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The compounds K4CoMo4O15 (tetra­potassium cobalt tetra­molybdate), K6CoMo5O19 (hexa­potassium cobalt pentamolybdate) and K10CoMo7O27 (deca­potassium cobalt hepta­molybdate) belong to a series of compounds with closely related crystal structures. In K4CoMo4O15, the Co atom and one of the two unique Mo atoms are at sites with threefold symmetry; two of the three unique K atoms lie at sites with \overline{3} symmetry. K6CoMo5O19 crystallizes in a new monoclinic structure type. Each [CoO6] octa­hedron is surrounded by one face-sharing [MoO6] octa­hedron and six corner-sharing [MoO4] tetra­hedra. All three compounds have this structural unit in common, but differ in the degree of connectivity between these units. They form layers in K4CoMo4O15 and zigzag chains in K6CoMo5O19, both by sharing [MoO4] tetra­hedra. In K10CoMo7O27, the structural units are isolated from each other.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105025242/sq1222sup1.cif
Contains datablocks I, II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105025242/sq1222Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105025242/sq1222IIsup3.hkl
Contains datablock II

Comment top

Quarternary compounds of alkali metals (A), 3 d transition metals (T), molybdenum and oxygen exist with a rich variety of crystal structures. The most common types are orthomolybdates AxTy(MoO4)z with networks of [TO6] octahedra and [MoO4] tetrahedra. In the course of a systematic investigation of crystalline phases in the Na–Fe–Mo–O system, four orthomolybdate structures, namely α-NaFe2(MoO4)3, β-NaFe2(MoO4)3, Na3Fe2(MoO4)3 and NaFe4(MoO4)5, were established (Muessig et al., 2003) and only one phase, Na3Fe2Mo5O16, with both [MoO4] tetrahedra and [MoO6] octahedra (Bramnik et al., 2003). This study has now been extended to the K–Co–Mo–O system. To date, only one orthomolybdate, K2Co2(MoO4)3, has been reported for this system in full detail (Klevtsova et al., 1980). Furthermore, a second orthomolybdate, K4Co(MoO4)3, is described as isostructural with K4Mn(MoO4)3 (Solodovnikov et al., 1998). For two other compounds, K4TMo4O15 and K10TMo7O27, crystal structures with both [MoO4] tetrahedra and [MoO6] octahedra have been established for T = Mn from single-crystal X-ray diffraction and are reported as isostructural for T = Co, but based on powder diffraction data only (Solodovnikov, Klevtsova et al., 1997; Solodovnikov, Zolotova et al., 1997). In this contribution, we present structural data for K4CoMo4O15 and for a new compound, K6CoMo5O19, both from single-crystal X-ray diffraction studies. The crystal structures of K4CoMo4O15, K6CoMo5O19, and K10CoMo7O27 are closely related to each other and can be considered as three members of one structure family of compounds K2nCoMo2 + nO7 + 4n, with n = 2, 3 and 5.

The present results confirm the proposed structure model for K4CoMo4O15 (Solodovnikov, Zolotova et al., 1997), while the crystal structure of the new compound, K6CoMo5O19, has been solved and refined. It is now evident from its crystal structure that K6CoMo5O19 fits into a series of structures of compounds with the general formula K2nCoMo2 + nO7 + 4n with n = 3. Other representatives are known for n = 2 (K4CoMo4O15; Solodovnikov, Zolotova et al., 1997) and n = 5 (K10CoMo7O27; Solodovnikov, Klevtsova et al., 1997). Bond lengths and charge balances are in agreement with formal oxidation states of Co2+ and Mo6+ for all compounds. The structures have one motif in common: [CoO6] and [MoO6] octahedra share faces and, in addition, each [CoO6] octahedron is further connected with six [MoO4] tetrahedra by sharing corners. The difference between these structures is the connectivity of these CoO6 octahedra with each other. If m is the number of neighbouring octahedral units linked by sharing of [MoO4] tetrahedra, the equation m + n = 5 holds for all three representatives.

A comparison of the different connectivity schemes is shown in Fig. 1. In all structures, the orientations of the face-sharing [MoO6] and [CoO6] pairs of octahedra alternate. Note that in Fig. 1 the smaller [MoO6] octahedra behind the [CoO6] octahedra cannot be seen.

In terms of the structural systematics outlined here, dimers of face-sharing octahedra (m = 1) linked by [MoO4] tetrahedra should be observed for the hypothetical compound K8CoMo6O23 (n = 4). This proposed member of the structure family has not yet been found.

Experimental top

All samples were prepared from K2MoO4 (Aldrich, 98%), CoO (Alfa Aesar, 99.999%) and MoO3 (Sigma–Aldrich, 99.5+%). Different ratios [Brief details?] were mixed in an agate mortar, pressed into pellets and placed in silica tubes, which were then sealed with an ambient air atmosphere inside. The samples were heated to temperatures between 773 and 923 K for 48 h and then cooled to room temperature. The samples thus obtained consist of several K–Mo–O and Co–Mo–O ternary and K–Co–Mo–O quarternary phases.

Computing details top

For both compounds, data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis RED (Oxford Diffraction, 2003); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. Different connectivity schemes for the same basic structural units in K2nCoMo2 + nO7 + 4n compounds for n = 2, 3 and 5 (from top to bottom, respectively). [MoO4] and [CoO6/MoO6] polyhedra are shown in light grey, while the K+ ions are shown as isolated black circles.
(I) tetrapotassium cobalt tetramolybdate top
Crystal data top
K4CoMo4O15Dx = 3.738 Mg m3
Mr = 839.09Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3Cell parameters from 2013 reflections
a = 10.292 (1) Åθ = 2.3–30.1°
c = 8.1271 (8) ŵ = 5.55 mm1
V = 745.53 (13) Å3T = 298 K
Z = 2Prism, blue
F(000) = 7820.04 × 0.04 × 0.03 mm
Data collection top
Oxford Xcalibur with Sapphire CCD area detector
diffractometer
1318 independent reflections
Radiation source: fine-focus sealed tube1041 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
ω and ϕ scansθmax = 30.0°, θmin = 3.4°
Absorption correction: numerical
[CrysAlis RED (Oxford Diffraction Ltd, 2003); analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid (Reference?)].
h = 1314
Tmin = 0.771, Tmax = 0.835k = 1414
3620 measured reflectionsl = 1011
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)] = 0.045 w = 1/[σ2(Fo2) + (0.0329P)2 + 3.9972P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.094(Δ/σ)max < 0.001
S = 1.09Δρmax = 1.72 e Å3
1318 reflectionsΔρmin = 1.09 e Å3
75 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0009 (4)
Crystal data top
K4CoMo4O15Z = 2
Mr = 839.09Mo Kα radiation
Trigonal, P3µ = 5.55 mm1
a = 10.292 (1) ÅT = 298 K
c = 8.1271 (8) Å0.04 × 0.04 × 0.03 mm
V = 745.53 (13) Å3
Data collection top
Oxford Xcalibur with Sapphire CCD area detector
diffractometer
1318 independent reflections
Absorption correction: numerical
[CrysAlis RED (Oxford Diffraction Ltd, 2003); analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid (Reference?)].
1041 reflections with I > 2σ(I)
Tmin = 0.771, Tmax = 0.835Rint = 0.047
3620 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04575 parameters
wR(F2) = 0.0940 restraints
S = 1.09Δρmax = 1.72 e Å3
1318 reflectionsΔρmin = 1.09 e Å3
Special details top

Experimental. Suitable single crystals for X-ray diffraction studies were selected under a light microscope and were fixed on glass fibres. Diffraction data were collected in ω- and ϕ-scan mode on the Xcalibur system from Oxford Diffraction, equipped with a Sapphire2 CCD detector and the ENHANCE X-ray source option.

