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The title compound, tetrakis­(ethyl­enedi­ammonium) tetra-[mu]-hydrogenphosphato-di-[mu]-hydro­xo- tetra-[mu]-phosphato-bis­(aqua­cobalt)­hexakis­(oxovanadium) trihydrate, was synthesized hydro­thermally at moderate temperature. The structure consists of diprotonated ethyl­enedi­ammonium cations and layers of the polyanions. The polyanion contains four PO4 tetrahedra and three VO5 square pyramids that are linked through corner-sharing by alternating P-O-V, which gives rise to a chain. The chains, connected by CoO4(H2O)2 octahedra, form layers, resulting in a two-dimensional layered structure. The Co-O distances are in the range 1.984 (3)-2.038 (4) Å, the P-O distances 1.508 (3)-1.575 (3) Å and the V-O distances 1.585 (3)-2.010 (3) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100007769/qa0314sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100007769/qa0314Isup2.hkl
Contains datablock I

CCDC reference: 147686

Comment top

Structures similar to the title compound that have been reported are as follows: [(VO)3(H2O)2(PO4)2(HPO4)]2− (Lu et al., 1998), [(VO)2(PO4)2]2−, [VO]3(HPO4)2(PO4)2]4− (Soghomonian et al., 1994), [V(OH)(PO4)2(H2)] (Soghomonian et al., 1998), [VO4(OH)4(PO4)2]2−, [(VO)5(OH)2(PO4)4]2−, [(VO)8(HPO4)3(PO4)4(OH)2]4−,[(VO)3(OH)2(PO4)2]2− (Soghomonian et al., 1995), [(VO)V(HPO4)3(H2O)2] (Haushalter et al., 1993), [V(H2O)2(VO)8(OH)4(HPO4)4(PO4)4(H2O)2]5− (Soghomonian et al., 1993) and [(VO)3(PO4)(HPO4)]2− (Brircsak et al., 1998). The polyanion structure of the title compound, (I), consists of {V3P4} basic units, which are built up from PO4 tetrahedra and VO5 square pyramids in a corner-sharing linkage mode, leading to a one-dimensional chain. The connection of P2—O8—V3—O20—P4—O9—V2—O1—P2 gives rise to an eight-membered ring in which P2 links P2—O2—V1—O4—P1 and V3 links V3—O3—P3; thus, an infinite one-dimensional chain is formed. The chains are connected by CoO4(H2O)2 octahedra resulting in the formation of layers of the polyanions. Connecting Co with P—V—O also produces two eight-membered rings, namely Co—O13—P4—O20—V3—O8—P2—O14—Co and Co—O13—P4—O9—V2—P2—O14—Co. The PO4 tetrahedra are slightly distorted, with P—O distances ranging from 1.057 to 1.575 Å and angles from 105.7 (2) to 113.3 (2)°. The VO5 square pyramids are also distorted, with V—O distances in the ring of 1.585 (3)–2.010 (3) Å and angles of 104.3 (2)–108.0 (2)°, in addition, the geometry within the CoO4(H2O)2 octahedra are as follows: Co—O13 2.038 (4) Å, Co—O14 1.984 (3) Å and Co—OW3 2.056 (5) Å; O14A—Co—O14, OW3A—Co—OW3 and O13—Co—O13A are all 180°, while the remaining angles are in the range 85.1 (2)–94.9 (2)°; therefore, the title compound exhibits a two-dimensional layered structure constructed from diprotonated ethylenediammonium cations, (H2en)2+, and the polyanion [Co(H2O)2(OH)2(VO)6(HPO4)4(PO4)4]8−, with the organic ammonium cations and water molecules intercalated between the layers.

Experimental top

The synthesis of the title compound was carried out by hydrothermal reaction of ethylenediamine, V2O5, H3PO4, CoCl2·6H2O and H2O (molar ratio 5:8:5:1:1000) in a 25 ml acid-digestion bomb at 413 K for 5 d. Blue crystals were isolated from solution after cooling to room temperature.

