inorganic compounds
The crystal structure of trirubidium phosphate dodecatungstate, Rb3PO4W12O36, has been refined from X-ray powder diffraction data using the Rietveld method. The compound was obtained under hydrothermal conditions and is isotypic with K2.4(H3O)0.6PO4W12O36. The regular PO4 tetrahedron (3m symmetry) is surrounded by 12 WO6 octahedra, building the heteropolymetallate anion. By close packing of these heteropolyanionic units, orthogonally intersecting channels are formed where the Rb atoms are located. The alkali metal ion is surrounded by 12 O atoms to give a polyhedron with 2.m symmetry.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806030832/wm2037sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S1600536806030832/wm2037Isup2.rtv |
Computing details top
Data collection: X'pert Data Collector (PANalytical, 2003); cell refinement: GSAS (Larson & Von Dreele, 2000) and EXPGUI (Toby, 2001); data reduction: X'pert Data Collector; program(s) used to solve structure: coordinates taken from an isotypic compound; program(s) used to refine structure: GSAS and EXPGUI; molecular graphics: DIAMOND (Brandenburg, 2004); software used to prepare material for publication: enCIFer (Allen et al., 2004).
trirubidium phosphate dodecatungstate top
Crystal data top
Rb3PO4W12O36 | Dx = 6.563 Mg m−3 |
Mr = 3133.54 | CuKα1, CuKα2 radiation, λ = 1.540500, 1.544300 Å |
Cubic, Pn3m | T = 295 K |
Hall symbol: -P 4bc 2bc | Particle morphology: spherical |
a = 11.66078 (13) Å | white |
V = 1585.56 (5) Å3 | flat_sheet, 10 × 10 mm |
Z = 2 |
Data collection top
PANalytical X'pert PRO diffractometer | Data collection mode: reflection |
Radiation source: fine-focus sealed tube, PANalytical X'pert | Scan method: continuous |
Graphite monochromator | 2θmin = 5.415°, 2θmax = 90.381°, 2θstep = 0.017° |
Specimen mounting: packed powder sample container |
Refinement top
Least-squares matrix: full | Profile function: CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in Thompson et al. (1987). Asymmetry correction of Finger et al. (1994). #1(GU) = 8.973 #2(GV) = -5.801 #3(GW) = 1.775 #4(GP) = 0.000 #5(LX) = 4.463 #6(LY) = 354.622 #7(S/L) = 0.0370 #8(H/L) = 0.0187 #9(trns) = -6.11 #10(shft)= -46.4015 #11(stec)= 72.55 #12(ptec)= -2.26 #13(sfec)= 0.00 #14(L11) = -2.530 #15(L22) = -2.425 #16(L33) = -2.644 #17(L12) = -0.026 #18(L13) = -0.123 #19(L23) = -0.272 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0 |
Rp = 0.038 | 56 parameters |
Rwp = 0.050 | 4 restraints |
Rexp = 0.049 | 0 constraints |
R(F2) = 0.0344 | (Δ/σ)max = 0.03 |