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
Mo10.65875 (6)0.01422 (6)0.63700 (6)0.01147 (17)
Mo20.66670.33331.14197 (12)0.0160 (3)
Co10.66670.33330.53410 (16)0.0067 (3)
K10.3920 (2)0.0873 (2)0.8608 (2)0.0274 (4)
K21.00000.00000.00000.0239 (9)
K30.00000.00000.50000.0295 (10)
O10.6376 (5)0.1466 (5)0.6613 (6)0.0170 (10)
O20.7817 (6)0.0071 (6)0.7902 (6)0.0200 (11)
O30.4792 (5)0.1839 (5)0.6590 (6)0.0173 (10)
O40.7266 (6)0.0116 (5)0.4418 (6)0.0207 (11)
O50.5178 (6)0.3414 (6)1.0504 (6)0.0267 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0100 (3)0.0106 (3)0.0134 (3)0.0048 (2)0.0008 (2)0.0001 (2)
Mo20.0174 (4)0.0174 (4)0.0132 (5)0.00868 (18)0.0000.000
Co10.0061 (4)0.0061 (4)0.0079 (7)0.0030 (2)0.0000.000
K10.0333 (10)0.0267 (10)0.0264 (8)0.0182 (8)0.0059 (7)0.0002 (7)
K20.0247 (13)0.0247 (13)0.0223 (19)0.0124 (7)0.0000.000
K30.0140 (12)0.0140 (12)0.060 (3)0.0070 (6)0.0000.000
O10.018 (3)0.018 (3)0.020 (2)0.012 (2)0.0035 (19)0.0040 (19)
O20.021 (3)0.018 (3)0.022 (2)0.012 (2)0.012 (2)0.004 (2)
O30.016 (3)0.013 (2)0.020 (2)0.005 (2)0.0001 (19)0.0017 (19)
O40.021 (3)0.021 (3)0.020 (2)0.011 (2)0.001 (2)0.003 (2)
O50.027 (3)0.033 (3)0.022 (3)0.017 (3)0.005 (2)0.001 (2)
Geometric parameters (Å, º) top
Mo1—O41.728 (5)K1—Mo1iv3.5124 (18)
Mo1—O21.751 (4)K1—K2xi3.8394 (19)
Mo1—O11.785 (5)K2—O2xii2.791 (4)
Mo1—O31.808 (5)K2—O2xiii2.791 (4)
Mo1—K1i3.5124 (18)K2—O2xiv2.791 (4)
Mo1—K3ii3.6169 (7)K2—O2xv2.791 (4)
Mo1—K13.8477 (19)K2—O2viii2.791 (4)
Mo1—K1iii4.1007 (18)K2—O2xvi2.791 (4)
Mo2—O5i1.743 (5)K2—K1xvii3.8394 (19)
Mo2—O5iv1.743 (5)K2—K1xviii3.8394 (19)
Mo2—O51.743 (5)K2—K1xix3.8394 (19)
Mo2—O3v2.220 (5)K2—K1xx3.8394 (19)
Mo2—O3vi2.220 (5)K2—K1iii3.8394 (19)
Mo2—O3vii2.220 (5)K2—K1xxi3.8394 (19)
Mo2—K13.5305 (19)K3—O4xxii2.797 (5)
Mo2—K1i3.5305 (19)K3—O4iii2.797 (5)
Mo2—K1iv3.5305 (19)K3—O4iv2.797 (5)
Mo2—K1vi4.0610 (18)K3—O4xxiii2.797 (5)
Mo2—K1v4.0610 (18)K3—O4xxiv2.797 (5)
Mo2—K1vii4.0610 (18)K3—O4xxv2.797 (5)
Co1—O12.068 (5)K3—O2xxii3.233 (5)
Co1—O1i2.068 (5)K3—O2iv3.233 (5)
Co1—O1iv2.068 (5)K3—O2xxiii3.233 (5)
Co1—O3iii2.185 (5)K3—O2iii3.233 (5)
Co1—O3viii2.185 (5)K3—O2xxiv3.233 (5)
Co1—O3ix2.185 (5)K3—O2xxv3.233 (5)
Co1—K1i3.781 (2)O1—K1i2.947 (5)
Co1—K13.781 (2)O2—K2xxvi2.791 (4)
Co1—K1iv3.781 (2)O2—K1i2.850 (5)
K1—O5x2.596 (6)O2—K1vi3.232 (5)
K1—O4iii2.682 (5)O2—K3ii3.233 (5)
K1—O52.739 (6)O3—Co1iii2.185 (5)
K1—O12.801 (5)O3—Mo2vi2.220 (5)
K1—O2iv2.850 (5)O4—K1iii2.682 (5)
K1—O5i2.868 (6)O4—K3ii2.797 (5)
K1—O1iv2.947 (5)O5—K1vii2.596 (6)
K1—O2vi3.232 (5)O5—K1iv2.868 (6)
O4—Mo1—O2112.0 (2)O1—K1—Co132.51 (10)
O4—Mo1—O1108.8 (2)O2iv—K1—Co189.33 (10)
O2—Mo1—O1107.7 (2)O5i—K1—Co183.57 (12)
O4—Mo1—O3108.4 (2)O1iv—K1—Co132.94 (9)
O2—Mo1—O3109.8 (2)O2vi—K1—Co1156.95 (11)
O1—Mo1—O3110.2 (2)Mo1iv—K1—Co159.65 (3)
O4—Mo1—K1i110.78 (17)Mo2—K1—Co184.94 (4)
O2—Mo1—K1i53.71 (16)O5x—K1—K2xi92.03 (13)
O1—Mo1—K1i56.96 (16)O4iii—K1—K2xi85.97 (12)
O3—Mo1—K1i140.81 (15)O5—K1—K2xi89.84 (12)
O4—Mo1—K3ii48.72 (17)O1—K1—K2xi161.74 (11)
O2—Mo1—K3ii63.27 (17)O2iv—K1—K2xi46.48 (9)
O1—Mo1—K3ii124.25 (15)O5i—K1—K2xi129.94 (11)
O3—Mo1—K3ii124.90 (15)O1iv—K1—K2xi105.28 (10)
K1i—Mo1—K3ii82.41 (3)O2vi—K1—K2xi45.50 (8)
O4—Mo1—K1140.10 (18)Mo1iv—K1—K2xi75.98 (3)
O2—Mo1—K1104.56 (17)Mo2—K1—K2xi110.37 (4)
O1—Mo1—K142.39 (15)Co1—K1—K2xi135.22 (5)
O3—Mo1—K172.08 (16)O2xii—K2—O2xiii93.40 (15)
K1i—Mo1—K178.46 (6)O2xii—K2—O2xiv86.60 (15)
K3ii—Mo1—K1160.86 (3)O2xiii—K2—O2xiv180.00 (19)
O4—Mo1—K1iii27.19 (17)O2xii—K2—O2xv93.40 (15)
O2—Mo1—K1iii137.10 (17)O2xiii—K2—O2xv86.60 (15)
O1—Mo1—K1iii102.47 (15)O2xiv—K2—O2xv93.40 (15)
O3—Mo1—K1iii86.87 (15)O2xii—K2—O2viii180.00 (15)
K1i—Mo1—K1iii130.50 (4)O2xiii—K2—O2viii86.60 (15)
K3ii—Mo1—K1iii74.68 (3)O2xiv—K2—O2viii93.40 (15)
K1—Mo1—K1iii118.26 (3)O2xv—K2—O2viii86.60 (15)
O5i—Mo2—O5iv103.1 (2)O2xii—K2—O2xvi86.60 (15)
O5i—Mo2—O5103.1 (2)O2xiii—K2—O2xvi93.40 (15)
O5iv—Mo2—O5103.1 (2)O2xiv—K2—O2xvi86.60 (15)
O5i—Mo2—O3v92.2 (2)O2xv—K2—O2xvi180.0
O5iv—Mo2—O3v88.1 (2)O2viii—K2—O2xvi93.40 (15)
O5—Mo2—O3v158.3 (2)O2xii—K2—K1xvii47.75 (10)
O5i—Mo2—O3vi88.1 (2)O2xiii—K2—K1xvii115.55 (10)
O5iv—Mo2—O3vi158.3 (2)O2xiv—K2—K1xvii64.45 (10)
O5—Mo2—O3vi92.2 (2)O2xv—K2—K1xvii55.67 (11)
O3v—Mo2—O3vi72.74 (19)O2viii—K2—K1xvii132.25 (10)
O5i—Mo2—O3vii158.3 (2)O2xvi—K2—K1xvii124.33 (11)
O5iv—Mo2—O3vii92.2 (2)O2xii—K2—K1xviii132.25 (10)
O5—Mo2—O3vii88.1 (2)O2xiii—K2—K1xviii64.45 (10)
O3v—Mo2—O3vii72.74 (19)O2xiv—K2—K1xviii115.55 (10)
O3vi—Mo2—O3vii72.74 (19)O2xv—K2—K1xviii124.33 (11)
O5i—Mo2—K153.74 (18)O2viii—K2—K1xviii47.75 (10)
O5iv—Mo2—K1114.34 (18)O2xvi—K2—K1xviii55.67 (11)
O5—Mo2—K149.47 (18)K1xvii—K2—K1xviii180.00 (5)
O3v—Mo2—K1141.54 (13)O2xii—K2—K1xix55.67 (11)
O3vi—Mo2—K187.31 (13)O2xiii—K2—K1xix47.75 (10)
O3vii—Mo2—K1132.75 (13)O2xiv—K2—K1xix132.25 (10)
O5i—Mo2—K1i49.47 (18)O2xv—K2—K1xix64.45 (10)
O5iv—Mo2—K1i53.74 (18)O2viii—K2—K1xix124.33 (11)
O5—Mo2—K1i114.34 (18)O2xvi—K2—K1xix115.55 (10)
O3v—Mo2—K1i87.31 (13)K1xvii—K2—K1xix68.29 (2)
O3vi—Mo2—K1i132.75 (13)K1xviii—K2—K1xix111.71 (2)
O3vii—Mo2—K1i141.54 (13)O2xii—K2—K1xx64.45 (10)
K1—Mo2—K1i82.63 (5)O2xiii—K2—K1xx55.67 (11)
O5i—Mo2—K1iv114.34 (18)O2xiv—K2—K1xx124.33 (11)
O5iv—Mo2—K1iv49.47 (18)O2xv—K2—K1xx132.25 (10)
O5—Mo2—K1iv53.74 (18)O2viii—K2—K1xx115.55 (10)
O3v—Mo2—K1iv132.75 (13)O2xvi—K2—K1xx47.75 (10)
O3vi—Mo2—K1iv141.54 (13)K1xvii—K2—K1xx111.71 (2)
O3vii—Mo2—K1iv87.31 (13)K1xviii—K2—K1xx68.29 (2)
K1—Mo2—K1iv82.63 (5)K1xix—K2—K1xx68.29 (2)
K1i—Mo2—K1iv82.63 (5)O2xii—K2—K1iii115.55 (10)
O5i—Mo2—K1vi25.38 (17)O2xiii—K2—K1iii124.33 (11)
O5iv—Mo2—K1vi120.88 (18)O2xiv—K2—K1iii55.67 (11)
O5—Mo2—K1vi112.52 (18)O2xv—K2—K1iii47.75 (10)
O3v—Mo2—K1vi75.76 (13)O2viii—K2—K1iii64.45 (10)
O3vi—Mo2—K1vi64.98 (13)O2xvi—K2—K1iii132.25 (10)
O3vii—Mo2—K1vi132.93 (13)K1xvii—K2—K1iii68.29 (2)
K1—Mo2—K1vi65.97 (4)K1xviii—K2—K1iii111.71 (2)
K1i—Mo2—K1vi68.78 (5)K1xix—K2—K1iii111.71 (2)
K1iv—Mo2—K1vi139.31 (3)K1xx—K2—K1iii180.0
O5i—Mo2—K1v112.52 (19)O2xii—K2—K1xxi124.33 (11)
O5iv—Mo2—K1v25.38 (17)O2xiii—K2—K1xxi132.25 (10)
O5—Mo2—K1v120.88 (19)O2xiv—K2—K1xxi47.75 (10)
O3v—Mo2—K1v64.98 (13)O2xv—K2—K1xxi115.55 (10)
O3vi—Mo2—K1v132.93 (13)O2viii—K2—K1xxi55.67 (11)
O3vii—Mo2—K1v75.76 (13)O2xvi—K2—K1xxi64.45 (10)
K1—Mo2—K1v139.31 (3)K1xvii—K2—K1xxi111.71 (2)
K1i—Mo2—K1v65.97 (4)K1xviii—K2—K1xxi68.29 (2)
K1iv—Mo2—K1v68.78 (5)K1xix—K2—K1xxi180.00 (5)
K1vi—Mo2—K1v119.997 (1)K1xx—K2—K1xxi111.71 (2)
O5i—Mo2—K1vii120.88 (18)K1iii—K2—K1xxi68.29 (2)
O5iv—Mo2—K1vii112.52 (18)O4xxii—K3—O4iii117.20 (5)
O5—Mo2—K1vii25.38 (17)O4xxii—K3—O4iv180.0 (3)
O3v—Mo2—K1vii132.93 (13)O4iii—K3—O4iv62.80 (5)
O3vi—Mo2—K1vii75.76 (13)O4xxii—K3—O4xxiii62.80 (5)
O3vii—Mo2—K1vii64.98 (13)O4iii—K3—O4xxiii62.80 (5)
K1—Mo2—K1vii68.78 (5)O4iv—K3—O4xxiii117.20 (5)
K1i—Mo2—K1vii139.31 (3)O4xxii—K3—O4xxiv62.80 (5)
K1iv—Mo2—K1vii65.97 (4)O4iii—K3—O4xxiv180.0
K1vi—Mo2—K1vii119.997 (1)O4iv—K3—O4xxiv117.20 (5)
K1v—Mo2—K1vii119.997 (1)O4xxiii—K3—O4xxiv117.20 (5)
O1—Co1—O1i97.19 (17)O4xxii—K3—O4xxv117.20 (5)
O1—Co1—O1iv97.19 (17)O4iii—K3—O4xxv117.20 (5)
O1i—Co1—O1iv97.19 (17)O4iv—K3—O4xxv62.80 (5)
O1—Co1—O3iii88.61 (18)O4xxiii—K3—O4xxv180.000 (1)
O1i—Co1—O3iii162.44 (19)O4xxiv—K3—O4xxv62.80 (5)
O1iv—Co1—O3iii98.52 (18)O4xxii—K3—O2xxii56.60 (13)
O1—Co1—O3viii98.52 (17)O4iii—K3—O2xxii117.74 (13)
O1i—Co1—O3viii88.61 (18)O4iv—K3—O2xxii123.40 (13)
O1iv—Co1—O3viii162.44 (19)O4xxiii—K3—O2xxii62.91 (13)
O3iii—Co1—O3viii74.10 (19)O4xxiv—K3—O2xxii62.26 (13)
O1—Co1—O3ix162.44 (19)O4xxv—K3—O2xxii117.09 (13)
O1i—Co1—O3ix98.52 (18)O4xxii—K3—O2iv123.40 (13)
O1iv—Co1—O3ix88.61 (18)O4iii—K3—O2iv62.26 (13)
O3iii—Co1—O3ix74.10 (19)O4iv—K3—O2iv56.60 (13)
O3viii—Co1—O3ix74.10 (19)O4xxiii—K3—O2iv117.09 (13)
O1—Co1—K1i50.79 (14)O4xxiv—K3—O2iv117.74 (13)
