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The crystal structure of the title compound, Cd2P2O7, has been reinvestigated by means of an image-plate diffraction system. The study confirms the previously determined structure [Calvo & Au (1969). Can. J. Chem. 47, 3409–3417], but provides a less biased model and higher precision. The structure consists of alternating layers of isolated P2O7 groups and edge-sharing CdO6 octa­hedra forming corrugated chains along [1\overline{1}0]. The layers and the parallel chains inter­connect by means of corner-sharing. This room-temperature structure is actually the average of a modulated structure, which might partly rectify the unusual bond valences.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806008397/wm6128sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806008397/wm6128Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](P-O) = 0.003 Å
  • R factor = 0.022
  • wR factor = 0.055
  • Data-to-parameter ratio = 11.8

checkCIF/PLATON results

No syntax errors found



Alert level A REFLT03_ALERT_3_A Reflection count < 85% complete (theta max?) From the CIF: _diffrn_reflns_theta_max 29.07 From the CIF: _diffrn_reflns_theta_full 29.07 From the CIF: _reflns_number_total 1189 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 1425 Completeness (_total/calc) 83.44%
Author Response: We planned two runs, one at phi=0 deg and one at pohi=90 deg. Unfortunately, the crystal mysteriously disappeared after the first run.
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.83
Author Response: same answer as above!

Alert level C PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced .......... ?
2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 2 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: X-AREA (Stoe & Cie, 2005); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: DIRDIF (Beurskens et al., 1996); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1996) and CrystalMaker (Palmer, 2004); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

