Two new POM-based compounds modified by lanthanide–Schiff base complexes with inter­esting NLO properties

Two POM-based lanthanide derivatives, namely {tri­aqua­[2,6-di­acetyl­pyridine bis­(semicarbazone)-κ⁵O,N,N′,N′′,O′]terbium(III)}-μ-oxido-[tricosa-μ₂-oxido-do­deca­oxido-μ₁₂-phosphato-dodeca­molybdenum(VI)] penta­hydrate (1), [Tb(C₁₁H₁₅N₇O₂)(H₂O)₃][PMo₁₂O₄₀]·5H₂O, and the dysprosium(III) analogue (2), have been isolated successfully by the reaction of Keggin–POM [PMo₁₂O₄₀]³⁻ (abbreviated as PMo₁₂), the Ln³⁺ ion and the Schiff base 2,6-di­acetyl­pyridine bis­(semicarbazone) (DAPSC) ligand under hydro­thermal conditions. [Ln(DAPSC)(H₂O)₃][PMo₁₂O₄₀]·5H₂O is a PMo₁₂-supported cluster featuring a lanthanide–Schiff base complex [denoted Ln–L(Schiff base)]. Single-crystal X-ray diffraction analysis reveals that the Ln^III ion is in a distorted tricapped trigonal prismatic arrangement, coordinated by six O atoms and three N atoms. Two O atoms and three N atoms are provided by one DAPSC ligand, while the additional O atoms originate from a PMo₁₂ cluster and three water mol­ecules. Hydrogen-bonding inter­actions between adjacent clusters form an inter­esting three-dimensional supra­molecular structure. The identities of 1 and 2 were characterized by IR spectroscopy, thermogravimetric analysis and powder X-ray diffraction. Inter­estingly, both compounds possess excellent two-photon absorption (TPA) responses to the third-order nonlinear optics (NLO) (2264 GM for 1 and 941 GM for 2), suggesting that they have potential applications in the field of nonlinear optics (NLO). To our knowledge, 1 and 2 are the first POM-based Ln–L(Schiff base) complexes showing excellent two-photon responses. Meanwhile, the electrochemical properties of both com­pounds were studied in detail.

Computing details

For both structures, data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005). Program(s) used to solve structure: SHELXT (Sheldrick, 2015a) for a-1; SHELXTL (Sheldrick, 2015a) for a-2. For both structures, program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

{Triaqua[2,6-diacetylpyridine bis(semicarbazone)-κ⁵O,N,N',N'',O']terbium(III)}-µ-oxido-[tricosa-µ₂-oxido-dodecaoxido-µ₁₂-phosphato-dodecamolybdenum(VI)] pentahydrate (a-1)

Crystal data

[Tb(C11H15N7O2)(H2O)3][PMo12O40]·5H2O	Z = 2
Mr = 2402.60	F(000) = 2260
Triclinic, P1	Dx = 3.111 Mg m^−3
a = 11.594 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 15.198 (5) Å	Cell parameters from 9457 reflections
c = 15.292 (5) Å	θ = 2.3–27.1°
α = 80.195 (3)°	µ = 4.34 mm^−1
β = 87.940 (4)°	T = 173 K
γ = 75.052 (4)°	Block-shaped, black
V = 2565.0 (13) Å^3	0.15 × 0.13 × 0.12 mm

Data collection

Bruker APEXII CCD diffractometer	8029 reflections with I > 2σ(I)
ω scans	Rint = 0.034
Absorption correction: multi-scan (SADABS; Bruker, 2005)	θmax = 25.5°, θmin = 1.4°
Tmin = 0.562, Tmax = 0.624	h = −14→12
18755 measured reflections	k = −18→18
9401 independent reflections	l = −18→18

Refinement

Refinement on F^2	34 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.030	H-atom parameters constrained
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0337P)^2 + 1.851P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max = 0.001
9401 reflections	Δρmax = 1.73 e Å^−3
749 parameters	Δρmin = −1.18 e Å^−3

