Potassium ytterbium diphosphate

KYbP₂O₇ consists of P₂O₇ double-tetra­hedral groups connected to YbO₆ octa­hedra, forming a framework whose channels are occupied by K⁺ cations.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](P-O) = 0.005 Å
• R factor = 0.035
• wR factor = 0.096
• Data-to-parameter ratio = 19.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.85
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.32

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      0.316
            Tmax scaled      0.077 Tmin scaled      0.070

   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, 2001); software used to prepare material for publication: SHELXL97.

potassium ytterbium diphosphate

Crystal data

KYb(P2O7)	F(000) = 700
Mr = 386.08	Dx = 3.842 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25 reflections
a = 7.538 (3) Å	θ = 10.2–15.1°
b = 10.832 (2) Å	µ = 15.10 mm^−1
c = 8.537 (4) Å	T = 298 K
β = 106.768 (7)°	Prism, colourless
V = 667.4 (4) Å^3	0.18 × 0.17 × 0.17 mm
Z = 4

Data collection

Enraf–Nonius CAD-4 diffractometer	1763 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.044
Graphite monochromator	θmax = 30.0°, θmin = 2.8°
ω/2θ scans	h = −10→10
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −15→15
Tmin = 0.223, Tmax = 0.243	l = −11→11
10491 measured reflections	2 standard reflections every 120 min
1957 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)] = 0.035	w = 1/[σ^2(Fo^2) + (0.0646P)^2 + 0.1042P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.096	(Δ/σ)max < 0.001
S = 1.17	Δρmax = 4.91 e Å^−3
1957 reflections	Δρmin = −3.27 e Å^−3
101 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0011 (1)

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
Yb	0.23224 (3)	0.097047 (18)	0.75123 (2)	0.00867 (12)
K	0.8193 (2)	0.32213 (15)	0.43407 (18)	0.0314 (3)
P1	0.1311 (2)	0.39934 (11)	0.81239 (17)	0.0099 (3)
P2	0.44564 (19)	0.35783 (12)	0.69023 (16)	0.0106 (3)
O1	0.1354 (8)	0.4055 (4)	0.9884 (6)	0.0244 (12)
O2	0.0713 (5)	0.2736 (4)	0.7388 (5)	0.0157 (8)
O3	0.0128 (5)	0.5010 (3)	0.7103 (4)	0.0146 (7)
O4	0.3388 (6)	0.4247 (4)	0.8055 (5)	0.0181 (8)
O5	0.3339 (8)	0.3856 (4)	0.5180 (6)	0.0235 (10)
O6	0.6360 (7)	0.4145 (3)	0.7376 (5)	0.0183 (9)
O7	0.4586 (5)	0.2223 (3)	0.7327 (5)	0.0161 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb	0.00885 (16)	0.00640 (17)	0.01053 (17)	−0.00015 (6)	0.00241 (10)	0.00046 (6)
K	0.0228 (7)	0.0415 (9)	0.0266 (7)	−0.0081 (6)	0.0017 (6)	0.0026 (6)
P1	0.0078 (7)	0.0122 (7)	0.0101 (6)	0.0039 (4)	0.0032 (5)	0.0013 (4)
P2	0.0079 (6)	0.0098 (6)	0.0138 (6)	−0.0013 (4)	0.0027 (5)	0.0009 (5)
O1	0.030 (3)	0.034 (3)	0.010 (2)	0.0126 (18)	0.007 (2)	0.0027 (16)
O2	0.0101 (17)	0.0166 (19)	0.021 (2)	−0.0009 (14)	0.0055 (15)	−0.0024 (15)
O3	0.0134 (18)	0.0130 (17)	0.0187 (18)	0.0049 (14)	0.0067 (15)	0.0045 (14)
O4	0.0095 (19)	0.0209 (19)	0.024 (2)	−0.0029 (15)	0.0055 (16)	−0.0121 (16)
O5	0.024 (3)	0.031 (2)	0.012 (2)	−0.0035 (19)	−0.0001 (18)	0.0034 (17)
O6	0.012 (2)	0.0122 (18)	0.032 (2)	−0.0014 (14)	0.0084 (18)	0.0027 (15)
O7	0.0064 (17)	0.0107 (17)	0.033 (2)	0.0005 (14)	0.0085 (16)	0.0018 (16)

