Literature DB >> 21202438

The alluaudite-like arsenate NaCaMg(3)(AsO(4))(3).

Abstract

The title compound, sodium calcium trimagnesium tris-(arsenate), an alluaudite-like arsenate, was prepared by solid-state reaction at high temperature. The structure is built up from edge-sharing MgO(6) octa-hedra in chains associated with the AsO(4) arsenate groups. The three-dimensional network leads to two different tunnels occupied statistically by Na(+) and Ca(2+). One As and one Mg atom lie on twofold rotation axes; one Na and one Ca are disordered over two sites with occupancies of 0.7 and 0.3 and these sites lie on a twofold rotation axis and an inversion centre, respectively.

Entities: CellLine Chemical Disease Gene

Year: 2008 PMID： 21202438 PMCID： PMC2961449 DOI： 10.1107/S1600536808014633

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For the alluaudite structure type, see: Moore (1971 ▶); Yakubovitch et al. (1977 ▶); Cu1.35Fe(PO4)3 (Warner et al., 1993 ▶); NaFe3.67(PO4)3 (Korzenski et al., 1998 ▶). For related alluaudite-like arsenates, see: NaCo3(AsO4)(HAsO4)2 (Kwang-Hwa & Pei-Fen, 1994 ▶); NaCaCdMg2(AsO4)3 (Khorari et al., 1997 ▶); Ag1.49Mn1.49Mn2(AsO4)3 (Ayed et al., 2002 ▶); Na1.72 Mn3.28(AsO4)3 (Brahim et al. 2003 ▶). For related literature, see: Leroux et al. (1995 ▶).

Experimental

Crystal data

NaCaMg3(AsO4)3 M = 552.74 Monoclinic, a = 11.880 (1) Å b = 12.817 (1) Å c = 6.741 (2) Å β = 112.45 (1)° V = 948.7 (3) Å3 Z = 4 Mo Kα radiation μ = 11.36 mm−1 T = 293 (2) K 0.6 × 0.2 × 0.15 mm

Data collection

Enraf–Nonius CAD-4 diffractometer Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.110, T max = 0.180 1358 measured reflections 1154 independent reflections 1133 reflections with I > 2σ(I) R int = 0.021 2 standard reflections frequency: 120 min intensity decay: 0.4%

Refinement

R[F 2 > 2σ(F 2)] = 0.022 wR(F 2) = 0.060 S = 1.29 1154 reflections 100 parameters Δρmax = 0.99 e Å−3 Δρmin = −1.00 e Å−3 Data collection: CAD-4 EXPRESS (Duisenberg, 1992 ▶; Macíček & Yordanov, 1992 ▶); cell refinement: CAD-4 EXPRESS; data reduction: MolEN (Fair, 1990 ▶); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1998 ▶); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808014633/br2069sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808014633/br2069Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

NaCaMg₃(AsO₄)₃	F₀₀₀ = 1048
M_r = 552.74	D_x = 3.870 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 25 reflections
a = 11.880 (1) Å	θ = 2.4–28º
b = 12.817 (1) Å	µ = 11.36 mm⁻¹
c = 6.741 (2) Å	T = 293 (2) K
β = 112.45 (1)º	Prismatic, colourless
V = 948.7 (3) Å³	0.6 × 0.2 × 0.15 mm
Z = 4

Enraf–Nonius CAD-4 diffractometer	R_int = 0.021
Radiation source: fine-focus sealed tube	θ_max = 28.0º
Monochromator: graphite	θ_min = 2.4º
T = 293(2) K	h = −15→14
ω/2θ scans	k = −1→16
Absorption correction: ψ scan(North et al., 1968)	l = 0→8
T_min = 0.110, T_max = 0.180	2 standard reflections
1358 measured reflections	every 120 min
1154 independent reflections	intensity decay: 0.4%
1133 reflections with I > 2σ(I)

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0244P)² + 8.0874P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.022	(Δ/σ)_max < 0.001
wR(F²) = 0.060	Δρ_max = 0.99 e Å⁻³
S = 1.29	Δρ_min = −1.00 e Å⁻³
1154 reflections	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
100 parameters	Extinction coefficient: 0.0071 (4)
Primary atom site location: structure-invariant direct methods

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.

