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Crystals of CsGd(PO3)4 have been grown by the flux technique from a mixture of CsH2PO4, Gd2O3 and H3PO4. CsGd(PO3)4 crystallizes in structure type IV of the MIMIII(PO3)4 (MI = alkali metal, MIII = rare earth or Bi) family of compounds. The structure consists of a three-dimensional framework made up of spiral (PO3)n chains linked by GdO8 polyhedra. Two infinite (PO3)n chains with a period of eight tetra­hedra run along the [101] direction. Gd and Cs cations are surrounded by eight and eleven O atoms, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805025705/wm6085sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805025705/wm6085Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](P-O) = 0.002 Å
  • R factor = 0.018
  • wR factor = 0.046
  • Data-to-parameter ratio = 42.6

checkCIF/PLATON results

No syntax errors found



Alert level G ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.177 0.271 Tmin and Tmax expected: 0.084 0.171 RR = 1.329 Please check that your absorption correction is appropriate.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 1 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 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); 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: SHELXL97.

Caesium gadolinium polyphosphate top
Crystal data top
CsGd(PO3)4F(000) = 1100
Mr = 606.04Dx = 4.070 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 9641 reflections
a = 10.3229 (2) Åθ = 2–40°
b = 8.9307 (2) ŵ = 11.04 mm1
c = 11.1826 (2) ÅT = 292 K
β = 106.371 (1)°Needle, colourless
V = 989.13 (3) Å30.26 × 0.20 × 0.16 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
6980 independent reflections
Radiation source: fine-focus sealed tube5595 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.071
Detector resolution: 9 pixels mm-1θmax = 42.1°, θmin = 3.0°
ω scansh = 1419
Absorption correction: analytical
(de Meulenaer & Tompa, 1965)
k = 1615
Tmin = 0.177, Tmax = 0.271l = 2120
19421 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: heavy-atom method
R[F2 > 2σ(F2)] = 0.018Secondary atom site location: difference Fourier map
wR(F2) = 0.046 w = 1/[σ2(Fo2) + (0.0187P)2 + 2.8091P]
where P = (Fo2 + 2Fc2)/3
S = 1.24(Δ/σ)max = 0.001
6980 reflectionsΔρmax = 0.89 e Å3
164 parametersΔρmin = 0.58 e Å3
Special details top

Experimental. Data were corrected for Lorentz-polarization effects and an analytical absorption correction (Meulenaer & Tompa, 1965) was applied. The structure was solved in the P 1 21/n 1 space group by the Patterson method (Cs and Gd) and subsequent difference Fourier syntheses (all other atoms).

