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Four new crystalline structures within the Na–Fe–Mo–O system are reported: sodium tetrairon pentamolydate (1), NaFe4(MoO4)5, α-sodium diiron trimolybdate (2), α-NaFe2(MoO4)3, β-sodium diiron trimolybdate (3), β-NaFe2(MoO4)3, trisodium diiron trimolybdate (4), Na3Fe2(MoO4)3. All these structures belong to orthomolybdate class of compound and are described as networks of [FeO6] octahedra and [MoO4] tetrahedra. They are compared with each other and with other related structures.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768103016598/os5002sup1.cif
Contains datablocks (1), (2), (3), (4), global

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103016598/os50021sup2.fcf
Contains datablock 1

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103016598/os50022sup3.fcf
Contains datablock 2

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103016598/os50023sup4.fcf
Contains datablock 3

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103016598/os50024sup5.fcf
Contains datablock 4

Computing details top

For all compounds, data collection: CrysAlis CCD (Oxford Diffraction Limited, 2001); cell refinement: CrysAlis RED (Oxford Diffraction Limited, 2001); data reduction: CrysAlis RED (Oxford Diffraction Limited, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: Diamond (Brandenburg, 2001) for (1), (3). Software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) for (1), (3).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(1) sodium tetrairon pentamolybdate top
Crystal data top
Fe4Mo5NaO20Z = 2
Mr = 1046.09F(000) = 970
Triclinic, P1Dx = 4.089 Mg m3
a = 6.9337 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 7.0196 (4) ÅCell parameters from 10278 reflections
c = 17.8033 (8) Åθ = 2.3–43.6°
α = 87.468 (4)°µ = 7.00 mm1
β = 87.615 (4)°T = 293 K
γ = 79.090 (4)°Prism, black
V = 849.54 (7) Å30.21 × 0.19 × 0.14 mm
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector11 independent reflections
Radiation source: fine-focus sealed tube9620 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Rotation method data acquisition using ω and phi scans(s)θmax = 43.6°, θmin = 2.3°
Absorption correction: numeric analytical
?
h = 1313
Tmin = 0.300, Tmax = 0.444k = 1313
37235 measured reflectionsl = 3434
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.032Secondary atom site location: difference Fourier map
wR(F2) = 0.078 w = 1/[σ2(Fo2) + (0.0311P)2 + 1.1496P]
where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max = 0.002
11711 reflectionsΔρmax = 1.54 e Å3
271 parametersΔρmin = 2.29 e Å3
Crystal data top
Fe4Mo5NaO20γ = 79.090 (4)°
Mr = 1046.09V = 849.54 (7) Å3
Triclinic, P1Z = 2
a = 6.9337 (3) ÅMo Kα radiation
b = 7.0196 (4) ŵ = 7.00 mm1
c = 17.8033 (8) ÅT = 293 K
α = 87.468 (4)°0.21 × 0.19 × 0.14 mm
β = 87.615 (4)°
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector11 independent reflections
Absorption correction: numeric analytical
?
9620 reflections with I > 2σ(I)
Tmin = 0.300, Tmax = 0.444Rint = 0.035
37235 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.032271 parameters
wR(F2) = 0.0780 restraints
S = 1.13Δρmax = 1.54 e Å3
11711 reflectionsΔρmin = 2.29 e Å3
Special details top

Experimental. CrysAlis RED, Oxford Diffraction Ltd., version 170.17, 2003 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R·C. Clark & J·S. Reid.