Geometric parameters (Å, º)

Yb—O1^i	2.150 (5)	P1—O2	1.513 (4)
Yb—O5^ii	2.191 (5)	P1—O3	1.523 (4)
Yb—O6^iii	2.202 (4)	P1—O4	1.607 (4)
Yb—O7	2.221 (4)	P1—Yb^ix	3.3945 (16)
Yb—O3^iv	2.225 (4)	P1—K^x	3.503 (2)
Yb—O2	2.250 (4)	P1—K^v	3.710 (2)
Yb—P2	3.3648 (15)	P1—K^vi	3.758 (2)
Yb—P1^iv	3.3945 (16)	P2—O5	1.499 (5)
Yb—P1	3.4360 (14)	P2—O6	1.505 (5)
Yb—P2^iii	3.4870 (15)	P2—O7	1.509 (4)
Yb—K^v	3.9616 (19)	P2—O4	1.612 (4)
Yb—K^iii	4.1036 (19)	P2—Yb^xi	3.4870 (15)
K—O3^vi	2.773 (4)	P2—K^ii	3.562 (2)
K—O2^vii	2.793 (4)	O1—Yb^ii	2.150 (5)
K—O7^i	2.808 (4)	O1—K^v	3.366 (6)
K—O2^viii	3.048 (4)	O2—K^x	2.793 (4)
K—O3^vii	3.075 (4)	O2—K^v	3.048 (4)
K—O6^i	3.156 (4)	O3—Yb^ix	2.225 (4)
K—O1^viii	3.366 (6)	O3—K^vi	2.773 (4)
K—O6	3.420 (5)	O3—K^x	3.075 (4)
K—O4^vi	3.423 (5)	O4—K^vi	3.423 (5)
K—P1^vii	3.503 (2)	O5—Yb^i	2.191 (5)
K—P2^i	3.562 (2)	O6—Yb^xi	2.202 (4)
K—P1^viii	3.710 (2)	O6—K^ii	3.156 (4)
P1—O1	1.495 (5)	O7—K^ii	2.808 (4)
O1^i—Yb—O5^ii	175.76 (19)	O3^vii—K—P1^vii	25.73 (7)
O1^i—Yb—O6^iii	92.69 (18)	O6^i—K—P1^vii	139.32 (9)
O5^ii—Yb—O6^iii	90.79 (17)	O1^viii—K—P1^vii	77.75 (10)
O1^i—Yb—O7	88.27 (17)	O6—K—P1^vii	62.73 (9)
O5^ii—Yb—O7	88.64 (18)	O4^vi—K—P1^vii	112.64 (8)
O6^iii—Yb—O7	101.84 (15)	O3^vi—K—P2^i	120.25 (10)
O1^i—Yb—O3^iv	95.85 (17)	O2^vii—K—P2^i	130.70 (10)
O5^ii—Yb—O3^iv	86.72 (17)	O7^i—K—P2^i	23.85 (8)
O6^iii—Yb—O3^iv	87.56 (15)	O2^viii—K—P2^i	90.39 (9)
O7—Yb—O3^iv	169.58 (14)	O3^vii—K—P2^i	155.95 (9)
O1^i—Yb—O2	86.88 (17)	O6^i—K—P2^i	24.96 (8)
O5^ii—Yb—O2	89.90 (16)	O1^viii—K—P2^i	95.09 (10)
O6^iii—Yb—O2	174.31 (16)	O6—K—P2^i	100.29 (9)
O7—Yb—O2	83.82 (13)	O4^vi—K—P2^i	90.51 (8)
O3^iv—Yb—O2	86.85 (14)	P1^vii—K—P2^i	151.23 (6)
O1^i—Yb—P2	83.26 (12)	O3^vi—K—P1^viii	85.13 (9)
O5^ii—Yb—P2	92.84 (14)	O2^vii—K—P1^viii	79.84 (9)
O6^iii—Yb—P2	122.04 (12)	O7^i—K—P1^viii	107.30 (10)
O7—Yb—P2	20.73 (10)	O2^viii—K—P1^viii	23.34 (7)
O3^iv—Yb—P2	150.40 (10)	O3^vii—K—P1^viii	115.06 (9)
O2—Yb—P2	63.55 (10)	O6^i—K—P1^viii	62.71 (9)
O1^i—Yb—P1^iv	79.03 (13)	O1^viii—K—P1^viii	23.76 (9)