O1i—Co1—K1i46.70 (13)O4xxv—K3—O2iv62.91 (13)
O1iv—Co1—K1i105.35 (14)O2xxii—K3—O2iv180.0
O3iii—Co1—K1i134.51 (13)O4xxii—K3—O2xxiii62.26 (13)
O3viii—Co1—K1i90.72 (12)O4iii—K3—O2xxiii62.91 (13)
O3ix—Co1—K1i143.12 (13)O4iv—K3—O2xxiii117.74 (13)
O1—Co1—K146.70 (13)O4xxiii—K3—O2xxiii56.60 (12)
O1i—Co1—K1105.35 (14)O4xxiv—K3—O2xxiii117.09 (13)
O1iv—Co1—K150.79 (14)O4xxv—K3—O2xxiii123.40 (12)
O3iii—Co1—K190.72 (12)O2xxii—K3—O2xxiii107.38 (12)
O3viii—Co1—K1143.12 (13)O2iv—K3—O2xxiii72.62 (12)
O3ix—Co1—K1134.51 (13)O4xxii—K3—O2iii117.09 (13)
K1i—Co1—K176.12 (5)O4iii—K3—O2iii56.60 (12)
O1—Co1—K1iv105.35 (14)O4iv—K3—O2iii62.91 (13)
O1i—Co1—K1iv50.79 (14)O4xxiii—K3—O2iii62.26 (13)
O1iv—Co1—K1iv46.70 (13)O4xxiv—K3—O2iii123.40 (12)
O3iii—Co1—K1iv143.12 (13)O4xxv—K3—O2iii117.74 (13)
O3viii—Co1—K1iv134.51 (13)O2xxii—K3—O2iii72.62 (12)
O3ix—Co1—K1iv90.72 (12)O2iv—K3—O2iii107.38 (12)
K1i—Co1—K1iv76.12 (5)O2xxiii—K3—O2iii107.38 (12)
K1—Co1—K1iv76.12 (5)O4xxii—K3—O2xxiv62.91 (13)
O5x—K1—O4iii97.29 (16)O4iii—K3—O2xxiv123.40 (12)
O5x—K1—O5126.42 (7)O4iv—K3—O2xxiv117.09 (13)
O4iii—K1—O5136.23 (16)O4xxiii—K3—O2xxiv117.74 (13)
O5x—K1—O194.37 (16)O4xxiv—K3—O2xxiv56.60 (12)
O4iii—K1—O176.27 (15)O4xxv—K3—O2xxiv62.26 (13)
O5—K1—O199.99 (16)O2xxii—K3—O2xxiv107.38 (12)
O5x—K1—O2iv135.49 (18)O2iv—K3—O2xxiv72.62 (12)
O4iii—K1—O2iv69.07 (15)O2xxiii—K3—O2xxiv72.62 (12)
O5—K1—O2iv76.70 (15)O2iii—K3—O2xxiv180.00 (15)
O1—K1—O2iv120.81 (14)O4xxii—K3—O2xxv117.74 (13)
O5x—K1—O5i81.06 (18)O4iii—K3—O2xxv117.09 (13)
O4iii—K1—O5i144.00 (16)O4iv—K3—O2xxv62.26 (13)
O5—K1—O5i58.2 (2)O4xxiii—K3—O2xxv123.40 (12)
O1—K1—O5i68.08 (15)O4xxiv—K3—O2xxv62.91 (13)
O2iv—K1—O5i134.73 (17)O4xxv—K3—O2xxv56.60 (12)
O5x—K1—O1iv158.28 (17)O2xxii—K3—O2xxv72.62 (12)
O4iii—K1—O1iv71.50 (14)O2iv—K3—O2xxv107.38 (12)
O5—K1—O1iv67.73 (15)O2xxiii—K3—O2xxv180.0
O1—K1—O1iv65.27 (19)O2iii—K3—O2xxv72.62 (12)
O2iv—K1—O1iv58.97 (13)O2xxiv—K3—O2xxv107.38 (12)
O5i—K1—O1iv97.05 (15)Mo1—O1—Co1141.1 (3)
O5x—K1—O2vi72.13 (15)Mo1—O1—K1112.2 (2)
O4iii—K1—O2vi128.09 (15)Co1—O1—K1100.80 (18)
O5—K1—O2vi71.78 (15)Mo1—O1—K1i92.53 (18)
O1—K1—O2vi152.54 (14)Co1—O1—K1i96.26 (18)
O2iv—K1—O2vi83.59 (16)K1—O1—K1i108.35 (16)
O5i—K1—O2vi85.93 (14)Mo1—O2—K2xxvi172.2 (3)
O1iv—K1—O2vi129.49 (14)Mo1—O2—K1i96.6 (2)
O5x—K1—Mo1iv155.27 (13)K2xxvi—O2—K1i85.77 (13)
O4iii—K1—Mo1iv60.85 (11)Mo1—O2—K1vi108.5 (2)
O5—K1—Mo1iv75.85 (11)K2xxvi—O2—K1vi78.83 (12)
O1—K1—Mo1iv91.43 (11)K1i—O2—K1vi90.04 (13)
O2iv—K1—Mo1iv29.69 (9)Mo1—O2—K3ii87.80 (18)
O5i—K1—Mo1iv123.24 (12)K2xxvi—O2—K3ii84.50 (13)
O1iv—K1—Mo1iv30.51 (9)K1i—O2—K3ii100.91 (16)
O2vi—K1—Mo1iv110.94 (10)K1vi—O2—K3ii159.32 (17)
O5x—K1—Mo2103.88 (13)Mo1—O3—Co1iii128.3 (2)
O4iii—K1—Mo2152.45 (13)Mo1—O3—Mo2vi138.7 (2)
O5—K1—Mo228.92 (11)Co1iii—O3—Mo2vi92.70 (18)
O1—K1—Mo284.65 (11)Mo1—O4—K1iii135.7 (3)
O2iv—K1—Mo2105.61 (12)Mo1—O4—K3ii103.6 (2)
O5i—K1—Mo229.35 (11)K1iii—O4—K3ii118.01 (18)
O1iv—K1—Mo282.59 (10)Mo2—O5—K1vii137.9 (3)
O2vi—K1—Mo275.98 (9)Mo2—O5—K1101.6 (2)
Mo1iv—K1—Mo2100.58 (5)K1vii—O5—K1107.7 (2)
O5x—K1—Co1125.96 (13)Mo2—O5—K1iv96.9 (2)
O4iii—K1—Co168.28 (11)K1vii—O5—K1iv98.94 (18)
O5—K1—Co185.26 (12)K1—O5—K1iv112.47 (18)
O5i—Mo2—K1—O5x40.0 (3)O3viii—Co1—K1—Mo2111.5 (2)
O5iv—Mo2—K1—O5x128.6 (3)O3ix—Co1—K1—Mo2116.43 (18)
O5—Mo2—K1—O5x144.8 (3)K1i—Co1—K1—Mo239.43 (5)
O3v—Mo2—K1—O5x7.9 (2)K1iv—Co1—K1—Mo239.43 (5)
O3vi—Mo2—K1—O5x49.64 (18)O1—Co1—K1—K2xi158.0 (2)
O3vii—Mo2—K1—O5x113.0 (2)O1i—Co1—K1—K2xi116.59 (15)
K1i—Mo2—K1—O5x84.09 (14)O1iv—Co1—K1—K2xi29.83 (17)
K1iv—Mo2—K1—O5x167.57 (13)O3iii—Co1—K1—K2xi70.60 (14)
K1vi—Mo2—K1—O5x14.09 (12)O3viii—Co1—K1—K2xi134.5 (2)
K1v—Mo2—K1—O5x122.81 (12)O3ix—Co1—K1—K2xi2.4 (2)
K1vii—Mo2—K1—O5x125.40 (13)K1i—Co1—K1—K2xi153.43 (7)
O5i—Mo2—K1—O4iii99.2 (3)K1iv—Co1—K1—K2xi74.58 (9)
O5iv—Mo2—K1—O4iii10.5 (3)O4—Mo1—O1—Co10.2 (5)
O5—Mo2—K1—O4iii76.0 (3)O2—Mo1—O1—Co1121.8 (4)
O3v—Mo2—K1—O4iii131.2 (3)O3—Mo1—O1—Co1118.5 (4)
O3vi—Mo2—K1—O4iii171.2 (3)K1i—Mo1—O1—Co1103.2 (4)
O3vii—Mo2—K1—O4iii107.8 (3)K3ii—Mo1—O1—Co152.5 (5)
K1i—Mo2—K1—O4iii55.1 (3)K1—Mo1—O1—Co1145.8 (6)
K1iv—Mo2—K1—O4iii28.4 (3)K1iii—Mo1—O1—Co127.3 (4)
K1vi—Mo2—K1—O4iii125.1 (3)O4—Mo1—O1—K1146.0 (2)
K1v—Mo2—K1—O4iii16.3 (3)O2—Mo1—O1—K192.4 (3)
K1vii—Mo2—K1—O4iii95.4 (3)O3—Mo1—O1—K127.2 (3)
O5i—Mo2—K1—O5175.2 (4)K1i—Mo1—O1—K1111.0 (2)
O5iv—Mo2—K1—O586.6 (2)K3ii—Mo1—O1—K1161.69 (9)
O3v—Mo2—K1—O5152.7 (3)K1iii—Mo1—O1—K1118.49 (16)
O3vi—Mo2—K1—O595.2 (3)O4—Mo1—O1—K1i103.0 (2)
O3vii—Mo2—K1—O531.8 (3)O2—Mo1—O1—K1i18.6 (2)
K1i—Mo2—K1—O5131.1 (2)O3—Mo1—O1—K1i138.24 (17)
K1iv—Mo2—K1—O547.6 (2)K3ii—Mo1—O1—K1i50.69 (18)
K1vi—Mo2—K1—O5158.9 (2)K1—Mo1—O1—K1i111.0 (2)
K1v—Mo2—K1—O592.4 (2)K1iii—Mo1—O1—K1i130.51 (9)
K1vii—Mo2—K1—O519.4 (2)O1i—Co1—O1—Mo1107.7 (5)
O5i—Mo2—K1—O153.2 (2)O1iv—Co1—O1—Mo1154.1 (5)
O5iv—Mo2—K1—O135.4 (2)O3iii—Co1—O1—Mo155.7 (4)
O5—Mo2—K1—O1122.0 (2)O3viii—Co1—O1—Mo118.0 (5)
O3v—Mo2—K1—O185.3 (2)O3ix—Co1—O1—Mo145.6 (8)
O3vi—Mo2—K1—O1142.83 (16)K1i—Co1—O1—Mo1101.9 (4)
O3vii—Mo2—K1—O1153.78 (19)K1—Co1—O1—Mo1148.0 (5)
K1i—Mo2—K1—O19.09 (10)K1iv—Co1—O1—Mo1158.9 (4)
K1iv—Mo2—K1—O174.38 (10)O1i—Co1—O1—K1104.4 (2)
K1vi—Mo2—K1—O179.10 (11)O1iv—Co1—O1—K16.1 (2)
K1v—Mo2—K1—O129.62 (13)O3iii—Co1—O1—K192.29 (18)
K1vii—Mo2—K1—O1141.41 (11)O3viii—Co1—O1—K1165.99 (16)
O5i—Mo2—K1—O2iv173.7 (2)O3ix—Co1—O1—K1102.4 (6)
O5iv—Mo2—K1—O2iv85.1 (2)K1i—Co1—O1—K1110.1 (2)
O5—Mo2—K1—O2iv1.5 (2)K1iv—Co1—O1—K153.10 (16)
O3v—Mo2—K1—O2iv154.2 (2)O1i—Co1—O1—K1i5.7 (2)
O3vi—Mo2—K1—O2iv96.65 (16)O1iv—Co1—O1—K1i104.0 (2)
O3vii—Mo2—K1—O2iv33.3 (2)O3iii—Co1—O1—K1i157.62 (16)
K1i—Mo2—K1—O2iv129.62 (10)O3viii—Co1—O1—K1i83.92 (17)
K1iv—Mo2—K1—O2iv46.15 (11)O3ix—Co1—O1—K1i147.5 (5)
K1vi—Mo2—K1—O2iv160.37 (13)K1—Co1—O1—K1i110.1 (2)
K1v—Mo2—K1—O2iv90.90 (13)K1iv—Co1—O1—K1i56.98 (13)
K1vii—Mo2—K1—O2iv20.88 (10)O5x—K1—O1—Mo18.5 (3)
O5iv—Mo2—K1—O5i88.6 (2)O4iii—K1—O1—Mo187.9 (2)
O5—Mo2—K1—O5i175.2 (4)O5—K1—O1—Mo1136.7 (2)
O3v—Mo2—K1—O5i32.1 (3)O2iv—K1—O1—Mo1142.9 (2)
O3vi—Mo2—K1—O5i89.6 (2)O5i—K1—O1—Mo187.1 (2)
O3vii—Mo2—K1—O5i153.0 (3)O1iv—K1—O1—Mo1163.6 (2)
K1i—Mo2—K1—O5i44.1 (2)O2vi—K1—O1—Mo167.2 (4)
K1iv—Mo2—K1—O5i127.6 (2)Mo1iv—K1—O1—Mo1147.4 (2)
K1vi—Mo2—K1—O5i25.9 (2)Mo2—K1—O1—Mo1112.1 (2)
K1v—Mo2—K1—O5i82.8 (2)Co1—K1—O1—Mo1158.9 (4)
K1vii—Mo2—K1—O5i165.4 (2)K2xi—K1—O1—Mo1101.6 (4)
O5i—Mo2—K1—O1iv118.9 (2)O5x—K1—O1—Co1167.46 (19)
O5iv—Mo2—K1—O1iv30.3 (2)O4iii—K1—O1—Co171.01 (19)
O5—Mo2—K1—O1iv56.3 (2)O5—K1—O1—Co164.4 (2)
O3v—Mo2—K1—O1iv151.0 (2)O2iv—K1—O1—Co116.0 (3)
O3vi—Mo2—K1—O1iv151.47 (16)O5i—K1—O1—Co1114.0 (2)
O3vii—Mo2—K1—O1iv88.1 (2)O1iv—K1—O1—Co14.69 (17)
K1i—Mo2—K1—O1iv74.80 (9)O2vi—K1—O1—Co1133.9 (3)
K1iv—Mo2—K1—O1iv8.68 (10)Mo1iv—K1—O1—Co111.51 (16)
K1vi—Mo2—K1—O1iv144.81 (12)Mo2—K1—O1—Co188.98 (16)
K1v—Mo2—K1—O1iv36.08 (13)K2xi—K1—O1—Co157.3 (5)
K1vii—Mo2—K1—O1iv75.70 (10)O5x—K1—O1—K1i92.16 (18)
O5i—Mo2—K1—O2vi107.2 (2)O4iii—K1—O1—K1i171.39 (19)
O5iv—Mo2—K1—O2vi164.2 (2)O5—K1—O1—K1i36.02 (19)
O5—Mo2—K1—O2vi77.6 (2)O2iv—K1—O1—K1i116.41 (18)
O3v—Mo2—K1—O2vi75.1 (2)O5i—K1—O1—K1i13.62 (15)
O3vi—Mo2—K1—O2vi17.56 (15)O1iv—K1—O1—K1i95.70 (15)
O3vii—Mo2—K1—O2vi45.83 (19)O2vi—K1—O1—K1i33.5 (4)
K1i—Mo2—K1—O2vi151.29 (10)Mo1iv—K1—O1—K1i111.90 (13)
K1iv—Mo2—K1—O2vi125.24 (10)Mo2—K1—O1—K1i11.41 (13)
K1vi—Mo2—K1—O2vi81.28 (10)Co1—K1—O1—K1i100.4 (2)
K1v—Mo2—K1—O2vi169.99 (10)K2xi—K1—O1—K1i157.7 (3)
K1vii—Mo2—K1—O2vi58.21 (9)O4—Mo1—O2—K1i100.3 (2)
O5i—Mo2—K1—Mo1iv143.7 (2)O1—Mo1—O2—K1i19.3 (2)
O5iv—Mo2—K1—Mo1iv55.0 (2)O3—Mo1—O2—K1i139.28 (19)
O5—Mo2—K1—Mo1iv31.5 (2)K3ii—Mo1—O2—K1i100.74 (17)
O3v—Mo2—K1—Mo1iv175.7 (2)K1—Mo1—O2—K1i63.43 (16)
O3vi—Mo2—K1—Mo1iv126.71 (13)K1iii—Mo1—O2—K1i113.16 (18)
O3vii—Mo2—K1—Mo1iv63.32 (18)O4—Mo1—O2—K1vi167.5 (2)
K1i—Mo2—K1—Mo1iv99.56 (6)O1—Mo1—O2—K1vi72.9 (2)
