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Acta Cryst. (2007). E63, m2245-m2246    [ doi:10.1107/S1600536807033119 ]

Bis(4,4'-bipyridinium) bis([mu]5-hydrogen phosphate)pentakis([mu]2-oxido)decaoxidopentamolybdate dihydrate

W.-H. Chen, Y. Xiang, Z.-F. Chen, Q.-M. Wu and Q.-X. Zeng

Abstract top

The title compound, (bipyH2)2[H2Mo5O23P2]·2H2O or (C10H10N2)2[Mo5O15(HPO4)2]·2H2O, contains the heteropolyanion [P2Mo5O21(OH)2]4-, two diprotonated 4,4'-bipyridine (bipy) molecules as cations and two water molecules. The heteropolyanion is built up from five MoO6 octahedra sharing four common edges and one common corner. The heteropolyanion has approximate noncrystallographic twofold rotation symmetry, the axis running through one Mo and one O atom. Five bridging O atoms between molybdenum centers connect the distorted MoO6 octahedra to form a ring system, with ten Mo-O distances having an average value of 1.923 (2) Å. Six O atoms of the PO3(OH) tetrahedra above and below the ring stabilize the polyanionic framework. The ten Mo-OP bond lengths differ markedly, between 2.219 (2) and 2.461 (2) Å. The ten short terminal Mo-O distances average 1.706 (2) Å. The P-O bond lengths range between 1.513 (2) and 1.567 (2) Å. The crystal packing exhibits a great number of N-H...O and O-H...O intermolecular classical hydrogen bonds, which link the cations, water molecules and polyanions to form a three-dimensional framework.

Comment top

Recently, many research activities have focused on the synthesis of open-framework metal phosphates with organic ligands because of their interesting structural chemistry and potential applications (Haushalter & Mundi, 1992; Lii et al., 1998; Wang et al., 1995). Many metal complexes containing polymolybdates have been synthesized and characterized (Luo et al., 2003; Wu et al., 2002). During our ongoing studies of related materials, we obtained the title compound (Fig.1). The unit cell contains two protonated 4,4'-bipyridine molecules, an (H2P2Mo5O23)4- anion and two water molecules. The heteropolyanion of (H2P2Mo5O23)4- is built up from five MoO6 octahedra (Fig. 2) sharing four common edges and one common corner, capped by two PO3(OH) tetrahedra. All the Mo atoms exhibit a 6+ oxidation state and possess distorted octahedral geometry. The Mo—O and P—O distances are in the range 1.693 (2)–2.461 (2) Å and 1.513 (2)–1.567 (2) Å. It is interesting to note that the protonated 4,4'-bipyridine cations and the water molecules play important roles for the crystal packing arrangement by linking (H2P2Mo5O23)4- anions via numerous N—H···O and O—H···O hydrogen-bonds. There are two types of protonated 4,4'-bipyridine molecules and two kinds of lattice-waters in the crystal packing. For example, O1W links two (H2P2Mo5O23)4- anions by three O—H···O(terminal oxygen) hydrogen bonds. However, O2W links two heteropolyanions via O—H···O(terminal oxygen) and O—H···O(double-bridging oxygen) hydrogen bonds. Similar to the lattice-water, the ligand 4,4-bpy with atoms N1 and N2 links two (H2P2Mo5O23)4- anions by N—H···O(terminal oxygen) and an N—H···O(double-bridging oxygen) hydrogen-bonds, and the other 4,4-bpy ligand with atoms N3 and N4 have two N—H···O(double- bridging oxygen) hydrogen bonds and an N—H···O(terminal oxygen) hydrogen bond. The crystal packing exhibits a great number of N—H···O and O—H···O intra- and intermolecular classic hydrogen bonds, which link the cations, water molecules and the polyanions to form a three-dimensional framework (Fig. 3). The most important geometric parameters of the title compound are listed for one example Mo-complex in Table 1. The classic hydrogen bonding interactions are given in Table 2. Ten weak intermolecular C—H···O hydrogen bonding contacts are not considered for clarity.

Related literature top

For related literature see: Haushalter & Mundi (1992); Lii et al., (1998); Wang et al., (1995); Wu et al. (2002).

For related literature, see: Luo et al. (2003).

Experimental top

All reagents were used as purchased without further purification. The synthesis was carried out in a rational way from a mixture of H2MoO4 (2 mmol 0.324 g). 4,4'-bipyridine(4 mmol 0.674 g), H3PO4(0.2 mmol 85wt%) and H2O(12 mmol). The mixture was loaded in a Teflon-lined autoclave (23 ml capacity) and was heated at 443k for 5 d under autogenous pressure. The solid product was collected by filtration, washed with water and dried at room temperature. Colorless crystals of the title compound were isolated.