O5^ii—Yb—P1^iv	104.14 (15)	O6—K—P1^viii	145.95 (8)
O6^iii—Yb—P1^iv	76.92 (12)	O4^vi—K—P1^viii	119.35 (8)
O7—Yb—P1^iv	167.14 (11)	P1^vii—K—P1^viii	95.85 (6)
O3^iv—Yb—P1^iv	20.46 (9)	P2^i—K—P1^viii	86.59 (5)
O2—Yb—P1^iv	97.44 (10)	O1—P1—O2	112.0 (2)
P2—Yb—P1^iv	154.76 (3)	O1—P1—O3	112.5 (2)
O1^i—Yb—P1	98.46 (13)	O2—P1—O3	111.0 (2)
O5^ii—Yb—P1	77.69 (13)	O1—P1—O4	106.9 (3)
O6^iii—Yb—P1	165.03 (12)	O2—P1—O4	108.4 (2)
O7—Yb—P1	68.75 (10)	O3—P1—O4	105.7 (2)
O3^iv—Yb—P1	101.12 (10)	O1—P1—Yb^ix	85.2 (2)
O2—Yb—P1	19.47 (10)	O2—P1—Yb^ix	111.83 (16)
P2—Yb—P1	50.24 (4)	O4—P1—Yb^ix	129.46 (16)
P1^iv—Yb—P1	114.92 (2)	O1—P1—Yb	104.68 (17)
O1^i—Yb—P2^iii	98.80 (14)	O3—P1—Yb	136.15 (16)
O5^ii—Yb—P2^iii	83.94 (13)	O4—P1—Yb	84.05 (15)
O6^iii—Yb—P2^iii	16.25 (12)	Yb^ix—P1—Yb	141.36 (5)
O7—Yb—P2^iii	86.94 (10)	O1—P1—K^x	138.7 (2)
O3^iv—Yb—P2^iii	101.82 (10)	O2—P1—K^x	50.38 (16)
O2—Yb—P2^iii	169.01 (10)	O3—P1—K^x	61.24 (15)
P2—Yb—P2^iii	107.57 (2)	O4—P1—K^x	114.11 (16)
P1^iv—Yb—P2^iii	92.89 (4)	Yb^ix—P1—K^x	72.99 (4)
P1—Yb—P2^iii	149.57 (3)	Yb—P1—K^x	75.62 (4)
O1^i—Yb—K^v	110.19 (16)	O1—P1—K^v	65.1 (2)
O5^ii—Yb—K^v	69.54 (15)	O2—P1—K^v	52.95 (16)
O6^iii—Yb—K^v	125.26 (12)	O3—P1—K^v	108.33 (16)
O7—Yb—K^v	126.88 (10)	O4—P1—K^v	145.41 (17)
O3^iv—Yb—K^v	42.70 (10)	Yb^ix—P1—K^v	84.59 (5)
O2—Yb—K^v	49.97 (10)	Yb—P1—K^v	67.21 (4)
P2—Yb—K^v	109.91 (4)	K^x—P1—K^v	78.06 (5)
P1^iv—Yb—K^v	60.87 (4)	O1—P1—K^vi	123.39 (18)
P1—Yb—K^v	59.70 (4)	O2—P1—K^vi	123.79 (17)
P2^iii—Yb—K^v	134.55 (4)	O4—P1—K^vi	65.59 (17)
O1^i—Yb—K^iii	127.32 (12)	Yb^ix—P1—K^vi	67.04 (4)
O5^ii—Yb—K^iii	56.81 (14)	Yb—P1—K^vi	128.15 (5)
O6^iii—Yb—K^iii	56.42 (12)	K^x—P1—K^vi	79.87 (5)
O7—Yb—K^iii	135.21 (11)	K^v—P1—K^vi	148.13 (5)
O3^iv—Yb—K^iii	47.52 (10)	O5—P2—O6	113.8 (3)
O2—Yb—K^iii	119.73 (10)	O5—P2—O7	114.2 (3)
P2—Yb—K^iii	148.25 (3)	O6—P2—O7	110.0 (2)
P1^iv—Yb—K^iii	54.72 (3)	O5—P2—O4	105.7 (3)
P1—Yb—K^iii	121.67 (4)	O6—P2—O4	104.9 (2)
P2^iii—Yb—K^iii	63.93 (3)	O7—P2—O4	107.5 (2)