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Tb1	0.24235 (2)	0.31771 (2)	0.13996 (2)	0.01610 (7)
Mo1	0.02511 (5)	0.86482 (4)	0.13377 (3)	0.02522 (12)
Mo2	0.14232 (4)	0.79672 (3)	0.53572 (3)	0.01715 (11)
Mo3	0.48896 (4)	0.84752 (3)	0.33192 (3)	0.01865 (11)
Mo4	0.41951 (4)	0.66265 (3)	0.50268 (3)	0.02055 (12)
Mo5	0.29596 (4)	0.94781 (3)	0.15949 (3)	0.01873 (11)
Mo6	0.21585 (4)	0.98195 (3)	0.37341 (3)	0.01795 (11)
Mo7	0.26099 (4)	0.54721 (3)	0.24152 (3)	0.02024 (11)
Mo8	0.33006 (5)	0.71965 (3)	0.09525 (3)	0.02248 (12)
Mo9	−0.03779 (4)	0.69491 (3)	0.29094 (3)	0.02058 (12)
Mo10	0.16666 (4)	0.58495 (3)	0.47871 (3)	0.01916 (11)
Mo11	−0.06060 (4)	0.90572 (4)	0.34628 (3)	0.02335 (12)
Mo12	0.51216 (4)	0.61611 (3)	0.27706 (3)	0.02329 (12)
P1	0.23022 (11)	0.76313 (8)	0.31379 (8)	0.0116 (3)
O1	0.2371 (3)	0.7198 (2)	0.4126 (2)	0.0149 (7)
O2	0.3002 (3)	0.6918 (2)	0.2578 (2)	0.0146 (7)
O3	0.0996 (3)	0.7937 (2)	0.2840 (2)	0.0151 (8)
O4	0.4646 (3)	0.7639 (2)	0.4379 (2)	0.0191 (8)
O5	0.2844 (3)	0.8462 (2)	0.2998 (2)	0.0128 (7)
O6	0.0351 (3)	0.6388 (3)	0.4007 (2)	0.0201 (8)
O7	0.3892 (3)	0.9461 (2)	0.3805 (2)	0.0184 (8)
O8	0.5280 (3)	0.7344 (3)	0.2807 (2)	0.0219 (8)
O9	0.2856 (3)	0.6025 (3)	0.1262 (2)	0.0214 (8)
O10	0.1014 (3)	0.6137 (2)	0.2398 (2)	0.0202 (8)
O11	0.4771 (3)	0.6034 (2)	0.3978 (2)	0.0206 (8)
O12	0.4549 (3)	0.9139 (2)	0.2156 (2)	0.0212 (8)
O13	0.2480 (3)	0.5331 (3)	0.3745 (2)	0.0239 (9)
O14	0.2442 (3)	1.0241 (2)	0.2457 (2)	0.0206 (8)
O15	0.4807 (3)	0.6536 (2)	0.1481 (2)	0.0227 (9)
O16	0.1848 (3)	1.0823 (2)	0.4109 (2)	0.0226 (9)
O17	0.2059 (3)	0.8971 (3)	0.4731 (2)	0.0189 (8)
O18	0.1127 (3)	0.6762 (2)	0.5528 (2)	0.0173 (8)
O19	0.0364 (3)	0.3871 (3)	0.1578 (2)	0.0249 (9)
O20	0.3179 (4)	1.0231 (3)	0.0708 (3)	0.0291 (10)
O21	0.1447 (3)	0.9357 (3)	0.1417 (2)	0.0219 (8)
O22	0.6246 (3)	0.8604 (3)	0.3516 (3)	0.0262 (9)
O23	0.1271 (4)	0.4954 (3)	0.5392 (3)	0.0282 (9)
O24	0.2378 (3)	0.2855 (3)	−0.0072 (2)	0.0260 (9)
O25	−0.0694 (3)	0.9406 (3)	0.2137 (3)	0.0248 (9)
O26	0.0633 (3)	0.9758 (2)	0.3352 (2)	0.0212 (8)
O27	0.3565 (4)	0.7206 (3)	−0.0137 (3)	0.0302 (10)
O28	0.2516 (4)	0.4424 (3)	0.2229 (3)	0.0243 (9)
O29	0.0125 (3)	0.8461 (2)	0.4559 (2)	0.0183 (8)
O30	0.1626 (3)	0.7777 (3)	0.0967 (2)	0.0231 (9)
O31	0.4275 (3)	0.5224 (2)	0.2641 (2)	0.0194 (8)
O32	0.0896 (4)	0.8326 (3)	0.6305 (2)	0.0253 (9)
O33	0.3558 (3)	0.8321 (3)	0.1126 (2)	0.0216 (8)
O34	0.3296 (3)	0.5670 (2)	0.5241 (2)	0.0213 (8)
O35	−0.1818 (4)	0.9819 (3)	0.3755 (3)	0.0324 (10)
O36	−0.1210 (3)	0.8046 (3)	0.3333 (2)	0.0221 (8)
O37	−0.0514 (3)	0.7719 (3)	0.1705 (2)	0.0248 (9)
O38	0.5353 (4)	0.6154 (3)	0.5736 (3)	0.0295 (10)
O39	−0.1474 (4)	0.6432 (3)	0.2824 (3)	0.0315 (10)
O40	0.3093 (3)	0.7323 (2)	0.5709 (2)	0.0196 (8)
O41	0.6531 (3)	0.5520 (3)	0.2748 (3)	0.0309 (10)
O42	−0.0414 (4)	0.9147 (3)	0.0358 (3)	0.0355 (11)
N1	−0.1267 (5)	0.4343 (4)	0.2398 (4)	0.0442 (16)
H1A	−0.1708	0.4590	0.1935	0.053*
H1B	−0.1568	0.4365	0.2919	0.053*
N2	0.0517 (4)	0.3561 (3)	0.3079 (3)	0.0246 (11)
H2A	0.0219	0.3653	0.3589	0.030*
N3	0.1653 (4)	0.3043 (3)	0.2985 (3)	0.0194 (10)
N4	0.3784 (4)	0.2078 (3)	0.2624 (3)	0.0172 (9)
N5	0.4149 (4)	0.1899 (3)	0.0962 (3)	0.0177 (10)
N6	0.4201 (4)	0.1855 (3)	0.0072 (3)	0.0191 (10)
H6C	0.4825	0.1540	−0.0161	0.023*
N7	0.3241 (5)	0.2201 (4)	−0.1251 (3)	0.0344 (13)
H7A	0.2642	0.2486	−0.1595	0.041*
H7B	0.3847	0.1832	−0.1450	0.041*
C1	0.3229 (5)	0.2329 (4)	−0.0416 (3)	0.0213 (12)
C2	0.5003 (5)	0.1392 (4)	0.1470 (3)	0.0178 (11)
C3	0.4814 (5)	0.1483 (4)	0.2427 (3)	0.0182 (11)
C4	0.5607 (5)	0.0964 (4)	0.3077 (4)	0.0257 (13)
H6B	0.6322	0.0582	0.2922	0.031*
C5	0.5351 (6)	0.1004 (4)	0.3955 (4)	0.0313 (15)
H5A	0.5891	0.0657	0.4397	0.038*
C6	0.4274 (5)	0.1573 (4)	0.4175 (4)	0.0270 (13)
H6A	0.4066	0.1591	0.4766	0.032*
