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inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 6| June 2012| Pages i40-i41
doi:10.1107/S1600536812018843

Wyllieite-type Ag1.09Mn3.46(AsO4)3

Wafa Frigui,a Mohamed Faouzi Zida* and Ahmed Drissa

aLaboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Université de Tunis ElManar, 2092 Manar II Tunis, Tunisia
*Correspondence e-mail: faouzi.zid@fst.rnu.tn

(Received 22 March 2012; accepted 26 April 2012; online 2 May 2012)

Single crystals of wyllieite-type silver(I) manganese(II) tris­orthoarsenate(V), Ag1.09Mn3.46(AsO4)3, were grown by a solid-state reaction. The three-dimensional framework is made up from four Mn2+/Mn3+ cations surrounded octa­hedrally by O atoms. The MnO6 octa­hedra are linked through edge- and corner-sharing. Three independent AsO4 tetra­hedra are linked to the framework through common corners, delimiting channels along [100] in which two partly occupied Ag+ sites reside, one on an inversion centre and with an occupancy of 0.631 (4), the other on a general site and with an occupancy of 0.774 (3), both within distorted tetra­hedral environments. One of the Mn sites is also located on an inversion centre and is partly occupied, with an occupancy of 0.916 (5). Related compounds with alluaudite-type or rosemaryite-type structures are compared and discussed.

Related literature

For background to framework structures with tetra­hedral and octa­hedral building units, see: Leclaire et al. (2002[Leclaire, A., Borel, M. M. & Raveau, B. (2002). J. Solid State Chem. 163, 534-539.]); Lii et al. (1990[Lii, K. H., Tsai, H. J. & Wang, S. L. (1990). J. Solid State Chem. 87, 396-401.]); Haddad et al. (1992[Haddad, A., Jouini, T. & Piffard, Y. (1992). Eur. J. Solid State Inorg. Chem. 29, 57-63.]); Hajji & Zid (2006[Hajji, M. & Zid, M. F. (2006). Acta Cryst. E62, i114-i116.]); Borel et al. (1997[Borel, M. M., Leclaire, A., Chardon, J., Provost, J., Rebbah, H. & Raveau, B. (1997). J. Solid State Chem. 132, 41-46.]); Masquelier et al. (1995[Masquelier, C., D'Yvoire, F. & Collin, G. (1995). J. Solid State Chem. 118, 33-42.]). For details of structural relationships with other compounds, see: Warner et al. (1993[Warner, T. E., Milius, W. & Maier, J. (1993). J. Solid State Chem. 106, 301-309.]); Korzenski et al. (1998[Korzenski, M. B., Schimek, G. L. & Kolis, J. W. (1998). J. Solid State Chem. 106, 301-309.]); Chouaibi et al. (2001[Chouaibi, N., Daidouh, A., Pico, C., Santrich, A. & Veiga, M. L. (2001). J. Solid State Chem. 159, 46-50.]); Pertlik (1987[Pertlik, F. (1987). Acta Cryst. C43, 381-383.]); Antenucci et al. (1995[Antenucci, D., Fransolet, A. M., Miehe, G. & Tarte, P. (1995). Eur. J. Mineral. 7, 175-179.]); Zid et al. (2005[Zid, M. F., Driss, A. & Jouini, T. (2005). Acta Cryst. E61, i46-i48.]); Ayed et al. (2004[Ayed, B., Abbdallah, A. H. & Hadded, A. (2004). Acta Cryst. E60, i52-i54.]); MacKay et al. (1996[MacKay, R., Wardojo, T. A. & Hwu, S.-J. (1996). J. Solid State Chem. 125, 255-260.]); Alvarez-Vega et al. (2006[Alvarez-Vega, M., Gallardo-Amores, J. M., Garcia-Alvarado, F. & Amador, U. (2006). Solid State Sci. 8, 952-957.]); Frigui et al. (2010[Frigui, W., Falah, C., Boughzala, H., Zid, M. F. & Driss, A. (2010). J. Soc. Chim. Tunis, 12, 179-188.], 2011a[Frigui, W., Falah, C., Ferhi, M., Zid, M. F. & Driss, A. (2011a). Ann. Chim. Sci. Mat. 36, 111-123.]); Hatert (2006[Hatert, F. (2006). Acta Cryst. C62, i1-i2.]); Moore & Ito (1973[Moore, P. B. & Ito, J. (1973). Mineral. Rec. 4, 131-136.], 1979[Moore, P. B. & Ito, J. (1979). Mineral. Mag. 43, 227-235.]); Yakubovich et al. (2005[Yakubovich, O. V., Massa, W., Gavrilenko, P. G. & Dimitrova, O. V. (2005). Eur. J. Mineral. 17, 741-747.]); Fransolet (1995[Fransolet, A.-M. (1995). Eur. J. Mineral. 7, 567-575.]); Moore & Molin-Case (1974[Moore, P. B. & Molin-Case, J. (1974). Am. Mineral. 59, 280-290.]). For preparative details, see: Frigui et al. (2010[Frigui, W., Falah, C., Boughzala, H., Zid, M. F. & Driss, A. (2010). J. Soc. Chim. Tunis, 12, 179-188.], 2011a[Frigui, W., Falah, C., Ferhi, M., Zid, M. F. & Driss, A. (2011a). Ann. Chim. Sci. Mat. 36, 111-123.],b[Frigui, W., Ben Amor, F., Zid, M. F. & Driss, A. (2011b). Jordan J. Chem. 6, 295-305.]). For the bond-valence method, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]).