Refinement top

The structure was solved by direct methods and refined on F2 using the SHELXTL97 software package. The hydrogen atoms that are bonded to water oxygen, nitrogen and carbon atoms were placed geometrically, with O—H, N—H and C—H distances of 0.98 Å for water, 0.88 Å for N atoms and 0.95 Å for C atoms of the pyridinium moieties, and Uiso(H) = 1.2Ueq for (O), (N) and (C) atoms, respectively. The H atoms of O1W and O2W were located in a difference Fourier map and refined with O—H distances approximately equal to 0.98 Å. Atoms H5B and H5C of O1W were treated as disordered and their site occupation set 1/2 due to similar electron density peaks. Finally, the coordinates of H5A, H5B, and H5C of O1W were fixed to stabilize the refinement. The hydroxyl H atoms of the phosphate groups were from difference Fourier maps, they were finally refined with isotropic displacement parameters, using a rotation mode with the HFIX 147 instruction of SHELXL97, with O—H distances 0.84 Å and Uiso(H21, H22) = 1.5Ueq for O4 and O7, respectively. More details and interpretation of the hydrogen bonding situation are given in the _exptl_special_details. All non-hydrogen atoms were refined with anisotropic thermal parameters.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1999); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. : The molecular structure of the title compound, with atom labels and with displacement ellipsoids drawn at the 50% probability level, for non-H atoms.
[Figure 2] Fig. 2. : The polyanion of the title compound, viewed approximately upon the five-membered Mo skeleton to show the non-crystallographic twofold axis symmetry, the axis running through Mo4 and O11.
[Figure 3] Fig. 3. : A packing diagram of the title compound, viewed along the a axis. Dashed lines indicate hydrogen bonds of the type N—H···O and O—H···O.
bis(4,4'-bipyridinium) bis(µ5-hydrogen phosphate)pentakis(µ2-oxido)decaoxidopentamolybdate dihydrate top
Crystal data top
(C10H10N2)2[Mo5O15(HPO4)2]·2H2OF(000) = 4912
Mr = 1264.09Dx = 2.462 Mg m−3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 58657 reflections
a = 11.823 (2) Åθ = 3.1–27.5°
b = 18.307 (4) ŵ = 1.99 mm−1
c = 31.517 (6) ÅT = 170 K
V = 6821 (2) Å3Needle, colorless
Z = 80.62 × 0.10 × 0.06 mm
Data collection top
Rigaku R-AXIS SPIDER
diffractometer		6885 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.032
graphiteθmax = 27.5°, θmin = 3.1°
ω oscillation scansh = −15→13
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		k = −23→23
Tmin = 0.788, Tmax = 0.888l = −40→40
58657 measured reflections2 standard reflections every 150 reflections
7810 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)] = 0.020Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.052H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0232P)2 + 8.9692P]
where P = (Fo2 + 2Fc2)/3
7810 reflections(Δ/σ)max = 0.001
507 parametersΔρmax = 0.55 e Å−3
0 restraintsΔρmin = −0.53 e Å−3
Crystal data top
(C10H10N2)2[Mo5O15(HPO4)2]·2H2OV = 6821 (2) Å3
Mr = 1264.09Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 11.823 (2) ŵ = 1.99 mm−1
b = 18.307 (4) ÅT = 170 K
c = 31.517 (6) Å0.62 × 0.10 × 0.06 mm
Data collection top
Rigaku R-AXIS SPIDER
diffractometer		6885 reflections with I > 2σ(I)
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		Rint = 0.032
Tmin = 0.788, Tmax = 0.888θmax = 27.5°
58657 measured reflections2 standard reflections every 150 reflections
7810 independent reflections intensity decay: none
Refinement top
R[F2 > 2σ(F2)] = 0.020H-atom parameters constrained
wR(F2) = 0.052Δρmax = 0.55 e Å−3
S = 1.04Δρmin = −0.53 e Å−3
7810 reflectionsAbsolute structure: ?
507 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Special details top

