Redetermination of tricalcium trilanthanum penta­kis(ortho­borate) from single-crystal data

Zhou, T.; Ye, N.

doi:10.1107/S1600536808014785

inorganic compounds

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Volume 64| Part 6| June 2008| Page i37

doi:10.1107/S1600536808014785

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Redetermination of tricalcium trilanthanum pentakis(orthoborate) from single-crystal data

Tianyong Zhou ^a and Ning Ye ^a ^*

^aFujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, People's Republic of China
^*Correspondence e-mail: nye@fjirsm.ac.cn

(Received 30 April 2008; accepted 15 May 2008; online 21 May 2008)

Single crystals of the title compound, Ca₃La₃(BO₃)₅, were obtained by spontaneous nucleation from a high-temperature melt. The crystal structure of Ca₃La₃(BO₃)₅ has been determined previously from X-ray powder data [Zhang, Liang, Chen, He & Xu (2001). J. Alloys Compd, 327, 96–99]. The present refinement shows a significant improvement in terms of the precision of the geometric parameters and the correct determination of the absolute configuration in space group P6₃mc with all atoms refined with anisotropic displacement parameters. The structure consists of isolated BO₃ triangles and distorted [CaO₈] and [LaO₁₀] polyhedra. Except for one O atom, all other atoms are situated on special positions: La, all O and one B atom on mirror planes, and two B atoms with site symmetry 3m.

Related literature

For phase equilibria in the system La₂O₃—CaO—B₂O₃, see: Zhang et al. (2001a ). For a previous structure analysis of Ca₃La₃(BO₃)₅ based on X-ray powder diffraction data, see: Zhang et al. (2001b ). For non-linear optical (NLO) applications of borate crystals containing triangular BO₃ anions, see: Chen et al. (1999 ). For a review of the geometry of the BO₃ group, see: Zobetz (1982 ). For the potential applications of Ca₃La₃(BO₃)₅ for photoluminescence, see: Zhang et al. (2005 ); Han et al. (2007 ).

Experimental

Crystal data

Ca₃La₃(BO₃)₅
M_r = 831.02
Hexagonal, P 6₃ m c
a = 10.530 (3) Å
c = 6.398 (2) Å
V = 614.4 (3) Å³
Z = 2
Mo Kα radiation
μ = 11.59 mm⁻¹
T = 293 (2) K
0.22 × 0.12 × 0.10 mm

Data collection

Rigaku Mercury CCD diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2000 ) T_min = 0.206, T_max = 0.304
4065 measured reflections
534 independent reflections
534 reflections with I > 2σ(I)
R_int = 0.035

Refinement

R[F² > 2σ(F²)] = 0.012
wR(F²) = 0.030
S = 0.89
534 reflections
53 parameters
1 restraint
Δρ_max = 0.41 e Å⁻³
Δρ_min = −0.59 e Å⁻³
Absolute structure: Flack (1983 ), 236 Friedel pairs
Flack parameter: −0.03 (3)

Table 1
Selected geometric parameters (Å, °)

Ca1—O4ⁱ	2.3139 (13)
Ca1—O1ⁱⁱ	2.376 (3)
Ca1—O3	2.382 (4)
Ca1—O1ⁱⁱⁱ	2.662 (3)
La1—O1^iv	2.501 (2)
La1—O4^v	2.516 (4)
La1—O2^vi	2.6639 (15)
La1—O3^vii	2.8112 (8)
B1—O4	1.358 (6)
B1—O1ⁱ	1.384 (3)
B2—O2^viii	1.374 (3)
B3—O3	1.389 (3)

O4—B1—O1ⁱ	119.7 (2)
O1ⁱ—B1—O1^x	120.6 (4)
O2^viii—B2—O2^xi	120
O3^ix—B3—O3	120
Symmetry codes: (i) -y+1, x-y+1, z; (ii) $[x-y+1, x, z+{\script{1\over 2}}]$ ; (iii) -x+y, -x+1, z; (iv) $[y-1, x, z-{\script{1\over 2}}]$ ; (v) x, y, z-1; (vi) $[x-y+1, x+1, z-{\script{1\over 2}}]$ ; (vii) $[x-y, x, z-{\script{1\over 2}}]$ ; (viii) $[y-1, -x+y-1, z-{\script{1\over 2}}]$ ; (ix) -x+y+1, -x+1, z; (x) -x+y, y, z; (xi) $[x-y+1, x, z-{\script{1\over 2}}]$ .