Experimental

Crystal data

  • Ag1.09Mn3.46(AsO4)3

  • Mr = 724.02

  • Monoclinic, P 21 /c

  • a = 6.7470 (7) Å

  • b = 12.9820 (9) Å

  • c = 11.2970 (8) Å

  • β = 98.85 (3)°

  • V = 977.72 (17) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 16.64 mm−1

  • T = 298 K

  • 0.25 × 0.15 × 0.10 mm
Data collection

  • Enraf–Nonius CAD-4 diffractometer

  • Absorption correction: ψ scan (North et al., 1968[North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.]) Tmin = 0.071, Tmax = 0.210

  • 2522 measured reflections

  • 2138 independent reflections

  • 1704 reflections with I > 2σ(I)

  • Rint = 0.038

  • 2 standard reflections every 120 min intensity decay: 1.1%
Refinement

  • R[F2 > 2σ(F2)] = 0.032

  • wR(F2) = 0.098

  • S = 1.08

  • 2138 reflections

  • 188 parameters

  • 1 restraint

  • Δρmax = 1.08 e Å−3

  • Δρmin = −1.37 e Å−3

Data collection: CAD-4 EXPRESS (Duisenberg, 1992[Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.]; Macíček & Yordanov, 1992[Macíček, J. & Yordanov, A. (1992). J. Appl. Cryst. 25, 73-80.]); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995[Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 1998[Brandenburg, K. (1998). DIAMOND. University of Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812018843/wm2611sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812018843/wm2611Isup2.hkl

checkCIF report


Comment top

La recherche de nouveaux matériaux inorganiques à charpentes ouvertes formées d'octaèdres et de tétraèdres est actuellement un domaine d'intense activité (Borel et al., 1997; Leclaire et al., 2002; Lii et al., 1990; Haddad et al., 1992; Masquelier et al., 1995; Hajji & Zid, 2006).