Experimental. Due to short H···H contacts detected with PLATON, atoms H4, H5B and H22 were omitted in a test-refinement and could be located at approximate positions as before. Additionally, a third H-atom at O1W could be found. Atom H22 at O7 of the second HPO4 moiety could be rotated away from a short H5B···H22 contact of 1.52 Å by using the BUMP instruction of SHELXL97. But then H22 lost its good donor property for the hydrogen bonding contact O7—H22···O1W. Atom H5B is a bifurcated donor for the contacts O1W—H5B···O7 and O1W—H5B···N4. The third H-atom H5C is a donor for the contact O1W—H5C···O23. It is thinkable that there is a kind of flip-flop disorder of H-atoms between H5b, H22 and also H4 of the bipyridine. We decided to reduce the problem by leaving atoms H5B and H5C at their observed positions with site occupation 1/2 each. The possibility of H-atom migration and tautomeric situations can lead to the observed H···H collisions in the measured subcell. The structure can be seen as a superstructure with different hydrogen bonds in adjacent subcells or as a statistical distribution of alternately protonated (O1W) and deprotonated (N4, O7) atoms. Some weak C—H···O hydrogen bonding contacts with Hbipy as donor molecules and terminal oxygen atoms of the polyanion as acceptors were also observed with PLATON. The classic hydrogen bonds including alternative bonds with H5B and H5C as donors are shown in the Table of hydrogen bonding geometry.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.673842 (17)0.395894 (11)0.164003 (6)0.01949 (5)
Mo20.222060 (17)0.435677 (11)0.110922 (6)0.01973 (5)
Mo30.300879 (18)0.259156 (12)0.092842 (7)0.02377 (5)
Mo40.568983 (17)0.235361 (11)0.129289 (6)0.01836 (5)
Mo50.488850 (17)0.531167 (11)0.136063 (7)0.01990 (5)
P10.49905 (5)0.39040 (3)0.071272 (19)0.01954 (12)
P20.39585 (5)0.35973 (3)0.182165 (18)0.01672 (11)
O10.19088 (17)0.46367 (11)0.06076 (6)0.0326 (4)
O20.37835 (14)0.36919 (9)0.08454 (5)0.0219 (3)
O30.24558 (18)0.18901 (11)0.12105 (8)0.0445 (5)
O40.51165 (18)0.36254 (11)0.02472 (6)0.0348 (5)
H210.55610.39000.01140.052*
O50.26267 (18)0.24150 (13)0.04182 (7)0.0436 (5)
O60.80289 (15)0.38793 (11)0.14037 (6)0.0323 (4)
O70.40830 (16)0.34044 (10)0.23039 (5)0.0273 (4)
H220.42920.37770.24380.041*
O80.70150 (17)0.41885 (11)0.21538 (6)0.0329 (4)
O90.28124 (14)0.39508 (9)0.17575 (5)0.0211 (3)
O100.63370 (14)0.29609 (9)0.17264 (5)0.0220 (3)
O110.33624 (14)0.50730 (9)0.12380 (5)0.0224 (4)
O120.45737 (15)0.22831 (9)0.08715 (5)0.0236 (4)
O130.40575 (14)0.28766 (9)0.15824 (5)0.0212 (3)
O140.51224 (15)0.47256 (9)0.07319 (5)0.0236 (4)
O150.64225 (14)0.49222 (9)0.14026 (5)0.0213 (3)
O160.51736 (17)0.60912 (10)0.10865 (6)0.0336 (4)
O170.58737 (14)0.35249 (9)0.09946 (5)0.0217 (3)
O180.48900 (14)0.41418 (9)0.17009 (5)0.0202 (3)
O190.47497 (15)0.56183 (10)0.18699 (6)0.0281 (4)
O200.54467 (15)0.15868 (10)0.15847 (6)0.0264 (4)
O210.19002 (14)0.33318 (10)0.10747 (6)0.0246 (4)
O220.69131 (15)0.21350 (10)0.10217 (6)0.0263 (4)
O230.10681 (15)0.46518 (10)0.13920 (6)0.0293 (4)
O1W0.0081 (2)0.45867 (14)0.22711 (7)0.0484 (6)
H5A0.07460.45650.24500.058*
H5B−0.05900.45800.24440.058*0.50
H5C0.03650.45710.19830.058*0.50
O2W0.1367 (2)0.07679 (19)0.03045 (8)0.0781 (10)
H6A0.21050.06280.01800.094*
H6B0.13960.06370.06090.094*
N11.1584 (2)0.70730 (15)−0.05533 (7)0.0388 (6)
H11.20670.7286−0.07260.047*
N20.7791 (2)0.53924 (13)0.08094 (7)0.0304 (5)
H20.73100.51760.09820.036*
N31.10428 (19)0.30064 (13)0.19184 (8)0.0331 (5)
H31.15650.33170.18350.040*
N40.6958 (2)0.05518 (14)0.25719 (9)0.0415 (6)