Computing details top

Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1995); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); software used to prepare material for publication: SHELXTL.

tetrakis(ethylenediammonium) tetra-µ-hydrogenphosphato-di-µ-hydroxo- tetra-µ-phosphato-bis(aquacobalt)hexakis(oxovanadium) trihydrate top
Crystal data top
(C2H10N2)4[Co(H2O)2(OH)2(VO)6(HPO4)4(PO4)4]·3H2OF(000) = 3220
Mr = 1596.94Dx = 2.213 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 20.709 (4) ÅCell parameters from 25 reflections
b = 9.968 (2) Åθ = 5.0–10.9°
c = 23.660 (5) ŵ = 1.86 mm1
β = 101.04 (3)°T = 293 K
V = 4793.7 (17) Å3Block, blue
Z = 40.50 × 0.40 × 0.38 mm
Data collection top
Siemens P4
diffractometer
3501 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.024
Graphite monochromatorθmax = 25.0°, θmin = 1.8°
2θ/ω scansh = 124
Absorption correction: empirical (using intensity measurements)
(North et al., 1968)
k = 111
Tmin = 0.359, Tmax = 0.494l = 2827
5341 measured reflections3 standard reflections every 97 reflections
4207 independent reflections intensity decay: none
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)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.137H-atom parameters constrained
S = 1.12Calculated w = 1/[σ2(Fo2) + (0.0913P)2]
where P = (Fo2 + 2Fc2)/3
4207 reflections(Δ/σ)max = 0.001
336 parametersΔρmax = 1.80 e Å3
0 restraintsΔρmin = 1.69 e Å3
Crystal data top
(C2H10N2)4[Co(H2O)2(OH)2(VO)6(HPO4)4(PO4)4]·3H2OV = 4793.7 (17) Å3
Mr = 1596.94Z = 4
Monoclinic, C2/cMo Kα radiation
a = 20.709 (4) ŵ = 1.86 mm1
b = 9.968 (2) ÅT = 293 K
c = 23.660 (5) Å0.50 × 0.40 × 0.38 mm
β = 101.04 (3)°
Data collection top
Siemens P4
diffractometer
3501 reflections with I > 2σ(I)
Absorption correction: empirical (using intensity measurements)
(North et al., 1968)
Rint = 0.024
Tmin = 0.359, Tmax = 0.4943 standard reflections every 97 reflections
5341 measured reflections intensity decay: none
4207 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0460 restraints
wR(F2) = 0.137H-atom parameters constrained
S = 1.12Δρmax = 1.80 e Å3
4207 reflectionsΔρmin = 1.69 e Å3
336 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 on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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
Co0.25000.25000.50000.0384 (3)
V10.22125 (3)0.09168 (7)0.27765 (3)0.0160 (2)
V20.17376 (4)0.40369 (7)0.32715 (3)0.0187 (2)
V30.06009 (4)0.07764 (7)0.43582 (3)0.0182 (2)
P10.28549 (5)0.37706 (10)0.32515 (4)0.0167 (3)