C'est dans ce cadre, que nous avons exploré les systèmes A–Mn–As–O (A = ion monovalent) qui demeurent relativement peu connus (Frigui et al., 2010, 2011a,b). Une nouvelle phase de formulation Ag1.09Mn3.46(AsO4)3 a été synthétisée par réaction à l'état solide. Un examen bibliographique montre que la structure est de type wyllieite (Moore & Ito, 1973, 1979; Fransolet, 1995; Yakubovich et al., 2005;). Elle peut être décrite à partir de l'unité asymétrique 'Ag2Mn4As3O12' (Fig. 1). Elle est construite à partir de trois octaèdres MnO6 qui se lient par partage d'arêtes pour former le groupement Mn3O14. Ce dernier est lié à l'octaèdre Mn3O6 et trois tétraèdres AsO4 au moyen de sommets. Dans la charpente anionique les octaèdres MnO6 forment, par partage d'arêtes, des chaînes infinies (Mn1–Mn2–Mn4)n disposées selon la direction [101]. Ces dernières se lient au moyen des tétraèdres AsO4 pour former des couches infinies parallèles au plan (010) (Fig. 2). Elles sont connectées d'une part, par des ponts mixtes Mn–O–As et d'autre part par partage d'arêtes avec l'octaèdre MnO6. Il en résulte une charpente tridimensionnelle, possédant des canaux parallèles à l'axe a où logent les cations Ag+ (Fig. 3). L'examen des facteurs géométriques dans la structure révèle qu'ils sont conformes avec ceux rencontrés dans la littérature (Ayed et al., 2004; MacKay et al., 1996; Alvarez-Vega et al., 2006; Frigui et al., 2010, 2011a). De plus, le calcul des différentes valences de liaison (BVS), utilisant la formule empirique de Brown (Brown & Altermatt, 1985), conduit aux valeurs des charges des ions suivants: Ag1(0,91), Ag2(1,06), As1(5,12), As2(5,04), As3(5,11), Mn1(2,11), Mn2(1,85), Mn3(1,69) e t Mn4 (2,63). La recherche de structures présentant des aspects communs avec celle de Ag1.09Mn3.46(AsO4)3, nous a conduit à la famille des alluaudites (Fig. 4) (Ayed et al., 2004; Warner et al., 1993; Korzenski et al., 1998; Chouaibi et al., 2001; Pertlik, 1987; Antenucci et al., 1995; Zid et al., 2005; Hatert, 2006). Les formules de ces deux minéraux, suggérées par Moore (Moore & Ito, 1979) sont X14X24M14M28(PO4)12 pour les alluaudites, et Xa2X1b2X24M14X2a4M2b4(PO4)12 pour les wyllieites, où X et M indiquent les positions des cations selon l'ordre de la taille des ions suivant: M2 < M1 < X1 < X2. Les formes alluaudite, rosemaryite et wyllieite cristallisent dans le même système monoclinique et présentent des paramètres de mailles similaires, cependant une différence cristallographique nette est observée dans la nature du type de réseaux de Bravais. En effet, le groupe d'espace choisi pour les structures type wyllieite ou bien rosemaryite est P21/c (ou P21/n) et celui adopté pour la forme mère alluaudite est le groupe C2/c (ou I2/a). Le choix du sous-groupe d'espace réduit (P21/c) dans la forme wyllieite provoque un effet sur les positions équivalentes de la structure alluaudite et conduit à un éclatement respectif des deux sites X1 e t M2 (Moore & Molin-Case, 1974).

Related literature top

For background to framework structures with tetrahedral and octahedral building units, see: Leclaire et al. (2002); Lii et al. (1990); Haddad et al. (1992); Hajji & Zid (2006); Borel et al. (1997); Masquelier et al. (1995). For details of structural relationships with other compounds, see: Warner et al. (1993); Korzenski et al. (1998); Chouaibi et al. (2001); Pertlik (1987); Antenucci et al. (1995); Zid et al. (2005); Ayed et al. (2004); MacKay et al. (1996); Alvarez-Vega et al. (2006); Frigui et al. (2010, 2011a); Hatert (2006); Moore & Ito (1973, 1979); Yakubovich et al. (2005); Fransolet (1995); Moore & Molin-Case (1974). For preparative details, see: Frigui et al. (2010, 2011a,b). For the bond-valence method, see: Brown & Altermatt (1985).

