RbGd(PO₃)₄

Single crystals of rubidium gadolinium polyphosphate were grown from a polyphosphate flux. The structure of the title compound is isotypic with CsGd(PO₃)₄ and consists of helical polyphosphate chains running along the [101] direction with a period of eight PO₄ tetra­hedra. These polyphosphate chains are connected by isolated GdO₈ dodeca­hedra and irregularly shaped RbO₁₁ polyhedra, forming a three-dimensional framework.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](P-O)= 0.004 Å
• R factor = 0.023
• wR factor = 0.056
• Data-to-parameter ratio = 13.0

checkCIF/PLATON results

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Computing details

Data collection: CAD-4 Software (Enraf–Nonius, 1989); cell refinement: CAD-4 Software; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Berndt, 2001) and ORTEP-3 (Farrugia, 1997).; software used to prepare material for publication: SHELXL97.

Rubidium gadolinium polyphosphate

Crystal data

RbGd(PO3)4	F(000) = 1028
Mr = 558.60	Dx = 3.765 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 25 reflections
a = 10.385 (2) Å	θ = 11–15°
b = 8.976 (2) Å	µ = 12.35 mm^−1
c = 11.008 (2) Å	T = 298 K
β = 106.2 (1)°	Truncated hexagonal pyramid, colourless
V = 985.4 (6) Å^3	0.18 × 0.18 × 0.14 mm
Z = 4

Data collection

Enraf–Nonius CAD-4 diffractometer	1878 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.024
Graphite monochromator	θmax = 27.0°, θmin = 2.4°
θ/2θ scans	h = 0→13
Absorption correction: ψ scan (North et al., 1968)	k = −1→11
Tmin = 0.129, Tmax = 0.178	l = −14→13
2537 measured reflections	2 standard reflections every 60 min
2137 independent reflections	intensity decay: 1.3%

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)] = 0.023	w = 1/[σ^2(Fo^2) + (0.0237P)^2 + 1.2148P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.056	(Δ/σ)max < 0.001
S = 1.07	Δρmax = 0.79 e Å^−3
2137 reflections	Δρmin = −0.78 e Å^−3
164 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0152 (4)

Special details

Experimental. Data were corrected for Lorentz-polarization effects and an empirical absorption correction (ψ scan; North et al., 1968) was applied. The structure was solved in the P 1 2₁/n 1 space group by the Patterson method (Gd and Rb) 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 (Ų)

