1,4-Di­methyl­pyridinium hexakis­(di­methyl­form­amide-[kappa]O)­calcium(II) dodecamolybdophosphate

In the title compound, (C₇H₁₀N)[Ca(C₃H₇NO)₆][PMo₁₂O₄₀], two types of cations {viz. 1,4-di­methyl­pyridinium and a [Ca(DMF)₆]²⁺ complex cation (DMF is di­methyl­form­amide)} and dodecamolybdophosphate (tetra­conta­oxo­phos­phido­dodeca­molybdate) anions form an infinite three-dimensional assembly via electrostatic forces.

S1. Comment

In crystal engineering and polyoxometalate (POM) chemistry, one of the major challenges is to establish reliable connections between new molecular and supramolecular structures on the basis of intermolecular interactions (Desiraju, 1995; Niu et al., 2003). Ideally, we would like to identify substructural units in a target supermolecule that can be assembled from logically chosen precursor molecules. We attempt here to use a simple method to realise such molecular assemblies. This paper deals with the preparation and crystal structure of a new supramolecular compound obtained from the reaction of 1,4-dimethylpyridinium iodide (DMPI), CaCl₂ and Keggin-type H₃PMo₁₂O₄₀. The synthesis and structure of the title compound, (I), in which infinite stacking assemblies are achieved, may serve as useful models for the design of functional molecular assemblies.

The title compound is built from three subunits, viz. two cations {1,4-dimethylpyridine (DMP) and a [Ca(dmf)₆]²⁺ complex cation (dmf is dimethylformamide} and dodecamolybdophosphate anions ([PMo₁₂O₄₀]³⁻; denoted POM). In the [Ca(dmf)₆]²⁺ complex cation, the Ca atom is coordinated in a distorted octahedral fashion by six O atoms of dmf ligands. The Ca—O bond lengths range from 2.275 (10) to 2.329 (9) Å (Table 1), with para-O—Ca—para-O angles from 162.5 (4) to 171.1 (4)° and ortho-O—Ca—ortho-O angles from 80.8 (4) to 104.7 (4)°. Because all dmf ligands are the same, the difference in bond lengths and angles (which causes a distorted octahedron) must be the result of internal pressure, induced by the crystal packing and intermolecular interactions. The Keggin structure [PMo₁₂O₄₀]³⁻ consists of one PO₄ tetrahedron (atom Oa) surrounded by four corner-sharing Mo₃O₁₃ sets formed by three edge-sharing MoO₆ octahedra (corner-sharing O atoms between Mo₃O₁₃ are denoted Ob, edge-sharing O atoms inside Mo₃O₁₃ are denoted Oc and unshared terminal O atoms are denoted Ot). The P—Oa bond distances are 1.530 (6)—1.547 (7) Å, with angles of 109.1 (3)–110.0 (4)°, showing that the PO₄ tetrahedron is distorted to small entent. In the MoO₆ octahedra, the Mo—Ot, Mo—Oa and Mo—Ob,c bond distances fall in the ranges 1.659 (7)–1.690 (7), 2.413 (6)–2.435 (6) and 1.850 (7)–1.978 (8) Å, and the mean values are 1.676, 2.426 and 1.912 Å, respectively. These results show that the MoO₆ octahedra of the polyanions in (I) are severely distorted because of the influence of the outer cations (Pope, 1983; Niu et al., 2002, 2003; Wang et al., 2002). The three subunits of (I) form an infinite three-dimensional assembly via electrostatic forces. Weak C—H···O, C—H···Mo and C=O···C interactions help to link the cations and anions together (Fig. 1 and Table 2). DMP cations and POM anions, as well as [Ca(dmf)₆]²⁺ cations and POM anions, participate in weak interactions, and DMP cations and Ca(dmf)₆²⁺ cations are also linked via carbonyl O and methyl C atoms [O5···C6' = 2.808 (8) Å]. This type of interaction is similar to a carbonyl–carbonyl interaction (Allen et al., 1998). On the other hand, the O5···C6 distance [3.399 (9) Å] is longer than the sum of van der Waals radii for C and O atoms (3.22 Å).

The packing structure is a multilayered system, in which different types of layers can be found in point of different subunits. For example, three types of layers can be found along [100] (a axis) for every two of the subunits (Figs. 2 and 3). The POM and DMP ions constitute graphite-like layers; two types of weak interactions (O···H and Mo···H) occur inside the layers, but no such interactions are present between layers. The POM ion forms zigzag ribbons through this kind of interactions. In the same way, the POM and [Ca(dmf)₆]²⁺ ions constitute interlaced layers; each POM ion forms weak interactions (O···H and Mo···H) with every [Ca(dmf)₆]²⁺ cation around it, and vice versa, thus building the framework of the crystal.

Table 2. C—H···O and C=O···C interaction geometry (Å, °)

S2. Experimental

All organic solvents and common materials used in the synthesis were of reagent grade and were used without further purification. H₃PMo₁₂O₄₀ was prepared according to the literature method (Claude et al., 1983). 1,4-Dimethylpyridinium iodide was prepared according to the method described by Ren et al. (2000). Compound (I) was prepared by mixing a CaCl₂/dmf solution (0.01 mol l⁻¹), a DMPI/dmf solution (0.01 mol l⁻¹) and a H₃PMo₁₂O₄₀/dmf solution (0.01 mol l⁻¹) in a 1:1:1 molar ratio. After 15 d of slow evaporation of water at room temperature, bright-green crystals of (I) were obtained from the solution; the crystals were transparent without further purification. Analysis calculated: C 12.46, H 2.18, N 4.07%; found: C 12.26, H 2.18, N 3.94%. IR (KBr, cm⁻¹): 1061, 957, 878, 797 (PMo₁₂O₄₀³⁻), 1654 (C=O), 1600, 1497, 1437 (pyridine ring), 1382 (–CH₃).

S3. Refinement

For other DMP salts (Khan et al., 1998; Fun et al., 1996; Houghton & Wallwork, 1999; Mckinney et al., 1997), disordered para-C and para-N atoms could be treated as 50%C + 50%N; however, our attempts to refine the title compound in the same way were unsuccessful. In fact, the DMP cation is rocking, and the populations of the two possible orientations, C1/C7/N1 and C1'/C7'/N1', are 72.5 (10) and 27.5 (10)%, respectively. In the [Ca(dmf)₆]²⁺ cation, the torsional motion of the NMe₂ groups of the dmf ligands leads to substantial disorder. Each NMe₂ moiety has two possible positions, with site occupancy factors of 72.5 (10) and 27.5 (10)%. These disorders in the cations contribute to the high s.u. values of bond lengths and angles (0.006–0.02 Å and 0.2–1.9°). A number of atoms have apparently high displacement parameters and some of them cannot be treated as anisotropic for the same reasons. All H atoms were positioned geometrically and allowed to ride on their parent atoms, with C—H distances in the range 0.93–0.96 Å, and with U_iso(H) = 1.5U_eq(C) for methyl H atoms and 1.2U_eq(C) for the other H atoms.

Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXL97.

Figures

	Fig. 1. A 30% probability displacement ellipsoid plot of (I), with the atom-numbering scheme (only some of the H-atom numbers are shown). The disorder of the DMP atoms is illustrate by dotted circles and lines, but the minor components of the disordered? dmf ligands have been omitted for clarity. C—H···Mo interactions are not shown.
	Fig. 2. A packing diagram of (I), as viewed along the b axis, depicted at the 10% probability level. All minor components of disordered groups have been omitted for clarity.
	Fig. 3. A schematic representation of the multilayered crystal structure of (I).

1,4-Dimethylpyridinium hexakis(dimethylformamide-κO)calcium(II) tetracontaoxophosphidododecamolybdate

Crystal data

(C7H10N)[Ca(C3H7NO)6][PMo12O40]	F(000) = 4632.0
Mr = 2409.07	Dx = 2.442 Mg m^−3
Orthorhombic, Pca21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2ac	Cell parameters from 380 reflections
a = 38.293 (6) Å	θ = 7.5–27.0°
b = 13.246 (2) Å	µ = 2.43 mm^−1
c = 12.888 (2) Å	T = 293 K
V = 6537.6 (17) Å^3	Block, green
Z = 4	0.49 × 0.11 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer	14090 independent reflections
Radiation source: fine-focus sealed tube	12008 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.038
ϕ and ω scans	θmax = 27.1°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −48→49
Tmin = 0.733, Tmax = 0.824	k = −14→16
39117 measured reflections	l = −16→16