4999 data points | Background function: GSAS Background function number 1 with 36 terms. Shifted Chebyshev function of 1st kind 1: 401.338 2: -392.220 3: 189.400 4: -71.8650 5: 22.7783 6: -11.2414 7: 9.37059 8: -3.30194 9: -28.6252 10: 30.4729 11: -13.2719 12: 3.64299 13: 8.58697 14: -9.19513 15: 5.13313 16: -5.69172 17: 7.36443 18: -6.43457 19: 3.53845 20: -2.72038 21: -1.20038 22: 2.11338 23: -0.273624 24: 1.28662 25: -0.943373 26: -1.13394 27: -8.730900E-0228: 2.37630 29: -3.257590E-0230: -3.29089 31: 2.07236 32: -1.00092 33: 0.866260 34: -0.594089 35: -2.60704 36: 0.669440 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
W | 0.46593 (7) | 0.46593 (7) | 0.25855 (14) | 0.0542 (10)* | |
P | 0.25 | 0.25 | 0.25 | 0.056 (8)* | |
O1 | 0.6518 (13) | 0.6518 (13) | 0.007 (2) | 0.097 (11)* | |
O2 | 0.0653 (9) | 0.0653 (9) | 0.764 (2) | 0.052 (6)* | |
O3 | 0.1277 (16) | 0.1277 (16) | 0.537 (2) | 0.079 (8)* | |
O4 | 0.3234 (10) | 0.3234 (10) | 0.3234 (10) | 0.014 (8)* | |
Rb | 0.25 | 0.75 | 0.75 | 0.069 (3)* |
Geometric parameters (Å, º) top
W—O1i | 1.913 (7) | O4—Wxi | 2.469 (12) |
W—O1ii | 1.913 (7) | O4—P | 1.48 (2) |
W—O2iii | 1.659 (16) | Rb—Wxvi | 4.1620 (2) |
W—O3iv | 1.907 (11) | Rb—Wxiii | 4.1620 (2) |
W—O3v | 1.907 (11) | Rb—Wxvii | 4.1620 (2) |
W—O4 | 2.469 (12) | Rb—Wxviii | 4.1620 (2) |
W—Rbvi | 4.1620 (2) | Rb—Wxix | 4.1620 (2) |
W—Rbvii | 4.1620 (2) | Rb—Wxx | 4.1620 (2) |
P—O4 | 1.48 (2) | Rb—Wxxi | 4.1620 (2) |
P—O4viii | 1.48 (2) | Rb—Wxxii | 4.1620 (2) |
P—O4ix | 1.48 (2) | Rb—O1xv | 3.27 (3) |
P—O4x | 1.48 (2) | Rb—O1xxiii | 3.27 (3) |
O1—Wi | 1.913 (7) | Rb—O1xxiv | 3.27 (3) |
O1—Wii | 1.913 (7) | Rb—O1xxv | 3.27 (3) |
O1—Rbxi | 3.27 (3) | Rb—O2xxvi | 3.050 (15) |
O2—Wxii | 1.659 (16) | Rb—O2xxvii | 3.050 (15) |
O2—Rbxiii | 3.050 (15) | Rb—O2xxviii | 3.050 (15) |
O3—Wix | 1.907 (11) | Rb—O2xxix | 3.050 (15) |
O3—Wxiv | 1.907 (11) | Rb—O3xxvi | 3.20 (2) |
O3—Rbxiii | 3.20 (2) | Rb—O3xxvii | 3.20 (2) |
O4—W | 2.469 (12) | Rb—O3xxviii | 3.20 (2) |
O4—Wxv | 2.469 (12) | Rb—O3xxix | 3.20 (2) |
O1i—W—O1xxx | 86.2 (14) | O1xxiv—Rb—O2xxvi | 92.6 (5) |
O1i—W—O2iii | 103.1 (9) | O1xxiv—Rb—O2xxvii | 92.6 (5) |
O1xxxi—W—O3xxxii | 86.2 (7) | O1xxiv—Rb—O2xxviii | 57.3 (6) |
O1xxxi—W—O3xxxiii | 155.0 (8) | O1xxiv—Rb—O2xxxvi | 116.8 (7) |
O1xxx—W—O2iii | 103.1 (9) | O1xxiv—Rb—O3xxvi | 47.6 (3) |
O1xxxiv—W—O3xxxii | 155.0 (8) | O1xxiv—Rb—O3xxvii | 47.6 (3) |
O1xxxiv—W—O3xxxiii | 86.2 (7) | O1xxiv—Rb—O3xxxvii | 111.2 (5) |
O2iii—W—O3xxxii | 101.8 (9) | O1xxiv—Rb—O3xxix | 170.6 (8) |
O2iii—W—O3xxxiii | 101.8 (9) | O1xxxv—Rb—O2xxvi | 116.8 (7) |
O3xxxii—W—O3xxxiii | 90.8 (13) | O1xxxv—Rb—O2xxvii | 57.3 (6) |
O4—P—O4viii | 109.4712 (4) | O1xxxv—Rb—O2xxviii | 92.6 (5) |
O4—P—O4ix | 109.4712 (9) | O1xxxv—Rb—O2xxxvi | 92.6 (5) |
O4—P—O4x | 109.4712 (5) | O1xxxviii—Rb—O3xxvi | 170.6 (8) |
O4viii—P—O4ix | 109.4712 (4) | O1xxxviii—Rb—O3xxvii | 111.2 (5) |
O4viii—P—O4x | 109.4712 (9) | O1xxxviii—Rb—O3xxxvii | 47.6 (3) |
O4ix—P—O4x | 109.4712 (4) | O1xxxviii—Rb—O3xxix | 47.6 (3) |
