Caesium calcium cyclo-triphosphate, CsCaP₃O₉

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.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](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

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Computing details

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

Crystal data

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) Å^3	Prism, colourless
Z = 4	0.05 × 0.04 × 0.03 mm

Data collection

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

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.0198P)^2 + 0.1458P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Cs—O3^i	3.1918 (15)	Ca—O3^ii	2.3443 (15)
Cs—O3	3.1918 (15)	Ca—O3^ix	2.3443 (15)
Cs—O4^ii	3.201 (2)	Ca—O4	2.355 (2)
Cs—O2^iii	3.2168 (17)	Ca—Cs^ii	4.1067 (6)
Cs—O2^iv	3.2168 (17)	Ca—Cs^x	4.2783 (3)
Cs—O3^ii	3.2628 (16)	P1—O2	1.4729 (15)
Cs—O3^v	3.2628 (16)	P1—O3	1.4791 (15)
Cs—O5^ii	3.409 (2)	P1—O5	1.6072 (9)
Cs—O5^iii	3.448 (2)	P1—O1	1.6108 (15)
Cs—O1^i	3.6166 (15)	P1—Cs^ii	3.9542 (5)
Cs—O1	3.6166 (15)	P1—Cs^xi	3.9669 (5)
Cs—O4	3.8029 (2)	P2—O6	1.466 (2)
Cs—O4^vi	3.8029 (2)	P2—O4	1.480 (2)
Ca—O6^vii	2.284 (2)	P2—O1	1.6196 (16)
Ca—O2^iii	2.3148 (16)	P2—O1^xii	1.6196 (16)
Ca—O2^viii	2.3148 (16)	P2—Cs^x	4.2147 (3)
O3^i—Cs—O3	58.37 (6)	O3^ii—Ca—Cs^ii	50.79 (4)
O3^i—Cs—O4^ii	59.56 (4)	O3^ix—Ca—Cs^ii	50.79 (4)
O3—Cs—O4^ii	59.56 (4)	O4—Ca—Cs^ii	51.02 (5)
O3^i—Cs—O2^iii	167.45 (4)	O6^vii—Ca—Cs	117.860 (7)
O3—Cs—O2^iii	111.44 (4)	O2^iii—Ca—Cs	47.76 (4)
O4^ii—Cs—O2^iii	123.66 (4)	O2^viii—Ca—Cs	132.72 (4)
O3^i—Cs—O2^iv	111.44 (4)	O3^ii—Ca—Cs	49.02 (4)
O3—Cs—O2^iv	167.45 (4)	O3^ix—Ca—Cs	121.20 (4)
O4^ii—Cs—O2^iv	123.66 (4)	O4—Ca—Cs	62.232 (7)
O2^iii—Cs—O2^iv	77.52 (6)	Cs^ii—Ca—Cs	71.179 (8)
O3^i—Cs—O3^ii	121.42 (2)	O6^vii—Ca—Cs^x	117.860 (7)
O3—Cs—O3^ii	81.72 (4)	O2^iii—Ca—Cs^x	132.72 (4)
O4^ii—Cs—O3^ii	63.67 (4)	O2^viii—Ca—Cs^x	47.76 (4)
O2^iii—Cs—O3^ii	59.99 (4)	O3^ii—Ca—Cs^x	121.20 (4)
O2^iv—Cs—O3^ii	110.73 (4)	O3^ix—Ca—Cs^x	49.02 (4)
O3^i—Cs—O3^v	81.72 (4)	O4—Ca—Cs^x	62.232 (7)
O3—Cs—O3^v	121.42 (2)	Cs^ii—Ca—Cs^x	71.179 (8)
O4^ii—Cs—O3^v	63.67 (4)	Cs—Ca—Cs^x	124.263 (14)
O2^iii—Cs—O3^v	110.73 (4)	O2—P1—O3	119.37 (10)
O2^iv—Cs—O3^v	59.99 (4)	O2—P1—O5	108.89 (11)
O3^ii—Cs—O3^v	86.02 (5)	O3—P1—O5	106.34 (10)
O3^i—Cs—O5^ii	110.61 (4)	O2—P1—O1	108.90 (9)
O3—Cs—O5^ii	110.61 (4)	O3—P1—O1	109.41 (9)
O4^ii—Cs—O5^ii	59.25 (5)	O5—P1—O1	102.61 (9)
O2^iii—Cs—O5^ii	79.16 (4)	O2—P1—Cs^ii	151.88 (7)
O2^iv—Cs—O5^ii	79.16 (4)	O3—P1—Cs^ii	52.15 (6)
O3^ii—Cs—O5^ii	43.42 (3)	O5—P1—Cs^ii	58.74 (8)
O3^v—Cs—O5^ii	43.42 (3)	O1—P1—Cs^ii	98.79 (6)
O3^i—Cs—O5^iii	137.36 (3)	O2—P1—Cs^xi	49.70 (7)