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.060	H-atom parameters constrained
wR(F^2) = 0.127	w = 1/[σ^2(Fo^2) + (0.0518P)^2 + 11.3547P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max = 0.002
14090 reflections	Δρmax = 1.08 e Å^−3
746 parameters	Δρmin = −0.63 e Å^−3
377 restraints	Absolute structure: Flack (1983), 6579 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.01 (5)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.4538 (4)	0.1607 (11)	0.0813 (11)	0.070 (5)	0.725 (10)
H1A	0.4526	0.2223	0.0470	0.084*	0.725 (10)
C2	0.4318 (4)	0.0836 (11)	0.0546 (12)	0.073 (5)*	0.725 (10)
H2A	0.4152	0.0929	0.0027	0.088*	0.725 (10)
C3	0.4342 (3)	−0.0058 (13)	0.1040 (10)	0.053 (4)*	0.725 (10)
C4	0.4578 (3)	−0.0162 (10)	0.1793 (11)	0.085 (4)*	0.725 (10)
H4A	0.4589	−0.0777	0.2139	0.101*	0.725 (10)
C5	0.4801 (5)	0.0578 (9)	0.2083 (15)	0.074 (6)*	0.725 (10)
H5A	0.4965	0.0478	0.2606	0.089*	0.725 (10)
C6	0.4092 (6)	−0.0898 (17)	0.0766 (17)	0.124 (8)*	0.725 (10)
H6A	0.4141	−0.1478	0.1190	0.185*	0.725 (10)
H6B	0.4120	−0.1073	0.0048	0.185*	0.725 (10)
H6C	0.3857	−0.0679	0.0887	0.185*	0.725 (10)
C7	0.5017 (6)	0.2318 (13)	0.1863 (17)	0.101 (7)*	0.725 (10)
H7A	0.4963	0.2898	0.1445	0.151*	0.725 (10)
H7B	0.5254	0.2116	0.1741	0.151*	0.725 (10)
H7C	0.4987	0.2485	0.2582	0.151*	0.725 (10)
N1	0.4775 (4)	0.1466 (9)	0.1581 (11)	0.069 (4)*	0.725 (10)
C1'	0.4387 (9)	0.1286 (19)	0.048 (2)	0.070 (5)	0.275 (10)
H1'A	0.4306	0.1805	0.0062	0.084*	0.275 (10)
C2'	0.4246 (8)	0.034 (2)	0.040 (2)	0.074 (13)*	0.275 (10)
H2'A	0.4077	0.0204	−0.0094	0.089*	0.275 (10)
C3'	0.4354 (7)	−0.0396 (18)	0.1051 (18)	0.080 (18)*	0.275 (10)
C4'	0.4578 (3)	−0.0162 (10)	0.1793 (11)	0.085 (4)*	0.275 (10)
H4'A	0.4626	−0.0647	0.2295	0.101*	0.275 (10)
C5'	0.4742 (11)	0.0751 (16)	0.187 (3)	0.080 (18)*	0.275 (10)
H5'A	0.4911	0.0875	0.2370	0.096*	0.275 (10)
C6'	0.4224 (13)	−0.146 (3)	0.091 (3)	0.124 (8)*	0.275 (10)
H6'A	0.4330	−0.1893	0.1420	0.185*	0.275 (10)
H6'B	0.4286	−0.1698	0.0227	0.185*	0.275 (10)
H6'C	0.3975	−0.1479	0.0986	0.185*	0.275 (10)
C7'	0.4795 (12)	0.2512 (18)	0.126 (4)	0.101 (7)*	0.275 (10)
H7'A	0.4979	0.2518	0.1765	0.151*	0.275 (10)
H7'B	0.4615	0.2974	0.1462	0.151*	0.275 (10)
H7'C	0.4888	0.2712	0.0596	0.151*	0.275 (10)
N1'	0.4646 (9)	0.1463 (13)	0.118 (2)	0.057 (10)*	0.275 (10)
O2	0.2912 (3)	0.6490 (9)	0.2363 (9)	0.111 (3)
C23	0.2794 (4)	0.5958 (13)	0.3072 (12)	0.111 (3)
H23A	0.2786	0.5266	0.2951	0.133*
N2	0.2684 (3)	0.6260 (12)	0.3939 (11)	0.111 (3)	0.725 (10)
C21	0.2549 (8)	0.5650 (19)	0.475 (2)	0.151 (10)	0.725 (10)
H21A	0.2493	0.4993	0.4483	0.226*	0.725 (10)
H21B	0.2342	0.5957	0.5026	0.226*	0.725 (10)
H21C	0.2721	0.5588	0.5288	0.226*	0.725 (10)
C22	0.2672 (8)	0.7315 (14)	0.402 (3)	0.155 (12)*	0.725 (10)
H22A	0.2745	0.7613	0.3381	0.233*	0.725 (10)
H22B	0.2826	0.7529	0.4569	0.233*	0.725 (10)
H22C	0.2438	0.7524	0.4182	0.233*	0.725 (10)
N2'	0.2684 (3)	0.6260 (12)	0.3939 (11)	0.1109 (14)	0.275 (10)
C21'	0.261 (3)	0.541 (4)	0.459 (6)	0.151 (10)	0.275 (10)
H21D	0.2816	0.4986	0.4624	0.226*	0.275 (10)
H21E	0.2422	0.5029	0.4301	0.226*	0.275 (10)
H21F	0.2552	0.5636	0.5270	0.226*	0.275 (10)
C22'	0.285 (2)	0.710 (4)	0.441 (6)	0.155 (12)*	0.275 (10)
H22D	0.2884	0.7627	0.3910	0.233*	0.275 (10)
H22E	0.3077	0.6893	0.4672	0.233*	0.275 (10)
H22F	0.2713	0.7345	0.4977	0.233*	0.275 (10)
O3	0.3487 (3)	0.4964 (6)	0.1815 (7)	0.086 (2)
C33	0.3471 (4)	0.4051 (9)	0.1787 (11)	0.086 (2)
H33A	0.3649	0.3714	0.2136	0.103*
N3	0.3247 (3)	0.3486 (8)	0.1350 (9)	0.086 (2)	0.725 (10)
C31	0.3233 (7)	0.2408 (12)	0.140 (2)	0.114 (8)*	0.725 (10)
H31A	0.3446	0.2158	0.1701	0.171*	0.725 (10)
H31B	0.3205	0.2136	0.0719	0.171*	0.725 (10)
H31C	0.3040	0.2206	0.1830	0.171*	0.725 (10)
C32	0.2969 (6)	0.3955 (18)	0.077 (2)	0.127 (9)*	0.725 (10)
H32A	0.3019	0.4659	0.0680	0.191*	0.725 (10)
H32B	0.2753	0.3880	0.1140	0.191*	0.725 (10)
H32C	0.2950	0.3637	0.0103	0.191*	0.725 (10)
N3'	0.3247 (3)	0.3486 (8)	0.1350 (9)	0.0861 (9)	0.275 (10)
C31'	0.3452 (18)	0.241 (5)	0.126 (6)	0.114 (8)*	0.275 (10)
H31D	0.3593	0.2311	0.1865	0.171*	0.275 (10)
H31E	0.3598	0.2418	0.0653	0.171*	0.275 (10)
H31F	0.3285	0.1874	0.1201	0.171*	0.275 (10)
C32'	0.3049 (18)	0.344 (6)	0.040 (4)	0.127 (9)*	0.275 (10)
H32D	0.2932	0.4068	0.0292	0.191*	0.275 (10)
H32E	0.2880	0.2904	0.0451	0.191*	0.275 (10)
H32F	0.3204	0.3305	−0.0167	0.191*	0.275 (10)
O4	0.3250 (3)	0.6339 (7)	−0.0222 (8)	0.091 (2)
C43	0.3357 (4)	0.6269 (11)	−0.1123 (10)	0.091 (2)
H43A	0.3418	0.5618	−0.1324	0.109*
N4	0.3397 (3)	0.6924 (8)	−0.1814 (9)	0.091 (2)	0.725 (10)
C41	0.3297 (8)	0.7943 (15)	−0.158 (2)	0.157 (11)*	0.725 (10)
H41A	0.3177	0.7962	−0.0930	0.236*	0.725 (10)
H41B	0.3146	0.8192	−0.2120	0.236*	0.725 (10)
H41C	0.3502	0.8359	−0.1545	0.236*	0.725 (10)
C42	0.3580 (5)	0.6782 (15)	−0.2779 (13)	0.080 (5)*	0.725 (10)
H42A	0.3710	0.6162	−0.2753	0.119*	0.725 (10)
H42B	0.3738	0.7336	−0.2888	0.119*	0.725 (10)
H42C	0.3415	0.6755	−0.3340	0.119*	0.725 (10)
N4'	0.3397 (3)	0.6924 (8)	−0.1814 (9)	0.0912 (10)	0.275 (10)
C41'	0.354 (2)	0.787 (3)	−0.146 (4)	0.157 (11)*	0.275 (10)
H41D	0.3508	0.7920	−0.0721	0.236*	0.275 (10)
H41E	0.3415	0.8415	−0.1792	0.236*	0.275 (10)
H41F	0.3781	0.7904	−0.1628	0.236*	0.275 (10)
C42'	0.3386 (14)	0.679 (4)	−0.2917 (15)	0.080 (5)*	0.275 (10)
H42D	0.3343	0.6089	−0.3072	0.119*	0.275 (10)
H42E	0.3606	0.6985	−0.3212	0.119*	0.275 (10)
H42F	0.3203	0.7193	−0.3206	0.119*	0.275 (10)
O5	0.3969 (2)	0.6563 (7)	0.0661 (9)	0.087 (2)
C53	0.4200 (3)	0.5910 (10)	0.0605 (12)	0.087 (2)
H53A	0.4180	0.5372	0.1065	0.104*
N5	0.4459 (3)	0.5886 (8)	−0.0002 (10)	0.087 (2)	0.725 (10)
C51	0.4725 (6)	0.5125 (15)	−0.007 (2)	0.103 (7)*	0.725 (10)
H51A	0.4693	0.4640	0.0470	0.154*	0.725 (10)
H51B	0.4951	0.5433	−0.0007	0.154*	0.725 (10)
