 parameters | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cs | 0.88820 (2) | 0.25 | 0.584738 (15) | 0.02104 (6) | |
Ca | 0.98661 (5) | 0.75 | 0.72159 (4) | 0.00923 (11) | |
P1 | 0.74820 (5) | 0.55310 (7) | 0.35240 (4) | 0.01042 (10) | |
P2 | 0.70743 (7) | 0.75 | 0.54177 (6) | 0.01197 (15) | |
O1 | 0.67746 (15) | 0.5850 (2) | 0.46443 (11) | 0.0162 (3) | |
O2 | 0.64565 (15) | 0.4838 (2) | 0.27912 (12) | 0.0229 (4) | |
O3 | 0.87732 (15) | 0.4558 (2) | 0.36703 (12) | 0.0196 (3) | |
O4 | 0.8540 (2) | 0.75 | 0.56819 (16) | 0.0221 (5) | |
O5 | 0.7892 (2) | 0.75 | 0.31724 (16) | 0.0142 (4) | |
O6 | 0.6039 (2) | 0.75 | 0.62422 (17) | 0.0236 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cs | 0.02398 (10) | 0.02403 (11) | 0.01511 (10) | 0 | 0.00151 (8) | 0 |
Ca | 0.0094 (2) | 0.0096 (3) | 0.0086 (2) | 0 | −0.00030 (19) | 0 |
P1 | 0.0134 (2) | 0.0076 (2) | 0.0103 (2) | −0.00068 (18) | −0.00013 (17) | −0.00092 (18) |
P2 | 0.0138 (3) | 0.0150 (4) | 0.0072 (3) | 0 | 0.0012 (3) | 0 |
O1 | 0.0202 (7) | 0.0136 (7) | 0.0148 (7) | −0.0020 (6) | 0.0035 (6) | 0.0004 (6) |
O2 | 0.0256 (8) | 0.0237 (9) | 0.0195 (8) | −0.0097 (7) | −0.0056 (6) | −0.0034 (7) |
O3 | 0.0210 (8) | 0.0174 (8) | 0.0203 (8) | 0.0093 (6) | 0.0019 (6) | 0.0010 (6) |
O4 | 0.0160 (10) | 0.0373 (14) | 0.0130 (11) | 0 | −0.0036 (8) | 0 |
O5 | 0.0209 (10) | 0.0096 (10) | 0.0121 (10) | 0 | 0.0059 (8) | 0 |
O6 | 0.0249 (12) | 0.0306 (13) | 0.0153 (10) | 0 | 0.0089 (9) | 0 |
Geometric parameters (Å, º) top
Cs—O3i | 3.1918 (15) | Ca—O3ii | 2.3443 (15) |
Cs—O3 | 3.1918 (15) | Ca—O3ix | 2.3443 (15) |
Cs—O4ii | 3.201 (2) | Ca—O4 | 2.355 (2) |
Cs—O2iii | 3.2168 (17) | Ca—Csii | 4.1067 (6) |
Cs—O2iv | 3.2168 (17) | Ca—Csx | 4.2783 (3) |
Cs—O3ii | 3.2628 (16) | P1—O2 | 1.4729 (15) |
Cs—O3v | 3.2628 (16) | P1—O3 | 1.4791 (15) |
Cs—O5ii | 3.409 (2) | P1—O5 | 1.6072 (9) |
Cs—O5iii | 3.448 (2) | P1—O1 | 1.6108 (15) |
Cs—O1i | 3.6166 (15) | P1—Csii | 3.9542 (5) |
Cs—O1 | 3.6166 (15) | P1—Csxi | 3.9669 (5) |
Cs—O4 | 3.8029 (2) | P2—O6 | 1.466 (2) |
Cs—O4vi | 3.8029 (2) | P2—O4 | 1.480 (2) |
Ca—O6vii | 2.284 (2) | P2—O1 | 1.6196 (16) |
Ca—O2iii | 2.3148 (16) | P2—O1xii | 1.6196 (16) |
Ca—O2viii | 2.3148 (16) | P2—Csx | 4.2147 (3) |
| | | |
O3i—Cs—O3 | 58.37 (6) | O3ii—Ca—Csii | 50.79 (4) |
O3i—Cs—O4ii | 59.56 (4) | O3ix—Ca—Csii | 50.79 (4) |