C7	0.3504 (5)	0.2119 (4)	0.3489 (3)	0.0173 (11)
C8	0.2318 (5)	0.2712 (4)	0.3671 (3)	0.0187 (12)
C9	−0.0113 (5)	0.3923 (4)	0.2308 (4)	0.0227 (12)
C10	0.6094 (5)	0.0735 (4)	0.1191 (4)	0.0298 (14)
H10A	0.6594	0.0441	0.1700	0.045*
H10B	0.5865	0.0276	0.0927	0.045*
H10C	0.6526	0.1068	0.0766	0.045*
C11	0.1978 (6)	0.2857 (4)	0.4604 (4)	0.0279 (14)
H11A	0.2634	0.2536	0.4998	0.042*
H11B	0.1788	0.3505	0.4632	0.042*
H11C	0.1295	0.2623	0.4777	0.042*
O1W	0.4127 (4)	0.3750 (3)	0.0936 (3)	0.0446 (13)
H1WA	0.4235	0.4034	0.1323	0.067*
H1WB	0.4679	0.3327	0.0831	0.067*
O2W	0.1500 (4)	0.1961 (3)	0.1589 (3)	0.0316 (10)
H2WA	0.1712	0.1439	0.1892	0.047*
H2WB	0.1134	0.1997	0.1131	0.047*
O3W	0.1740 (4)	0.4580 (3)	0.0338 (3)	0.0351 (11)
H3WA	0.1113	0.4973	0.0361	0.053*
H3WB	0.2293	0.4782	0.0100	0.053*
O4W	0.0164 (4)	0.6230 (3)	0.0497 (3)	0.0484 (13)
H4WA	0.0706	0.6433	0.0735	0.073*
H4WB	−0.0083	0.6044	0.1041	0.073*
O5W	0.2386 (7)	0.7966 (6)	0.7880 (5)	0.056 (2)	0.689 (9)
H5WB	0.1713	0.8329	0.7667	0.084*	0.689 (9)
H5WA	0.2547	0.7662	0.7444	0.084*	0.689 (9)
O5WA	0.1319 (19)	0.8749 (13)	0.8022 (12)	0.070 (4)	0.311 (9)
H5WC	0.0608	0.8695	0.8050	0.105*	0.311 (9)
H5WD	0.1825	0.8258	0.7957	0.105*	0.311 (9)
O6W	−0.3488 (6)	0.5016 (4)	0.0809 (4)	0.079 (2)
H6WA	−0.4246	0.5284	0.0674	0.119*
H6WB	−0.3438	0.5348	0.1209	0.119*
O7W	−0.0673 (6)	0.2361 (5)	0.0811 (4)	0.090 (2)
H7WA	−0.0642	0.1878	0.0546	0.135*
H7WB	−0.1185	0.2729	0.0420	0.135*
O8W	0.5957 (6)	0.3574 (5)	0.2083 (5)	0.087 (2)
H8WC	0.5852	0.4199	0.1946	0.131*
H8WD	0.5332	0.3744	0.2458	0.131*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Tb1	0.01623 (15)	0.01465 (14)	0.01679 (13)	−0.00304 (11)	0.00386 (10)	−0.00305 (10)
Mo1	0.0210 (3)	0.0320 (3)	0.0204 (2)	−0.0073 (2)	−0.0068 (2)	0.0040 (2)
Mo2	0.0198 (3)	0.0151 (2)	0.0152 (2)	−0.00216 (19)	0.00415 (19)	−0.00338 (18)
Mo3	0.0138 (3)	0.0191 (3)	0.0227 (2)	−0.0034 (2)	0.00200 (19)	−0.00409 (19)
Mo4	0.0151 (3)	0.0218 (3)	0.0206 (2)	−0.0003 (2)	−0.0038 (2)	0.00197 (19)
Mo5	0.0260 (3)	0.0145 (2)	0.0159 (2)	−0.0071 (2)	0.0029 (2)	−0.00067 (18)
Mo6	0.0216 (3)	0.0122 (2)	0.0194 (2)	−0.0025 (2)	0.0050 (2)	−0.00465 (18)
Mo7	0.0204 (3)	0.0137 (2)	0.0289 (3)	−0.0065 (2)	0.0064 (2)	−0.00764 (19)
Mo8	0.0314 (3)	0.0197 (3)	0.0186 (2)	−0.0095 (2)	0.0075 (2)	−0.00628 (19)
Mo9	0.0135 (3)	0.0228 (3)	0.0268 (3)	−0.0069 (2)	−0.0003 (2)	−0.0045 (2)
Mo10	0.0250 (3)	0.0154 (2)	0.0180 (2)	−0.0080 (2)	0.0040 (2)	−0.00183 (18)
Mo11	0.0122 (3)	0.0254 (3)	0.0297 (3)	0.0042 (2)	−0.0020 (2)	−0.0103 (2)
Mo12	0.0125 (3)	0.0202 (3)	0.0373 (3)	0.0005 (2)	0.0028 (2)	−0.0129 (2)
P1	0.0104 (7)	0.0106 (7)	0.0131 (6)	−0.0015 (5)	0.0013 (5)	−0.0022 (5)
O1	0.0112 (19)	0.0154 (18)	0.0160 (17)	0.0003 (15)	0.0006 (14)	−0.0024 (14)
O2	0.0128 (19)	0.0124 (18)	0.0175 (17)	−0.0013 (15)	0.0018 (15)	−0.0028 (14)
O3	0.0117 (19)	0.0142 (18)	0.0180 (18)	−0.0009 (15)	−0.0029 (15)	−0.0012 (14)
O4	0.016 (2)	0.020 (2)	0.0194 (18)	−0.0030 (16)	0.0033 (15)	−0.0041 (15)
O5	0.0096 (19)	0.0138 (18)	0.0146 (17)	−0.0024 (14)	0.0019 (14)	−0.0025 (14)
O6	0.018 (2)	0.024 (2)	0.0217 (19)	−0.0102 (17)	0.0051 (16)	−0.0092 (16)
O7	0.017 (2)	0.019 (2)	0.0204 (18)	−0.0051 (16)	0.0050 (16)	−0.0068 (15)
O8	0.019 (2)	0.022 (2)	0.0229 (19)	−0.0037 (17)	0.0081 (16)	−0.0053 (16)
O9	0.020 (2)	0.022 (2)	0.024 (2)	−0.0088 (17)	0.0067 (16)	−0.0066 (16)
O10	0.016 (2)	0.021 (2)	0.0247 (19)	−0.0053 (16)	0.0012 (16)	−0.0070 (16)
O11	0.017 (2)	0.0140 (19)	0.028 (2)	−0.0011 (16)	0.0001 (16)	0.0001 (16)
O12	0.023 (2)	0.019 (2)	0.0221 (19)	−0.0090 (17)	0.0072 (16)	−0.0028 (15)
O13	0.028 (2)	0.021 (2)	0.024 (2)	−0.0103 (18)	0.0083 (17)	−0.0049 (16)
O14	0.024 (2)	0.0144 (19)	0.0221 (19)	−0.0037 (16)	0.0021 (16)	−0.0009 (15)
O15	0.023 (2)	0.019 (2)	0.028 (2)	−0.0062 (17)	0.0132 (17)	−0.0095 (16)
