Rubidium terbium polyphosphate

The title compound, RbTb(PO₃)₄, belongs to type IV of the M^IM^III(PO₃)₄ polyphosphate family. It was synthesized by the flux-growth method. In this condensed polyphosphate, PO₄ tetra­hedra share vertices to produce corrugated ribbons along the a-axis direction with a repeating unit of eight tetra­hedra. Isolated TbO₈ polyhedra link the phosphate anions into a three-dimensional framework with channels containing Rb⁺ cations.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](P-O) = 0.005 Å
• R factor = 0.025
• wR factor = 0.097
• Data-to-parameter ratio = 14.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.80
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.27

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.271
            Tmax scaled      0.109 Tmin scaled      0.088

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   2 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
   2 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: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

rubidium terbium tetraphosphate

Crystal data

RbTb(PO3)4	F(000) = 1032
Mr = 560.27	Dx = 3.846 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 25 reflections
a = 10.3224 (2) Å	θ = 10.2–15.1°
b = 8.9071 (3) Å	µ = 13.03 mm^−1
c = 10.9608 (3) Å	T = 298 K
β = 106.211 (2)°	Prism, colourless
V = 967.70 (5) Å^3	0.18 × 0.17 × 0.17 mm
Z = 4

Data collection

Enraf-Nonius CAD-4 diffractometer	2138 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.040
Graphite monochromator	θmax = 27.8°, θmin = 2.4°
ω/2θ scans	h = −13→13
Absorption correction: ψ scan (North et al., 1968)	k = −11→10
Tmin = 0.325, Tmax = 0.403	l = −11→14
6667 measured reflections	2 standard reflections every 120 min
2289 independent reflections	intensity decay: 2%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.025	w = 1/[σ^2(Fo^2) + (0.0501P)^2 + 5.0496P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.097	(Δ/σ)max = 0.001
S = 1.27	Δρmax = 1.51 e Å^−3
2289 reflections	Δρmin = −2.12 e Å^−3
164 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0243 (9)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Tb	1.00094 (3)	0.22745 (3)	0.81726 (3)	0.00404 (15)