K1iv—Mo2—K1—Mo1iv16.08 (5)O3—Mo1—O2—K1vi47.0 (2)
K1vi—Mo2—K1—Mo1iv169.56 (8)K1i—Mo1—O2—K1vi92.26 (19)
K1v—Mo2—K1—Mo1iv60.84 (9)K3ii—Mo1—O2—K1vi167.0 (2)
K1vii—Mo2—K1—Mo1iv50.95 (4)K1—Mo1—O2—K1vi28.83 (19)
O5i—Mo2—K1—Co185.9 (2)K1iii—Mo1—O2—K1vi154.58 (11)
O5iv—Mo2—K1—Co12.8 (2)O4—Mo1—O2—K3ii0.5 (2)
O5—Mo2—K1—Co189.4 (2)O1—Mo1—O2—K3ii120.06 (17)
O3v—Mo2—K1—Co1117.9 (2)O3—Mo1—O2—K3ii119.98 (18)
O3vi—Mo2—K1—Co1175.47 (13)K1i—Mo1—O2—K3ii100.74 (17)
O3vii—Mo2—K1—Co1121.14 (17)K1—Mo1—O2—K3ii164.17 (5)
K1i—Mo2—K1—Co141.74 (5)K1iii—Mo1—O2—K3ii12.4 (3)
K1iv—Mo2—K1—Co141.74 (5)O4—Mo1—O3—Co1iii16.5 (4)
K1vi—Mo2—K1—Co1111.74 (5)O2—Mo1—O3—Co1iii139.2 (3)
K1v—Mo2—K1—Co13.02 (8)O1—Mo1—O3—Co1iii102.4 (3)
K1vii—Mo2—K1—Co1108.76 (4)K1i—Mo1—O3—Co1iii164.53 (12)
O5i—Mo2—K1—K2xi137.5 (2)K3ii—Mo1—O3—Co1iii68.5 (3)
O5iv—Mo2—K1—K2xi133.9 (2)K1—Mo1—O3—Co1iii121.4 (3)
O5—Mo2—K1—K2xi47.3 (2)K1iii—Mo1—O3—Co1iii0.3 (3)
O3v—Mo2—K1—K2xi105.4 (2)O4—Mo1—O3—Mo2vi155.8 (4)
O3vi—Mo2—K1—K2xi47.87 (13)O2—Mo1—O3—Mo2vi33.2 (4)
O3vii—Mo2—K1—K2xi15.52 (18)O1—Mo1—O3—Mo2vi85.2 (4)
K1i—Mo2—K1—K2xi178.40 (5)K1i—Mo1—O3—Mo2vi23.1 (5)
K1iv—Mo2—K1—K2xi94.92 (7)K3ii—Mo1—O3—Mo2vi103.8 (4)
K1vi—Mo2—K1—K2xi111.60 (7)K1—Mo1—O3—Mo2vi66.3 (3)
K1v—Mo2—K1—K2xi139.68 (6)K1iii—Mo1—O3—Mo2vi172.7 (4)
K1vii—Mo2—K1—K2xi27.90 (3)O2—Mo1—O4—K1iii160.6 (3)
O1—Co1—K1—O5x15.5 (2)O1—Mo1—O4—K1iii80.5 (4)
O1i—Co1—K1—O5x100.9 (2)O3—Mo1—O4—K1iii39.3 (4)
O1iv—Co1—K1—O5x172.3 (2)K1i—Mo1—O4—K1iii141.4 (3)
O3iii—Co1—K1—O5x71.9 (2)K3ii—Mo1—O4—K1iii160.0 (5)
O3viii—Co1—K1—O5x8.0 (3)K1—Mo1—O4—K1iii44.5 (5)
O3ix—Co1—K1—O5x140.1 (2)O2—Mo1—O4—K3ii0.6 (3)
K1i—Co1—K1—O5x64.08 (17)O1—Mo1—O4—K3ii119.5 (2)
K1iv—Co1—K1—O5x142.92 (16)O3—Mo1—O4—K3ii120.7 (2)
O1—Co1—K1—O4iii98.6 (2)K1i—Mo1—O4—K3ii58.59 (19)
O1i—Co1—K1—O4iii176.00 (18)K1—Mo1—O4—K3ii155.49 (11)
O1iv—Co1—K1—O4iii89.2 (2)K1iii—Mo1—O4—K3ii160.0 (5)
O3iii—Co1—K1—O4iii11.19 (17)O5i—Mo2—O5—K1vii137.7 (5)
O3viii—Co1—K1—O4iii75.1 (2)O5iv—Mo2—O5—K1vii115.3 (5)
O3ix—Co1—K1—O4iii57.0 (2)O3v—Mo2—O5—K1vii4.1 (9)
K1i—Co1—K1—O4iii147.17 (13)O3vi—Mo2—O5—K1vii49.1 (4)
K1iv—Co1—K1—O4iii133.99 (13)O3vii—Mo2—O5—K1vii23.5 (4)
O1—Co1—K1—O5117.0 (2)K1—Mo2—O5—K1vii133.7 (5)
O1i—Co1—K1—O531.61 (18)K1i—Mo2—O5—K1vii171.2 (3)
O1iv—Co1—K1—O555.2 (2)K1iv—Mo2—O5—K1vii111.6 (5)
O3iii—Co1—K1—O5155.57 (17)K1vi—Mo2—O5—K1vii112.9 (4)
O3viii—Co1—K1—O5140.5 (2)K1v—Mo2—O5—K1vii95.7 (4)
O3ix—Co1—K1—O587.4 (2)O5i—Mo2—O5—K14.0 (3)
K1i—Co1—K1—O568.45 (11)O5iv—Mo2—O5—K1111.0 (2)
K1iv—Co1—K1—O510.40 (11)O3v—Mo2—O5—K1129.6 (5)
O1i—Co1—K1—O185.39 (15)O3vi—Mo2—O5—K184.6 (2)
O1iv—Co1—K1—O1172.2 (3)O3vii—Mo2—O5—K1157.2 (2)
O3iii—Co1—K1—O187.4 (2)K1i—Mo2—O5—K155.1 (2)
O3viii—Co1—K1—O123.5 (3)K1iv—Mo2—O5—K1114.7 (2)
O3ix—Co1—K1—O1155.6 (3)K1vi—Mo2—O5—K120.9 (2)
K1i—Co1—K1—O148.56 (19)K1v—Mo2—O5—K1130.62 (13)
K1iv—Co1—K1—O1127.40 (19)K1vii—Mo2—O5—K1133.7 (5)
O1—Co1—K1—O2iv166.3 (2)O5i—Mo2—O5—K1iv110.7 (2)
O1i—Co1—K1—O2iv108.33 (17)O5iv—Mo2—O5—K1iv3.7 (3)
O1iv—Co1—K1—O2iv21.56 (19)O3v—Mo2—O5—K1iv115.7 (5)
O3iii—Co1—K1—O2iv78.86 (17)O3vi—Mo2—O5—K1iv160.71 (17)
O3viii—Co1—K1—O2iv142.8 (2)O3vii—Mo2—O5—K1iv88.07 (18)
O3ix—Co1—K1—O2iv10.7 (2)K1—Mo2—O5—K1iv114.7 (2)
K1i—Co1—K1—O2iv145.16 (11)K1i—Mo2—O5—K1iv59.58 (19)
K1iv—Co1—K1—O2iv66.31 (12)K1vi—Mo2—O5—K1iv135.55 (10)
O1—Co1—K1—O5i58.5 (2)K1v—Mo2—O5—K1iv15.9 (2)
O1i—Co1—K1—O5i26.88 (17)K1vii—Mo2—O5—K1iv111.6 (5)
O1iv—Co1—K1—O5i113.6 (2)O5x—K1—O5—Mo244.0 (4)
O3iii—Co1—K1—O5i145.93 (16)O4iii—K1—O5—Mo2139.6 (2)
O3viii—Co1—K1—O5i82.0 (2)O1—K1—O5—Mo259.0 (2)
O3ix—Co1—K1—O5i145.9 (2)O2iv—K1—O5—Mo2178.5 (2)
K1i—Co1—K1—O5i9.96 (11)O5i—K1—O5—Mo22.8 (2)
K1iv—Co1—K1—O5i68.89 (10)O1iv—K1—O5—Mo2116.9 (2)
O1—Co1—K1—O1iv172.2 (3)O2vi—K1—O5—Mo293.9 (2)
O1i—Co1—K1—O1iv86.77 (15)Mo1iv—K1—O5—Mo2148.0 (2)
O3iii—Co1—K1—O1iv100.4 (2)Co1—K1—O5—Mo288.1 (2)
O3viii—Co1—K1—O1iv164.3 (3)K2xi—K1—O5—Mo2136.4 (2)
O3ix—Co1—K1—O1iv32.3 (2)O5x—K1—O5—K1vii105.4 (2)
K1i—Co1—K1—O1iv123.60 (17)O4iii—K1—O5—K1vii71.0 (3)
K1iv—Co1—K1—O1iv44.75 (17)O1—K1—O5—K1vii151.56 (18)
O1—Co1—K1—O2vi121.9 (3)O2iv—K1—O5—K1vii32.04 (17)
O1i—Co1—K1—O2vi36.5 (3)O5i—K1—O5—K1vii152.2 (2)
O1iv—Co1—K1—O2vi50.2 (3)O1iv—K1—O5—K1vii93.64 (19)
O3iii—Co1—K1—O2vi150.6 (3)O2vi—K1—O5—K1vii55.50 (16)
O3viii—Co1—K1—O2vi145.5 (3)Mo1iv—K1—O5—K1vii62.60 (15)
O3ix—Co1—K1—O2vi82.5 (3)Mo2—K1—O5—K1vii149.4 (3)
K1i—Co1—K1—O2vi73.4 (2)Co1—K1—O5—K1vii122.47 (16)
K1iv—Co1—K1—O2vi5.5 (2)K2xi—K1—O5—K1vii12.97 (16)
O1—Co1—K1—Mo1iv166.63 (19)O5x—K1—O5—K1iv146.6 (2)
O1i—Co1—K1—Mo1iv107.98 (14)O4iii—K1—O5—K1iv37.0 (3)
O1iv—Co1—K1—Mo1iv21.21 (16)O1—K1—O5—K1iv43.6 (2)
O3iii—Co1—K1—Mo1iv79.21 (13)O2iv—K1—O5—K1iv75.96 (19)
O3viii—Co1—K1—Mo1iv143.1 (2)O5i—K1—O5—K1iv99.83 (18)
O3ix—Co1—K1—Mo1iv11.04 (18)O1iv—K1—O5—K1iv14.36 (16)
K1i—Co1—K1—Mo1iv144.81 (4)O2vi—K1—O5—K1iv163.5 (2)
K1iv—Co1—K1—Mo1iv65.97 (4)Mo1iv—K1—O5—K1iv45.39 (15)
O1—Co1—K1—Mo287.98 (19)Mo2—K1—O5—K1iv102.6 (3)
O1i—Co1—K1—Mo22.59 (14)Co1—K1—O5—K1iv14.48 (16)
O1iv—Co1—K1—Mo284.18 (17)K2xi—K1—O5—K1iv120.97 (17)
O3iii—Co1—K1—Mo2175.40 (13)
Symmetry codes: (i) y+1, xy, z; (ii) x+1, y, z; (iii) x+1, y, z+1; (iv) x+y+1, x+1, z; (v) y+1, x+y+1, z+2; (vi) x+1, y, z+2; (vii) xy, x, z+2; (viii) y+1, x+y+1, z+1; (ix) xy, x, z+1; (x) y, x+y, z+2; (xi) x1, y, z+1; (xii) y+1, xy1, z1; (xiii) x+2, y, z+1; (xiv) x, y, z1; (xv) xy, x1, z+1; (xvi) x+y+2, x+1, z1; (xvii) x+y+1, x, z1; (xviii) xy+1, x, z+1; (xix) y+1, x+y, z+1; (xx) x+1, y, z1; (xxi) y+1, xy, z1; (xxii) xy1, x1, z+1; (xxiii) y, xy1, z; (xxiv) x1, y, z; (xxv) y, x+y+1, z+1; (xxvi) x, y, z+1.
(II) hexapotassium cobalt pentamolybdate top
Crystal data top
K6CoMo5O19F(000) = 2012
Mr = 1077.23Dx = 3.523 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.0804 (6) ÅCell parameters from 6106 reflections
b = 10.3856 (4) Åθ = 3.3–30.3°
c = 24.2048 (11) ŵ = 5.11 mm1
β = 90.728 (5)°T = 298 K
V = 2031.10 (19) Å3Prism, blue
Z = 40.08 × 0.07 × 0.06 mm
Data collection top
Oxford Xcalibur with Sapphire CCD area detector
diffractometer
5522 independent reflections
Radiation source: fine-focus sealed tube4488 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
ω and ϕ scansθmax = 30.1°, θmin = 2.6°
Absorption correction: numerical
[CrysAlis RED (Oxford Diffraction, 2003); analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid (Reference?).
h = 1011
Tmin = 0.640, Tmax = 0.772k = 1414
27463 measured reflectionsl = 3232
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)] = 0.044 w = 1/[σ2(Fo2) + (0.0257P)2 + 23.4209P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.114(Δ/σ)max < 0.001
S = 1.35Δρmax = 1.76 e Å3
5522 reflectionsΔρmin = 1.36 e Å3
281 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00024 (5)
Crystal data top
K6CoMo5O19V = 2031.10 (19) Å3
Mr = 1077.23Z = 4
Monoclinic, P21/nMo Kα radiation
a = 8.0804 (6) ŵ = 5.11 mm1
b = 10.3856 (4) ÅT = 298 K
c = 24.2048 (11) Å0.08 × 0.07 × 0.06 mm
β = 90.728 (5)°
Data collection top
Oxford Xcalibur with Sapphire CCD area detector
diffractometer
5522 independent reflections
Absorption correction: numerical
[CrysAlis RED (Oxford Diffraction, 2003); analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid (Reference?).
4488 reflections with I > 2σ(I)
Tmin = 0.640, Tmax = 0.772Rint = 0.042
27463 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.114 w = 1/[σ2(Fo2) + (0.0257P)2 + 23.4209P]
where P = (Fo2 + 2Fc2)/3
S = 1.35Δρmax = 1.76 e Å3
5522 reflectionsΔρmin = 1.36 e Å3
281 parameters
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*/Ueq
Mo10.33560 (9)0.41918 (6)0.17553 (3)0.01676 (16)
Mo20.35812 (8)0.40807 (6)0.06042 (3)0.01195 (14)
Mo30.70519 (9)0.09636 (6)0.18804 (3)0.01528 (15)
Mo40.37039 (8)0.07013 (6)0.06681 (3)0.01235 (14)
Mo50.14112 (8)0.25850 (6)0.05900 (3)0.01339 (15)
Co10.53059 (13)0.25021 (9)0.05966 (4)0.0121 (2)