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
Gd0.497879 (11)0.273491 (14)0.180789 (11)0.00726 (4)
Cs0.67903 (2)0.56590 (3)0.459719 (19)0.01910 (6)
P10.64512 (6)0.09227 (9)0.25790 (7)0.00809 (11)
P20.45955 (7)0.32517 (9)0.13266 (7)0.00799 (11)
P30.24454 (6)0.47205 (9)0.21423 (6)0.00771 (11)
P40.17229 (6)0.60738 (9)0.02627 (7)0.00818 (11)
O10.13635 (19)0.5429 (3)0.09486 (19)0.0106 (3)
O20.3514 (2)0.5836 (3)0.2739 (2)0.0111 (3)
O30.5209 (2)0.2067 (3)0.2421 (2)0.0116 (3)
O40.6009 (2)0.0399 (3)0.1762 (2)0.0123 (3)
O50.4394 (2)0.2544 (3)0.0091 (2)0.0133 (3)
O60.1682 (2)0.4037 (3)0.2944 (2)0.0121 (3)
O70.7638 (2)0.1780 (3)0.2463 (2)0.0139 (4)
O80.0641 (2)0.7111 (3)0.0963 (2)0.0126 (4)
O90.3129 (2)0.6654 (3)0.0140 (2)0.0135 (4)
O100.5363 (2)0.4673 (3)0.1652 (2)0.0130 (4)
O110.31122 (19)0.3412 (3)0.1532 (2)0.0106 (3)
O120.6668 (2)0.0479 (3)0.4002 (2)0.0139 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd0.00551 (6)0.00778 (7)0.00655 (6)0.00047 (3)0.00147 (4)0.00069 (3)
Cs0.02011 (9)0.02358 (11)0.01103 (9)0.00406 (6)0.00018 (6)0.00080 (6)
P10.0065 (2)0.0081 (3)0.0074 (2)0.00007 (18)0.00168 (17)0.0006 (2)
P20.0073 (2)0.0076 (3)0.0073 (2)0.00007 (18)0.00079 (17)0.0001 (2)
P30.0062 (2)0.0087 (3)0.0065 (2)0.00102 (18)0.00098 (17)0.00025 (19)
P40.0060 (2)0.0095 (3)0.0063 (2)0.00002 (18)0.00268 (17)0.0001 (2)
O10.0076 (6)0.0161 (9)0.0064 (7)0.0018 (6)0.0009 (5)0.0022 (6)
O20.0095 (7)0.0126 (8)0.0099 (8)0.0037 (6)0.0003 (5)0.0013 (6)
O30.0120 (7)0.0113 (8)0.0096 (8)0.0041 (6)0.0003 (6)0.0031 (6)
O40.0157 (8)0.0096 (8)0.0104 (8)0.0018 (6)0.0018 (6)0.0037 (6)
O50.0115 (7)0.0174 (9)0.0104 (8)0.0024 (7)0.0022 (6)0.0024 (7)
O60.0113 (7)0.0144 (9)0.0108 (8)0.0036 (6)0.0034 (6)0.0011 (7)
O70.0083 (7)0.0158 (10)0.0150 (9)0.0027 (6)0.0009 (6)0.0015 (7)
O80.0114 (8)0.0129 (9)0.0114 (8)0.0033 (6)0.0002 (6)0.0040 (7)
O90.0071 (6)0.0220 (11)0.0093 (8)0.0051 (6)0.0013 (5)0.0016 (7)
O100.0088 (7)0.0102 (9)0.0184 (10)0.0011 (6)0.0012 (6)0.0018 (7)
O110.0062 (6)0.0117 (8)0.0122 (8)0.0008 (5)0.0000 (5)0.0026 (6)
O120.0193 (9)0.0115 (9)0.0074 (8)0.0006 (7)0.0018 (6)0.0024 (6)
Geometric parameters (Å, º) top
Gd—O9i2.327 (2)P2—Csvii3.7855 (7)
Gd—O42.349 (2)P2—Csx3.8451 (7)
Gd—O10i2.363 (2)P3—O61.481 (2)
Gd—O5ii2.394 (3)P3—O21.497 (2)
Gd—O7iii2.403 (2)P3—O111.603 (2)
Gd—O6iv2.406 (2)P3—O11.609 (2)
Gd—O2i2.426 (2)P3—Csviii3.6052 (7)
Gd—O8v2.456 (2)P4—O91.487 (2)
Gd—Cs4.0936 (3)P4—O81.492 (2)
Gd—Csvi4.4703 (3)P4—O12xi1.605 (3)
Gd—Csvii4.6417 (3)P4—O11.608 (2)
Cs—O4iii3.077 (2)P4—Csxi4.0992 (8)
Cs—O2viii3.086 (2)O2—Gdx2.426 (2)
Cs—O5ix3.087 (2)O2—Csviii3.086 (2)
Cs—O6viii3.115 (2)O2—Csx3.684 (2)
Cs—O10i3.220 (2)O3—Csx3.236 (2)
Cs—O3i3.237 (2)O4—Csvi3.077 (2)