Experimental top

La synthèse de la phase Ag1.09Mn3.46(AsO4)3 a été réalisée dans un creuset en porcelaine. Les réactifs, AgNO3 (Fluka, 85230), C9H9MnO6.2H2O (Fluka, 63538) e t NH4H2AsO4 (préparé au laboratoire, ASTM 01–775), sont pris dans les proportions Ag:Mn:As égales à 3:5:6. Le mélange finement broyé, est préchauffé lentement dans un four à moufle jusqu'à 623 K en vue d'éliminer NH3, H2O, CO2 et NO2. Il est ensuite porté jusqu'à une température de synthèse proche de celle de la fusion à 1143 K. Le produit est alors abandonné à cette température pendant 4 semaines pour favoriser la germination et la croissance des cristaux. Le résidu final a subi en premier lieu un refroidissement lent (5 K/demi journée) jusqu'à 1043 K puis rapide (50 K.h-1) jusqu'à la température ambiante. Des cristaux de couleur rouge, de taille suffisante pour les mesures des intensités, ont été séparés du flux par l'eau bouillante. Une analyse qualitative au M.E.B de marque FEI et de type Quanta 200 confirme la présence des différents éléments chimiques attendus: As, Mn, Ag et l'oxygène.

Refinement top

L'examen de Fourier-Différence révèle que l'ion Mn3 présente une agitation thermique élevée comparait à celle de Mn1 et Mn2. Dans l'affinement final, et pour des raisons de neutralité électrique, les taux d'occupation des cations Mn32+, Ag1+ et Ag2+ ont été menés en utilisant la condition SUMP autorisée par le programme SHELX. L'affinement de tous les paramètres variables conduit à des ellipsoïdes bien définis. Les densités d'électrons maximum et minimum restants dans la Fourier-différence sont situées respectivements à 0,79 Å de A s2 et à 0,54 Å de Mn4.