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*/Ueq
Mo10.72970 (3)0.93852 (3)0.094013 (11)0.00895 (3)
Mo20.68051 (3)0.22041 (3)0.309457 (11)0.01007 (4)
Mo30.21711 (3)0.82601 (3)0.285406 (10)0.00866 (3)
Mo40.72965 (3)0.68980 (3)0.473930 (10)0.00867 (3)
Mo50.24818 (3)0.54462 (3)0.086520 (11)0.00985 (4)
Fe10.75239 (5)0.69668 (5)0.265675 (18)0.00869 (5)
Fe20.81431 (5)0.17149 (5)0.507320 (19)0.00903 (5)
Fe30.77718 (5)0.42412 (5)0.125698 (18)0.00898 (5)
Fe41.17232 (5)1.08132 (5)0.114821 (19)0.01041 (6)
O10.8756 (3)0.8648 (3)0.49781 (11)0.0148 (3)
O20.5156 (3)0.2131 (3)0.50552 (14)0.0224 (4)
O30.8002 (4)0.8836 (3)0.00156 (11)0.0213 (4)
O40.4354 (3)0.2959 (4)0.33180 (14)0.0241 (4)
O50.8183 (3)0.2012 (3)0.39139 (11)0.0182 (4)
O60.4597 (3)0.7133 (3)0.26435 (13)0.0195 (4)
O71.1677 (4)0.7869 (3)0.11036 (14)0.0250 (5)
O80.7503 (4)0.4661 (4)0.01112 (12)0.0240 (4)
O90.4804 (3)1.0328 (3)0.10127 (14)0.0227 (4)
O100.7688 (3)0.7137 (3)0.15068 (10)0.0126 (3)
O110.8557 (3)1.1265 (3)0.11898 (11)0.0130 (3)
O120.7763 (3)0.3974 (3)0.24658 (10)0.0131 (3)
O130.0867 (3)0.3883 (3)0.12592 (11)0.0145 (3)
O140.0519 (3)0.6656 (3)0.26884 (12)0.0169 (3)
O150.1620 (3)1.0480 (3)0.23241 (11)0.0172 (3)
O160.1948 (4)0.8830 (3)0.37977 (11)0.0211 (4)
O170.7987 (3)0.4674 (3)0.52384 (12)0.0190 (4)
O180.7133 (4)0.0097 (3)0.26918 (13)0.0232 (4)
O190.7568 (4)0.6465 (4)0.37741 (11)0.0243 (5)
O200.4795 (3)0.4586 (4)0.12356 (13)0.0226 (4)
Na10.1189 (3)0.3361 (3)0.3029 (3)0.0945 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01045 (8)0.00738 (6)0.00965 (7)0.00317 (6)0.00216 (6)0.00103 (5)
Mo20.01052 (8)0.00899 (7)0.01100 (7)0.00297 (6)0.00057 (6)0.00155 (5)
Mo30.00790 (8)0.00930 (7)0.00877 (7)0.00168 (6)0.00036 (5)0.00003 (5)
Mo40.00969 (8)0.00895 (7)0.00815 (7)0.00369 (6)0.00060 (5)0.00023 (5)
Mo50.01054 (8)0.00900 (7)0.01074 (7)0.00416 (6)0.00222 (6)0.00084 (5)
Fe10.00955 (14)0.00881 (11)0.00812 (11)0.00273 (10)0.00006 (10)0.00084 (9)
Fe20.00848 (14)0.00896 (11)0.00956 (11)0.00136 (10)0.00034 (10)0.00052 (9)
Fe30.00952 (14)0.00798 (11)0.00946 (12)0.00154 (10)0.00043 (10)0.00103 (9)
Fe40.01065 (15)0.00930 (12)0.01119 (12)0.00189 (10)0.00037 (10)0.00002 (9)
O10.0132 (8)0.0136 (7)0.0191 (8)0.0060 (6)0.0012 (6)0.0021 (6)
O20.0123 (9)0.0234 (10)0.0316 (11)0.0032 (7)0.0011 (8)0.0023 (8)
O30.0317 (12)0.0207 (9)0.0120 (7)0.0062 (8)0.0018 (7)0.0006 (6)
O40.0113 (9)0.0299 (11)0.0299 (11)0.0021 (8)0.0009 (8)0.0025 (9)
O50.0196 (10)0.0202 (8)0.0139 (7)0.0018 (7)0.0036 (7)0.0024 (6)
O60.0109 (8)0.0185 (8)0.0280 (10)0.0001 (7)0.0023 (7)0.0040 (7)
O70.0325 (13)0.0117 (8)0.0314 (11)0.0071 (8)0.0108 (9)0.0047 (7)
O80.0318 (13)0.0281 (11)0.0127 (8)0.0086 (9)0.0022 (8)0.0015 (7)
O90.0119 (9)0.0213 (9)0.0347 (12)0.0018 (7)0.0050 (8)0.0016 (8)
O100.0166 (8)0.0102 (6)0.0108 (6)0.0028 (6)0.0001 (6)0.0016 (5)
O110.0123 (8)0.0113 (6)0.0165 (7)0.0044 (6)0.0009 (6)0.0021 (5)
O120.0137 (8)0.0117 (6)0.0135 (7)0.0025 (6)0.0011 (6)0.0022 (5)
O130.0127 (8)0.0116 (7)0.0197 (8)0.0048 (6)0.0045 (6)0.0012 (6)
O140.0136 (9)0.0178 (8)0.0208 (8)0.0066 (7)0.0031 (7)0.0005 (6)
O150.0226 (10)0.0128 (7)0.0160 (8)0.0028 (7)0.0062 (7)0.0034 (6)
O160.0291 (12)0.0240 (9)0.0100 (7)0.0043 (8)0.0004 (7)0.0016 (6)
O170.0242 (11)0.0123 (7)0.0200 (8)0.0035 (7)0.0009 (7)0.0027 (6)
O180.0327 (13)0.0141 (8)0.0244 (10)0.0086 (8)0.0023 (9)0.0014 (7)
O190.0383 (14)0.0273 (10)0.0099 (7)0.0124 (10)0.0003 (8)0.0014 (7)
O200.0148 (10)0.0299 (11)0.0249 (10)0.0083 (8)0.0014 (8)0.0028 (8)
Na10.0278 (10)0.0208 (8)0.237 (4)0.0006 (7)0.0510 (17)0.0092 (15)
Geometric parameters (Å, º) top
Mo1—O91.732 (2)Fe3—O82.059 (2)
Mo1—O31.736 (2)Fe3—O11vii2.0646 (18)
Mo1—O111.7947 (17)Fe3—O102.0897 (18)
Mo1—O101.8171 (18)Fe3—O13i2.113 (2)
Mo2—O41.717 (2)Fe3—O122.1518 (19)
Mo2—O51.763 (2)Fe4—O72.078 (2)
Mo2—O181.768 (2)Fe4—O3viii2.081 (2)
Mo2—O121.8345 (17)Fe4—O15i2.096 (2)
Mo2—Na1i3.288 (2)Fe4—O9i2.104 (2)
Mo3—O161.738 (2)Fe4—O13ix2.1396 (19)
Mo3—O61.751 (2)Fe4—O112.157 (2)
Mo3—O151.772 (2)O1—Fe2vi2.115 (2)
Mo3—O141.7927 (19)O1—Fe2ii2.1271 (19)
Mo3—Na1ii3.541 (2)O2—Mo4iii1.738 (2)
Mo3—Na13.628 (2)O3—Fe4viii2.081 (2)
Mo4—O2iii1.738 (2)O4—Na12.237 (3)
Mo4—O191.754 (2)O5—Na1i2.840 (4)
Mo4—O171.757 (2)O7—Mo5i1.752 (2)
Mo4—O11.8072 (18)O8—Mo5iv1.743 (2)
Mo5—O8iv1.743 (2)O9—Fe4v2.104 (2)
Mo5—O201.749 (3)O11—Fe3ii2.0646 (18)
Mo5—O7v1.752 (2)O12—Na1i2.570 (3)
Mo5—O131.8113 (17)O13—Fe3v2.113 (2)
Fe1—O192.005 (2)O13—Fe4x2.1396 (19)
Fe1—O62.011 (2)O14—Fe1v2.049 (2)
Fe1—O18ii2.031 (2)O14—Na12.329 (3)
Fe1—O102.0451 (18)O15—Fe4v2.096 (2)
Fe1—O14i2.049 (2)O15—Na1ii2.391 (3)
Fe1—O122.1172 (18)O16—Fe2iii2.030 (2)
Fe1—Na1i3.295 (2)O18—Fe1vii2.031 (2)
Fe2—O16iii2.030 (2)Na1—O15vii2.391 (3)
Fe2—O22.037 (2)Na1—O12v2.570 (3)
Fe2—O52.065 (2)Na1—O5v2.840 (4)
Fe2—O172.092 (2)Na1—Mo2v3.288 (2)
Fe2—O1vi2.115 (2)Na1—Fe1v3.295 (2)
Fe2—O1vii2.1271 (19)Na1—Mo3vii3.541 (2)
Fe3—O202.034 (2)
O9—Mo1—O3110.55 (12)O10—Fe3—O1280.26 (7)
O9—Mo1—O11106.98 (10)O13i—Fe3—O1288.30 (8)
O3—Mo1—O11106.95 (10)O7—Fe4—O3viii93.13 (9)
O9—Mo1—O10106.31 (10)O7—Fe4—O15i87.94 (9)
O3—Mo1—O10108.21 (9)O3viii—Fe4—O15i176.61 (10)
O11—Mo1—O10117.78 (9)O7—Fe4—O9i92.14 (10)
O4—Mo2—O5109.91 (11)O3viii—Fe4—O9i80.11 (10)
O4—Mo2—O18108.73 (12)O15i—Fe4—O9i96.64 (10)
O5—Mo2—O18109.17 (11)O7—Fe4—O13ix163.12 (9)
O4—Mo2—O12111.67 (11)O3viii—Fe4—O13ix91.08 (8)
O5—Mo2—O12105.71 (10)O15i—Fe4—O13ix88.80 (8)
O18—Mo2—O12111.59 (9)O9i—Fe4—O13ix104.69 (8)
O4—Mo2—Na1i145.79 (10)O7—Fe4—O1186.60 (9)
O5—Mo2—Na1i59.69 (10)O3viii—Fe4—O1195.40 (9)
O18—Mo2—Na1i105.38 (10)O15i—Fe4—O1187.87 (8)
O12—Mo2—Na1i51.14 (9)O9i—Fe4—O11175.27 (9)
O16—Mo3—O6109.20 (12)O13ix—Fe4—O1176.73 (7)
O16—Mo3—O15106.97 (10)Mo4—O1—Fe2vi126.98 (10)
O6—Mo3—O15109.22 (11)Mo4—O1—Fe2ii133.57 (12)
O16—Mo3—O14108.53 (10)Fe2vi—O1—Fe2ii97.33 (7)
O6—Mo3—O14110.25 (10)Mo4iii—O2—Fe2159.73 (14)
O15—Mo3—O14112.57 (10)Mo1—O3—Fe4viii159.30 (14)
O16—Mo3—Na1ii69.79 (11)Mo2—O4—Na1150.88 (18)
O6—Mo3—Na1ii117.79 (8)Mo2—O5—Fe2146.35 (13)
O15—Mo3—Na1ii37.46 (10)Mo2—O5—Na1i87.91 (10)
O14—Mo3—Na1ii129.58 (8)Fe2—O5—Na1i124.39 (12)
O16—Mo3—Na199.11 (10)Mo3—O6—Fe1152.61 (13)
O6—Mo3—Na185.09 (8)Mo5i—O7—Fe4157.61 (14)
O15—Mo3—Na1143.36 (9)Mo5iv—O8—Fe3168.91 (16)
O14—Mo3—Na132.66 (8)Mo1—O9—Fe4v167.01 (14)
Na1ii—Mo3—Na1156.57 (10)Mo1—O10—Fe1124.81 (9)
O2iii—Mo4—O19108.47 (13)Mo1—O10—Fe3133.03 (10)
O2iii—Mo4—O17109.97 (11)Fe1—O10—Fe3100.87 (8)
O19—Mo4—O17108.27 (11)Mo1—O11—Fe3ii134.26 (11)
O2iii—Mo4—O1108.07 (10)Mo1—O11—Fe4120.94 (9)
O19—Mo4—O1110.21 (10)Fe3ii—O11—Fe4102.46 (7)
O17—Mo4—O1111.80 (10)Mo2—O12—Fe1125.88 (9)
O8iv—Mo5—O20112.77 (12)Mo2—O12—Fe3128.99 (10)
O8iv—Mo5—O7v108.17 (12)Fe1—O12—Fe396.61 (7)
O20—Mo5—O7v109.27 (12)Mo2—O12—Na1i95.10 (11)
O8iv—Mo5—O13107.92 (10)Fe1—O12—Na1i88.80 (8)
O20—Mo5—O13106.70 (11)Fe3—O12—Na1i114.61 (12)
O7v—Mo5—O13112.07 (10)Mo5—O13—Fe3v130.03 (11)
O19—Fe1—O692.45 (10)Mo5—O13—Fe4x118.75 (9)
O19—Fe1—O18ii95.94 (10)Fe3v—O13—Fe4x101.42 (8)
O6—Fe1—O18ii90.21 (10)Mo3—O14—Fe1v134.45 (12)
O19—Fe1—O10172.81 (9)Mo3—O14—Na1122.79 (13)
O6—Fe1—O1090.70 (9)Fe1v—O14—Na197.44 (9)
O18ii—Fe1—O1090.51 (8)Mo3—O15—Fe4v126.21 (11)
O19—Fe1—O14i86.30 (10)Mo3—O15—Na1ii115.76 (13)
O6—Fe1—O14i177.15 (9)Fe4v—O15—Na1ii117.38 (13)
O18ii—Fe1—O14i92.47 (10)Mo3—O16—Fe2iii156.25 (14)
O10—Fe1—O14i90.26 (8)Mo4—O17—Fe2138.43 (13)
O19—Fe1—O1291.63 (9)Mo2—O18—Fe1vii157.87 (14)
O6—Fe1—O1286.42 (8)Mo4—O19—Fe1160.02 (15)
O18ii—Fe1—O12171.83 (9)Mo5—O20—Fe3155.00 (14)
O10—Fe1—O1282.11 (7)O4—Na1—O14101.12 (12)
O14i—Fe1—O1291.05 (8)O4—Na1—O15vii94.43 (13)
O19—Fe1—Na1i71.64 (11)O14—Na1—O15vii133.1 (2)
O6—Fe1—Na1i132.66 (8)O4—Na1—O12v170.1 (2)
O18ii—Fe1—Na1i134.50 (9)O14—Na1—O12v74.55 (10)
O10—Fe1—Na1i101.53 (10)O15vii—Na1—O12v82.63 (11)
O14i—Fe1—Na1i44.49 (7)O4—Na1—O5v125.82 (18)
O12—Fe1—Na1i51.24 (7)O14—Na1—O5v115.02 (12)
O16iii—Fe2—O290.62 (10)O15vii—Na1—O5v89.16 (9)
O16iii—Fe2—O5174.64 (9)O12v—Na1—O5v63.79 (8)
O2—Fe2—O588.08 (10)O4—Na1—Mo2v154.32 (15)
O16iii—Fe2—O1790.60 (9)O14—Na1—Mo2v102.73 (9)
O2—Fe2—O1790.31 (9)O15vii—Na1—Mo2v76.02 (8)
O5—Fe2—O1794.61 (9)O12v—Na1—Mo2v33.76 (5)
O16iii—Fe2—O1vi92.88 (9)O5v—Na1—Mo2v32.40 (5)
O2—Fe2—O1vi176.43 (9)O4—Na1—Fe1v138.17 (10)
O5—Fe2—O1vi88.48 (9)O14—Na1—Fe1v38.07 (6)
O17—Fe2—O1vi89.01 (8)O15vii—Na1—Fe1v119.56 (12)
O16iii—Fe2—O1vii86.02 (9)O12v—Na1—Fe1v39.97 (5)
O2—Fe2—O1vii98.23 (9)O5v—Na1—Fe1v81.35 (8)
O5—Fe2—O1vii89.01 (8)Mo2v—Na1—Fe1v64.68 (4)
O17—Fe2—O1vii170.84 (9)O4—Na1—Mo3vii84.71 (9)
O1vi—Fe2—O1vii82.67 (7)O14—Na1—Mo3vii159.85 (18)
O20—Fe3—O882.27 (10)O15vii—Na1—Mo3vii26.78 (6)
O20—Fe3—O11vii100.59 (9)O12v—Na1—Mo3vii96.47 (7)
O8—Fe3—O11vii93.07 (9)O5v—Na1—Mo3vii74.98 (7)
O20—Fe3—O1093.22 (9)Mo2v—Na1—Mo3vii76.12 (4)
O8—Fe3—O1097.32 (9)Fe1v—Na1—Mo3vii136.43 (7)
O11vii—Fe3—O10163.72 (8)O4—Na1—Mo377.02 (9)
O20—Fe3—O13i179.04 (9)O14—Na1—Mo324.55 (6)
O8—Fe3—O13i96.77 (9)O15vii—Na1—Mo3139.84 (17)
O11vii—Fe3—O13i79.32 (7)O12v—Na1—Mo399.09 (8)
O10—Fe3—O13i87.02 (7)O5v—Na1—Mo3127.84 (11)
O20—Fe3—O1292.66 (9)Mo2v—Na1—Mo3125.41 (6)