O3—Cs—O4ii | 59.56 (4) | O4—Ca—Csii | 51.02 (5) |
O3i—Cs—O2iii | 167.45 (4) | O6vii—Ca—Cs | 117.860 (7) |
O3—Cs—O2iii | 111.44 (4) | O2iii—Ca—Cs | 47.76 (4) |
O4ii—Cs—O2iii | 123.66 (4) | O2viii—Ca—Cs | 132.72 (4) |
O3i—Cs—O2iv | 111.44 (4) | O3ii—Ca—Cs | 49.02 (4) |
O3—Cs—O2iv | 167.45 (4) | O3ix—Ca—Cs | 121.20 (4) |
O4ii—Cs—O2iv | 123.66 (4) | O4—Ca—Cs | 62.232 (7) |
O2iii—Cs—O2iv | 77.52 (6) | Csii—Ca—Cs | 71.179 (8) |
O3i—Cs—O3ii | 121.42 (2) | O6vii—Ca—Csx | 117.860 (7) |
O3—Cs—O3ii | 81.72 (4) | O2iii—Ca—Csx | 132.72 (4) |
O4ii—Cs—O3ii | 63.67 (4) | O2viii—Ca—Csx | 47.76 (4) |
O2iii—Cs—O3ii | 59.99 (4) | O3ii—Ca—Csx | 121.20 (4) |
O2iv—Cs—O3ii | 110.73 (4) | O3ix—Ca—Csx | 49.02 (4) |
O3i—Cs—O3v | 81.72 (4) | O4—Ca—Csx | 62.232 (7) |
O3—Cs—O3v | 121.42 (2) | Csii—Ca—Csx | 71.179 (8) |
O4ii—Cs—O3v | 63.67 (4) | Cs—Ca—Csx | 124.263 (14) |
O2iii—Cs—O3v | 110.73 (4) | O2—P1—O3 | 119.37 (10) |
O2iv—Cs—O3v | 59.99 (4) | O2—P1—O5 | 108.89 (11) |
O3ii—Cs—O3v | 86.02 (5) | O3—P1—O5 | 106.34 (10) |
O3i—Cs—O5ii | 110.61 (4) | O2—P1—O1 | 108.90 (9) |
O3—Cs—O5ii | 110.61 (4) | O3—P1—O1 | 109.41 (9) |
O4ii—Cs—O5ii | 59.25 (5) | O5—P1—O1 | 102.61 (9) |
O2iii—Cs—O5ii | 79.16 (4) | O2—P1—Csii | 151.88 (7) |
O2iv—Cs—O5ii | 79.16 (4) | O3—P1—Csii | 52.15 (6) |
O3ii—Cs—O5ii | 43.42 (3) | O5—P1—Csii | 58.74 (8) |
O3v—Cs—O5ii | 43.42 (3) | O1—P1—Csii | 98.79 (6) |
O3i—Cs—O5iii | 137.36 (3) | O2—P1—Csxi | 49.70 (7) |
O3—Cs—O5iii | 137.36 (3) | O3—P1—Csxi | 125.88 (6) |
O4ii—Cs—O5iii | 158.06 (5) | O5—P1—Csxi | 59.70 (8) |
O2iii—Cs—O5iii | 44.03 (3) | O1—P1—Csxi | 124.44 (6) |
O2iv—Cs—O5iii | 44.03 (3) | Csii—P1—Csxi | 109.848 (12) |
O3ii—Cs—O5iii | 101.20 (4) | O2—P1—Cs | 120.29 (7) |
O3v—Cs—O5iii | 101.20 (4) | O3—P1—Cs | 47.55 (6) |
O5ii—Cs—O5iii | 98.81 (2) | O5—P1—Cs | 130.77 (8) |
O3i—Cs—O1i | 42.94 (3) | O1—P1—Cs | 64.74 (6) |
O3—Cs—O1i | 87.20 (4) | Csii—P1—Cs | 75.746 (9) |
O4ii—Cs—O1i | 101.14 (3) | Csxi—P1—Cs | 166.707 (15) |
O2iii—Cs—O1i | 135.09 (4) | O6—P2—O4 | 120.79 (14) |
O2iv—Cs—O1i | 80.27 (4) | O6—P2—O1 | 108.25 (8) |
O3ii—Cs—O1i | 164.36 (4) | O4—P2—O1 | 108.45 (8) |
O3v—Cs—O1i | 90.40 (3) | O6—P2—O1xii | 108.25 (8) |
O5ii—Cs—O1i | 133.56 (3) | O4—P2—O1xii | 108.45 (8) |
O5iii—Cs—O1i | 94.43 (3) | O1—P2—O1xii | 100.81 (11) |
O3i—Cs—O1 | 87.20 (4) | O6—P2—Csx | 101.48 (4) |
