Rb₃PO₄W₁₂O₃₆ from X-ray powder data

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 K_2.4(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.

Key indicators

• Powder X-ray study
• T = 295 K
• Mean [sigma](P-O) = 0.012 Å
• R factor = 0.000
• wR factor = 0.000
• Data-to-parameter ratio = 5.1

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  O3     ..  O4      ..       2.62 Ang.
PLAT731_ALERT_1_B Bond    Calc   4.1620(8), Rep 4.16201(17) ......       4.71 su-Ra
              W    -RB      1.555   4.546
PLAT731_ALERT_1_B Bond    Calc   4.1620(8), Rep 4.16201(17) ......       4.71 su-Ra
              W    -RB      1.555   5.654
PLAT731_ALERT_1_B Bond    Calc   4.1620(8), Rep 4.16201(17) ......       4.71 su-Ra
              RB   -W       1.555   4.456
PLAT731_ALERT_1_B Bond    Calc   4.1620(8), Rep 4.16201(17) ......       4.71 su-Ra
              RB   -W       1.555   6.465

Alert level C
REFI023_ALERT_1_C  _refine_diff_density_max is missing
            Maximum value of final difference map (e A-3).
            The following tests will not be performed
            DIFMN_01,DIFMX_01,DIFMX_02
REFI024_ALERT_1_C  _refine_diff_density_min is missing
            Minimum value of final difference map (e A-3).
            The following tests will not be performed
            DIFMN_01,DIFMN_02,DIFMN_03
RADNW01_ALERT_1_C  The radiation wavelength lies outside the expected range
            for the supplied radiation type. Expected range 1.54175-1.54180
            Wavelength given =    1.54430
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT127_ALERT_1_C Implicit Hall Symbol  Inconsistent with Explicit    -P 4bc 2bc
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT799_ALERT_4_C Numeric Label on Displacement Par. Record ......          ?

Alert level G
RADNT01_ALERT_1_G  Extra text has been found in the _diffrn_radiation_type field.
            Radiation given as CuK\a~1~ CuK\a~2~
            Radiation identified as Cu K\a

   0 ALERT level A = In general: serious problem
   5 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

  11 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

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

Crystal data

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) Å^3	flat_sheet, 10 × 10 mm
Z = 2

Data collection

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

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(F^2) = 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 (Ų)

	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)*

Atomic displacement parameters (Ų)

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

Geometric parameters (Å, º)