H40.64420.02360.26550.050*
C11.1859 (3)0.64345 (19)−0.03824 (9)0.0388 (7)
H1A1.25670.6216−0.04480.047*
C21.1126 (2)0.60884 (16)−0.01112 (9)0.0315 (6)
H2A1.13240.56330.00130.038*
C31.0093 (2)0.64131 (14)−0.00206 (7)0.0225 (5)
C40.9837 (2)0.70774 (16)−0.02057 (9)0.0339 (6)
H4A0.91340.7308−0.01480.041*
C51.0605 (3)0.74020 (18)−0.04738 (10)0.0417 (7)
H51.04370.7859−0.06010.050*
C60.7391 (2)0.57677 (16)0.04779 (9)0.0311 (6)
H60.65980.57980.04320.037*
C70.8120 (2)0.61103 (15)0.02029 (8)0.0262 (5)
H70.78370.6382−0.00310.031*
C80.9276 (2)0.60545 (13)0.02716 (7)0.0213 (5)
C90.9667 (2)0.56597 (14)0.06186 (8)0.0270 (5)
H91.04560.56140.06700.032*
C100.8895 (2)0.53352 (15)0.08870 (9)0.0306 (6)
H100.91520.50700.11280.037*
C111.1214 (2)0.26356 (15)0.22744 (9)0.0291 (6)
H111.18800.27140.24370.035*
C121.0420 (2)0.21368 (14)0.24067 (8)0.0253 (5)
H121.05390.18650.26600.030*
C130.9441 (2)0.20307 (13)0.21692 (8)0.0219 (5)
C140.9291 (2)0.24402 (16)0.17998 (9)0.0313 (6)
H140.86290.23820.16330.038*
C151.0119 (2)0.29308 (18)0.16812 (10)0.0375 (7)
H151.00300.32140.14310.045*
C160.7041 (2)0.07013 (16)0.21599 (10)0.0356 (7)
H160.65470.04730.19620.043*
C170.7839 (2)0.11843 (15)0.20234 (9)0.0294 (6)
H170.79010.12950.17300.035*
C180.8559 (2)0.15142 (14)0.23123 (8)0.0240 (5)
C190.8440 (2)0.13527 (17)0.27439 (9)0.0337 (6)
H190.89140.15790.29490.040*
C200.7622 (3)0.08594 (19)0.28668 (10)0.0422 (7)
H200.75300.07380.31580.051*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01621 (10)0.02008 (10)0.02219 (10)−0.00188 (7)0.00135 (8)0.00065 (8)
Mo20.01688 (10)0.02155 (10)0.02075 (10)0.00192 (7)0.00012 (8)0.00032 (8)
Mo30.01946 (10)0.02123 (11)0.03062 (11)−0.00034 (8)−0.00211 (9)−0.00514 (8)
Mo40.01718 (10)0.01714 (10)0.02077 (10)0.00070 (7)0.00317 (8)−0.00003 (7)
Mo50.01883 (10)0.01682 (10)0.02407 (10)−0.00144 (7)0.00478 (8)−0.00049 (8)
P10.0208 (3)0.0208 (3)0.0170 (3)0.0005 (2)0.0042 (2)0.0008 (2)
P20.0161 (3)0.0168 (3)0.0172 (3)−0.0008 (2)0.0034 (2)0.0014 (2)
O10.0368 (11)0.0358 (11)0.0253 (9)0.0069 (9)−0.0058 (8)0.0010 (8)
O20.0181 (8)0.0215 (8)0.0259 (8)0.0009 (7)0.0031 (7)0.0000 (7)
O30.0312 (11)0.0299 (11)0.0724 (15)−0.0077 (9)0.0030 (11)0.0052 (10)
O40.0471 (12)0.0362 (11)0.0212 (9)−0.0060 (9)0.0104 (9)−0.0043 (8)
O50.0348 (11)0.0538 (14)0.0422 (12)0.0135 (10)−0.0133 (10)−0.0234 (10)
O60.0196 (9)0.0342 (10)0.0433 (11)0.0016 (8)0.0054 (8)0.0061 (9)
O70.0356 (10)0.0265 (9)0.0199 (8)0.0025 (8)0.0009 (8)0.0034 (7)
O80.0393 (11)0.0321 (10)0.0271 (9)−0.0067 (9)−0.0053 (8)−0.0007 (8)
O90.0176 (8)0.0234 (9)0.0222 (8)0.0003 (6)0.0037 (7)0.0029 (7)
O100.0220 (8)0.0210 (8)0.0229 (8)0.0004 (7)−0.0002 (7)0.0016 (7)
O110.0199 (8)0.0203 (8)0.0272 (9)0.0020 (7)0.0025 (7)0.0006 (7)
O120.0234 (9)0.0233 (9)0.0242 (8)0.0023 (7)0.0001 (7)−0.0056 (7)
O130.0216 (8)0.0186 (8)0.0233 (8)−0.0008 (7)0.0049 (7)−0.0018 (7)
O140.0275 (9)0.0212 (9)0.0219 (8)−0.0006 (7)0.0044 (7)0.0024 (7)
O150.0172 (8)0.0201 (8)0.0264 (8)−0.0031 (6)0.0053 (7)0.0014 (7)
O160.0355 (11)0.0233 (10)0.0421 (11)−0.0030 (8)0.0092 (9)0.0046 (8)
O170.0183 (8)0.0231 (8)0.0237 (8)0.0009 (7)0.0027 (7)0.0014 (7)
O180.0175 (8)0.0173 (8)0.0259 (8)−0.0022 (6)0.0020 (7)0.0010 (7)
O190.0245 (9)0.0283 (10)0.0315 (9)−0.0022 (7)0.0050 (8)−0.0094 (8)
O200.0278 (9)0.0223 (9)0.0293 (9)−0.0012 (7)0.0033 (8)0.0035 (7)
O210.0160 (8)0.0255 (9)0.0323 (9)−0.0018 (7)0.0009 (7)−0.0022 (7)
O220.0243 (9)0.0246 (9)0.0300 (9)0.0025 (7)0.0095 (8)0.0010 (7)
O230.0206 (9)0.0343 (10)0.0331 (10)0.0052 (8)0.0008 (8)−0.0014 (8)
O1W0.0473 (14)0.0580 (15)0.0398 (12)0.0031 (11)0.0049 (10)0.0056 (11)