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2004 ); software used to prepare material for publication: enCIFer (Allen et al., 2004 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808014785/wm2179sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808014785/wm2179Isup2.hkl

checkCIF report

Comment top

Borate crystals containing parallel aligned BO₃ anions are predicted to have large nonlinear optical (NLO) coefficients, moderate birefringence and wide transparency in the UV-region. Therefore they are considered to be good candidates for NLO applications (Chen, 1999). The title compound Ca₃La₃(BO₃)₅, (I), has been investigated previously by Zhang et al. (2001a) during analysis of phase equilibria in the system La₂O₃—CaO—B₂O₃, and NLO and luminescent properties of this material have also been reported (Zhang, 2005; Han, 2007). The crystal structure of Ca₃La₃ (BO₃)₅ was originally determined from X-ray powder diffraction data in conjunction with IR spectroscopy (Zhang et al., 2001b).

The structure of compound (I) can be described in terms of BO₃ triangles and complex irregular [CaO₈] and [LaO₁₀] polyhedra. Each of the three crystallographically different B atoms is coordinated to three O atoms to form planar BO₃ triangles. The B—O bond lengths range from 1.384 (3) to 1.389 (3) Å, which is in good agreement with the results of geometric studies of the BO₃ unit (Zobetz, 1982). Two of the three BO₃ groups exhibit 3m symmetry, and the third BO₃ group has m symmetry with O–B–O angles very close to 120°. The La³⁺ cations are 10-fold coordinated by oxygen atoms with La—O bond lengths ranging from 2.501 (2) to 2.812 (2) Å. The [LaO₁₀] polyhedra are connected to each other and to the borate groups by sharing corners and edges forming a three-dimensional network with channels running parallel to [001]. In these channels the Ca²⁺ cations are situated and are surrounded by eight oxygen atoms with Ca—O bond lengths ranging from 2.3139 (13) to 2.662 (3) Å (Table 1).

Related literature top

For phase equilibria in the system La₂O₃—CaO—B₂O₃, see: Zhang et al. (2001a). For a previous structure analysis of Ca₃La₃(BO₃)₅ based on X-ray powder diffraction data, see: Zhang et al. (2001b). For non-linear optical (NLO) applications of borate crystals containing triangular BO₃ anions, see: Chen et al. (1999). For a review of the geometry of the BO₃ group, see: Zobetz (1982). Fo the potential applications of Ca₃La₃(BO₃)₅ for photoluminescence, see: Zhang et al. (2005); Han et al. (2007).

Experimental top

Single crystals of compound (I) were grown using a LiBO₂-containing flux. The composition of the mixture for crystal growth was 1:1:4:3 of CaCO₃ (Sinopharm Regent, AR), La₂O₃ (Materials, 99.8%), H₃BO₃ (Sinopharm Regent, 99.99%), and Li₂CO₃ (Sinopharm Reagent, AR). The mixture was heated in a platinum crucible to 1373 K, held at this temperature for several hours, and then cooled at a rate of 10 K/h from 1373 to 873 K. The remaining solified flux attached to the crystals was readily dissolved in water. Crystals with an average size of 0.5 mm and mostly rod shaped habit were obtained.

Computing details top

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear (Rigaku, 2000); data reduction: CrystalClear (Rigaku, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2004); software used to prepare material for publication: enCIFer (Allen et al., 2004).