Cadmium diphosphate top
Crystal data top
Cd2(P2O7)Z = 2
Mr = 398.74F(000) = 364
Triclinic, P1Dx = 4.964 (2) Mg m3
Dm = 4.90 Mg m3
Dm measured by Calvo & Au (1969)
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.6075 (13) ÅCell parameters from 4542 reflections
b = 6.6371 (13) Åθ = 3.1–29.4°
c = 6.7887 (14) ŵ = 8.57 mm1
α = 95.82 (3)°T = 292 K
β = 115.13 (3)°Platelet, colourless
γ = 82.24 (3)°0.50 × 0.40 × 0.15 mm
V = 266.75 (11) Å3
Data collection top
Stoe IPDS-2
diffractometer
1189 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus1162 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.052
Detector resolution: 6.67 pixels mm-1θmax = 29.1°, θmin = 3.1°
ω scansh = 88
Absorption correction: integration
(X-RED; Stoe & Cie, 2005)
k = 98
Tmin = 0.162, Tmax = 0.314l = 99
2251 measured reflections
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)] = 0.022 w = 1/[σ2(Fo2) + (0.0173P)2 + 0.5407P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055(Δ/σ)max = 0.001
S = 1.25Δρmax = 0.54 e Å3
1189 reflectionsΔρmin = 0.88 e Å3
101 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.292 (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
Cd10.27522 (4)0.36011 (4)0.33760 (4)0.01039 (12)
Cd20.11672 (4)0.16059 (3)0.74836 (4)0.00682 (12)
P10.36229 (15)0.86612 (13)0.18989 (15)0.00487 (19)
P20.23622 (15)0.65878 (12)0.75488 (14)0.00449 (19)
O10.4032 (4)0.7487 (4)0.9858 (4)0.0078 (5)
O20.0690 (5)0.8336 (4)0.6354 (4)0.0099 (5)
O30.6004 (4)0.8650 (4)0.3669 (4)0.0082 (5)
O40.3913 (4)0.5669 (4)0.6495 (4)0.0079 (5)
O50.2578 (5)0.0810 (4)0.1129 (4)0.0091 (5)
O60.1009 (5)0.5043 (4)0.7858 (5)0.0112 (5)
O70.2109 (4)0.7452 (4)0.2351 (4)0.0096 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.00774 (18)0.01239 (17)0.01146 (19)0.00300 (11)0.00504 (13)0.00500 (11)
Cd20.00723 (17)0.00594 (16)0.00851 (18)0.00034 (10)0.00447 (13)0.00074 (10)
P10.0038 (4)0.0065 (4)0.0049 (4)0.0010 (3)0.0022 (3)0.0009 (3)
P20.0046 (4)0.0042 (4)0.0053 (4)0.0015 (3)0.0026 (3)0.0006 (3)
O10.0040 (12)0.0133 (11)0.0068 (12)0.0027 (9)0.0032 (10)0.0026 (9)
O20.0108 (13)0.0076 (11)0.0095 (13)0.0006 (9)0.0030 (11)0.0001 (9)
O30.0038 (12)0.0110 (11)0.0081 (12)0.0011 (9)0.0009 (10)0.0004 (9)
O40.0075 (12)0.0090 (11)0.0096 (12)0.0022 (9)0.0056 (10)0.0007 (9)
O50.0110 (13)0.0057 (10)0.0090 (12)0.0011 (9)0.0030 (10)0.0019 (8)
O60.0097 (13)0.0085 (11)0.0188 (14)0.0042 (9)0.0086 (11)0.0000 (9)
O70.0080 (13)0.0116 (11)0.0130 (13)0.0015 (9)0.0069 (10)0.0042 (9)
Geometric parameters (Å, º) top
Cd1—O52.260 (2)O1—O22.516 (4)
Cd1—O4i2.283 (3)O1—O62.567 (4)
Cd1—O42.296 (3)O1—O74.698 (4)
Cd1—O6ii2.338 (3)O1—O35.052 (4)
Cd1—O3i2.410 (3)O1—O56.831 (4)
Cd1—O72.648 (3)O2—Cd2v2.245 (2)
Cd2—O7ii2.217 (3)O2—Cd2ii2.364 (3)
Cd2—O2iii2.245 (2)O2—O62.452 (4)
Cd2—O62.263 (2)O2—O42.554 (4)
Cd2—O3i2.294 (3)O3—Cd2i2.294 (3)
Cd2—O5iv2.334 (3)O3—Cd1i2.410 (3)
Cd2—O2ii2.364 (3)O3—O1vi2.448 (4)
P1—O71.505 (3)O3—O5v2.542 (4)
P1—O31.521 (3)O3—O72.551 (4)
P1—O5v1.537 (3)O3—O55.764 (4)
P1—O1vi1.626 (3)O4—Cd1i2.283 (3)
P1—P2vi2.9503 (16)O4—O62.552 (4)
P2—O41.516 (3)O5—P1iii1.537 (3)
P2—O21.520 (3)O5—Cd2vi2.334 (3)
P2—O61.532 (3)O5—O74.396 (3)
P2—O11.597 (3)O6—Cd1ii2.338 (3)
O1—P1iv1.626 (3)O7—Cd2ii2.217 (3)
O1—O42.447 (3)O7—O1vi2.514 (4)
O1—O5vii2.506 (3)O7—O5v2.555 (4)
O5—Cd1—O4i93.56 (10)P1—O3—Cd1i119.78 (15)
O5—Cd1—O4159.61 (9)Cd2i—O3—Cd1i106.58 (11)
O4i—Cd1—O480.41 (10)Cd2i—O3—O1vi79.01 (10)
O5—Cd1—O6ii102.73 (10)Cd1i—O3—O1vi122.29 (12)