	x	y	z	U_iso*/U_eq	Occ. (<1)
As1	0.26904 (3)	0.38625 (2)	0.37969 (5)	0.00207 (13)
As2	0.5000	0.21057 (3)	0.2500	0.00248 (14)
Mg1	0.5000	0.23783 (13)	0.7500	0.0043 (3)
Mg2	0.78584 (10)	0.15824 (9)	0.37643 (18)	0.0030 (2)
Na1	0.5000	0.511 (3)	0.7500	0.019 (2)	0.70
Ca1	0.5000	0.523 (3)	0.7500	0.019 (2)	0.30
Ca2	0.5000	0.0000	0.0000	0.0132 (3)	0.70
Na2	0.5000	0.0000	0.0000	0.0132 (3)	0.30
O1	0.4635 (2)	0.28350 (19)	0.0247 (4)	0.0063 (5)
O2	0.2837 (2)	0.31609 (19)	0.1792 (4)	0.0061 (5)
O3	0.3415 (2)	0.32937 (19)	0.6218 (4)	0.0053 (5)
O4	0.1175 (2)	0.39767 (19)	0.3197 (4)	0.0074 (5)
O5	0.6086 (2)	0.1221 (2)	0.2626 (4)	0.0105 (5)
O6	0.3381 (2)	0.50307 (19)	0.3963 (4)	0.0082 (5)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
As1	0.00076 (18)	0.00152 (19)	0.00403 (19)	0.00028 (10)	0.00101 (12)	0.00027 (10)
As2	0.0017 (2)	0.0013 (2)	0.0040 (2)	0.000	0.00054 (16)	0.000
Mg1	0.0020 (7)	0.0036 (7)	0.0080 (7)	0.000	0.0027 (6)	0.000
Mg2	0.0021 (5)	0.0022 (5)	0.0053 (5)	0.0000 (4)	0.0022 (4)	−0.0001 (4)
Na1	0.0091 (8)	0.035 (7)	0.0131 (8)	0.000	0.0032 (7)	0.000
Ca1	0.0091 (8)	0.035 (7)	0.0131 (8)	0.000	0.0032 (7)	0.000
Ca2	0.0161 (6)	0.0036 (5)	0.0107 (5)	−0.0026 (4)	−0.0051 (5)	−0.0003 (4)
Na2	0.0161 (6)	0.0036 (5)	0.0107 (5)	−0.0026 (4)	−0.0051 (5)	−0.0003 (4)
O1	0.0039 (11)	0.0094 (11)	0.0060 (11)	0.0020 (9)	0.0022 (9)	0.0025 (9)
O2	0.0080 (11)	0.0064 (11)	0.0045 (11)	0.0004 (9)	0.0031 (9)	−0.0010 (8)
O3	0.0050 (10)	0.0072 (11)	0.0033 (11)	0.0043 (9)	0.0010 (8)	0.0022 (8)
O4	0.0006 (10)	0.0065 (11)	0.0142 (12)	0.0005 (8)	0.0016 (9)	0.0000 (9)
O5	0.0034 (11)	0.0071 (11)	0.0169 (13)	0.0038 (9)	−0.0007 (9)	−0.0040 (9)
O6	0.0089 (11)	0.0022 (10)	0.0138 (12)	−0.0025 (9)	0.0047 (10)	−0.0007 (9)

As1—O2	1.687 (2)	Na1—O1^ix	2.99 (3)
As1—O6	1.690 (2)	Na1—O1^viii	2.99 (3)
As1—O3	1.692 (2)	Ca1—O6	2.439 (5)
As1—O4	1.694 (2)	Ca1—O6ⁱⁱ	2.439 (5)
As2—O1ⁱ	1.693 (2)	Ca1—O6^viii	2.497 (6)
As2—O1	1.693 (2)	Ca1—O6^ix	2.497 (6)
As2—O5ⁱ	1.695 (2)	Ca1—O1^ix	2.85 (4)
As2—O5	1.695 (2)	Ca1—O1^viii	2.85 (4)
Mg1—O3ⁱⁱ	2.104 (2)	Ca1—O3	3.04 (4)
Mg1—O3	2.104 (2)	Ca1—O3ⁱⁱ	3.04 (4)
Mg1—O1ⁱⁱⁱ	2.139 (2)	Ca2—O5	2.346 (3)
Mg1—O1ⁱ	2.139 (2)	Ca2—O5^x	2.346 (3)
Mg1—O4^iv	2.164 (3)	Ca2—O4^vii	2.453 (3)
Mg1—O4^v	2.164 (3)	Ca2—O4^xi	2.453 (3)
Mg2—O5	2.001 (3)	Ca2—O4^xii	2.538 (3)
Mg2—O3^vi	2.068 (3)	Ca2—O4^vi	2.538 (3)
Mg2—O6^vii	2.072 (3)	Ca2—O5ⁱ	2.872 (3)
Mg2—O2^v	2.077 (3)	Ca2—O5^xiii	2.872 (3)
Mg2—O1^v	2.098 (3)	Na2—O5	2.346 (3)
Mg2—O2ⁱ	2.163 (3)	Na2—O5^x	2.346 (3)
Na1—O6	2.428 (3)	Na2—O4^vii	2.453 (3)
Na1—O6ⁱⁱ	2.428 (3)	Na2—O4^xi	2.453 (3)
Na1—O6^viii	2.481 (4)	Na2—O4^xii	2.538 (3)
Na1—O6^ix	2.481 (4)	Na2—O4^vi	2.538 (3)
Na1—O3	2.91 (3)	Na2—O5ⁱ	2.872 (3)
Na1—O3ⁱⁱ	2.91 (3)	Na2—O5^xiii	2.872 (3)