O8—Fe3—O12174.28 (9)Fe1v—Na1—Mo361.36 (4)
O11vii—Fe3—O1290.45 (7)Mo3vii—Na1—Mo3156.57 (10)
O2iii—Mo4—O1—Fe2vi175.91 (13)O11vii—Fe3—O12—Mo242.05 (13)
O19—Mo4—O1—Fe2vi65.72 (17)O10—Fe3—O12—Mo2151.39 (14)
O17—Mo4—O1—Fe2vi54.75 (15)O13i—Fe3—O12—Mo2121.35 (13)
O2iii—Mo4—O1—Fe2ii24.55 (18)O20—Fe3—O12—Fe189.95 (9)
O19—Mo4—O1—Fe2ii93.82 (16)O8—Fe3—O12—Fe162.5 (9)
O17—Mo4—O1—Fe2ii145.71 (14)O11vii—Fe3—O12—Fe1169.43 (8)
O16iii—Fe2—O2—Mo4iii58.2 (4)O10—Fe3—O12—Fe12.86 (8)
O5—Fe2—O2—Mo4iii127.0 (4)O13i—Fe3—O12—Fe190.13 (8)
O17—Fe2—O2—Mo4iii32.4 (4)O20—Fe3—O12—Na1i178.35 (11)
O1vi—Fe2—O2—Mo4iii111.3 (13)O8—Fe3—O12—Na1i154.2 (8)
O1vii—Fe2—O2—Mo4iii144.3 (4)O11vii—Fe3—O12—Na1i77.72 (10)
O9—Mo1—O3—Fe4viii48.9 (4)O10—Fe3—O12—Na1i88.84 (10)
O11—Mo1—O3—Fe4viii67.2 (4)O13i—Fe3—O12—Na1i1.58 (9)
O10—Mo1—O3—Fe4viii165.0 (4)O8iv—Mo5—O13—Fe3v71.28 (16)
O5—Mo2—O4—Na1164.2 (3)O20—Mo5—O13—Fe3v167.27 (13)
O18—Mo2—O4—Na144.7 (3)O7v—Mo5—O13—Fe3v47.71 (17)
O12—Mo2—O4—Na178.8 (3)O8iv—Mo5—O13—Fe4x67.82 (15)
Na1i—Mo2—O4—Na1130.8 (3)O20—Mo5—O13—Fe4x53.63 (14)
O4—Mo2—O5—Fe221.0 (3)O7v—Mo5—O13—Fe4x173.19 (13)
O18—Mo2—O5—Fe298.2 (2)O16—Mo3—O14—Fe1v70.29 (18)
O12—Mo2—O5—Fe2141.6 (2)O6—Mo3—O14—Fe1v170.15 (15)
Na1i—Mo2—O5—Fe2164.8 (3)O15—Mo3—O14—Fe1v47.92 (19)
O4—Mo2—O5—Na1i143.81 (10)Na1ii—Mo3—O14—Fe1v8.4 (2)
O18—Mo2—O5—Na1i97.01 (10)Na1—Mo3—O14—Fe1v148.0 (3)
O12—Mo2—O5—Na1i23.15 (10)O16—Mo3—O14—Na177.68 (19)
O16iii—Fe2—O5—Mo267.4 (11)O6—Mo3—O14—Na141.9 (2)
O2—Fe2—O5—Mo28.7 (2)O15—Mo3—O14—Na1164.11 (17)
O17—Fe2—O5—Mo298.9 (2)Na1ii—Mo3—O14—Na1156.4 (2)
O1vi—Fe2—O5—Mo2172.3 (2)O16—Mo3—O15—Fe4v177.58 (14)
O1vii—Fe2—O5—Mo289.6 (2)O6—Mo3—O15—Fe4v59.51 (17)
O16iii—Fe2—O5—Na1i131.1 (10)O14—Mo3—O15—Fe4v63.30 (17)
O2—Fe2—O5—Na1i152.78 (13)Na1ii—Mo3—O15—Fe4v170.4 (2)
O17—Fe2—O5—Na1i62.63 (13)Na1—Mo3—O15—Fe4v49.0 (2)
O1vi—Fe2—O5—Na1i26.26 (12)O16—Mo3—O15—Na1ii7.17 (16)
O1vii—Fe2—O5—Na1i108.95 (12)O6—Mo3—O15—Na1ii110.90 (14)
O16—Mo3—O6—Fe149.3 (3)O14—Mo3—O15—Na1ii126.29 (13)
O15—Mo3—O6—Fe167.4 (3)Na1—Mo3—O15—Na1ii140.63 (16)
O14—Mo3—O6—Fe1168.4 (3)O6—Mo3—O16—Fe2iii69.3 (4)
Na1ii—Mo3—O6—Fe127.4 (3)O15—Mo3—O16—Fe2iii172.6 (4)
Na1—Mo3—O6—Fe1147.2 (3)O14—Mo3—O16—Fe2iii50.9 (4)
O19—Fe1—O6—Mo368.6 (3)Na1ii—Mo3—O16—Fe2iii177.3 (4)
O18ii—Fe1—O6—Mo327.4 (3)Na1—Mo3—O16—Fe2iii18.7 (4)
O10—Fe1—O6—Mo3117.9 (3)O2iii—Mo4—O17—Fe292.94 (19)
O14i—Fe1—O6—Mo3132.4 (16)O19—Mo4—O17—Fe225.4 (2)
O12—Fe1—O6—Mo3160.0 (3)O1—Mo4—O17—Fe2147.01 (17)
Na1i—Fe1—O6—Mo3135.6 (3)O16iii—Fe2—O17—Mo4157.97 (19)
O3viii—Fe4—O7—Mo5i54.0 (5)O2—Fe2—O17—Mo467.35 (19)
O15i—Fe4—O7—Mo5i122.8 (5)O5—Fe2—O17—Mo420.8 (2)
O9i—Fe4—O7—Mo5i26.2 (5)O1vi—Fe2—O17—Mo4109.15 (19)
O13ix—Fe4—O7—Mo5i158.2 (3)O1vii—Fe2—O17—Mo4133.8 (4)
O11—Fe4—O7—Mo5i149.2 (5)O4—Mo2—O18—Fe1vii84.4 (4)
O20—Fe3—O8—Mo5iv114.6 (8)O5—Mo2—O18—Fe1vii35.5 (4)
O11vii—Fe3—O8—Mo5iv14.3 (8)O12—Mo2—O18—Fe1vii152.0 (4)
O10—Fe3—O8—Mo5iv153.2 (8)Na1i—Mo2—O18—Fe1vii98.2 (4)
O13i—Fe3—O8—Mo5iv65.3 (8)O2iii—Mo4—O19—Fe159.6 (5)
O12—Fe3—O8—Mo5iv142.2 (7)O17—Mo4—O19—Fe1178.9 (4)
O3—Mo1—O9—Fe4v91.0 (7)O1—Mo4—O19—Fe158.5 (5)
O11—Mo1—O9—Fe4v152.9 (7)O6—Fe1—O19—Mo477.4 (5)
O10—Mo1—O9—Fe4v26.2 (7)O18ii—Fe1—O19—Mo413.0 (5)
O9—Mo1—O10—Fe171.48 (15)O10—Fe1—O19—Mo4166.7 (5)
O3—Mo1—O10—Fe1169.75 (13)O14i—Fe1—O19—Mo4105.1 (5)
O11—Mo1—O10—Fe148.39 (15)O12—Fe1—O19—Mo4163.9 (5)
O9—Mo1—O10—Fe392.94 (16)Na1i—Fe1—O19—Mo4148.1 (5)
O3—Mo1—O10—Fe325.83 (18)O8iv—Mo5—O20—Fe340.1 (4)
O11—Mo1—O10—Fe3147.18 (13)O7v—Mo5—O20—Fe380.2 (3)
O19—Fe1—O10—Mo1158.8 (7)O13—Mo5—O20—Fe3158.4 (3)
O6—Fe1—O10—Mo185.21 (13)O8—Fe3—O20—Mo526.4 (3)
O18ii—Fe1—O10—Mo15.00 (14)O11vii—Fe3—O20—Mo5118.1 (3)
O14i—Fe1—O10—Mo197.48 (13)O10—Fe3—O20—Mo570.6 (3)
O12—Fe1—O10—Mo1171.50 (14)O13i—Fe3—O20—Mo534 (5)
Na1i—Fe1—O10—Mo1140.83 (11)O12—Fe3—O20—Mo5150.9 (3)
O19—Fe1—O10—Fe332.7 (8)Mo2—O4—Na1—O14101.2 (3)
O6—Fe1—O10—Fe383.26 (9)Mo2—O4—Na1—O15vii34.3 (4)
O18ii—Fe1—O10—Fe3173.47 (10)Mo2—O4—Na1—O12v38.0 (9)
O14i—Fe1—O10—Fe394.05 (9)Mo2—O4—Na1—O5v126.5 (3)
O12—Fe1—O10—Fe33.03 (8)Mo2—O4—Na1—Mo2v100.9 (5)
Na1i—Fe1—O10—Fe350.70 (8)Mo2—O4—Na1—Fe1v111.6 (3)
O20—Fe3—O10—Mo177.87 (15)Mo2—O4—Na1—Mo3vii59.3 (3)
O8—Fe3—O10—Mo14.74 (16)Mo2—O4—Na1—Mo3105.9 (3)
O11vii—Fe3—O10—Mo1134.0 (2)Mo3—O14—Na1—O411.1 (2)
O13i—Fe3—O10—Mo1101.19 (15)Fe1v—O14—Na1—O4168.70 (15)
O12—Fe3—O10—Mo1170.02 (16)Mo3—O14—Na1—O15vii118.09 (16)
O20—Fe3—O10—Fe189.15 (10)Fe1v—O14—Na1—O15vii84.35 (18)
O8—Fe3—O10—Fe1171.77 (10)Mo3—O14—Na1—O12v178.05 (13)
O11vii—Fe3—O10—Fe159.0 (3)Fe1v—O14—Na1—O12v20.49 (11)
O13i—Fe3—O10—Fe191.79 (9)Mo3—O14—Na1—O5v127.44 (13)
O12—Fe3—O10—Fe13.00 (8)Fe1v—O14—Na1—O5v30.12 (17)
O9—Mo1—O11—Fe3ii18.63 (17)Mo3—O14—Na1—Mo2v159.25 (11)
O3—Mo1—O11—Fe3ii99.85 (15)Fe1v—O14—Na1—Mo2v1.70 (14)
O10—Mo1—O11—Fe3ii138.15 (13)Mo3—O14—Na1—Fe1v157.55 (19)
O9—Mo1—O11—Fe4177.92 (12)Mo3—O14—Na1—Mo3vii116.4 (3)
O3—Mo1—O11—Fe459.44 (14)Fe1v—O14—Na1—Mo3vii86.1 (3)
O10—Mo1—O11—Fe462.56 (13)Fe1v—O14—Na1—Mo3157.55 (19)
O7—Fe4—O11—Mo115.69 (12)O16—Mo3—Na1—O480.97 (15)
O3viii—Fe4—O11—Mo177.13 (12)O6—Mo3—Na1—O427.72 (14)
O15i—Fe4—O11—Mo1103.75 (12)O15—Mo3—Na1—O4143.71 (14)
O9i—Fe4—O11—Mo159.0 (10)O14—Mo3—Na1—O4168.8 (3)
O13ix—Fe4—O11—Mo1166.97 (13)Na1ii—Mo3—Na1—O4140.3 (2)
O7—Fe4—O11—Fe3ii179.34 (10)O16—Mo3—Na1—O14110.26 (18)
O3viii—Fe4—O11—Fe3ii87.83 (9)O6—Mo3—Na1—O14141.05 (19)
O15i—Fe4—O11—Fe3ii91.28 (9)O15—Mo3—Na1—O1425.1 (3)
O9i—Fe4—O11—Fe3ii106.0 (10)Na1ii—Mo3—Na1—O1450.9 (4)
O13ix—Fe4—O11—Fe3ii2.01 (8)O16—Mo3—Na1—O15vii162.33 (18)
O4—Mo2—O12—Fe153.14 (16)O6—Mo3—Na1—O15vii53.64 (17)
O5—Mo2—O12—Fe166.36 (15)O15—Mo3—Na1—O15vii62.35 (18)
O18—Mo2—O12—Fe1175.07 (13)O14—Mo3—Na1—O15vii87.4 (2)
Na1i—Mo2—O12—Fe192.21 (15)Na1ii—Mo3—Na1—O15vii138.3 (2)
O4—Mo2—O12—Fe387.06 (15)O16—Mo3—Na1—O12v108.35 (14)
O5—Mo2—O12—Fe3153.44 (13)O6—Mo3—Na1—O12v142.95 (15)
O18—Mo2—O12—Fe334.87 (17)O15—Mo3—Na1—O12v27.0 (2)
Na1i—Mo2—O12—Fe3127.59 (17)O14—Mo3—Na1—O12v1.90 (13)
O4—Mo2—O12—Na1i145.35 (12)Na1ii—Mo3—Na1—O12v49.0 (4)
O5—Mo2—O12—Na1i25.84 (12)O16—Mo3—Na1—O5v44.59 (17)
O18—Mo2—O12—Na1i92.72 (13)O6—Mo3—Na1—O5v153.29 (16)
O19—Fe1—O12—Mo230.70 (15)O15—Mo3—Na1—O5v90.7 (2)
O6—Fe1—O12—Mo261.65 (14)O14—Mo3—Na1—O5v65.67 (16)
O18ii—Fe1—O12—Mo2127.4 (6)Na1ii—Mo3—Na1—O5v14.8 (4)
O10—Fe1—O12—Mo2152.86 (14)O16—Mo3—Na1—Mo2v85.17 (17)
O14i—Fe1—O12—Mo2117.03 (13)O6—Mo3—Na1—Mo2v166.14 (17)
Na1i—Fe1—O12—Mo295.42 (17)O15—Mo3—Na1—Mo2v50.2 (2)
O19—Fe1—O12—Fe3179.36 (10)O14—Mo3—Na1—Mo2v25.09 (13)
O6—Fe1—O12—Fe388.30 (9)Na1ii—Mo3—Na1—Mo2v25.8 (4)
O18ii—Fe1—O12—Fe322.5 (7)O16—Mo3—Na1—Fe1v94.70 (10)
O10—Fe1—O12—Fe32.91 (8)O6—Mo3—Na1—Fe1v156.61 (10)
O14i—Fe1—O12—Fe393.03 (9)O15—Mo3—Na1—Fe1v40.63 (17)
Na1i—Fe1—O12—Fe3114.63 (13)O14—Mo3—Na1—Fe1v15.56 (14)
O19—Fe1—O12—Na1i64.72 (13)Na1ii—Mo3—Na1—Fe1v35.3 (3)
O6—Fe1—O12—Na1i157.07 (13)O16—Mo3—Na1—Mo3vii120.7 (3)
O18ii—Fe1—O12—Na1i137.2 (6)O6—Mo3—Na1—Mo3vii12.0 (3)
O10—Fe1—O12—Na1i111.72 (12)O15—Mo3—Na1—Mo3vii104.0 (3)
O14i—Fe1—O12—Na1i21.61 (12)O14—Mo3—Na1—Mo3vii129.1 (4)
O20—Fe3—O12—Mo258.58 (14)Na1ii—Mo3—Na1—Mo3vii180.0
O8—Fe3—O12—Mo286.0 (9)
Symmetry codes: (i) x+1, y, z; (ii) x, y+1, z; (iii) x+1, y+1, z+1; (iv) x+1, y+1, z; (v) x1, y, z; (vi) x+2, y+1, z+1; (vii) x, y1, z; (viii) x+2, y+2, z; (ix) x+1, y+1, z; (x) x1, y1, z.
(2) top
Crystal data top
Fe2Mo3NaO12Z = 2
Mr = 614.51F(000) = 570
?, P1Dx = 3.955 Mg m3
a = 6.9253 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 6.9513 (4) ÅCell parameters from 3616 reflections
c = 11.0600 (9) Åθ = 4.4–33.6°
α = 80.205 (6)°µ = 6.39 mm1
β = 83.679 (6)°T = 293 K
γ = 80.818 (5)°Prism, black
V = 516.06 (6) Å30.20 × 0.11 × 0.10 mm
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector2705 independent reflections
Radiation source: fine-focus sealed tube2454 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
Rotation method data acquisition using ω and phi scans(s)θmax = 33.6°, θmin = 4.4°
Absorption correction: numeric analytical
?
h = 109
Tmin = 0.321, Tmax = 0.565k = 910
4259 measured reflectionsl = 1414
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) + (0.0365P)2 + 2.671P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.081(Δ/σ)max < 0.001
S = 1.14Δρmax = 0.98 e Å3
2705 reflectionsΔρmin = 2.03 e Å3
164 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0156 (8)
Crystal data top
Fe2Mo3NaO12γ = 80.818 (5)°
Mr = 614.51V = 516.06 (6) Å3
?, P1Z = 2
a = 6.9253 (4) ÅMo Kα radiation
b = 6.9513 (4) ŵ = 6.39 mm1
c = 11.0600 (9) ÅT = 293 K
α = 80.205 (6)°0.20 × 0.11 × 0.10 mm
β = 83.679 (6)°
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector2705 independent reflections
Absorption correction: numeric analytical
?
2454 reflections with I > 2σ(I)
Tmin = 0.321, Tmax = 0.565Rint = 0.027
4259 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.031164 parameters
wR(F2) = 0.0810 restraints
S = 1.14Δρmax = 0.98 e Å3
2705 reflectionsΔρmin = 2.03 e Å3
Special details top

Experimental. CrysAlis RED, Oxford Diffraction Ltd., version 170.17, 2003 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R·C. Clark & J·S. Reid.