O3—Cs—O5^iii	137.36 (3)	O3—P1—Cs^xi	125.88 (6)
O4^ii—Cs—O5^iii	158.06 (5)	O5—P1—Cs^xi	59.70 (8)
O2^iii—Cs—O5^iii	44.03 (3)	O1—P1—Cs^xi	124.44 (6)
O2^iv—Cs—O5^iii	44.03 (3)	Cs^ii—P1—Cs^xi	109.848 (12)
O3^ii—Cs—O5^iii	101.20 (4)	O2—P1—Cs	120.29 (7)
O3^v—Cs—O5^iii	101.20 (4)	O3—P1—Cs	47.55 (6)
O5^ii—Cs—O5^iii	98.81 (2)	O5—P1—Cs	130.77 (8)
O3^i—Cs—O1^i	42.94 (3)	O1—P1—Cs	64.74 (6)
O3—Cs—O1^i	87.20 (4)	Cs^ii—P1—Cs	75.746 (9)
O4^ii—Cs—O1^i	101.14 (3)	Cs^xi—P1—Cs	166.707 (15)
O2^iii—Cs—O1^i	135.09 (4)	O6—P2—O4	120.79 (14)
O2^iv—Cs—O1^i	80.27 (4)	O6—P2—O1	108.25 (8)
O3^ii—Cs—O1^i	164.36 (4)	O4—P2—O1	108.45 (8)
O3^v—Cs—O1^i	90.40 (3)	O6—P2—O1^xii	108.25 (8)
O5^ii—Cs—O1^i	133.56 (3)	O4—P2—O1^xii	108.45 (8)
O5^iii—Cs—O1^i	94.43 (3)	O1—P2—O1^xii	100.81 (11)
O3^i—Cs—O1	87.20 (4)	O6—P2—Cs^x	101.48 (4)
O3—Cs—O1	42.94 (3)	O4—P2—Cs^x	63.883 (10)
O4^ii—Cs—O1	101.14 (3)	O1—P2—Cs^x	147.97 (6)
O2^iii—Cs—O1	80.27 (4)	O1^xii—P2—Cs^x	57.64 (6)
O2^iv—Cs—O1	135.09 (4)	O6—P2—Cs	101.48 (4)
O3^ii—Cs—O1	90.40 (3)	O4—P2—Cs	63.883 (10)
O3^v—Cs—O1	164.36 (4)	O1—P2—Cs	57.64 (5)
O5^ii—Cs—O1	133.56 (3)	O1^xii—P2—Cs	147.97 (6)
O5^iii—Cs—O1	94.43 (3)	Cs^x—P2—Cs	127.629 (19)
O1^i—Cs—O1	88.96 (5)	P1—O1—P2	125.47 (10)
O3^i—Cs—O4^vi	57.56 (4)	P1—O1—Cs	91.51 (6)
O3—Cs—O4^vi	115.69 (4)	P2—O1—Cs	100.13 (7)
O4^ii—Cs—O4^vi	92.06 (3)	P1—O2—Ca^xi	149.16 (11)
O2^iii—Cs—O4^vi	131.03 (4)	P1—O2—Cs^xi	109.86 (8)
O2^iv—Cs—O4^vi	53.93 (4)	Ca^xi—O2—Cs^xi	100.05 (5)
O3^ii—Cs—O4^vi	138.70 (4)	P1—O3—Ca^ii	139.36 (10)
O3^v—Cs—O4^vi	52.73 (4)	P1—O3—Cs	112.45 (8)
O5^ii—Cs—O4^vi	95.89 (3)	Ca^ii—O3—Cs	94.53 (5)
O5^iii—Cs—O4^vi	90.19 (3)	P1—O3—Cs^ii	106.88 (8)
O1^i—Cs—O4^vi	39.55 (4)	Ca^ii—O3—Cs^ii	98.13 (5)
O1—Cs—O4^vi	128.51 (4)	Cs—O3—Cs^ii	98.28 (4)
O6^vii—Ca—O2^iii	90.51 (6)	P2—O4—Ca	136.78 (13)
O6^vii—Ca—O2^viii	90.51 (6)	P2—O4—Cs^ii	129.13 (11)
O2^iii—Ca—O2^viii	99.62 (9)	Ca—O4—Cs^ii	94.09 (7)
O6^vii—Ca—O3^ii	97.45 (6)	P2—O4—Cs^x	95.66 (3)
O2^iii—Ca—O3^ii	88.10 (6)	Ca—O4—Cs^x	84.54 (3)
O2^viii—Ca—O3^ii	168.89 (6)	Cs^ii—O4—Cs^x	87.94 (3)
O6^vii—Ca—O3^ix	97.45 (6)	P2—O4—Cs	95.66 (3)
O2^iii—Ca—O3^ix	168.89 (6)	Ca—O4—Cs	84.54 (3)
O2^viii—Ca—O3^ix	88.10 (6)	Cs^ii—O4—Cs	87.94 (3)
O3^ii—Ca—O3^ix	83.20 (8)	Cs^x—O4—Cs	168.02 (6)
O6^vii—Ca—O4	176.71 (8)	P1^xii—O5—P1	135.84 (13)
O2^iii—Ca—O4	87.37 (5)	P1^xii—O5—Cs^ii	97.50 (8)
O2^viii—Ca—O4	87.37 (5)	P1—O5—Cs^ii	97.50 (8)
O3^ii—Ca—O4	85.00 (6)	P1^xii—O5—Cs^xi	96.57 (8)
O3^ix—Ca—O4	85.00 (6)	P1—O5—Cs^xi	96.57 (8)
O6^vii—Ca—Cs^ii	132.27 (6)	Cs^ii—O5—Cs^xi	141.97 (6)
O2^iii—Ca—Cs^ii	118.14 (4)	P2—O6—Ca^xiii	166.31 (16)
O2^viii—Ca—Cs^ii	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.