Cs—O11ix3.305 (2)O5—Gdii2.394 (3)
Cs—O7iii3.341 (3)O5—Csvii3.087 (2)
Cs—O8v3.379 (3)O6—Gdxii2.406 (2)
Cs—O12i3.509 (3)O6—Csviii3.115 (2)
Cs—O7i3.588 (3)O7—Gdvi2.403 (2)
Cs—P3viii3.6052 (7)O7—Csvi3.341 (3)
P1—O71.481 (2)O7—Csx3.588 (3)
P1—O41.484 (2)O8—Gdxi2.456 (2)
P1—O121.593 (2)O8—Csxi3.379 (3)
P1—O31.610 (2)O9—Gdx2.327 (2)
P1—Csvi3.7017 (8)O10—Gdx2.363 (2)
P1—Csx3.7537 (8)O10—Csx3.220 (2)
P2—O51.480 (3)O11—Csvii3.305 (2)
P2—O101.486 (2)O12—P4v1.605 (3)
P2—O31.607 (2)O12—Csx3.509 (3)
P2—O111.617 (2)
O9i—Gd—O4117.72 (9)O3i—Cs—O7i42.74 (5)
O9i—Gd—O10i80.10 (9)O11ix—Cs—O7i80.11 (6)
O4—Gd—O10i141.43 (8)O7iii—Cs—O7i80.407 (7)
O9i—Gd—O5ii70.82 (8)O8v—Cs—O7i127.81 (6)
O4—Gd—O5ii71.35 (9)O12i—Cs—O7i41.36 (6)
O10i—Gd—O5ii84.91 (9)O4iii—Cs—P3viii120.02 (4)
O9i—Gd—O7iii139.47 (9)O2viii—Cs—P3viii24.29 (4)
O4—Gd—O7iii74.98 (9)O5ix—Cs—P3viii90.83 (5)
O10i—Gd—O7iii70.81 (8)O6viii—Cs—P3viii24.07 (4)
O5ii—Gd—O7iii78.88 (8)O10i—Cs—P3viii156.86 (5)
O9i—Gd—O6iv78.25 (9)O3i—Cs—P3viii145.75 (5)
O4—Gd—O6iv76.14 (8)O11ix—Cs—P3viii65.08 (4)
O10i—Gd—O6iv142.42 (8)O7iii—Cs—P3viii120.98 (4)
O5ii—Gd—O6iv115.80 (9)O8v—Cs—P3viii86.26 (4)
O7iii—Gd—O6iv140.72 (8)O12i—Cs—P3viii113.98 (4)
O9i—Gd—O2i75.57 (8)O7i—Cs—P3viii142.77 (4)
O4—Gd—O2i144.84 (8)O7—P1—O4118.41 (15)
O10i—Gd—O2i69.77 (8)O7—P1—O12109.23 (13)
O5ii—Gd—O2i140.80 (8)O4—P1—O12110.44 (14)
O7iii—Gd—O2i117.49 (8)O7—P1—O3108.38 (14)
O6iv—Gd—O2i75.27 (9)O4—P1—O3109.87 (13)
O9i—Gd—O8v142.91 (8)O12—P1—O398.69 (14)
O4—Gd—O8v79.78 (8)O7—P1—Csvi64.44 (11)
O10i—Gd—O8v107.00 (8)O4—P1—Csvi54.15 (10)
O5ii—Gd—O8v144.76 (8)O12—P1—Csvi127.20 (10)
O7iii—Gd—O8v74.38 (8)O3—P1—Csvi133.87 (9)
O6iv—Gd—O8v74.77 (8)O7—P1—Csx72.13 (11)
O2i—Gd—O8v73.30 (8)O4—P1—Csx167.86 (10)
O9i—Gd—Cs123.81 (7)O12—P1—Csx68.84 (10)
O4—Gd—Cs118.09 (5)O3—P1—Csx59.10 (9)
O10i—Gd—Cs51.77 (6)Csvi—P1—Csx136.53 (2)
O5ii—Gd—Cs122.79 (6)O5—P2—O10121.21 (15)
O7iii—Gd—Cs54.71 (7)O5—P2—O3110.56 (15)
O6iv—Gd—Cs121.25 (6)O10—P2—O3107.91 (13)
O2i—Gd—Cs62.83 (5)O5—P2—O11106.33 (12)
O8v—Gd—Cs55.56 (6)O10—P2—O11110.51 (13)
O9i—Gd—Csvi109.91 (6)O3—P2—O1197.80 (13)
O4—Gd—Csvi40.24 (6)O5—P2—Csvii51.39 (10)
O10i—Gd—Csvi102.88 (6)O10—P2—Csvii157.79 (9)
O5ii—Gd—Csvi40.87 (5)O3—P2—Csvii93.82 (9)
O7iii—Gd—Csvi53.14 (7)O11—P2—Csvii60.54 (8)
O6iv—Gd—Csvi113.24 (6)O5—P2—Csx152.39 (10)
O2i—Gd—Csvi170.37 (5)O10—P2—Csx54.57 (10)
O8v—Gd—Csvi103.94 (6)O3—P2—Csx56.10 (9)
Cs—Gd—Csvi107.850 (4)O11—P2—Csx99.80 (8)
O9i—Gd—Csvii55.10 (7)Csvii—P2—Csx143.27 (2)
O4—Gd—Csvii70.48 (5)O6—P3—O2117.10 (14)
O10i—Gd—Csvii135.15 (5)O6—P3—O11108.81 (14)
O5ii—Gd—Csvii79.02 (6)O2—P3—O11108.89 (13)
O7iii—Gd—Csvii143.41 (7)O6—P3—O1107.52 (12)
O6iv—Gd—Csvii37.88 (6)O2—P3—O1111.11 (13)
O2i—Gd—Csvii97.94 (5)O11—P3—O1102.39 (12)