O16	0.025 (2)	0.015 (2)	0.027 (2)	−0.0039 (17)	0.0123 (17)	−0.0071 (16)
O17	0.018 (2)	0.022 (2)	0.0180 (18)	−0.0055 (16)	0.0034 (15)	−0.0078 (15)
O18	0.019 (2)	0.0154 (19)	0.0170 (18)	−0.0032 (15)	0.0081 (15)	−0.0034 (14)
O19	0.016 (2)	0.026 (2)	0.026 (2)	0.0029 (17)	0.0046 (17)	0.0002 (16)
O20	0.042 (3)	0.022 (2)	0.024 (2)	−0.0130 (19)	0.0017 (19)	−0.0003 (17)
O21	0.026 (2)	0.018 (2)	0.0192 (19)	−0.0035 (17)	−0.0015 (16)	−0.0007 (15)
O22	0.017 (2)	0.026 (2)	0.035 (2)	−0.0057 (18)	0.0022 (18)	−0.0057 (18)
O23	0.033 (3)	0.021 (2)	0.030 (2)	−0.0105 (19)	0.0053 (18)	0.0001 (17)
O24	0.023 (2)	0.030 (2)	0.022 (2)	0.0023 (18)	−0.0032 (17)	−0.0109 (17)
O25	0.015 (2)	0.025 (2)	0.029 (2)	0.0023 (17)	−0.0069 (17)	−0.0008 (17)
O26	0.015 (2)	0.018 (2)	0.028 (2)	0.0012 (16)	0.0005 (16)	−0.0045 (16)
O27	0.039 (3)	0.031 (2)	0.025 (2)	−0.016 (2)	0.0079 (19)	−0.0072 (18)
O28	0.028 (2)	0.019 (2)	0.029 (2)	−0.0086 (17)	0.0088 (18)	−0.0085 (16)
O29	0.0089 (19)	0.022 (2)	0.0236 (19)	−0.0032 (16)	0.0031 (15)	−0.0043 (15)
O30	0.023 (2)	0.025 (2)	0.0218 (19)	−0.0083 (18)	0.0009 (17)	−0.0038 (16)
O31	0.018 (2)	0.0133 (19)	0.027 (2)	−0.0028 (16)	0.0064 (16)	−0.0066 (15)
O32	0.031 (2)	0.023 (2)	0.0209 (19)	−0.0033 (18)	0.0084 (17)	−0.0091 (16)
O33	0.021 (2)	0.020 (2)	0.025 (2)	−0.0070 (17)	0.0058 (16)	−0.0056 (16)
O34	0.018 (2)	0.017 (2)	0.0231 (19)	0.0017 (16)	−0.0030 (16)	0.0028 (15)
O35	0.019 (2)	0.033 (3)	0.041 (2)	0.0070 (19)	−0.0016 (19)	−0.013 (2)
O36	0.010 (2)	0.027 (2)	0.026 (2)	0.0003 (16)	−0.0003 (16)	−0.0033 (16)
O37	0.018 (2)	0.030 (2)	0.025 (2)	−0.0029 (17)	−0.0099 (17)	−0.0034 (17)
O38	0.022 (2)	0.030 (2)	0.031 (2)	−0.0045 (18)	−0.0065 (18)	0.0052 (18)
O39	0.021 (2)	0.036 (3)	0.041 (2)	−0.0117 (19)	−0.0029 (19)	−0.008 (2)
O40	0.022 (2)	0.020 (2)	0.0168 (18)	−0.0052 (16)	−0.0009 (16)	−0.0023 (15)
O41	0.014 (2)	0.028 (2)	0.050 (3)	0.0008 (18)	0.0028 (19)	−0.016 (2)
O42	0.040 (3)	0.037 (3)	0.030 (2)	−0.015 (2)	−0.013 (2)	0.0050 (19)
N1	0.024 (3)	0.056 (4)	0.037 (3)	0.015 (3)	0.004 (2)	−0.002 (3)
N2	0.018 (3)	0.031 (3)	0.022 (2)	0.000 (2)	0.011 (2)	−0.007 (2)
N3	0.015 (3)	0.017 (2)	0.024 (2)	−0.0035 (19)	0.004 (2)	0.0032 (19)
N4	0.013 (2)	0.018 (2)	0.020 (2)	−0.0001 (19)	−0.0006 (18)	−0.0057 (18)
N5	0.015 (2)	0.021 (2)	0.017 (2)	−0.0031 (19)	0.0025 (19)	−0.0039 (18)
N6	0.018 (3)	0.025 (3)	0.016 (2)	−0.004 (2)	0.0061 (19)	−0.0084 (18)
N7	0.019 (3)	0.062 (4)	0.019 (2)	0.000 (3)	0.000 (2)	−0.015 (2)
C1	0.019 (3)	0.026 (3)	0.020 (3)	−0.005 (2)	0.007 (2)	−0.008 (2)
C2	0.014 (3)	0.019 (3)	0.022 (3)	−0.005 (2)	0.002 (2)	−0.005 (2)
C3	0.014 (3)	0.020 (3)	0.020 (3)	−0.003 (2)	0.000 (2)	−0.005 (2)
C4	0.018 (3)	0.027 (3)	0.029 (3)	−0.001 (3)	−0.001 (2)	−0.007 (2)
C5	0.028 (4)	0.036 (4)	0.026 (3)	−0.004 (3)	−0.005 (3)	0.001 (3)
C6	0.028 (4)	0.034 (4)	0.021 (3)	−0.010 (3)	0.002 (3)	−0.010 (2)
C7	0.019 (3)	0.018 (3)	0.017 (3)	−0.010 (2)	−0.002 (2)	−0.002 (2)
C8	0.022 (3)	0.019 (3)	0.019 (3)	−0.011 (2)	0.009 (2)	−0.005 (2)
C9	0.017 (3)	0.022 (3)	0.027 (3)	−0.001 (2)	0.007 (2)	−0.007 (2)
C10	0.023 (3)	0.032 (3)	0.029 (3)	0.003 (3)	0.003 (3)	−0.006 (3)
C11	0.030 (4)	0.034 (4)	0.024 (3)	−0.012 (3)	0.005 (3)	−0.011 (3)
O1W	0.038 (3)	0.034 (3)	0.072 (3)	−0.019 (2)	0.031 (3)	−0.030 (2)
O2W	0.029 (3)	0.021 (2)	0.044 (3)	−0.0088 (19)	−0.004 (2)	0.0021 (18)
O3W	0.039 (3)	0.021 (2)	0.036 (2)	0.0029 (19)	0.009 (2)	0.0033 (18)
O4W	0.043 (3)	0.057 (3)	0.038 (3)	0.010 (3)	−0.014 (2)	−0.021 (2)
O5W	0.058 (5)	0.062 (5)	0.042 (4)	−0.009 (4)	−0.009 (4)	−0.004 (4)
O5WA	0.094 (9)	0.055 (8)	0.060 (8)	−0.017 (7)	−0.010 (7)	−0.008 (7)
O6W	0.096 (5)	0.069 (4)	0.078 (4)	−0.029 (4)	0.052 (4)	−0.026 (3)
O7W	0.078 (5)	0.157 (7)	0.059 (4)	−0.061 (5)	−0.010 (3)	−0.034 (4)
O8W	0.069 (4)	0.071 (4)	0.136 (6)	−0.034 (4)	0.012 (4)	−0.035 (4)