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*/Ueq
Mo10.24084 (5)0.10003 (5)0.14829 (4)0.00931 (11)
Mo20.29352 (6)0.28215 (6)0.18759 (4)0.01106 (11)
Mo30.27507 (5)0.29702 (6)0.45490 (4)0.00914 (11)
Fe10.18523 (10)0.17115 (10)0.49169 (6)0.01079 (15)
Fe20.22673 (9)0.22574 (9)0.11109 (6)0.00912 (14)
Na10.1449 (5)0.4105 (4)0.1825 (5)0.0754 (15)
O10.1854 (5)0.1492 (5)0.0730 (3)0.0134 (7)
O20.2019 (5)0.4883 (5)0.0913 (3)0.0157 (7)
O30.0680 (5)0.2519 (5)0.1270 (4)0.0157 (7)
O40.4820 (5)0.2054 (5)0.1055 (4)0.0173 (7)
O50.1598 (5)0.2336 (6)0.3193 (4)0.0192 (8)
O60.2230 (6)0.0876 (6)0.3043 (4)0.0228 (8)
O70.5182 (5)0.2093 (6)0.4969 (4)0.0226 (8)
O80.1231 (5)0.1336 (5)0.4939 (3)0.0152 (7)
O90.2497 (6)0.2997 (6)0.2949 (4)0.0224 (8)
O100.2104 (6)0.5362 (5)0.5330 (4)0.0225 (8)
O110.5392 (5)0.3423 (6)0.2296 (4)0.0218 (8)
O120.2560 (6)0.0662 (5)0.1151 (4)0.0214 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.00706 (17)0.00943 (17)0.0108 (2)0.00111 (13)0.00230 (13)0.00097 (14)
Mo20.00997 (18)0.00875 (17)0.0142 (2)0.00137 (13)0.00341 (14)0.00057 (14)
Mo30.00863 (17)0.00980 (16)0.0097 (2)0.00336 (13)0.00204 (13)0.00078 (14)
Fe10.0094 (3)0.0104 (3)0.0122 (3)0.0004 (2)0.0025 (2)0.0008 (2)
Fe20.0077 (3)0.0086 (3)0.0110 (3)0.0014 (2)0.0024 (2)0.0001 (2)
Na10.0297 (16)0.0267 (14)0.183 (5)0.0092 (13)0.046 (2)0.041 (2)
O10.0159 (16)0.0120 (14)0.0113 (16)0.0004 (12)0.0033 (13)0.0006 (13)
O20.0202 (17)0.0115 (14)0.0149 (17)0.0024 (13)0.0014 (14)0.0028 (13)
O30.0100 (14)0.0149 (15)0.0237 (19)0.0048 (12)0.0047 (14)0.0019 (14)
O40.0106 (15)0.0161 (16)0.024 (2)0.0016 (13)0.0008 (14)0.0004 (15)
O50.0148 (16)0.0212 (17)0.0204 (19)0.0001 (14)0.0051 (15)0.0002 (15)
O60.030 (2)0.0234 (18)0.0132 (18)0.0004 (16)0.0043 (16)0.0001 (15)
O70.0120 (16)0.030 (2)0.026 (2)0.0044 (15)0.0009 (15)0.0068 (17)
O80.0135 (15)0.0153 (15)0.0188 (18)0.0055 (13)0.0057 (14)0.0023 (14)
O90.028 (2)0.030 (2)0.0112 (18)0.0100 (17)0.0012 (15)0.0045 (16)
O100.027 (2)0.0138 (16)0.025 (2)0.0044 (15)0.0050 (17)0.0028 (16)
O110.0124 (16)0.0275 (19)0.024 (2)0.0026 (14)0.0009 (15)0.0002 (17)
O120.0253 (19)0.0093 (14)0.031 (2)0.0063 (14)0.0037 (17)0.0022 (15)
Geometric parameters (Å, º) top
Mo1—O61.733 (4)Fe2—O2viii2.015 (3)
Mo1—O41.761 (3)Fe2—O3ii2.044 (3)
Mo1—O31.776 (4)Fe2—Na1ix3.366 (3)
Mo1—O11.792 (3)Na1—O11vii2.262 (5)
Mo1—Na1i3.520 (3)Na1—O3viii2.313 (5)
Mo1—Na13.581 (3)Na1—O12.314 (5)
Mo2—O111.718 (4)Na1—O2ii2.648 (5)
Mo2—O51.767 (4)Na1—O5ii2.783 (6)
Mo2—O121.789 (4)Na1—O2viii2.987 (7)
Mo2—O21.792 (4)Na1—Mo2ii3.290 (3)
Mo2—Na1ii3.290 (3)Na1—Fe2ix3.366 (3)
Mo3—O71.738 (4)Na1—Mo1viii3.520 (3)
Mo3—O101.752 (4)O2—Fe2i2.015 (3)
Mo3—O91.761 (4)O2—Na1ii2.648 (5)
Mo3—O81.797 (4)O2—Na1i2.987 (7)
Fe1—O7iii2.034 (4)O3—Fe2ii2.044 (3)
Fe1—O62.054 (4)O3—Na1i2.313 (5)
Fe1—O5iv2.055 (4)O4—Fe2vii2.007 (4)
Fe1—O10v2.076 (4)O5—Fe1x2.055 (4)
Fe1—O82.108 (4)O5—Na1ii2.783 (6)
Fe1—O8vi2.123 (4)O7—Fe1xi2.034 (4)
Fe2—O9ii2.006 (4)O8—Fe1vi2.123 (4)
Fe2—O4vii2.007 (4)O9—Fe2ii2.006 (4)
Fe2—O122.015 (4)O10—Fe1v2.076 (4)
Fe2—O12.016 (4)O11—Na1vii2.262 (5)
O6—Mo1—O4108.08 (19)O3viii—Na1—O1133.0 (3)
O6—Mo1—O3106.7 (2)O11vii—Na1—O2ii171.0 (3)
O4—Mo1—O3111.02 (17)O3viii—Na1—O2ii71.10 (14)
O6—Mo1—O1105.78 (17)O1—Na1—O2ii82.74 (15)
O4—Mo1—O1111.94 (17)O11vii—Na1—O5ii123.8 (2)
O3—Mo1—O1112.94 (16)O3viii—Na1—O5ii113.73 (17)
O6—Mo1—Na1i95.89 (17)O1—Na1—O5ii85.72 (16)
O4—Mo1—Na1i83.46 (13)O2ii—Na1—O5ii62.96 (13)
O3—Mo1—Na1i35.37 (12)O11vii—Na1—O2viii100.5 (2)
O1—Mo1—Na1i147.05 (13)O3viii—Na1—O2viii70.95 (18)
O6—Mo1—Na172.39 (16)O1—Na1—O2viii63.72 (17)
O4—Mo1—Na1119.37 (13)O2ii—Na1—O2viii70.76 (17)
O3—Mo1—Na1127.24 (12)O5ii—Na1—O2viii127.07 (16)
O1—Mo1—Na133.64 (14)O11vii—Na1—Mo2ii151.08 (19)
Na1i—Mo1—Na1156.39 (14)O3viii—Na1—Mo2ii99.50 (13)
O11—Mo2—O5109.94 (19)O1—Na1—Mo2ii73.89 (12)
O11—Mo2—O12109.6 (2)O2ii—Na1—Mo2ii32.93 (9)
O5—Mo2—O12108.85 (18)O5ii—Na1—Mo2ii32.48 (9)
O11—Mo2—O2109.98 (18)O2viii—Na1—Mo2ii95.34 (13)
O5—Mo2—O2105.78 (18)O11vii—Na1—Fe2ix144.67 (16)
O12—Mo2—O2112.66 (18)O3viii—Na1—Fe2ix36.60 (10)
O11—Mo2—Na1ii144.94 (16)O1—Na1—Fe2ix116.36 (16)
O5—Mo2—Na1ii57.77 (16)O2ii—Na1—Fe2ix36.75 (8)
O12—Mo2—Na1ii105.49 (15)O5ii—Na1—Fe2ix81.71 (11)
O2—Mo2—Na1ii53.43 (14)O2viii—Na1—Fe2ix75.90 (12)
O7—Mo3—O10110.3 (2)Mo2ii—Na1—Fe2ix62.90 (5)
O7—Mo3—O9108.2 (2)O11vii—Na1—Mo1viii82.35 (14)
O10—Mo3—O9109.7 (2)O3viii—Na1—Mo1viii26.38 (9)
O7—Mo3—O8108.16 (18)O1—Na1—Mo1viii140.2 (2)
O10—Mo3—O8109.98 (18)O2ii—Na1—Mo1viii97.48 (12)
O9—Mo3—O8110.52 (18)O5ii—Na1—Mo1viii129.88 (15)
O7iii—Fe1—O688.97 (17)O2viii—Na1—Mo1viii78.73 (12)
O7iii—Fe1—O5iv88.46 (16)Mo2ii—Na1—Mo1viii124.72 (8)
O6—Fe1—O5iv174.82 (17)Fe2ix—Na1—Mo1viii62.38 (5)
O7iii—Fe1—O10v88.11 (17)O11vii—Na1—Mo180.67 (13)
O6—Fe1—O10v89.94 (17)O3viii—Na1—Mo1158.4 (2)
O5iv—Fe1—O10v94.47 (16)O1—Na1—Mo125.40 (10)
O7iii—Fe1—O8177.76 (16)O2ii—Na1—Mo196.76 (11)
O6—Fe1—O893.26 (16)O5ii—Na1—Mo173.58 (11)
O5iv—Fe1—O889.30 (15)O2viii—Na1—Mo188.36 (13)
O10v—Fe1—O892.16 (15)Mo2ii—Na1—Mo175.73 (6)
O7iii—Fe1—O8vi99.01 (15)Fe2ix—Na1—Mo1133.48 (10)
O6—Fe1—O8vi87.28 (15)Mo1viii—Na1—Mo1156.39 (14)
O5iv—Fe1—O8vi88.69 (15)Mo1—O1—Fe2122.44 (18)
O10v—Fe1—O8vi172.30 (15)Mo1—O1—Na1121.0 (2)
O8—Fe1—O8vi80.84 (15)Fe2—O1—Na1114.6 (2)
O9ii—Fe2—O4vii91.60 (17)Mo2—O2—Fe2i131.6 (2)
O9ii—Fe2—O1294.29 (17)Mo2—O2—Na1ii93.64 (18)
O4vii—Fe2—O1289.91 (16)Fe2i—O2—Na1ii91.40 (15)
O9ii—Fe2—O1176.27 (16)Mo2—O2—Na1i131.14 (18)
O4vii—Fe2—O192.06 (15)Fe2i—O2—Na1i91.50 (14)
O12—Fe2—O185.01 (16)Na1ii—O2—Na1i109.24 (17)
O9ii—Fe2—O2viii90.58 (16)Mo1—O3—Fe2ii138.11 (19)
O4vii—Fe2—O2viii88.68 (15)Mo1—O3—Na1i118.24 (18)
O12—Fe2—O2viii174.97 (17)Fe2ii—O3—Na1i100.98 (16)
O1—Fe2—O2viii90.21 (15)Mo1—O4—Fe2vii150.6 (2)
O9ii—Fe2—O3ii85.24 (16)Mo2—O5—Fe1x143.8 (2)
O4vii—Fe2—O3ii176.83 (16)Mo2—O5—Na1ii89.74 (18)
O12—Fe2—O3ii90.59 (15)Fe1x—O5—Na1ii123.82 (19)
O1—Fe2—O3ii91.10 (15)Mo1—O6—Fe1160.2 (3)
O2viii—Fe2—O3ii91.08 (15)Mo3—O7—Fe1xi156.5 (3)
O9ii—Fe2—Na1ix73.06 (15)Mo3—O8—Fe1128.50 (19)
O4vii—Fe2—Na1ix136.17 (12)Mo3—O8—Fe1vi130.62 (18)
O12—Fe2—Na1ix131.06 (13)Fe1—O8—Fe1vi99.16 (15)
O1—Fe2—Na1ix104.66 (14)Mo3—O9—Fe2ii164.9 (3)
O2viii—Fe2—Na1ix51.85 (12)Mo3—O10—Fe1v140.7 (2)
O3ii—Fe2—Na1ix42.42 (11)Mo2—O11—Na1vii150.7 (3)
O11vii—Na1—O3viii108.48 (19)Mo2—O12—Fe2155.1 (3)
O11vii—Na1—O191.64 (18)
O6—Mo1—Na1—O11vii72.7 (2)O11—Mo2—O2—Fe2i49.5 (3)
O4—Mo1—Na1—O11vii28.6 (3)O5—Mo2—O2—Fe2i69.2 (3)
O3—Mo1—Na1—O11vii170.6 (2)O12—Mo2—O2—Fe2i172.0 (2)
O1—Mo1—Na1—O11vii114.4 (3)Na1ii—Mo2—O2—Fe2i95.1 (3)
Na1i—Mo1—Na1—O11vii135.5 (3)O11—Mo2—O2—Na1ii144.57 (19)
O6—Mo1—Na1—O3viii170.1 (5)O5—Mo2—O2—Na1ii25.90 (19)
O4—Mo1—Na1—O3viii88.7 (5)O12—Mo2—O2—Na1ii92.9 (2)
O3—Mo1—Na1—O3viii72.2 (5)O11—Mo2—O2—Na1i95.8 (2)
O1—Mo1—Na1—O3viii2.8 (4)O5—Mo2—O2—Na1i145.5 (2)
Na1i—Mo1—Na1—O3viii107.3 (6)O12—Mo2—O2—Na1i26.7 (3)
O6—Mo1—Na1—O1172.9 (3)Na1ii—Mo2—O2—Na1i119.6 (3)
O4—Mo1—Na1—O185.9 (3)O6—Mo1—O3—Fe2ii81.0 (3)
O3—Mo1—Na1—O175.0 (3)O4—Mo1—O3—Fe2ii161.5 (3)
Na1i—Mo1—Na1—O1110.1 (4)O1—Mo1—O3—Fe2ii34.8 (4)
O6—Mo1—Na1—O2ii116.0 (2)Na1i—Mo1—O3—Fe2ii157.3 (5)
O4—Mo1—Na1—O2ii142.76 (19)Na1—Mo1—O3—Fe2ii0.7 (4)
O3—Mo1—Na1—O2ii18.1 (3)O6—Mo1—O3—Na1i76.3 (3)
O1—Mo1—Na1—O2ii56.9 (2)O4—Mo1—O3—Na1i41.2 (3)
Na1i—Mo1—Na1—O2ii53.2 (5)O1—Mo1—O3—Na1i167.9 (2)
O6—Mo1—Na1—O5ii56.81 (19)Na1—Mo1—O3—Na1i156.6 (3)
O4—Mo1—Na1—O5ii158.06 (17)O6—Mo1—O4—Fe2vii44.5 (5)
O3—Mo1—Na1—O5ii41.1 (2)O3—Mo1—O4—Fe2vii161.1 (4)
O1—Mo1—Na1—O5ii116.1 (2)O1—Mo1—O4—Fe2vii71.6 (5)
Na1i—Mo1—Na1—O5ii6.0 (4)Na1i—Mo1—O4—Fe2vii138.6 (5)
O6—Mo1—Na1—O2viii173.61 (19)Na1—Mo1—O4—Fe2vii35.1 (5)
O4—Mo1—Na1—O2viii72.36 (18)O11—Mo2—O5—Fe1x16.3 (4)
O3—Mo1—Na1—O2viii88.5 (2)O12—Mo2—O5—Fe1x103.7 (4)
O1—Mo1—Na1—O2viii13.5 (2)O2—Mo2—O5—Fe1x135.0 (3)
Na1i—Mo1—Na1—O2viii123.6 (4)Na1ii—Mo2—O5—Fe1x159.5 (4)
O6—Mo1—Na1—Mo2ii90.46 (17)O11—Mo2—O5—Na1ii143.20 (17)
O4—Mo1—Na1—Mo2ii168.30 (15)O12—Mo2—O5—Na1ii96.80 (18)
O3—Mo1—Na1—Mo2ii7.4 (2)O2—Mo2—O5—Na1ii24.50 (17)
O1—Mo1—Na1—Mo2ii82.4 (2)O4—Mo1—O6—Fe183.9 (8)
Na1i—Mo1—Na1—Mo2ii27.7 (4)O3—Mo1—O6—Fe135.5 (8)
O6—Mo1—Na1—Fe2ix117.7 (3)O1—Mo1—O6—Fe1156.0 (7)
O4—Mo1—Na1—Fe2ix141.1 (2)Na1i—Mo1—O6—Fe11.1 (7)
O3—Mo1—Na1—Fe2ix19.8 (3)Na1—Mo1—O6—Fe1160.1 (8)
O1—Mo1—Na1—Fe2ix55.2 (3)O7iii—Fe1—O6—Mo1101.0 (7)
Na1i—Mo1—Na1—Fe2ix54.9 (6)O5iv—Fe1—O6—Mo1161.2 (13)
O6—Mo1—Na1—Mo1viii117.2 (4)O10v—Fe1—O6—Mo112.9 (7)
O4—Mo1—Na1—Mo1viii16.0 (4)O8—Fe1—O6—Mo179.2 (7)
O3—Mo1—Na1—Mo1viii144.9 (3)O8vi—Fe1—O6—Mo1159.9 (7)
O1—Mo1—Na1—Mo1viii69.9 (4)O10—Mo3—O7—Fe1xi83.8 (7)
Na1i—Mo1—Na1—Mo1viii180.0O9—Mo3—O7—Fe1xi36.2 (7)
O6—Mo1—O1—Fe2169.9 (2)O8—Mo3—O7—Fe1xi155.9 (6)
O4—Mo1—O1—Fe252.5 (3)O7—Mo3—O8—Fe1170.7 (2)
O3—Mo1—O1—Fe273.7 (3)O10—Mo3—O8—Fe150.2 (3)
Na1i—Mo1—O1—Fe260.9 (4)O9—Mo3—O8—Fe171.1 (3)
Na1—Mo1—O1—Fe2162.9 (4)O7—Mo3—O8—Fe1vi27.5 (3)
O6—Mo1—O1—Na17.0 (3)O10—Mo3—O8—Fe1vi148.0 (3)
O4—Mo1—O1—Na1110.4 (2)O9—Mo3—O8—Fe1vi90.7 (3)
O3—Mo1—O1—Na1123.4 (2)O7iii—Fe1—O8—Mo3107 (4)
Na1i—Mo1—O1—Na1136.3 (3)O6—Fe1—O8—Mo379.4 (3)
O9ii—Fe2—O1—Mo193 (2)O5iv—Fe1—O8—Mo3105.1 (3)
O4vii—Fe2—O1—Mo176.2 (2)O10v—Fe1—O8—Mo310.6 (3)
O12—Fe2—O1—Mo113.5 (2)O8vi—Fe1—O8—Mo3166.1 (4)
O2viii—Fe2—O1—Mo1164.9 (2)O7iii—Fe1—O8—Fe1vi86 (4)
O3ii—Fe2—O1—Mo1104.0 (2)O6—Fe1—O8—Fe1vi86.71 (17)
Na1ix—Fe2—O1—Mo1144.73 (19)O5iv—Fe1—O8—Fe1vi88.79 (16)
O9ii—Fe2—O1—Na1103 (2)O10v—Fe1—O8—Fe1vi176.77 (17)
O4vii—Fe2—O1—Na187.70 (19)O8vi—Fe1—O8—Fe1vi0.0
O12—Fe2—O1—Na1177.4 (2)O7—Mo3—O9—Fe2ii73.6 (10)
O2viii—Fe2—O1—Na10.99 (19)O10—Mo3—O9—Fe2ii166.1 (9)
O3ii—Fe2—O1—Na192.08 (19)O8—Mo3—O9—Fe2ii44.7 (10)
Na1ix—Fe2—O1—Na151.4 (2)O7—Mo3—O10—Fe1v97.0 (4)
O11vii—Na1—O1—Mo164.0 (3)O9—Mo3—O10—Fe1v22.1 (4)
O3viii—Na1—O1—Mo1178.6 (2)O8—Mo3—O10—Fe1v143.8 (3)
O2ii—Na1—O1—Mo1123.0 (2)O5—Mo2—O11—Na1vii173.1 (5)
O5ii—Na1—O1—Mo159.8 (2)O12—Mo2—O11—Na1vii53.5 (5)
O2viii—Na1—O1—Mo1164.9 (2)O2—Mo2—O11—Na1vii70.9 (5)
Mo2ii—Na1—O1—Mo190.6 (2)Na1ii—Mo2—O11—Na1vii125.0 (5)
Fe2ix—Na1—O1—Mo1138.3 (2)O11—Mo2—O12—Fe279.2 (6)
Mo1viii—Na1—O1—Mo1143.99 (19)O5—Mo2—O12—Fe241.0 (6)
O11vii—Na1—O1—Fe2100.2 (2)O2—Mo2—O12—Fe2158.0 (5)
O3viii—Na1—O1—Fe217.3 (3)Na1ii—Mo2—O12—Fe2101.7 (6)
O2ii—Na1—O1—Fe272.8 (2)O9ii—Fe2—O12—Mo22.3 (6)
O5ii—Na1—O1—Fe2136.07 (19)O4vii—Fe2—O12—Mo289.3 (6)
O2viii—Na1—O1—Fe20.74 (15)O1—Fe2—O12—Mo2178.7 (6)
Mo2ii—Na1—O1—Fe2105.27 (17)O2viii—Fe2—O12—Mo2162.9 (15)
Fe2ix—Na1—O1—Fe257.5 (3)O3ii—Fe2—O12—Mo287.6 (6)
Mo1viii—Na1—O1—Fe220.2 (3)Na1ix—Fe2—O12—Mo273.5 (6)
Mo1—Na1—O1—Fe2164.2 (3)
Symmetry codes: (i) x, y+1, z; (ii) x, y, z; (iii) x1, y, z; (iv) x, y, z1; (v) x, y+1, z1; (vi) x, y, z1; (vii) x1, y, z; (viii) x, y1, z; (ix) x, y1, z; (x) x, y, z+1; (xi) x+1, y, z.
(3) top
Crystal data top
Fe2Mo3NaO12Z = 2
Mr = 614.51F(000) = 570
?, P1Dx = 3.945 Mg m3
a = 6.834 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 6.893 (1) ÅCell parameters from 1012 reflections
c = 11.667 (3) Åθ = 3.0–30.3°
α = 76.23 (2)°µ = 6.37 mm1
β = 75.78 (2)°T = 293 K
γ = 87.76 (2)°Prism, black
V = 517.33 (17) Å30.07 × 0.02 × 0.01 mm
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector2180 independent reflections
Radiation source: fine-focus sealed tube1188 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
Rotation method data acquisition using ω and phi scans(s)θmax = 30.3°, θmin = 3.0°
Absorption correction: numeric analytical
?
h = 98
Tmin = 0.683, Tmax = 0.923k = 99
4315 measured reflectionsl = 1516
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.036Secondary atom site location: difference Fourier map
wR(F2) = 0.129 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.59(Δ/σ)max = 0.007
2180 reflectionsΔρmax = 0.85 e Å3
163 parametersΔρmin = 0.90 e Å3
Crystal data top
Fe2Mo3NaO12γ = 87.76 (2)°
Mr = 614.51V = 517.33 (17) Å3
?, P1Z = 2
a = 6.834 (1) ÅMo Kα radiation
b = 6.893 (1) ŵ = 6.37 mm1
c = 11.667 (3) ÅT = 293 K
α = 76.23 (2)°0.07 × 0.02 × 0.01 mm
β = 75.78 (2)°
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector2180 independent reflections
Absorption correction: numeric analytical
?
1188 reflections with I > 2σ(I)
Tmin = 0.683, Tmax = 0.923Rint = 0.061
4315 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.036163 parameters
wR(F2) = 0.1290 restraints
S = 0.59Δρmax = 0.85 e Å3
2180 reflectionsΔρmin = 0.90 e Å3
Special details top