H51C	0.4709	0.4793	−0.0735	0.154*	0.725 (10)
C52	0.4465 (7)	0.6653 (18)	−0.078 (2)	0.128 (10)*	0.725 (10)
H52A	0.4266	0.6575	−0.1229	0.192*	0.725 (10)
H52B	0.4675	0.6592	−0.1185	0.192*	0.725 (10)
H52C	0.4458	0.7305	−0.0460	0.192*	0.725 (10)
N5'	0.4459 (3)	0.5886 (8)	−0.0002 (10)	0.0866 (10)	0.275 (10)
C51'	0.4650 (17)	0.501 (4)	0.037 (6)	0.103 (7)*	0.275 (10)
H51D	0.4666	0.5042	0.1116	0.154*	0.275 (10)
H51E	0.4881	0.5014	0.0082	0.154*	0.275 (10)
H51F	0.4530	0.4409	0.0171	0.154*	0.275 (10)
C52'	0.463 (2)	0.650 (5)	−0.075 (5)	0.128 (10)*	0.275 (10)
H52D	0.4493	0.6526	−0.1374	0.192*	0.275 (10)
H52E	0.4856	0.6223	−0.0906	0.192*	0.275 (10)
H52F	0.4658	0.7173	−0.0481	0.192*	0.275 (10)
O6	0.3701 (3)	0.7275 (7)	0.2864 (7)	0.096 (2)
C63	0.3867 (4)	0.7623 (12)	0.3582 (11)	0.096 (2)
H63A	0.3791	0.8246	0.3826	0.116*
N6	0.4128 (3)	0.7255 (9)	0.4044 (9)	0.096 (2)	0.725 (10)
C61	0.4252 (7)	0.6320 (19)	0.367 (4)	0.100 (8)	0.725 (10)
H61A	0.4105	0.6094	0.3111	0.151*	0.725 (10)
H61B	0.4248	0.5832	0.4218	0.151*	0.725 (10)
H61C	0.4487	0.6400	0.3420	0.151*	0.725 (10)
C62	0.4298 (12)	0.7679 (18)	0.495 (3)	0.101 (9)	0.725 (10)
H62A	0.4501	0.8051	0.4732	0.151*	0.725 (10)
H62B	0.4367	0.7144	0.5405	0.151*	0.725 (10)
H62C	0.4139	0.8122	0.5298	0.151*	0.725 (10)
N6'	0.4128 (3)	0.7255 (9)	0.4044 (9)	0.0964 (9)	0.275 (10)
C61'	0.4353 (19)	0.642 (6)	0.383 (11)	0.100 (8)	0.275 (10)
H61D	0.4257	0.6023	0.3274	0.151*	0.275 (10)
H61E	0.4374	0.6005	0.4439	0.151*	0.275 (10)
H61F	0.4580	0.6662	0.3631	0.151*	0.275 (10)
C62'	0.426 (3)	0.798 (6)	0.478 (9)	0.101 (9)	0.275 (10)
H62D	0.4470	0.8275	0.4518	0.151*	0.275 (10)
H62E	0.4307	0.7646	0.5427	0.151*	0.275 (10)
H62F	0.4088	0.8498	0.4888	0.151*	0.275 (10)
O7	0.3238 (3)	0.8291 (7)	0.1205 (10)	0.103 (3)
C73	0.3132 (4)	0.8889 (10)	0.1840 (14)	0.103 (3)
H73A	0.3265	0.8924	0.2443	0.124*
N7	0.2873 (3)	0.9470 (9)	0.1826 (13)	0.103 (3)	0.725 (10)
C71	0.2764 (8)	0.999 (2)	0.2745 (17)	0.151 (10)*	0.725 (10)
H71A	0.2921	0.9833	0.3302	0.227*	0.725 (10)
H71B	0.2532	0.9771	0.2929	0.227*	0.725 (10)
H71C	0.2764	1.0701	0.2621	0.227*	0.725 (10)
C72	0.2664 (5)	0.9541 (18)	0.0932 (15)	0.113 (8)	0.725 (10)
H72A	0.2781	0.9228	0.0359	0.170*	0.725 (10)
H72B	0.2621	1.0239	0.0775	0.170*	0.725 (10)
H72C	0.2445	0.9206	0.1052	0.170*	0.725 (10)
N7'	0.2873 (3)	0.9470 (9)	0.1826 (13)	0.1033 (8)	0.275 (10)
C71'	0.2675 (14)	0.860 (3)	0.151 (7)	0.151 (10)*	0.275 (10)
H71D	0.2780	0.8005	0.1787	0.227*	0.275 (10)
H71E	0.2673	0.8566	0.0763	0.227*	0.275 (10)
H71F	0.2440	0.8665	0.1758	0.227*	0.275 (10)
C72'	0.2683 (12)	1.040 (2)	0.187 (6)	0.113 (8)	0.275 (10)
H72D	0.2694	1.0734	0.1212	0.170*	0.275 (10)
H72E	0.2785	1.0832	0.2393	0.170*	0.275 (10)
H72F	0.2444	1.0270	0.2049	0.170*	0.275 (10)
Ca1	0.34225 (6)	0.66370 (19)	0.1451 (2)	0.0661 (6)
O11	0.40917 (15)	0.2816 (4)	0.6882 (5)	0.0408 (15)
O12	0.40646 (16)	0.1973 (4)	0.5136 (5)	0.0407 (14)
O13	0.37516 (15)	0.1216 (4)	0.6671 (5)	0.0377 (13)
O14	0.35313 (14)	0.2817 (4)	0.5886 (5)	0.0379 (13)
O21	0.49602 (19)	0.0362 (6)	0.4711 (6)	0.068 (2)
O22	0.3884 (2)	0.3864 (7)	0.9813 (6)	0.073 (2)
O23	0.3747 (2)	0.0473 (6)	0.2557 (6)	0.066 (2)
O24	0.3183 (2)	0.0770 (6)	0.9329 (7)	0.077 (3)
O25	0.4510 (2)	0.3937 (6)	0.3091 (7)	0.069 (2)
O26	0.4357 (2)	−0.1064 (6)	0.7835 (7)	0.077 (2)
O27	0.2782 (2)	0.3976 (7)	0.7824 (7)	0.080 (3)
O28	0.3450 (2)	0.5554 (6)	0.4446 (8)	0.081 (3)
O29	0.4534 (2)	0.5600 (6)	0.6476 (7)	0.075 (2)
O30	0.3164 (2)	−0.1115 (6)	0.5527 (8)	0.073 (2)
O31	0.2699 (2)	0.2061 (6)	0.4052 (8)	0.083 (3)
O32	0.50381 (19)	0.2066 (6)	0.8129 (7)	0.070 (2)
O41	0.46563 (17)	0.2200 (5)	0.4199 (6)	0.0528 (17)
O42	0.42893 (17)	0.0519 (5)	0.3976 (6)	0.0519 (17)
O43	0.47356 (17)	0.1807 (5)	0.6216 (5)	0.0495 (17)
O44	0.43829 (17)	0.0145 (5)	0.6025 (5)	0.0474 (16)
O46	0.37223 (19)	0.2093 (5)	0.8748 (5)	0.0504 (17)
O47	0.43887 (18)	0.2835 (5)	0.8713 (5)	0.0534 (17)
O48	0.35045 (17)	0.3770 (5)	0.7935 (6)	0.0487 (16)
O49	0.41431 (19)	0.4516 (5)	0.7892 (6)	0.0555 (18)
O51	0.34272 (16)	0.1826 (5)	0.3896 (5)	0.0487 (16)
O52	0.40713 (18)	0.2232 (5)	0.3134 (5)	0.0526 (17)
O53	0.36629 (16)	0.0162 (5)	0.4693 (6)	0.0472 (16)
O56	0.32187 (17)	0.0135 (5)	0.7286 (6)	0.0526 (18)
O57	0.38060 (19)	0.0154 (5)	0.8356 (6)	0.0534 (18)
O58	0.31478 (17)	0.2135 (5)	0.7695 (6)	0.0534 (18)
O61	0.38712 (18)	0.3870 (5)	0.4160 (6)	0.0501 (17)
O62	0.44484 (17)	0.3888 (5)	0.5220 (5)	0.0508 (17)
O66	0.37799 (17)	−0.0728 (4)	0.6536 (6)	0.0479 (16)
O67	0.44085 (17)	0.1038 (5)	0.7793 (5)	0.0494 (16)
O71	0.28484 (16)	0.2848 (5)	0.5999 (6)	0.0544 (17)
O72	0.32122 (17)	0.4543 (5)	0.6186 (6)	0.0509 (17)
O76	0.39000 (17)	0.4744 (5)	0.5950 (6)	0.0501 (16)
O77	0.31716 (17)	0.3633 (5)	0.4369 (5)	0.0502 (17)
O81	0.47096 (18)	0.3651 (5)	0.7109 (6)	0.0567 (18)
O86	0.31089 (16)	0.1012 (5)	0.5452 (6)	0.0510 (18)
P1	0.38593 (6)	0.22059 (17)	0.61419 (19)	0.0326 (4)
Mo1	0.45909 (2)	0.09734 (7)	0.50234 (8)	0.0537 (2)
Mo2	0.39290 (2)	0.33640 (7)	0.86142 (8)	0.0530 (2)
Mo3	0.38367 (2)	0.11011 (7)	0.36380 (8)	0.0529 (2)
Mo4	0.34012 (3)	0.10554 (7)	0.82361 (8)	0.0568 (3)
Mo5	0.43216 (3)	0.32239 (7)	0.39998 (8)	0.0521 (2)
Mo6	0.41463 (2)	−0.00554 (7)	0.73405 (8)	0.0551 (2)
Mo7	0.31082 (2)	0.34814 (8)	0.71199 (8)	0.0568 (3)
Mo8	0.35224 (2)	0.44311 (7)	0.49904 (9)	0.0585 (3)
Mo9	0.43310 (3)	0.44847 (7)	0.65662 (8)	0.0577 (3)
Mo10	0.34045 (2)	−0.01011 (6)	0.58749 (8)	0.0522 (2)
Mo11	0.30470 (2)	0.22709 (7)	0.47991 (9)	0.0584 (3)
Mo12	0.46577 (2)	0.22994 (7)	0.75414 (8)	0.0571 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.084 (14)	0.076 (12)	0.051 (12)	0.021 (10)	−0.004 (10)	0.026 (9)
C1'	0.084 (14)	0.076 (12)	0.051 (12)	0.021 (10)	−0.004 (10)	0.026 (9)
O2	0.075 (5)	0.140 (7)	0.117 (8)	−0.003 (5)	0.040 (5)	0.003 (6)
C23	0.075 (5)	0.140 (7)	0.117 (8)	−0.003 (5)	0.040 (5)	0.003 (6)