O2—As1—O6	109.24 (12)	O6—Ca1—O6^ix	92.2 (3)
O2—As1—O3	111.91 (11)	O6ⁱⁱ—Ca1—O6^ix	86.1 (2)
O6—As1—O3	105.22 (12)	O6—Ca1—O1^ix	121.1 (13)
O2—As1—O4	106.26 (12)	O6ⁱⁱ—Ca1—O1^ix	70.7 (6)
O6—As1—O4	112.57 (12)	O6^viii—Ca1—O1^ix	83.7 (7)
O3—As1—O4	111.73 (12)	O6^ix—Ca1—O1^ix	110.2 (10)
O1ⁱ—As2—O1	112.96 (17)	O6—Ca1—O1^viii	70.7 (6)
O1ⁱ—As2—O5ⁱ	110.10 (13)	O6ⁱⁱ—Ca1—O1^viii	121.1 (13)
O1—As2—O5ⁱ	113.27 (12)	O6^viii—Ca1—O1^viii	110.2 (10)
O1ⁱ—As2—O5	113.27 (12)	O6^ix—Ca1—O1^viii	83.7 (7)
O1—As2—O5	110.10 (13)	O6ⁱⁱ—Ca1—O3	111.3 (13)
O5ⁱ—As2—O5	96.04 (18)	O6^viii—Ca1—O3	60.9 (6)
O3ⁱⁱ—Mg1—O3	112.20 (15)	O6^ix—Ca1—O3	105.3 (12)
O3ⁱⁱ—Mg1—O1ⁱⁱⁱ	86.41 (10)	O6—Ca1—O3ⁱⁱ	111.3 (13)
O3—Mg1—O1ⁱⁱⁱ	75.96 (9)	O6^viii—Ca1—O3ⁱⁱ	105.3 (12)
O3ⁱⁱ—Mg1—O1ⁱ	75.96 (9)	O6^ix—Ca1—O3ⁱⁱ	60.9 (6)
O3—Mg1—O1ⁱ	86.41 (10)	O3—Ca1—O3ⁱⁱ	70.2 (9)
O3—Mg1—O4^iv	87.51 (9)	O5—Ca2—O4^vii	74.30 (9)
O1ⁱⁱⁱ—Mg1—O4^iv	94.61 (10)	O5^x—Ca2—O4^vii	105.70 (9)
O1ⁱ—Mg1—O4^iv	111.02 (10)	O5—Ca2—O4^xi	105.70 (9)
O3ⁱⁱ—Mg1—O4^v	87.51 (9)	O5^x—Ca2—O4^xi	74.30 (9)
O3—Mg1—O4^v	159.81 (11)	O5—Ca2—O4^xii	103.17 (9)
O1ⁱⁱⁱ—Mg1—O4^v	111.02 (10)	O5^x—Ca2—O4^xii	76.83 (9)
O1ⁱ—Mg1—O4^v	94.61 (10)	O4^vii—Ca2—O4^xii	62.31 (10)
O4^iv—Mg1—O4^v	73.28 (14)	O4^xi—Ca2—O4^xii	117.69 (10)
O5—Mg2—O3^vi	108.84 (12)	O5—Ca2—O4^vi	76.83 (9)
O5—Mg2—O6^vii	92.76 (11)	O5^x—Ca2—O4^vi	103.17 (9)
O3^vi—Mg2—O6^vii	86.82 (11)	O4^vii—Ca2—O4^vi	117.69 (10)
O5—Mg2—O2^v	90.41 (11)	O4^xi—Ca2—O4^vi	62.31 (10)
O6^vii—Mg2—O2^v	101.79 (11)	O5—Ca2—O5ⁱ	56.66 (10)
O3^vi—Mg2—O1^v	77.62 (10)	O4^vii—Ca2—O5ⁱ	91.59 (8)
O6^vii—Mg2—O1^v	95.10 (11)	O4^xi—Ca2—O5ⁱ	88.41 (8)
O2^v—Mg2—O1^v	82.14 (10)	O4^xii—Ca2—O5ⁱ	64.46 (7)
O5—Mg2—O2ⁱ	82.74 (10)	O4^vi—Ca2—O5ⁱ	115.54 (7)
O3^vi—Mg2—O2ⁱ	90.36 (10)	O5^x—Ca2—O5^xiii	56.66 (10)
O2^v—Mg2—O2ⁱ	82.81 (10)	O4^vii—Ca2—O5^xiii	88.41 (8)
O1^v—Mg2—O2ⁱ	89.86 (10)	O4^xi—Ca2—O5^xiii	91.59 (8)
O6—Na1—O6^viii	86.76 (12)	O4^xii—Ca2—O5^xiii	115.54 (7)
O6ⁱⁱ—Na1—O6^viii	92.89 (13)	O4^vi—Ca2—O5^xiii	64.46 (7)
O6—Na1—O6^ix	92.89 (13)	O5—Na2—O4^vii	74.30 (9)
O6ⁱⁱ—Na1—O6^ix	86.76 (12)	O5^x—Na2—O4^vii	105.70 (9)
O6—Na1—O3	59.6 (5)	O5—Na2—O4^xi	105.70 (9)
O6ⁱⁱ—Na1—O3	116.0 (11)	O5^x—Na2—O4^xi	74.30 (9)
O6^viii—Na1—O3	63.1 (5)	O5—Na2—O4^xii	103.17 (9)
O6^ix—Na1—O3	109.6 (10)	O5^x—Na2—O4^xii	76.83 (9)
O6—Na1—O3ⁱⁱ	116.0 (11)	O4^vii—Na2—O4^xii	62.31 (10)
O6^viii—Na1—O3ⁱⁱ	109.6 (10)	O4^xi—Na2—O4^xii	117.69 (10)
O6^ix—Na1—O3ⁱⁱ	63.1 (5)	O5—Na2—O4^vi	76.83 (9)
O3—Na1—O3ⁱⁱ	73.7 (8)	O5^x—Na2—O4^vi	103.17 (9)
O6—Na1—O1^ix	116.3 (11)	O4^vii—Na2—O4^vi	117.69 (10)
O6ⁱⁱ—Na1—O1^ix	68.4 (5)	O4^xi—Na2—O4^vi	62.31 (10)
O6^viii—Na1—O1^ix	81.2 (6)	O4^vii—Na2—O5ⁱ	91.59 (8)
O6^ix—Na1—O1^ix	106.4 (9)	O4^xi—Na2—O5ⁱ	88.41 (8)
O6—Na1—O1^viii	68.4 (5)	O4^xii—Na2—O5ⁱ	64.46 (7)
O6ⁱⁱ—Na1—O1^viii	116.3 (11)	O4^vi—Na2—O5ⁱ	115.54 (7)
O6^viii—Na1—O1^viii	106.4 (9)	O4^vii—Na2—O5^xiii	88.41 (8)
O6^ix—Na1—O1^viii	81.2 (6)	O4^xi—Na2—O5^xiii	91.59 (8)
O6—Ca1—O6^viii	86.1 (2)	O4^xii—Na2—O5^xiii	115.54 (7)
O6ⁱⁱ—Ca1—O6^viii	92.2 (3)	O4^vi—Na2—O5^xiii	64.46 (7)

