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The structure of sodium calcium magnesium iron phosphate, (Na0,38,Ca0,31)MgFe2P3O12, consists of an [MgFe2(PO4)3]- framework, built up by chains of edge-sharing (FeO6-FeO6-MgO6) octahedra running along the [\overline 101] direction. The chains are linked together via the common corners of phosphate tetrahedra to form sheets parallel to the ab plane. Adjacent sheets are also connected through PO4 tetrahedra, thus giving rise to an open framework with two different kinds of channels where the Na+ and Ca2+ cations are located.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805006756/dn6200sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805006756/dn6200Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](Mg-O) = 0.004 Å
  • Disorder in solvent or counterion
  • R factor = 0.031
  • wR factor = 0.088
  • Data-to-parameter ratio = 10.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 34.00 Perc.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 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 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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, 1998); software used to prepare material for publication: SHELXL97.

sodium calcium magnesium iron phosphate top
Crystal data top
(Na0.38·Ca0.31)MgFe2P3O12F(000) = 862
Mr = 442.07Dx = 3.405 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 25 reflections
a = 11.852 (2) Åθ = 10–15°
b = 12.458 (1) ŵ = 4.27 mm1
c = 6.3861 (6) ÅT = 298 K
β = 113.84 (1)°Prism, brown
V = 862.5 (2) Å30.20 × 0.08 × 0.04 mm
Z = 4
Data collection top
Enraf–Nonius CAD-4
diffractometer
904 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.021
Graphite monochromatorθmax = 28.0°, θmin = 2.5°
ω/2θ scansh = 015
Absorption correction: ψ scan
(North et al., 1968)
k = 216
Tmin = 0.672, Tmax = 0.847l = 87
1292 measured reflections2 standard reflections every 120 min
1045 independent reflections intensity decay: 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)] = 0.031 w = 1/[σ2(Fo2) + (0.0266P)2 + 12.2021P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.088(Δ/σ)max < 0.001
S = 1.11Δρmax = 1.21 e Å3
1045 reflectionsΔρmin = 0.73 e Å3
97 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.0019 (4)
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)
Fe10.78242 (5)0.84605 (5)0.8697 (1)0.0091 (2)
P10.74054 (9)0.60906 (8)0.6295 (2)0.0049 (2)
P20.50000.7872 (1)0.75000.0044 (3)
Mg10.50000.7644 (2)0.25000.0107 (4)
Na11.00000.9968 (7)0.25000.026 (2)0.376 (9)
Ca10.50001.00000.50000.027 (2)0.312 (4)
O10.8322 (3)0.8350 (2)0.6045 (5)0.0079 (6)
O20.3769 (3)0.8977 (2)0.1809 (5)0.0123 (6)
O30.7763 (3)0.8217 (2)1.1820 (5)0.0070 (5)
O40.8174 (3)0.9980 (2)0.8791 (5)0.0102 (6)