Experimental. CrysAlis RED, Oxford Diffraction Ltd., version 170.17, 2003 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R·C. Clark & J·S. Reid.

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*/Ueq
Mo10.34846 (18)0.24785 (15)0.10452 (10)0.0104 (3)
Mo20.75174 (18)0.24724 (15)0.50071 (10)0.0084 (3)
Mo30.19510 (18)0.20023 (15)0.25315 (10)0.0096 (3)
Fe10.3263 (3)0.6913 (2)0.19259 (16)0.0087 (4)
Fe20.3054 (3)0.2959 (2)0.40831 (16)0.0100 (4)
Na10.1862 (10)0.6040 (8)0.1423 (6)0.0307 (16)
O10.7263 (14)0.3914 (12)0.6142 (8)0.015 (2)
O20.6696 (15)0.0028 (12)0.5788 (8)0.018 (2)
O30.6114 (14)0.3338 (13)0.3914 (8)0.016 (2)
O40.3607 (14)0.3737 (12)0.2240 (8)0.014 (2)
O50.3092 (16)0.0063 (13)0.1674 (9)0.023 (2)
O60.3816 (13)0.2899 (13)0.1962 (8)0.014 (2)
O71.0024 (14)0.2534 (13)0.4214 (8)0.017 (2)
O80.0346 (14)0.3244 (13)0.2016 (9)0.018 (2)
O90.1767 (17)0.0537 (13)0.2059 (10)0.032 (3)
O100.1525 (15)0.3439 (13)0.0413 (8)0.018 (2)
O110.5773 (14)0.2916 (14)0.0084 (9)0.018 (2)
O120.2605 (17)0.2659 (15)0.4136 (8)0.028 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0099 (8)0.0109 (5)0.0118 (6)0.0002 (4)0.0026 (5)0.0054 (4)
Mo20.0087 (7)0.0082 (5)0.0090 (5)0.0012 (4)0.0028 (5)0.0029 (4)
Mo30.0100 (8)0.0102 (5)0.0090 (5)0.0011 (4)0.0023 (5)0.0026 (4)
Fe10.0098 (12)0.0091 (8)0.0080 (8)0.0021 (7)0.0027 (8)0.0029 (7)
Fe20.0130 (12)0.0079 (8)0.0090 (9)0.0009 (7)0.0030 (8)0.0010 (7)
Na10.033 (4)0.013 (3)0.041 (4)0.001 (2)0.007 (3)0.002 (3)
O10.019 (6)0.011 (4)0.019 (5)0.006 (4)0.007 (5)0.009 (4)
O20.020 (6)0.013 (4)0.022 (5)0.004 (4)0.009 (5)0.005 (4)
O30.003 (6)0.028 (5)0.015 (5)0.004 (4)0.000 (4)0.003 (4)
O40.009 (6)0.009 (4)0.023 (5)0.001 (3)0.005 (4)0.002 (4)
O50.031 (7)0.016 (4)0.025 (5)0.002 (4)0.013 (5)0.005 (4)
O60.004 (6)0.021 (5)0.016 (5)0.000 (4)0.000 (4)0.006 (4)
O70.009 (6)0.027 (5)0.017 (5)0.000 (4)0.004 (4)0.010 (4)
O80.004 (6)0.022 (5)0.028 (6)0.002 (4)0.002 (5)0.010 (4)
O90.032 (8)0.012 (5)0.042 (7)0.003 (4)0.000 (6)0.001 (5)
O100.021 (6)0.017 (4)0.016 (5)0.002 (4)0.009 (5)0.000 (4)
O110.011 (6)0.023 (5)0.022 (5)0.011 (4)0.007 (5)0.008 (4)
O120.039 (8)0.031 (6)0.010 (5)0.004 (5)0.004 (5)0.002 (4)
Geometric parameters (Å, º) top
Mo1—O101.720 (9)Fe2—O32.073 (9)
Mo1—O51.734 (9)Fe2—O1iv2.118 (8)
Mo1—O111.763 (10)Na1—O9iii2.302 (10)
Mo1—O41.827 (9)Na1—O10ii2.382 (12)
Mo1—Na1i3.536 (7)Na1—O102.412 (10)
Mo1—Na13.680 (6)Na1—O62.623 (11)
Mo1—Na1ii3.704 (7)Na1—O82.801 (11)
Mo2—O71.732 (10)Na1—O3i2.832 (11)
Mo2—O21.754 (8)Na1—O11i2.883 (12)
Mo2—O31.759 (8)Na1—O4i3.006 (11)
Mo2—O11.808 (9)Na1—Mo1i3.536 (7)
Mo3—O91.705 (9)Na1—Na1ii3.664 (13)
Mo3—O121.763 (9)O1—Fe2iv2.118 (8)
Mo3—O61.766 (9)O1—Fe1iv2.132 (9)
Mo3—O81.798 (10)O2—Fe2vi2.032 (9)
Mo3—Na13.329 (6)O3—Na1i2.832 (11)
Fe1—O8ii1.977 (9)O4—Na1i3.006 (11)
Fe1—O6i2.017 (9)O5—Fe1viii2.037 (9)
Fe1—O5iii2.037 (9)O6—Fe1i2.017 (9)
Fe1—O11i2.063 (10)O7—Fe2ix2.066 (9)
Fe1—O1iv2.132 (9)O8—Fe1ii1.977 (9)
Fe1—O42.145 (8)O9—Na1viii2.302 (10)
Fe2—O12v1.986 (9)O10—Na1ii2.382 (12)
Fe2—O42.031 (9)O11—Fe1i2.063 (10)
Fe2—O2vi2.032 (9)O11—Na1i2.883 (12)
Fe2—O7vii2.066 (9)O12—Fe2x1.986 (9)
O10—Mo1—O5110.1 (4)O8—Na1—O3i82.2 (3)
O10—Mo1—O11109.4 (4)O9iii—Na1—O11i81.6 (4)
O5—Mo1—O11110.2 (5)O10ii—Na1—O11i103.8 (4)
O10—Mo1—O4108.8 (4)O10—Na1—O11i70.2 (3)
O5—Mo1—O4109.2 (4)O6—Na1—O11i99.8 (3)
O11—Mo1—O4109.1 (4)O8—Na1—O11i150.9 (3)
O10—Mo1—Na1i140.7 (3)O3i—Na1—O11i114.4 (3)
O5—Mo1—Na1i109.1 (3)O9iii—Na1—O4i89.7 (4)
O11—Mo1—Na1i54.1 (3)O10ii—Na1—O4i161.9 (4)
O4—Mo1—Na1i58.2 (3)O10—Na1—O4i98.6 (3)
O10—Mo1—Na132.5 (3)O6—Na1—O4i61.0 (3)
O5—Mo1—Na1134.2 (3)O8—Na1—O4i120.8 (3)
O11—Mo1—Na179.2 (3)O3i—Na1—O4i58.6 (3)
O4—Mo1—Na1109.3 (3)O11i—Na1—O4i59.5 (3)
Na1i—Mo1—Na1111.83 (12)O9iii—Na1—Mo3139.4 (4)
O10—Mo1—Na1ii30.3 (3)O10ii—Na1—Mo3108.8 (3)
O5—Mo1—Na1ii98.4 (4)O10—Na1—Mo379.5 (3)
O11—Mo1—Na1ii138.7 (3)O6—Na1—Mo331.8 (2)
O4—Mo1—Na1ii87.8 (3)O8—Na1—Mo332.7 (2)
Na1i—Mo1—Na1ii141.41 (19)O3i—Na1—Mo366.2 (2)
Na1—Mo1—Na1ii59.50 (17)O11i—Na1—Mo3130.4 (3)
O7—Mo2—O2111.2 (4)O4i—Na1—Mo388.6 (2)
O7—Mo2—O3106.4 (4)O9iii—Na1—Mo1i78.3 (3)
O2—Mo2—O3108.4 (4)O10ii—Na1—Mo1i131.0 (3)
O7—Mo2—O1109.1 (4)O10—Na1—Mo1i89.1 (3)
O2—Mo2—O1106.8 (4)O6—Na1—Mo1i85.0 (3)
O3—Mo2—O1114.9 (4)O8—Na1—Mo1i148.5 (3)
O9—Mo3—O12108.5 (5)O3i—Na1—Mo1i85.0 (2)
O9—Mo3—O6109.6 (5)O11i—Na1—Mo1i29.7 (2)
O12—Mo3—O6110.2 (5)O4i—Na1—Mo1i31.11 (19)
O9—Mo3—O8113.7 (5)Mo3—Na1—Mo1i116.06 (18)
O12—Mo3—O8108.0 (5)O9iii—Na1—Na1ii113.6 (4)
O6—Mo3—O8106.7 (4)O10ii—Na1—Na1ii40.5 (2)
O9—Mo3—Na1140.5 (4)O10—Na1—Na1ii39.8 (3)
O12—Mo3—Na1110.7 (4)O6—Na1—Na1ii103.6 (3)
O6—Mo3—Na151.5 (3)O8—Na1—Na1ii75.9 (3)
O8—Mo3—Na157.3 (3)O3i—Na1—Na1ii158.1 (4)
O8ii—Fe1—O6i175.7 (4)O11i—Na1—Na1ii86.1 (3)
O8ii—Fe1—O5iii89.8 (4)O4i—Na1—Na1ii135.7 (3)
O6i—Fe1—O5iii89.3 (4)Mo3—Na1—Na1ii95.1 (2)
O8ii—Fe1—O11i96.1 (4)Mo1i—Na1—Na1ii114.6 (3)
O6i—Fe1—O11i88.1 (4)O9iii—Na1—Mo1136.0 (4)
O5iii—Fe1—O11i92.8 (4)O10ii—Na1—Mo1100.4 (3)
O8ii—Fe1—O1iv91.7 (4)O10—Na1—Mo122.5 (2)
O6i—Fe1—O1iv84.3 (4)O6—Na1—Mo162.7 (2)
O5iii—Fe1—O1iv99.5 (4)O8—Na1—Mo195.8 (2)
O11i—Fe1—O1iv165.4 (3)O3i—Na1—Mo1124.0 (3)
O8ii—Fe1—O493.5 (4)O11i—Na1—Mo155.2 (2)
O6i—Fe1—O487.3 (3)O4i—Na1—Mo176.3 (2)
O5iii—Fe1—O4176.3 (4)Mo3—Na1—Mo182.55 (12)
O11i—Fe1—O488.4 (4)Mo1i—Na1—Mo168.17 (12)
O1iv—Fe1—O478.8 (3)Na1ii—Na1—Mo160.58 (16)
O12v—Fe2—O4170.8 (4)Mo2—O1—Fe2iv128.2 (5)
O12v—Fe2—O2vi93.4 (4)Mo2—O1—Fe1iv132.6 (4)
O4—Fe2—O2vi95.5 (4)Fe2iv—O1—Fe1iv98.6 (4)
O12v—Fe2—O7vii92.6 (4)Mo2—O2—Fe2vi149.0 (6)
O4—Fe2—O7vii90.5 (4)Mo2—O3—Fe2128.6 (5)
O2vi—Fe2—O7vii86.2 (4)Mo2—O3—Na1i118.3 (4)
O12v—Fe2—O388.7 (4)Fe2—O3—Na1i108.5 (4)
O4—Fe2—O388.4 (4)Mo1—O4—Fe2135.9 (4)
O2vi—Fe2—O392.7 (4)Mo1—O4—Fe1119.5 (4)
O7vii—Fe2—O3178.3 (4)Fe2—O4—Fe1100.9 (4)
O12v—Fe2—O1iv89.5 (4)Mo1—O4—Na1i90.7 (4)
O4—Fe2—O1iv81.7 (3)Fe2—O4—Na1i103.7 (3)
O2vi—Fe2—O1iv176.8 (3)Fe1—O4—Na1i94.5 (3)
O7vii—Fe2—O1iv92.3 (4)Mo1—O5—Fe1viii162.3 (7)
O3—Fe2—O1iv88.8 (4)Mo3—O6—Fe1i149.6 (6)
O9iii—Na1—O10ii80.4 (4)Mo3—O6—Na196.7 (4)
O9iii—Na1—O10140.7 (5)Fe1i—O6—Na1110.6 (4)
O10ii—Na1—O1080.3 (4)Mo2—O7—Fe2ix150.7 (5)
O9iii—Na1—O6142.7 (4)Mo3—O8—Fe1ii139.7 (5)
O10ii—Na1—O6133.7 (4)Mo3—O8—Na190.0 (4)
O10—Na1—O671.0 (3)Fe1ii—O8—Na1130.2 (5)
O9iii—Na1—O8126.5 (4)Mo3—O9—Na1viii174.1 (7)
O10ii—Na1—O877.0 (3)Mo1—O10—Na1ii128.4 (5)
O10—Na1—O881.5 (3)Mo1—O10—Na1125.0 (5)
O6—Na1—O863.5 (3)Na1ii—O10—Na199.7 (4)
O9iii—Na1—O3i78.6 (4)Mo1—O11—Fe1i137.5 (5)
O10ii—Na1—O3i132.6 (4)Mo1—O11—Na1i96.1 (4)
O10—Na1—O3i137.8 (4)Fe1i—O11—Na1i125.9 (4)
O6—Na1—O3i66.9 (3)Mo3—O12—Fe2x169.6 (7)
O9—Mo3—Na1—O9iii171.1 (10)Na1—Mo1—O4—Na1i104.3 (2)
O12—Mo3—Na1—O9iii16.1 (7)Na1ii—Mo1—O4—Na1i160.8 (2)
O6—Mo3—Na1—O9iii116.0 (7)O12v—Fe2—O4—Mo1176 (2)
O8—Mo3—Na1—O9iii82.6 (7)O2vi—Fe2—O4—Mo120.5 (7)
O9—Mo3—Na1—O10ii73.8 (7)O7vii—Fe2—O4—Mo165.7 (7)
O12—Mo3—Na1—O10ii113.3 (5)O3—Fe2—O4—Mo1113.1 (7)
O6—Mo3—Na1—O10ii146.7 (5)O1iv—Fe2—O4—Mo1157.9 (7)
O8—Mo3—Na1—O10ii14.7 (4)O12v—Fe2—O4—Fe119 (3)
O9—Mo3—Na1—O102.1 (7)O2vi—Fe2—O4—Fe1177.5 (4)
O12—Mo3—Na1—O10170.8 (5)O7vii—Fe2—O4—Fe191.3 (4)
O6—Mo3—Na1—O1070.9 (4)O3—Fe2—O4—Fe190.0 (4)
O8—Mo3—Na1—O1090.5 (4)O1iv—Fe2—O4—Fe11.0 (4)
O9—Mo3—Na1—O673.0 (7)O12v—Fe2—O4—Na1i79 (3)
O12—Mo3—Na1—O699.9 (5)O2vi—Fe2—O4—Na1i85.1 (4)
O8—Mo3—Na1—O6161.4 (5)O7vii—Fe2—O4—Na1i171.3 (4)
O9—Mo3—Na1—O888.4 (7)O3—Fe2—O4—Na1i7.5 (4)
O12—Mo3—Na1—O898.7 (5)O1iv—Fe2—O4—Na1i96.5 (4)
O6—Mo3—Na1—O8161.4 (5)O8ii—Fe1—O4—Mo171.7 (6)
O9—Mo3—Na1—O3i157.1 (6)O6i—Fe1—O4—Mo1112.5 (5)
O12—Mo3—Na1—O3i15.8 (4)O5iii—Fe1—O4—Mo1134 (6)
O6—Mo3—Na1—O3i84.1 (4)O11i—Fe1—O4—Mo124.4 (5)
O8—Mo3—Na1—O3i114.5 (4)O1iv—Fe1—O4—Mo1162.7 (6)
O9—Mo3—Na1—O11i54.5 (7)O8ii—Fe1—O4—Fe290.1 (4)
O12—Mo3—Na1—O11i118.4 (5)O6i—Fe1—O4—Fe285.7 (4)
O6—Mo3—Na1—O11i18.5 (5)O5iii—Fe1—O4—Fe264 (6)
O8—Mo3—Na1—O11i142.9 (5)O11i—Fe1—O4—Fe2173.9 (4)
O9—Mo3—Na1—O4i101.1 (6)O1iv—Fe1—O4—Fe21.0 (4)
O12—Mo3—Na1—O4i71.8 (4)O8ii—Fe1—O4—Na1i165.0 (4)
O6—Mo3—Na1—O4i28.1 (4)O6i—Fe1—O4—Na1i19.2 (3)
O8—Mo3—Na1—O4i170.5 (4)O5iii—Fe1—O4—Na1i41 (6)
O9—Mo3—Na1—Mo1i85.9 (6)O11i—Fe1—O4—Na1i69.0 (3)
O12—Mo3—Na1—Mo1i87.0 (4)O1iv—Fe1—O4—Na1i103.9 (3)
O6—Mo3—Na1—Mo1i13.0 (4)O10—Mo1—O5—Fe1viii101.4 (19)
O8—Mo3—Na1—Mo1i174.3 (4)O11—Mo1—O5—Fe1viii19 (2)
O9—Mo3—Na1—Na1ii34.7 (7)O4—Mo1—O5—Fe1viii139.1 (19)
O12—Mo3—Na1—Na1ii152.4 (4)Na1i—Mo1—O5—Fe1viii77.1 (19)
O6—Mo3—Na1—Na1ii107.7 (4)Na1—Mo1—O5—Fe1viii75 (2)
O8—Mo3—Na1—Na1ii53.7 (4)Na1ii—Mo1—O5—Fe1viii130.3 (19)
O9—Mo3—Na1—Mo124.7 (6)O9—Mo3—O6—Fe1i65.8 (11)
O12—Mo3—Na1—Mo1148.2 (4)O12—Mo3—O6—Fe1i53.5 (10)
O6—Mo3—Na1—Mo148.3 (4)O8—Mo3—O6—Fe1i170.6 (9)
O8—Mo3—Na1—Mo1113.1 (4)Na1—Mo3—O6—Fe1i154.3 (11)
O10—Mo1—Na1—O9iii114.2 (8)O9—Mo3—O6—Na1139.8 (5)
O5—Mo1—Na1—O9iii164.9 (7)O12—Mo3—O6—Na1100.8 (4)
O11—Mo1—Na1—O9iii87.4 (6)O8—Mo3—O6—Na116.3 (4)
O4—Mo1—Na1—O9iii19.3 (6)O9iii—Na1—O6—Mo3105.1 (7)
Na1i—Mo1—Na1—O9iii43.3 (5)O10ii—Na1—O6—Mo345.9 (6)
Na1ii—Mo1—Na1—O9iii94.5 (6)O10—Na1—O6—Mo3100.8 (4)
O10—Mo1—Na1—O10ii27.3 (8)O8—Na1—O6—Mo311.1 (3)
O5—Mo1—Na1—O10ii78.0 (6)O3i—Na1—O6—Mo381.7 (4)
O11—Mo1—Na1—O10ii174.3 (4)O11i—Na1—O6—Mo3165.8 (4)
O4—Mo1—Na1—O10ii67.7 (4)O4i—Na1—O6—Mo3147.4 (4)
Na1i—Mo1—Na1—O10ii130.2 (3)Mo1i—Na1—O6—Mo3168.3 (3)
Na1ii—Mo1—Na1—O10ii7.6 (2)Na1ii—Na1—O6—Mo377.5 (4)
O5—Mo1—Na1—O1050.7 (8)Mo1—Na1—O6—Mo3123.7 (4)
O11—Mo1—Na1—O10158.4 (7)O9iii—Na1—O6—Fe1i61.3 (8)
O4—Mo1—Na1—O1095.0 (7)O10ii—Na1—O6—Fe1i147.6 (5)
Na1i—Mo1—Na1—O10157.5 (6)O10—Na1—O6—Fe1i92.7 (4)
Na1ii—Mo1—Na1—O1019.7 (6)O8—Na1—O6—Fe1i177.6 (5)
O10—Mo1—Na1—O6106.8 (7)O3i—Na1—O6—Fe1i84.8 (4)
O5—Mo1—Na1—O656.0 (6)O11i—Na1—O6—Fe1i27.7 (4)
O11—Mo1—Na1—O651.7 (4)O4i—Na1—O6—Fe1i19.1 (3)
O4—Mo1—Na1—O6158.3 (4)Mo3—Na1—O6—Fe1i166.5 (6)
Na1i—Mo1—Na1—O695.7 (3)Mo1i—Na1—O6—Fe1i1.9 (3)
Na1ii—Mo1—Na1—O6126.4 (3)Na1ii—Na1—O6—Fe1i116.0 (4)
O10—Mo1—Na1—O850.5 (7)Mo1—Na1—O6—Fe1i69.9 (3)
O5—Mo1—Na1—O80.2 (6)O2—Mo2—O7—Fe2ix96.5 (11)
O11—Mo1—Na1—O8107.9 (4)O3—Mo2—O7—Fe2ix145.6 (10)
O4—Mo1—Na1—O8145.5 (4)O1—Mo2—O7—Fe2ix21.1 (11)
Na1i—Mo1—Na1—O8151.9 (3)O9—Mo3—O8—Fe1ii47.8 (9)
Na1ii—Mo1—Na1—O870.2 (3)O12—Mo3—O8—Fe1ii72.7 (9)
O10—Mo1—Na1—O3i135.1 (7)O6—Mo3—O8—Fe1ii168.8 (7)
O5—Mo1—Na1—O3i84.4 (6)Na1—Mo3—O8—Fe1ii176.1 (9)
O11—Mo1—Na1—O3i23.3 (5)O9—Mo3—O8—Na1136.1 (5)
O4—Mo1—Na1—O3i130.0 (4)O12—Mo3—O8—Na1103.4 (4)
Na1i—Mo1—Na1—O3i67.4 (3)O6—Mo3—O8—Na115.1 (4)
Na1ii—Mo1—Na1—O3i154.8 (4)O9iii—Na1—O8—Mo3126.7 (5)
O10—Mo1—Na1—O11i126.9 (7)O10ii—Na1—O8—Mo3165.8 (4)
O5—Mo1—Na1—O11i177.7 (6)O10—Na1—O8—Mo383.8 (4)
O11—Mo1—Na1—O11i74.6 (5)O6—Na1—O8—Mo310.8 (3)
O4—Mo1—Na1—O11i32.0 (4)O3i—Na1—O8—Mo357.1 (3)
Na1i—Mo1—Na1—O11i30.6 (2)O11i—Na1—O8—Mo370.7 (9)
Na1ii—Mo1—Na1—O11i107.3 (3)O4i—Na1—O8—Mo311.1 (5)
O10—Mo1—Na1—O4i170.9 (7)Mo1i—Na1—O8—Mo39.7 (7)
O5—Mo1—Na1—O4i120.2 (5)Na1ii—Na1—O8—Mo3124.1 (4)
O11—Mo1—Na1—O4i12.5 (4)Mo1—Na1—O8—Mo366.4 (3)
O4—Mo1—Na1—O4i94.2 (4)O9iii—Na1—O8—Fe1ii50.0 (8)
Na1i—Mo1—Na1—O4i31.60 (19)O10ii—Na1—O8—Fe1ii17.5 (5)
Na1ii—Mo1—Na1—O4i169.4 (3)O10—Na1—O8—Fe1ii99.5 (6)
O10—Mo1—Na1—Mo380.5 (6)O6—Na1—O8—Fe1ii172.5 (6)
O5—Mo1—Na1—Mo329.8 (5)O3i—Na1—O8—Fe1ii119.6 (6)
O11—Mo1—Na1—Mo377.9 (3)O11i—Na1—O8—Fe1ii112.6 (8)
O4—Mo1—Na1—Mo3175.5 (3)O4i—Na1—O8—Fe1ii165.6 (5)
Na1i—Mo1—Na1—Mo3121.99 (16)Mo3—Na1—O8—Fe1ii176.7 (8)
Na1ii—Mo1—Na1—Mo3100.2 (2)Mo1i—Na1—O8—Fe1ii173.6 (4)
O10—Mo1—Na1—Mo1i157.5 (6)Na1ii—Na1—O8—Fe1ii59.2 (5)
O5—Mo1—Na1—Mo1i151.8 (5)Mo1—Na1—O8—Fe1ii116.9 (5)
O11—Mo1—Na1—Mo1i44.1 (3)O12—Mo3—O9—Na1viii90 (7)
O4—Mo1—Na1—Mo1i62.6 (3)O6—Mo3—O9—Na1viii30 (7)
Na1i—Mo1—Na1—Mo1i0.0O8—Mo3—O9—Na1viii149 (7)
Na1ii—Mo1—Na1—Mo1i137.8 (2)Na1—Mo3—O9—Na1viii83 (7)
O10—Mo1—Na1—Na1ii19.7 (6)O5—Mo1—O10—Na1ii71.4 (7)
O5—Mo1—Na1—Na1ii70.4 (5)O11—Mo1—O10—Na1ii167.4 (6)
O11—Mo1—Na1—Na1ii178.1 (4)O4—Mo1—O10—Na1ii48.2 (7)
O4—Mo1—Na1—Na1ii75.3 (4)Na1i—Mo1—O10—Na1ii110.7 (6)
Na1i—Mo1—Na1—Na1ii137.8 (2)Na1—Mo1—O10—Na1ii144.9 (10)
O7—Mo2—O1—Fe2iv83.5 (7)O5—Mo1—O10—Na1143.7 (6)
O2—Mo2—O1—Fe2iv156.3 (6)O11—Mo1—O10—Na122.5 (7)
O3—Mo2—O1—Fe2iv35.9 (7)O4—Mo1—O10—Na196.6 (6)
O7—Mo2—O1—Fe1iv107.4 (7)Na1i—Mo1—O10—Na134.1 (9)
O2—Mo2—O1—Fe1iv12.9 (8)Na1ii—Mo1—O10—Na1144.9 (10)
O3—Mo2—O1—Fe1iv133.2 (6)O9iii—Na1—O10—Mo191.1 (9)
O7—Mo2—O2—Fe2vi27.4 (11)O10ii—Na1—O10—Mo1152.8 (8)
O3—Mo2—O2—Fe2vi89.3 (10)O6—Na1—O10—Mo164.2 (6)
O1—Mo2—O2—Fe2vi146.3 (10)O8—Na1—O10—Mo1129.0 (6)
O7—Mo2—O3—Fe2161.0 (6)O3i—Na1—O10—Mo160.7 (9)
O2—Mo2—O3—Fe241.3 (8)O11i—Na1—O10—Mo144.2 (6)
O1—Mo2—O3—Fe278.1 (7)O4i—Na1—O10—Mo18.9 (7)
O7—Mo2—O3—Na1i8.0 (6)Mo3—Na1—O10—Mo195.9 (6)
O2—Mo2—O3—Na1i111.7 (5)Mo1i—Na1—O10—Mo120.8 (6)
O1—Mo2—O3—Na1i128.9 (5)Na1ii—Na1—O10—Mo1152.8 (8)
O12v—Fe2—O3—Mo225.5 (7)O9iii—Na1—O10—Na1ii61.7 (7)
O4—Fe2—O3—Mo2163.2 (7)O10ii—Na1—O10—Na1ii0.0
O2vi—Fe2—O3—Mo267.8 (7)O6—Na1—O10—Na1ii143.1 (4)
O7vii—Fe2—O3—Mo2116 (12)O8—Na1—O10—Na1ii78.2 (4)
O1iv—Fe2—O3—Mo2115.0 (7)O3i—Na1—O10—Na1ii146.5 (6)
O12v—Fe2—O3—Na1i179.4 (4)O11i—Na1—O10—Na1ii108.5 (4)
O4—Fe2—O3—Na1i8.2 (4)O4i—Na1—O10—Na1ii161.7 (4)
O2vi—Fe2—O3—Na1i87.2 (4)Mo3—Na1—O10—Na1ii111.3 (3)
O7vii—Fe2—O3—Na1i39 (12)Mo1i—Na1—O10—Na1ii132.0 (3)
O1iv—Fe2—O3—Na1i89.9 (4)Mo1—Na1—O10—Na1ii152.8 (8)
O10—Mo1—O4—Fe2110.7 (7)O10—Mo1—O11—Fe1i33.2 (9)
O5—Mo1—O4—Fe29.5 (8)O5—Mo1—O11—Fe1i88.0 (7)
O11—Mo1—O4—Fe2130.0 (7)O4—Mo1—O11—Fe1i152.2 (7)
Na1i—Mo1—O4—Fe2110.6 (7)Na1i—Mo1—O11—Fe1i172.5 (9)
Na1—Mo1—O4—Fe2145.1 (6)Na1—Mo1—O11—Fe1i45.3 (6)
Na1ii—Mo1—O4—Fe288.6 (7)Na1ii—Mo1—O11—Fe1i42.9 (10)
O10—Mo1—O4—Fe143.1 (6)O10—Mo1—O11—Na1i139.3 (4)
O5—Mo1—O4—Fe1163.3 (5)O5—Mo1—O11—Na1i99.5 (4)
O11—Mo1—O4—Fe176.3 (5)O4—Mo1—O11—Na1i20.3 (4)
Na1i—Mo1—O4—Fe195.6 (5)Na1—Mo1—O11—Na1i127.2 (3)
Na1—Mo1—O4—Fe18.7 (6)Na1ii—Mo1—O11—Na1i129.7 (4)
Na1ii—Mo1—O4—Fe165.2 (5)O9—Mo3—O12—Fe2x32 (4)
O10—Mo1—O4—Na1i138.7 (4)O6—Mo3—O12—Fe2x152 (4)
O5—Mo1—O4—Na1i101.1 (4)O8—Mo3—O12—Fe2x92 (4)
O11—Mo1—O4—Na1i19.3 (4)Na1—Mo3—O12—Fe2x153 (3)
Symmetry codes: (i) x+1, y+1, z; (ii) x, y+1, z; (iii) x, y+1, z; (iv) x+1, y+1, z+1; (v) x, y, z+1; (vi) x+1, y, z+1; (vii) x1, y, z; (viii) x, y1, z; (ix) x+1, y, z; (x) x, y, z1.
(4) top
Crystal data top
Fe2Mo3Na3O12Z = 4
Mr = 660.49F(000) = 1228
?, C2/cDx = 3.809 Mg m3
a = 12.646 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.685 (3) ÅCell parameters from 507 reflections
c = 7.206 (2) Åθ = 2.3–30.1°
α = 90°µ = 5.81 mm1
β = 112.56 (3)°T = 293 K
γ = 90°Prism, black
V = 1151.6 (5) Å30.08 × 0.04 × 0.04 mm
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector1055 independent reflections
Radiation source: fine-focus sealed tube791 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.043
Rotation method data acquisition using ω and phi scans(s)θmax = 26.4°, θmin = 2.3°
Absorption correction: numeric analytical
?
h = 1313
Tmin = 0.766, Tmax = 0.886k = 1716
2221 measured reflectionsl = 88
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)] = 0.062 w = 1/[σ2(Fo2) + (0.1072P)2 + 11.9291P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.196(Δ/σ)max = 0.001
S = 1.14Δρmax = 1.34 e Å3
1055 reflectionsΔρmin = 2.63 e Å3
95 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0003 (5)
Crystal data top
Fe2Mo3Na3O12γ = 90°
Mr = 660.49V = 1151.6 (5) Å3
?, C2/cZ = 4
a = 12.646 (3) ÅMo Kα radiation
b = 13.685 (3) ŵ = 5.81 mm1
c = 7.206 (2) ÅT = 293 K
α = 90°0.08 × 0.04 × 0.04 mm
β = 112.56 (3)°
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector1055 independent reflections
Absorption correction: numeric analytical
?
791 reflections with I > 2σ(I)
Tmin = 0.766, Tmax = 0.886Rint = 0.043
2221 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0620 restraints
wR(F2) = 0.196 w = 1/[σ2(Fo2) + (0.1072P)2 + 11.9291P]
where P = (Fo2 + 2Fc2)/3
S = 1.14Δρmax = 1.34 e Å3
1055 reflectionsΔρmin = 2.63 e Å3
95 parameters
Special details top