W—O1^i	1.913 (7)	O4—W^xi	2.469 (12)
W—O1^ii	1.913 (7)	O4—P	1.48 (2)
W—O2^iii	1.659 (16)	Rb—W^xvi	4.1620 (2)
W—O3^iv	1.907 (11)	Rb—W^xiii	4.1620 (2)
W—O3^v	1.907 (11)	Rb—W^xvii	4.1620 (2)
W—O4	2.469 (12)	Rb—W^xviii	4.1620 (2)
W—Rb^vi	4.1620 (2)	Rb—W^xix	4.1620 (2)
W—Rb^vii	4.1620 (2)	Rb—W^xx	4.1620 (2)
P—O4	1.48 (2)	Rb—W^xxi	4.1620 (2)
P—O4^viii	1.48 (2)	Rb—W^xxii	4.1620 (2)
P—O4^ix	1.48 (2)	Rb—O1^xv	3.27 (3)
P—O4^x	1.48 (2)	Rb—O1^xxiii	3.27 (3)
O1—W^i	1.913 (7)	Rb—O1^xxiv	3.27 (3)
O1—W^ii	1.913 (7)	Rb—O1^xxv	3.27 (3)
O1—Rb^xi	3.27 (3)	Rb—O2^xxvi	3.050 (15)
O2—W^xii	1.659 (16)	Rb—O2^xxvii	3.050 (15)
O2—Rb^xiii	3.050 (15)	Rb—O2^xxviii	3.050 (15)
O3—W^ix	1.907 (11)	Rb—O2^xxix	3.050 (15)
O3—W^xiv	1.907 (11)	Rb—O3^xxvi	3.20 (2)
O3—Rb^xiii	3.20 (2)	Rb—O3^xxvii	3.20 (2)
O4—W	2.469 (12)	Rb—O3^xxviii	3.20 (2)
O4—W^xv	2.469 (12)	Rb—O3^xxix	3.20 (2)
O1^i—W—O1^xxx	86.2 (14)	O1^xxiv—Rb—O2^xxvi	92.6 (5)
O1^i—W—O2^iii	103.1 (9)	O1^xxiv—Rb—O2^xxvii	92.6 (5)
O1^xxxi—W—O3^xxxii	86.2 (7)	O1^xxiv—Rb—O2^xxviii	57.3 (6)
O1^xxxi—W—O3^xxxiii	155.0 (8)	O1^xxiv—Rb—O2^xxxvi	116.8 (7)
O1^xxx—W—O2^iii	103.1 (9)	O1^xxiv—Rb—O3^xxvi	47.6 (3)
O1^xxxiv—W—O3^xxxii	155.0 (8)	O1^xxiv—Rb—O3^xxvii	47.6 (3)
O1^xxxiv—W—O3^xxxiii	86.2 (7)	O1^xxiv—Rb—O3^xxxvii	111.2 (5)
O2^iii—W—O3^xxxii	101.8 (9)	O1^xxiv—Rb—O3^xxix	170.6 (8)
O2^iii—W—O3^xxxiii	101.8 (9)	O1^xxxv—Rb—O2^xxvi	116.8 (7)
O3^xxxii—W—O3^xxxiii	90.8 (13)	O1^xxxv—Rb—O2^xxvii	57.3 (6)
O4—P—O4^viii	109.4712 (4)	O1^xxxv—Rb—O2^xxviii	92.6 (5)
O4—P—O4^ix	109.4712 (9)	O1^xxxv—Rb—O2^xxxvi	92.6 (5)
O4—P—O4^x	109.4712 (5)	O1^xxxviii—Rb—O3^xxvi	170.6 (8)
O4^viii—P—O4^ix	109.4712 (4)	O1^xxxviii—Rb—O3^xxvii	111.2 (5)
O4^viii—P—O4^x	109.4712 (9)	O1^xxxviii—Rb—O3^xxxvii	47.6 (3)
O4^ix—P—O4^x	109.4712 (4)	O1^xxxviii—Rb—O3^xxix	47.6 (3)
W^xxxi—O1—W^xxxiv	150.7 (15)	O2^xxvi—Rb—O2^xxvii	174.0 (10)
W^i—O1—Rb^xi	103.8 (7)	O2^xxvi—Rb—O2^xxviii	90.15 (5)
W^xxx—O1—Rb^xi	103.8 (7)	O2^xxvi—Rb—O2^xxxvi	90.15 (5)
W^xii—O2—Rb^xiii	168.1 (14)	O2^xxvi—Rb—O3^xxvi	53.9 (7)
W^ix—O3—W^xiv	127.4 (14)	O2^xxvi—Rb—O3^xxvii	132.1 (8)
W^ix—O3—Rb^xiii	106.4 (7)	O2^xxvi—Rb—O3^xxxvii	87.7 (4)
W^xiv—O3—Rb^xiii	106.4 (7)	O2^xxvi—Rb—O3^xxix	87.7 (4)
O1^xv—Rb—O1^xxiii	138.9 (6)	O2^xxvii—Rb—O2^xxviii	90.15 (5)
O1^xv—Rb—O1^xxiv	138.9 (6)	O2^xxvii—Rb—O2^xxxvi	90.15 (5)
O1^xv—Rb—O1^xxxv	59.5 (9)	O2^xxvii—Rb—O3^xxvi	132.1 (8)
O1^xv—Rb—O2^xxvi	57.3 (6)	O2^xxvii—Rb—O3^xxvii	53.9 (7)
O1^xv—Rb—O2^xxvii	116.8 (7)	O2^xxvii—Rb—O3^xxxvii	87.7 (4)
O1^xv—Rb—O2^xxviii	92.6 (5)	O2^xxvii—Rb—O3^xxix	87.7 (4)
O1^xv—Rb—O2^xxxvi	92.6 (5)	O2^xxviii—Rb—O2^xxxvi	174.0 (10)
O1^xv—Rb—O3^xxvi	111.2 (5)	O2^xxxvii—Rb—O3^xxvi	87.7 (4)
O1^xv—Rb—O3^xxvii	170.6 (8)	O2^xxxvii—Rb—O3^xxvii	87.7 (4)
O1^xv—Rb—O3^xxxvii	47.6 (3)	O2^xxxvii—Rb—O3^xxxvii	53.9 (7)
O1^xv—Rb—O3^xxix	47.6 (3)	O2^xxxvii—Rb—O3^xxix	132.1 (8)
O1^xxiii—Rb—O1^xxiv	59.5 (9)	O2^xxix—Rb—O3^xxvi	87.7 (4)
O1^xxiii—Rb—O1^xxxv	138.9 (6)	O2^xxix—Rb—O3^xxvii	87.7 (4)
O1^xxiii—Rb—O2^xxvi	92.6 (5)	O2^xxix—Rb—O3^xxxvii	132.1 (8)
O1^xxiii—Rb—O2^xxvii	92.6 (5)	O2^xxix—Rb—O3^xxix	53.9 (7)
O1^xxiii—Rb—O2^xxviii	116.8 (7)	O3^xxvi—Rb—O3^xxvii	78.2 (10)
O1^xxiii—Rb—O2^xxxvi	57.3 (6)	O3^xxvi—Rb—O3^xxxvii	127.1 (6)
O1^xxiii—Rb—O3^xxvi	47.6 (3)	O3^xxvi—Rb—O3^xxix	127.1 (6)
O1^xxiii—Rb—O3^xxvii	47.6 (3)	O3^xxvii—Rb—O3^xxxvii	127.1 (6)
O1^xxiii—Rb—O3^xxxvii	170.6 (8)	O3^xxvii—Rb—O3^xxix	127.1 (6)
O1^xxiii—Rb—O3^xxix	111.2 (5)	O3^xxxvii—Rb—O3^xxix	78.2 (10)
O1^xxiv—Rb—O1^xxxv	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.