N2	0.075 (5)	0.140 (7)	0.117 (8)	−0.003 (5)	0.040 (5)	0.003 (6)
C21	0.052 (15)	0.195 (19)	0.21 (2)	0.042 (15)	0.013 (16)	−0.05 (2)
N2'	0.0753 (8)	0.1399 (19)	0.117 (2)	0.00 (2)	0.040 (19)	0.003 (15)
C21'	0.052 (15)	0.195 (19)	0.21 (2)	0.042 (15)	0.013 (16)	−0.05 (2)
O3	0.130 (6)	0.066 (4)	0.062 (4)	−0.002 (4)	0.008 (4)	−0.001 (4)
C33	0.130 (6)	0.066 (4)	0.062 (4)	−0.002 (4)	0.008 (4)	−0.001 (4)
N3	0.130 (6)	0.066 (4)	0.062 (4)	−0.002 (4)	0.008 (4)	−0.001 (4)
N3'	0.1296 (7)	0.0663 (12)	0.062 (2)	−0.0018 (18)	0.0079 (6)	−0.001 (8)
O4	0.119 (6)	0.069 (4)	0.086 (6)	−0.022 (4)	0.011 (5)	−0.008 (4)
C43	0.119 (6)	0.069 (4)	0.086 (6)	−0.022 (4)	0.011 (5)	−0.008 (4)
N4	0.119 (6)	0.069 (4)	0.086 (6)	−0.022 (4)	0.011 (5)	−0.008 (4)
N4'	0.1195 (8)	0.0685 (15)	0.086 (2)	−0.0222 (15)	0.0112 (5)	−0.008 (11)
O5	0.065 (4)	0.077 (5)	0.117 (6)	−0.010 (3)	0.015 (4)	−0.021 (4)
C53	0.065 (4)	0.077 (5)	0.117 (6)	−0.010 (3)	0.015 (4)	−0.021 (4)
N5	0.065 (4)	0.077 (5)	0.117 (6)	−0.010 (3)	0.015 (4)	−0.021 (4)
N5'	0.0655 (6)	0.0773 (15)	0.117 (2)	−0.0104 (18)	0.0149 (7)	−0.021 (7)
O6	0.127 (7)	0.095 (5)	0.068 (5)	−0.019 (5)	−0.014 (4)	−0.009 (4)
C63	0.127 (7)	0.095 (5)	0.068 (5)	−0.019 (5)	−0.014 (4)	−0.009 (4)
N6	0.127 (7)	0.095 (5)	0.068 (5)	−0.019 (5)	−0.014 (4)	−0.009 (4)
C61	0.103 (17)	0.054 (9)	0.144 (19)	−0.021 (12)	0.050 (18)	−0.022 (10)
C62	0.129 (18)	0.084 (19)	0.090 (18)	0.030 (17)	−0.033 (12)	−0.022 (19)
N6'	0.1267 (7)	0.0948 (19)	0.068 (4)	−0.019 (19)	−0.014 (9)	−0.009 (17)
C61'	0.103 (17)	0.054 (9)	0.144 (19)	−0.021 (12)	0.050 (18)	−0.022 (10)
C62'	0.129 (18)	0.084 (19)	0.090 (18)	0.030 (17)	−0.033 (12)	−0.022 (19)
O7	0.093 (5)	0.077 (5)	0.140 (8)	0.016 (4)	0.013 (5)	−0.017 (5)
C73	0.093 (5)	0.077 (5)	0.140 (8)	0.016 (4)	0.013 (5)	−0.017 (5)
N7	0.093 (5)	0.077 (5)	0.140 (8)	0.016 (4)	0.013 (5)	−0.017 (5)
C72	0.101 (16)	0.110 (18)	0.13 (2)	0.003 (13)	0.027 (16)	0.024 (15)
N7'	0.0930 (8)	0.077 (2)	0.1405 (17)	0.0159 (18)	0.0134 (5)	−0.017 (10)
C72'	0.101 (16)	0.110 (18)	0.13 (2)	0.003 (13)	0.027 (16)	0.024 (15)
Ca1	0.0601 (14)	0.0661 (15)	0.0721 (17)	−0.0027 (11)	0.0079 (12)	−0.0057 (13)
O11	0.033 (3)	0.045 (4)	0.045 (4)	0.002 (3)	−0.005 (3)	−0.011 (3)
O12	0.045 (3)	0.038 (3)	0.039 (4)	0.007 (3)	0.005 (3)	−0.004 (3)
O13	0.035 (3)	0.037 (3)	0.041 (4)	0.004 (2)	−0.001 (3)	−0.010 (3)
O14	0.032 (3)	0.039 (3)	0.043 (3)	0.003 (2)	0.001 (3)	−0.011 (3)
O21	0.062 (4)	0.084 (6)	0.059 (5)	0.036 (4)	0.014 (4)	0.000 (4)
O22	0.091 (6)	0.082 (6)	0.046 (5)	−0.020 (4)	0.011 (4)	−0.029 (4)
O23	0.061 (4)	0.079 (5)	0.057 (5)	−0.001 (4)	0.000 (4)	−0.026 (4)
O24	0.103 (7)	0.071 (5)	0.057 (5)	−0.001 (5)	0.037 (5)	0.004 (4)
O25	0.082 (6)	0.062 (5)	0.064 (5)	0.000 (4)	0.028 (4)	0.003 (4)
O26	0.072 (5)	0.069 (5)	0.089 (7)	0.015 (4)	−0.009 (5)	0.026 (5)
O27	0.065 (5)	0.098 (6)	0.077 (6)	0.026 (5)	0.005 (5)	−0.025 (5)
O28	0.085 (6)	0.059 (5)	0.100 (7)	0.014 (4)	0.004 (5)	0.023 (5)
O29	0.086 (6)	0.052 (5)	0.087 (6)	−0.022 (4)	0.003 (5)	−0.012 (4)
O30	0.066 (5)	0.048 (4)	0.107 (7)	−0.020 (4)	−0.003 (5)	−0.015 (4)
O31	0.057 (5)	0.077 (5)	0.113 (8)	0.013 (4)	−0.030 (5)	−0.026 (5)
O32	0.052 (4)	0.080 (5)	0.077 (6)	0.002 (4)	−0.030 (4)	−0.011 (5)
O41	0.043 (4)	0.060 (4)	0.055 (4)	0.005 (3)	0.002 (3)	−0.007 (4)
O42	0.048 (4)	0.060 (4)	0.048 (4)	0.016 (3)	0.003 (3)	−0.004 (3)
O43	0.045 (4)	0.060 (4)	0.044 (4)	−0.001 (3)	−0.003 (3)	−0.009 (3)
O44	0.056 (4)	0.040 (3)	0.046 (4)	0.004 (3)	0.005 (3)	−0.009 (3)
O46	0.070 (4)	0.042 (4)	0.040 (4)	0.001 (3)	0.003 (3)	−0.005 (3)
O47	0.059 (4)	0.056 (4)	0.046 (4)	0.001 (3)	−0.008 (3)	−0.011 (3)
O48	0.045 (4)	0.052 (4)	0.049 (4)	0.001 (3)	0.006 (3)	−0.012 (3)
O49	0.064 (4)	0.038 (4)	0.065 (5)	−0.006 (3)	−0.003 (4)	−0.011 (3)
O51	0.041 (3)	0.053 (4)	0.052 (4)	0.008 (3)	0.001 (3)	−0.010 (3)
O52	0.058 (4)	0.057 (4)	0.043 (4)	0.009 (3)	0.000 (3)	−0.003 (3)
O53	0.045 (3)	0.040 (3)	0.056 (4)	0.002 (3)	0.002 (3)	−0.019 (3)
O56	0.046 (4)	0.044 (4)	0.068 (5)	−0.010 (3)	0.012 (4)	−0.005 (3)
O57	0.060 (4)	0.054 (4)	0.046 (4)	−0.001 (3)	0.000 (3)	0.006 (3)
O58	0.043 (4)	0.055 (4)	0.062 (5)	−0.004 (3)	0.014 (3)	−0.014 (4)
O61	0.058 (4)	0.044 (4)	0.048 (4)	0.009 (3)	−0.005 (3)	0.005 (3)
O62	0.053 (4)	0.050 (4)	0.050 (4)	−0.006 (3)	0.001 (3)	−0.005 (3)
O66	0.056 (4)	0.037 (3)	0.052 (4)	−0.002 (3)	0.004 (3)	−0.013 (3)
O67	0.052 (4)	0.055 (4)	0.042 (4)	0.003 (3)	−0.001 (3)	−0.012 (3)
O71	0.040 (3)	0.061 (4)	0.062 (5)	0.005 (3)	0.001 (3)	−0.017 (4)
O72	0.048 (4)	0.046 (4)	0.058 (5)	0.011 (3)	0.009 (3)	−0.009 (3)
O76	0.055 (4)	0.037 (3)	0.057 (4)	0.002 (3)	0.001 (3)	−0.004 (3)
O77	0.046 (4)	0.059 (4)	0.046 (4)	0.014 (3)	0.001 (3)	−0.004 (3)
O81	0.053 (4)	0.056 (4)	0.062 (5)	−0.015 (3)	−0.006 (4)	−0.004 (4)
O86	0.036 (3)	0.052 (4)	0.066 (5)	−0.006 (3)	0.003 (3)	−0.011 (3)
P1	0.0310 (10)	0.0315 (10)	0.0351 (11)	0.0019 (8)	0.0027 (8)	−0.0062 (9)
Mo1	0.0477 (5)	0.0669 (6)	0.0465 (5)	0.0236 (4)	0.0063 (4)	−0.0017 (5)
Mo2	0.0562 (5)	0.0593 (6)	0.0435 (5)	−0.0078 (4)	0.0025 (4)	−0.0203 (4)
Mo3	0.0525 (5)	0.0628 (6)	0.0434 (5)	−0.0007 (4)	0.0036 (4)	−0.0211 (4)
Mo4	0.0704 (6)	0.0470 (5)	0.0529 (6)	−0.0075 (4)	0.0228 (5)	−0.0055 (4)
Mo5	0.0598 (5)	0.0493 (5)	0.0472 (5)	−0.0006 (4)	0.0153 (4)	0.0003 (4)
Mo6	0.0530 (5)	0.0458 (5)	0.0665 (7)	0.0051 (4)	−0.0007 (5)	0.0107 (4)
Mo7	0.0475 (5)	0.0682 (6)	0.0546 (6)	0.0190 (4)	0.0084 (4)	−0.0118 (5)
Mo8	0.0529 (5)	0.0461 (5)	0.0765 (7)	0.0123 (4)	0.0028 (5)	0.0092 (5)
Mo9	0.0681 (6)	0.0447 (5)	0.0604 (6)	−0.0197 (4)	−0.0015 (5)	−0.0075 (4)
Mo10	0.0550 (5)	0.0412 (5)	0.0604 (6)	−0.0138 (4)	−0.0013 (5)	−0.0105 (4)
Mo11	0.0459 (5)	0.0578 (6)	0.0716 (7)	0.0133 (4)	−0.0185 (5)	−0.0237 (5)
Mo12	0.0428 (5)	0.0623 (6)	0.0662 (6)	0.0047 (4)	−0.0152 (5)	−0.0185 (5)