Geometric parameters (Å, º)

Tb1—O2W	2.336 (4)	Mo11—O35	1.675 (4)
Tb1—O19	2.374 (4)	Mo11—O29	1.880 (4)
Tb1—O24	2.388 (4)	Mo11—O36	1.887 (4)
Tb1—O1W	2.395 (4)	Mo11—O26	1.984 (4)
Tb1—O3W	2.418 (4)	Mo11—O25	2.006 (4)
Tb1—O28	2.479 (4)	Mo11—O3	2.459 (3)
Tb1—N3	2.547 (4)	Mo12—O41	1.675 (4)
Tb1—N5	2.562 (4)	Mo12—O8	1.864 (4)
Tb1—N4	2.563 (4)	Mo12—O11	1.865 (4)
Mo1—O42	1.676 (4)	Mo12—O31	1.965 (4)
Mo1—O37	1.854 (4)	Mo12—O15	1.976 (4)
Mo1—O30	1.928 (4)	Mo12—O2	2.435 (3)
Mo1—O25	1.938 (4)	P1—O3	1.527 (4)
Mo1—O21	1.981 (4)	P1—O5	1.530 (3)
Mo1—O3	2.450 (3)	P1—O1	1.537 (3)
Mo2—O32	1.675 (4)	P1—O2	1.543 (3)
Mo2—O29	1.886 (4)	O19—C9	1.234 (6)
Mo2—O18	1.923 (4)	O24—C1	1.262 (6)
Mo2—O17	1.954 (4)	N1—C9	1.339 (7)
Mo2—O40	1.978 (4)	N1—H1A	0.8600
Mo2—O1	2.461 (3)	N1—H1B	0.8600
Mo3—O22	1.678 (4)	N2—C9	1.363 (7)
Mo3—O7	1.886 (4)	N2—N3	1.366 (6)
Mo3—O12	1.890 (4)	N2—H2A	0.8600
Mo3—O4	1.943 (4)	N3—C8	1.275 (7)
Mo3—O8	1.950 (4)	N4—C7	1.358 (6)
Mo3—O5	2.445 (3)	N4—C3	1.358 (7)
Mo4—O38	1.684 (4)	N5—C2	1.279 (7)
Mo4—O40	1.850 (4)	N5—N6	1.371 (6)
Mo4—O4	1.865 (4)	N6—C1	1.344 (7)
Mo4—O34	1.975 (4)	N6—H6C	0.8600
Mo4—O11	1.983 (4)	N7—C1	1.323 (7)
Mo4—O1	2.445 (3)	N7—H7A	0.8600
Mo5—O20	1.677 (4)	N7—H7B	0.8600
Mo5—O21	1.844 (4)	C2—C10	1.494 (7)
Mo5—O14	1.884 (4)	C2—C3	1.497 (7)
Mo5—O33	1.962 (4)	C3—C4	1.371 (8)
Mo5—O12	1.967 (4)	C4—C5	1.374 (8)
Mo5—O5	2.442 (3)	C4—H6B	0.9300
Mo6—O16	1.668 (4)	C5—C6	1.389 (8)
Mo6—O17	1.842 (4)	C5—H5A	0.9300
Mo6—O26	1.912 (4)	C6—C7	1.406 (8)
Mo6—O7	1.943 (4)	C6—H6A	0.9300
Mo6—O14	1.992 (4)	C7—C8	1.483 (8)
Mo6—O5	2.457 (3)	C8—C11	1.504 (7)
Mo7—O28	1.696 (4)	C10—H10A	0.9600
Mo7—O10	1.864 (4)	C10—H10B	0.9600
Mo7—O9	1.866 (4)	C10—H10C	0.9600
Mo7—O31	1.902 (4)	C11—H11A	0.9600
Mo7—O13	2.013 (4)	C11—H11B	0.9600
Mo7—O2	2.409 (3)	C11—H11C	0.9600
Mo8—O27	1.682 (4)	O1W—H1WA	0.8195
Mo8—O33	1.872 (4)	O1W—H1WB	0.8153
Mo8—O15	1.906 (4)	O2W—H2WA	0.8292
Mo8—O30	1.915 (4)	O2W—H2WB	0.8185
Mo8—O9	1.957 (4)	O3W—H3WA	0.8176
Mo8—O2	2.476 (3)	O3W—H3WB	0.8276
Mo9—O39	1.676 (4)	O4W—H4WA	0.8813
Mo9—O6	1.871 (4)	O4W—H4WB	0.8933
Mo9—O36	1.903 (4)	O5W—H5WB	0.8689
Mo9—O10	1.987 (4)	O5W—H5WA	0.8633
Mo9—O37	1.994 (4)	O5WA—H5WC	0.8478
Mo9—O3	2.443 (3)	O5WA—H5WD	0.8405
Mo10—O23	1.667 (4)	O6W—H6WA	0.8834
Mo10—O6	1.890 (4)	O6W—H6WB	0.8690
Mo10—O18	1.906 (3)	O7W—H7WA	0.8891
Mo10—O34	1.972 (4)	O7W—H7WB	0.8741
Mo10—O13	1.996 (4)	O8W—H8WC	0.9148
Mo10—O1	2.448 (3)	O8W—H8WD	0.9197
O2W—Tb1—O19	74.69 (14)	O23—Mo10—O34	101.16 (18)
O2W—Tb1—O24	77.18 (15)	O6—Mo10—O34	155.53 (15)
O19—Tb1—O24	99.63 (13)	O18—Mo10—O34	88.19 (15)
O2W—Tb1—O1W	148.99 (15)	O23—Mo10—O13	103.37 (18)
O19—Tb1—O1W	134.63 (14)	O6—Mo10—O13	85.26 (16)
O24—Tb1—O1W	86.29 (15)	O18—Mo10—O13	156.02 (15)
O2W—Tb1—O3W	123.30 (15)	O34—Mo10—O13	85.10 (16)
O19—Tb1—O3W	68.47 (14)	O23—Mo10—O1	170.73 (16)
O24—Tb1—O3W	68.59 (14)	O6—Mo10—O1	84.17 (14)
O1W—Tb1—O3W	72.34 (16)	O18—Mo10—O1	73.07 (13)
O2W—Tb1—O28	136.13 (14)	O34—Mo10—O1	72.35 (13)
O19—Tb1—O28	78.67 (13)	O13—Mo10—O1	82.96 (13)
O24—Tb1—O28	142.08 (13)	O35—Mo11—O29	103.17 (18)
O1W—Tb1—O28	70.33 (14)	O35—Mo11—O36	102.67 (19)
O3W—Tb1—O28	75.90 (14)	O29—Mo11—O36	92.62 (16)
O2W—Tb1—N3	73.97 (15)	O35—Mo11—O26	102.84 (18)
O19—Tb1—N3	63.81 (13)	O29—Mo11—O26	85.77 (15)
O24—Tb1—N3	149.65 (14)	O36—Mo11—O26	154.12 (15)
O1W—Tb1—N3	123.72 (15)	O35—Mo11—O25	100.79 (18)
O3W—Tb1—N3	121.21 (14)	O29—Mo11—O25	155.40 (15)