Experimental. CrysAlis RED, Oxford Diffraction Ltd., version 170.17, 2003 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R·C. Clark & J·S. Reid.

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*/Ueq
Mo10.77270 (11)0.39090 (10)0.37603 (18)0.0174 (5)
Mo21.00000.21172 (13)0.25000.0209 (6)
Fe31.2099 (3)0.3406 (2)0.6236 (4)0.0446 (9)
Na11.00000.4971 (13)0.25000.068 (4)
Na21.00000.2297 (6)0.75000.0206 (19)
Na31.00000.00000.00000.047 (3)
O11.0405 (10)0.2821 (8)0.4705 (15)0.026 (3)
O20.6280 (10)0.4147 (8)0.3183 (17)0.026 (3)
O30.8315 (11)0.3309 (9)0.6060 (17)0.030 (3)
O40.8471 (12)0.5040 (10)0.3971 (18)0.040 (3)
O51.1078 (12)0.1311 (9)0.255 (2)0.044 (4)
O60.7875 (11)0.3193 (11)0.1836 (18)0.039 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0167 (9)0.0227 (8)0.0113 (8)0.0038 (6)0.0036 (5)0.0010 (5)
Mo20.0320 (13)0.0152 (10)0.0110 (10)0.0000.0032 (8)0.000
Fe30.050 (2)0.0470 (19)0.0382 (19)0.0026 (14)0.0186 (15)0.0016 (13)
Na10.028 (7)0.138 (14)0.033 (7)0.0000.007 (5)0.000
Na20.015 (5)0.027 (5)0.021 (5)0.0000.008 (3)0.000
Na30.071 (8)0.024 (5)0.027 (6)0.012 (5)0.002 (5)0.004 (4)
O10.025 (7)0.042 (7)0.013 (6)0.009 (5)0.009 (5)0.012 (5)
O20.030 (7)0.014 (5)0.034 (7)0.004 (5)0.013 (5)0.001 (5)
O30.034 (8)0.037 (7)0.019 (6)0.006 (6)0.008 (5)0.003 (5)
O40.040 (8)0.051 (8)0.026 (7)0.015 (7)0.010 (6)0.010 (6)
O50.049 (9)0.021 (7)0.046 (9)0.005 (6)0.001 (7)0.005 (6)
O60.024 (8)0.068 (10)0.021 (7)0.002 (7)0.006 (5)0.003 (6)
Geometric parameters (Å, º) top
Mo1—O31.740 (12)Na1—Na2i3.739 (19)
Mo1—O21.744 (12)Na2—O1vi2.372 (11)
Mo1—O61.765 (13)Na2—O12.372 (11)
Mo1—O41.788 (12)Na2—O3vi2.417 (13)
Mo1—Na1i3.454 (8)Na2—O32.417 (13)
Mo1—Na2ii3.611 (4)Na2—O2ii2.481 (14)
Mo1—Na13.634 (7)Na2—O2vii2.481 (13)
Mo2—O5iii1.744 (14)Na2—Fe3vi3.470 (5)
Mo2—O51.744 (14)Na2—Mo1ii3.611 (4)
Mo2—O11.758 (10)Na2—Mo1vii3.611 (4)
Mo2—O1iii1.758 (10)Na2—Mo2x3.6114 (12)
Mo2—Na33.4118 (17)Na3—O2xi2.529 (11)
Mo2—Na3iii3.4118 (17)Na3—O2xii2.529 (11)
Mo2—Na23.6114 (12)Na3—O52.555 (13)
Mo2—Na2iv3.6114 (12)Na3—O5xiii2.555 (13)
Fe3—O12.153 (12)Na3—O2xiv2.707 (11)
Fe3—O5v2.163 (15)Na3—O2xv2.707 (11)
Fe3—O3vi2.207 (12)Na3—Mo2xiii3.4118 (17)
Fe3—O4i2.231 (14)Na3—Na3xvi3.6030 (10)
Fe3—O6iii2.245 (13)Na3—Na3iii3.6030 (10)
Fe3—O6vii2.370 (15)Na3—Na2iv3.623 (8)
Fe3—Na23.470 (5)Na3—Na2xvii3.623 (8)
Na1—O4viii2.536 (13)O2—Na2ii2.481 (13)
Na1—O4i2.536 (13)O2—Na3xviii2.529 (11)
Na1—O42.539 (13)O2—Na3xix2.707 (11)
Na1—O4iii2.539 (13)O3—Fe3vi2.207 (12)
Na1—Mo1i3.454 (8)O4—Fe3i2.231 (14)
Na1—Mo1viii3.454 (8)O4—Na1i2.536 (13)
Na1—Na1i3.6038 (13)O5—Fe3v2.163 (15)
Na1—Na1ix3.6038 (13)O6—Fe3iii2.245 (13)
Na1—Mo1iii3.634 (7)O6—Fe3xx2.370 (15)
O3—Mo1—O2109.9 (6)O1—Na2—Fe337.7 (3)
O3—Mo1—O6110.5 (6)O3vi—Na2—Fe339.1 (3)
O2—Mo1—O6109.5 (5)O3—Na2—Fe3105.9 (4)
O3—Mo1—O4108.0 (6)O2ii—Na2—Fe3143.4 (3)
O2—Mo1—O4109.2 (6)O2vii—Na2—Fe383.9 (3)
O6—Mo1—O4109.6 (6)O1vi—Na2—Fe3vi37.7 (3)
O3—Mo1—Na1i62.8 (5)O1—Na2—Fe3vi121.8 (4)
O2—Mo1—Na1i125.9 (4)O3vi—Na2—Fe3vi105.9 (4)
O6—Mo1—Na1i123.5 (4)O3—Na2—Fe3vi39.1 (3)
O4—Mo1—Na1i45.3 (5)O2ii—Na2—Fe3vi83.9 (3)
O3—Mo1—Na2ii92.4 (4)O2vii—Na2—Fe3vi143.4 (3)
O2—Mo1—Na2ii38.0 (4)Fe3—Na2—Fe3vi128.1 (3)
O6—Mo1—Na2ii85.9 (4)O1vi—Na2—Mo1ii81.7 (3)
O4—Mo1—Na2ii146.9 (5)O1—Na2—Mo1ii114.9 (3)
Na1i—Mo1—Na2ii145.86 (7)O3vi—Na2—Mo1ii165.9 (3)
O3—Mo1—Na1109.7 (4)O3—Na2—Mo1ii63.5 (3)
O2—Mo1—Na1136.4 (4)O2ii—Na2—Mo1ii25.7 (3)
O6—Mo1—Na172.1 (5)O2vii—Na2—Mo1ii100.0 (4)
O4—Mo1—Na140.0 (5)Fe3—Na2—Mo1ii152.51 (6)
Na1i—Mo1—Na161.06 (3)Fe3vi—Na2—Mo1ii60.85 (6)
Na2ii—Mo1—Na1152.97 (7)O1vi—Na2—Mo1vii114.9 (3)
O5iii—Mo2—O5101.6 (9)O1—Na2—Mo1vii81.7 (3)
O5iii—Mo2—O1108.6 (6)O3vi—Na2—Mo1vii63.5 (3)
O5—Mo2—O1112.0 (6)O3—Na2—Mo1vii165.9 (3)
O5iii—Mo2—O1iii112.0 (6)O2ii—Na2—Mo1vii100.0 (4)
O5—Mo2—O1iii108.6 (6)O2vii—Na2—Mo1vii25.7 (3)
O1—Mo2—O1iii113.6 (8)Fe3—Na2—Mo1vii60.85 (6)
O5iii—Mo2—Na367.1 (5)Fe3vi—Na2—Mo1vii152.51 (6)
O5—Mo2—Na346.8 (4)Mo1ii—Na2—Mo1vii125.6 (3)
O1—Mo2—Na3152.1 (4)O1vi—Na2—Mo2161.9 (4)
O1iii—Mo2—Na392.7 (4)O1—Na2—Mo224.6 (3)
O5iii—Mo2—Na3iii46.8 (4)O3vi—Na2—Mo297.5 (3)
O5—Mo2—Na3iii67.1 (5)O3—Na2—Mo287.0 (3)
O1—Mo2—Na3iii92.7 (4)O2ii—Na2—Mo289.9 (3)
O1iii—Mo2—Na3iii152.1 (4)O2vii—Na2—Mo283.9 (3)
Na3—Mo2—Na3iii63.74 (4)Fe3—Na2—Mo258.33 (6)
O5iii—Mo2—Na276.3 (5)Fe3vi—Na2—Mo2125.77 (12)
O5—Mo2—Na2108.8 (5)Mo1ii—Na2—Mo294.79 (9)
O1—Mo2—Na234.1 (4)Mo1vii—Na2—Mo281.62 (7)
O1iii—Mo2—Na2138.9 (4)O1vi—Na2—Mo2x24.6 (3)
Na3—Mo2—Na2125.77 (15)O1—Na2—Mo2x161.9 (4)
Na3iii—Mo2—Na262.03 (14)O3vi—Na2—Mo2x87.0 (3)
O5iii—Mo2—Na2iv108.8 (5)O3—Na2—Mo2x97.5 (3)
O5—Mo2—Na2iv76.3 (5)O2ii—Na2—Mo2x83.9 (3)
O1—Mo2—Na2iv138.9 (4)O2vii—Na2—Mo2x89.9 (3)
O1iii—Mo2—Na2iv34.1 (4)Fe3—Na2—Mo2x125.77 (12)
Na3—Mo2—Na2iv62.03 (14)Fe3vi—Na2—Mo2x58.33 (6)
Na3iii—Mo2—Na2iv125.77 (15)Mo1ii—Na2—Mo2x81.62 (7)
Na2—Mo2—Na2iv172.2 (3)Mo1vii—Na2—Mo2x94.79 (9)
O1—Fe3—O5v166.0 (5)Mo2—Na2—Mo2x172.2 (3)
O1—Fe3—O3vi84.5 (4)O2xi—Na3—O2xii180.0 (4)
O5v—Fe3—O3vi103.3 (5)O2xi—Na3—O572.1 (4)
O1—Fe3—O4i95.0 (5)O2xii—Na3—O5107.9 (4)
O5v—Fe3—O4i97.1 (5)O2xi—Na3—O5xiii107.9 (4)
O3vi—Fe3—O4i86.4 (5)O2xii—Na3—O5xiii72.1 (4)
O1—Fe3—O6iii80.5 (4)O5—Na3—O5xiii180.0 (7)
O5v—Fe3—O6iii90.4 (5)O2xi—Na3—O2xiv69.9 (5)
O3vi—Fe3—O6iii163.9 (5)O2xii—Na3—O2xiv110.1 (5)
O4i—Fe3—O6iii100.6 (5)O5—Na3—O2xiv102.1 (4)
O1—Fe3—O6vii90.6 (4)O5xiii—Na3—O2xiv77.9 (4)
O5v—Fe3—O6vii77.8 (5)O2xi—Na3—O2xv110.1 (5)
O3vi—Fe3—O6vii90.3 (5)O2xii—Na3—O2xv69.9 (5)
O4i—Fe3—O6vii173.1 (5)O5—Na3—O2xv77.9 (4)
O6iii—Fe3—O6vii84.2 (5)O5xiii—Na3—O2xv102.1 (4)
O1—Fe3—Na242.3 (3)O2xiv—Na3—O2xv180.0 (5)
O5v—Fe3—Na2140.8 (4)O2xi—Na3—Mo292.5 (2)
O3vi—Fe3—Na243.7 (3)O2xii—Na3—Mo287.5 (2)
O4i—Fe3—Na2100.0 (4)O5—Na3—Mo229.8 (3)
O6iii—Fe3—Na2120.3 (4)O5xiii—Na3—Mo2150.2 (3)
O6vii—Fe3—Na281.5 (3)O2xiv—Na3—Mo289.4 (2)
O4viii—Na1—O4i179.3 (10)O2xv—Na3—Mo290.6 (2)
O4viii—Na1—O490.5 (4)O2xi—Na3—Mo2xiii87.5 (2)
O4i—Na1—O489.5 (4)O2xii—Na3—Mo2xiii92.5 (2)
O4viii—Na1—O4iii89.5 (4)O5—Na3—Mo2xiii150.2 (3)
O4i—Na1—O4iii90.5 (4)O5xiii—Na3—Mo2xiii29.8 (3)
O4—Na1—O4iii175.7 (10)O2xiv—Na3—Mo2xiii90.6 (2)
O4viii—Na1—Mo1i150.6 (7)O2xv—Na3—Mo2xiii89.4 (2)
O4i—Na1—Mo1i30.0 (3)Mo2—Na3—Mo2xiii180.0
O4—Na1—Mo1i101.4 (4)O2xi—Na3—Na3xvi131.4 (3)
O4iii—Na1—Mo1i76.7 (3)O2xii—Na3—Na3xvi48.6 (3)
O4viii—Na1—Mo1viii30.0 (3)O5—Na3—Na3xvi120.9 (3)
O4i—Na1—Mo1viii150.6 (7)O5xiii—Na3—Na3xvi59.1 (3)
O4—Na1—Mo1viii76.7 (3)O2xiv—Na3—Na3xvi135.5 (2)
O4iii—Na1—Mo1viii101.4 (4)O2xv—Na3—Na3xvi44.5 (2)
Mo1i—Na1—Mo1viii127.3 (5)Mo2—Na3—Na3xvi121.872 (19)
O4viii—Na1—Na1i135.2 (3)Mo2xiii—Na3—Na3xvi58.128 (19)
O4i—Na1—Na1i44.8 (3)O2xi—Na3—Na3iii48.6 (3)
O4—Na1—Na1i44.7 (3)O2xii—Na3—Na3iii131.4 (3)
O4iii—Na1—Na1i135.1 (3)O5—Na3—Na3iii59.1 (3)
Mo1i—Na1—Na1i61.9 (2)O5xiii—Na3—Na3iii120.9 (3)
Mo1viii—Na1—Na1i116.8 (4)O2xiv—Na3—Na3iii44.5 (2)
O4viii—Na1—Na1ix44.8 (3)O2xv—Na3—Na3iii135.5 (2)
O4i—Na1—Na1ix135.2 (3)Mo2—Na3—Na3iii58.128 (19)
O4—Na1—Na1ix135.1 (3)Mo2xiii—Na3—Na3iii121.872 (19)
O4iii—Na1—Na1ix44.7 (3)Na3xvi—Na3—Na3iii180.0
Mo1i—Na1—Na1ix116.8 (4)O2xi—Na3—Na2iv136.8 (3)
Mo1viii—Na1—Na1ix61.9 (2)O2xii—Na3—Na2iv43.2 (3)
Na1i—Na1—Na1ix177.5 (11)O5—Na3—Na2iv69.3 (3)
O4viii—Na1—Mo182.9 (4)O5xiii—Na3—Na2iv110.7 (3)
O4i—Na1—Mo196.8 (3)O2xiv—Na3—Na2iv136.8 (2)
O4—Na1—Mo126.9 (3)O2xv—Na3—Na2iv43.2 (2)
O4iii—Na1—Mo1157.2 (7)Mo2—Na3—Na2iv61.69 (7)
Mo1i—Na1—Mo1118.94 (3)Mo2xiii—Na3—Na2iv118.31 (7)
Mo1viii—Na1—Mo182.60 (4)Na3xvi—Na3—Na2iv60.18 (7)
Na1i—Na1—Mo157.0 (2)Na3iii—Na3—Na2iv119.82 (7)
Na1ix—Na1—Mo1124.2 (3)O2xi—Na3—Na2xvii43.2 (3)
O4viii—Na1—Mo1iii96.8 (3)O2xii—Na3—Na2xvii136.8 (3)
O4i—Na1—Mo1iii82.9 (4)O5—Na3—Na2xvii110.7 (3)
O4—Na1—Mo1iii157.2 (7)O5xiii—Na3—Na2xvii69.3 (3)
O4iii—Na1—Mo1iii26.9 (3)O2xiv—Na3—Na2xvii43.2 (2)
Mo1i—Na1—Mo1iii82.60 (4)O2xv—Na3—Na2xvii136.8 (2)
Mo1viii—Na1—Mo1iii118.94 (3)Mo2—Na3—Na2xvii118.31 (7)
Na1i—Na1—Mo1iii124.2 (3)Mo2xiii—Na3—Na2xvii61.69 (7)
Na1ix—Na1—Mo1iii57.0 (2)Na3xvi—Na3—Na2xvii119.82 (7)
Mo1—Na1—Mo1iii132.8 (5)Na3iii—Na3—Na2xvii60.18 (7)
O4viii—Na1—Na2i90.4 (5)Na2iv—Na3—Na2xvii180.00 (14)
O4i—Na1—Na2i90.4 (5)Mo2—O1—Fe3123.7 (6)
O4—Na1—Na2i87.9 (5)Mo2—O1—Na2121.3 (6)
O4iii—Na1—Na2i87.9 (5)Fe3—O1—Na2100.0 (4)
Mo1i—Na1—Na2i63.7 (3)Mo1—O2—Na2ii116.3 (5)
Mo1viii—Na1—Na2i63.7 (3)Mo1—O2—Na3xviii123.4 (6)
Na1i—Na1—Na2i88.8 (6)Na2ii—O2—Na3xviii92.6 (4)
Na1ix—Na1—Na2i88.8 (6)Mo1—O2—Na3xix137.1 (6)
Mo1—Na1—Na2i113.6 (3)Na2ii—O2—Na3xix88.5 (4)
Mo1iii—Na1—Na2i113.6 (3)Na3xviii—O2—Na3xix86.9 (3)
O1vi—Na2—O1144.8 (7)Mo1—O3—Fe3vi130.8 (6)
O1vi—Na2—O3vi84.5 (4)Mo1—O3—Na2131.6 (6)
O1—Na2—O3vi75.5 (4)Fe3vi—O3—Na297.1 (4)
O1vi—Na2—O375.5 (4)Mo1—O4—Fe3i132.3 (7)
O1—Na2—O384.5 (4)Mo1—O4—Na1i104.7 (6)
O3vi—Na2—O3110.1 (7)Fe3i—O4—Na1i100.1 (6)
O1vi—Na2—O2ii94.1 (4)Mo1—O4—Na1113.1 (8)
O1—Na2—O2ii114.2 (4)Fe3i—O4—Na1106.6 (6)
O3vi—Na2—O2ii160.5 (5)Na1i—O4—Na190.5 (4)
O3—Na2—O2ii88.3 (4)Mo2—O5—Fe3v126.8 (7)
O1vi—Na2—O2vii114.2 (4)Mo2—O5—Na3103.4 (6)
O1—Na2—O2vii94.1 (4)Fe3v—O5—Na3127.5 (6)
O3vi—Na2—O2vii88.3 (4)Mo1—O6—Fe3iii138.5 (8)
O3—Na2—O2vii160.5 (5)Mo1—O6—Fe3xx119.6 (7)
O2ii—Na2—O2vii74.4 (6)Fe3iii—O6—Fe3xx95.8 (5)
O1vi—Na2—Fe3121.8 (4)
O3—Mo1—Na1—O4viii159.7 (6)O1iii—Mo2—Na3—O2xiv130.8 (5)
O2—Mo1—Na1—O4viii46.1 (8)Na3iii—Mo2—Na3—O2xiv33.5 (2)
O6—Mo1—Na1—O4viii53.7 (6)Na2—Mo2—Na3—O2xiv33.5 (2)
O4—Mo1—Na1—O4viii105.4 (8)Na2iv—Mo2—Na3—O2xiv146.5 (2)
Na1i—Mo1—Na1—O4viii159.1 (8)O5iii—Mo2—Na3—O2xv161.9 (5)
Na2ii—Mo1—Na1—O4viii16.7 (9)O5—Mo2—Na3—O2xv64.0 (7)
O3—Mo1—Na1—O4i19.6 (7)O1—Mo2—Na3—O2xv111.4 (8)
O2—Mo1—Na1—O4i134.6 (7)O1iii—Mo2—Na3—O2xv49.2 (5)
O6—Mo1—Na1—O4i125.6 (7)Na3iii—Mo2—Na3—O2xv146.5 (2)
O4—Mo1—Na1—O4i75.2 (8)Na2—Mo2—Na3—O2xv146.5 (2)
Na1i—Mo1—Na1—O4i21.6 (3)Na2iv—Mo2—Na3—O2xv33.5 (2)
Na2ii—Mo1—Na1—O4i162.6 (4)O5iii—Mo2—Na3—Mo2xiii51.6 (5)
O3—Mo1—Na1—O494.8 (8)O5—Mo2—Na3—Mo2xiii82.4 (7)
O2—Mo1—Na1—O459.3 (8)O1—Mo2—Na3—Mo2xiii35.1 (8)
O6—Mo1—Na1—O4159.1 (8)O1iii—Mo2—Na3—Mo2xiii164.4 (4)
Na1i—Mo1—Na1—O453.7 (7)Na3iii—Mo2—Na3—Mo2xiii0 (100)
Na2ii—Mo1—Na1—O4122.1 (8)Na2—Mo2—Na3—Mo2xiii0 (100)
O3—Mo1—Na1—O4iii88.3 (10)Na2iv—Mo2—Na3—Mo2xiii180.00 (7)
O2—Mo1—Na1—O4iii117.5 (12)O5iii—Mo2—Na3—Na3xvi128.4 (5)
O6—Mo1—Na1—O4iii17.7 (10)O5—Mo2—Na3—Na3xvi97.6 (7)
O4—Mo1—Na1—O4iii176.9 (8)O1—Mo2—Na3—Na3xvi144.9 (8)
Na1i—Mo1—Na1—O4iii129.5 (12)O1iii—Mo2—Na3—Na3xvi15.6 (4)
Na2ii—Mo1—Na1—O4iii54.7 (14)Na3iii—Mo2—Na3—Na3xvi180.0
O3—Mo1—Na1—Mo1i41.2 (7)Na2—Mo2—Na3—Na3xvi180.0
O2—Mo1—Na1—Mo1i113.0 (6)Na2iv—Mo2—Na3—Na3xvi0.0
O6—Mo1—Na1—Mo1i147.2 (6)O5iii—Mo2—Na3—Na3iii51.6 (5)
O4—Mo1—Na1—Mo1i53.7 (7)O5—Mo2—Na3—Na3iii82.4 (7)
Na1i—Mo1—Na1—Mo1i0.0O1—Mo2—Na3—Na3iii35.1 (8)
Na2ii—Mo1—Na1—Mo1i175.8 (3)O1iii—Mo2—Na3—Na3iii164.4 (4)
O3—Mo1—Na1—Mo1viii170.0 (4)Na2—Mo2—Na3—Na3iii0.0
O2—Mo1—Na1—Mo1viii15.8 (7)Na2iv—Mo2—Na3—Na3iii180.0