K^v—Yb—K^iii	70.66 (4)	O5—P2—Yb	99.3 (2)
O3^vi—K—O2^vii	105.60 (12)	O6—P2—Yb	139.68 (16)
O3^vi—K—O7^i	109.38 (12)	O4—P2—Yb	86.42 (16)
O2^vii—K—O7^i	144.72 (14)	O5—P2—Yb^xi	99.3 (2)
O3^vi—K—O2^viii	63.61 (11)	O7—P2—Yb^xi	133.98 (16)
O2^vii—K—O2^viii	94.68 (12)	O4—P2—Yb^xi	91.62 (16)
O7^i—K—O2^viii	104.66 (12)	Yb—P2—Yb^xi	161.06 (5)
O3^vi—K—O3^vii	74.28 (12)	O5—P2—K^ii	144.0 (2)
O2^vii—K—O3^vii	50.20 (11)	O6—P2—K^ii	62.25 (16)
O7^i—K—O3^vii	137.62 (12)	O7—P2—K^ii	48.80 (16)
O2^viii—K—O3^vii	113.65 (11)	O4—P2—K^ii	109.84 (17)
O3^vi—K—O6^i	120.74 (13)	Yb—P2—K^ii	77.46 (4)
O2^vii—K—O6^i	114.71 (12)	Yb^xi—P2—K^ii	85.54 (5)
O7^i—K—O6^i	48.47 (11)	P1—O1—Yb^ii	161.9 (4)
O2^viii—K—O6^i	71.31 (12)	P1—O1—K^v	91.1 (2)
O3^vii—K—O6^i	163.25 (11)	Yb^ii—O1—K^v	98.53 (17)
O3^vi—K—O1^viii	99.88 (12)	P1—O2—Yb	130.8 (2)
O2^vii—K—O1^viii	57.97 (12)	P1—O2—K^x	104.96 (19)
O7^i—K—O1^viii	118.74 (13)	Yb—O2—K^x	114.60 (16)
O2^viii—K—O1^viii	45.43 (11)	P1—O2—K^v	103.71 (19)
O3^vii—K—O1^viii	101.27 (12)	Yb—O2—K^v	95.61 (13)
O6^i—K—O1^viii	70.27 (12)	K^x—O2—K^v	102.10 (13)
O3^vi—K—O6	118.07 (11)	P1—O3—Yb^ix	128.8 (2)
O2^vii—K—O6	70.39 (12)	P1—O3—K^vi	119.2 (2)
O7^i—K—O6	88.99 (12)	Yb^ix—O3—K^vi	104.33 (14)
O2^viii—K—O6	165.01 (12)	P1—O3—K^x	93.03 (17)
O3^vii—K—O6	55.98 (10)	Yb^ix—O3—K^x	100.23 (14)
O6^i—K—O6	115.45 (13)	K^vi—O3—K^x	105.72 (12)
O1^viii—K—O6	122.32 (12)	P1—O4—P2	127.5 (3)
O3^vi—K—O4^vi	46.05 (10)	P1—O4—K^vi	89.09 (18)
O2^vii—K—O4^vi	137.17 (12)	P2—O4—K^vi	98.31 (19)
O7^i—K—O4^vi	70.29 (11)	P2—O5—Yb^i	164.9 (4)
O2^viii—K—O4^vi	96.33 (11)	P2—O6—Yb^xi	139.6 (3)
O3^vii—K—O4^vi	87.69 (10)	P2—O6—K^ii	92.79 (17)
O6^i—K—O4^vi	108.03 (11)	Yb^xi—O6—K^ii	125.68 (19)
O1^viii—K—O4^vi	141.23 (12)	P2—O6—K	103.8 (2)
O6—K—O4^vi	94.08 (10)	Yb^xi—O6—K	91.13 (14)
O3^vi—K—P1^vii	88.51 (9)	K^ii—O6—K	87.37 (11)
O2^vii—K—P1^vii	24.66 (8)	P2—O7—Yb	127.8 (2)
O7^i—K—P1^vii	151.51 (10)	P2—O7—K^ii	107.35 (19)
O2^viii—K—P1^vii	103.14 (9)	Yb—O7—K^ii	118.68 (16)

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