K10.5151 (2)0.24526 (18)0.30639 (8)0.0243 (4)
K20.1978 (3)0.06480 (19)0.19656 (8)0.0282 (4)
K30.8639 (2)0.00366 (18)0.06670 (8)0.0225 (4)
K40.1413 (2)0.35491 (17)0.04668 (9)0.0245 (4)
K50.4913 (3)0.75918 (18)0.18770 (8)0.0261 (4)
K60.1386 (3)0.40468 (19)0.16073 (9)0.0306 (5)
O10.3421 (7)0.3196 (5)0.0041 (2)0.0160 (11)
O20.3465 (7)0.1467 (5)0.0016 (2)0.0168 (11)
O30.6609 (7)0.1789 (5)0.1247 (2)0.0181 (12)
O40.3458 (7)0.3293 (5)0.1109 (2)0.0159 (11)
O50.0463 (7)0.1703 (6)0.0057 (2)0.0210 (12)
O60.8534 (8)0.0235 (5)0.1772 (3)0.0234 (13)
O70.2023 (7)0.3627 (5)0.1070 (2)0.0215 (12)
O80.3419 (7)0.5766 (5)0.0501 (2)0.0195 (12)
O90.3407 (7)0.1020 (5)0.0617 (2)0.0181 (12)
O100.0469 (7)0.4077 (5)0.0533 (3)0.0230 (13)
O110.2223 (7)0.1301 (5)0.1130 (2)0.0210 (13)
O120.0536 (7)0.1946 (6)0.1186 (2)0.0226 (13)
O130.5658 (7)0.1005 (6)0.0942 (2)0.0214 (12)
O140.5266 (8)0.0308 (6)0.2173 (3)0.0309 (15)
O150.5487 (7)0.3756 (6)0.0888 (3)0.0232 (13)
O160.7845 (8)0.2123 (6)0.2346 (3)0.0277 (14)
O170.2701 (9)0.3165 (6)0.2292 (3)0.0303 (15)
O180.1940 (9)0.5456 (6)0.1716 (3)0.0346 (17)
O190.5268 (9)0.4815 (7)0.1948 (3)0.0374 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0248 (4)0.0142 (3)0.0112 (3)0.0021 (3)0.0002 (3)0.0024 (2)
Mo20.0148 (3)0.0111 (3)0.0099 (3)0.0011 (2)0.0010 (2)0.0010 (2)
Mo30.0195 (3)0.0136 (3)0.0127 (3)0.0015 (2)0.0014 (3)0.0010 (2)
Mo40.0156 (3)0.0106 (3)0.0108 (3)0.0000 (2)0.0005 (2)0.0003 (2)
Mo50.0134 (3)0.0133 (3)0.0134 (3)0.0009 (2)0.0002 (2)0.0006 (2)
Co10.0153 (5)0.0103 (4)0.0107 (5)0.0007 (4)0.0003 (4)0.0001 (4)
K10.0271 (10)0.0206 (8)0.0253 (10)0.0030 (7)0.0005 (8)0.0010 (7)
K20.0374 (11)0.0238 (9)0.0233 (10)0.0021 (8)0.0026 (9)0.0008 (7)
K30.0248 (9)0.0252 (9)0.0175 (9)0.0018 (7)0.0053 (7)0.0040 (7)
K40.0235 (9)0.0173 (8)0.0324 (11)0.0016 (7)0.0059 (8)0.0015 (7)
K50.0397 (12)0.0207 (9)0.0179 (9)0.0024 (8)0.0049 (8)0.0031 (7)
K60.0318 (11)0.0227 (9)0.0375 (12)0.0026 (8)0.0028 (9)0.0086 (8)
O10.015 (3)0.019 (3)0.014 (3)0.004 (2)0.001 (2)0.003 (2)
O20.021 (3)0.019 (3)0.011 (3)0.004 (2)0.001 (2)0.004 (2)
O30.023 (3)0.017 (3)0.014 (3)0.003 (2)0.006 (2)0.003 (2)
O40.018 (3)0.018 (3)0.011 (3)0.001 (2)0.000 (2)0.003 (2)
O50.020 (3)0.025 (3)0.018 (3)0.003 (2)0.001 (2)0.003 (2)
O60.029 (3)0.019 (3)0.022 (3)0.011 (2)0.003 (3)0.004 (2)
O70.025 (3)0.021 (3)0.018 (3)0.003 (2)0.010 (2)0.002 (2)
O80.021 (3)0.010 (2)0.028 (3)0.000 (2)0.001 (2)0.002 (2)
O90.019 (3)0.011 (2)0.024 (3)0.003 (2)0.003 (2)0.000 (2)
O100.024 (3)0.015 (3)0.030 (3)0.002 (2)0.003 (3)0.001 (2)
O110.025 (3)0.020 (3)0.018 (3)0.003 (2)0.010 (2)0.000 (2)
O120.022 (3)0.026 (3)0.019 (3)0.001 (2)0.005 (2)0.005 (2)
O130.022 (3)0.024 (3)0.018 (3)0.005 (2)0.006 (2)0.007 (2)
O140.027 (3)0.033 (3)0.033 (4)0.006 (3)0.011 (3)0.001 (3)
O150.017 (3)0.028 (3)0.025 (3)0.001 (2)0.007 (3)0.001 (3)
O160.040 (4)0.024 (3)0.019 (3)0.001 (3)0.008 (3)0.000 (3)
O170.045 (4)0.027 (3)0.019 (3)0.001 (3)0.005 (3)0.004 (3)
O180.045 (4)0.028 (3)0.031 (4)0.016 (3)0.015 (3)0.004 (3)
O190.042 (4)0.038 (4)0.033 (4)0.010 (3)0.010 (3)0.004 (3)
Geometric parameters (Å, º) top
Mo1—O191.734 (7)K3—O5vi2.574 (6)
Mo1—O181.744 (6)K3—O62.684 (7)
Mo1—O171.768 (6)K3—O132.701 (6)
Mo1—O41.825 (5)K3—O5vii2.769 (6)
Mo1—K2i3.459 (2)K3—O2vi2.827 (6)
Mo1—K53.759 (2)K3—O12vii2.849 (6)
Mo1—K63.847 (2)K3—O32.884 (6)
Mo1—K23.881 (2)K3—O11vii3.359 (6)
Mo1—K13.909 (2)K3—Mo5vii3.5320 (19)
Mo2—O151.728 (6)K3—Mo4vi3.803 (2)
Mo2—O71.743 (6)K4—O10viii2.586 (6)
Mo2—O81.773 (5)K4—O15vi2.701 (6)
Mo2—O11.818 (5)K4—O5v2.745 (6)
Mo2—K6ii3.565 (2)K4—O10v2.894 (7)
Mo2—K5iii3.753 (2)K4—O112.904 (6)
Mo2—K4iv3.996 (2)K4—O22.943 (6)
Mo2—K4v4.091 (2)K4—O8viii2.952 (6)
Mo2—K4vi4.092 (2)K4—O7v3.154 (6)
Mo3—O61.750 (6)K4—O18viii3.219 (7)
Mo3—O141.753 (6)K4—Mo5v3.550 (2)
Mo3—O161.765 (6)K4—Co1vi3.875 (2)
Mo3—O31.788 (5)K5—O16x2.639 (7)
Mo3—K33.3833 (19)K5—O13iv2.766 (6)
Mo3—K6vii3.508 (2)K5—O15iii2.788 (7)
Mo3—K13.615 (2)K5—O192.903 (7)
Mo3—K5viii3.905 (2)K5—O14iv2.924 (7)
Mo3—K2vii3.997 (2)K5—O17i2.994 (7)
Mo3—K24.121 (2)K5—O11iv3.035 (7)
Mo4—O131.733 (6)K5—O183.289 (8)
Mo4—O111.762 (5)K5—O7iii3.417 (7)
Mo4—O21.776 (5)K5—Mo4iv3.548 (2)
Mo4—O91.808 (5)K5—Mo2iii3.753 (2)
Mo4—K43.5199 (19)K6—O16ix2.758 (7)
Mo4—K5viii3.548 (2)K6—O7ii2.789 (6)
Mo4—K23.726 (2)K6—O122.873 (6)
Mo4—K3vi3.803 (2)K6—O19ix2.946 (8)
Mo4—K34.047 (2)K6—O3ix2.974 (6)
Mo5—O101.731 (6)K6—O103.018 (7)
Mo5—O121.746 (6)K6—O183.069 (8)
Mo5—O51.751 (6)K6—O8ii3.130 (6)
Mo5—O42.191 (6)K6—O14i3.345 (8)
Mo5—O12.205 (5)K6—Mo3ix3.508 (2)
Mo5—O92.290 (5)K6—Mo2ii3.566 (2)
Mo5—K3ix3.5320 (19)O2—Co1vi2.092 (5)
Mo5—K4v3.550 (2)O2—K3vi2.827 (6)
Mo5—K63.690 (2)O3—K6vii2.974 (6)
Mo5—K23.912 (2)O5—K3vi2.574 (6)
Mo5—K4iv4.0260 (19)O5—K4v2.745 (6)
Mo5—K3vi4.0323 (19)O5—K3ix2.769 (6)
Co1—O32.024 (5)O6—K1xiii2.654 (6)
Co1—O8iii2.088 (5)O6—K2vii2.962 (7)
Co1—O2vi2.092 (5)O7—K6ii2.789 (6)
Co1—O42.118 (5)O7—K1xiv2.804 (6)
Co1—O12.144 (6)O7—K4v3.154 (6)
Co1—O92.174 (6)O7—K5iii3.417 (7)
Co1—K33.772 (2)O8—Co1iii2.088 (5)
Co1—K4vi3.875 (2)O8—K4iv2.952 (6)
Co1—K6vii3.942 (3)O8—K6ii3.130 (6)
K1—O6x2.654 (6)O10—K4iv2.586 (6)
K1—O18xi2.731 (6)O10—K4v2.894 (7)
K1—O172.804 (7)O11—K5viii3.035 (7)
K1—O7xii2.804 (6)O11—K1xi3.042 (6)
K1—O162.823 (7)O11—K3ix3.359 (6)
K1—O11i3.042 (6)O12—K3ix2.849 (6)
K1—O143.103 (7)O13—K5viii2.766 (6)
K1—K2i3.738 (3)O14—K5viii2.924 (7)
K1—K6xi3.758 (3)O14—K6xi3.345 (8)
K1—K4i3.929 (3)O15—K4vi2.701 (6)
K2—O122.584 (6)O15—K5iii2.788 (7)
K2—O142.721 (7)O16—K5xiii2.639 (7)
K2—O172.790 (7)O16—K6vii2.758 (7)
K2—O112.870 (6)O17—K5xi2.994 (7)
K2—O6ix2.962 (7)O17—K2i3.152 (7)
K2—O17xi3.152 (7)O18—K1i2.731 (6)
K2—O18xi3.304 (8)O18—K4iv3.219 (7)
K2—O19xi3.328 (8)O18—K2i3.304 (8)
K2—Mo1xi3.459 (2)O19—K6vii2.946 (8)
K2—K1xi3.738 (3)O19—K2i3.328 (8)
K2—K5xi3.791 (3)
O19—Mo1—O18108.4 (4)O5vi—K3—O5vii85.35 (19)
O19—Mo1—O17107.6 (3)O6—K3—O5vii127.2 (2)
O18—Mo1—O17107.0 (3)O13—K3—O5vii148.89 (19)
O19—Mo1—O4111.8 (3)O5vi—K3—O2vi98.40 (18)
O18—Mo1—O4112.0 (3)O6—K3—O2vi126.75 (17)
O17—Mo1—O4109.8 (3)O13—K3—O2vi79.51 (17)
O19—Mo1—K2i71.1 (3)O5vii—K3—O2vi69.39 (17)
O18—Mo1—K2i70.2 (2)O5vi—K3—O12vii129.16 (19)
O17—Mo1—K2i65.1 (2)O6—K3—O12vii68.88 (18)
O4—Mo1—K2i174.88 (17)O13—K3—O12vii129.55 (19)
O19—Mo1—K548.1 (2)O5vii—K3—O12vii58.47 (17)
O18—Mo1—K561.0 (3)O2vi—K3—O12vii100.06 (17)
O17—Mo1—K5127.8 (2)O5vi—K3—O3160.16 (19)
O4—Mo1—K5121.92 (17)O6—K3—O362.60 (16)
K2i—Mo1—K563.19 (5)O13—K3—O367.07 (18)
O19—Mo1—K6157.4 (3)O5vii—K3—O398.09 (17)
O18—Mo1—K651.1 (3)O2vi—K3—O365.16 (16)
O17—Mo1—K674.8 (2)O12vii—K3—O367.43 (17)
O4—Mo1—K687.47 (18)O5vi—K3—O11vii73.46 (17)
K2i—Mo1—K690.66 (5)O6—K3—O11vii71.07 (17)
K5—Mo1—K6112.09 (5)O13—K3—O11vii122.69 (17)
O19—Mo1—K2125.1 (2)O5vii—K3—O11vii88.32 (16)
O18—Mo1—K2122.2 (2)O2vi—K3—O11vii157.02 (16)
O17—Mo1—K240.7 (2)O12vii—K3—O11vii71.26 (16)
O4—Mo1—K269.13 (17)O3—K3—O11vii125.99 (16)
K2i—Mo1—K2105.75 (3)O5vi—K3—Mo3155.62 (15)
K5—Mo1—K2167.69 (5)O6—K3—Mo330.86 (12)
K6—Mo1—K271.82 (5)O13—K3—Mo363.36 (13)
O19—Mo1—K168.5 (2)O5vii—K3—Mo3118.21 (13)
O18—Mo1—K1128.9 (2)O2vi—K3—Mo396.09 (12)
O17—Mo1—K140.3 (2)O12vii—K3—Mo366.61 (12)
O4—Mo1—K1116.00 (17)O3—K3—Mo331.90 (11)
K2i—Mo1—K160.61 (5)O11vii—K3—Mo399.50 (11)
K5—Mo1—K1104.49 (4)O5vi—K3—Mo5vii107.33 (14)
K6—Mo1—K1114.60 (5)O6—K3—Mo5vii98.04 (15)
K2—Mo1—K163.87 (4)O13—K3—Mo5vii150.23 (14)
O15—Mo2—O7109.3 (3)O5vii—K3—Mo5vii29.19 (12)
O15—Mo2—O8108.5 (3)O2vi—K3—Mo5vii85.43 (12)
O7—Mo2—O8107.7 (3)O12vii—K3—Mo5vii29.35 (12)
O15—Mo2—O1108.5 (3)O3—K3—Mo5vii83.33 (12)
O7—Mo2—O1111.1 (3)O11vii—K3—Mo5vii76.96 (10)
O8—Mo2—O1111.8 (3)Mo3—K3—Mo5vii93.26 (5)
O15—Mo2—K6ii105.9 (2)O5vi—K3—Co1130.28 (15)
O7—Mo2—K6ii50.09 (19)O6—K3—Co193.84 (13)
O8—Mo2—K6ii61.4 (2)O13—K3—Co168.45 (13)
O1—Mo2—K6ii145.12 (18)O5vii—K3—Co184.52 (13)