Geometric parameters (Å, º)

C1—N1	1.355 (8)	N6—C61	1.411 (13)
C1—C2	1.369 (12)	N6—C62	1.445 (13)
C1—H1A	0.9300	C61—H61A	0.9600
C2—C3	1.347 (12)	C61—H61B	0.9600
C2—H2A	0.9300	C61—H61C	0.9600
C3—C4	1.333 (11)	C62—H62A	0.9600
C3—C6	1.51 (2)	C62—H62B	0.9600
C4—C5	1.353 (11)	C62—H62C	0.9600
C4—H4A	0.9300	C61'—H61D	0.9600
C5—N1	1.346 (8)	C61'—H61E	0.9600
C5—H5A	0.9300	C61'—H61F	0.9600
C6—H6A	0.9600	C62'—H62D	0.9600
C6—H6B	0.9600	C62'—H62E	0.9600
C6—H6C	0.9600	C62'—H62F	0.9600
C7—N1	1.50 (2)	O7—C73	1.209 (13)
C7—H7A	0.9600	O7—Ca1	2.324 (10)
C7—H7B	0.9600	C73—N7	1.255 (12)
C7—H7C	0.9600	C73—H73A	0.9300
C1'—N1'	1.354 (8)	N7—C72	1.408 (13)
C1'—C2'	1.370 (13)	N7—C71	1.431 (14)
C1'—H1'A	0.9300	C71—H71A	0.9600
C2'—C3'	1.346 (13)	C71—H71B	0.9600
C2'—H2'A	0.9300	C71—H71C	0.9600
C3'—C6'	1.51 (2)	C72—H72A	0.9600
C5'—N1'	1.349 (8)	C72—H72B	0.9600
C5'—H5'A	0.9300	C72—H72C	0.9600
C6'—H6'A	0.9600	C71'—H71D	0.9600
C6'—H6'B	0.9600	C71'—H71E	0.9600
C6'—H6'C	0.9600	C71'—H71F	0.9600
C7'—N1'	1.51 (2)	C72'—H72D	0.9600
C7'—H7'A	0.9600	C72'—H72E	0.9600
C7'—H7'B	0.9600	C72'—H72F	0.9600
C7'—H7'C	0.9600	O11—P1	1.535 (6)
O2—C23	1.239 (13)	O11—Mo12	2.426 (6)
O2—Ca1	2.289 (10)	O11—Mo9	2.427 (6)
C23—N2	1.259 (13)	O11—Mo2	2.429 (6)
C23—H23A	0.9300	O12—P1	1.547 (7)
N2—C22	1.403 (14)	O12—Mo3	2.413 (6)
N2—C21	1.417 (14)	O12—Mo1	2.416 (6)
C21—H21A	0.9600	O12—Mo5	2.420 (6)
C21—H21B	0.9600	O13—P1	1.534 (6)
C21—H21C	0.9600	O13—Mo6	2.422 (6)
C22—H22A	0.9600	O13—Mo10	2.422 (6)
C22—H22B	0.9600	O13—Mo4	2.432 (6)
C22—H22C	0.9600	O14—P1	1.530 (6)
C21'—H21D	0.9600	O14—Mo8	2.430 (6)
C21'—H21E	0.9600	O14—Mo11	2.434 (6)
C21'—H21F	0.9600	O14—Mo7	2.435 (6)
C22'—H22D	0.9600	O21—Mo1	1.678 (6)
C22'—H22E	0.9600	O22—Mo2	1.690 (7)
C22'—H22F	0.9600	O23—Mo3	1.659 (7)
O3—C33	1.212 (11)	O24—Mo4	1.681 (8)
O3—Ca1	2.278 (9)	O25—Mo5	1.669 (8)
C33—N3	1.271 (12)	O26—Mo6	1.686 (8)
C33—H33A	0.9300	O27—Mo7	1.677 (8)
N3—C31	1.430 (13)	O28—Mo8	1.668 (8)
N3—C32	1.441 (14)	O29—Mo9	1.674 (7)
C31—H31A	0.9600	O30—Mo10	1.689 (7)
C31—H31B	0.9600	O31—Mo11	1.668 (8)
C31—H31C	0.9600	O32—Mo12	1.671 (7)
C32—H32A	0.9600	O41—Mo5	1.884 (7)
C32—H32B	0.9600	O41—Mo1	1.958 (7)
C32—H32C	0.9600	O42—Mo1	1.876 (7)
C31'—H31D	0.9600	O42—Mo3	1.946 (6)
C31'—H31E	0.9600	O43—Mo12	1.853 (7)
C31'—H31F	0.9600	O43—Mo1	1.972 (7)
C32'—H32D	0.9600	O44—Mo1	1.872 (7)
C32'—H32E	0.9600	O44—Mo6	1.941 (7)
C32'—H32F	0.9600	O46—Mo2	1.869 (7)
O4—C43	1.235 (12)	O46—Mo4	1.959 (7)
O4—Ca1	2.289 (11)	O47—Mo2	1.899 (7)
C43—N4	1.253 (12)	O47—Mo12	1.960 (7)
C43—H43A	0.9300	O48—Mo7	1.884 (7)
N4—C41	1.434 (14)	O48—Mo2	1.923 (7)
N4—C42	1.441 (13)	O49—Mo9	1.855 (8)
C41—H41A	0.9600	O49—Mo2	1.966 (7)
C41—H41B	0.9600	O51—Mo3	1.869 (6)
C41—H41C	0.9600	O51—Mo11	1.955 (6)
C42—H42A	0.9600	O52—Mo3	1.864 (7)
C42—H42B	0.9600	O52—Mo5	1.972 (7)
C42—H42C	0.9600	O53—Mo10	1.850 (7)
C41'—H41D	0.9600	O53—Mo3	1.959 (7)
C41'—H41E	0.9600	O56—Mo4	1.864 (7)
C41'—H41F	0.9600	O56—Mo10	1.978 (8)
C42'—H42D	0.9600	O57—Mo6	1.868 (7)
C42'—H42E	0.9600	O57—Mo4	1.963 (7)
C42'—H42F	0.9600	O58—Mo4	1.864 (7)
O5—C53	1.238 (12)	O58—Mo7	1.937 (7)
O5—Ca1	2.329 (9)	O61—Mo8	1.866 (7)
C53—N5	1.266 (12)	O61—Mo5	1.936 (7)
C53—H53A	0.9300	O62—Mo5	1.866 (7)
N5—C52	1.430 (14)	O62—Mo9	1.959 (7)
N5—C51	1.435 (13)	O66—Mo10	1.866 (7)
C51—H51A	0.9600	O66—Mo6	1.959 (7)
C51—H51B	0.9600	O67—Mo6	1.857 (7)
C51—H51C	0.9600	O67—Mo12	1.951 (7)
C52—H52A	0.9600	O71—Mo11	1.885 (7)
C52—H52B	0.9600	O71—Mo7	1.945 (7)
C52—H52C	0.9600	O72—Mo7	1.894 (7)
C51'—H51D	0.9600	O72—Mo8	1.951 (7)
C51'—H51E	0.9600	O76—Mo9	1.863 (7)
C51'—H51F	0.9600	O76—Mo8	1.948 (7)
C52'—H52D	0.9600	O77—Mo8	1.888 (7)
C52'—H52E	0.9600	O77—Mo11	1.947 (7)
C52'—H52F	0.9600	O81—Mo12	1.885 (7)
O6—C63	1.212 (12)	O81—Mo9	1.952 (7)
O6—Ca1	2.275 (10)	O86—Mo11	1.883 (7)
C63—N6	1.262 (13)	O86—Mo10	1.937 (7)
C63—H63A	0.9300
N1—C1—C2	119.6 (14)	Mo3—O12—Mo1	89.5 (2)
N1—C1—H1A	120.2	P1—O12—Mo5	125.3 (3)
C2—C1—H1A	120.2	Mo3—O12—Mo5	89.5 (2)
C3—C2—C1	119.6 (16)	Mo1—O12—Mo5	90.0 (2)
C3—C2—H2A	120.2	P1—O13—Mo6	125.8 (3)
C1—C2—H2A	120.2	P1—O13—Mo10	125.1 (4)
C4—C3—C2	118.8 (15)	Mo6—O13—Mo10	89.55 (18)
C4—C3—C6	121.5 (11)	P1—O13—Mo4	126.3 (3)
C2—C3—C6	119.6 (10)	Mo6—O13—Mo4	89.3 (2)
C3—C4—C5	123.6 (15)	Mo10—O13—Mo4	89.2 (2)
C3—C4—H4A	118.2	P1—O14—Mo8	125.4 (3)
C5—C4—H4A	118.2	P1—O14—Mo11	126.3 (3)
N1—C5—C4	117.0 (15)	Mo8—O14—Mo11	88.7 (2)
N1—C5—H5A	121.5	P1—O14—Mo7	126.6 (4)
C4—C5—H5A	121.5	Mo8—O14—Mo7	89.02 (19)
C3—C6—H6A	109.5	Mo11—O14—Mo7	88.64 (18)
C3—C6—H6B	109.5	Mo5—O41—Mo1	125.8 (4)
H6A—C6—H6B	109.5	Mo1—O42—Mo3	125.6 (4)
C3—C6—H6C	109.5	Mo12—O43—Mo1	150.5 (4)
H6A—C6—H6C	109.5	Mo1—O44—Mo6	151.8 (4)
H6B—C6—H6C	109.5	Mo2—O46—Mo4	150.1 (4)
N1—C7—H7A	109.5	Mo2—O47—Mo12	124.7 (4)
N1—C7—H7B	109.5	Mo7—O48—Mo2	151.3 (4)
H7A—C7—H7B	109.5	Mo9—O49—Mo2	125.5 (3)
N1—C7—H7C	109.5	Mo3—O51—Mo11	152.4 (4)
H7A—C7—H7C	109.5	Mo3—O52—Mo5	124.9 (4)
H7B—C7—H7C	109.5	Mo10—O53—Mo3	150.8 (3)
C5—N1—C1	121.4 (13)	Mo4—O56—Mo10	124.9 (3)
C5—N1—C7	119.6 (9)	Mo6—O57—Mo4	125.9 (4)
C1—N1—C7	119.0 (8)	Mo4—O58—Mo7	152.9 (4)
N1'—C1'—C2'	119.7 (16)	Mo8—O61—Mo5	151.0 (4)
N1'—C1'—H1'A	120.1	Mo5—O62—Mo9	151.3 (4)
C2'—C1'—H1'A	120.1	Mo10—O66—Mo6	126.2 (3)
C3'—C2'—C1'	119.7 (17)	Mo6—O67—Mo12	151.7 (4)
C3'—C2'—H2'A	120.1	Mo11—O71—Mo7	125.3 (3)
C1'—C2'—H2'A	120.1	Mo7—O72—Mo8	125.0 (3)
C2'—C3'—C6'	120.2 (10)	Mo9—O76—Mo8	152.7 (4)
N1'—C5'—H5'A	121.7	Mo8—O77—Mo11	124.9 (4)
C3'—C6'—H6'A	109.5	Mo12—O81—Mo9	124.4 (3)
C3'—C6'—H6'B	109.5	Mo11—O86—Mo10	150.9 (4)
H6'A—C6'—H6'B	109.5	O14—P1—O13	109.1 (3)
C3'—C6'—H6'C	109.5	O14—P1—O11	109.4 (3)
H6'A—C6'—H6'C	109.5	O13—P1—O11	109.2 (4)
H6'B—C6'—H6'C	109.5	O14—P1—O12	110.0 (4)
N1'—C7'—H7'A	109.5	O13—P1—O12	109.8 (3)
N1'—C7'—H7'B	109.5	O11—P1—O12	109.3 (3)
H7'A—C7'—H7'B	109.5	O21—Mo1—O44	103.9 (3)
N1'—C7'—H7'C	109.5	O21—Mo1—O42	101.0 (4)
H7'A—C7'—H7'C	109.5	O44—Mo1—O42	92.6 (3)
H7'B—C7'—H7'C	109.5	O21—Mo1—O41	99.3 (3)
C5'—N1'—C1'	120.9 (14)	O44—Mo1—O41	156.3 (3)
C5'—N1'—C7'	119.7 (10)	O42—Mo1—O41	87.4 (3)
C1'—N1'—C7'	118.9 (9)	O21—Mo1—O43	102.7 (4)
C23—O2—Ca1	137.7 (11)	O44—Mo1—O43	84.9 (3)
O2—C23—N2	126.6 (18)	O42—Mo1—O43	156.0 (3)
O2—C23—H23A	116.7	O41—Mo1—O43	85.6 (3)
N2—C23—H23A	116.7	O21—Mo1—O12	169.0 (3)
C23—N2—C22	113.3 (19)	O44—Mo1—O12	85.7 (2)
C23—N2—C21	126.5 (19)	O42—Mo1—O12	72.9 (2)
C22—N2—C21	119.9 (15)	O41—Mo1—O12	71.6 (2)
N2—C21—H21A	109.5	O43—Mo1—O12	83.1 (2)
N2—C21—H21B	109.5	O22—Mo2—O46	103.0 (4)
H21A—C21—H21B	109.5	O22—Mo2—O47	100.3 (4)
N2—C21—H21C	109.5	O46—Mo2—O47	93.1 (3)
H21A—C21—H21C	109.5	O22—Mo2—O48	102.7 (4)
H21B—C21—H21C	109.5	O46—Mo2—O48	86.3 (3)
N2—C22—H22A	109.5	O47—Mo2—O48	156.5 (3)