O6—Mo1—Na1—Mo1viii84.0 (5)O5iii—Mo2—Na3—Na2iv128.4 (5)
O4—Mo1—Na1—Mo1viii75.1 (7)O5—Mo2—Na3—Na2iv97.6 (7)
Na1i—Mo1—Na1—Mo1viii128.8 (6)O1—Mo2—Na3—Na2iv144.9 (8)
Na2ii—Mo1—Na1—Mo1viii47.0 (8)O1iii—Mo2—Na3—Na2iv15.6 (4)
O3—Mo1—Na1—Na1i41.2 (7)Na3iii—Mo2—Na3—Na2iv180.0
O2—Mo1—Na1—Na1i113.0 (6)Na2—Mo2—Na3—Na2iv180.0
O6—Mo1—Na1—Na1i147.2 (6)O5iii—Mo2—Na3—Na2xvii51.6 (5)
O4—Mo1—Na1—Na1i53.7 (7)O5—Mo2—Na3—Na2xvii82.4 (7)
Na2ii—Mo1—Na1—Na1i175.8 (3)O1—Mo2—Na3—Na2xvii35.1 (8)
O3—Mo1—Na1—Na1ix141.5 (8)O1iii—Mo2—Na3—Na2xvii164.4 (4)
O2—Mo1—Na1—Na1ix64.4 (11)Na3iii—Mo2—Na3—Na2xvii0.0
O6—Mo1—Na1—Na1ix35.4 (9)Na2—Mo2—Na3—Na2xvii0.0
O4—Mo1—Na1—Na1ix123.7 (11)Na2iv—Mo2—Na3—Na2xvii180.0
Na1i—Mo1—Na1—Na1ix177.4 (12)O5iii—Mo2—O1—Fe3150.4 (7)
Na2ii—Mo1—Na1—Na1ix1.6 (13)O5—Mo2—O1—Fe339.0 (9)
O3—Mo1—Na1—Mo1iii67.0 (4)O1iii—Mo2—O1—Fe384.4 (6)
O2—Mo1—Na1—Mo1iii138.8 (6)Na3—Mo2—O1—Fe374.4 (10)
O6—Mo1—Na1—Mo1iii39.0 (4)Na3iii—Mo2—O1—Fe3105.4 (6)
O4—Mo1—Na1—Mo1iii161.8 (6)Na2—Mo2—O1—Fe3130.5 (11)
Na1i—Mo1—Na1—Mo1iii108.2 (4)Na2iv—Mo2—O1—Fe355.2 (10)
Na2ii—Mo1—Na1—Mo1iii76.0 (6)O5iii—Mo2—O1—Na219.9 (8)
O3—Mo1—Na1—Na2i113.0 (4)O5—Mo2—O1—Na291.4 (8)
O2—Mo1—Na1—Na2i41.2 (6)O1iii—Mo2—O1—Na2145.1 (8)
O6—Mo1—Na1—Na2i141.0 (4)Na3—Mo2—O1—Na256.1 (11)
O4—Mo1—Na1—Na2i18.2 (6)Na3iii—Mo2—O1—Na225.1 (6)
Na1i—Mo1—Na1—Na2i71.8 (4)Na2iv—Mo2—O1—Na2174.3 (3)
Na2ii—Mo1—Na1—Na2i104.0 (6)O5v—Fe3—O1—Mo228 (2)
O1—Fe3—Na2—O1vi140.4 (7)O3vi—Fe3—O1—Mo2152.2 (8)
O5v—Fe3—Na2—O1vi60.7 (8)O4i—Fe3—O1—Mo2121.9 (7)
O3vi—Fe3—Na2—O1vi19.9 (6)O6iii—Fe3—O1—Mo222.0 (7)
O4i—Fe3—Na2—O1vi53.9 (5)O6vii—Fe3—O1—Mo262.0 (7)
O6iii—Fe3—Na2—O1vi162.6 (5)Na2—Fe3—O1—Mo2138.7 (10)
O6vii—Fe3—Na2—O1vi119.3 (5)O5v—Fe3—O1—Na2111 (2)
O5v—Fe3—Na2—O1159.0 (7)O3vi—Fe3—O1—Na213.5 (5)
O3vi—Fe3—Na2—O1160.3 (7)O4i—Fe3—O1—Na299.4 (5)
O4i—Fe3—Na2—O186.4 (6)O6iii—Fe3—O1—Na2160.7 (6)
O6iii—Fe3—Na2—O122.2 (7)O6vii—Fe3—O1—Na276.7 (5)
O6vii—Fe3—Na2—O1100.4 (6)O1vi—Na2—O1—Mo2149.9 (7)
O1—Fe3—Na2—O3vi160.3 (7)O3vi—Na2—O1—Mo2152.7 (8)
O5v—Fe3—Na2—O3vi40.7 (8)O3—Na2—O1—Mo294.9 (7)
O4i—Fe3—Na2—O3vi73.8 (6)O2ii—Na2—O1—Mo29.2 (8)
O6iii—Fe3—Na2—O3vi177.5 (7)O2vii—Na2—O1—Mo265.5 (7)
O6vii—Fe3—Na2—O3vi99.4 (6)Fe3—Na2—O1—Mo2140.0 (10)
O1—Fe3—Na2—O357.8 (5)Fe3vi—Na2—O1—Mo2107.4 (7)
O5v—Fe3—Na2—O3143.2 (6)Mo1ii—Na2—O1—Mo237.5 (8)
O3vi—Fe3—Na2—O3102.4 (7)Mo1vii—Na2—O1—Mo288.0 (6)
O4i—Fe3—Na2—O328.6 (5)Mo2x—Na2—O1—Mo2167.9 (7)
O6iii—Fe3—Na2—O380.1 (6)O1vi—Na2—O1—Fe370.1 (3)
O6vii—Fe3—Na2—O3158.2 (4)O3vi—Na2—O1—Fe312.7 (5)
O1—Fe3—Na2—O2ii51.6 (7)O3—Na2—O1—Fe3125.1 (5)
O5v—Fe3—Na2—O2ii107.4 (7)O2ii—Na2—O1—Fe3149.2 (4)
O3vi—Fe3—Na2—O2ii148.2 (7)O2vii—Na2—O1—Fe374.4 (5)
O4i—Fe3—Na2—O2ii138.0 (6)Fe3vi—Na2—O1—Fe3112.6 (4)
O6iii—Fe3—Na2—O2ii29.3 (7)Mo1ii—Na2—O1—Fe3177.5 (3)
O6vii—Fe3—Na2—O2ii48.8 (6)Mo1vii—Na2—O1—Fe352.0 (4)
O1—Fe3—Na2—O2vii104.9 (6)Mo2—Na2—O1—Fe3140.0 (10)
O5v—Fe3—Na2—O2vii54.1 (7)Mo2x—Na2—O1—Fe327.9 (15)
O3vi—Fe3—Na2—O2vii94.8 (6)O3—Mo1—O2—Na2ii66.9 (7)
O4i—Fe3—Na2—O2vii168.7 (4)O6—Mo1—O2—Na2ii54.7 (8)
O6iii—Fe3—Na2—O2vii82.7 (5)O4—Mo1—O2—Na2ii174.8 (5)
O6vii—Fe3—Na2—O2vii4.6 (4)Na1i—Mo1—O2—Na2ii137.2 (4)
O1—Fe3—Na2—Fe3vi94.6 (5)Na1—Mo1—O2—Na2ii139.0 (4)
O5v—Fe3—Na2—Fe3vi106.4 (6)O3—Mo1—O2—Na3xviii179.7 (6)
O3vi—Fe3—Na2—Fe3vi65.7 (5)O6—Mo1—O2—Na3xviii58.1 (8)
O4i—Fe3—Na2—Fe3vi8.2 (3)O4—Mo1—O2—Na3xviii62.0 (7)
O6iii—Fe3—Na2—Fe3vi116.8 (4)Na1i—Mo1—O2—Na3xviii110.0 (6)
O6vii—Fe3—Na2—Fe3vi165.1 (3)Na2ii—Mo1—O2—Na3xviii112.8 (9)
O1—Fe3—Na2—Mo1ii4.9 (6)Na1—Mo1—O2—Na3xviii26.2 (9)
O5v—Fe3—Na2—Mo1ii154.0 (6)O3—Mo1—O2—Na3xix52.4 (9)
O3vi—Fe3—Na2—Mo1ii165.2 (8)O6—Mo1—O2—Na3xix174.0 (8)
O4i—Fe3—Na2—Mo1ii91.4 (6)O4—Mo1—O2—Na3xix65.9 (9)
O6iii—Fe3—Na2—Mo1ii17.3 (8)Na1i—Mo1—O2—Na3xix17.9 (10)
O6vii—Fe3—Na2—Mo1ii95.4 (6)Na2ii—Mo1—O2—Na3xix119.3 (11)
O1—Fe3—Na2—Mo1vii116.8 (5)Na1—Mo1—O2—Na3xix101.7 (8)
O5v—Fe3—Na2—Mo1vii42.2 (6)O2—Mo1—O3—Fe3vi31.8 (10)
O3vi—Fe3—Na2—Mo1vii82.9 (5)O6—Mo1—O3—Fe3vi152.7 (8)
O4i—Fe3—Na2—Mo1vii156.7 (3)O4—Mo1—O3—Fe3vi87.3 (10)
O6iii—Fe3—Na2—Mo1vii94.6 (4)Na1i—Mo1—O3—Fe3vi89.2 (8)
O6vii—Fe3—Na2—Mo1vii16.5 (3)Na2ii—Mo1—O3—Fe3vi66.3 (8)
O1—Fe3—Na2—Mo218.3 (5)Na1—Mo1—O3—Fe3vi129.6 (8)
O5v—Fe3—Na2—Mo2140.7 (6)O2—Mo1—O3—Na2158.6 (7)
O3vi—Fe3—Na2—Mo2178.6 (5)O6—Mo1—O3—Na237.6 (11)
O4i—Fe3—Na2—Mo2104.7 (4)O4—Mo1—O3—Na282.4 (9)
O6iii—Fe3—Na2—Mo23.9 (5)Na1i—Mo1—O3—Na280.4 (8)
O6vii—Fe3—Na2—Mo282.0 (3)Na2ii—Mo1—O3—Na2124.0 (8)
O1—Fe3—Na2—Mo2x169.7 (6)Na1—Mo1—O3—Na240.1 (9)
O5v—Fe3—Na2—Mo2x31.3 (7)O1vi—Na2—O3—Mo1159.8 (10)
O3vi—Fe3—Na2—Mo2x9.4 (5)O1—Na2—O3—Mo19.0 (9)
O4i—Fe3—Na2—Mo2x83.2 (4)O3vi—Na2—O3—Mo181.4 (8)
O6iii—Fe3—Na2—Mo2x168.1 (4)O2ii—Na2—O3—Mo1105.4 (9)
O6vii—Fe3—Na2—Mo2x90.0 (4)O2vii—Na2—O3—Mo177.8 (16)
O5iii—Mo2—Na2—O1vi92.1 (13)Fe3—Na2—O3—Mo140.4 (9)
O5—Mo2—Na2—O1vi170.2 (13)Fe3vi—Na2—O3—Mo1172.1 (12)
O1—Mo2—Na2—O1vi68.5 (18)Mo1ii—Na2—O3—Mo1112.3 (9)
O1iii—Mo2—Na2—O1vi15.8 (9)Mo1vii—Na2—O3—Mo121 (2)
Na3—Mo2—Na2—O1vi140.1 (12)Mo2—Na2—O3—Mo115.5 (8)
Na3iii—Mo2—Na2—O1vi140.1 (12)Mo2x—Na2—O3—Mo1170.9 (8)
Na2iv—Mo2—Na2—O1vi39.9 (12)O1vi—Na2—O3—Fe3vi12.3 (4)
O5iii—Mo2—Na2—O1160.6 (8)O1—Na2—O3—Fe3vi163.1 (5)
O5—Mo2—Na2—O1101.6 (9)O3vi—Na2—O3—Fe3vi90.8 (4)
O1iii—Mo2—Na2—O152.8 (13)O2ii—Na2—O3—Fe3vi82.4 (5)
Na3—Mo2—Na2—O1151.4 (7)O2vii—Na2—O3—Fe3vi110.0 (12)
Na3iii—Mo2—Na2—O1151.4 (7)Fe3—Na2—O3—Fe3vi131.8 (4)
Na2iv—Mo2—Na2—O128.6 (7)Mo1ii—Na2—O3—Fe3vi75.5 (4)
O5iii—Mo2—Na2—O3vi172.8 (6)Mo1vii—Na2—O3—Fe3vi151.2 (13)
O5—Mo2—Na2—O3vi75.0 (6)Mo2—Na2—O3—Fe3vi172.4 (4)
O1—Mo2—Na2—O3vi26.6 (8)Mo2x—Na2—O3—Fe3vi1.2 (4)
O1iii—Mo2—Na2—O3vi79.4 (7)O3—Mo1—O4—Fe3i116.5 (9)
Na3—Mo2—Na2—O3vi124.8 (4)O2—Mo1—O4—Fe3i3.0 (10)
Na3iii—Mo2—Na2—O3vi124.8 (4)O6—Mo1—O4—Fe3i122.9 (8)
Na2iv—Mo2—Na2—O3vi55.2 (4)Na1i—Mo1—O4—Fe3i119.0 (11)
O5iii—Mo2—Na2—O377.3 (6)Na2ii—Mo1—O4—Fe3i8.9 (14)
O5—Mo2—Na2—O3175.1 (6)Na1—Mo1—O4—Fe3i144.1 (12)
O1—Mo2—Na2—O383.3 (8)O3—Mo1—O4—Na1i2.4 (7)
O1iii—Mo2—Na2—O330.5 (7)O2—Mo1—O4—Na1i122.0 (6)
Na3—Mo2—Na2—O3125.4 (3)O6—Mo1—O4—Na1i118.1 (6)
Na3iii—Mo2—Na2—O3125.4 (3)Na2ii—Mo1—O4—Na1i127.9 (5)
Na2iv—Mo2—Na2—O354.6 (3)Na1—Mo1—O4—Na1i97.0 (7)
O5iii—Mo2—Na2—O2ii11.0 (5)O3—Mo1—O4—Na199.4 (6)
O5—Mo2—Na2—O2ii86.8 (6)O2—Mo1—O4—Na1141.1 (6)
O1—Mo2—Na2—O2ii171.6 (8)O6—Mo1—O4—Na121.1 (8)
O1iii—Mo2—Na2—O2ii118.8 (7)Na1i—Mo1—O4—Na197.0 (7)
Na3—Mo2—Na2—O2ii37.1 (3)Na2ii—Mo1—O4—Na1135.2 (5)
Na3iii—Mo2—Na2—O2ii37.1 (3)O4viii—Na1—O4—Mo173.1 (7)
Na2iv—Mo2—Na2—O2ii142.9 (3)O4i—Na1—O4—Mo1106.2 (8)
O5iii—Mo2—Na2—O2vii85.3 (6)O4iii—Na1—O4—Mo1163.4 (6)
O5—Mo2—Na2—O2vii12.4 (6)Mo1i—Na1—O4—Mo1134.0 (6)
O1—Mo2—Na2—O2vii114.1 (7)Mo1viii—Na1—O4—Mo1100.0 (6)
O1iii—Mo2—Na2—O2vii166.8 (6)Na1i—Na1—O4—Mo1106.2 (8)
Na3—Mo2—Na2—O2vii37.3 (3)Na1ix—Na1—O4—Mo177.3 (14)
Na3iii—Mo2—Na2—O2vii37.3 (3)Mo1iii—Na1—O4—Mo136.1 (13)
Na2iv—Mo2—Na2—O2vii142.7 (3)Na2i—Na1—O4—Mo1163.4 (6)
O5iii—Mo2—Na2—Fe3171.9 (5)O4viii—Na1—O4—Fe3i80.0 (6)
O5—Mo2—Na2—Fe374.1 (5)O4i—Na1—O4—Fe3i100.7 (7)
O1—Mo2—Na2—Fe327.5 (7)O4iii—Na1—O4—Fe3i10.3 (4)
O1iii—Mo2—Na2—Fe380.3 (6)Mo1i—Na1—O4—Fe3i72.9 (5)
Na3—Mo2—Na2—Fe3123.88 (10)Mo1viii—Na1—O4—Fe3i53.1 (4)
Na3iii—Mo2—Na2—Fe3123.88 (10)Na1i—Na1—O4—Fe3i100.7 (7)
Na2iv—Mo2—Na2—Fe356.12 (10)Na1ix—Na1—O4—Fe3i75.8 (14)
O5iii—Mo2—Na2—Fe3vi71.4 (5)Mo1—Na1—O4—Fe3i153.1 (10)
O5—Mo2—Na2—Fe3vi169.2 (5)Mo1iii—Na1—O4—Fe3i170.9 (6)
O1—Mo2—Na2—Fe3vi89.2 (8)Na2i—Na1—O4—Fe3i10.3 (4)
O1iii—Mo2—Na2—Fe3vi36.4 (7)O4viii—Na1—O4—Na1i179.3 (10)
Na3—Mo2—Na2—Fe3vi119.4 (3)O4i—Na1—O4—Na1i0.0
Na3iii—Mo2—Na2—Fe3vi119.4 (3)O4iii—Na1—O4—Na1i90.4 (5)
Na2iv—Mo2—Na2—Fe3vi60.6 (3)Mo1i—Na1—O4—Na1i27.8 (4)
O5iii—Mo2—Na2—Mo1ii14.3 (5)Mo1viii—Na1—O4—Na1i153.8 (7)
O5—Mo2—Na2—Mo1ii112.0 (5)Na1ix—Na1—O4—Na1i176.5 (16)
O1—Mo2—Na2—Mo1ii146.4 (7)Mo1—Na1—O4—Na1i106.2 (8)
O1iii—Mo2—Na2—Mo1ii93.6 (6)Mo1iii—Na1—O4—Na1i70.2 (9)
Na3—Mo2—Na2—Mo1ii62.27 (14)Na2i—Na1—O4—Na1i90.4 (5)
Na3iii—Mo2—Na2—Mo1ii62.27 (14)O5iii—Mo2—O5—Fe3v153.9 (12)
Na2iv—Mo2—Na2—Mo1ii117.73 (14)O1—Mo2—O5—Fe3v38.2 (11)
O5iii—Mo2—Na2—Mo1vii111.1 (5)O1iii—Mo2—O5—Fe3v88.0 (9)
O5—Mo2—Na2—Mo1vii13.3 (5)Na3—Mo2—O5—Fe3v163.6 (13)
O1—Mo2—Na2—Mo1vii88.3 (7)Na3iii—Mo2—O5—Fe3v121.6 (9)
O1iii—Mo2—Na2—Mo1vii141.1 (6)Na2—Mo2—O5—Fe3v74.5 (9)
Na3—Mo2—Na2—Mo1vii63.07 (11)Na2iv—Mo2—O5—Fe3v99.3 (9)
Na3iii—Mo2—Na2—Mo1vii63.07 (11)O5iii—Mo2—O5—Na342.5 (3)
Na2iv—Mo2—Na2—Mo1vii116.93 (11)O1—Mo2—O5—Na3158.2 (5)
O5iii—Mo2—Na2—Mo2x48.0 (5)O1iii—Mo2—O5—Na375.6 (7)
O5—Mo2—Na2—Mo2x49.7 (5)Na3iii—Mo2—O5—Na374.8 (4)
O1—Mo2—Na2—Mo2x151.4 (7)Na2—Mo2—O5—Na3121.8 (4)
O1iii—Mo2—Na2—Mo2x155.9 (6)Na2iv—Mo2—O5—Na364.3 (4)
Na3—Mo2—Na2—Mo2x0.000 (3)O2xi—Na3—O5—Mo2130.8 (7)
Na3iii—Mo2—Na2—Mo2x0.000 (2)O2xii—Na3—O5—Mo249.2 (7)
Na2iv—Mo2—Na2—Mo2x180.000 (1)O5xiii—Na3—O5—Mo2158 (100)
O5iii—Mo2—Na3—O2xi87.9 (5)O2xiv—Na3—O5—Mo266.8 (6)
O5—Mo2—Na3—O2xi46.2 (7)O2xv—Na3—O5—Mo2113.2 (6)
O1—Mo2—Na3—O2xi1.2 (8)Mo2xiii—Na3—O5—Mo2180.0
O1iii—Mo2—Na3—O2xi159.3 (5)Na3xvi—Na3—O5—Mo2101.1 (6)
Na3iii—Mo2—Na3—O2xi36.3 (3)Na3iii—Na3—O5—Mo278.9 (6)
Na2—Mo2—Na3—O2xi36.3 (3)Na2iv—Na3—O5—Mo268.9 (5)
Na2iv—Mo2—Na3—O2xi143.7 (3)Na2xvii—Na3—O5—Mo2111.1 (5)
O5iii—Mo2—Na3—O2xii92.1 (5)O2xi—Na3—O5—Fe3v65.7 (7)
O5—Mo2—Na3—O2xii133.8 (7)O2xii—Na3—O5—Fe3v114.3 (7)
O1—Mo2—Na3—O2xii178.8 (8)O5xiii—Na3—O5—Fe3v39 (100)
O1iii—Mo2—Na3—O2xii20.7 (5)O2xiv—Na3—O5—Fe3v129.7 (7)
Na3iii—Mo2—Na3—O2xii143.7 (3)O2xv—Na3—O5—Fe3v50.3 (7)
Na2—Mo2—Na3—O2xii143.7 (3)Mo2—Na3—O5—Fe3v163.5 (13)
Na2iv—Mo2—Na3—O2xii36.3 (3)Mo2xiii—Na3—O5—Fe3v16.5 (13)
O5iii—Mo2—Na3—O5134.1 (7)Na3xvi—Na3—O5—Fe3v62.3 (8)
O1—Mo2—Na3—O547.4 (10)Na3iii—Na3—O5—Fe3v117.7 (8)
O1iii—Mo2—Na3—O5113.2 (8)Na2iv—Na3—O5—Fe3v94.5 (8)
Na3iii—Mo2—Na3—O582.4 (7)Na2xvii—Na3—O5—Fe3v85.5 (8)
Na2—Mo2—Na3—O582.4 (7)O3—Mo1—O6—Fe3iii157.8 (9)
Na2iv—Mo2—Na3—O597.6 (7)O2—Mo1—O6—Fe3iii80.9 (11)
O5iii—Mo2—Na3—O5xiii45.9 (7)O4—Mo1—O6—Fe3iii38.8 (12)
O5—Mo2—Na3—O5xiii180.0Na1i—Mo1—O6—Fe3iii87.5 (10)
O1—Mo2—Na3—O5xiii132.6 (10)Na2ii—Mo1—O6—Fe3iii111.2 (10)
O1iii—Mo2—Na3—O5xiii66.8 (8)Na1—Mo1—O6—Fe3iii52.9 (9)
Na3iii—Mo2—Na3—O5xiii97.6 (7)O3—Mo1—O6—Fe3xx57.3 (8)
Na2—Mo2—Na3—O5xiii97.6 (7)O2—Mo1—O6—Fe3xx64.0 (8)
Na2iv—Mo2—Na3—O5xiii82.4 (7)O4—Mo1—O6—Fe3xx176.2 (6)
O5iii—Mo2—Na3—O2xiv18.1 (5)Na1i—Mo1—O6—Fe3xx127.5 (6)
O5—Mo2—Na3—O2xiv116.0 (7)Na2ii—Mo1—O6—Fe3xx33.7 (6)
O1—Mo2—Na3—O2xiv68.6 (8)Na1—Mo1—O6—Fe3xx162.2 (7)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+3/2, y+1/2, z+1; (iii) x+2, y, z+1/2; (iv) x, y, z1; (v) x+5/2, y+1/2, z+1; (vi) x+2, y, z+3/2; (vii) x+1/2, y+1/2, z+1/2; (viii) x, y+1, z1/2; (ix) x+2, y+1, z; (x) x, y, z+1; (xi) x+1/2, y1/2, z; (xii) x+3/2, y+1/2, z; (xiii) x+2, y, z; (xiv) x+3/2, y1/2, z+1/2; (xv) x+1/2, y+1/2, z1/2; (xvi) x+2, y, z1/2; (xvii) x+2, y, z+1; (xviii) x1/2, y+1/2, z; (xix) x+3/2, y+1/2, z+1/2; (xx) x1/2, y+1/2, z1/2.