O15—Mo2—K5iii44.2 (2)O2vi—K3—Co133.21 (11)
O7—Mo2—K5iii65.4 (2)O12vii—K3—Co183.95 (13)
O8—Mo2—K5iii126.7 (2)O3—K3—Co132.02 (11)
O1—Mo2—K5iii119.89 (18)O11vii—K3—Co1154.22 (12)
K6ii—Mo2—K5iii81.78 (5)Mo3—K3—Co163.01 (4)
O15—Mo2—K4iv141.2 (2)Mo5vii—K3—Co184.93 (4)
O7—Mo2—K4iv105.5 (2)O5vi—K3—Mo4vi72.45 (14)
O8—Mo2—K4iv42.81 (19)O6—K3—Mo4vi147.16 (15)
O1—Mo2—K4iv73.60 (18)O13—K3—Mo4vi81.26 (13)
K6ii—Mo2—K4iv83.53 (5)O5vii—K3—Mo4vi71.22 (13)
K5iii—Mo2—K4iv165.28 (4)O2vi—K3—Mo4vi26.17 (11)
O15—Mo2—K4v153.0 (2)O12vii—K3—Mo4vi119.24 (13)
O7—Mo2—K4v46.5 (2)O3—K3—Mo4vi90.07 (12)
O8—Mo2—K4v92.69 (19)O11vii—K3—Mo4vi141.29 (11)
O1—Mo2—K4v77.33 (17)Mo3—K3—Mo4vi119.05 (6)
K6ii—Mo2—K4v69.28 (4)Mo5vii—K3—Mo4vi96.26 (5)
K5iii—Mo2—K4v109.55 (5)Co1—K3—Mo4vi58.20 (3)
K4iv—Mo2—K4v65.75 (5)O10viii—K4—O15vi99.99 (19)
O15—Mo2—K4vi28.4 (2)O10viii—K4—O5v122.22 (19)
O7—Mo2—K4vi136.1 (2)O15vi—K4—O5v137.22 (19)
O8—Mo2—K4vi101.33 (19)O10viii—K4—O10v73.7 (2)
O1—Mo2—K4vi86.75 (17)O15vi—K4—O10v140.85 (19)
K6ii—Mo2—K4vi127.71 (5)O5v—K4—O10v57.65 (17)
K5iii—Mo2—K4vi70.96 (4)O10viii—K4—O11142.8 (2)
K4iv—Mo2—K4vi118.14 (3)O15vi—K4—O1169.73 (18)
K4v—Mo2—K4vi161.87 (5)O5v—K4—O1179.22 (18)
O6—Mo3—O14110.7 (3)O10v—K4—O11136.65 (18)
O6—Mo3—O16109.7 (3)O10viii—K4—O2153.03 (19)
O14—Mo3—O16107.5 (3)O15vi—K4—O270.99 (17)
O6—Mo3—O3110.0 (3)O5v—K4—O268.02 (17)
O14—Mo3—O3112.1 (3)O10v—K4—O296.97 (17)
O16—Mo3—O3106.7 (3)O11—K4—O259.35 (15)
O6—Mo3—K351.9 (2)O10viii—K4—O8viii89.12 (18)
O14—Mo3—K3123.7 (2)O15vi—K4—O8viii76.37 (18)
O16—Mo3—K3128.7 (2)O5v—K4—O8viii96.17 (17)
O3—Mo3—K358.47 (18)O10v—K4—O8viii65.10 (17)
O6—Mo3—K6vii111.9 (2)O11—K4—O8viii120.67 (16)
O14—Mo3—K6vii136.9 (2)O2—K4—O8viii64.22 (15)
O16—Mo3—K6vii50.9 (2)O10viii—K4—O7v71.63 (17)
O3—Mo3—K6vii57.95 (18)O15vi—K4—O7v129.86 (18)
K3—Mo3—K6vii88.59 (5)O5v—K4—O7v75.38 (17)
O6—Mo3—K1136.2 (2)O10v—K4—O7v85.74 (17)
O14—Mo3—K159.1 (2)O11—K4—O7v87.63 (16)
O16—Mo3—K149.9 (2)O2—K4—O7v133.95 (16)
O3—Mo3—K1113.06 (18)O8viii—K4—O7v148.90 (17)
K3—Mo3—K1171.43 (5)O10viii—K4—O18viii70.8 (2)
K6vii—Mo3—K185.20 (5)O15vi—K4—O18viii60.58 (19)
O6—Mo3—K5viii70.5 (2)O5v—K4—O18viii136.38 (18)
O14—Mo3—K5viii44.4 (2)O10v—K4—O18viii141.88 (19)
O16—Mo3—K5viii140.4 (2)O11—K4—O18viii73.28 (18)
O3—Mo3—K5viii110.14 (18)O2—K4—O18viii121.05 (18)
K3—Mo3—K5viii84.00 (5)O8viii—K4—O18viii126.90 (17)
K6vii—Mo3—K5viii168.09 (5)O7v—K4—O18viii70.35 (17)
K1—Mo3—K5viii101.12 (4)O10viii—K4—Mo4161.34 (15)
O6—Mo3—K2vii42.8 (2)O15vi—K4—Mo462.03 (13)
O14—Mo3—K2vii140.5 (2)O5v—K4—Mo476.30 (13)
O16—Mo3—K2vii70.7 (2)O10v—K4—Mo4123.00 (13)
O3—Mo3—K2vii105.77 (19)O11—K4—Mo429.92 (11)
K3—Mo3—K2vii68.36 (5)O2—K4—Mo430.26 (11)
K6vii—Mo3—K2vii73.98 (5)O8viii—K4—Mo491.10 (11)
K1—Mo3—K2vii115.29 (5)O7v—K4—Mo4114.98 (12)
K5viii—Mo3—K2vii111.53 (4)O18viii—K4—Mo494.39 (14)
O6—Mo3—K2129.4 (2)O10viii—K4—Mo5v97.25 (15)
O14—Mo3—K228.9 (2)O15vi—K4—Mo5v151.52 (15)
O16—Mo3—K2112.1 (2)O5v—K4—Mo5v28.84 (12)
O3—Mo3—K283.84 (19)O10v—K4—Mo5v28.94 (11)
K3—Mo3—K2114.05 (5)O11—K4—Mo5v108.06 (13)
K6vii—Mo3—K2116.27 (5)O2—K4—Mo5v83.43 (12)
K1—Mo3—K263.98 (4)O8viii—K4—Mo5v81.42 (12)
K5viii—Mo3—K259.22 (4)O7v—K4—Mo5v77.24 (11)
K2vii—Mo3—K2169.05 (6)O18viii—K4—Mo5v147.52 (14)
O13—Mo4—O11108.4 (3)Mo4—K4—Mo5v101.24 (5)
O13—Mo4—O2110.3 (3)O10viii—K4—Co1vi120.90 (15)
O11—Mo4—O2109.8 (3)O15vi—K4—Co1vi68.53 (13)
O13—Mo4—O9109.0 (3)O5v—K4—Co1vi82.85 (13)
O11—Mo4—O9107.6 (3)O10v—K4—Co1vi81.62 (13)
O2—Mo4—O9111.6 (3)O11—K4—Co1vi89.44 (12)
O13—Mo4—K4112.03 (19)O2—K4—Co1vi32.20 (10)
O11—Mo4—K455.30 (19)O8viii—K4—Co1vi32.15 (10)
O2—Mo4—K456.60 (18)O7v—K4—Co1vi158.20 (12)
O9—Mo4—K4138.78 (18)O18viii—K4—Co1vi129.10 (14)
O13—Mo4—K5viii49.77 (19)Mo4—K4—Co1vi59.53 (3)
O11—Mo4—K5viii58.8 (2)Mo5v—K4—Co1vi83.18 (5)
O2—Mo4—K5viii122.34 (18)O16x—K5—O13iv121.7 (2)
O9—Mo4—K5viii125.87 (19)O16x—K5—O15iii126.2 (2)
K4—Mo4—K5viii80.40 (5)O13iv—K5—O15iii65.53 (18)
O13—Mo4—K295.5 (2)O16x—K5—O1973.0 (2)
O11—Mo4—K248.19 (19)O13iv—K5—O19123.3 (2)
O2—Mo4—K2151.64 (19)O15iii—K5—O1964.0 (2)
O9—Mo4—K268.62 (18)O16x—K5—O14iv86.5 (2)
K4—Mo4—K2103.34 (5)O13iv—K5—O14iv70.76 (19)
K5viii—Mo4—K266.10 (5)O15iii—K5—O14iv134.8 (2)
O13—Mo4—K3vi143.4 (2)O19—K5—O14iv159.2 (2)
O11—Mo4—K3vi106.0 (2)O16x—K5—O17i92.4 (2)
O2—Mo4—K3vi44.57 (18)O13iv—K5—O17i127.43 (19)
O9—Mo4—K3vi71.20 (19)O15iii—K5—O17i126.94 (19)
K4—Mo4—K3vi78.25 (5)O19—K5—O17i103.2 (2)
K5viii—Mo4—K3vi158.52 (5)O14iv—K5—O17i73.22 (18)
K2—Mo4—K3vi116.92 (5)O16x—K5—O11iv166.85 (19)
O13—Mo4—K330.50 (19)O13iv—K5—O11iv58.29 (16)
O11—Mo4—K3137.5 (2)O15iii—K5—O11iv66.71 (17)
O2—Mo4—K399.90 (18)O19—K5—O11iv118.76 (19)
O9—Mo4—K387.78 (18)O14iv—K5—O11iv81.21 (18)
K4—Mo4—K3131.28 (4)O17i—K5—O11iv79.55 (18)
K5viii—Mo4—K379.90 (5)O16x—K5—O18116.98 (19)
K2—Mo4—K3108.41 (5)O13iv—K5—O18115.14 (18)
K3vi—Mo4—K3116.43 (3)O15iii—K5—O1858.89 (17)
O10—Mo5—O12102.9 (3)O19—K5—O1853.75 (19)
O10—Mo5—O5102.8 (3)O14iv—K5—O18138.46 (18)
O12—Mo5—O5103.4 (3)O17i—K5—O1872.12 (18)
O10—Mo5—O494.2 (2)O11iv—K5—O1870.65 (16)
O12—Mo5—O488.0 (2)O16x—K5—O7iii80.99 (18)
O5—Mo5—O4156.6 (2)O13iv—K5—O7iii63.91 (16)
O10—Mo5—O191.2 (2)O15iii—K5—O7iii53.13 (16)
O12—Mo5—O1156.5 (3)O19—K5—O7iii66.04 (18)
O5—Mo5—O191.4 (2)O14iv—K5—O7iii115.37 (17)
O4—Mo5—O172.1 (2)O17i—K5—O7iii168.56 (17)
O10—Mo5—O9161.2 (2)O11iv—K5—O7iii108.56 (15)
O12—Mo5—O990.0 (2)O18—K5—O7iii102.47 (15)
O5—Mo5—O987.2 (2)O16x—K5—Mo4iv149.20 (16)
O4—Mo5—O972.3 (2)O13iv—K5—Mo4iv28.59 (12)
O1—Mo5—O972.4 (2)O15iii—K5—Mo4iv60.99 (13)
O10—Mo5—K3ix114.6 (2)O19—K5—Mo4iv124.84 (16)
O12—Mo5—K3ix53.1 (2)O14iv—K5—Mo4iv75.22 (15)
O5—Mo5—K3ix50.47 (19)O17i—K5—Mo4iv105.38 (14)
O4—Mo5—K3ix134.68 (15)O11iv—K5—Mo4iv29.76 (10)
O1—Mo5—K3ix136.54 (15)O18—K5—Mo4iv92.65 (13)
O9—Mo5—K3ix84.16 (14)O7iii—K5—Mo4iv84.69 (11)
O10—Mo5—K4v54.0 (2)O16x—K5—Mo2iii105.83 (16)
O12—Mo5—K4v116.1 (2)O13iv—K5—Mo2iii59.71 (13)
O5—Mo5—K4v49.1 (2)O15iii—K5—Mo2iii25.60 (12)
O4—Mo5—K4v142.36 (14)O19—K5—Mo2iii63.64 (16)
O1—Mo5—K4v87.48 (15)O14iv—K5—Mo2iii128.03 (14)
O9—Mo5—K4v131.79 (15)O17i—K5—Mo2iii151.88 (15)
K3ix—Mo5—K4v81.56 (5)O11iv—K5—Mo2iii85.62 (11)
O10—Mo5—K654.0 (2)O18—K5—Mo2iii80.49 (12)
O12—Mo5—K649.2 (2)O7iii—K5—Mo2iii27.64 (10)
O5—Mo5—K6116.2 (2)Mo4iv—K5—Mo2iii69.08 (4)
O4—Mo5—K686.79 (14)O16x—K5—Mo196.24 (14)
O1—Mo5—K6138.25 (15)O13iv—K5—Mo1120.47 (14)
O9—Mo5—K6135.26 (15)O15iii—K5—Mo154.97 (13)
K3ix—Mo5—K683.55 (5)O19—K5—Mo126.38 (15)
K4v—Mo5—K688.35 (5)O14iv—K5—Mo1163.17 (14)
O10—Mo5—K2125.1 (2)O17i—K5—Mo190.05 (13)
O12—Mo5—K231.3 (2)O11iv—K5—Mo194.18 (12)
O5—Mo5—K2113.8 (2)O18—K5—Mo127.63 (11)
O4—Mo5—K266.77 (15)O7iii—K5—Mo181.45 (10)
O1—Mo5—K2125.59 (15)Mo4iv—K5—Mo1108.44 (5)
O9—Mo5—K262.37 (15)Mo2iii—K5—Mo167.21 (4)
K3ix—Mo5—K268.04 (5)O16ix—K6—O7ii152.7 (2)
K4v—Mo5—K2145.64 (5)O16ix—K6—O1278.88 (18)
K6—Mo5—K273.13 (5)O7ii—K6—O12126.14 (19)
O10—Mo5—K4iv26.1 (2)O16ix—K6—O19ix78.4 (2)
O12—Mo5—K4iv116.2 (2)O7ii—K6—O19ix74.4 (2)
O5—Mo5—K4iv117.9 (2)O12—K6—O19ix143.8 (2)
O4—Mo5—K4iv72.94 (14)O16ix—K6—O3ix59.51 (17)
O1—Mo5—K4iv70.59 (14)O7ii—K6—O3ix116.72 (17)
O9—Mo5—K4iv135.15 (14)O12—K6—O3ix65.92 (17)
K3ix—Mo5—K4iv140.67 (5)O19ix—K6—O3ix78.31 (18)
K4v—Mo5—K4iv70.50 (5)O16ix—K6—O10133.22 (19)
K6—Mo5—K4iv68.89 (4)O7ii—K6—O1071.32 (17)
K2—Mo5—K4iv125.15 (5)O12—K6—O1054.93 (16)
O10—Mo5—K3vi121.8 (2)O19ix—K6—O10134.9 (2)
O12—Mo5—K3vi111.9 (2)O3ix—K6—O1091.74 (17)
O5—Mo5—K3vi25.91 (19)O16ix—K6—O18119.6 (2)
O4—Mo5—K3vi130.77 (14)O7ii—K6—O1877.48 (18)
O1—Mo5—K3vi74.59 (15)O12—K6—O1885.18 (18)
O9—Mo5—K3vi63.62 (15)O19ix—K6—O18130.72 (19)
K3ix—Mo5—K3vi62.19 (5)O3ix—K6—O18150.97 (18)
K4v—Mo5—K3vi68.97 (4)O10—K6—O1867.98 (18)
K6—Mo5—K3vi140.63 (5)O16ix—K6—O8ii118.70 (18)
K2—Mo5—K3vi107.73 (4)O7ii—K6—O8ii56.98 (16)
K4iv—Mo5—K3vi126.78 (4)O12—K6—O8ii91.37 (17)
O3—Co1—O8iii98.6 (2)O19ix—K6—O8ii75.48 (18)