N2—C22—H22B	109.5	O22—Mo2—O49	99.9 (4)
H22A—C22—H22B	109.5	O46—Mo2—O49	156.9 (3)
N2—C22—H22C	109.5	O47—Mo2—O49	86.1 (3)
H22A—C22—H22C	109.5	O48—Mo2—O49	85.4 (3)
H22B—C22—H22C	109.5	O22—Mo2—O11	169.7 (3)
H21D—C21'—H21E	109.5	O46—Mo2—O11	85.7 (2)
H21D—C21'—H21F	109.5	O47—Mo2—O11	73.3 (2)
H21E—C21'—H21F	109.5	O48—Mo2—O11	83.2 (2)
H22D—C22'—H22E	109.5	O49—Mo2—O11	71.9 (3)
H22D—C22'—H22F	109.5	O23—Mo3—O52	102.1 (4)
H22E—C22'—H22F	109.5	O23—Mo3—O51	103.5 (3)
C33—O3—Ca1	163.6 (11)	O52—Mo3—O51	93.1 (3)
O3—C33—N3	129.5 (15)	O23—Mo3—O42	100.0 (3)
O3—C33—H33A	115.2	O52—Mo3—O42	88.1 (3)
N3—C33—H33A	115.2	O51—Mo3—O42	155.7 (3)
C33—N3—C31	126.2 (15)	O23—Mo3—O53	101.2 (4)
C33—N3—C32	118.3 (15)	O52—Mo3—O53	156.3 (3)
C31—N3—C32	115.4 (13)	O51—Mo3—O53	85.3 (3)
N3—C31—H31A	109.5	O42—Mo3—O53	84.0 (3)
N3—C31—H31B	109.5	O23—Mo3—O12	170.7 (3)
H31A—C31—H31B	109.5	O52—Mo3—O12	73.7 (3)
N3—C31—H31C	109.5	O51—Mo3—O12	85.1 (2)
H31A—C31—H31C	109.5	O42—Mo3—O12	71.9 (2)
H31B—C31—H31C	109.5	O53—Mo3—O12	82.6 (2)
N3—C32—H32A	109.5	O24—Mo4—O58	103.1 (4)
N3—C32—H32B	109.5	O24—Mo4—O56	102.5 (4)
H32A—C32—H32B	109.5	O58—Mo4—O56	93.5 (3)
N3—C32—H32C	109.5	O24—Mo4—O46	100.8 (4)
H32A—C32—H32C	109.5	O58—Mo4—O46	85.1 (3)
H32B—C32—H32C	109.5	O56—Mo4—O46	156.3 (3)
H31D—C31'—H31E	109.5	O24—Mo4—O57	101.0 (4)
H31D—C31'—H31F	109.5	O58—Mo4—O57	155.1 (3)
H31E—C31'—H31F	109.5	O56—Mo4—O57	87.1 (3)
H32D—C32'—H32E	109.5	O46—Mo4—O57	84.5 (3)
H32D—C32'—H32F	109.5	O24—Mo4—O13	171.5 (3)
H32E—C32'—H32F	109.5	O58—Mo4—O13	84.8 (3)
C43—O4—Ca1	143.5 (11)	O56—Mo4—O13	73.7 (3)
O4—C43—N4	131.0 (15)	O46—Mo4—O13	82.6 (2)
O4—C43—H43A	114.5	O57—Mo4—O13	71.5 (3)
N4—C43—H43A	114.5	O25—Mo5—O62	102.3 (4)
C43—N4—C41	118.2 (16)	O25—Mo5—O41	102.0 (4)
C43—N4—C42	125.6 (14)	O62—Mo5—O41	92.8 (3)
C41—N4—C42	115.5 (13)	O25—Mo5—O61	102.1 (4)
N4—C41—H41A	109.5	O62—Mo5—O61	86.2 (3)
N4—C41—H41B	109.5	O41—Mo5—O61	155.5 (3)
H41A—C41—H41B	109.5	O25—Mo5—O52	100.9 (4)
N4—C41—H41C	109.5	O62—Mo5—O52	156.5 (3)
H41A—C41—H41C	109.5	O41—Mo5—O52	85.9 (3)
H41B—C41—H41C	109.5	O61—Mo5—O52	85.5 (3)
N4—C42—H42A	109.5	O25—Mo5—O12	171.1 (3)
N4—C42—H42B	109.5	O62—Mo5—O12	85.4 (3)
H42A—C42—H42B	109.5	O41—Mo5—O12	72.6 (3)
N4—C42—H42C	109.5	O61—Mo5—O12	82.9 (2)
H42A—C42—H42C	109.5	O52—Mo5—O12	71.9 (3)
H42B—C42—H42C	109.5	O26—Mo6—O67	103.9 (4)
H41D—C41'—H41E	109.5	O26—Mo6—O57	100.8 (4)
H41D—C41'—H41F	109.5	O67—Mo6—O57	92.4 (3)
H41E—C41'—H41F	109.5	O26—Mo6—O44	102.4 (4)
H42D—C42'—H42E	109.5	O67—Mo6—O44	85.1 (3)
H42D—C42'—H42F	109.5	O57—Mo6—O44	156.6 (3)
H42E—C42'—H42F	109.5	O26—Mo6—O66	100.5 (4)
C53—O5—Ca1	134.1 (9)	O67—Mo6—O66	155.3 (3)
O5—C53—N5	127.9 (14)	O57—Mo6—O66	86.5 (3)
O5—C53—H53A	116.1	O44—Mo6—O66	86.2 (3)
N5—C53—H53A	116.1	O26—Mo6—O13	169.9 (3)
C53—N5—C52	115.5 (15)	O67—Mo6—O13	84.6 (3)
C53—N5—C51	127.9 (15)	O57—Mo6—O13	73.2 (3)
C52—N5—C51	116.2 (13)	O44—Mo6—O13	83.4 (2)
N5—C51—H51A	109.5	O66—Mo6—O13	71.4 (2)
N5—C51—H51B	109.5	O27—Mo7—O48	102.7 (4)
H51A—C51—H51B	109.5	O27—Mo7—O72	102.1 (4)
N5—C51—H51C	109.5	O48—Mo7—O72	91.9 (3)
H51A—C51—H51C	109.5	O27—Mo7—O58	102.2 (4)
H51B—C51—H51C	109.5	O48—Mo7—O58	84.9 (3)
N5—C52—H52A	109.5	O72—Mo7—O58	155.6 (3)
N5—C52—H52B	109.5	O27—Mo7—O71	100.9 (4)
H52A—C52—H52B	109.5	O48—Mo7—O71	156.0 (3)
N5—C52—H52C	109.5	O72—Mo7—O71	87.5 (3)
H52A—C52—H52C	109.5	O58—Mo7—O71	85.8 (3)
H52B—C52—H52C	109.5	O27—Mo7—O14	171.9 (4)
H51D—C51'—H51E	109.5	O48—Mo7—O14	84.3 (2)
H51D—C51'—H51F	109.5	O72—Mo7—O14	73.3 (2)
H51E—C51'—H51F	109.5	O58—Mo7—O14	82.2 (2)
H52D—C52'—H52E	109.5	O71—Mo7—O14	72.5 (2)
H52D—C52'—H52F	109.5	O28—Mo8—O61	103.5 (4)
H52E—C52'—H52F	109.5	O28—Mo8—O77	101.6 (4)
C63—O6—Ca1	176.2 (12)	O61—Mo8—O77	92.4 (3)
O6—C63—N6	128.9 (16)	O28—Mo8—O76	101.6 (4)
O6—C63—H63A	115.6	O61—Mo8—O76	85.3 (3)
N6—C63—H63A	115.6	O77—Mo8—O76	156.5 (3)
C63—N6—C61	116.3 (17)	O28—Mo8—O72	99.4 (4)
C63—N6—C62	125.9 (15)	O61—Mo8—O72	156.8 (3)
C61—N6—C62	117.7 (14)	O77—Mo8—O72	86.8 (3)
N6—C61—H61A	109.5	O76—Mo8—O72	86.2 (3)
N6—C61—H61B	109.5	O28—Mo8—O14	170.7 (3)
H61A—C61—H61B	109.5	O61—Mo8—O14	84.9 (2)
N6—C61—H61C	109.5	O77—Mo8—O14	73.7 (3)
H61A—C61—H61C	109.5	O76—Mo8—O14	82.8 (2)
H61B—C61—H61C	109.5	O72—Mo8—O14	72.6 (2)
N6—C62—H62A	109.5	O29—Mo9—O49	103.0 (4)
N6—C62—H62B	109.5	O29—Mo9—O76	102.7 (4)
H62A—C62—H62B	109.5	O49—Mo9—O76	92.6 (3)
N6—C62—H62C	109.5	O29—Mo9—O81	100.3 (4)
H62A—C62—H62C	109.5	O49—Mo9—O81	88.3 (3)
H62B—C62—H62C	109.5	O76—Mo9—O81	156.2 (3)
H61D—C61'—H61E	109.5	O29—Mo9—O62	100.8 (4)
H61D—C61'—H61F	109.5	O49—Mo9—O62	156.1 (3)
H61E—C61'—H61F	109.5	O76—Mo9—O62	84.3 (3)
H62D—C62'—H62E	109.5	O81—Mo9—O62	85.4 (3)
H62D—C62'—H62F	109.5	O29—Mo9—O11	172.3 (4)
H62E—C62'—H62F	109.5	O49—Mo9—O11	73.7 (3)
C73—O7—Ca1	128.8 (11)	O76—Mo9—O11	84.5 (2)
O7—C73—N7	131.1 (18)	O81—Mo9—O11	72.8 (2)
O7—C73—H73A	114.5	O62—Mo9—O11	82.4 (2)
N7—C73—H73A	114.5	O30—Mo10—O53	102.9 (4)
C73—N7—C72	120.2 (17)	O30—Mo10—O66	100.8 (4)
C73—N7—C71	120.8 (19)	O53—Mo10—O66	92.8 (3)
C72—N7—C71	118.6 (13)	O30—Mo10—O86	102.3 (4)
N7—C71—H71A	109.5	O53—Mo10—O86	86.4 (3)
N7—C71—H71B	109.5	O66—Mo10—O86	156.5 (3)
H71A—C71—H71B	109.5	O30—Mo10—O56	100.0 (4)
N7—C71—H71C	109.5	O53—Mo10—O56	156.9 (3)
H71A—C71—H71C	109.5	O66—Mo10—O56	85.8 (3)
H71B—C71—H71C	109.5	O86—Mo10—O56	85.9 (3)
N7—C72—H72A	109.5	O30—Mo10—O13	170.0 (4)
N7—C72—H72B	109.5	O53—Mo10—O13	85.4 (2)
H72A—C72—H72B	109.5	O66—Mo10—O13	72.8 (2)
N7—C72—H72C	109.5	O86—Mo10—O13	83.8 (2)
H72A—C72—H72C	109.5	O56—Mo10—O13	72.2 (2)
H72B—C72—H72C	109.5	O31—Mo11—O86	102.2 (4)
H71D—C71'—H71E	109.5	O31—Mo11—O71	102.6 (4)
H71D—C71'—H71F	109.5	O86—Mo11—O71	92.5 (3)
H71E—C71'—H71F	109.5	O31—Mo11—O77	100.7 (4)
H72D—C72'—H72E	109.5	O86—Mo11—O77	156.5 (3)
H72D—C72'—H72F	109.5	O71—Mo11—O77	87.5 (3)
H72E—C72'—H72F	109.5	O31—Mo11—O51	101.6 (4)
O6—Ca1—O3	98.4 (4)	O86—Mo11—O51	84.6 (3)
O6—Ca1—O2	91.2 (4)	O71—Mo11—O51	155.7 (3)
O3—Ca1—O2	84.5 (4)	O77—Mo11—O51	85.8 (3)
O6—Ca1—O4	162.5 (4)	O31—Mo11—O14	172.2 (3)
O3—Ca1—O4	93.3 (3)	O86—Mo11—O14	84.8 (2)
O2—Ca1—O4	102.9 (4)	O71—Mo11—O14	73.4 (2)
O6—Ca1—O7	84.4 (4)	O77—Mo11—O14	72.7 (2)
O3—Ca1—O7	168.0 (4)	O51—Mo11—O14	82.2 (2)
O2—Ca1—O7	83.7 (4)	O32—Mo12—O43	102.3 (4)
O4—Ca1—O7	86.9 (4)	O32—Mo12—O81	102.6 (4)
O6—Ca1—O5	86.8 (4)	O43—Mo12—O81	92.5 (3)
O3—Ca1—O5	87.2 (4)	O32—Mo12—O67	101.1 (4)
O2—Ca1—O5	171.1 (4)	O43—Mo12—O67	86.0 (3)
O4—Ca1—O5	80.8 (4)	O81—Mo12—O67	156.0 (3)
O7—Ca1—O5	104.7 (4)	O32—Mo12—O47	100.1 (4)
P1—O11—Mo12	126.0 (3)	O43—Mo12—O47	157.2 (3)
P1—O11—Mo9	126.5 (4)	O81—Mo12—O47	86.5 (3)
Mo12—O11—Mo9	88.76 (19)	O67—Mo12—O47	85.7 (3)
P1—O11—Mo2	125.4 (3)	O32—Mo12—O11	171.8 (3)