O4i—Cd1—O6ii140.14 (10)Cd2i—O3—O5v110.18 (13)
O4—Cd1—O6ii94.07 (10)Cd1i—O3—O5v142.61 (13)
O5—Cd1—O3i87.81 (9)O1vi—O3—O5v60.26 (11)
O4i—Cd1—O3i101.75 (10)Cd2i—O3—O7137.85 (12)
O4—Cd1—O3i74.56 (9)Cd1i—O3—O787.76 (11)
O6ii—Cd1—O3i114.84 (10)O1vi—O3—O760.35 (10)
O5—Cd1—O7127.01 (9)O5v—O3—O760.23 (11)
O4i—Cd1—O774.14 (9)P1—O3—O195.95 (12)
O4—Cd1—O770.28 (9)Cd2i—O3—O1145.15 (10)
O6ii—Cd1—O766.95 (9)O1vi—O3—O1126.09 (11)
O3i—Cd1—O7144.80 (8)O5v—O3—O1103.87 (10)
O7ii—Cd2—O2iii98.88 (10)O7—O3—O167.26 (9)
O7ii—Cd2—O676.13 (10)P1—O3—O564.60 (10)
O2iii—Cd2—O6166.83 (11)Cd2i—O3—O5103.49 (8)
O7ii—Cd2—O3i160.31 (10)Cd1i—O3—O565.94 (6)
O2iii—Cd2—O3i88.25 (10)O1vi—O3—O557.22 (9)
O6—Cd2—O3i92.82 (10)O5v—O3—O598.57 (10)
O7ii—Cd2—O5iv87.31 (10)O7—O3—O546.06 (8)
O2iii—Cd2—O5iv91.72 (9)O1—O3—O578.02 (6)
O6—Cd2—O5iv100.13 (10)P2—O4—Cd1i135.22 (14)
O3i—Cd2—O5iv110.93 (10)P2—O4—Cd1123.02 (14)
O7ii—Cd2—O2ii88.90 (10)Cd1i—O4—Cd199.59 (10)
O2iii—Cd2—O2ii75.37 (11)Cd1i—O4—O199.69 (11)
O6—Cd2—O2ii92.21 (10)Cd1—O4—O1160.58 (13)
O3i—Cd2—O2ii75.09 (10)Cd1i—O4—O6158.84 (14)
O5iv—Cd2—O2ii165.82 (9)Cd1—O4—O698.86 (11)
O7—P1—O3114.94 (16)O1—O4—O661.75 (11)
O7—P1—O5v114.27 (16)Cd1i—O4—O2124.46 (11)
O3—P1—O5v112.48 (15)Cd1—O4—O2109.55 (12)
O7—P1—O1vi106.77 (14)O1—O4—O260.35 (11)
O3—P1—O1vi102.09 (14)O6—O4—O257.39 (11)
O5v—P1—O1vi104.78 (15)P1iii—O5—Cd1124.47 (16)
O7—P1—P2vi90.46 (11)P1iii—O5—Cd2vi122.26 (14)
O3—P1—P2vi125.06 (11)Cd1—O5—Cd2vi112.52 (11)
O5v—P1—P2vi97.26 (11)P1iii—O5—O7150.57 (14)
O4—P2—O2114.55 (16)Cd2vi—O5—O784.11 (8)
O4—P2—O6113.72 (14)P1iii—O5—O3132.13 (13)
O2—P2—O6106.92 (16)Cd2vi—O5—O389.34 (8)
O4—P2—O1103.60 (14)P1iii—O5—O1110.41 (12)
O2—P2—O1107.62 (14)Cd2vi—O5—O1126.84 (8)
O6—P2—O1110.26 (16)O3—O5—O146.35 (4)
P2—O1—P1iv132.56 (17)P2—O6—Cd2133.13 (16)
P1iv—O1—O4169.57 (16)P2—O6—Cd1ii108.83 (15)
P2—O1—O5vii115.01 (15)Cd2—O6—Cd1ii109.01 (11)
O4—O1—O5vii140.17 (15)Cd2—O6—O2150.13 (15)
P1iv—O1—O2109.67 (14)Cd1ii—O6—O272.60 (11)
O4—O1—O261.93 (11)Cd2—O6—O4100.50 (12)
O5vii—O1—O281.75 (12)Cd1ii—O6—O4128.31 (14)
P1iv—O1—O6109.62 (14)O2—O6—O461.34 (11)
O4—O1—O661.14 (10)Cd2—O6—O1132.41 (14)
O5vii—O1—O6113.74 (13)Cd1ii—O6—O1117.66 (12)
O2—O1—O657.67 (11)O2—O6—O160.11 (11)
P1iv—O1—O7145.57 (13)O4—O6—O157.11 (10)
O5vii—O1—O7110.26 (11)P1—O7—Cd2ii130.49 (15)
O6—O1—O771.23 (9)Cd2ii—O7—O1vi141.04 (14)
P2—O1—O366.36 (10)Cd2ii—O7—O3140.33 (13)
P1iv—O1—O3142.18 (12)O1vi—O7—O357.78 (10)
O5vii—O1—O3109.41 (10)Cd2ii—O7—O5v97.56 (12)
O2—O1—O365.74 (9)O1vi—O7—O5v59.24 (10)
O6—O1—O399.06 (10)O3—O7—O5v59.70 (11)
P1iv—O1—O5159.01 (11)P1—O7—Cd1129.13 (15)
O5vii—O1—O5145.04 (12)Cd2ii—O7—Cd1100.32 (10)
O2—O1—O563.35 (8)O1vi—O7—Cd1104.30 (11)
O6—O1—O549.48 (8)O3—O7—Cd1106.39 (12)
O3—O1—O555.63 (5)O5v—O7—Cd1161.96 (13)
P2—O2—Cd2v122.45 (15)P1—O7—O5119.05 (13)
P2—O2—Cd2ii123.45 (14)Cd2ii—O7—O5107.18 (9)
Cd2v—O2—Cd2ii104.63 (11)O1vi—O7—O585.56 (9)
Cd2v—O2—O6139.52 (14)O3—O7—O5109.24 (11)
Cd2ii—O2—O6115.07 (12)O5v—O7—O5144.08 (13)
Cd2v—O2—O185.91 (11)P1—O7—O1111.11 (13)
Cd2ii—O2—O1153.02 (13)Cd2ii—O7—O177.60 (8)
O6—O2—O162.22 (11)O1vi—O7—O1138.50 (12)
Cd2v—O2—O4123.18 (13)O3—O7—O182.68 (10)
Cd2ii—O2—O496.54 (11)O5v—O7—O1113.42 (10)
O6—O2—O461.27 (10)Cd1—O7—O173.11 (7)
O1—O2—O457.72 (10)O5—O7—O197.32 (8)
P1—O3—Cd2i116.43 (15)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x, y1, z; (iv) x, y, z+1; (v) x, y+1, z; (vi) x, y, z1; (vii) x, y+1, z+1.
 

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