P20.18977 (5)0.11582 (11)0.37636 (5)0.0173 (3)
P30.05823 (5)0.18513 (11)0.49544 (5)0.0189 (3)
P40.10602 (6)0.37116 (11)0.43938 (5)0.0197 (3)
O10.15114 (15)0.2081 (3)0.32945 (13)0.0204 (6)
O20.2313 (2)0.0123 (3)0.35033 (12)0.0225 (7)
O30.01460 (15)0.1583 (3)0.49552 (13)0.0223 (7)
O40.2742 (2)0.2248 (3)0.32873 (13)0.0224 (7)
O50.2353 (2)0.5501 (3)0.35506 (13)0.0249 (7)
O60.3551 (2)0.4121 (3)0.35639 (13)0.0242 (7)
O70.2579 (2)0.1666 (3)0.21342 (13)0.0238 (7)
O80.14280 (15)0.0382 (3)0.40686 (13)0.0224 (7)
O90.1405 (2)0.4499 (3)0.39867 (14)0.0265 (7)
O100.0673 (2)0.2855 (3)0.54122 (14)0.0297 (8)
O110.1469 (2)0.1401 (4)0.26592 (15)0.0313 (8)
O120.2244 (2)0.0819 (3)0.23882 (13)0.0219 (7)
O130.1549 (2)0.3132 (4)0.49062 (15)0.0381 (9)
O140.2390 (2)0.2028 (4)0.41724 (13)0.0298 (8)
O150.09492 (15)0.0546 (3)0.49691 (13)0.0229 (7)
O160.1187 (2)0.4633 (3)0.2776 (2)0.0358 (8)
O170.0604 (2)0.4661 (3)0.4658 (2)0.0389 (9)
O180.0925 (2)0.2473 (3)0.43606 (13)0.0240 (7)
O190.0037 (2)0.0049 (3)0.39172 (14)0.0292 (7)
O200.0640 (2)0.2602 (3)0.40825 (13)0.0236 (7)
N10.36370 (10)0.0199 (2)0.41107 (8)0.0300 (9)
H1A0.37983 (10)0.0588 (2)0.42487 (8)0.045*
H1B0.35447 (10)0.0698 (2)0.43971 (8)0.045*
H1C0.32718 (10)0.0067 (2)0.38496 (8)0.045*
N20.38178 (10)0.3256 (2)0.40340 (8)0.0342 (10)
H2A0.36805 (10)0.4030 (2)0.38644 (8)0.051*
H2B0.35231 (10)0.2961 (2)0.42334 (8)0.051*
H2C0.42020 (10)0.3381 (2)0.42711 (8)0.051*
N30.06603 (10)0.1107 (2)0.22898 (8)0.0295 (9)
H3A0.08493 (10)0.1114 (2)0.19822 (8)0.044*
H3B0.09652 (10)0.1230 (2)0.26058 (8)0.044*
H3C0.04629 (10)0.0320 (2)0.23115 (8)0.044*
N40.19249 (10)0.2383 (2)0.42662 (8)0.0356 (10)
H4A0.19799 (10)0.2025 (2)0.39342 (8)0.053*
H4B0.18399 (10)0.3255 (2)0.42174 (8)0.053*
H4C0.15899 (10)0.1981 (2)0.43834 (8)0.053*
C10.4131 (3)0.0901 (5)0.3839 (3)0.0400 (13)
H1D0.4531 (3)0.1022 (5)0.4124 (3)0.060*
H1E0.4236 (3)0.0342 (5)0.3533 (3)0.060*
C20.3897 (3)0.2256 (5)0.3591 (2)0.0357 (12)
H2D0.3479 (3)0.2144 (5)0.3329 (2)0.054*
H2E0.4211 (3)0.2597 (5)0.3370 (2)0.054*
C30.0163 (2)0.2205 (5)0.2240 (2)0.0304 (11)
H3D0.0376 (2)0.3062 (5)0.2211 (2)0.046*
H3E0.0167 (2)0.2079 (5)0.1893 (2)0.046*
C40.2541 (3)0.2195 (7)0.4711 (2)0.0433 (14)
H4D0.2907 (3)0.2622 (7)0.4581 (2)0.065*
H4E0.2637 (3)0.1245 (7)0.4761 (2)0.065*
OW10.0471 (3)0.3095 (6)0.3347 (2)0.081 (2)
OW20.00000.1262 (5)0.25000.0420 (13)
OW30.2777 (2)0.4354 (5)0.4750 (2)0.0500 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0348 (6)0.0514 (7)0.0285 (5)0.0088 (5)0.0050 (4)0.0071 (5)