Mo12—O11—Mo2	89.5 (2)	O43—Mo12—O11	85.4 (3)
Mo9—O11—Mo2	88.79 (19)	O81—Mo12—O11	73.9 (3)
P1—O12—Mo3	125.6 (3)	O67—Mo12—O11	82.1 (2)
P1—O12—Mo1	125.7 (4)	O47—Mo12—O11	72.5 (2)
N1—C1—C2—C3	−0.9 (13)	Mo3—O52—Mo5—O12	−1.4 (3)
C1—C2—C3—C4	1.1 (15)	P1—O12—Mo5—O62	40.3 (4)
C1—C2—C3—C6	178.4 (14)	Mo3—O12—Mo5—O62	175.2 (3)
C2—C3—C4—C5	−1 (2)	Mo1—O12—Mo5—O62	−95.3 (3)
C6—C3—C4—C5	−178.3 (18)	P1—O12—Mo5—O41	134.6 (5)
C3—C4—C5—N1	1 (3)	Mo3—O12—Mo5—O41	−90.4 (3)
C4—C5—N1—C1	−1 (3)	Mo1—O12—Mo5—O41	−0.9 (3)
C4—C5—N1—C7	−179.7 (17)	P1—O12—Mo5—O61	−46.5 (4)
C2—C1—N1—C5	1 (2)	Mo3—O12—Mo5—O61	88.5 (3)
C2—C1—N1—C7	179.7 (13)	Mo1—O12—Mo5—O61	178.0 (3)
N1'—C1'—C2'—C3'	3 (2)	P1—O12—Mo5—O52	−134.1 (5)
C1'—C2'—C3'—C6'	−174 (2)	Mo3—O12—Mo5—O52	0.9 (2)
C2'—C1'—N1'—C5'	−7 (5)	Mo1—O12—Mo5—O52	90.4 (3)
C2'—C1'—N1'—C7'	−179 (2)	Mo12—O67—Mo6—O26	129.9 (8)
Ca1—O2—C23—N2	120.4 (18)	Mo12—O67—Mo6—O57	−128.3 (8)
O2—C23—N2—C22	6 (3)	Mo12—O67—Mo6—O44	28.3 (8)
O2—C23—N2—C21	−180 (2)	Mo12—O67—Mo6—O66	−41.6 (13)
Ca1—O3—C33—N3	−23 (5)	Mo12—O67—Mo6—O13	−55.5 (8)
O3—C33—N3—C31	−176 (2)	Mo4—O57—Mo6—O26	−168.7 (5)
O3—C33—N3—C32	2 (3)	Mo4—O57—Mo6—O67	86.7 (5)
Ca1—O4—C43—N4	−88 (3)	Mo4—O57—Mo6—O44	3.4 (11)
O4—C43—N4—C41	−2 (3)	Mo4—O57—Mo6—O66	−68.6 (5)
O4—C43—N4—C42	168.4 (18)	Mo4—O57—Mo6—O13	3.0 (4)
Ca1—O5—C53—N5	165.9 (11)	Mo1—O44—Mo6—O26	−135.9 (9)
O5—C53—N5—C52	−7 (3)	Mo1—O44—Mo6—O67	−32.7 (8)
O5—C53—N5—C51	−179.3 (19)	Mo1—O44—Mo6—O57	52.0 (13)
O6—C63—N6—C61	1 (3)	Mo1—O44—Mo6—O66	124.1 (8)
O6—C63—N6—C62	−175 (3)	Mo1—O44—Mo6—O13	52.4 (8)
Ca1—O7—C73—N7	−134.1 (17)	Mo10—O66—Mo6—O26	172.4 (5)
O7—C73—N7—C72	−4 (3)	Mo10—O66—Mo6—O67	−15.9 (10)
O7—C73—N7—C71	169 (2)	Mo10—O66—Mo6—O57	72.1 (5)
C33—O3—Ca1—O6	176 (4)	Mo10—O66—Mo6—O44	−85.6 (5)
C33—O3—Ca1—O2	85 (4)	Mo10—O66—Mo6—O13	−1.3 (4)
C33—O3—Ca1—O4	−17 (4)	P1—O13—Mo6—O26	−172 (2)
C33—O3—Ca1—O7	74 (4)	Mo10—O13—Mo6—O26	−37 (2)
C33—O3—Ca1—O5	−98 (4)	Mo4—O13—Mo6—O26	52 (2)
C23—O2—Ca1—O6	−70.6 (18)	P1—O13—Mo6—O67	40.1 (4)
C23—O2—Ca1—O3	27.7 (17)	Mo10—O13—Mo6—O67	174.8 (3)
C23—O2—Ca1—O4	119.8 (17)	Mo4—O13—Mo6—O67	−96.1 (3)
C23—O2—Ca1—O7	−154.8 (18)	P1—O13—Mo6—O57	134.2 (5)
C43—O4—Ca1—O6	38 (2)	Mo10—O13—Mo6—O57	−91.1 (3)
C43—O4—Ca1—O3	−93.7 (17)	Mo4—O13—Mo6—O57	−2.0 (3)
C43—O4—Ca1—O2	−178.8 (16)	P1—O13—Mo6—O44	−45.6 (4)
C43—O4—Ca1—O7	98.3 (17)	Mo10—O13—Mo6—O44	89.0 (2)
C43—O4—Ca1—O5	−7.1 (16)	Mo4—O13—Mo6—O44	178.2 (2)
C73—O7—Ca1—O6	−43.0 (14)	P1—O13—Mo6—O66	−133.8 (5)
C73—O7—Ca1—O3	61 (3)	Mo10—O13—Mo6—O66	0.8 (2)
C73—O7—Ca1—O2	48.8 (14)	Mo4—O13—Mo6—O66	90.0 (3)
C73—O7—Ca1—O4	152.1 (14)	Mo2—O48—Mo7—O27	129.9 (9)
C73—O7—Ca1—O5	−128.2 (13)	Mo2—O48—Mo7—O72	−127.2 (8)
C53—O5—Ca1—O6	90.9 (14)	Mo2—O48—Mo7—O58	28.5 (8)
C53—O5—Ca1—O3	−7.7 (14)	Mo2—O48—Mo7—O71	−39.0 (14)
C53—O5—Ca1—O4	−101.5 (14)	Mo2—O48—Mo7—O14	−54.1 (8)
C53—O5—Ca1—O7	174.2 (13)	Mo8—O72—Mo7—O27	−170.4 (5)
Mo8—O14—P1—O13	−177.8 (4)	Mo8—O72—Mo7—O48	86.2 (5)
Mo11—O14—P1—O13	−58.6 (5)	Mo8—O72—Mo7—O58	4.3 (10)
Mo7—O14—P1—O13	62.0 (5)	Mo8—O72—Mo7—O71	−69.8 (4)
Mo8—O14—P1—O11	62.7 (5)	Mo8—O72—Mo7—O14	2.7 (4)
Mo11—O14—P1—O11	−178.0 (4)	Mo4—O58—Mo7—O27	−131.9 (9)
Mo7—O14—P1—O11	−57.4 (5)	Mo4—O58—Mo7—O48	−30.1 (9)
Mo8—O14—P1—O12	−57.3 (5)	Mo4—O58—Mo7—O72	53.4 (14)
Mo11—O14—P1—O12	61.9 (5)	Mo4—O58—Mo7—O71	127.8 (9)
Mo7—O14—P1—O12	−177.5 (3)	Mo4—O58—Mo7—O14	54.9 (9)
Mo6—O13—P1—O14	−177.2 (4)	Mo11—O71—Mo7—O27	171.8 (5)
Mo10—O13—P1—O14	63.2 (5)	Mo11—O71—Mo7—O48	−19.2 (11)
Mo4—O13—P1—O14	−56.4 (5)	Mo11—O71—Mo7—O72	69.9 (5)
Mo6—O13—P1—O11	−57.7 (5)	Mo11—O71—Mo7—O58	−86.6 (5)
Mo10—O13—P1—O11	−177.3 (3)	Mo11—O71—Mo7—O14	−3.4 (4)
Mo4—O13—P1—O11	63.1 (5)	P1—O14—Mo7—O48	39.7 (4)
Mo6—O13—P1—O12	62.2 (5)	Mo8—O14—Mo7—O48	−95.5 (3)
Mo10—O13—P1—O12	−57.4 (5)	Mo11—O14—Mo7—O48	175.8 (3)
Mo4—O13—P1—O12	−177.0 (4)	P1—O14—Mo7—O72	133.4 (5)
Mo12—O11—P1—O14	−177.9 (4)	Mo8—O14—Mo7—O72	−1.8 (2)
Mo9—O11—P1—O14	−57.7 (5)	Mo11—O14—Mo7—O72	−90.5 (3)
Mo2—O11—P1—O14	61.9 (5)	P1—O14—Mo7—O58	−45.9 (4)
Mo12—O11—P1—O13	62.7 (5)	Mo8—O14—Mo7—O58	178.9 (3)
Mo9—O11—P1—O13	−177.1 (3)	Mo11—O14—Mo7—O58	90.2 (3)
Mo2—O11—P1—O13	−57.5 (5)	P1—O14—Mo7—O71	−133.9 (5)
Mo12—O11—P1—O12	−57.5 (5)	Mo8—O14—Mo7—O71	90.9 (3)
Mo9—O11—P1—O12	62.7 (5)	Mo11—O14—Mo7—O71	2.1 (3)
Mo2—O11—P1—O12	−177.7 (3)	Mo5—O61—Mo8—O28	128.6 (8)
Mo3—O12—P1—O14	−57.1 (5)	Mo5—O61—Mo8—O77	−128.8 (8)
Mo1—O12—P1—O14	−177.2 (3)	Mo5—O61—Mo8—O76	27.7 (8)
Mo5—O12—P1—O14	62.4 (5)	Mo5—O61—Mo8—O72	−41.2 (13)
Mo3—O12—P1—O13	62.9 (5)	Mo5—O61—Mo8—O14	−55.5 (8)
Mo1—O12—P1—O13	−57.1 (5)	Mo11—O77—Mo8—O28	−169.5 (5)
Mo5—O12—P1—O13	−177.6 (4)	Mo11—O77—Mo8—O61	86.2 (4)
Mo3—O12—P1—O11	−177.2 (3)	Mo11—O77—Mo8—O76	2.4 (10)
Mo1—O12—P1—O11	62.8 (5)	Mo11—O77—Mo8—O72	−70.6 (4)
Mo5—O12—P1—O11	−57.7 (5)	Mo11—O77—Mo8—O14	2.2 (3)
Mo6—O44—Mo1—O21	135.0 (8)	Mo9—O76—Mo8—O28	−134.2 (9)
Mo6—O44—Mo1—O42	−123.0 (8)	Mo9—O76—Mo8—O61	−31.3 (9)
Mo6—O44—Mo1—O41	−33.5 (14)	Mo9—O76—Mo8—O77	53.9 (14)
Mo6—O44—Mo1—O43	33.1 (8)	Mo9—O76—Mo8—O72	127.0 (9)
Mo6—O44—Mo1—O12	−50.4 (8)	Mo9—O76—Mo8—O14	54.1 (9)
Mo3—O42—Mo1—O21	−166.6 (5)	Mo7—O72—Mo8—O28	172.4 (5)
Mo3—O42—Mo1—O44	88.6 (5)	Mo7—O72—Mo8—O61	−17.7 (11)
Mo3—O42—Mo1—O41	−67.6 (5)	Mo7—O72—Mo8—O77	71.2 (5)
Mo3—O42—Mo1—O43	5.3 (11)	Mo7—O72—Mo8—O76	−86.4 (5)
Mo3—O42—Mo1—O12	3.9 (4)	Mo7—O72—Mo8—O14	−2.7 (4)
Mo5—O41—Mo1—O21	172.1 (5)	P1—O14—Mo8—O61	39.8 (5)
Mo5—O41—Mo1—O44	−19.2 (10)	Mo11—O14—Mo8—O61	−95.5 (3)
Mo5—O41—Mo1—O42	71.4 (5)	Mo7—O14—Mo8—O61	175.9 (3)
Mo5—O41—Mo1—O43	−85.7 (5)	P1—O14—Mo8—O77	133.9 (5)
Mo5—O41—Mo1—O12	−1.4 (4)	Mo11—O14—Mo8—O77	−1.4 (2)
Mo12—O43—Mo1—O21	−134.2 (8)	Mo7—O14—Mo8—O77	−90.1 (2)
Mo12—O43—Mo1—O44	−31.0 (8)	P1—O14—Mo8—O76	−46.0 (4)
Mo12—O43—Mo1—O42	53.9 (13)	Mo11—O14—Mo8—O76	178.7 (3)
Mo12—O43—Mo1—O41	127.2 (8)	Mo7—O14—Mo8—O76	90.0 (3)
Mo12—O43—Mo1—O12	55.2 (8)	P1—O14—Mo8—O72	−134.3 (5)
P1—O12—Mo1—O21	−169.7 (17)	Mo11—O14—Mo8—O72	90.4 (3)
Mo3—O12—Mo1—O21	55.0 (18)	Mo7—O14—Mo8—O72	1.7 (2)
Mo5—O12—Mo1—O21	−34.4 (18)	Mo2—O49—Mo9—O29	−169.9 (5)
P1—O12—Mo1—O44	38.6 (4)	Mo2—O49—Mo9—O76	86.4 (5)
Mo3—O12—Mo1—O44	−96.7 (3)	Mo2—O49—Mo9—O81	−69.8 (5)
Mo5—O12—Mo1—O44	173.8 (3)	Mo2—O49—Mo9—O62	4.8 (11)
P1—O12—Mo1—O42	132.7 (5)	Mo2—O49—Mo9—O11	2.9 (4)
Mo3—O12—Mo1—O42	−2.6 (3)	Mo8—O76—Mo9—O29	131.1 (9)
Mo5—O12—Mo1—O42	−92.1 (3)	Mo8—O76—Mo9—O49	−124.9 (9)
P1—O12—Mo1—O41	−134.4 (5)	Mo8—O76—Mo9—O81	−33.3 (15)
Mo3—O12—Mo1—O41	90.4 (3)	Mo8—O76—Mo9—O62	31.3 (9)
Mo5—O12—Mo1—O41	0.9 (2)	Mo8—O76—Mo9—O11	−51.6 (9)
P1—O12—Mo1—O43	−46.8 (4)	Mo12—O81—Mo9—O29	173.4 (5)
Mo3—O12—Mo1—O43	178.0 (3)	Mo12—O81—Mo9—O49	70.5 (5)
Mo5—O12—Mo1—O43	88.5 (3)	Mo12—O81—Mo9—O76	−22.1 (11)
Mo4—O46—Mo2—O22	131.8 (8)	Mo12—O81—Mo9—O62	−86.5 (5)