Rb	1.30823 (7)	0.56693 (9)	1.04241 (7)	0.0211 (2)
P1	1.24701 (14)	0.47452 (17)	0.72263 (15)	0.0041 (3)
P2	1.54047 (14)	−0.32752 (17)	1.36366 (14)	0.0045 (3)
P3	1.35412 (14)	−0.09338 (17)	1.24093 (15)	0.0045 (3)
P4	1.32560 (14)	0.10792 (18)	1.02293 (14)	0.0046 (3)
O1	1.1700 (4)	0.4066 (5)	0.8040 (4)	0.0082 (9)
O2	1.3539 (4)	0.5852 (5)	0.7847 (4)	0.0074 (8)
O3	1.3125 (4)	0.3428 (5)	0.6586 (4)	0.0067 (8)
O4	1.1390 (4)	0.5471 (5)	0.6017 (4)	0.0072 (9)
O5	1.4625 (4)	−0.4686 (5)	1.3302 (5)	0.0105 (9)
O6	1.5626 (5)	−0.2562 (5)	1.4900 (5)	0.0097 (9)
O7	1.4766 (5)	−0.2075 (5)	1.2535 (4)	0.0081 (9)
O8	1.3992 (4)	0.0383 (5)	1.3240 (4)	0.0098 (9)
O9	1.2640 (4)	0.3210 (6)	1.2454 (4)	0.0104 (9)
O10	1.3318 (5)	−0.0485 (5)	1.0966 (4)	0.0116 (9)
O11	1.1853 (4)	0.1644 (6)	0.9839 (4)	0.0105 (9)
O12	1.4340 (5)	0.2108 (5)	1.0940 (5)	0.0096 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Tb	0.0029 (2)	0.0037 (2)	0.0049 (2)	0.00052 (9)	0.00011 (13)	0.00070 (9)
Rb	0.0207 (4)	0.0300 (4)	0.0117 (4)	0.0039 (3)	0.0030 (3)	−0.0021 (3)
P1	0.0032 (6)	0.0049 (8)	0.0043 (7)	0.0006 (5)	0.0011 (5)	0.0007 (5)
P2	0.0036 (6)	0.0034 (7)	0.0056 (7)	0.0004 (5)	−0.0001 (5)	−0.0005 (6)
P3	0.0027 (6)	0.0044 (7)	0.0053 (7)	0.0000 (5)	−0.0006 (5)	0.0012 (6)
P4	0.0041 (6)	0.0051 (7)	0.0036 (7)	0.0001 (5)	−0.0006 (5)	0.0003 (6)
O1	0.0091 (19)	0.008 (2)	0.008 (2)	−0.0034 (17)	0.0039 (17)	0.0010 (17)
O2	0.0073 (19)	0.008 (2)	0.007 (2)	−0.0036 (16)	0.0022 (17)	−0.0042 (16)
O3	0.0039 (18)	0.005 (2)	0.010 (2)	−0.0010 (15)	0.0012 (16)	−0.0027 (17)
O4	0.0035 (18)	0.012 (2)	0.007 (2)	0.0005 (16)	0.0020 (16)	0.0005 (17)
O5	0.006 (2)	0.006 (2)	0.019 (2)	−0.0014 (17)	0.0029 (18)	−0.0013 (19)
O6	0.009 (2)	0.013 (2)	0.008 (2)	−0.0003 (17)	0.0031 (18)	−0.0009 (17)
O7	0.009 (2)	0.005 (2)	0.010 (2)	0.0032 (17)	0.0027 (18)	0.0032 (17)
O8	0.012 (2)	0.006 (2)	0.012 (2)	−0.0012 (17)	0.0037 (18)	−0.0015 (18)
O9	0.0037 (19)	0.014 (2)	0.013 (2)	0.0021 (18)	0.0002 (17)	−0.0051 (19)
O10	0.018 (2)	0.007 (2)	0.008 (2)	−0.0012 (18)	0.0003 (18)	0.0022 (18)
O11	0.0060 (19)	0.016 (2)	0.008 (2)	0.0041 (18)	−0.0002 (17)	0.0007 (18)
O12	0.008 (2)	0.012 (2)	0.008 (2)	−0.0054 (17)	0.0017 (18)	−0.0014 (18)