V10.0164 (4)0.0159 (4)0.0163 (4)0.0008 (3)0.0045 (3)0.0004 (3)
V20.0192 (4)0.0165 (4)0.0210 (4)0.0008 (3)0.0051 (3)0.0005 (3)
V30.0172 (4)0.0189 (4)0.0190 (4)0.0007 (3)0.0044 (3)0.0026 (3)
P10.0182 (6)0.0150 (5)0.0174 (5)0.0004 (4)0.0045 (4)0.0005 (4)
P20.0184 (5)0.0165 (5)0.0179 (5)0.0006 (4)0.0055 (4)0.0020 (4)
P30.0197 (6)0.0165 (5)0.0214 (6)0.0023 (4)0.0062 (4)0.0020 (4)
P40.0209 (6)0.0175 (5)0.0227 (6)0.0005 (4)0.0094 (5)0.0015 (4)
O10.0195 (15)0.0183 (15)0.024 (2)0.0005 (12)0.0069 (12)0.0016 (12)
O20.023 (2)0.024 (2)0.0193 (15)0.0068 (13)0.0033 (12)0.0022 (13)
O30.020 (2)0.024 (2)0.024 (2)0.0012 (13)0.0069 (13)0.0018 (13)
O40.029 (2)0.0169 (15)0.021 (2)0.0035 (13)0.0034 (13)0.0007 (12)
O50.027 (2)0.026 (2)0.024 (2)0.0089 (14)0.0112 (13)0.0048 (13)
O60.022 (2)0.024 (2)0.026 (2)0.0048 (13)0.0044 (13)0.0011 (13)
O70.029 (2)0.021 (2)0.023 (2)0.0038 (14)0.0118 (13)0.0005 (13)
O80.020 (2)0.0197 (15)0.029 (2)0.0034 (13)0.0081 (13)0.0050 (13)
O90.033 (2)0.0173 (15)0.034 (2)0.0047 (14)0.0183 (15)0.0022 (13)
O100.039 (2)0.024 (2)0.029 (2)0.005 (2)0.013 (2)0.0022 (14)
O110.023 (2)0.038 (2)0.034 (2)0.0046 (15)0.0079 (14)0.005 (2)
O120.031 (2)0.0171 (15)0.0184 (15)0.0027 (13)0.0061 (13)0.0009 (12)
O130.027 (2)0.062 (2)0.026 (2)0.009 (2)0.0077 (15)0.001 (2)
O140.028 (2)0.042 (2)0.020 (2)0.010 (2)0.0076 (14)0.0162 (14)
O150.021 (2)0.0217 (15)0.027 (2)0.0010 (13)0.0061 (13)0.0067 (13)
O160.035 (2)0.027 (2)0.041 (2)0.003 (2)0.006 (2)0.004 (2)
O170.049 (2)0.023 (2)0.056 (2)0.006 (2)0.038 (2)0.000 (2)
O180.026 (2)0.0187 (15)0.026 (2)0.0026 (13)0.0021 (13)0.0062 (13)
O190.029 (2)0.027 (2)0.029 (2)0.0049 (14)0.0023 (14)0.0001 (14)
O200.029 (2)0.020 (2)0.022 (2)0.0047 (13)0.0062 (13)0.0019 (13)
N10.031 (2)0.026 (2)0.030 (2)0.002 (2)0.001 (2)0.001 (2)
N20.036 (2)0.032 (2)0.035 (2)0.001 (2)0.008 (2)0.008 (2)
N30.022 (2)0.043 (2)0.025 (2)0.004 (2)0.008 (2)0.002 (2)
N40.035 (2)0.041 (2)0.032 (2)0.003 (2)0.009 (2)0.001 (2)
C10.035 (3)0.035 (3)0.051 (3)0.006 (2)0.014 (3)0.006 (2)
C20.039 (3)0.037 (3)0.032 (3)0.001 (2)0.011 (2)0.005 (2)
C30.029 (3)0.034 (3)0.026 (2)0.005 (2)0.001 (2)0.001 (2)
C40.040 (3)0.059 (4)0.031 (3)0.010 (3)0.006 (2)0.004 (3)
OW10.098 (4)0.085 (4)0.066 (3)0.035 (3)0.032 (3)0.021 (3)
OW20.029 (3)0.039 (3)0.058 (4)0.0000.008 (3)0.000
OW30.033 (2)0.068 (3)0.045 (2)0.008 (2)0.001 (2)0.022 (2)
Geometric parameters (Å, º) top
Co—O14i1.984 (3)P1—O5iv1.546 (3)
Co—O141.984 (3)P2—O81.528 (3)
Co—O132.038 (4)P2—O141.532 (3)