	x	y	z	Uiso*/Ueq
Gd	0.49925 (2)	0.27258 (3)	0.18283 (2)	0.00615 (10)
Rb	0.69271 (6)	0.56828 (7)	0.45770 (5)	0.02362 (15)
P1	0.64547 (12)	−0.09374 (14)	0.25926 (11)	0.0074 (2)
P2	0.45989 (12)	−0.32739 (14)	0.13745 (11)	0.0070 (2)
P3	0.24733 (12)	−0.47457 (14)	0.22319 (11)	0.0068 (2)
P4	0.17479 (12)	−0.60731 (14)	−0.02223 (11)	0.0073 (2)
O1	0.1403 (3)	−0.5456 (4)	0.1023 (3)	0.0096 (7)
O2	0.3541 (3)	−0.5840 (4)	0.2843 (3)	0.0093 (7)
O3	0.5224 (3)	−0.2075 (4)	0.2460 (3)	0.0112 (7)
O4	0.6011 (3)	0.0380 (4)	0.1756 (3)	0.0125 (7)
O5	0.4375 (4)	−0.2563 (4)	0.0106 (3)	0.0128 (7)
O6	0.1704 (3)	−0.4063 (4)	0.3045 (3)	0.0099 (7)
O7	0.7625 (3)	−0.1800 (4)	0.2463 (3)	0.0134 (7)
O8	0.0669 (3)	−0.7099 (4)	−0.0936 (3)	0.0122 (7)
O9	0.3155 (3)	−0.6623 (4)	0.0160 (3)	0.0129 (7)
O10	0.5380 (3)	−0.4674 (4)	0.1704 (3)	0.0104 (7)
O11	0.3138 (3)	−0.3434 (4)	0.1603 (3)	0.0082 (7)
O12	0.6682 (3)	−0.0489 (4)	0.4033 (3)	0.0123 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Gd	0.00708 (14)	0.00607 (14)	0.00537 (13)	0.00036 (9)	0.00183 (9)	0.00075 (8)
Rb	0.0247 (3)	0.0334 (3)	0.0125 (3)	−0.0040 (2)	0.0048 (2)	0.0025 (2)
P1	0.0076 (5)	0.0069 (6)	0.0073 (6)	−0.0009 (5)	0.0015 (4)	−0.0013 (4)
P2	0.0079 (5)	0.0066 (6)	0.0070 (5)	−0.0012 (5)	0.0025 (4)	−0.0008 (4)
P3	0.0083 (5)	0.0074 (6)	0.0055 (5)	0.0001 (5)	0.0031 (4)	−0.0005 (5)
P4	0.0089 (5)	0.0086 (6)	0.0040 (5)	0.0003 (5)	0.0011 (4)	0.0004 (5)
O1	0.0097 (16)	0.0127 (17)	0.0080 (16)	−0.0022 (14)	0.0053 (13)	−0.0017 (14)
O2	0.0128 (16)	0.0090 (17)	0.0073 (16)	0.0040 (14)	0.0046 (13)	−0.0001 (13)
O3	0.0113 (17)	0.0134 (18)	0.0095 (17)	−0.0026 (14)	0.0040 (13)	−0.0025 (14)
O4	0.0183 (18)	0.0111 (18)	0.0084 (16)	0.0021 (15)	0.0040 (14)	0.0017 (14)
O5	0.0152 (17)	0.0182 (19)	0.0064 (16)	−0.0010 (15)	0.0052 (14)	0.0004 (14)
O6	0.0116 (16)	0.0110 (17)	0.0085 (16)	0.0005 (14)	0.0052 (13)	−0.0015 (13)
O7	0.0114 (16)	0.0131 (18)	0.0150 (18)	0.0038 (15)	0.0028 (14)	−0.0027 (15)
O8	0.0132 (17)	0.0133 (18)	0.0093 (16)	−0.0051 (14)	0.0020 (14)	−0.0021 (14)
O9	0.0131 (17)	0.0188 (19)	0.0062 (16)	0.0024 (16)	0.0014 (13)	0.0023 (14)
O10	0.0080 (15)	0.0080 (17)	0.0157 (17)	0.0009 (14)	0.0039 (13)	0.0018 (14)
O11	0.0080 (15)	0.0052 (16)	0.0122 (16)	−0.0005 (13)	0.0043 (13)	0.0016 (13)
O12	0.0176 (18)	0.0110 (17)	0.0055 (16)	0.0001 (15)	−0.0014 (13)	−0.0018 (13)

Geometric parameters (Å, º)