Geometric parameters (Å, º)

Tb—O11	2.309 (4)	P2—O7	1.609 (5)
Tb—O8^i	2.347 (4)	P2—Rb^ix	3.7205 (17)
Tb—O5^ii	2.350 (5)	P2—Rb^x	3.7837 (17)
Tb—O6^iii	2.386 (5)	P3—O8	1.478 (5)
Tb—O9^i	2.390 (4)	P3—O9^xi	1.481 (4)
Tb—O1	2.399 (4)	P3—O10	1.585 (5)
Tb—O12^i	2.413 (5)	P3—O7	1.598 (5)
Tb—O2^iv	2.457 (4)	P3—Rb^xi	3.5650 (17)
Tb—Rb^i	4.0697 (8)	P3—Rb^x	3.6794 (18)
Tb—Rb^v	4.3180 (7)	P4—O11	1.479 (4)
Tb—Rb	4.5743 (8)	P4—O12	1.487 (5)
Rb—O8^iii	2.923 (4)	P4—O10	1.602 (5)
Rb—O6^i	2.964 (5)	P4—O4^iv	1.603 (4)
Rb—O1	2.970 (5)	O2—Tb^vii	2.457 (4)
Rb—O2	2.995 (4)	O3—P2^viii	1.609 (4)
Rb—O5^vi	3.127 (5)	O3—Rb^iv	3.303 (4)
Rb—O7^vi	3.188 (5)	O4—P4^vii	1.603 (4)
Rb—O9	3.244 (5)	O5—Tb^xii	2.350 (5)
Rb—O3^vii	3.303 (4)	O5—Rb^x	3.127 (5)
Rb—O12	3.415 (5)	O6—Tb^xi	2.386 (5)
Rb—O9^iii	3.472 (5)	O6—Rb^ix	2.964 (5)
Rb—O10^vi	3.474 (5)	O7—Rb^x	3.188 (5)
Rb—P1	3.4822 (17)	O8—Tb^ix	2.347 (4)
P1—O1	1.480 (4)	O8—Rb^xi	2.923 (4)
P1—O2	1.494 (4)	O9—P3^iii	1.481 (4)
P1—O3	1.609 (4)	O9—Tb^ix	2.390 (4)
P1—O4	1.610 (5)	O9—Rb^xi	3.472 (5)
P2—O6	1.482 (5)	O10—Rb^x	3.474 (5)
P2—O5	1.482 (5)	O12—Tb^ix	2.413 (5)
P2—O3^viii	1.609 (4)
O11—Tb—O8^i	117.96 (17)	O6^i—Rb—O10^vi	59.17 (12)
O11—Tb—O5^ii	80.18 (17)	O1—Rb—O10^vi	128.18 (12)
O8^i—Tb—O5^ii	141.79 (15)	O2—Rb—O10^vi	94.93 (12)
O11—Tb—O6^iii	71.60 (16)	O5^vi—Rb—O10^vi	86.32 (12)
O8^i—Tb—O6^iii	71.42 (16)	O7^vi—Rb—O10^vi	41.98 (11)
O5^ii—Tb—O6^iii	85.05 (16)	O9—Rb—O10^vi	124.42 (11)
O11—Tb—O9^i	139.33 (16)	O3^vii—Rb—O10^vi	51.38 (11)
O8^i—Tb—O9^i	75.23 (16)	O12—Rb—O10^vi	151.97 (11)
O5^ii—Tb—O9^i	70.63 (16)	O9^iii—Rb—O10^vi	42.32 (11)
O6^iii—Tb—O9^i	78.09 (16)	O8^iii—Rb—P1	122.08 (10)
O11—Tb—O1	75.92 (16)	O6^i—Rb—P1	91.96 (10)
O8^i—Tb—O1	75.52 (15)	O1—Rb—P1	24.94 (8)
O5^ii—Tb—O1	142.58 (15)	O2—Rb—P1	25.26 (8)
O6^iii—Tb—O1	113.43 (16)	O5^vi—Rb—P1	152.81 (9)
O9^i—Tb—O1	142.64 (16)	O7^vi—Rb—P1	142.03 (9)
O11—Tb—O12^i	142.82 (15)	O9—Rb—P1	120.66 (9)
O8^i—Tb—O12^i	79.93 (16)	O3^vii—Rb—P1	64.90 (8)
O5^ii—Tb—O12^i	106.23 (16)	O12—Rb—P1	84.31 (9)
O6^iii—Tb—O12^i	144.33 (16)	O9^iii—Rb—P1	144.66 (8)
O9^i—Tb—O12^i	74.34 (15)	O10^vi—Rb—P1	112.93 (8)