Figures top

	Fig. 1. The structure of (I) in a projection approximatly along the [001] direction with displacement ellipsoids drawn at the 85% probability level.
	Fig. 2. Packing diagram of the structure of (I). [CaO₈] polyhedra are yellow, [LaO₁₀] polyhedra are blue and [BO₃] units are green.

tricalcium trilanthanum pentakis(orthoborate) top

Crystal data top

Ca₃La₃(BO₃)₅	D_x = 4.492 Mg m⁻³
M_r = 831.02	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₃mc	Cell parameters from 1909 reflections
Hall symbol: P 6c -2c	θ = 2.2–27.5°
a = 10.530 (3) Å	µ = 11.59 mm⁻¹
c = 6.398 (2) Å	T = 293 K
V = 614.4 (3) Å³	Rod, colourless
Z = 2	0.22 × 0.12 × 0.10 mm
F(000) = 752

Data collection top

Rigaku Mercury CCD diffractometer	534 independent reflections
Radiation source: Sealed Tube	534 reflections with I > 2σ(I)
Graphite Monochromator monochromator	R_int = 0.035
Detector resolution: 14.6306 pixels mm^-1	θ_max = 27.5°, θ_min = 2.2°
CCD_Profile_fitting scans	h = −13→13
Absorption correction: multi-scan (CrystalClear; Rigaku, 2000)	k = −13→13
T_min = 0.206, T_max = 0.304	l = −8→7
4065 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.02P)² + 1.5843P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.012	(Δ/σ)_max < 0.001
wR(F²) = 0.030	Δρ_max = 0.41 e Å⁻³
S = 0.89	Δρ_min = −0.59 e Å⁻³
534 reflections	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
53 parameters	Extinction coefficient: 0.0632 (12)
1 restraint	Absolute structure: Flack (1983), 236 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.03 (3)

Crystal data top

Ca₃La₃(BO₃)₅	Z = 2
M_r = 831.02	Mo Kα radiation
Hexagonal, P6₃mc	µ = 11.59 mm⁻¹
a = 10.530 (3) Å	T = 293 K
c = 6.398 (2) Å	0.22 × 0.12 × 0.10 mm
V = 614.4 (3) Å³

Data collection top

Rigaku Mercury CCD diffractometer	534 independent reflections
Absorption correction: multi-scan (CrystalClear; Rigaku, 2000)	534 reflections with I > 2σ(I)
T_min = 0.206, T_max = 0.304	R_int = 0.035
4065 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.012	1 restraint
wR(F²) = 0.030	Δρ_max = 0.41 e Å⁻³
S = 0.89	Δρ_min = −0.59 e Å⁻³
534 reflections	Absolute structure: Flack (1983), 236 Friedel pairs
53 parameters	Absolute structure parameter: −0.03 (3)

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Ca1	0.47334 (5)	0.52666 (5)	0.76261 (15)	0.00673 (19)
La1	0.156065 (12)	0.843935 (12)	0.08229 (8)	0.00493 (11)
B1	0.1989 (3)	0.8011 (3)	0.5473 (8)	0.0049 (10)
B2	0	0	0.2435 (15)	0.0086 (17)
B3	0.6667	0.3333	0.598 (3)	0.0092 (19)
O1	0.6272 (3)	0.9278 (2)	0.4462 (4)	0.0067 (5)
O2	0.07534 (16)	0.92466 (16)	0.7399 (6)	0.0097 (7)
O3	0.59052 (16)	0.40948 (16)	0.5984 (8)	0.0083 (6)
O4	0.22657 (17)	0.77343 (17)	0.7443 (5)	0.0066 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ca1	0.0060 (3)	0.0060 (3)	0.0073 (4)	0.0023 (3)	−0.0001 (2)	0.0001 (2)
La1	0.00442 (12)	0.00442 (12)	0.00474 (14)	0.00129 (9)	0.00003 (8)	−0.00003 (8)
B1	0.0052 (15)	0.0052 (15)	0.007 (3)	0.0044 (18)	−0.0006 (10)	0.0006 (10)
B2	0.011 (3)	0.011 (3)	0.003 (4)	0.0057 (13)	0	0
B3	0.009 (2)	0.009 (2)	0.009 (6)	0.0046 (11)	0	0
O1	0.0069 (10)	0.0056 (10)	0.0073 (11)	0.0029 (9)	−0.0014 (10)	0.0016 (9)
O2	0.0090 (12)	0.0090 (12)	0.0124 (16)	0.0055 (14)	−0.0005 (7)	0.0005 (7)
O3	0.0101 (10)	0.0101 (10)	0.0067 (17)	0.0065 (11)	0.0005 (9)	−0.0005 (9)
O4	0.0067 (11)	0.0067 (11)	0.0055 (16)	0.0026 (13)	−0.0014 (7)	0.0014 (7)