Computing details top

Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. Unité asymétrique dans Ag1.09Mn3.46(AsO4)3. Les éllipsoïdes ont été définis avec 50% de probabilité. [Code de symétrie]: (i) 1 + x,y,z; (ii) x,1/2 - y,z- 1/2; (iii) 1 - x,1/2 + y,1/2 - z; (iv) x,1/2 - y,1/2 + z; (v) 1 + x,1/2 - y,1/2 + z; (vi) 1 - x,-1/2 + y,1/2 - z; (vii) 1 - x,-y,1 - z; (viii) -1 + x,y,z.
[Figure 2] Fig. 2. Représentation des couches infinies parallèles au plan (010)
[Figure 3] Fig. 3. Projection de la structure de Ag1.09Mn3.46(AsO4)3 selon a mettant en evidence les cannaux où logent les cations.
[Figure 4] Fig. 4. Projection de la structure, selon c, de Ag1.49Mn3(AsO4)3
silver(I) manganese(II) trisorthoarsenate(V) top
Crystal data top
Ag1.09Mn3.46(AsO4)3F(000) = 1330
Mr = 724.02Dx = 4.919 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25 reflections
a = 6.7470 (7) Åθ = 11–15°
b = 12.9820 (9) ŵ = 16.64 mm−1
c = 11.2970 (8) ÅT = 298 K
β = 98.85 (3)°Prism, red
V = 977.72 (17) Å30.25 × 0.15 × 0.10 mm
Z = 4
Data collection top
Enraf–Nonius CAD-4
diffractometer		1704 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.038
Graphite monochromatorθmax = 27.0°, θmin = 2.4°
ω/2θ scansh = −8→0
Absorption correction: ψ scan
(North et al., 1968)		k = −1→16
Tmin = 0.071, Tmax = 0.210l = −14→14
2522 measured reflections2 standard reflections every 120 min
2138 independent reflections intensity decay: 1.1%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032 w = 1/[σ2(Fo2) + (0.0433P)2 + 6.7709P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.098(Δ/σ)max < 0.001
S = 1.08Δρmax = 1.08 e Å−3
2138 reflectionsΔρmin = −1.37 e Å−3
188 parametersExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.00067 (14)
Crystal data top
Ag1.09Mn3.46(AsO4)3V = 977.72 (17) Å3
Mr = 724.02Z = 4
Monoclinic, P21/cMo Kα radiation
a = 6.7470 (7) ŵ = 16.64 mm−1
b = 12.9820 (9) ÅT = 298 K
c = 11.2970 (8) Å0.25 × 0.15 × 0.10 mm
β = 98.85 (3)°
Data collection top
Enraf–Nonius CAD-4
diffractometer		1704 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)		Rint = 0.038
Tmin = 0.071, Tmax = 0.2102 standard reflections every 120 min
2522 measured reflections intensity decay: 1.1%
2138 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.032188 parameters
wR(F2) = 0.0981 restraint
S = 1.08Δρmax = 1.08 e Å−3
2138 reflectionsΔρmin = −1.37 e Å−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
xyzUiso*/UeqOcc. (<1)
As10.58985 (10)0.11831 (5)0.23334 (6)0.00808 (18)
As20.87952 (9)0.39792 (5)0.26469 (6)0.00878 (18)
As30.23349 (9)0.28782 (5)−0.00773 (6)0.00740 (18)
Mn10.40485 (14)0.35350 (7)0.27517 (9)0.0080 (2)
Mn20.73285 (15)0.23422 (8)0.49855 (8)0.0099 (2)
Mn30.50000.00000.50000.0143 (5)0.916 (5)
Mn40.07641 (16)0.16561 (8)0.21311 (9)0.0144 (2)
Ag10.75155 (11)−0.01201 (7)0.00310 (6)0.0239 (3)0.774 (3)
Ag20.00000.50000.00000.0305 (5)0.631 (4)