O28—Tb1—N3	63.09 (13)	O36—Mo11—O25	87.47 (16)
O2W—Tb1—N5	80.41 (14)	O26—Mo11—O25	83.58 (15)
O19—Tb1—N5	152.55 (14)	O35—Mo11—O3	171.41 (16)
O24—Tb1—N5	63.15 (13)	O29—Mo11—O3	84.35 (13)
O1W—Tb1—N5	68.69 (14)	O36—Mo11—O3	72.51 (14)
O3W—Tb1—N5	118.38 (14)	O26—Mo11—O3	81.63 (13)
O28—Tb1—N5	128.32 (14)	O25—Mo11—O3	72.20 (13)
N3—Tb1—N5	119.91 (13)	O41—Mo12—O8	104.06 (18)
O2W—Tb1—N4	81.13 (14)	O41—Mo12—O11	103.21 (19)
O19—Tb1—N4	124.48 (13)	O8—Mo12—O11	89.06 (16)
O24—Tb1—N4	122.66 (13)	O41—Mo12—O31	99.30 (18)
O1W—Tb1—N4	86.19 (16)	O8—Mo12—O31	156.22 (16)
O3W—Tb1—N4	155.57 (15)	O11—Mo12—O31	89.92 (15)
O28—Tb1—N4	86.15 (13)	O41—Mo12—O15	99.45 (18)
N3—Tb1—N4	61.70 (14)	O8—Mo12—O15	88.55 (15)
N5—Tb1—N4	61.23 (13)	O11—Mo12—O15	157.12 (16)
O42—Mo1—O37	102.18 (18)	O31—Mo12—O15	83.25 (15)
O42—Mo1—O30	101.0 (2)	O41—Mo12—O2	168.43 (16)
O37—Mo1—O30	91.27 (17)	O8—Mo12—O2	84.58 (14)
O42—Mo1—O25	101.8 (2)	O11—Mo12—O2	84.36 (14)
O37—Mo1—O25	91.26 (17)	O31—Mo12—O2	71.68 (13)
O30—Mo1—O25	155.95 (16)	O15—Mo12—O2	72.76 (13)
O42—Mo1—O21	102.41 (18)	O3—P1—O5	109.98 (19)
O37—Mo1—O21	155.31 (15)	O3—P1—O1	108.94 (19)
O30—Mo1—O21	81.98 (16)	O5—P1—O1	109.96 (19)
O25—Mo1—O21	85.81 (16)	O3—P1—O2	109.1 (2)
O42—Mo1—O3	173.49 (18)	O5—P1—O2	108.70 (19)
O37—Mo1—O3	73.74 (14)	O1—P1—O2	110.15 (19)
O30—Mo1—O3	84.32 (14)	P1—O1—Mo4	125.55 (19)
O25—Mo1—O3	73.47 (14)	P1—O1—Mo10	126.27 (19)
O21—Mo1—O3	81.94 (13)	Mo4—O1—Mo10	90.77 (11)
O32—Mo2—O29	103.74 (18)	P1—O1—Mo2	126.18 (19)
O32—Mo2—O18	101.13 (17)	Mo4—O1—Mo2	87.87 (11)
O29—Mo2—O18	91.86 (15)	Mo10—O1—Mo2	88.18 (11)
O32—Mo2—O17	104.09 (17)	P1—O2—Mo7	127.60 (19)
O29—Mo2—O17	84.78 (15)	P1—O2—Mo12	124.10 (19)
O18—Mo2—O17	154.63 (14)	Mo7—O2—Mo12	90.09 (11)
O32—Mo2—O40	100.65 (17)	P1—O2—Mo8	126.21 (18)
O29—Mo2—O40	155.42 (15)	Mo7—O2—Mo8	87.76 (11)
O18—Mo2—O40	86.37 (15)	Mo12—O2—Mo8	89.15 (11)
O17—Mo2—O40	86.41 (15)	P1—O3—Mo9	126.26 (19)
O32—Mo2—O1	170.37 (15)	P1—O3—Mo1	126.11 (19)
O29—Mo2—O1	83.95 (14)	Mo9—O3—Mo1	88.73 (11)
O18—Mo2—O1	72.49 (13)	P1—O3—Mo11	125.90 (19)
O17—Mo2—O1	82.15 (13)	Mo9—O3—Mo11	87.63 (12)
O40—Mo2—O1	72.13 (13)	Mo1—O3—Mo11	90.09 (11)
O22—Mo3—O7	101.32 (18)	Mo4—O4—Mo3	156.1 (2)
O22—Mo3—O12	102.42 (18)	P1—O5—Mo5	126.47 (18)
O7—Mo3—O12	91.11 (16)	P1—O5—Mo3	127.61 (19)
O22—Mo3—O4	101.65 (17)	Mo5—O5—Mo3	88.27 (11)
O7—Mo3—O4	88.82 (15)	P1—O5—Mo6	124.64 (18)
O12—Mo3—O4	155.46 (16)	Mo5—O5—Mo6	89.73 (11)
O22—Mo3—O8	102.16 (17)	Mo3—O5—Mo6	87.83 (11)
O7—Mo3—O8	156.17 (16)	Mo9—O6—Mo10	154.7 (2)
O12—Mo3—O8	87.81 (15)	Mo3—O7—Mo6	125.20 (19)
O4—Mo3—O8	82.52 (15)	Mo12—O8—Mo3	151.1 (2)
O22—Mo3—O5	174.05 (15)	Mo7—O9—Mo8	124.71 (19)
O7—Mo3—O5	74.06 (13)	Mo7—O10—Mo9	152.3 (2)
O12—Mo3—O5	74.22 (13)	Mo12—O11—Mo4	148.7 (2)
O4—Mo3—O5	82.19 (13)	Mo3—O12—Mo5	123.80 (18)
O8—Mo3—O5	82.76 (14)	Mo10—O13—Mo7	147.1 (2)
O38—Mo4—O40	102.47 (18)	Mo5—O14—Mo6	126.14 (19)
O38—Mo4—O4	102.20 (18)	Mo8—O15—Mo12	125.18 (19)
O40—Mo4—O4	94.59 (16)	Mo6—O17—Mo2	151.1 (2)
O38—Mo4—O34	101.15 (17)	Mo10—O18—Mo2	126.25 (18)
O40—Mo4—O34	88.80 (16)	C9—O19—Tb1	123.4 (4)
O4—Mo4—O34	155.07 (15)	Mo5—O21—Mo1	154.3 (2)
O38—Mo4—O11	101.28 (18)	C1—O24—Tb1	124.0 (3)
O40—Mo4—O11	155.92 (15)	Mo1—O25—Mo11	123.53 (19)
O4—Mo4—O11	84.23 (15)	Mo6—O26—Mo11	147.0 (2)
O34—Mo4—O11	82.75 (15)	Mo7—O28—Tb1	159.2 (2)
O38—Mo4—O1	172.69 (16)	Mo11—O29—Mo2	154.9 (2)
O40—Mo4—O1	74.48 (14)	Mo8—O30—Mo1	153.3 (2)
O4—Mo4—O1	84.76 (14)	Mo7—O31—Mo12	124.86 (18)
