CsLa(PO₃)₄

The title compound, caesium lanthanum tetrametaphosphate, CsLa(PO₃)₄, was grown using the flux method and its structure determined by single-crystal X-ray diffraction methods. This compound is isostructural with CsNd(PO₃)₄. The structure is built up from infinite helical chains, (PO₃)_n, which are connected by isolated LaO₈ dodecahedra and irregularly shaped Cs polyhedra. These chains are formed by corner-sharing of PO₄ tetrahedra and run along the b axis.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](P-O) = 0.005 Å
• R factor = 0.022
• wR factor = 0.049
• Data-to-parameter ratio = 12.6

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.61 Ratio
PLAT241_ALERT_2_B Check High   U(eq) as Compared to Neighbors ....        O10

Alert level C
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....         P3
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....         P4

Alert level G
REFLT03_ALERT_4_G  WARNING: Large fraction of Friedel related reflns may
                     be needed to determine absolute structure
           From the CIF: _diffrn_reflns_theta_max           28.04
           From the CIF: _reflns_number_total               2073
           Count of symmetry unique reflns         1503
           Completeness (_total/calc)            137.92%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       570
           Fraction of Friedel pairs measured     0.379
           Are heavy atom types Z>Si present          yes

   0 ALERT level A = In general: serious problem
   2 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
   4 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

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Computing details

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(I)

Crystal data

CsLa(PO3)4	F(000) = 536
Mr = 587.70	Dx = 3.341 Mg m^−3
Monoclinic, P21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2yb	Cell parameters from 961 reflections
a = 7.218 (3) Å	θ = 3.2–28.0°
b = 9.254 (3) Å	µ = 7.33 mm^−1
c = 8.864 (3) Å	T = 293 K
β = 99.377 (5)°	Prism, colorless
V = 584.2 (4) Å^3	0.14 × 0.06 × 0.04 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer	2073 independent reflections
Radiation source: fine-focus sealed tube	1993 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.023
φ and ω scans	θmax = 28.0°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −9→9
Tmin = 0.453, Tmax = 0.746	k = −12→8
3731 measured reflections	l = −10→11

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0197P)^2 + 0.0183P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.022	(Δ/σ)max < 0.001
wR(F^2) = 0.049	Δρmax = 1.25 e Å^−3
S = 1.02	Δρmin = −0.72 e Å^−3
2073 reflections	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
164 parameters	Extinction coefficient: 0.0191 (8)
1 restraint	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.006 (16)