O2W0.0599 (17)0.127 (3)0.0471 (15)0.0313 (18)0.0066 (13)0.0466 (17)
N10.0390 (14)0.0514 (16)0.0259 (12)−0.0203 (12)0.0101 (11)0.0036 (11)
N20.0302 (12)0.0294 (12)0.0314 (12)−0.0051 (9)0.0138 (10)0.0022 (10)
N30.0209 (11)0.0327 (12)0.0458 (14)−0.0022 (9)0.0081 (10)0.0101 (11)
N40.0327 (13)0.0318 (13)0.0598 (17)−0.0071 (11)0.0152 (13)0.0056 (12)
C10.0270 (14)0.0536 (19)0.0358 (15)−0.0034 (13)0.0124 (13)−0.0033 (14)
C20.0282 (14)0.0348 (15)0.0316 (14)−0.0001 (11)0.0080 (12)0.0024 (11)
C30.0210 (12)0.0274 (13)0.0191 (11)−0.0056 (10)0.0020 (10)−0.0020 (9)
C40.0302 (14)0.0318 (14)0.0397 (15)−0.0005 (12)0.0057 (12)0.0054 (12)
C50.0482 (19)0.0388 (17)0.0382 (16)−0.0099 (14)0.0037 (15)0.0121 (13)
C60.0222 (13)0.0364 (15)0.0347 (14)−0.0035 (11)0.0053 (12)−0.0026 (12)
C70.0230 (13)0.0321 (14)0.0234 (12)−0.0020 (10)0.0009 (10)−0.0005 (10)
C80.0220 (12)0.0207 (12)0.0211 (11)−0.0022 (9)0.0049 (10)−0.0029 (9)
C90.0231 (13)0.0279 (13)0.0299 (13)0.0016 (10)0.0038 (11)0.0025 (11)
C100.0327 (15)0.0310 (14)0.0281 (13)0.0003 (11)0.0049 (12)0.0062 (11)
C110.0218 (12)0.0298 (14)0.0357 (14)0.0006 (10)0.0018 (11)−0.0015 (11)
C120.0244 (12)0.0239 (12)0.0276 (12)0.0021 (10)0.0021 (10)0.0001 (10)
C130.0221 (12)0.0196 (11)0.0239 (11)0.0022 (9)0.0052 (10)−0.0018 (9)
C140.0236 (13)0.0400 (16)0.0303 (14)−0.0012 (11)−0.0012 (11)0.0065 (12)
C150.0301 (15)0.0444 (17)0.0380 (15)−0.0010 (13)0.0040 (12)0.0174 (13)
C160.0285 (14)0.0295 (14)0.0489 (17)−0.0025 (11)0.0062 (13)−0.0090 (13)
C170.0244 (13)0.0289 (13)0.0348 (14)0.0008 (11)0.0044 (11)−0.0053 (11)
C180.0196 (12)0.0215 (12)0.0308 (12)0.0033 (9)0.0042 (10)0.0001 (10)
C190.0265 (14)0.0435 (17)0.0313 (14)−0.0006 (12)0.0039 (12)0.0077 (12)
C200.0342 (16)0.0523 (19)0.0401 (16)0.0019 (14)0.0115 (14)0.0157 (15)
Geometric parameters (Å, °) top
Mo1—O61.7041 (19)N1—C51.328 (4)
Mo1—O81.7045 (19)N1—H10.88
Mo1—O101.9073 (17)N2—C101.332 (4)
Mo1—O151.9518 (17)N2—C61.337 (4)
Mo1—O182.2191 (17)N2—H20.88
Mo1—O172.4114 (17)N3—C111.327 (4)
Mo2—O11.7024 (19)N3—C151.330 (4)
Mo2—O231.7155 (18)N3—H30.88
Mo2—O211.9174 (18)N4—C161.331 (4)
Mo2—O111.9251 (18)N4—C201.341 (4)
Mo2—O92.2839 (17)N4—H40.88
Mo2—O22.3637 (17)C1—C21.372 (4)
Mo3—O31.693 (2)C1—H1A0.95
Mo3—O51.701 (2)C2—C31.389 (4)
Mo3—O211.9409 (18)C2—H2A0.95
Mo3—O121.9427 (18)C3—C41.382 (4)
Mo3—O22.2283 (17)C3—C81.487 (3)
Mo3—O132.4613 (17)C4—C51.376 (4)
Mo4—O201.7026 (17)C4—H4A0.95
Mo4—O221.7270 (17)C5—H50.95
Mo4—O121.8766 (18)C6—C71.374 (4)
Mo4—O101.9204 (17)C6—H60.95
Mo4—O132.3396 (17)C7—C81.387 (4)
Mo4—O172.3515 (17)C7—H70.95
Mo5—O161.7020 (18)C8—C91.390 (4)
Mo5—O191.7084 (18)C9—C101.379 (4)
Mo5—O111.8962 (18)C9—H90.95
Mo5—O151.9532 (17)C10—H100.95
Mo5—O142.2703 (17)C11—C121.374 (4)
Mo5—O182.3952 (17)C11—H110.95
P1—O141.5134 (18)C12—C131.391 (4)
P1—O171.5365 (18)C12—H120.95
P1—O21.5369 (17)C13—C141.396 (4)
P1—O41.5606 (18)C13—C181.479 (3)
P2—O91.5152 (17)C14—C151.380 (4)
P2—O131.5242 (17)C14—H140.95
P2—O181.5333 (17)C15—H150.95
P2—O71.5674 (17)C16—C171.363 (4)
O4—H210.84C16—H160.95
O7—H220.84C17—C181.385 (4)
O1W—H5A0.97C17—H170.95
O1W—H5B0.96C18—C191.399 (4)
O1W—H5C0.97C19—C201.379 (4)
O2W—H6A0.99C19—H190.95
O2W—H6B0.99C20—H200.95
N1—C11.328 (4)
O6—Mo1—O8105.34 (10)P2—O9—Mo2122.16 (9)
O6—Mo1—O10101.73 (8)Mo1—O10—Mo4123.52 (9)
O8—Mo1—O1098.53 (8)Mo5—O11—Mo2150.13 (10)
O6—Mo1—O1594.65 (8)Mo4—O12—Mo3125.75 (9)
O8—Mo1—O15100.26 (8)P2—O13—Mo4127.63 (10)
O10—Mo1—O15150.77 (7)P2—O13—Mo3123.99 (9)
O6—Mo1—O18158.81 (8)Mo4—O13—Mo390.12 (6)
O8—Mo1—O1893.99 (8)P1—O14—Mo5119.48 (9)
O10—Mo1—O1883.52 (7)Mo1—O15—Mo5122.24 (8)