O10.5493 (7)0.0060 (3)0.1633 (4)0.0126 (10)
O20.7681 (7)0.1779 (3)0.1698 (4)0.0132 (9)
O30.6539 (7)0.1019 (3)0.3815 (4)0.0130 (10)
O40.3803 (7)0.1906 (3)0.2135 (4)0.0117 (9)
O50.0876 (7)0.3269 (4)0.2693 (4)0.0172 (10)
O60.2259 (7)−0.0884 (4)0.3793 (4)0.0136 (10)
O70.0586 (8)0.0122 (4)0.1655 (4)0.0191 (11)
O80.7207 (6)0.3394 (3)0.3436 (4)0.0104 (9)
O90.4128 (6)0.2108 (3)−0.0446 (4)0.0092 (9)
O100.1085 (8)0.1383 (4)0.3815 (5)0.0209 (11)
O110.3397 (7)0.3798 (3)0.0854 (4)0.0155 (10)
O120.0524 (7)0.2180 (4)0.0434 (4)0.0137 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
As10.0147 (3)0.0049 (3)0.0058 (3)−0.0002 (2)0.0051 (2)0.0003 (2)
As20.0092 (3)0.0131 (3)0.0046 (3)−0.0024 (2)0.0028 (2)0.0001 (2)
As30.0097 (3)0.0049 (3)0.0088 (3)0.0000 (2)0.0049 (2)−0.0016 (2)
Mn10.0108 (5)0.0069 (4)0.0065 (5)−0.0005 (3)0.0021 (4)−0.0010 (3)
Mn20.0142 (5)0.0077 (5)0.0072 (5)−0.0006 (4)0.0001 (4)−0.0010 (3)
Mn30.0232 (9)0.0055 (7)0.0182 (9)0.0008 (6)0.0161 (7)0.0004 (6)
Mn40.0176 (5)0.0147 (5)0.0114 (5)−0.0004 (4)0.0039 (4)−0.0010 (4)
Ag10.0227 (4)0.0383 (5)0.0117 (4)−0.0005 (3)0.0058 (3)0.0009 (3)
Ag20.0409 (9)0.0123 (7)0.0465 (10)0.0030 (6)0.0331 (7)−0.0008 (6)
O10.022 (2)0.006 (2)0.010 (2)−0.0022 (18)0.0046 (19)−0.0020 (17)
O20.021 (2)0.008 (2)0.012 (2)0.0001 (19)0.0088 (19)0.0036 (18)
O30.027 (3)0.008 (2)0.004 (2)0.0001 (19)0.0034 (19)0.0011 (17)
O40.018 (2)0.011 (2)0.007 (2)0.0017 (18)0.0019 (18)−0.0006 (17)
O50.009 (2)0.032 (3)0.012 (2)−0.002 (2)0.0069 (18)0.003 (2)
O60.021 (2)0.013 (2)0.005 (2)0.0040 (19)−0.0025 (18)−0.0011 (18)
O70.026 (3)0.024 (3)0.008 (2)0.016 (2)0.004 (2)0.005 (2)
O80.010 (2)0.012 (2)0.012 (2)0.0018 (17)0.0083 (18)0.0055 (18)
O90.010 (2)0.013 (2)0.006 (2)0.0021 (17)0.0054 (17)−0.0005 (17)
O100.033 (3)0.011 (2)0.018 (3)−0.014 (2)−0.001 (2)0.003 (2)
O110.023 (3)0.009 (2)0.015 (2)−0.0083 (19)0.005 (2)−0.0061 (19)
O120.013 (2)0.019 (2)0.010 (2)−0.0068 (19)0.0066 (18)−0.0042 (19)
Geometric parameters (Å, º) top
As1—O11.661 (4)Mn2—O9iv2.256 (4)
As1—O31.677 (4)Mn2—O6vi2.333 (5)
As1—O21.681 (5)Mn3—O11iv2.204 (5)
As1—O41.683 (5)Mn3—O11vii2.204 (5)
As2—O5i1.674 (5)Mn3—O32.246 (5)
As2—O81.677 (4)Mn3—O3vi2.246 (5)
As2—O6ii1.682 (4)Mn3—O6vi2.413 (5)
As2—O7ii1.701 (5)Mn3—O62.413 (5)
As3—O91.671 (4)Mn4—O101.915 (5)
As3—O111.678 (4)Mn4—O122.017 (5)
As3—O121.693 (5)Mn4—O72.062 (5)
As3—O10iii1.695 (5)Mn4—O2viii2.069 (5)
Mn1—O1ii2.105 (4)Mn4—O42.075 (5)
Mn1—O112.148 (5)Mn4—O52.186 (6)
Mn1—O52.159 (5)Ag1—O12.439 (5)
Mn1—O82.160 (5)Ag1—O7ix2.454 (5)
Mn1—O9iv2.193 (4)Ag1—O1ix2.547 (5)
Mn1—O42.224 (4)Ag1—O7i2.566 (5)
Mn2—O32.183 (5)Ag2—O10x2.418 (5)
Mn2—O82.212 (4)Ag2—O10iii2.418 (5)
Mn2—O12v2.226 (5)Ag2—O6iii2.478 (5)
Mn2—O2iv2.227 (5)Ag2—O6x2.478 (5)
O1—As1—O3111.2 (2)O3—Mn2—O9iv88.97 (17)
O1—As1—O2106.1 (2)O8—Mn2—O9iv73.49 (16)
O3—As1—O2113.2 (2)O12v—Mn2—O9iv145.34 (18)
O1—As1—O4110.7 (2)O2iv—Mn2—O9iv89.79 (17)