O50.6013 (3)0.8635 (2)0.7462 (5)0.0096 (6)
O60.9561 (3)0.7834 (2)1.0323 (5)0.0079 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0104 (3)0.0086 (3)0.0086 (3)0.0004 (2)0.0043 (2)0.0009 (2)
P10.0074 (5)0.0038 (4)0.0039 (4)0.0000 (3)0.0028 (3)0.0002 (3)
P20.0044 (6)0.0058 (6)0.0027 (6)0.0000.0010 (5)0.000
Mg10.0101 (9)0.012 (1)0.0115 (9)0.0000.0061 (8)0.000
Na10.010 (3)0.041 (5)0.020 (4)0.0000.001 (3)0.000
Ca10.027 (3)0.012 (2)0.025 (2)0.003 (2)0.007 (2)0.0005 (18)
O10.013 (2)0.006 (2)0.004 (1)0.0020 (11)0.0032 (11)0.0012 (10)
O20.009 (2)0.014 (2)0.015 (2)0.0013 (12)0.0060 (12)0.0013 (10)
O30.010 (2)0.008 (2)0.004 (2)0.0002 (10)0.0029 (10)0.0005 (10)
O40.016 (2)0.004 (2)0.012 (2)0.0002 (11)0.0069 (12)0.0014 (11)
O50.006 (2)0.009 (2)0.013 (2)0.0011 (11)0.0023 (11)0.0032 (11)
O60.007 (2)0.010 (2)0.005 (2)0.0000 (10)0.0009 (10)0.0028 (10)
Geometric parameters (Å, º) top
Fe1—O41.934 (3)Mg1—Fe1ii3.2744 (11)
Fe1—O51.978 (3)Mg1—Na1vii3.334 (9)
Fe1—O12.011 (3)Mg1—Ca13.3409 (19)
Fe1—O32.048 (3)Mg1—Ca1x3.3409 (19)
Fe1—O62.049 (3)Na1—O4xi2.480 (3)
Fe1—O3i2.185 (3)Na1—O4xii2.480 (3)
Fe1—Mg1ii3.2744 (11)Na1—O4iv2.610 (3)
Fe1—Na1iii3.319 (5)Na1—O4xiii2.610 (3)
Fe1—Na1iv3.558 (5)Na1—O1iv2.778 (7)
P1—O2v1.516 (3)Na1—O1xiii2.778 (7)
P1—O4vi1.536 (3)Na1—O6xii2.947 (9)
P1—O1ii1.556 (3)Na1—O6xi2.947 (9)
P1—O3i1.558 (3)Na1—Na1iv3.1940 (6)
P1—Na1vii3.221 (4)Na1—Na1xiv3.1940 (6)
P1—Ca1vi3.3196 (11)Na1—P1xv3.221 (4)
P2—O5viii1.539 (3)Na1—P1xvi3.221 (4)
P2—O51.539 (3)Ca1—O5xvii2.297 (3)
P2—O6ix1.547 (3)Ca1—O52.297 (3)
P2—O6i1.547 (3)Ca1—O2xvii2.346 (3)
P2—Ca1viii3.0946 (12)Ca1—O22.346 (3)
P2—Ca13.0946 (12)Ca1—O2xviii2.540 (3)
Mg1—O2x2.135 (4)Ca1—O2x2.540 (3)
Mg1—O22.135 (3)Ca1—O5xiii2.921 (3)
Mg1—O6ix2.152 (3)Ca1—O5viii2.921 (3)
Mg1—O6ii2.152 (3)Ca1—P2xvii3.0946 (12)
Mg1—O1ix2.204 (3)Ca1—Ca1x3.1931 (3)
Mg1—O1ii2.204 (3)Ca1—Ca1viii3.1931 (3)
Mg1—Fe1ix3.2744 (11)
O4—Fe1—O595.11 (13)O4xi—Na1—O6xi68.62 (16)
O4—Fe1—O187.78 (12)O4xii—Na1—O6xi112.1 (3)
O5—Fe1—O1108.22 (12)O4iv—Na1—O6xi99.2 (2)
O4—Fe1—O3101.89 (12)O4xiii—Na1—O6xi83.35 (18)
O5—Fe1—O386.81 (12)O1iv—Na1—O6xi123.83 (9)
O1—Fe1—O3161.50 (12)O1xiii—Na1—O6xi143.55 (12)
O4—Fe1—O6101.44 (12)O6xii—Na1—O6xi51.15 (19)
O5—Fe1—O6161.92 (12)O5xvii—Ca1—O5180.0
O1—Fe1—O679.86 (12)O5xvii—Ca1—O2xvii99.31 (11)
O3—Fe1—O682.75 (11)O5—Ca1—O2xvii80.69 (11)
O4—Fe1—O3i172.84 (12)O5xvii—Ca1—O280.69 (11)
O5—Fe1—O3i79.45 (11)O5—Ca1—O299.31 (11)
O1—Fe1—O3i89.50 (11)O2xvii—Ca1—O2180.00 (13)
O3—Fe1—O3i82.58 (11)O5xvii—Ca1—O2xviii72.69 (10)
O6—Fe1—O3i84.58 (11)O5—Ca1—O2xviii107.31 (10)
Mg1ii—Fe1—Na1iv58.24 (13)O2xvii—Ca1—O2xviii66.57 (13)
Na1iii—Fe1—Na1iv55.218 (11)O2—Ca1—O2xviii113.43 (13)
O2v—P1—O4vi112.34 (18)O5xvii—Ca1—O2x107.31 (10)
O2v—P1—O1ii111.19 (17)O5—Ca1—O2x72.69 (10)
O4vi—P1—O1ii107.63 (16)O2xvii—Ca1—O2x113.43 (13)