O3—Cs—O1 | 42.94 (3) | O4—P2—Csx | 63.883 (10) |
O4ii—Cs—O1 | 101.14 (3) | O1—P2—Csx | 147.97 (6) |
O2iii—Cs—O1 | 80.27 (4) | O1xii—P2—Csx | 57.64 (6) |
O2iv—Cs—O1 | 135.09 (4) | O6—P2—Cs | 101.48 (4) |
O3ii—Cs—O1 | 90.40 (3) | O4—P2—Cs | 63.883 (10) |
O3v—Cs—O1 | 164.36 (4) | O1—P2—Cs | 57.64 (5) |
O5ii—Cs—O1 | 133.56 (3) | O1xii—P2—Cs | 147.97 (6) |
O5iii—Cs—O1 | 94.43 (3) | Csx—P2—Cs | 127.629 (19) |
O1i—Cs—O1 | 88.96 (5) | P1—O1—P2 | 125.47 (10) |
O3i—Cs—O4vi | 57.56 (4) | P1—O1—Cs | 91.51 (6) |
O3—Cs—O4vi | 115.69 (4) | P2—O1—Cs | 100.13 (7) |
O4ii—Cs—O4vi | 92.06 (3) | P1—O2—Caxi | 149.16 (11) |
O2iii—Cs—O4vi | 131.03 (4) | P1—O2—Csxi | 109.86 (8) |
O2iv—Cs—O4vi | 53.93 (4) | Caxi—O2—Csxi | 100.05 (5) |
O3ii—Cs—O4vi | 138.70 (4) | P1—O3—Caii | 139.36 (10) |
O3v—Cs—O4vi | 52.73 (4) | P1—O3—Cs | 112.45 (8) |
O5ii—Cs—O4vi | 95.89 (3) | Caii—O3—Cs | 94.53 (5) |
O5iii—Cs—O4vi | 90.19 (3) | P1—O3—Csii | 106.88 (8) |
O1i—Cs—O4vi | 39.55 (4) | Caii—O3—Csii | 98.13 (5) |
O1—Cs—O4vi | 128.51 (4) | Cs—O3—Csii | 98.28 (4) |
O6vii—Ca—O2iii | 90.51 (6) | P2—O4—Ca | 136.78 (13) |
O6vii—Ca—O2viii | 90.51 (6) | P2—O4—Csii | 129.13 (11) |
O2iii—Ca—O2viii | 99.62 (9) | Ca—O4—Csii | 94.09 (7) |
O6vii—Ca—O3ii | 97.45 (6) | P2—O4—Csx | 95.66 (3) |
O2iii—Ca—O3ii | 88.10 (6) | Ca—O4—Csx | 84.54 (3) |
O2viii—Ca—O3ii | 168.89 (6) | Csii—O4—Csx | 87.94 (3) |
O6vii—Ca—O3ix | 97.45 (6) | P2—O4—Cs | 95.66 (3) |
O2iii—Ca—O3ix | 168.89 (6) | Ca—O4—Cs | 84.54 (3) |
O2viii—Ca—O3ix | 88.10 (6) | Csii—O4—Cs | 87.94 (3) |
O3ii—Ca—O3ix | 83.20 (8) | Csx—O4—Cs | 168.02 (6) |
O6vii—Ca—O4 | 176.71 (8) | P1xii—O5—P1 | 135.84 (13) |
O2iii—Ca—O4 | 87.37 (5) | P1xii—O5—Csii | 97.50 (8) |
O2viii—Ca—O4 | 87.37 (5) | P1—O5—Csii | 97.50 (8) |
O3ii—Ca—O4 | 85.00 (6) | P1xii—O5—Csxi | 96.57 (8) |
O3ix—Ca—O4 | 85.00 (6) | P1—O5—Csxi | 96.57 (8) |
O6vii—Ca—Csii | 132.27 (6) | Csii—O5—Csxi | 141.97 (6) |
O2iii—Ca—Csii | 118.14 (4) | P2—O6—Caxiii | 166.31 (16) |
O2viii—Ca—Csii | 118.14 (4) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) −x+2, −y+1, −z+1; (iii) −x+3/2, −y+1, z+1/2; (iv) −x+3/2, y−1/2, z+1/2; (v) −x+2, y−1/2, −z+1; (vi) x, y−1, z; (vii) x+1/2, y, −z+3/2; (viii) −x+3/2, y+1/2, z+1/2; (ix) −x+2, y+1/2, −z+1; (x) x, y+1, z; (xi) −x+3/2, −y+1, z−1/2; (xii) x, −y+3/2, z; (xiii) x−1/2, y, −z+3/2. |