O3—As1—O4106.6 (2)O3—Mn2—O6vi73.47 (17)
O2—As1—O4109.1 (2)O8—Mn2—O6vi162.80 (17)
O5i—As2—O8109.6 (2)O12v—Mn2—O6vi93.92 (17)
O5i—As2—O6ii108.4 (2)O2iv—Mn2—O6vi85.10 (17)
O8—As2—O6ii110.6 (2)O9iv—Mn2—O6vi114.06 (17)
O5i—As2—O7ii108.7 (3)O11iv—Mn3—O11vii180.0 (2)
O8—As2—O7ii106.3 (2)O11iv—Mn3—O398.46 (17)
O6ii—As2—O7ii113.2 (2)O11vii—Mn3—O381.54 (17)
O9—As3—O11109.1 (2)O11iv—Mn3—O3vi81.54 (17)
O9—As3—O12110.6 (2)O11vii—Mn3—O3vi98.46 (17)
O11—As3—O12115.4 (2)O3—Mn3—O3vi180.0
O9—As3—O10iii116.9 (2)O11iv—Mn3—O6vi78.51 (17)
O11—As3—O10iii100.1 (2)O11vii—Mn3—O6vi101.49 (17)
O12—As3—O10iii104.6 (3)O3—Mn3—O6vi70.87 (17)
O1ii—Mn1—O11100.20 (18)O3vi—Mn3—O6vi109.13 (17)
O1ii—Mn1—O5104.8 (2)O11iv—Mn3—O6101.49 (17)
O11—Mn1—O586.86 (18)O11vii—Mn3—O678.51 (17)
O1ii—Mn1—O882.81 (18)O3—Mn3—O6109.13 (17)
O11—Mn1—O8114.17 (18)O3vi—Mn3—O670.87 (17)
O5—Mn1—O8156.39 (18)O6vi—Mn3—O6180.00 (19)
O1ii—Mn1—O9iv94.00 (18)O10—Mn4—O12170.8 (2)
O11—Mn1—O9iv163.49 (17)O10—Mn4—O794.2 (2)
O5—Mn1—O9iv81.37 (18)O12—Mn4—O794.9 (2)
O8—Mn1—O9iv75.76 (16)O10—Mn4—O2viii101.8 (2)
O1ii—Mn1—O4175.83 (18)O12—Mn4—O2viii79.54 (19)
O11—Mn1—O481.08 (17)O7—Mn4—O2viii89.83 (19)
O5—Mn1—O479.20 (19)O10—Mn4—O493.8 (2)
O8—Mn1—O493.05 (17)O12—Mn4—O483.35 (18)
O9iv—Mn1—O485.35 (17)O7—Mn4—O499.78 (19)
O3—Mn2—O891.75 (17)O2viii—Mn4—O4161.04 (18)
O3—Mn2—O12v119.67 (18)O10—Mn4—O584.0 (2)
O8—Mn2—O12v85.69 (17)O12—Mn4—O586.98 (19)
O3—Mn2—O2iv155.86 (18)O7—Mn4—O5177.62 (19)
O8—Mn2—O2iv110.95 (18)O2viii—Mn4—O589.03 (18)
O12v—Mn2—O2iv71.89 (18)O4—Mn4—O581.91 (17)
Symmetry codes: (i) x+1, y, z; (ii) −x+1, y+1/2, −z+1/2; (iii) x, −y+1/2, z−1/2; (iv) x, −y+1/2, z+1/2; (v) x+1, −y+1/2, z+1/2; (vi) −x+1, −y, −z+1; (vii) −x+1, y−1/2, −z+1/2; (viii) x−1, y, z; (ix) −x+1, −y, −z; (x) −x, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formulaAg1.09Mn3.46(AsO4)3
Mr724.02
Crystal system, space groupMonoclinic, P21/c
Temperature (K)298
a, b, c (Å)6.7470 (7), 12.9820 (9), 11.2970 (8)
β (°) 98.85 (3)
V (Å3)977.72 (17)
Z4
Radiation typeMo Kα
µ (mm−1)16.64
Crystal size (mm)0.25 × 0.15 × 0.10
Data collection
DiffractometerEnraf–Nonius CAD-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.071, 0.210
No. of measured, independent and
observed [I > 2σ(I)] reflections		2522, 2138, 1704
Rint0.038
(sin θ/λ)max (Å−1)0.638
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.098, 1.08
No. of reflections2138
No. of parameters188
No. of restraints1
Δρmax, Δρmin (e Å−3)1.08, −1.37

Computer programs: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992), XCAD4 (Harms & Wocadlo, 1995), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1998), WinGX (Farrugia, 1999).

 

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ISSN: 2056-9890
Volume 68| Part 6| June 2012| Pages i40-i41
doi:10.1107/S1600536812018843
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