Gd—O9^i	2.325 (3)	P2—O11	1.611 (3)
Gd—O4	2.368 (3)	P2—Rb^vii	3.7372 (14)
Gd—O10^i	2.379 (3)	P2—Rb^x	3.7952 (13)
Gd—O5^ii	2.401 (3)	P3—O6	1.487 (3)
Gd—O7^iii	2.416 (3)	P3—O2	1.493 (3)
Gd—O6^iv	2.417 (3)	P3—O1	1.610 (3)
Gd—O8^v	2.430 (3)	P3—O11	1.616 (3)
Gd—O2^i	2.473 (3)	P3—Rb^ix	3.4953 (13)
Gd—Rb	4.1051 (6)	P4—O9	1.488 (4)
Gd—Rb^vi	4.3297 (6)	P4—O8	1.494 (4)
Gd—Rb^vii	4.6091 (6)	P4—O1	1.608 (3)
Rb—O4^iii	2.925 (3)	P4—O12^xi	1.616 (4)
Rb—O5^viii	2.971 (4)	O2—Gd^x	2.473 (3)
Rb—O6^ix	2.986 (3)	O2—Rb^ix	3.016 (3)
Rb—O2^ix	3.016 (3)	O3—Rb^x	3.212 (4)
Rb—O10^i	3.139 (3)	O4—Rb^vi	2.925 (3)
Rb—O3^i	3.212 (4)	O5—Gd^ii	2.401 (3)
Rb—O7^iii	3.287 (4)	O5—Rb^vii	2.971 (4)
Rb—O11^viii	3.330 (3)	O6—Gd^xii	2.417 (3)
Rb—O8^v	3.458 (4)	O6—Rb^ix	2.986 (3)
Rb—O7^i	3.462 (4)	O7—Gd^vi	2.416 (3)
Rb—O12^i	3.485 (4)	O7—Rb^vi	3.287 (4)
Rb—P3^ix	3.4953 (13)	O7—Rb^x	3.462 (4)
P1—O7	1.481 (4)	O8—Gd^xi	2.430 (3)
P1—O4	1.491 (4)	O8—Rb^xi	3.458 (4)
P1—O12	1.589 (3)	O9—Gd^x	2.325 (3)
P1—O3	1.611 (4)	O10—Gd^x	2.379 (3)
P1—Rb^vi	3.5887 (13)	O10—Rb^x	3.139 (3)
P1—Rb^x	3.6904 (14)	O11—Rb^vii	3.330 (3)
P2—O10	1.485 (4)	O12—P4^v	1.616 (4)
P2—O5	1.493 (4)	O12—Rb^x	3.485 (4)
P2—O3	1.605 (4)
O9^i—Gd—O4	118.24 (12)	O5^viii—Rb—O12^i	59.41 (9)
O9^i—Gd—O10^i	79.78 (12)	O6^ix—Rb—O12^i	128.67 (9)
O4—Gd—O10^i	141.83 (12)	O2^ix—Rb—O12^i	95.30 (9)
O9^i—Gd—O5^ii	71.44 (12)	O10^i—Rb—O12^i	86.28 (8)
O4—Gd—O5^ii	71.39 (12)	O3^i—Rb—O12^i	42.12 (8)
O10^i—Gd—O5^ii	85.20 (12)	O7^iii—Rb—O12^i	124.66 (8)
O9^i—Gd—O7^iii	138.79 (12)	O11^viii—Rb—O12^i	51.67 (8)
O4—Gd—O7^iii	74.96 (12)	O8^v—Rb—O12^i	151.97 (8)
O10^i—Gd—O7^iii	70.81 (12)	O7^i—Rb—O12^i	42.28 (8)
O5^ii—Gd—O7^iii	77.80 (12)	O4^iii—Rb—P3^ix	122.08 (7)
O9^i—Gd—O6^iv	76.21 (12)	O5^viii—Rb—P3^ix	92.09 (7)
O4—Gd—O6^iv	75.58 (11)	O6^ix—Rb—P3^ix	24.98 (6)
O10^i—Gd—O6^iv	142.47 (11)	O2^ix—Rb—P3^ix	25.16 (6)
O5^ii—Gd—O6^iv	113.26 (11)	O10^i—Rb—P3^ix	152.36 (7)
O7^iii—Gd—O6^iv	142.75 (12)	O3^i—Rb—P3^ix	141.99 (7)
O9^i—Gd—O8^v	143.20 (12)	O7^iii—Rb—P3^ix	120.25 (7)
O4—Gd—O8^v	79.78 (12)	O11^viii—Rb—P3^ix	64.98 (6)
O10^i—Gd—O8^v	106.22 (12)	O8^v—Rb—P3^ix	83.90 (6)
O5^ii—Gd—O8^v	144.17 (12)	O7^i—Rb—P3^ix	145.14 (6)