O1—Tb—O12^i	78.12 (16)	O1—P1—O2	116.6 (3)
O11—Tb—O2^iv	76.19 (15)	O1—P1—O3	109.1 (3)
O8^i—Tb—O2^iv	143.93 (15)	O2—P1—O3	109.5 (2)
O5^ii—Tb—O2^iv	69.89 (15)	O1—P1—O4	107.2 (2)
O6^iii—Tb—O2^iv	142.00 (15)	O2—P1—O4	111.3 (3)
O9^i—Tb—O2^iv	117.06 (16)	O3—P1—O4	102.2 (2)
O1—Tb—O2^iv	76.66 (15)	O1—P1—Rb	57.79 (19)
O12^i—Tb—O2^iv	72.23 (15)	O2—P1—Rb	58.80 (17)
O11—Tb—Rb^i	123.59 (12)	O3—P1—Rb	129.11 (18)
O8^i—Tb—Rb^i	117.76 (11)	O4—P1—Rb	128.55 (17)
O5^ii—Tb—Rb^i	49.96 (12)	O6—P2—O5	121.8 (3)
O6^iii—Tb—Rb^i	119.77 (12)	O6—P2—O3^viii	105.8 (3)
O9^i—Tb—Rb^i	52.85 (12)	O5—P2—O3^viii	111.2 (2)
O1—Tb—Rb^i	126.68 (11)	O6—P2—O7	109.9 (3)
O12^i—Tb—Rb^i	56.90 (12)	O5—P2—O7	107.3 (3)
O2^iv—Tb—Rb^i	64.22 (11)	O3^viii—P2—O7	98.5 (2)
O11—Tb—Rb^v	110.46 (11)	O6—P2—Rb^ix	48.86 (19)
O8^i—Tb—Rb^v	39.63 (11)	O5—P2—Rb^ix	158.7 (2)
O5^ii—Tb—Rb^v	103.92 (11)	O3^viii—P2—Rb^ix	62.55 (16)
O6^iii—Tb—Rb^v	40.98 (12)	O7—P2—Rb^ix	93.98 (18)
O9^i—Tb—Rb^v	53.41 (12)	O6—P2—Rb^x	150.3 (2)
O1—Tb—Rb^v	111.21 (11)	O5—P2—Rb^x	53.11 (19)
O12^i—Tb—Rb^v	103.51 (11)	O3^viii—P2—Rb^x	102.55 (17)
O2^iv—Tb—Rb^v	170.45 (11)	O7—P2—Rb^x	56.38 (18)
Rb^i—Tb—Rb^v	106.250 (11)	Rb^ix—P2—Rb^x	146.06 (5)
O11—Tb—Rb	55.93 (12)	O8—P3—O9^xi	118.2 (3)
O8^i—Tb—Rb	69.16 (11)	O8—P3—O10	110.4 (3)
O5^ii—Tb—Rb	135.99 (11)	O9^xi—P3—O10	109.7 (3)
O6^iii—Tb—Rb	78.61 (12)	O8—P3—O7	110.3 (3)
O9^i—Tb—Rb	142.07 (12)	O9^xi—P3—O7	108.5 (3)
O1—Tb—Rb	35.54 (11)	O10—P3—O7	97.9 (3)
O12^i—Tb—Rb	110.82 (12)	O8—P3—Rb^xi	52.94 (18)
O2^iv—Tb—Rb	99.63 (11)	O9^xi—P3—Rb^xi	65.5 (2)
Rb^i—Tb—Rb	161.315 (19)	O10—P3—Rb^xi	126.82 (19)
Rb^v—Tb—Rb	89.863 (14)	O7—P3—Rb^xi	134.85 (18)
O8^iii—Rb—O6^i	55.97 (13)	O8—P3—Rb^x	169.51 (19)
O8^iii—Rb—O1	99.17 (12)	O9^xi—P3—Rb^x	70.3 (2)
O6^i—Rb—O1	85.86 (13)	O10—P3—Rb^x	70.03 (18)
O8^iii—Rb—O2	143.83 (13)	O7—P3—Rb^x	59.73 (18)
O6^i—Rb—O2	97.90 (13)	Rb^xi—P3—Rb^x	135.76 (5)
O1—Rb—O2	50.19 (12)	O11—P4—O12	118.4 (3)
O8^iii—Rb—O5^vi	73.97 (12)	O11—P4—O10	109.9 (3)
O6^i—Rb—O5^vi	114.85 (13)	O12—P4—O10	110.7 (3)
O1—Rb—O5^vi	145.38 (13)	O11—P4—O4^iv	107.8 (2)