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
La1	0.20222 (4)	−0.09932 (3)	0.30272 (3)	0.00782 (9)
Cs1	0.32599 (7)	0.06604 (4)	−0.17489 (6)	0.03065 (13)
P1	0.9168 (2)	0.17812 (16)	0.07312 (16)	0.0095 (3)
P2	0.69456 (19)	−0.02300 (16)	0.22824 (17)	0.0105 (3)
P3	0.6474 (2)	0.02504 (15)	0.54399 (17)	0.0102 (3)
P4	0.9393 (2)	−0.20722 (15)	0.62514 (17)	0.0118 (3)
O1	0.8567 (6)	0.2511 (5)	−0.0743 (5)	0.0190 (9)
O2	0.9607 (6)	0.3021 (4)	0.1993 (5)	0.0179 (9)
O3	1.0737 (5)	0.0722 (5)	0.0894 (5)	0.0124 (8)
O4	0.7305 (5)	0.1060 (4)	0.1170 (5)	0.0161 (9)
O5	0.4950 (5)	−0.0665 (5)	0.1825 (5)	0.0170 (10)
O6	0.8433 (5)	−0.1333 (4)	0.2329 (5)	0.0181 (9)
O7	0.7231 (6)	0.0573 (5)	0.3886 (5)	0.0191 (9)
O8	0.4626 (6)	−0.0448 (5)	0.5110 (5)	0.0229 (10)
O9	0.6624 (8)	0.1584 (5)	0.6349 (6)	0.0297 (12)
O10	0.7875 (7)	−0.0875 (7)	0.6333 (6)	0.0442 (15)
O11	0.8521 (8)	−0.3499 (5)	0.5941 (5)	0.0292 (12)
O12	1.0770 (6)	−0.1512 (5)	0.5349 (5)	0.0257 (11)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
La1	0.00746 (13)	0.00934 (14)	0.00701 (13)	0.00021 (12)	0.00226 (9)	−0.00030 (12)
Cs1	0.0372 (3)	0.0235 (2)	0.0360 (3)	−0.00028 (17)	0.0202 (2)	−0.00060 (18)
P1	0.0117 (6)	0.0108 (6)	0.0064 (6)	−0.0004 (5)	0.0023 (5)	0.0008 (5)
P2	0.0093 (7)	0.0132 (7)	0.0095 (7)	−0.0018 (5)	0.0029 (5)	0.0009 (5)
P3	0.0102 (7)	0.0105 (7)	0.0099 (7)	−0.0002 (5)	0.0015 (5)	−0.0014 (5)
P4	0.0128 (7)	0.0120 (7)	0.0109 (7)	0.0013 (5)	0.0031 (6)	0.0039 (5)
O1	0.026 (2)	0.018 (2)	0.013 (2)	−0.0003 (18)	0.0039 (18)	0.0034 (17)
O2	0.026 (2)	0.012 (2)	0.014 (2)	0.0044 (16)	−0.0011 (18)	−0.0059 (16)
O3	0.0119 (19)	0.016 (2)	0.0096 (19)	0.0023 (17)	0.0032 (15)	0.0031 (16)
O4	0.013 (2)	0.020 (2)	0.017 (2)	0.0024 (16)	0.0068 (17)	0.0113 (17)
O5	0.0110 (18)	0.030 (3)	0.0098 (19)	−0.0041 (15)	0.0018 (16)	−0.0028 (15)
O6	0.0135 (18)	0.018 (3)	0.024 (2)	0.0006 (15)	0.0082 (17)	0.0008 (16)
O7	0.019 (2)	0.023 (2)	0.017 (2)	−0.0119 (18)	0.0083 (18)	−0.0089 (18)
O8	0.0101 (19)	0.044 (3)	0.014 (2)	−0.0112 (18)	0.0007 (17)	−0.0029 (19)
O9	0.051 (3)	0.018 (2)	0.022 (2)	−0.015 (2)	0.011 (2)	−0.0112 (19)
O10	0.042 (3)	0.060 (4)	0.035 (3)	0.039 (3)	0.018 (2)	0.014 (3)
O11	0.048 (3)	0.019 (2)	0.016 (2)	−0.018 (2)	−0.009 (2)	0.0059 (18)
O12	0.024 (2)	0.036 (3)	0.022 (2)	0.0024 (19)	0.015 (2)	0.0106 (19)

Geometric parameters (Å, º)

