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From single-crystal X-ray data, cesium titanium pyrophos­phate, CsTiP2O7, is found to crystallize in the KAlP2O7 structure type. It possesses a three-dimensional tunnel structure built by the corner-sharing of distorted TiO6 octahedra and P2O7 pyrophosphate groups. The Cs+ cations are in the tunnels.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100003036/br1285sup1.cif
Contains datablocks CsTiP2O7, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100003036/br1285Isup2.hkl
Contains datablock I

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL/PC (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1997); software used to prepare material for publication: SHELXTL/PC.

'caesium titanium pyrophosphate' top
Crystal data top
CsTiP2O7F(000) = 652
Mr = 354.75Dx = 3.699 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 7.7247 (6) ÅCell parameters from 4699 reflections
b = 10.2237 (7) Åθ = 2.7–27.0°
c = 8.3429 (6) ŵ = 7.46 mm1
β = 104.788 (1)°T = 153 K
V = 637.05 (8) Å3Plate, purple-blue
Z = 40.23 × 0.20 × 0.09 mm
Data collection top
Bruker Smart 1000 CCD
diffractometer
1279 independent reflections
Radiation source: standard-focus sealed tube1272 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ω scansθmax = 27.0°, θmin = 2.7°
Absorption correction: numerical
face indexed (SHELXTL/PC; Sheldrick, 1997)
h = 910
Tmin = 0.198, Tmax = 0.520k = 1212
4699 measured reflectionsl = 1010
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023 w = 1/[σ2(Fo2) + (0.0400Fo2)2]
wR(F2) = 0.068(Δ/σ)max = 0.001
S = 1.42Δρmax = 1.15 e Å3
1279 reflectionsΔρmin = 1.14 e Å3
101 parametersExtinction correction: SHELXTL/PC (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0082 (7)
Special details top

Experimental. X-ray data were collected on a Bruker Smart- 1000 CCD system. The crystal-to-detector distance was 5.023 cm. Crystal decay was monitored by recollecting 50 initial frames at the end of data collection. Each exposure was 10 s and covered -0.3° in ω. Data were collected in groups of 606, 435, 230 frames at φ settings of 0°, 90°, and 180°.