2 in total

2. Structural features of two novel alluaudite-like arsenates Cd_1.16Zn_2.34(AsO₄)_1.5(HAsO₄)(H₂AsO₄)_0.5 and Cd_0.74Mg_2.76(AsO₄)_1.5(HAsO₄)(H₂AsO₄)_0.5.

Authors: Jovica Stojanović; Tamara Dorđević; Ljiljana Karanović
Journal: J Alloys Compd Date: 2012-04-15 Impact factor: 5.316

2 in total

The alluaudite-like arsenate NaCaMg(3)(AsO(4))(3).

Related literature

Experimental

Crystal data

Data collection

Refinement

1. A short history of SHELX.

2. Na(1.72)Mn(3.2)8(AsO(4))(3).

1. Structure cristalline de type alluaudite K0.4Na3.6Co(MoO4)3.

2. Structural features of two novel alluaudite-like arsenates Cd_1.16Zn_2.34(AsO₄)_1.5(HAsO₄)(H₂AsO₄)_0.5 and Cd_0.74Mg_2.76(AsO₄)_1.5(HAsO₄)(H₂AsO₄)_0.5.

The alluaudite-like arsenate NaCaMg(3)(AsO(4))(3).

Related literature

Experimental

Crystal data

Data collection

Refinement

1. A short history of SHELX.

2. Na(1.72)Mn(3.2)8(AsO(4))(3).

1. Structure cristalline de type alluaudite K0.4Na3.6Co(MoO4)3.

2. Structural features of two novel alluaudite-like arsenates Cd1.16Zn2.34(AsO4)1.5(HAsO4)(H2AsO4)0.5 and Cd0.74Mg2.76(AsO4)1.5(HAsO4)(H2AsO4)0.5.

2. Structural features of two novel alluaudite-like arsenates Cd_1.16Zn_2.34(AsO₄)_1.5(HAsO₄)(H₂AsO₄)_0.5 and Cd_0.74Mg_2.76(AsO₄)_1.5(HAsO₄)(H₂AsO₄)_0.5.