Co—O13i2.038 (4)P2—O11.542 (3)
Co—OW3i2.056 (5)P2—O21.544 (3)
Co—OW32.056 (5)P3—O101.513 (3)
V1—O111.586 (3)P3—O31.531 (3)
V1—O121.966 (3)P3—O15v1.535 (3)
V1—O71.971 (3)P3—O181.575 (3)
V1—O41.979 (3)P4—O201.508 (3)
V1—O21.985 (3)P4—O91.522 (3)
V2—O161.586 (3)P4—O131.536 (4)
V2—O51.966 (3)P4—O171.551 (3)
V2—O7ii1.983 (3)O5—P1vi1.546 (3)
V2—O91.999 (3)O7—V2iii1.983 (3)
V2—O12.009 (3)O12—P1ii1.543 (3)
V3—O191.585 (3)O15—P3v1.535 (3)
V3—O201.940 (3)N1—C11.483 (6)
V3—O151.987 (3)N2—C21.479 (6)
V3—O82.002 (3)N3—C31.492 (5)
V3—O32.010 (3)N4—C41.501 (6)
P1—O61.529 (3)C1—C21.515 (7)
P1—O41.541 (3)C3—C3vii1.515 (9)
P1—O12iii1.543 (3)C4—C4viii1.535 (10)
O14i—Co—O14180.0O15—V3—O384.72 (13)
O14i—Co—O1387.73 (14)O8—V3—O3150.00 (13)
O14—Co—O1392.27 (14)O6—P1—O4109.7 (2)
O14i—Co—O13i92.27 (14)O6—P1—O12iii110.4 (2)
O14—Co—O13i87.73 (14)O4—P1—O12iii108.8 (2)
O13—Co—O13i180.0O6—P1—O5iv109.0 (2)
O14i—Co—OW3i85.14 (15)O4—P1—O5iv108.4 (2)
O14—Co—OW3i94.86 (15)O12iii—P1—O5iv110.5 (2)
O13—Co—OW3i89.5 (2)O8—P2—O14113.3 (2)
O13i—Co—OW3i90.5 (2)O8—P2—O1110.6 (2)
O14i—Co—OW394.86 (15)O14—P2—O1107.9 (2)
O14—Co—OW385.14 (15)O8—P2—O2107.7 (2)
O13—Co—OW390.5 (2)O14—P2—O2106.0 (2)
O13i—Co—OW389.5 (2)O1—P2—O2111.3 (2)
OW3i—Co—OW3180.0O10—P3—O3111.9 (2)
O11—V1—O12107.7 (2)O10—P3—O15v110.1 (2)
O11—V1—O7104.7 (2)O3—P3—O15v111.2 (2)
O12—V1—O785.49 (13)O10—P3—O18106.4 (2)
O11—V1—O4108.0 (2)O3—P3—O18110.2 (2)
O12—V1—O4144.23 (14)O15v—P3—O18106.8 (2)
O7—V1—O488.07 (13)O20—P4—O9111.4 (2)
O11—V1—O2104.3 (2)O20—P4—O13109.9 (2)
O12—V1—O286.42 (12)O9—P4—O13112.0 (2)
O7—V1—O2150.92 (14)O20—P4—O17107.8 (2)
O4—V1—O282.37 (12)O9—P4—O17109.7 (2)
O16—V2—O5107.3 (2)O13—P4—O17105.7 (2)
O16—V2—O7ii104.7 (2)P2—O1—V2120.5 (2)
O5—V2—O7ii87.05 (13)P2—O2—V1136.1 (2)
O16—V2—O9102.9 (2)P3—O3—V3131.5 (2)
O5—V2—O981.41 (13)P1—O4—V1134.3 (2)
O7ii—V2—O9152.16 (14)P1vi—O5—V2130.1 (2)
O16—V2—O1104.2 (2)V1—O7—V2iii130.9 (2)
O5—V2—O1148.31 (14)P2—O8—V3136.6 (2)
O7ii—V2—O182.06 (12)P4—O9—V2134.1 (2)
O9—V2—O194.64 (12)P1ii—O12—V1133.0 (2)
O19—V3—O20106.3 (2)P4—O13—Co132.8 (2)
O19—V3—O15107.1 (2)P2—O14—Co134.0 (2)
O20—V3—O15146.51 (13)P3v—O15—V3122.0 (2)
O19—V3—O8104.8 (2)P4—O20—V3125.5 (2)
O20—V3—O888.57 (13)N1—C1—C2113.2 (4)
O15—V3—O884.47 (13)N2—C2—C1113.4 (4)
O19—V3—O3105.1 (2)N3—C3—C3vii110.1 (3)
O20—V3—O385.20 (13)N4—C4—C4viii110.6 (6)
Symmetry codes: (i) x+1/2, y1/2, z+1; (ii) x+1/2, y1/2, z+1/2; (iii) x+1/2, y+1/2, z+1/2; (iv) x, y+1, z; (v) x, y, z+1; (vi) x, y1, z; (vii) x, y, z+1/2; (viii) x+1/2, y+1/2, z+1.