O7^iii—Gd—O8^v	74.47 (12)	O12^i—Rb—P3^ix	113.20 (6)
O6^iv—Gd—O8^v	78.31 (11)	O7—P1—O4	118.4 (2)
O9^i—Gd—O2^i	75.89 (11)	O7—P1—O12	109.3 (2)
O4—Gd—O2^i	144.36 (11)	O4—P1—O12	110.5 (2)
O10^i—Gd—O2^i	69.46 (11)	O7—P1—O3	108.2 (2)
O5^ii—Gd—O2^i	141.61 (12)	O4—P1—O3	110.2 (2)
O7^iii—Gd—O2^i	117.43 (12)	O12—P1—O3	98.29 (19)
O6^iv—Gd—O2^i	76.93 (11)	O7—P1—Rb^vi	66.33 (15)
O8^v—Gd—O2^i	72.77 (11)	O4—P1—Rb^vi	52.30 (14)
O9^i—Gd—Rb	123.04 (9)	O12—P1—Rb^vi	126.51 (14)
O4—Gd—Rb	117.92 (8)	O3—P1—Rb^vi	134.72 (14)
O10^i—Gd—Rb	49.61 (8)	O7—P1—Rb^x	69.52 (15)
O5^ii—Gd—Rb	119.62 (9)	O4—P1—Rb^x	170.08 (15)
O7^iii—Gd—Rb	53.19 (9)	O12—P1—Rb^x	70.06 (14)
O6^iv—Gd—Rb	127.02 (8)	O3—P1—Rb^x	60.26 (13)
O8^v—Gd—Rb	57.24 (9)	Rb^vi—P1—Rb^x	135.84 (4)
O2^i—Gd—Rb	64.24 (8)	O10—P2—O5	121.5 (2)
O9^i—Gd—Rb^vi	110.47 (8)	O10—P2—O3	107.79 (19)
O4—Gd—Rb^vi	39.62 (8)	O5—P2—O3	109.6 (2)
O10^i—Gd—Rb^vi	103.97 (8)	O10—P2—O11	111.13 (19)
O5^ii—Gd—Rb^vi	41.03 (9)	O5—P2—O11	105.99 (19)
O7^iii—Gd—Rb^vi	52.99 (9)	O3—P2—O11	98.42 (18)
O6^iv—Gd—Rb^vi	111.25 (8)	O10—P2—Rb^vii	158.53 (14)
O8^v—Gd—Rb^vi	103.29 (8)	O5—P2—Rb^vii	48.68 (14)
O2^i—Gd—Rb^vi	170.36 (8)	O3—P2—Rb^vii	93.64 (14)
Rb—Gd—Rb^vi	106.172 (8)	O11—P2—Rb^vii	62.97 (12)
O9^i—Gd—Rb^vii	56.64 (9)	O10—P2—Rb^x	53.19 (14)
O4—Gd—Rb^vii	68.89 (8)	O5—P2—Rb^x	150.12 (15)
O10^i—Gd—Rb^vii	136.30 (8)	O3—P2—Rb^x	56.84 (13)
O5^ii—Gd—Rb^vii	78.55 (9)	O11—P2—Rb^x	102.54 (13)
O7^iii—Gd—Rb^vii	141.50 (9)	Rb^vii—P2—Rb^x	146.35 (4)
O6^iv—Gd—Rb^vii	35.36 (8)	O6—P3—O2	117.1 (2)
O8^v—Gd—Rb^vii	110.65 (9)	O6—P3—O1	107.32 (19)
O2^i—Gd—Rb^vii	99.89 (8)	O2—P3—O1	111.54 (19)
Rb—Gd—Rb^vii	161.541 (15)	O6—P3—O11	108.84 (19)
Rb^vi—Gd—Rb^vii	89.723 (11)	O2—P3—O11	108.66 (19)
O4^iii—Rb—O5^viii	56.31 (10)	O1—P3—O11	102.32 (18)
O4^iii—Rb—O6^ix	99.11 (9)	O6—P3—Rb^ix	57.98 (14)
O5^viii—Rb—O6^ix	86.12 (9)	O2—P3—Rb^ix	59.15 (13)
O4^iii—Rb—O2^ix	144.00 (9)	O1—P3—Rb^ix	128.66 (13)
O5^viii—Rb—O2^ix	98.18 (9)	O11—P3—Rb^ix	128.94 (13)
O6^ix—Rb—O2^ix	50.13 (9)	O9—P4—O8	118.6 (2)
O4^iii—Rb—O10^i	74.11 (9)	O9—P4—O1	107.94 (19)
O5^viii—Rb—O10^i	115.17 (9)	O8—P4—O1	110.36 (19)