O8v—Gd—Csvii110.20 (6)O6—P3—Csviii59.08 (9)
Cs—Gd—Csvii157.736 (7)O2—P3—Csviii58.04 (9)
Csvi—Gd—Csvii91.678 (5)O11—P3—Csviii127.03 (8)
O4iii—Cs—O2viii140.42 (6)O1—P3—Csviii130.57 (9)
O4iii—Cs—O5ix53.32 (6)O9—P4—O8117.73 (15)
O2viii—Cs—O5ix96.88 (6)O9—P4—O12xi110.27 (15)
O4iii—Cs—O6viii98.08 (6)O8—P4—O12xi110.76 (13)
O2viii—Cs—O6viii48.36 (6)O9—P4—O1107.87 (12)
O5ix—Cs—O6viii84.10 (7)O8—P4—O1110.37 (13)
O4iii—Cs—O10i71.13 (6)O12xi—P4—O198.02 (14)
O2viii—Cs—O10i148.23 (6)O9—P4—Csxi68.78 (11)
O5ix—Cs—O10i110.95 (6)O8—P4—Csxi51.52 (10)
O6viii—Cs—O10i146.29 (6)O12xi—P4—Csxi147.33 (10)
O4iii—Cs—O3i87.83 (6)O1—P4—Csxi113.58 (10)
O2viii—Cs—O3i121.78 (6)P4—O1—P3124.64 (13)
O5ix—Cs—O3i91.24 (6)P3—O2—Gdx128.98 (13)
O6viii—Cs—O3i168.04 (6)P3—O2—Csviii97.67 (11)
O10i—Cs—O3i45.60 (6)Gdx—O2—Csviii133.35 (8)
O4iii—Cs—O11ix98.82 (6)P3—O2—Csx117.04 (12)
O2viii—Cs—O11ix57.71 (6)Gdx—O2—Csx81.30 (5)
O5ix—Cs—O11ix45.50 (6)Csviii—O2—Csx76.36 (5)
O6viii—Cs—O11ix75.83 (6)P2—O3—P1129.22 (17)
O10i—Cs—O11ix136.34 (6)P2—O3—Csx99.57 (11)
O3i—Cs—O11ix93.04 (6)P1—O3—Csx95.63 (9)
O4iii—Cs—O7iii46.53 (6)P1—O4—Gd139.09 (15)
O2viii—Cs—O7iii141.67 (6)P1—O4—Csvi102.84 (11)
O5ix—Cs—O7iii99.49 (6)Gd—O4—Csvi110.23 (8)
O6viii—Cs—O7iii99.30 (6)P2—O5—Gdii142.75 (16)
O10i—Cs—O7iii49.74 (6)P2—O5—Csvii106.61 (12)
O3i—Cs—O7iii92.32 (6)Gdii—O5—Csvii108.63 (8)
O11ix—Cs—O7iii144.65 (5)P3—O6—Gdxii149.17 (14)
O4iii—Cs—O8v96.15 (6)P3—O6—Csviii96.85 (10)
O2viii—Cs—O8v95.79 (6)Gdxii—O6—Csviii113.81 (8)
O5ix—Cs—O8v141.91 (6)P1—O7—Gdvi148.91 (15)
O6viii—Cs—O8v77.96 (6)P1—O7—Csvi91.98 (12)
O10i—Cs—O8v71.86 (6)Gdvi—O7—Csvi89.35 (8)
O3i—Cs—O8v111.88 (5)P1—O7—Csx84.74 (12)
O11ix—Cs—O8v151.33 (6)Gdvi—O7—Csx94.45 (7)
O7iii—Cs—O8v51.83 (6)Csvi—O7—Csx176.20 (7)
O4iii—Cs—O12i88.42 (6)P4—O8—Gdxi128.81 (15)
O2viii—Cs—O12i97.18 (6)P4—O8—Csxi108.26 (11)
O5ix—Cs—O12i58.71 (6)Gdxi—O8—Csxi87.61 (7)
O6viii—Cs—O12i127.37 (6)P4—O9—Gdx146.63 (15)
O10i—Cs—O12i85.11 (6)P2—O10—Gdx139.94 (13)
O3i—Cs—O12i41.99 (5)P2—O10—Csx103.33 (12)
O11ix—Cs—O12i51.61 (5)Gdx—O10—Csx93.03 (7)
O7iii—Cs—O12i120.93 (6)P3—O11—P2131.48 (15)
O8v—Cs—O12i153.46 (5)P3—O11—Csvii132.32 (10)
O4iii—Cs—O7i50.73 (6)P2—O11—Csvii94.24 (10)
O2viii—Cs—O7i136.04 (6)P1—O12—P4v134.56 (18)
O5ix—Cs—O7i53.70 (6)P1—O12—Csx86.12 (10)
O6viii—Cs—O7i136.57 (5)P4v—O12—Csx139.26 (12)
O10i—Cs—O7i60.35 (6)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z; (iii) x+3/2, y+1/2, z+1/2; (iv) x+1/2, y+1/2, z+1/2; (v) x+1/2, y1/2, z+1/2; (vi) x+3/2, y1/2, z+1/2; (vii) x1/2, y+1/2, z1/2; (viii) x+1, y, z+1; (ix) x+1/2, y+1/2, z+1/2; (x) x, y1, z; (xi) x1/2, y1/2, z1/2; (xii) x+1/2, y1/2, z+1/2.
 

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