O15—Mo1—O1873.04 (6)P1—O17—Mo4125.47 (9)
O6—Mo1—O1789.01 (8)P1—O17—Mo1128.83 (10)
O8—Mo1—O17164.57 (8)Mo4—O17—Mo190.13 (6)
O10—Mo1—O1772.50 (6)P2—O18—Mo1129.10 (10)
O15—Mo1—O1783.87 (6)P2—O18—Mo5133.78 (10)
O18—Mo1—O1772.85 (6)Mo1—O18—Mo595.56 (6)
O1—Mo2—O23102.46 (9)Mo2—O21—Mo3124.29 (9)
O1—Mo2—O21101.49 (9)H5A—O1W—H5B109.9
O23—Mo2—O21100.41 (8)H5A—O1W—H5C105.2
O1—Mo2—O1198.20 (9)H5B—O1W—H5C144.7
O23—Mo2—O11103.47 (8)H6A—O2W—H6B106.9
O21—Mo2—O11144.79 (7)C1—N1—C5122.5 (3)
O1—Mo2—O9174.32 (8)C1—N1—H1118.8
O23—Mo2—O983.16 (8)C5—N1—H1118.8
O21—Mo2—O978.04 (7)C10—N2—C6122.0 (2)
O11—Mo2—O979.53 (7)C10—N2—H2119.0
O1—Mo2—O289.87 (8)C6—N2—H2119.0
O23—Mo2—O2164.98 (8)C11—N3—C15123.2 (2)
O21—Mo2—O268.32 (6)C11—N3—H3118.4
O11—Mo2—O282.92 (7)C15—N3—H3118.4
O9—Mo2—O284.70 (6)C16—N4—C20123.2 (3)
O3—Mo3—O5104.46 (12)C16—N4—H4118.4
O3—Mo3—O2198.28 (9)C20—N4—H4118.4
O5—Mo3—O21100.25 (9)N1—C1—C2120.3 (3)
O3—Mo3—O12101.29 (9)N1—C1—H1A119.9
O5—Mo3—O1296.34 (9)C2—C1—H1A119.9
O21—Mo3—O12150.23 (7)C1—C2—C3119.1 (3)
O3—Mo3—O2154.95 (9)C1—C2—H2A120.5
O5—Mo3—O299.78 (10)C3—C2—H2A120.5
O21—Mo3—O270.99 (7)C4—C3—C2118.8 (2)
O12—Mo3—O281.98 (7)C4—C3—C8120.5 (2)
O3—Mo3—O1385.16 (9)C2—C3—C8120.7 (2)
O5—Mo3—O13164.92 (9)C5—C4—C3119.7 (3)
O21—Mo3—O1389.61 (7)C5—C4—H4A120.2
O12—Mo3—O1370.08 (6)C3—C4—H4A120.2
O2—Mo3—O1372.52 (6)N1—C5—C4119.7 (3)
O20—Mo4—O22102.57 (9)N1—C5—H5120.2
O20—Mo4—O12101.94 (8)C4—C5—H5120.2
O22—Mo4—O12102.86 (8)N2—C6—C7120.4 (3)
O20—Mo4—O1099.22 (8)N2—C6—H6119.8
O22—Mo4—O1098.78 (8)C7—C6—H6119.8
O12—Mo4—O10145.43 (7)C6—C7—C8119.1 (2)
O20—Mo4—O1389.28 (7)C6—C7—H7120.5
O22—Mo4—O13168.14 (7)C8—C7—H7120.5
O12—Mo4—O1373.99 (7)C7—C8—C9119.3 (2)
O10—Mo4—O1379.29 (7)C7—C8—C3120.7 (2)
O20—Mo4—O17169.55 (7)C9—C8—C3120.0 (2)
O22—Mo4—O1786.33 (7)C10—C9—C8119.1 (3)
O12—Mo4—O1781.07 (7)C10—C9—H9120.4
O10—Mo4—O1773.72 (7)C8—C9—H9120.4
O13—Mo4—O1781.89 (6)N2—C10—C9120.1 (3)
O16—Mo5—O19102.73 (9)N2—C10—H10119.9
O16—Mo5—O11106.15 (9)C9—C10—H10119.9
O19—Mo5—O11100.13 (8)N3—C11—C12119.5 (3)
O16—Mo5—O1599.01 (8)N3—C11—H11120.2
O19—Mo5—O1598.37 (8)C12—C11—H11120.2
O11—Mo5—O15144.41 (7)C11—C12—C13119.8 (2)
O16—Mo5—O1485.93 (8)C11—C12—H12120.1
O19—Mo5—O14170.78 (8)C13—C12—H12120.1
O11—Mo5—O1480.16 (7)C12—C13—C14118.6 (2)
O15—Mo5—O1476.91 (7)C12—C13—C18120.8 (2)
O16—Mo5—O18167.66 (8)C14—C13—C18120.5 (2)
O19—Mo5—O1882.72 (8)C15—C14—C13119.0 (3)
O11—Mo5—O1883.45 (6)C15—C14—H14120.5
O15—Mo5—O1869.06 (6)C13—C14—H14120.5
O14—Mo5—O1888.17 (6)N3—C15—C14119.8 (3)
O14—P1—O17110.84 (10)N3—C15—H15120.1
O14—P1—O2109.63 (10)C14—C15—H15120.1
O17—P1—O2111.07 (9)N4—C16—C17119.5 (3)
O14—P1—O4110.65 (11)N4—C16—H16120.2
O17—P1—O4109.33 (11)C17—C16—H16120.2
O2—P1—O4105.19 (11)C16—C17—C18120.1 (3)
O9—P2—O13111.86 (10)C16—C17—H17120.0
O9—P2—O18109.36 (10)C18—C17—H17120.0
O13—P2—O18112.63 (10)C17—C18—C19119.0 (2)
O9—P2—O7108.03 (10)C17—C18—C13120.8 (2)
O13—P2—O7106.11 (10)C19—C18—C13120.2 (2)
O18—P2—O7108.65 (10)C20—C19—C18118.8 (3)
P1—O2—Mo3129.94 (10)C20—C19—H19120.6
P1—O2—Mo2133.75 (10)C18—C19—H19120.6
Mo3—O2—Mo295.91 (6)N4—C20—C19119.4 (3)
P1—O4—H21109.5N4—C20—H20120.3
P2—O7—H22109.5C19—C20—H20120.3
O14—P1—O2—Mo3−176.12 (11)O11—Mo5—O15—Mo1−39.14 (17)
O17—P1—O2—Mo3−53.29 (15)O14—Mo5—O15—Mo1−90.36 (10)
O4—P1—O2—Mo364.89 (15)O18—Mo5—O15—Mo12.73 (8)
O14—P1—O2—Mo2−5.27 (16)O14—P1—O17—Mo4155.65 (10)
O17—P1—O2—Mo2117.56 (13)O2—P1—O17—Mo433.52 (14)
O4—P1—O2—Mo2−124.26 (14)O4—P1—O17—Mo4−82.12 (13)
O3—Mo3—O2—P1110.1 (2)O14—P1—O17—Mo130.40 (15)
O5—Mo3—O2—P1−84.55 (14)O2—P1—O17—Mo1−91.73 (13)
O21—Mo3—O2—P1177.89 (15)O4—P1—O17—Mo1152.64 (11)