O34—Mo4—O1	72.35 (13)	Mo8—O33—Mo5	147.7 (2)
O11—Mo4—O1	81.48 (13)	Mo10—O34—Mo4	123.86 (17)
O20—Mo5—O21	103.93 (18)	Mo11—O36—Mo9	127.2 (2)
O20—Mo5—O14	102.53 (18)	Mo1—O37—Mo9	125.48 (19)
O21—Mo5—O14	93.15 (16)	Mo4—O40—Mo2	125.52 (18)
O20—Mo5—O33	99.55 (18)	C9—N1—H1A	120.0
O21—Mo5—O33	86.72 (16)	C9—N1—H1B	120.0
O14—Mo5—O33	157.25 (15)	H1A—N1—H1B	120.0
O20—Mo5—O12	99.95 (18)	C9—N2—N3	115.4 (4)
O21—Mo5—O12	155.44 (15)	C9—N2—H2A	122.3
O14—Mo5—O12	87.17 (16)	N3—N2—H2A	122.3
O33—Mo5—O12	83.73 (15)	C8—N3—N2	119.2 (5)
O20—Mo5—O5	171.72 (16)	C8—N3—Tb1	124.1 (4)
O21—Mo5—O5	83.50 (14)	N2—N3—Tb1	114.7 (3)
O14—Mo5—O5	73.06 (13)	C7—N4—C3	119.0 (4)
O33—Mo5—O5	84.35 (13)	C7—N4—Tb1	119.6 (3)
O12—Mo5—O5	73.09 (13)	C3—N4—Tb1	121.3 (3)
O16—Mo6—O17	103.75 (17)	C2—N5—N6	119.0 (4)
O16—Mo6—O26	102.99 (17)	C2—N5—Tb1	126.0 (3)
O17—Mo6—O26	89.46 (16)	N6—N5—Tb1	114.5 (3)
O16—Mo6—O7	101.31 (17)	C1—N6—N5	116.6 (4)
O17—Mo6—O7	91.13 (15)	C1—N6—H6C	121.7
O26—Mo6—O7	154.82 (15)	N5—N6—H6C	121.7
O16—Mo6—O14	100.44 (16)	C1—N7—H7A	120.0
O17—Mo6—O14	155.80 (15)	C1—N7—H7B	120.0
O26—Mo6—O14	85.73 (16)	H7A—N7—H7B	120.0
O7—Mo6—O14	83.48 (15)	O24—C1—N7	124.1 (5)
O16—Mo6—O5	169.95 (14)	O24—C1—N6	120.0 (5)
O17—Mo6—O5	84.79 (14)	N7—C1—N6	115.9 (5)
O26—Mo6—O5	82.11 (13)	N5—C2—C10	126.2 (5)
O7—Mo6—O5	72.88 (13)	N5—C2—C3	113.5 (5)
O14—Mo6—O5	71.07 (13)	C10—C2—C3	120.3 (5)
O28—Mo7—O10	102.63 (17)	N4—C3—C4	121.6 (5)
O28—Mo7—O9	100.31 (17)	N4—C3—C2	116.3 (4)
O10—Mo7—O9	92.49 (16)	C4—C3—C2	122.0 (5)
O28—Mo7—O31	100.48 (17)	C3—C4—C5	120.4 (5)
O10—Mo7—O31	156.17 (15)	C3—C4—H6B	119.8
O9—Mo7—O31	89.05 (16)	C5—C4—H6B	119.8
O28—Mo7—O13	101.84 (17)	C4—C5—C6	119.0 (5)
O10—Mo7—O13	85.60 (16)	C4—C5—H5A	120.5
O9—Mo7—O13	157.65 (15)	C6—C5—H5A	120.5
O31—Mo7—O13	84.04 (16)	C5—C6—C7	118.8 (5)
O28—Mo7—O2	172.17 (15)	C5—C6—H6A	120.6
O10—Mo7—O2	84.14 (14)	C7—C6—H6A	120.6
O9—Mo7—O2	75.23 (14)	N4—C7—C6	121.1 (5)
O31—Mo7—O2	73.26 (13)	N4—C7—C8	116.9 (4)
O13—Mo7—O2	82.41 (13)	C6—C7—C8	121.9 (5)
O27—Mo8—O33	102.64 (18)	N3—C8—C7	114.1 (5)
O27—Mo8—O15	102.76 (19)	N3—C8—C11	125.7 (5)
O33—Mo8—O15	91.15 (16)	C7—C8—C11	120.2 (5)
O27—Mo8—O30	102.40 (18)	O19—C9—N1	122.7 (5)
O33—Mo8—O30	87.22 (16)	O19—C9—N2	121.5 (5)
O15—Mo8—O30	154.52 (15)	N1—C9—N2	115.8 (5)
O27—Mo8—O9	100.00 (17)	C2—C10—H10A	109.5
O33—Mo8—O9	157.29 (15)	C2—C10—H10B	109.5
O15—Mo8—O9	85.54 (16)	H10A—C10—H10B	109.5
O30—Mo8—O9	86.25 (16)	C2—C10—H10C	109.5
O27—Mo8—O2	171.09 (16)	H10A—C10—H10C	109.5
O33—Mo8—O2	85.37 (14)	H10B—C10—H10C	109.5
O15—Mo8—O2	72.86 (13)	C8—C11—H11A	109.5
O30—Mo8—O2	81.67 (13)	C8—C11—H11B	109.5
O9—Mo8—O2	72.17 (13)	H11A—C11—H11B	109.5
O39—Mo9—O6	104.80 (18)	C8—C11—H11C	109.5
O39—Mo9—O36	102.10 (18)	H11A—C11—H11C	109.5
O6—Mo9—O36	93.69 (16)	H11B—C11—H11C	109.5
O39—Mo9—O10	102.83 (18)	Tb1—O1W—H1WA	105.5
O6—Mo9—O10	85.14 (15)	Tb1—O1W—H1WB	109.8
O36—Mo9—O10	154.49 (15)	H1WA—O1W—H1WB	117.2
O39—Mo9—O37	99.03 (18)	Tb1—O2W—H2WA	129.8
O6—Mo9—O37	155.49 (15)	Tb1—O2W—H2WB	107.7
O36—Mo9—O37	86.74 (16)	H2WA—O2W—H2WB	115.8
O10—Mo9—O37	84.10 (15)	Tb1—O3W—H3WA	125.9
O39—Mo9—O3	169.40 (17)	Tb1—O3W—H3WB	113.1
O6—Mo9—O3	84.95 (13)	H3WA—O3W—H3WB	114.3
O36—Mo9—O3	72.67 (14)	H4WA—O4W—H4WB	89.5
O10—Mo9—O3	81.85 (13)	H5WB—O5W—H5WA	96.4
O37—Mo9—O3	71.77 (13)	H5WC—O5WA—H5WD	113.1
O23—Mo10—O6	102.94 (18)	H6WA—O6W—H6WB	95.5
O23—Mo10—O18	100.51 (17)	H7WA—O7W—H7WB	92.1
O6—Mo10—O18	91.57 (15)	H8WC—O8W—H8WD	82.1