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. Anisotropic displacement parameters were used for all atoms. All sites are fully occupied.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cs0.19698 (2)0.800752 (16)0.04465 (2)0.01042 (14)
Ti0.23894 (7)0.39850 (4)0.25875 (6)0.00422 (16)
P10.13198 (10)0.09468 (6)0.33116 (9)0.00459 (18)
P20.42723 (9)0.12928 (6)0.18254 (9)0.00494 (18)
O10.0063 (3)0.50010 (16)0.2667 (2)0.0056 (4)
O20.0908 (2)0.23357 (18)0.2678 (2)0.0074 (4)
O30.1571 (3)0.41543 (18)0.0153 (3)0.0080 (4)
O40.3206 (2)0.05270 (18)0.2972 (2)0.0073 (4)
O50.3213 (3)0.10378 (17)0.0055 (3)0.0096 (4)
O60.4368 (3)0.27299 (18)0.2293 (3)0.0073 (4)
O70.6125 (2)0.07001 (18)0.2253 (2)0.0075 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs0.00989 (19)0.01156 (18)0.00913 (19)0.00092 (5)0.00120 (11)0.00256 (4)
Ti0.0056 (3)0.0040 (3)0.0032 (3)0.00026 (16)0.0014 (2)0.00017 (15)
P10.0056 (4)0.0041 (3)0.0045 (4)0.0009 (2)0.0021 (3)0.0001 (2)
P20.0059 (3)0.0046 (3)0.0048 (4)0.0003 (2)0.0022 (3)0.0001 (2)
O10.0061 (9)0.0050 (9)0.0063 (9)0.0022 (6)0.0028 (7)0.0011 (6)
O20.0091 (9)0.0053 (8)0.0075 (9)0.0005 (7)0.0016 (7)0.0010 (7)
O30.0088 (9)0.0091 (9)0.0063 (9)0.0018 (7)0.0023 (8)0.0003 (7)
O40.0074 (9)0.0063 (8)0.0094 (10)0.0014 (7)0.0041 (7)0.0017 (6)
O50.0122 (10)0.0088 (10)0.0066 (10)0.0001 (7)0.0007 (7)0.0005 (7)
O60.0069 (9)0.0065 (8)0.0100 (10)0.0001 (7)0.0045 (7)0.0003 (7)
O70.0066 (9)0.0077 (9)0.0090 (9)0.0012 (7)0.0036 (7)0.0003 (7)
Geometric parameters (Å, º) top
Cs—O2i2.9840 (18)P1—O41.612 (2)
Cs—O6ii2.9859 (19)P1—Csix3.6488 (8)
Cs—O2iii3.105 (2)P1—Csi3.6556 (8)
Cs—O1iv3.1544 (18)P1—Csxi3.9508 (7)
Cs—O7ii3.1577 (18)P2—O71.511 (2)
Cs—O1iii3.2186 (19)P2—O51.517 (2)
Cs—O7v3.267 (2)P2—O61.517 (2)
Cs—O5vi3.2843 (18)P2—O41.615 (2)
Cs—O4vi3.3105 (19)P2—Csx3.6479 (7)
Cs—O3i3.452 (2)P2—Csxi3.8372 (7)
Cs—P2ii3.6479 (7)P2—Csv3.9166 (8)
Cs—P1iii3.6488 (8)O1—P1iii1.5155 (19)
Ti—O31.974 (2)O1—Csviii3.1544 (18)
Ti—O5vii1.994 (2)O1—Csix3.2186 (19)
Ti—O22.0499 (19)O2—Csi2.9840 (18)
Ti—O62.058 (2)O2—Csix3.105 (2)
Ti—O7ii2.0810 (19)O3—P1xii1.503 (2)
Ti—O12.091 (2)O3—Csi3.452 (2)
Ti—Csviii3.9552 (5)O4—Csxi3.3105 (19)
Ti—Csi4.1887 (5)O5—Tixii1.994 (2)
Ti—Csix4.2247 (6)O5—Csxi3.2843 (18)
Ti—Csx4.3619 (6)O6—Csx2.9859 (19)
P1—O3vii1.503 (2)O7—Tix2.0810 (19)
P1—O1ix1.5155 (19)O7—Csx3.1577 (18)