Wxxxi—O1—Wxxxiv | 150.7 (15) | O2xxvi—Rb—O2xxvii | 174.0 (10) |
Wi—O1—Rbxi | 103.8 (7) | O2xxvi—Rb—O2xxviii | 90.15 (5) |
Wxxx—O1—Rbxi | 103.8 (7) | O2xxvi—Rb—O2xxxvi | 90.15 (5) |
Wxii—O2—Rbxiii | 168.1 (14) | O2xxvi—Rb—O3xxvi | 53.9 (7) |
Wix—O3—Wxiv | 127.4 (14) | O2xxvi—Rb—O3xxvii | 132.1 (8) |
Wix—O3—Rbxiii | 106.4 (7) | O2xxvi—Rb—O3xxxvii | 87.7 (4) |
Wxiv—O3—Rbxiii | 106.4 (7) | O2xxvi—Rb—O3xxix | 87.7 (4) |
O1xv—Rb—O1xxiii | 138.9 (6) | O2xxvii—Rb—O2xxviii | 90.15 (5) |
O1xv—Rb—O1xxiv | 138.9 (6) | O2xxvii—Rb—O2xxxvi | 90.15 (5) |
O1xv—Rb—O1xxxv | 59.5 (9) | O2xxvii—Rb—O3xxvi | 132.1 (8) |
O1xv—Rb—O2xxvi | 57.3 (6) | O2xxvii—Rb—O3xxvii | 53.9 (7) |
O1xv—Rb—O2xxvii | 116.8 (7) | O2xxvii—Rb—O3xxxvii | 87.7 (4) |
O1xv—Rb—O2xxviii | 92.6 (5) | O2xxvii—Rb—O3xxix | 87.7 (4) |
O1xv—Rb—O2xxxvi | 92.6 (5) | O2xxviii—Rb—O2xxxvi | 174.0 (10) |
O1xv—Rb—O3xxvi | 111.2 (5) | O2xxxvii—Rb—O3xxvi | 87.7 (4) |
O1xv—Rb—O3xxvii | 170.6 (8) | O2xxxvii—Rb—O3xxvii | 87.7 (4) |
O1xv—Rb—O3xxxvii | 47.6 (3) | O2xxxvii—Rb—O3xxxvii | 53.9 (7) |
O1xv—Rb—O3xxix | 47.6 (3) | O2xxxvii—Rb—O3xxix | 132.1 (8) |
O1xxiii—Rb—O1xxiv | 59.5 (9) | O2xxix—Rb—O3xxvi | 87.7 (4) |
O1xxiii—Rb—O1xxxv | 138.9 (6) | O2xxix—Rb—O3xxvii | 87.7 (4) |
O1xxiii—Rb—O2xxvi | 92.6 (5) | O2xxix—Rb—O3xxxvii | 132.1 (8) |
O1xxiii—Rb—O2xxvii | 92.6 (5) | O2xxix—Rb—O3xxix | 53.9 (7) |
O1xxiii—Rb—O2xxviii | 116.8 (7) | O3xxvi—Rb—O3xxvii | 78.2 (10) |
O1xxiii—Rb—O2xxxvi | 57.3 (6) | O3xxvi—Rb—O3xxxvii | 127.1 (6) |
O1xxiii—Rb—O3xxvi | 47.6 (3) | O3xxvi—Rb—O3xxix | 127.1 (6) |
O1xxiii—Rb—O3xxvii | 47.6 (3) | O3xxvii—Rb—O3xxxvii | 127.1 (6) |
O1xxiii—Rb—O3xxxvii | 170.6 (8) | O3xxvii—Rb—O3xxix | 127.1 (6) |
O1xxiii—Rb—O3xxix | 111.2 (5) | O3xxxvii—Rb—O3xxix | 78.2 (10) |
O1xxiv—Rb—O1xxxv | 138.9 (6) |
Symmetry codes: (i) z+1/2, −x+1, y−1/2; (ii) −y+1, z+1/2, x−1/2; (iii) x+1/2, y+1/2, −z+1; (iv) z, −x+1/2, −y+1/2; (v) −y+1/2, z, −x+1/2; (vi) x+1/2, y−1/2, −z+1; (vii) −z+1, x+1/2, y−1/2; (viii) −z+1/2, x, −y+1/2; (ix) −y+1/2, −z+1/2, x; (x) y, −z+1/2, −x+1/2; (xi) y, z, x; (xii) x−1/2, y−1/2, −z+1; (xiii) y−1/2, −z+1, x+1/2; (xiv) −z+1/2, −x+1/2, y; (xv) z, x, y; (xvi) x−1/2, y+1/2, −z+1; (xvii) −x+1, −y+1, −z+1; (xviii) −y+1, −z+1, −x+1; (xix) y−1/2, z+1/2, −x+1; (xx) −y+1, z+1/2, x+1/2; (xxi) x−1/2, −y+1, z+1/2; (xxii) −x+1, y+1/2, z+1/2; (xxiii) −z+1/2, x, −y+3/2; (xxiv) −z+1/2, −x+3/2, y; (xxv) z, −x+3/2, −y+3/2; (xxvi) −z+1, x+1/2, y+1/2; (xxvii) −z+1, −x+1, −y+1; (xxviii) z−1/2, −x+1, y+1/2; (xxix) z−1/2, x+1/2, −y+1; (xxx) −y, z+3/2, x−1/2; (xxxi) z+1/2, −x, y+1/2; (xxxii) z−1, −x+1/2, −y+3/2; (xxxiii) −y+1/2, z−1, −x+3/2; (xxxiv) −y, z+1/2, x+1/2; (xxxv) z−1, −x+5/2, −y+3/2; (xxxvi) z−1/2, x+3/2, −y; (xxxvii) z−1/2, −x, y+3/2; (xxxviii) z−1, −x+3/2, −y+5/2. |