Geometric parameters (Å, º) top

Ca1—O4ⁱ	2.3139 (13)	La1—O1ⁱ	2.678 (3)
Ca1—O4ⁱⁱ	2.3139 (13)	La1—O3^xiv	2.8112 (8)
Ca1—O1ⁱⁱⁱ	2.376 (3)	La1—O3^xv	2.8112 (8)
Ca1—O1^iv	2.376 (3)	La1—B2^xvi	3.028 (3)
Ca1—O3	2.382 (4)	La1—B1	3.076 (5)
Ca1—O3^v	2.444 (5)	B1—O4	1.358 (6)
Ca1—O1ⁱⁱ	2.662 (3)	B1—O1ⁱ	1.384 (3)
Ca1—O1^vi	2.662 (3)	B1—O1^xiii	1.384 (3)
Ca1—B1ⁱ	2.858 (4)	B1—Ca1ⁱ	2.858 (4)
Ca1—B1ⁱⁱ	2.858 (4)	B1—Ca1ⁱⁱ	2.858 (4)
Ca1—Ca1^v	3.3435 (11)	B2—O2^xvii	1.374 (3)
Ca1—Ca1^vii	3.3435 (11)	B2—O2^xviii	1.374 (3)
La1—O1^viii	2.501 (2)	B2—O2^xix	1.374 (3)
La1—O1^ix	2.501 (2)	B2—La1^xx	3.028 (3)
La1—O4^x	2.516 (4)	B2—La1ⁱ	3.028 (3)
La1—O2^x	2.639 (3)	B2—La1^xxi	3.028 (3)
La1—O2^xi	2.6639 (15)	B3—O3^xxii	1.389 (3)
La1—O2^xii	2.6639 (15)	B3—O3^xxiii	1.389 (3)
La1—O1^xiii	2.678 (3)	B3—O3	1.389 (3)