P1—O21.5201 (19)O7—Csv3.267 (2)
O2i—Cs—O6ii156.22 (6)O6—Ti—Csix126.07 (6)
O2i—Cs—O2iii86.82 (5)O7ii—Ti—Csix130.97 (6)
O6ii—Cs—O2iii110.22 (5)O1—Ti—Csix47.83 (5)
O2i—Cs—O1iv47.90 (5)Csviii—Ti—Csix75.736 (10)
O6ii—Cs—O1iv135.65 (5)Csi—Ti—Csix61.449 (9)
O2iii—Cs—O1iv104.67 (5)O3—Ti—Csx115.71 (6)
O2i—Cs—O7ii124.81 (5)O5vii—Ti—Csx65.43 (6)
O6ii—Cs—O7ii47.61 (5)O2—Ti—Csx108.12 (5)
O2iii—Cs—O7ii79.11 (5)O6—Ti—Csx36.96 (5)
O1iv—Cs—O7ii170.66 (5)O7ii—Ti—Csx71.79 (5)
O2i—Cs—O1iii98.86 (5)O1—Ti—Csx152.37 (5)
O6ii—Cs—O1iii104.66 (5)Csviii—Ti—Csx100.318 (10)
O2iii—Cs—O1iii52.56 (5)Csi—Ti—Csx133.444 (12)
O1iv—Cs—O1iii75.90 (6)Csix—Ti—Csx128.209 (13)
O7ii—Cs—O1iii112.68 (5)O3—Ti—Cs62.36 (6)
O2i—Cs—O7v79.13 (5)O5vii—Ti—Cs113.30 (5)
O6ii—Cs—O7v87.31 (5)O2—Ti—Cs142.06 (5)
O2iii—Cs—O7v160.61 (5)O6—Ti—Cs120.48 (6)
O1iv—Cs—O7v55.95 (5)O7ii—Ti—Cs39.79 (5)
O7ii—Cs—O7v119.94 (6)O1—Ti—Cs65.15 (5)
O1iii—Cs—O7v116.29 (5)Csviii—Ti—Cs61.065 (8)
O2i—Cs—O5vi101.28 (5)Csi—Ti—Cs103.961 (11)
O6ii—Cs—O5vi84.18 (5)Csix—Ti—Cs112.939 (11)
O2iii—Cs—O5vi121.60 (5)Csx—Ti—Cs108.977 (10)
O1iv—Cs—O5vi53.95 (5)O3vii—P1—O1ix113.33 (12)
O7ii—Cs—O5vi131.48 (5)O3vii—P1—O2112.37 (11)
O1iii—Cs—O5vi69.07 (5)O1ix—P1—O2110.66 (10)
O7v—Cs—O5vi49.87 (5)O3vii—P1—O4105.96 (11)
O2i—Cs—O4vi132.62 (5)O1ix—P1—O4106.26 (11)
O6ii—Cs—O4vi66.37 (5)O2—P1—O4107.81 (11)
O2iii—Cs—O4vi88.78 (5)O3vii—P1—Csix70.53 (8)
O1iv—Cs—O4vi88.31 (4)O1ix—P1—Csix94.31 (8)
O7ii—Cs—O4vi100.40 (5)O2—P1—Csix57.34 (8)
O1iii—Cs—O4vi45.05 (5)O4—P1—Csix158.43 (7)
O7v—Cs—O4vi90.95 (5)O3vii—P1—Csi141.01 (9)
O5vi—Cs—O4vi44.37 (5)O1ix—P1—Csi58.98 (7)
O2i—Cs—O3i53.98 (5)O2—P1—Csi52.47 (7)
O6ii—Cs—O3i128.21 (5)O4—P1—Csi112.88 (7)
O2iii—Cs—O3i44.65 (5)Csix—P1—Csi72.100 (14)
O1iv—Cs—O3i95.89 (5)O3vii—P1—Csxi124.29 (8)
O7ii—Cs—O3i80.72 (5)O1ix—P1—Csxi50.94 (8)
O1iii—Cs—O3i90.51 (5)O2—P1—Csxi123.22 (8)
O7v—Cs—O3i129.68 (5)O4—P1—Csxi55.32 (7)
O5vi—Cs—O3i146.15 (5)Csix—P1—Csxi144.71 (2)
O4vi—Cs—O3i132.81 (5)Csi—P1—Csxi82.611 (15)
O2i—Cs—P2ii141.76 (4)O7—P2—O5113.84 (12)
O6ii—Cs—P2ii23.87 (4)O7—P2—O6110.28 (10)
O2iii—Cs—P2ii97.90 (4)O5—P2—O6113.30 (11)
O1iv—Cs—P2ii156.46 (4)O7—P2—O4105.14 (10)
O7ii—Cs—P2ii24.31 (4)O5—P2—O4105.27 (11)
O1iii—Cs—P2ii114.14 (4)O6—P2—O4108.41 (11)