O2v—P1—O3i108.75 (17)O2—Ca1—O2x66.57 (13)
O4vi—P1—O3i109.37 (16)O2xviii—Ca1—O2x180.0
O1ii—P1—O3i107.44 (16)O5xvii—Ca1—O5xiii53.67 (12)
Na1vii—P1—Ca1vi129.94 (15)O5—Ca1—O5xiii126.33 (12)
O5viii—P2—O5103.7 (2)O2xvii—Ca1—O5xiii85.11 (9)
O5viii—P2—O6ix112.6 (2)O2—Ca1—O5xiii94.89 (9)
O5—P2—O6ix108.5 (2)O2xviii—Ca1—O5xiii113.62 (9)
O5viii—P2—O6i108.5 (2)O2x—Ca1—O5xiii66.38 (9)
O5—P2—O6i112.6 (2)O5xvii—Ca1—O5viii126.33 (12)
O6ix—P2—O6i110.7 (2)O5—Ca1—O5viii53.67 (12)
Ca1viii—P2—Ca162.12 (3)O2xvii—Ca1—O5viii94.89 (9)
O2x—Mg1—O277.96 (17)O2—Ca1—O5viii85.11 (9)
O2x—Mg1—O6ix114.73 (12)O2xviii—Ca1—O5viii66.38 (9)
O2—Mg1—O6ix90.69 (12)O2x—Ca1—O5viii113.62 (9)
O2x—Mg1—O6ii90.69 (12)O5xiii—Ca1—O5viii180.0
O2—Mg1—O6ii114.73 (12)P1ii—O1—Fe1122.73 (17)
O6ix—Mg1—O6ii147.86 (19)P1ii—O1—Mg1ii135.42 (17)
O2x—Mg1—O1ix161.59 (13)Fe1—O1—Mg1ii101.84 (12)
O2—Mg1—O1ix85.70 (11)P1ii—O1—Na1iv91.57 (16)
O6ix—Mg1—O1ix73.47 (11)Fe1—O1—Na1iv94.63 (11)
O6ii—Mg1—O1ix88.48 (11)Mg1ii—O1—Na1iv83.17 (16)
O2x—Mg1—O1ii85.70 (11)P1ix—O2—Mg1125.56 (18)
O2—Mg1—O1ii161.59 (13)P1ix—O2—Ca1116.91 (17)
O6ix—Mg1—O1ii88.48 (11)Mg1—O2—Ca196.29 (12)
O6ii—Mg1—O1ii73.47 (11)P1ix—O2—Ca1x133.43 (18)
O1ix—Mg1—O1ii111.61 (17)Mg1—O2—Ca1x90.79 (11)
Ca1—Mg1—Ca1x57.09 (4)Ca1—O2—Ca1x81.50 (9)
O4xi—Na1—O4xii179.3 (4)P1i—O3—Fe1137.45 (18)
O4xi—Na1—O4iv77.67 (9)P1i—O3—Fe1i120.92 (16)
O4xii—Na1—O4iv102.31 (9)Fe1—O3—Fe1i97.42 (11)
O4xi—Na1—O4xiii102.31 (9)P1xix—O4—Fe1142.6 (2)
O4xii—Na1—O4xiii77.67 (9)P1xix—O4—Na1iii104.2 (2)
O4iv—Na1—O4xiii177.2 (4)Fe1—O4—Na1iii96.7 (2)
O4xi—Na1—O1iv56.32 (13)P1xix—O4—Na1iv112.5 (2)
O4xii—Na1—O1iv123.1 (3)Fe1—O4—Na1iv102.1 (2)
O4iv—Na1—O1iv60.93 (13)Na1iii—O4—Na1iv77.69 (9)
O4xiii—Na1—O1iv116.6 (3)P2—O5—Fe1130.82 (18)
O4xi—Na1—O1xiii123.1 (3)P2—O5—Ca1105.84 (14)
O4xii—Na1—O1xiii56.32 (13)Fe1—O5—Ca1122.48 (14)
O4iv—Na1—O1xiii116.6 (3)P2—O5—Ca1viii81.54 (12)
O4xiii—Na1—O1xiii60.93 (13)Fe1—O5—Ca1viii117.79 (13)
O1iv—Na1—O1xiii82.0 (3)Ca1—O5—Ca1viii74.38 (8)
O4xi—Na1—O6xii112.1 (3)P2i—O6—Fe1125.19 (16)
O4xii—Na1—O6xii68.62 (16)P2i—O6—Mg1ii119.21 (17)
O4iv—Na1—O6xii83.35 (18)Fe1—O6—Mg1ii102.37 (12)
O4xiii—Na1—O6xii99.2 (2)P2i—O6—Na1iii99.08 (15)
O1iv—Na1—O6xii143.55 (12)Fe1—O6—Na1iii81.09 (10)
O1xiii—Na1—O6xii123.83 (9)Mg1ii—O6—Na1iii126.04 (14)
Symmetry codes: (i) x+3/2, y+3/2, z+2; (ii) x+3/2, y+3/2, z+1; (iii) x, y, z+1; (iv) x+2, y+2, z+1; (v) x+1/2, y+3/2, z+1/2; (vi) x+3/2, y1/2, z+3/2; (vii) x1/2, y1/2, z; (viii) x+1, y, z+3/2; (ix) x1/2, y+3/2, z1/2; (x) x+1, y, z+1/2; (xi) x+2, y, z+3/2; (xii) x, y, z1; (xiii) x, y+2, z1/2; (xiv) x+2, y+2, z; (xv) x+1/2, y+1/2, z; (xvi) x+3/2, y+1/2, z+1/2; (xvii) x+1, y+2, z+1; (xviii) x, y+2, z+1/2; (xix) x+3/2, y+1/2, z+3/2.
 

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