O12—Mo3—O2—P110.55 (13)O20—Mo4—O17—P1−89.7 (4)
O13—Mo3—O2—P182.10 (13)O22—Mo4—O17—P1121.51 (13)
O3—Mo3—O2—Mo2−63.3 (2)O12—Mo4—O17—P117.86 (11)
O5—Mo3—O2—Mo2102.08 (8)O10—Mo4—O17—P1−138.24 (13)
O21—Mo3—O2—Mo24.52 (6)O13—Mo4—O17—P1−57.09 (11)
O12—Mo3—O2—Mo2−162.82 (7)O20—Mo4—O17—Mo150.8 (4)
O13—Mo3—O2—Mo2−91.27 (6)O22—Mo4—O17—Mo1−98.01 (7)
O1—Mo2—O2—P179.95 (15)O12—Mo4—O17—Mo1158.35 (7)
O23—Mo2—O2—P1−134.6 (3)O10—Mo4—O17—Mo12.25 (6)
O21—Mo2—O2—P1−177.62 (16)O13—Mo4—O17—Mo183.40 (6)
O11—Mo2—O2—P1−18.33 (13)O6—Mo1—O17—P1−121.35 (13)
O9—Mo2—O2—P1−98.41 (14)O8—Mo1—O17—P179.9 (3)
O1—Mo2—O2—Mo3−107.09 (8)O10—Mo1—O17—P1136.03 (13)
O23—Mo2—O2—Mo338.4 (3)O15—Mo1—O17—P1−26.56 (12)
O21—Mo2—O2—Mo3−4.66 (7)O18—Mo1—O17—P147.55 (11)
O11—Mo2—O2—Mo3154.63 (7)O6—Mo1—O17—Mo4100.35 (8)
O9—Mo2—O2—Mo374.56 (6)O8—Mo1—O17—Mo4−58.4 (3)
O13—P2—O9—Mo2−64.72 (13)O10—Mo1—O17—Mo4−2.28 (6)
O18—P2—O9—Mo260.76 (13)O15—Mo1—O17—Mo4−164.87 (6)
O7—P2—O9—Mo2178.85 (10)O18—Mo1—O17—Mo4−90.76 (6)
O1—Mo2—O9—P2−4.4 (9)O9—P2—O18—Mo1−171.70 (11)
O23—Mo2—O9—P2−176.36 (13)O13—P2—O18—Mo1−46.66 (15)
O21—Mo2—O9—P281.43 (12)O7—P2—O18—Mo170.59 (14)
O11—Mo2—O9—P2−71.25 (11)O9—P2—O18—Mo5−9.58 (16)
O2—Mo2—O9—P212.51 (11)O13—P2—O18—Mo5115.46 (13)
O6—Mo1—O10—Mo4−81.83 (12)O7—P2—O18—Mo5−127.29 (13)
O8—Mo1—O10—Mo4170.45 (11)O6—Mo1—O18—P2112.6 (2)
O15—Mo1—O10—Mo440.9 (2)O8—Mo1—O18—P2−91.35 (14)
O18—Mo1—O10—Mo477.36 (10)O10—Mo1—O18—P26.79 (12)
O17—Mo1—O10—Mo43.35 (9)O15—Mo1—O18—P2169.12 (14)
O20—Mo4—O10—Mo1−175.50 (11)O17—Mo1—O18—P280.43 (12)
O22—Mo4—O10—Mo180.13 (11)O6—Mo1—O18—Mo5−54.5 (2)
O12—Mo4—O10—Mo1−48.27 (18)O8—Mo1—O18—Mo5101.52 (8)
O13—Mo4—O10—Mo1−88.00 (10)O10—Mo1—O18—Mo5−160.34 (7)
O17—Mo4—O10—Mo1−3.41 (9)O15—Mo1—O18—Mo51.99 (6)
O16—Mo5—O11—Mo2139.11 (19)O17—Mo1—O18—Mo5−86.70 (6)
O19—Mo5—O11—Mo2−114.3 (2)O16—Mo5—O18—P2−153.0 (3)
O15—Mo5—O11—Mo25.9 (3)O19—Mo5—O18—P289.92 (14)
O14—Mo5—O11—Mo256.30 (19)O11—Mo5—O18—P2−11.21 (13)
O18—Mo5—O11—Mo2−32.97 (19)O15—Mo5—O18—P2−168.19 (15)
O1—Mo2—O11—Mo5−114.2 (2)O14—Mo5—O18—P2−91.51 (14)
O23—Mo2—O11—Mo5140.78 (19)O16—Mo5—O18—Mo113.2 (4)
O21—Mo2—O11—Mo59.4 (3)O19—Mo5—O18—Mo1−103.93 (8)
O9—Mo2—O11—Mo560.50 (19)O11—Mo5—O18—Mo1154.94 (7)
O2—Mo2—O11—Mo5−25.39 (19)O15—Mo5—O18—Mo1−2.04 (6)
O20—Mo4—O12—Mo383.35 (12)O14—Mo5—O18—Mo174.64 (6)
O22—Mo4—O12—Mo3−170.60 (11)O1—Mo2—O21—Mo391.66 (12)
O10—Mo4—O12—Mo3−43.20 (19)O23—Mo2—O21—Mo3−163.19 (11)
O13—Mo4—O12—Mo3−2.40 (10)O11—Mo2—O21—Mo3−31.05 (19)
O17—Mo4—O12—Mo3−86.47 (11)O9—Mo2—O21—Mo3−82.55 (11)
O3—Mo3—O12—Mo4−78.23 (14)O2—Mo2—O21—Mo36.45 (9)
O5—Mo3—O12—Mo4175.61 (13)O3—Mo3—O21—Mo2149.94 (13)
O21—Mo3—O12—Mo451.9 (2)O5—Mo3—O21—Mo2−103.64 (13)
O2—Mo3—O12—Mo476.57 (11)O12—Mo3—O21—Mo219.2 (2)
O13—Mo3—O12—Mo42.34 (9)O2—Mo3—O21—Mo2−6.72 (10)
O9—P2—O13—Mo4149.46 (10)O13—Mo3—O21—Mo264.89 (11)
O18—P2—O13—Mo425.80 (15)C5—N1—C1—C2−0.2 (5)
O7—P2—O13—Mo4−92.95 (13)N1—C1—C2—C30.4 (4)
O9—P2—O13—Mo327.92 (13)C1—C2—C3—C4−0.2 (4)
O18—P2—O13—Mo3−95.74 (12)C1—C2—C3—C8180.0 (3)
O7—P2—O13—Mo3145.51 (10)C2—C3—C4—C5−0.1 (4)
O20—Mo4—O13—P2123.86 (13)C8—C3—C4—C5179.7 (3)
O22—Mo4—O13—P2−57.4 (4)C1—N1—C5—C4−0.1 (5)
O12—Mo4—O13—P2−133.50 (13)C3—C4—C5—N10.2 (5)
O10—Mo4—O13—P224.33 (12)C10—N2—C6—C70.1 (4)
O17—Mo4—O13—P2−50.53 (12)N2—C6—C7—C80.7 (4)
O20—Mo4—O13—Mo3−101.10 (7)C6—C7—C8—C9−0.6 (4)
O22—Mo4—O13—Mo377.7 (4)C6—C7—C8—C3179.6 (2)
O12—Mo4—O13—Mo31.54 (6)C4—C3—C8—C735.2 (4)
O10—Mo4—O13—Mo3159.37 (7)C2—C3—C8—C7−145.0 (3)
O17—Mo4—O13—Mo384.51 (6)C4—C3—C8—C9−144.6 (3)
O3—Mo3—O13—P2−120.11 (13)C2—C3—C8—C935.2 (4)
O5—Mo3—O13—P2109.4 (3)C7—C8—C9—C10−0.2 (4)