O7v—Cs—P2ii101.41 (4)O7—P2—Csx59.36 (7)
O5vi—Cs—P2ii108.00 (4)O5—P2—Csx146.68 (8)
O4vi—Cs—P2ii85.55 (3)O6—P2—Csx52.79 (7)
O3i—Cs—P2ii104.93 (3)O4—P2—Csx107.95 (7)
O2i—Cs—P1iii76.27 (4)O7—P2—Csxi93.35 (7)
O6ii—Cs—P1iii112.45 (4)O5—P2—Csxi57.60 (7)
O2iii—Cs—P1iii24.35 (4)O6—P2—Csxi155.96 (7)
O1iv—Cs—P1iii110.68 (4)O4—P2—Csxi59.06 (7)
O7ii—Cs—P1iii69.29 (4)Csx—P2—Csxi147.335 (19)
O1iii—Cs—P1iii76.39 (3)O7—P2—Csv54.06 (8)
O7v—Cs—P1iii153.90 (3)O5—P2—Csv80.94 (8)
O5vi—Cs—P1iii144.62 (4)O6—P2—Csv87.37 (8)
O4vi—Cs—P1iii112.16 (4)O4—P2—Csv158.15 (7)
O3i—Cs—P1iii24.23 (4)Csx—P2—Csv69.153 (13)
P2ii—Cs—P1iii92.654 (17)Csxi—P2—Csv111.030 (18)
O3—Ti—O5vii175.64 (8)P1iii—O1—Ti142.48 (14)
O3—Ti—O294.29 (8)P1iii—O1—Csviii96.70 (8)
O5vii—Ti—O289.21 (8)Ti—O1—Csviii95.74 (7)
O3—Ti—O689.12 (8)P1iii—O1—Csix107.61 (10)
O5vii—Ti—O693.73 (8)Ti—O1—Csix103.38 (6)
O2—Ti—O685.99 (8)Csviii—O1—Csix104.10 (6)
O3—Ti—O7ii91.06 (8)P1—O2—Ti135.41 (11)
O5vii—Ti—O7ii85.33 (8)P1—O2—Csi103.70 (9)
O2—Ti—O7ii174.00 (8)Ti—O2—Csi111.28 (8)
O6—Ti—O7ii96.83 (8)P1—O2—Csix98.31 (9)
O3—Ti—O186.36 (8)Ti—O2—Csix108.35 (8)
O5vii—Ti—O191.34 (8)Csi—O2—Csix89.80 (5)
O2—Ti—O185.13 (7)P1xii—O3—Ti165.86 (14)
O6—Ti—O1169.71 (8)P1xii—O3—Csi85.25 (8)
O7ii—Ti—O192.50 (7)Ti—O3—Csi97.30 (7)
O3—Ti—Csviii119.87 (6)P1—O4—P2126.54 (12)
O5vii—Ti—Csviii55.94 (5)P1—O4—Csxi101.08 (8)
O2—Ti—Csviii119.00 (6)P2—O4—Csxi96.20 (8)
O6—Ti—Csviii137.26 (6)P2—O5—Tixii163.30 (13)
O7ii—Ti—Csviii55.61 (6)P2—O5—Csxi99.45 (9)
O1—Ti—Csviii52.52 (5)Tixii—O5—Csxi93.86 (6)
O3—Ti—Csi54.83 (6)P2—O6—Ti130.21 (11)
O5vii—Ti—Csi127.86 (6)P2—O6—Csx103.34 (9)
O2—Ti—Csi41.59 (5)Ti—O6—Csx118.56 (8)
O6—Ti—Csi97.56 (6)P2—O7—Tix145.76 (12)
O7ii—Ti—Csi142.51 (5)P2—O7—Csx96.33 (9)
O1—Ti—Csi72.29 (5)Tix—O7—Csx115.27 (7)
Csviii—Ti—Csi124.438 (13)P2—O7—Csv103.95 (9)
O3—Ti—Csix110.01 (6)Tix—O7—Csv92.68 (7)
O5vii—Ti—Csix70.86 (6)Csx—O7—Csv83.96 (4)
O2—Ti—Csix44.22 (6)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+1/2, z+1/2; (iii) x, y+1/2, z+1/2; (iv) x, y+3/2, z1/2; (v) x+1, y+1, z; (vi) x, y+1, z; (vii) x, y+1/2, z+1/2; (viii) x, y+3/2, z+1/2; (ix) x, y1/2, z+1/2; (x) x+1, y1/2, z+1/2; (xi) x, y1, z; (xii) x, y+1/2, z1/2.
 

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