Experimental details

Crystal data
Chemical formula(C2H10N2)4[Co(H2O)2(OH)2(VO)6(HPO4)4(PO4)4]·3H2O
Mr1596.94
Crystal system, space groupMonoclinic, C2/c
Temperature (K)293
a, b, c (Å)20.709 (4), 9.968 (2), 23.660 (5)
β (°) 101.04 (3)
V3)4793.7 (17)
Z4
Radiation typeMo Kα
µ (mm1)1.86
Crystal size (mm)0.50 × 0.40 × 0.38
Data collection
DiffractometerSiemens P4
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(North et al., 1968)
Tmin, Tmax0.359, 0.494
No. of measured, independent and
observed [I > 2σ(I)] reflections
5341, 4207, 3501
Rint0.024
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.137, 1.12
No. of reflections4207
No. of parameters336
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.80, 1.69

Computer programs: XSCANS (Siemens, 1994), XSCANS, SHELXTL (Siemens, 1995), SHELXS86 (Sheldrick, 1990), SHELXL93 (Sheldrick, 1993), SHELXTL.

Selected geometric parameters (Å, º) top
Co—O141.984 (3)V3—O82.002 (3)
Co—O132.038 (4)V3—O32.010 (3)
Co—OW32.056 (5)P1—O61.529 (3)
V1—O111.586 (3)P1—O41.541 (3)
V1—O121.966 (3)P2—O81.528 (3)
V1—O71.971 (3)P2—O141.532 (3)
V1—O41.979 (3)P2—O11.542 (3)
V1—O21.985 (3)P2—O21.544 (3)
V2—O161.586 (3)P3—O101.513 (3)
V2—O51.966 (3)P3—O31.531 (3)
V2—O91.999 (3)P3—O181.575 (3)
V2—O12.009 (3)P4—O201.508 (3)
V3—O191.585 (3)P4—O91.522 (3)
V3—O201.940 (3)P4—O131.536 (4)
V3—O151.987 (3)P4—O171.551 (3)
O14—Co—O1392.27 (14)O15—V3—O384.72 (13)
O14—Co—OW385.14 (15)O8—V3—O3150.00 (13)
O13—Co—OW390.5 (2)O6—P1—O4109.7 (2)
O11—V1—O12107.7 (2)O8—P2—O14113.3 (2)
O11—V1—O7104.7 (2)O8—P2—O1110.6 (2)
O12—V1—O785.49 (13)O14—P2—O1107.9 (2)
O11—V1—O4108.0 (2)O8—P2—O2107.7 (2)
O12—V1—O4144.23 (14)O14—P2—O2106.0 (2)
O7—V1—O488.07 (13)O1—P2—O2111.3 (2)
O11—V1—O2104.3 (2)O10—P3—O3111.9 (2)
O12—V1—O286.42 (12)O10—P3—O18106.4 (2)
O7—V1—O2150.92 (14)O3—P3—O18110.2 (2)
O4—V1—O282.37 (12)O20—P4—O9111.4 (2)
O16—V2—O5107.3 (2)O20—P4—O13109.9 (2)
O16—V2—O9102.9 (2)O9—P4—O13112.0 (2)
O5—V2—O981.41 (13)O20—P4—O17107.8 (2)
O16—V2—O1104.2 (2)O9—P4—O17109.7 (2)
O5—V2—O1148.31 (14)O13—P4—O17105.7 (2)
O9—V2—O194.64 (12)P2—O1—V2120.5 (2)
O19—V3—O20106.3 (2)P2—O2—V1136.1 (2)
O19—V3—O15107.1 (2)P3—O3—V3131.5 (2)
O20—V3—O15146.51 (13)P1—O4—V1134.3 (2)
O19—V3—O8104.8 (2)P2—O8—V3136.6 (2)
O20—V3—O888.57 (13)P4—O9—V2134.1 (2)
O15—V3—O884.47 (13)P4—O13—Co132.8 (2)
O19—V3—O3105.1 (2)P2—O14—Co134.0 (2)
O20—V3—O385.20 (13)P4—O20—V3125.5 (2)
 

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