La1—O12^i	2.426 (4)	P2—O4	1.597 (4)
La1—O1^ii	2.432 (4)	P3—O8	1.468 (4)
La1—O8	2.463 (4)	P3—O9	1.468 (5)
La1—O9^iii	2.472 (5)	P3—O10	1.573 (5)
La1—O3^i	2.526 (4)	P3—O7	1.590 (4)
La1—O5	2.535 (4)	P4—O12	1.468 (4)
La1—O11^iv	2.537 (5)	P4—O11	1.469 (5)
La1—O6^i	2.583 (4)	P4—O10	1.568 (5)
Cs1—O6^v	3.049 (4)	P4—O2^viii	1.608 (4)
Cs1—O2^ii	3.186 (4)	O1—La1^v	2.432 (4)
Cs1—O3^i	3.193 (4)	O2—P4^ix	1.608 (4)
Cs1—O8^vi	3.267 (5)	O2—Cs1^v	3.186 (4)
Cs1—O9^vi	3.287 (5)	O3—La1^x	2.526 (4)
Cs1—O5	3.430 (4)	O3—Cs1^x	3.193 (4)
Cs1—O12^vii	3.519 (5)	O5—Cs1^ii	3.642 (4)
Cs1—O4	3.591 (4)	O6—La1^x	2.583 (4)
Cs1—O5^v	3.642 (4)	O6—Cs1^ii	3.049 (4)
Cs1—O11^v	3.809 (5)	O8—Cs1^xi	3.267 (5)
P1—O1	1.473 (4)	O9—La1^iv	2.472 (5)
P1—O3	1.487 (4)	O9—Cs1^xi	3.287 (5)
P1—O2	1.597 (4)	O11—La1^iii	2.537 (5)
P1—O4	1.605 (4)	O11—Cs1^ii	3.809 (5)
P2—O6	1.477 (4)	O12—La1^x	2.426 (4)
P2—O5	1.487 (4)	O12—Cs1^xii	3.519 (5)
P2—O7	1.588 (4)
O12^i—La1—O1^ii	123.68 (15)	O2^ii—Cs1—O11^v	88.75 (11)
O12^i—La1—O8	75.47 (15)	O3^i—Cs1—O11^v	124.74 (11)
O1^ii—La1—O8	138.52 (15)	O8^vi—Cs1—O11^v	48.19 (11)
O12^i—La1—O9^iii	79.58 (16)	O9^vi—Cs1—O11^v	66.83 (13)
O1^ii—La1—O9^iii	71.29 (16)	O5—Cs1—O11^v	170.60 (10)
O8—La1—O9^iii	78.02 (18)	O12^vii—Cs1—O11^v	49.65 (11)
O12^i—La1—O3^i	128.10 (14)	O4—Cs1—O11^v	141.94 (10)
O1^ii—La1—O3^i	75.01 (14)	O5^v—Cs1—O11^v	81.70 (10)
O8—La1—O3^i	125.08 (15)	O1—P1—O3	119.9 (2)
O9^iii—La1—O3^i	145.15 (15)	O1—P1—O2	106.7 (2)
O12^i—La1—O5	146.23 (14)	O3—P1—O2	110.2 (2)
O1^ii—La1—O5	76.29 (13)	O1—P1—O4	105.6 (2)
O8—La1—O5	72.77 (13)	O3—P1—O4	110.9 (2)
O9^iii—La1—O5	82.90 (15)	O2—P1—O4	102.0 (2)
O3^i—La1—O5	80.77 (13)	O6—P2—O5	119.2 (2)
O12^i—La1—O11^iv	76.92 (16)	O6—P2—O7	108.1 (3)
O1^ii—La1—O11^iv	143.28 (15)	O5—P2—O7	110.5 (2)
O8—La1—O11^iv	71.78 (16)	O6—P2—O4	110.1 (2)
O9^iii—La1—O11^iv	145.42 (16)	O5—P2—O4	106.4 (2)
O3^i—La1—O11^iv	68.82 (14)	O7—P2—O4	101.1 (2)
O5—La1—O11^iv	103.35 (16)	O8—P3—O9	117.6 (3)
O12^i—La1—O6^i	71.43 (15)	O8—P3—O10	107.3 (3)
O1^ii—La1—O6^i	72.47 (14)	O9—P3—O10	107.3 (3)
O8—La1—O6^i	144.87 (14)	O8—P3—O7	109.8 (2)