O21—Mo3—O13—P2−21.76 (11)C3—C8—C9—C10179.6 (2)
O12—Mo3—O13—P2136.03 (12)C6—N2—C10—C9−0.9 (4)
O2—Mo3—O13—P248.40 (11)C8—C9—C10—N21.0 (4)
O3—Mo3—O13—Mo4102.35 (9)C15—N3—C11—C121.2 (4)
O5—Mo3—O13—Mo4−28.1 (4)N3—C11—C12—C13−0.7 (4)
O21—Mo3—O13—Mo4−159.31 (7)C11—C12—C13—C14−0.2 (4)
O12—Mo3—O13—Mo4−1.52 (6)C11—C12—C13—C18−178.0 (2)
O2—Mo3—O13—Mo4−89.15 (6)C12—C13—C14—C150.5 (4)
O17—P1—O14—Mo5−61.89 (13)C18—C13—C14—C15178.4 (3)
O2—P1—O14—Mo561.08 (13)C11—N3—C15—C14−0.9 (5)
O4—P1—O14—Mo5176.65 (11)C13—C14—C15—N30.0 (5)
O16—Mo5—O14—P1179.84 (13)C20—N4—C16—C170.5 (5)
O19—Mo5—O14—P119.6 (5)N4—C16—C17—C180.2 (4)
O11—Mo5—O14—P1−72.97 (12)C16—C17—C18—C19−1.0 (4)
O15—Mo5—O14—P179.61 (12)C16—C17—C18—C13179.0 (2)
O18—Mo5—O14—P110.69 (11)C12—C13—C18—C17−154.0 (2)
O6—Mo1—O15—Mo5159.52 (11)C14—C13—C18—C1728.2 (4)
O8—Mo1—O15—Mo5−93.95 (11)C12—C13—C18—C1926.0 (4)
O10—Mo1—O15—Mo535.3 (2)C14—C13—C18—C19−151.8 (3)
O18—Mo1—O15—Mo5−2.88 (9)C17—C18—C19—C201.2 (4)
O17—Mo1—O15—Mo571.02 (10)C13—C18—C19—C20−178.9 (3)
O16—Mo5—O15—Mo1−174.01 (11)C16—N4—C20—C19−0.4 (5)
O19—Mo5—O15—Mo181.58 (11)C18—C19—C20—N4−0.5 (5)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H5A···O8i0.972.073.008 (3)162
O1W—H5B···N4ii0.962.443.135 (4)129
O2W—H6A···O1iii0.992.543.059 (3)112
O2W—H6B···O11iii0.992.253.221 (3)166
O2W—H6B···O16iii0.992.533.121 (4)118
N1—H1···O22iv0.881.862.728 (3)170
N3—H3···O9v0.881.892.761 (3)169
N3—H3···O21v0.882.432.907 (3)115
N4—H4···O19vi0.882.172.680 (3)116
N4—H4···O1Wiii0.882.473.135 (4)132
O4—H21···O2Wvii0.841.742.538 (3)159
O7—H22···O1Wviii0.841.982.805 (3)169
N2—H2···O150.881.752.618 (3)166
O1W—H5C···O230.972.053.009 (3)173
Symmetry codes: (i) x−1/2, y, −z+1/2; (ii) −x+1/2, y+1/2, z; (iii) −x+1/2, y−1/2, z; (iv) −x+2, −y+1, −z; (v) x+1, y, z; (vi) −x+1, y−1/2, −z+1/2; (vii) x+1/2, −y+1/2, −z; (viii) x+1/2, y, −z+1/2.
Table 1
Selected geometric parameters (Å, °) top
Mo1—O61.7041 (19)Mo1—O172.4114 (17)
Mo1—O81.7045 (19)P1—O141.5134 (18)
Mo1—O101.9073 (17)P1—O171.5365 (18)
Mo1—O151.9518 (17)P1—O21.5369 (17)
Mo1—O182.2191 (17)P1—O41.5606 (18)
O6—Mo1—O8105.34 (10)O8—Mo1—O17164.57 (8)
O6—Mo1—O10101.73 (8)O10—Mo1—O1772.50 (6)
O8—Mo1—O1098.53 (8)O15—Mo1—O1783.87 (6)
O6—Mo1—O1594.65 (8)O18—Mo1—O1772.85 (6)
O8—Mo1—O15100.26 (8)O14—P1—O17110.84 (10)
O10—Mo1—O15150.77 (7)O14—P1—O2109.63 (10)
O6—Mo1—O18158.81 (8)O17—P1—O2111.07 (9)
O8—Mo1—O1893.99 (8)O14—P1—O4110.65 (11)
O10—Mo1—O1883.52 (7)O17—P1—O4109.33 (11)
O15—Mo1—O1873.04 (6)O2—P1—O4105.19 (11)
O6—Mo1—O1789.01 (8)
C2—C3—C8—C935.2 (4)C12—C13—C18—C1926.0 (4)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H5A···O8i0.972.073.008 (3)162
O1W—H5B···N4ii0.962.443.135 (4)129
O2W—H6A···O1iii0.992.543.059 (3)112
O2W—H6B···O11iii0.992.253.221 (3)166
O2W—H6B···O16iii0.992.533.121 (4)118
N1—H1···O22iv0.881.862.728 (3)170
N3—H3···O9v0.881.892.761 (3)169
N3—H3···O21v0.882.432.907 (3)115
N4—H4···O19vi0.882.172.680 (3)116
N4—H4···O1Wiii0.882.473.135 (4)132
O4—H21···O2Wvii0.841.742.538 (3)159
O7—H22···O1Wviii0.841.982.805 (3)169
N2—H2···O150.881.752.618 (3)166
O1W—H5C···O230.972.053.009 (3)173
Symmetry codes: (i) x−1/2, y, −z+1/2; (ii) −x+1/2, y+1/2, z; (iii) −x+1/2, y−1/2, z; (iv) −x+2, −y+1, −z; (v) x+1, y, z; (vi) −x+1, y−1/2, −z+1/2; (vii) x+1/2, −y+1/2, −z; (viii) x+1/2, y, −z+1/2.
Acknowledgements top

This work was supported by the Science and Technology Development Foundation of Fuzhou University (No. 2004-xq-05) and the Scientific Research Foundation of Fujian Education Department (No. JB04010).

references
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