Experimental details

(1)(2)(3)(4)
Crystal data
Chemical formulaFe4Mo5NaO20Fe2Mo3NaO12Fe2Mo3NaO12Fe2Mo3Na3O12
Mr1046.09614.51614.51660.49
Crystal system, space groupTriclinic, P1?, P1?, P1?, C2/c
Temperature (K)293293293293
a, b, c (Å)6.9337 (3), 7.0196 (4), 17.8033 (8)6.9253 (4), 6.9513 (4), 11.0600 (9)6.834 (1), 6.893 (1), 11.667 (3)12.646 (3), 13.685 (3), 7.206 (2)
α, β, γ (°)87.468 (4), 87.615 (4), 79.090 (4)80.205 (6), 83.679 (6), 80.818 (5)76.23 (2), 75.78 (2), 87.76 (2)90, 112.56 (3), 90
V3)849.54 (7)516.06 (6)517.33 (17)1151.6 (5)
Z2224
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)7.006.396.375.81
Crystal size (mm)0.21 × 0.19 × 0.140.20 × 0.11 × 0.100.07 × 0.02 × 0.010.08 × 0.04 × 0.04
Data collection
DiffractometerOxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detectorOxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detectorOxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detectorOxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector
Absorption correctionNumeric analyticalNumeric analyticalNumeric analyticalNumeric analytical
Tmin, Tmax0.300, 0.4440.321, 0.5650.683, 0.9230.766, 0.886
No. of measured, independent and
observed [I > 2σ(I)] reflections
37235, 11, 9620 4259, 2705, 2454 4315, 2180, 1188 2221, 1055, 791
Rint0.0350.0270.0610.043
(sin θ/λ)max1)0.9700.7780.7100.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.078, 1.13 0.031, 0.081, 1.14 0.036, 0.129, 0.59 0.062, 0.196, 1.14
No. of reflections11711270521801055
No. of parameters27116416395
w = 1/[σ2(Fo2) + (0.0311P)2 + 1.1496P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0365P)2 + 2.671P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.1072P)2 + 11.9291P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.54, 2.290.98, 2.030.85, 0.901.34, 2.63

Computer programs: CrysAlis CCD (Oxford Diffraction Limited, 2001), CrysAlis RED (Oxford Diffraction Limited, 2001), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), Diamond (Brandenburg, 2001).

 

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