O9^iii—La1—O6^i	106.73 (16)	O9—P3—O7	108.2 (3)
O3^i—La1—O6^i	70.45 (13)	O10—P3—O7	106.1 (3)
O5—La1—O6^i	141.82 (14)	O12—P4—O11	121.5 (3)
O11^iv—La1—O6^i	89.37 (15)	O12—P4—O10	108.4 (3)
O6^v—Cs1—O2^ii	116.76 (11)	O11—P4—O10	111.2 (3)
O6^v—Cs1—O3^i	81.18 (10)	O12—P4—O2^viii	105.8 (3)
O2^ii—Cs1—O3^i	67.77 (11)	O11—P4—O2^viii	109.9 (2)
O6^v—Cs1—O8^vi	108.13 (12)	O10—P4—O2^viii	97.1 (3)
O2^ii—Cs1—O8^vi	89.11 (11)	P1—O1—La1^v	170.5 (3)
O3^i—Cs1—O8^vi	156.67 (11)	P1—O2—P4^ix	130.2 (3)
O6^v—Cs1—O9^vi	89.16 (12)	P1—O2—Cs1^v	116.8 (2)
O2^ii—Cs1—O9^vi	133.68 (11)	P4^ix—O2—Cs1^v	106.90 (18)
O3^i—Cs1—O9^vi	158.27 (11)	P1—O3—La1^x	131.9 (2)
O8^vi—Cs1—O9^vi	45.06 (11)	P1—O3—Cs1^x	117.2 (2)
O6^v—Cs1—O5	123.67 (11)	La1^x—O3—Cs1^x	110.74 (13)
O2^ii—Cs1—O5	85.29 (10)	P2—O4—P1	133.4 (3)
O3^i—Cs1—O5	59.23 (10)	P2—O4—Cs1	99.96 (18)
O8^vi—Cs1—O5	124.30 (11)	P1—O4—Cs1	118.90 (19)
O9^vi—Cs1—O5	112.67 (12)	P2—O5—La1	139.0 (2)
O6^v—Cs1—O12^vii	104.79 (11)	P2—O5—Cs1	109.8 (2)
O2^ii—Cs1—O12^vii	42.58 (10)	La1—O5—Cs1	103.63 (12)
O3^i—Cs1—O12^vii	105.20 (10)	P2—O5—Cs1^ii	85.81 (18)
O8^vi—Cs1—O12^vii	52.16 (10)	La1—O5—Cs1^ii	102.61 (13)
O9^vi—Cs1—O12^vii	96.05 (11)	Cs1—O5—Cs1^ii	112.99 (11)
O5—Cs1—O12^vii	122.23 (10)	P2—O6—La1^x	128.2 (2)
O6^v—Cs1—O4	106.49 (10)	P2—O6—Cs1^ii	110.9 (2)
O2^ii—Cs1—O4	124.81 (10)	La1^x—O6—Cs1^ii	120.67 (14)
O3^i—Cs1—O4	87.90 (10)	P2—O7—P3	132.4 (3)
O8^vi—Cs1—O4	108.88 (10)	P3—O8—La1	142.9 (3)
O9^vi—Cs1—O4	76.17 (11)	P3—O8—Cs1^xi	94.7 (2)
O5—Cs1—O4	41.09 (9)	La1—O8—Cs1^xi	113.81 (14)
O12^vii—Cs1—O4	147.57 (10)	P3—O9—La1^iv	151.2 (3)
O6^v—Cs1—O5^v	43.81 (10)	P3—O9—Cs1^xi	93.9 (2)
O2^ii—Cs1—O5^v	160.56 (10)	La1^iv—O9—Cs1^xi	114.79 (16)
O3^i—Cs1—O5^v	104.08 (10)	P4—O10—P3	147.3 (4)
O8^vi—Cs1—O5^v	96.90 (10)	P4—O11—La1^iii	146.8 (3)
O9^vi—Cs1—O5^v	56.89 (10)	P4—O11—Cs1^ii	115.6 (2)
O5—Cs1—O5^v	106.08 (7)	La1^iii—O11—Cs1^ii	96.80 (13)
O12^vii—Cs1—O5^v	131.32 (10)	P4—O12—La1^x	155.6 (3)
O4—Cs1—O5^v	70.60 (9)	P4—O12—Cs1^xii	96.5 (2)
O6^v—Cs1—O11^v	65.60 (11)	La1^x—O12—Cs1^xii	106.89 (15)

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