O2—Rb—O5^vi	141.89 (12)	O12—P4—O4^iv	109.7 (3)
O8^iii—Rb—O7^vi	91.07 (12)	O10—P4—O4^iv	98.6 (3)
O6^i—Rb—O7^vi	92.63 (13)	P1—O1—Tb	146.2 (3)
O1—Rb—O7^vi	166.44 (12)	P1—O1—Rb	97.3 (2)
O2—Rb—O7^vi	116.93 (12)	Tb—O1—Rb	116.46 (16)
O5^vi—Rb—O7^vi	46.44 (12)	P1—O2—Tb^vii	126.8 (2)
O8^iii—Rb—O9	48.28 (12)	P1—O2—Rb	95.9 (2)
O6^i—Rb—O9	103.92 (12)	Tb^vii—O2—Rb	137.18 (17)
O1—Rb—O9	98.84 (12)	P2^viii—O3—P1	131.0 (3)
O2—Rb—O9	140.60 (12)	P2^viii—O3—Rb^iv	91.84 (18)
O5^vi—Rb—O9	50.91 (11)	P1—O3—Rb^iv	135.0 (2)
O7^vi—Rb—O9	94.61 (12)	P4^vii—O4—P1	124.5 (3)
O8^iii—Rb—O3^vii	101.92 (12)	P2—O5—Tb^xii	139.2 (3)
O6^i—Rb—O3^vii	45.95 (11)	P2—O5—Rb^x	104.6 (2)
O1—Rb—O3^vii	76.80 (12)	Tb^xii—O5—Rb^x	94.91 (15)
O2—Rb—O3^vii	57.31 (11)	P2—O6—Tb^xi	142.4 (3)
O5^vi—Rb—O3^vii	137.65 (12)	P2—O6—Rb^ix	109.0 (2)
O7^vi—Rb—O3^vii	92.47 (11)	Tb^xi—O6—Rb^ix	107.15 (17)
O9—Rb—O3^vii	149.39 (10)	P3—O7—P2	129.5 (3)
O8^iii—Rb—O12	97.68 (12)	P3—O7—Rb^x	94.6 (2)
O6^i—Rb—O12	145.64 (12)	P2—O7—Rb^x	98.8 (2)
O1—Rb—O12	76.47 (12)	P3—O8—Tb^ix	138.8 (3)
O2—Rb—O12	93.09 (12)	P3—O8—Rb^xi	103.3 (2)
O5^vi—Rb—O12	71.09 (12)	Tb^ix—O8—Rb^xi	109.57 (16)
O7^vi—Rb—O12	111.11 (12)	P3^iii—O9—Tb^ix	148.8 (3)
O9—Rb—O12	51.59 (11)	P3^iii—O9—Rb	89.9 (2)
O3^vii—Rb—O12	148.95 (11)	Tb^ix—O9—Rb	91.20 (14)
O8^iii—Rb—O9^iii	52.91 (12)	P3^iii—O9—Rb^xi	86.0 (2)
O6^i—Rb—O9^iii	55.05 (12)	Tb^ix—O9—Rb^xi	93.04 (15)
O1—Rb—O9^iii	139.67 (11)	Rb—O9—Rb^xi	175.69 (14)
O2—Rb—O9^iii	135.74 (12)	P3—O10—P4	134.1 (3)
O5^vi—Rb—O9^iii	62.25 (11)	P3—O10—Rb^x	84.58 (19)
O7^vi—Rb—O9^iii	43.84 (11)	P4—O10—Rb^x	141.3 (2)
O9—Rb—O9^iii	83.283 (18)	P4—O11—Tb	146.7 (3)
O3^vii—Rb—O9^iii	81.40 (11)	P4—O12—Tb^ix	129.2 (3)
O12—Rb—O9^iii	129.60 (11)	P4—O12—Rb	106.8 (2)
O8^iii—Rb—O10^vi	91.52 (12)	Tb^ix—O12—Rb	86.79 (13)

Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) x−1/2, −y−1/2, z−1/2; (iii) −x+5/2, y+1/2, −z+5/2; (iv) −x+5/2, y−1/2, −z+3/2; (v) −x+2, −y+1, −z+2; (vi) x, y+1, z; (vii) −x+5/2, y+1/2, −z+3/2; (viii) −x+3, −y, −z+2; (ix) x+1/2, −y+1/2, z+1/2; (x) x, y−1, z; (xi) −x+5/2, y−1/2, −z+5/2; (xii) x+1/2, −y−1/2, z+1/2.