O3—Co1—O2vi96.7 (2)O3ix—K6—O8ii61.35 (15)
O8iii—Co1—O2vi97.1 (2)O10—K6—O8ii61.52 (16)
O3—Co1—O492.9 (2)O18—K6—O8ii119.56 (18)
O8iii—Co1—O494.8 (2)O16ix—K6—O14i76.80 (18)
O2vi—Co1—O4163.4 (2)O7ii—K6—O14i96.83 (18)
O3—Co1—O1165.9 (2)O12—K6—O14i117.99 (18)
O8iii—Co1—O189.3 (2)O19ix—K6—O14i83.43 (18)
O2vi—Co1—O193.9 (2)O3ix—K6—O14i135.05 (17)
O4—Co1—O174.7 (2)O10—K6—O14i128.67 (17)
O3—Co1—O994.8 (2)O18—K6—O14i60.69 (17)
O8iii—Co1—O9164.1 (2)O8ii—K6—O14i149.79 (16)
O2vi—Co1—O989.6 (2)O16ix—K6—Mo3ix29.77 (13)
O4—Co1—O976.0 (2)O7ii—K6—Mo3ix144.49 (14)
O1—Co1—O975.9 (2)O12—K6—Mo3ix64.59 (12)
O3—Co1—K349.06 (16)O19ix—K6—Mo3ix82.00 (15)
O8iii—Co1—K3104.73 (16)O3ix—K6—Mo3ix30.63 (11)
O2vi—Co1—K347.75 (15)O10—K6—Mo3ix110.83 (13)
O4—Co1—K3138.85 (15)O18—K6—Mo3ix137.40 (14)
O1—Co1—K3139.86 (16)O8ii—K6—Mo3ix91.83 (11)
O9—Co1—K390.46 (14)O14i—K6—Mo3ix106.57 (13)
O3—Co1—K4vi105.42 (17)O16ix—K6—Mo2ii136.28 (16)
O8iii—Co1—K4vi48.81 (16)O7ii—K6—Mo2ii28.66 (12)
O2vi—Co1—K4vi48.57 (16)O12—K6—Mo2ii116.05 (14)
O4—Co1—K4vi140.65 (15)O19ix—K6—Mo2ii65.97 (15)
O1—Co1—K4vi88.60 (15)O3ix—K6—Mo2ii88.07 (12)
O9—Co1—K4vi134.63 (16)O10—K6—Mo2ii69.87 (12)
K3—Co1—K4vi74.44 (4)O18—K6—Mo2ii103.06 (14)
O3—Co1—K6vii47.46 (16)O8ii—K6—Mo2ii29.81 (10)
O8iii—Co1—K6vii52.16 (17)O14i—K6—Mo2ii120.94 (13)
O2vi—Co1—K6vii108.93 (16)Mo3ix—K6—Mo2ii116.69 (6)
O4—Co1—K6vii87.51 (15)O16ix—K6—Mo5106.25 (15)
O1—Co1—K6vii136.34 (15)O7ii—K6—Mo598.97 (14)
O9—Co1—K6vii138.38 (16)O12—K6—Mo527.41 (12)
K3—Co1—K6vii77.18 (5)O19ix—K6—Mo5150.47 (16)
K4vi—Co1—K6vii80.43 (5)O3ix—K6—Mo579.40 (12)
O6x—K1—O18xi154.8 (2)O10—K6—Mo527.65 (11)
O6x—K1—O1798.0 (2)O18—K6—Mo573.17 (13)
O18xi—K1—O1784.1 (2)O8ii—K6—Mo576.93 (11)
O6x—K1—O7xii92.21 (19)O14i—K6—Mo5126.09 (13)
O18xi—K1—O7xii83.1 (2)Mo3ix—K6—Mo588.57 (5)
O17—K1—O7xii166.7 (2)Mo2ii—K6—Mo594.22 (5)
O6x—K1—O1683.77 (19)Mo2—O1—Co1130.6 (3)
O18xi—K1—O16120.8 (2)Mo2—O1—Mo5136.4 (3)
O17—K1—O1699.5 (2)Co1—O1—Mo592.7 (2)
O7xii—K1—O1689.92 (19)Mo4—O2—Co1vi144.4 (3)
O6x—K1—O11i76.90 (18)Mo4—O2—K3vi109.3 (2)
O18xi—K1—O11i78.55 (19)Co1vi—O2—K3vi99.0 (2)
O17—K1—O11i82.48 (18)Mo4—O2—K493.1 (2)
O7xii—K1—O11i91.68 (18)Co1vi—O2—K499.2 (2)
O16—K1—O11i160.65 (18)K3vi—O2—K4106.57 (19)
O6x—K1—O14137.58 (19)Mo3—O3—Co1159.9 (3)
O18xi—K1—O1467.33 (19)Mo3—O3—K389.6 (2)
O17—K1—O1475.73 (19)Co1—O3—K398.9 (2)
O7xii—K1—O14102.24 (19)Mo3—O3—K6vii91.4 (2)
O16—K1—O1456.98 (17)Co1—O3—K6vii102.4 (2)
O11i—K1—O14140.89 (18)K3—O3—K6vii110.49 (19)
O6x—K1—Mo3109.42 (15)Mo1—O4—Co1137.7 (3)
O18xi—K1—Mo395.72 (15)Mo1—O4—Mo5128.4 (3)
O17—K1—Mo383.61 (14)Co1—O4—Mo593.9 (2)
O7xii—K1—Mo3101.00 (13)Mo5—O5—K3vi136.8 (3)
O16—K1—Mo328.59 (13)Mo5—O5—K4v102.0 (2)
O11i—K1—Mo3165.42 (14)K3vi—O5—K4v108.3 (2)
O14—K1—Mo328.98 (12)Mo5—O5—K3ix100.3 (3)
O6x—K1—K2i51.89 (15)K3vi—O5—K3ix94.65 (19)
O18xi—K1—K2i113.09 (17)K4v—O5—K3ix114.1 (2)
O17—K1—K2i55.41 (14)Mo3—O6—K1xiii153.5 (3)
O7xii—K1—K2i127.81 (14)Mo3—O6—K397.2 (2)
O16—K1—K2i117.01 (14)K1xiii—O6—K3101.6 (2)
O11i—K1—K2i48.76 (11)Mo3—O6—K2vii113.5 (3)
O14—K1—K2i129.93 (15)K1xiii—O6—K2vii83.27 (17)
Mo3—K1—K2i124.38 (6)K3—O6—K2vii95.3 (2)
O6x—K1—K6xi135.65 (16)Mo2—O7—K6ii101.3 (2)
O18xi—K1—K6xi53.66 (17)Mo2—O7—K1xiv165.8 (3)
O17—K1—K6xi124.94 (15)K6ii—O7—K1xiv84.42 (17)
O7xii—K1—K6xi47.61 (12)Mo2—O7—K4v109.9 (3)
O16—K1—K6xi79.13 (14)K6ii—O7—K4v94.58 (18)
O11i—K1—K6xi115.64 (12)K1xiv—O7—K4v82.30 (16)
O14—K1—K6xi57.41 (14)Mo2—O7—K5iii87.0 (2)
Mo3—K1—K6xi69.56 (5)K6ii—O7—K5iii100.65 (18)
K2i—K1—K6xi163.87 (7)K1xiv—O7—K5iii79.16 (15)
O6x—K1—Mo181.21 (15)K4v—O7—K5iii154.6 (2)
O18xi—K1—Mo1106.54 (17)Mo2—O8—Co1iii142.9 (3)
O17—K1—Mo124.06 (14)Mo2—O8—K4iv113.1 (3)
O7xii—K1—Mo1169.05 (15)Co1iii—O8—K4iv99.0 (2)
O16—K1—Mo180.71 (13)Mo2—O8—K6ii88.8 (2)
O11i—K1—Mo195.30 (12)Co1iii—O8—K6ii96.1 (2)
O14—K1—Mo177.44 (14)K4iv—O8—K6ii112.10 (18)
Mo3—K1—Mo173.30 (4)Mo4—O9—Co1127.5 (3)
K2i—K1—Mo153.73 (4)Mo4—O9—Mo5142.8 (3)
K6xi—K1—Mo1134.53 (6)Co1—O9—Mo589.66 (19)
O6x—K1—K4i103.68 (15)Mo5—O10—K4iv136.8 (3)
O18xi—K1—K4i54.26 (15)Mo5—O10—K4v97.1 (2)
O17—K1—K4i116.12 (15)K4iv—O10—K4v106.3 (2)
O7xii—K1—K4i52.69 (13)Mo5—O10—K698.3 (3)
O16—K1—K4i141.63 (14)K4iv—O10—K6102.3 (2)
O11i—K1—K4i47.14 (11)K4v—O10—K6117.2 (2)
O14—K1—K4i116.87 (13)Mo4—O11—K2104.6 (2)
Mo3—K1—K4i138.47 (6)Mo4—O11—K494.8 (2)
K2i—K1—K4i95.69 (6)K2—O11—K4160.0 (2)
K6xi—K1—K4i69.31 (5)Mo4—O11—K5viii91.4 (2)
Mo1—K1—K4i137.34 (6)K2—O11—K5viii84.43 (17)
O12—K2—O14129.2 (2)K4—O11—K5viii100.34 (18)
O12—K2—O1779.0 (2)Mo4—O11—K1xi175.0 (3)
O14—K2—O1782.5 (2)K2—O11—K1xi78.38 (15)
O12—K2—O1183.57 (19)K4—O11—K1xi82.69 (15)
O14—K2—O1187.8 (2)K5viii—O11—K1xi84.81 (16)
O17—K2—O11147.60 (19)Mo4—O11—K3ix103.8 (2)
O12—K2—O6ix68.39 (18)K2—O11—K3ix83.83 (15)
O14—K2—O6ix154.49 (19)K4—O11—K3ix86.69 (16)
O17—K2—O6ix121.9 (2)K5viii—O11—K3ix162.7 (2)
O11—K2—O6ix75.12 (17)K1xi—O11—K3ix80.35 (14)
O12—K2—O17xi151.2 (2)Mo5—O12—K2128.2 (3)
O14—K2—O17xi73.5 (2)Mo5—O12—K3ix97.6 (3)
O17—K2—O17xi126.12 (8)K2—O12—K3ix100.4 (2)
O11—K2—O17xi79.54 (17)Mo5—O12—K6103.4 (3)
O6ix—K2—O17xi84.69 (18)K2—O12—K6112.2 (2)
O12—K2—O18xi148.0 (2)K3ix—O12—K6114.5 (2)
O14—K2—O18xi64.42 (19)Mo4—O13—K3130.5 (3)
O17—K2—O18xi74.38 (18)Mo4—O13—K5viii101.6 (3)
O11—K2—O18xi128.19 (18)K3—O13—K5viii127.0 (2)
O6ix—K2—O18xi111.79 (18)Mo3—O14—K2133.0 (4)
O17xi—K2—O18xi51.79 (17)Mo3—O14—K5viii110.7 (3)
O12—K2—O19xi117.83 (19)K2—O14—K5viii89.3 (2)
O14—K2—O19xi111.2 (2)Mo3—O14—K192.0 (3)
O17—K2—O19xi97.68 (19)K2—O14—K189.83 (19)
O11—K2—O19xi114.62 (18)K5viii—O14—K1149.2 (2)
O6ix—K2—O19xi61.58 (18)Mo3—O14—K6xi107.1 (3)
O17xi—K2—O19xi51.61 (17)K2—O14—K6xi117.8 (2)
O18xi—K2—O19xi50.33 (17)K5viii—O14—K6xi82.11 (17)
O12—K2—Mo1xi147.33 (15)K1—O14—K6xi71.19 (15)
O14—K2—Mo1xi82.27 (15)Mo2—O15—K4vi133.8 (3)
O17—K2—Mo1xi100.03 (14)Mo2—O15—K5iii110.2 (3)
O11—K2—Mo1xi109.22 (13)K4vi—O15—K5iii112.4 (2)
O6ix—K2—Mo1xi85.57 (13)Mo3—O16—K5xiii145.2 (3)
O17xi—K2—Mo1xi30.57 (12)Mo3—O16—K6vii99.4 (3)
O18xi—K2—Mo1xi29.77 (11)K5xiii—O16—K6vii99.8 (2)
O19xi—K2—Mo1xi29.52 (12)Mo3—O16—K1101.5 (3)
O12—K2—Mo475.58 (14)K5xiii—O16—K193.9 (2)
O14—K2—Mo474.43 (15)K6vii—O16—K1119.5 (2)
O17—K2—Mo4120.80 (15)Mo1—O17—K2114.8 (3)
O11—K2—Mo427.23 (11)Mo1—O17—K1115.7 (3)
O6ix—K2—Mo496.37 (13)K2—O17—K194.9 (2)
O17xi—K2—Mo498.25 (12)Mo1—O17—K5xi146.5 (3)
O18xi—K2—Mo4133.95 (14)K2—O17—K5xi81.80 (18)
O19xi—K2—Mo4141.43 (14)K1—O17—K5xi89.92 (18)
Mo1xi—K2—Mo4128.63 (6)Mo1—O17—K2i84.4 (2)
O12—K2—K1xi104.24 (15)K2—O17—K2i160.6 (2)
O14—K2—K1xi109.66 (15)K1—O17—K2i77.52 (17)
O17—K2—K1xi158.67 (16)K5xi—O17—K2i80.43 (16)
O11—K2—K1xi52.86 (12)Mo1—O18—K1i165.6 (4)
O6ix—K2—K1xi44.84 (11)Mo1—O18—K6102.6 (3)
O17xi—K2—K1xi47.08 (13)K1i—O18—K680.55 (19)
O18xi—K2—K1xi94.65 (12)Mo1—O18—K4iv111.8 (3)
O19xi—K2—K1xi61.90 (14)K1i—O18—K4iv82.22 (18)
Mo1xi—K2—K1xi65.66 (5)K6—O18—K4iv88.1 (2)
Mo4—K2—K1xi80.04 (5)Mo1—O18—K591.3 (3)
O12—K2—K5xi94.56 (15)K1i—O18—K585.28 (19)
O14—K2—K5xi109.56 (16)K6—O18—K5165.8 (2)
O17—K2—K5xi51.43 (14)K4iv—O18—K589.00 (17)
O11—K2—K5xi158.21 (14)Mo1—O18—K2i80.1 (3)
O6ix—K2—K5xi83.99 (13)K1i—O18—K2i85.58 (18)
O17xi—K2—K5xi92.62 (13)K6—O18—K2i109.4 (2)
O18xi—K2—K5xi54.73 (13)K4iv—O18—K2i156.7 (2)
O19xi—K2—K5xi47.59 (13)K5—O18—K2i70.19 (16)
Mo1xi—K2—K5xi62.26 (5)Mo1—O19—K5105.5 (3)
Mo4—K2—K5xi169.11 (7)Mo1—O19—K6vii129.9 (4)
K1xi—K2—K5xi107.29 (7)K5—O19—K6vii110.0 (2)
O5vi—K3—O6129.76 (19)Mo1—O19—K2i79.4 (3)
O5vi—K3—O13100.21 (19)K5—O19—K2i74.58 (18)
O6—K3—O1371.74 (19)K6vii—O19—K2i143.4 (3)
Symmetry codes: (i) x+1/2, y+1/2, z+1/2; (ii) x, y+1, z; (iii) x+1, y+1, z; (iv) x, y+1, z; (v) x, y, z; (vi) x+1, y, z; (vii) x+1, y, z; (viii) x, y1, z; (ix) x1, y, z; (x) x+3/2, y+1/2, z+1/2; (xi) x+1/2, y1/2, z+1/2; (xii) x+1/2, y+1/2, z+1/2; (xiii) x+3/2, y1/2, z+1/2; (xiv) x1/2, y+1/2, z1/2.