O6^ix—Rb—O10^i	144.97 (9)	O9—P4—O12^xi	109.3 (2)
O2^ix—Rb—O10^i	141.46 (9)	O8—P4—O12^xi	110.4 (2)
O4^iii—Rb—O3^i	91.53 (9)	O1—P4—O12^xi	98.33 (19)
O5^viii—Rb—O3^i	93.12 (9)	P3—O1—P4	125.1 (2)
O6^ix—Rb—O3^i	166.61 (9)	P3—O2—Gd^x	127.50 (18)
O2^ix—Rb—O3^i	116.96 (9)	P3—O2—Rb^ix	95.69 (15)
O10^i—Rb—O3^i	46.29 (9)	Gd^x—O2—Rb^ix	136.72 (13)
O4^iii—Rb—O7^iii	48.09 (9)	P2—O3—P1	129.7 (2)
O5^viii—Rb—O7^iii	104.06 (9)	P2—O3—Rb^x	98.43 (16)
O6^ix—Rb—O7^iii	98.37 (9)	P1—O3—Rb^x	93.93 (15)
O2^ix—Rb—O7^iii	139.97 (9)	P1—O4—Gd	138.4 (2)
O10^i—Rb—O7^iii	51.16 (9)	P1—O4—Rb^vi	103.91 (17)
O3^i—Rb—O7^iii	94.79 (9)	Gd—O4—Rb^vi	109.31 (13)
O4^iii—Rb—O11^viii	102.24 (9)	P2—O5—Gd^ii	142.5 (2)
O5^viii—Rb—O11^viii	45.93 (9)	P2—O5—Rb^vii	109.14 (17)
O6^ix—Rb—O11^viii	77.00 (9)	Gd^ii—O5—Rb^vii	106.93 (12)
O2^ix—Rb—O11^viii	57.62 (9)	P3—O6—Gd^xii	146.2 (2)
O10^i—Rb—O11^viii	137.91 (9)	P3—O6—Rb^ix	97.04 (16)
O3^i—Rb—O11^viii	92.88 (9)	Gd^xii—O6—Rb^ix	116.71 (12)
O7^iii—Rb—O11^viii	149.44 (8)	P1—O7—Gd^vi	148.8 (2)
O4^iii—Rb—O8^v	97.34 (9)	P1—O7—Rb^vi	89.30 (16)
O5^viii—Rb—O8^v	145.50 (9)	Gd^vi—O7—Rb^vi	90.76 (11)
O6^ix—Rb—O8^v	75.89 (9)	P1—O7—Rb^x	86.85 (16)
O2^ix—Rb—O8^v	92.55 (9)	Gd^vi—O7—Rb^x	93.15 (11)
O10^i—Rb—O8^v	71.13 (9)	Rb^vi—O7—Rb^x	175.97 (11)
O3^i—Rb—O8^v	110.96 (9)	P4—O8—Gd^xi	129.7 (2)
O7^iii—Rb—O8^v	51.46 (8)	P4—O8—Rb^xi	107.09 (17)
O11^viii—Rb—O8^v	148.65 (8)	Gd^xi—O8—Rb^xi	86.54 (10)
O4^iii—Rb—O7^i	53.43 (9)	P4—O9—Gd^x	146.3 (2)
O5^viii—Rb—O7^i	55.47 (9)	P2—O10—Gd^x	139.0 (2)
O6^ix—Rb—O7^i	140.31 (9)	P2—O10—Rb^x	104.57 (17)
O2^ix—Rb—O7^i	136.18 (9)	Gd^x—O10—Rb^x	95.13 (11)
O10^i—Rb—O7^i	62.20 (8)	P2—O11—P3	131.7 (2)
O3^i—Rb—O7^i	43.90 (8)	P2—O11—Rb^vii	91.50 (14)
O7^iii—Rb—O7^i	83.531 (13)	P3—O11—Rb^vii	134.48 (16)
O11^viii—Rb—O7^i	81.69 (8)	P1—O12—P4^v	134.4 (2)
O8^v—Rb—O7^i	129.61 (8)	P1—O12—Rb^x	84.56 (14)
O4^iii—Rb—O12^i	91.97 (9)	P4^v—O12—Rb^x	141.06 (17)

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, −y−1/2, z+1/2; (vi) −x+3/2, y−1/2, −z+1/2; (vii) x−1/2, −y+1/2, z−1/2; (viii) x+1/2, −y+1/2, z+1/2; (ix) −x+1, −y, −z+1; (x) x, y−1, z; (xi) x−1/2, −y−1/2, z−1/2; (xii) −x+1/2, y−1/2, −z+1/2.