Mo4—O46—Mo2—O47	−126.9 (8)	Mo12—O81—Mo9—O11	−3.0 (4)
Mo4—O46—Mo2—O48	29.5 (8)	Mo5—O62—Mo9—O29	−131.7 (8)
Mo4—O46—Mo2—O49	−39.8 (13)	Mo5—O62—Mo9—O49	53.5 (13)
Mo4—O46—Mo2—O11	−53.9 (8)	Mo5—O62—Mo9—O76	−29.9 (8)
Mo12—O47—Mo2—O22	−170.6 (5)	Mo5—O62—Mo9—O81	128.6 (9)
Mo12—O47—Mo2—O46	85.6 (4)	Mo5—O62—Mo9—O11	55.4 (8)
Mo12—O47—Mo2—O48	−2.3 (10)	P1—O11—Mo9—O49	133.0 (5)
Mo12—O47—Mo2—O49	−71.2 (4)	Mo12—O11—Mo9—O49	−91.4 (3)
Mo12—O47—Mo2—O11	1.1 (4)	Mo2—O11—Mo9—O49	−1.9 (3)
Mo7—O48—Mo2—O22	−132.0 (9)	P1—O11—Mo9—O76	38.7 (4)
Mo7—O48—Mo2—O46	−29.5 (8)	Mo12—O11—Mo9—O76	174.3 (3)
Mo7—O48—Mo2—O47	59.8 (13)	Mo2—O11—Mo9—O76	−96.2 (3)
Mo7—O48—Mo2—O49	128.9 (9)	P1—O11—Mo9—O81	−133.7 (5)
Mo7—O48—Mo2—O11	56.6 (8)	Mo12—O11—Mo9—O81	1.9 (3)
Mo9—O49—Mo2—O22	170.6 (5)	Mo2—O11—Mo9—O81	91.4 (3)
Mo9—O49—Mo2—O46	−17.8 (11)	P1—O11—Mo9—O62	−46.2 (4)
Mo9—O49—Mo2—O47	70.9 (5)	Mo12—O11—Mo9—O62	89.4 (2)
Mo9—O49—Mo2—O48	−87.2 (5)	Mo2—O11—Mo9—O62	178.9 (3)
Mo9—O49—Mo2—O11	−2.9 (4)	Mo3—O53—Mo10—O30	130.9 (8)
P1—O11—Mo2—O22	−172.2 (19)	Mo3—O53—Mo10—O66	−127.4 (8)
Mo12—O11—Mo2—O22	52 (2)	Mo3—O53—Mo10—O86	29.1 (8)
Mo9—O11—Mo2—O22	−37 (2)	Mo3—O53—Mo10—O56	−41.6 (13)
P1—O11—Mo2—O46	40.4 (4)	Mo3—O53—Mo10—O13	−54.9 (8)
Mo12—O11—Mo2—O46	−95.2 (3)	Mo6—O66—Mo10—O30	−170.7 (5)
Mo9—O11—Mo2—O46	176.0 (3)	Mo6—O66—Mo10—O53	85.6 (5)
P1—O11—Mo2—O47	134.9 (5)	Mo6—O66—Mo10—O86	−1.7 (10)
Mo12—O11—Mo2—O47	−0.7 (2)	Mo6—O66—Mo10—O56	−71.3 (4)
Mo9—O11—Mo2—O47	−89.5 (3)	Mo6—O66—Mo10—O13	1.3 (4)
P1—O11—Mo2—O48	−46.5 (4)	Mo11—O86—Mo10—O30	−134.1 (9)
Mo12—O11—Mo2—O48	177.9 (3)	Mo11—O86—Mo10—O53	−31.8 (9)
Mo9—O11—Mo2—O48	89.2 (2)	Mo11—O86—Mo10—O66	56.9 (13)
P1—O11—Mo2—O49	−133.8 (5)	Mo11—O86—Mo10—O56	126.5 (9)
Mo12—O11—Mo2—O49	90.6 (3)	Mo11—O86—Mo10—O13	54.0 (8)
Mo9—O11—Mo2—O49	1.8 (2)	Mo4—O56—Mo10—O30	172.0 (5)
Mo5—O52—Mo3—O23	−170.0 (4)	Mo4—O56—Mo10—O53	−15.5 (10)
Mo5—O52—Mo3—O51	85.4 (4)	Mo4—O56—Mo10—O66	71.8 (4)
Mo5—O52—Mo3—O42	−70.3 (4)	Mo4—O56—Mo10—O86	−86.3 (4)
Mo5—O52—Mo3—O53	0.2 (10)	Mo4—O56—Mo10—O13	−1.5 (4)
Mo5—O52—Mo3—O12	1.4 (3)	P1—O13—Mo10—O30	−174.4 (17)
Mo11—O51—Mo3—O23	130.1 (8)	Mo6—O13—Mo10—O30	50.5 (19)
Mo11—O51—Mo3—O52	−126.6 (8)	Mo4—O13—Mo10—O30	−38.9 (19)
Mo11—O51—Mo3—O42	−34.4 (13)	P1—O13—Mo10—O53	40.0 (4)
Mo11—O51—Mo3—O53	29.7 (8)	Mo6—O13—Mo10—O53	−95.2 (2)
Mo11—O51—Mo3—O12	−53.3 (8)	Mo4—O13—Mo10—O53	175.5 (2)
Mo1—O42—Mo3—O23	171.5 (5)	P1—O13—Mo10—O66	134.3 (4)
Mo1—O42—Mo3—O52	69.5 (5)	Mo6—O13—Mo10—O66	−0.9 (2)
Mo1—O42—Mo3—O51	−23.8 (10)	Mo4—O13—Mo10—O66	−90.2 (3)
Mo1—O42—Mo3—O53	−88.2 (5)	P1—O13—Mo10—O86	−46.9 (4)
Mo1—O42—Mo3—O12	−4.0 (4)	Mo6—O13—Mo10—O86	177.9 (3)
Mo10—O53—Mo3—O23	−131.5 (8)	Mo4—O13—Mo10—O86	88.6 (3)
Mo10—O53—Mo3—O52	58.2 (12)	P1—O13—Mo10—O56	−134.6 (4)
Mo10—O53—Mo3—O51	−28.6 (8)	Mo6—O13—Mo10—O56	90.3 (3)
Mo10—O53—Mo3—O42	129.5 (8)	Mo4—O13—Mo10—O56	1.0 (2)
Mo10—O53—Mo3—O12	57.1 (8)	Mo10—O86—Mo11—O31	132.0 (9)
P1—O12—Mo3—O52	133.8 (5)	Mo10—O86—Mo11—O71	−124.6 (9)
Mo1—O12—Mo3—O52	−90.9 (3)	Mo10—O86—Mo11—O77	−35.1 (14)
Mo5—O12—Mo3—O52	−0.9 (2)	Mo10—O86—Mo11—O51	31.2 (8)
P1—O12—Mo3—O51	39.1 (4)	Mo10—O86—Mo11—O14	−51.5 (8)
Mo1—O12—Mo3—O51	174.4 (3)	Mo7—O71—Mo11—O31	−169.7 (5)
Mo5—O12—Mo3—O51	−95.6 (3)	Mo7—O71—Mo11—O86	87.2 (5)
P1—O12—Mo3—O42	−132.8 (5)	Mo7—O71—Mo11—O77	−69.3 (5)
Mo1—O12—Mo3—O42	2.5 (2)	Mo7—O71—Mo11—O51	5.0 (11)
Mo5—O12—Mo3—O42	92.5 (3)	Mo7—O71—Mo11—O14	3.4 (4)
P1—O12—Mo3—O53	−46.7 (4)	Mo8—O77—Mo11—O31	173.6 (5)
Mo1—O12—Mo3—O53	88.6 (2)	Mo8—O77—Mo11—O86	−19.3 (10)
Mo5—O12—Mo3—O53	178.6 (2)	Mo8—O77—Mo11—O71	71.2 (4)
Mo7—O58—Mo4—O24	130.2 (9)	Mo8—O77—Mo11—O51	−85.3 (4)
Mo7—O58—Mo4—O56	−126.0 (9)	Mo8—O77—Mo11—O14	−2.2 (3)
Mo7—O58—Mo4—O46	30.3 (9)	Mo3—O51—Mo11—O31	−132.0 (8)
Mo7—O58—Mo4—O57	−35.3 (14)	Mo3—O51—Mo11—O86	−30.7 (8)
Mo7—O58—Mo4—O13	−52.8 (9)	Mo3—O51—Mo11—O71	53.2 (13)
Mo10—O56—Mo4—O24	−170.7 (5)	Mo3—O51—Mo11—O77	127.9 (8)
Mo10—O56—Mo4—O58	85.0 (5)	Mo3—O51—Mo11—O14	54.8 (8)
Mo10—O56—Mo4—O46	−0.7 (10)	P1—O14—Mo11—O86	40.0 (5)
Mo10—O56—Mo4—O57	−70.1 (4)	Mo8—O14—Mo11—O86	174.6 (3)
Mo10—O56—Mo4—O13	1.5 (4)	Mo7—O14—Mo11—O86	−96.3 (3)
Mo2—O46—Mo4—O24	−132.1 (8)	P1—O14—Mo11—O71	134.1 (5)
Mo2—O46—Mo4—O58	−29.6 (8)	Mo8—O14—Mo11—O71	−91.2 (3)
Mo2—O46—Mo4—O56	57.9 (12)	Mo7—O14—Mo11—O71	−2.2 (3)
Mo2—O46—Mo4—O57	127.8 (8)	P1—O14—Mo11—O77	−133.3 (5)
Mo2—O46—Mo4—O13	55.8 (8)	Mo8—O14—Mo11—O77	1.4 (2)
Mo6—O57—Mo4—O24	173.0 (5)	Mo7—O14—Mo11—O77	90.4 (2)
Mo6—O57—Mo4—O58	−21.4 (10)	P1—O14—Mo11—O51	−45.2 (5)
Mo6—O57—Mo4—O56	70.8 (5)	Mo8—O14—Mo11—O51	89.4 (2)
Mo6—O57—Mo4—O46	−87.0 (5)	Mo7—O14—Mo11—O51	178.5 (3)
Mo6—O57—Mo4—O13	−3.0 (4)	Mo1—O43—Mo12—O32	130.1 (8)
P1—O13—Mo4—O58	38.4 (4)	Mo1—O43—Mo12—O81	−126.5 (8)
Mo6—O13—Mo4—O58	174.2 (3)	Mo1—O43—Mo12—O67	29.6 (8)
Mo10—O13—Mo4—O58	−96.2 (3)	Mo1—O43—Mo12—O47	−39.3 (14)
P1—O13—Mo4—O56	133.6 (5)	Mo1—O43—Mo12—O11	−52.8 (8)
Mo6—O13—Mo4—O56	−90.6 (3)	Mo9—O81—Mo12—O32	−169.4 (5)
Mo10—O13—Mo4—O56	−1.0 (2)	Mo9—O81—Mo12—O43	87.4 (5)
P1—O13—Mo4—O46	−47.3 (4)	Mo9—O81—Mo12—O67	1.5 (11)
Mo6—O13—Mo4—O46	88.5 (2)	Mo9—O81—Mo12—O47	−69.8 (5)
Mo10—O13—Mo4—O46	178.1 (2)	Mo9—O81—Mo12—O11	3.0 (4)
P1—O13—Mo4—O57	−133.9 (5)	Mo6—O67—Mo12—O32	−130.2 (8)
Mo6—O13—Mo4—O57	1.9 (2)	Mo6—O67—Mo12—O43	−28.4 (8)
Mo10—O13—Mo4—O57	91.4 (3)	Mo6—O67—Mo12—O81	58.9 (12)
Mo9—O62—Mo5—O25	130.8 (9)	Mo6—O67—Mo12—O47	130.3 (8)
Mo9—O62—Mo5—O41	−126.2 (8)	Mo6—O67—Mo12—O11	57.5 (8)
Mo9—O62—Mo5—O61	29.2 (8)	Mo2—O47—Mo12—O32	175.3 (5)
Mo9—O62—Mo5—O52	−40.2 (13)	Mo2—O47—Mo12—O43	−15.2 (10)
Mo9—O62—Mo5—O12	−53.9 (8)	Mo2—O47—Mo12—O81	73.1 (5)
Mo1—O41—Mo5—O25	−171.2 (5)	Mo2—O47—Mo12—O67	−84.2 (4)
Mo1—O41—Mo5—O62	85.7 (5)	Mo2—O47—Mo12—O11	−1.1 (4)
Mo1—O41—Mo5—O61	−1.1 (10)	P1—O11—Mo12—O43	40.0 (5)
Mo1—O41—Mo5—O52	−70.8 (5)	Mo9—O11—Mo12—O43	−96.0 (3)
Mo1—O41—Mo5—O12	1.4 (4)	Mo2—O11—Mo12—O43	175.3 (3)
Mo8—O61—Mo5—O25	−129.8 (8)	P1—O11—Mo12—O81	134.0 (5)
Mo8—O61—Mo5—O62	−28.1 (8)	Mo9—O11—Mo12—O81	−2.0 (3)
Mo8—O61—Mo5—O41	60.2 (12)	Mo2—O11—Mo12—O81	−90.8 (3)
Mo8—O61—Mo5—O52	130.0 (8)	P1—O11—Mo12—O67	−46.6 (5)
Mo8—O61—Mo5—O12	57.7 (8)	Mo9—O11—Mo12—O67	177.4 (3)
Mo3—O52—Mo5—O25	173.2 (4)	Mo2—O11—Mo12—O67	88.6 (3)
Mo3—O52—Mo5—O62	−15.8 (10)	P1—O11—Mo12—O47	−134.6 (5)
Mo3—O52—Mo5—O41	71.7 (4)	Mo9—O11—Mo12—O47	89.5 (3)
Mo3—O52—Mo5—O61	−85.3 (4)	Mo2—O11—Mo12—O47	0.7 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···O32^i	0.93	2.57	3.390 (3)	148
C4—H4′A···O32^i	0.93	2.52	3.390 (3)	156
C7—H7B···O26^i	0.96	2.48	3.176 (8)	129
C51—H51B···O62^ii	0.96	2.49	3.446 (6)	176
C53—O5···C6′^iii	1.24 (1)	2.81 (1)	3.501 (7)	114 (1)

Symmetry codes: (i) −x+1, −y, z−1/2; (ii) −x+1, −y+1, z−1/2; (iii) x, y+1, z.