Experimental details

(I)(II)
Crystal data
Chemical formulaK4CoMo4O15K6CoMo5O19
Mr839.091077.23
Crystal system, space groupTrigonal, P3Monoclinic, P21/n
Temperature (K)298298
a, b, c (Å)10.292 (1), 10.292 (1), 8.1271 (8)8.0804 (6), 10.3856 (4), 24.2048 (11)
α, β, γ (°)90, 90, 12090, 90.728 (5), 90
V3)745.53 (13)2031.10 (19)
Z24
Radiation typeMo KαMo Kα
µ (mm1)5.555.11
Crystal size (mm)0.04 × 0.04 × 0.030.08 × 0.07 × 0.06
Data collection
DiffractometerOxford Xcalibur with Sapphire CCD area detector
diffractometer
Oxford Xcalibur with Sapphire CCD area detector
diffractometer
Absorption correctionNumerical
[CrysAlis RED (Oxford Diffraction Ltd, 2003); analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid (Reference?)].
Numerical
[CrysAlis RED (Oxford Diffraction, 2003); analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid (Reference?).
Tmin, Tmax0.771, 0.8350.640, 0.772
No. of measured, independent and
observed [I > 2σ(I)] reflections
3620, 1318, 1041 27463, 5522, 4488
Rint0.0470.042
(sin θ/λ)max1)0.7040.705
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.094, 1.09 0.044, 0.114, 1.35
No. of reflections13185522
No. of parameters75281
w = 1/[σ2(Fo2) + (0.0329P)2 + 3.9972P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0257P)2 + 23.4209P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.72, 1.091.76, 1.36

Computer programs: CrysAlis CCD (Oxford Diffraction, 2003), CrysAlis RED (Oxford Diffraction, 2003), CrysAlis RED, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2001), SHELXL97.

 

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