O4ⁱ—Ca1—O4ⁱⁱ	93.58 (15)	O1^ix—La1—O3^xiv	116.83 (10)
O4ⁱ—Ca1—O1ⁱⁱⁱ	151.80 (11)	O4^x—La1—O3^xiv	64.52 (12)
O4ⁱⁱ—Ca1—O1ⁱⁱⁱ	80.01 (9)	O2^x—La1—O3^xiv	122.29 (12)
O4ⁱ—Ca1—O1^iv	80.01 (9)	O2^xi—La1—O3^xiv	155.42 (13)
O4ⁱⁱ—Ca1—O1^iv	151.80 (11)	O2^xii—La1—O3^xiv	121.81 (10)
O1ⁱⁱⁱ—Ca1—O1^iv	92.72 (12)	O1^xiii—La1—O3^xiv	88.50 (10)
O4ⁱ—Ca1—O3	126.18 (10)	O1ⁱ—La1—O3^xiv	65.77 (12)
O4ⁱⁱ—Ca1—O3	126.18 (10)	O1^viii—La1—O3^xv	116.83 (9)
O1ⁱⁱⁱ—Ca1—O3	77.64 (10)	O1^ix—La1—O3^xv	69.51 (8)
O1^iv—Ca1—O3	77.64 (10)	O4^x—La1—O3^xv	64.52 (12)
O4ⁱ—Ca1—O3^v	73.69 (10)	O2^x—La1—O3^xv	122.29 (12)
O4ⁱⁱ—Ca1—O3^v	73.69 (10)	O2^xi—La1—O3^xv	121.81 (10)
O1ⁱⁱⁱ—Ca1—O3^v	78.17 (9)	O2^xii—La1—O3^xv	155.42 (13)
O1^iv—Ca1—O3^v	78.17 (9)	O1^xiii—La1—O3^xv	65.77 (12)
O3—Ca1—O3^v	144.65 (19)	O1ⁱ—La1—O3^xv	88.50 (10)
O4ⁱ—Ca1—O1ⁱⁱ	56.39 (9)	O3^xiv—La1—O3^xv	50.66 (12)
O4ⁱⁱ—Ca1—O1ⁱⁱ	112.85 (10)	O4—B1—O1ⁱ	119.7 (2)
O1ⁱⁱⁱ—Ca1—O1ⁱⁱ	151.00 (8)	O4—B1—O1^xiii	119.7 (2)
O1^iv—Ca1—O1ⁱⁱ	86.53 (8)	O1ⁱ—B1—O1^xiii	120.6 (4)
O3—Ca1—O1ⁱⁱ	73.88 (10)	O2^xvii—B2—O2^xviii	120.00 (1)
O3^v—Ca1—O1ⁱⁱ	129.62 (7)	O2^xvii—B2—O2^xix	120.00 (1)
O4ⁱ—Ca1—O1^vi	112.85 (10)	O2^xviii—B2—O2^xix	120.00 (1)
O4ⁱⁱ—Ca1—O1^vi	56.39 (9)	O3^xxii—B3—O3^xxiii	120.00 (1)
O1ⁱⁱⁱ—Ca1—O1^vi	86.53 (8)	O3^xxii—B3—O3	120.00 (1)
O1^iv—Ca1—O1^vi	151.00 (8)	O3^xxiii—B3—O3	120.00 (1)
O3—Ca1—O1^vi	73.88 (10)	B1ⁱⁱ—O1—Ca1^xv	147.6 (3)
O3^v—Ca1—O1^vi	129.62 (7)	B1ⁱⁱ—O1—La1^xxiv	114.0 (3)
O1ⁱⁱ—Ca1—O1^vi	80.50 (11)	Ca1^xv—O1—La1^xxiv	94.81 (8)
O1^viii—La1—O1^ix	138.96 (12)	B1ⁱⁱ—O1—Ca1ⁱ	83.5 (2)
O1^viii—La1—O4^x	73.88 (6)	Ca1^xv—O1—Ca1ⁱ	82.95 (8)
O1^ix—La1—O4^x	73.88 (6)	La1^xxiv—O1—Ca1ⁱ	87.75 (8)
O1^viii—La1—O2^x	71.80 (6)	B1ⁱⁱ—O1—La1ⁱⁱ	92.9 (2)
O1^ix—La1—O2^x	71.80 (6)	Ca1^xv—O1—La1ⁱⁱ	89.98 (9)
O4^x—La1—O2^x	64.64 (11)	La1^xxiv—O1—La1ⁱⁱ	111.47 (9)
O1^viii—La1—O2^xi	121.07 (8)	Ca1ⁱ—O1—La1ⁱⁱ	160.08 (10)
O1^ix—La1—O2^xi	71.30 (9)	B2^xxv—O2—La1^xxvi	123.0 (5)
O4^x—La1—O2^xi	137.71 (9)	B2^xxv—O2—La1^xxvii	91.42 (19)
O2^x—La1—O2^xi	82.07 (7)	La1^xxvi—O2—La1^xxvii	107.69 (7)
O1^viii—La1—O2^xii	71.30 (9)	B2^xxv—O2—La1^xxviii	91.42 (19)
O1^ix—La1—O2^xii	121.07 (8)	La1^xxvi—O2—La1^xxviii	107.69 (7)
O4^x—La1—O2^xii	137.71 (9)	La1^xxvii—O2—La1^xxviii	135.45 (14)
O2^x—La1—O2^xii	82.07 (7)	B3—O3—Ca1	154.0 (8)
O2^xi—La1—O2^xii	53.07 (13)	B3—O3—Ca1^vii	118.3 (8)
O1^viii—La1—O1^xiii	137.03 (9)	Ca1—O3—Ca1^vii	87.71 (10)
O1^ix—La1—O1^xiii	83.72 (6)	B3—O3—La1^xxix	94.64 (7)
O4^x—La1—O1^xiii	129.92 (8)	Ca1—O3—La1^xxix	86.76 (7)
O2^x—La1—O1^xiii	146.79 (6)	Ca1^vii—O3—La1^xxix	85.94 (9)
O2^xi—La1—O1^xiii	68.76 (8)	B3—O3—La1ⁱⁱⁱ	94.64 (7)
O2^xii—La1—O1^xiii	92.23 (9)	Ca1—O3—La1ⁱⁱⁱ	86.76 (7)
O1^viii—La1—O1ⁱ	83.72 (6)	Ca1^vii—O3—La1ⁱⁱⁱ	85.94 (9)
O1^ix—La1—O1ⁱ	137.03 (9)	La1^xxix—O3—La1ⁱⁱⁱ	169.80 (13)
O4^x—La1—O1ⁱ	129.92 (8)	B1—O4—Ca1ⁱⁱ	98.91 (12)
O2^x—La1—O1ⁱ	146.79 (6)	B1—O4—Ca1ⁱ	98.91 (12)
O2^xi—La1—O1ⁱ	92.23 (9)	Ca1ⁱⁱ—O4—Ca1ⁱ	145.78 (15)
O2^xii—La1—O1ⁱ	68.76 (8)	B1—O4—La1^xxvi	127.4 (3)
O1^xiii—La1—O1ⁱ	53.37 (10)	Ca1ⁱⁱ—O4—La1^xxvi	96.00 (9)
O1^viii—La1—O3^xiv	69.51 (8)	Ca1ⁱ—O4—La1^xxvi	96.00 (9)

Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x+y, −x+1, z; (iii) x−y+1, x, z+1/2; (iv) −x+1, −x+y, z+1/2; (v) −x+1, −y+1, z+1/2; (vi) x, x−y+1, z; (vii) −x+1, −y+1, z−1/2; (viii) y−1, x, z−1/2; (ix) −x+1, −y+2, z−1/2; (x) x, y, z−1; (xi) x−y+1, x+1, z−1/2; (xii) y−1, −x+y, z−1/2; (xiii) −x+y, y, z; (xiv) x−y, x, z−1/2; (xv) y, −x+y+1, z−1/2; (xvi) x, y+1, z; (xvii) y−1, −x+y−1, z−1/2; (xviii) x−y+1, x, z−1/2; (xix) −x, −y+1, z−1/2; (xx) −x+y−1, −x, z; (xxi) x, y−1, z; (xxii) −x+y+1, −x+1, z; (xxiii) −y+1, x−y, z; (xxiv) −x+1, −y+2, z+1/2; (xxv) −x, −y+1, z+1/2; (xxvi) x, y, z+1; (xxvii) y−1, −x+y, z+1/2; (xxviii) x−y+1, x+1, z+1/2; (xxix) y, −x+y, z+1/2.

Experimental details

Crystal data
Chemical formula	Ca₃La₃(BO₃)₅
M_r	831.02
Crystal system, space group	Hexagonal, P6₃mc
Temperature (K)	293
a, c (Å)	10.530 (3), 6.398 (2)
V (Å³)	614.4 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	11.59
Crystal size (mm)	0.22 × 0.12 × 0.10

Data collection
Diffractometer	Rigaku Mercury CCD diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2000)
T_min, T_max	0.206, 0.304
No. of measured, independent and observed [I > 2σ(I)] reflections	4065, 534, 534
R_int	0.035
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.012, 0.030, 0.89
No. of reflections	534
No. of parameters	53
No. of restraints	1
Δρ_max, Δρ_min (e Å⁻³)	0.41, −0.59
Absolute structure	Flack (1983), 236 Friedel pairs
Absolute structure parameter	−0.03 (3)

Computer programs: CrystalClear (Rigaku, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2004), enCIFer (Allen et al., 2004).

Selected geometric parameters (Å, º) top

Ca1—O4ⁱ	2.3139 (13)	La1—O3^vii	2.8112 (8)
Ca1—O1ⁱⁱ	2.376 (3)	B1—O4	1.358 (6)
Ca1—O3	2.382 (4)	B1—O1ⁱ	1.384 (3)
Ca1—O1ⁱⁱⁱ	2.662 (3)	B2—O2^viii	1.374 (3)
La1—O1^iv	2.501 (2)	B3—O3^ix	1.389 (3)
La1—O4^v	2.516 (4)	B3—O3	1.389 (3)
La1—O2^vi	2.6639 (15)

O4—B1—O1ⁱ	119.7 (2)	O2^viii—B2—O2^xi	120.00 (1)
O1ⁱ—B1—O1^x	120.6 (4)	O3^ix—B3—O3	120.00 (1)

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

Acknowledgements

This project was supported by the National Science Foundation of China (grant No. 60608018).

References

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