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O18^i	0.86	2.17	2.872 (6)	138
N6—H6C···O33^ii	0.86	2.37	3.106 (6)	143
N7—H7A···O37^iii	0.86	2.58	3.229 (7)	133
N7—H7A···O39^iii	0.86	2.46	3.280 (7)	159
N7—H7B···O12^ii	0.86	2.41	3.262 (7)	174
C4—H6B···O35^iv	0.93	2.45	3.153 (8)	132
C11—H11B···O23	0.96	2.59	3.489 (8)	156

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

{Triaqua[2,6-diacetylpyridine bis(semicarbazone)-κ⁵O,N,N',N'',O']dysprosium(III)}-µ-oxido-[tricosa-µ₂-oxido-dodecaoxido-µ₁₂-phosphato-dodecamolybdenum(VI)] pentahydrate (a-2)

Crystal data

[Dy(C11H15N7O2)(H2O)3][PMo12O40]·5H2O	Z = 2
Mr = 2406.18	F(000) = 2262
Triclinic, P1	Dx = 3.127 Mg m^−3
a = 11.566 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 15.218 (3) Å	Cell parameters from 7279 reflections
c = 15.257 (3) Å	θ = 2.3–26.8°
α = 80.092 (3)°	µ = 4.44 mm^−1
β = 87.602 (3)°	T = 173 K
γ = 75.013 (2)°	Block-shaped, black
V = 2555.3 (10) Å^3	0.11 × 0.11 × 0.10 mm

Data collection

Bruker Apex2 CCD diffractometer	7280 reflections with I > 2σ(I)
ω scans	Rint = 0.035
Absorption correction: multi-scan (SADABS; Bruker, 2005)	θmax = 25.5°, θmin = 1.4°
Tmin = 0.641, Tmax = 0.665	h = −13→13
18194 measured reflections	k = −18→18
9300 independent reflections	l = −18→15

Refinement

Refinement on F^2	96 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.039	H-atom parameters constrained
wR(F^2) = 0.111	w = 1/[σ^2(Fo^2) + (0.0636P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.002
9300 reflections	Δρmax = 2.33 e Å^−3
741 parameters	Δρmin = −1.51 e Å^−3

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Dy1	0.24430 (3)	0.31717 (2)	0.64154 (2)	0.01742 (10)
Mo1	0.02453 (7)	0.86502 (5)	0.63389 (5)	0.02685 (18)
Mo2	0.14287 (6)	0.79585 (4)	1.03541 (4)	0.01863 (16)
Mo3	−0.03854 (6)	0.69575 (5)	0.79205 (5)	0.02204 (16)
Mo4	0.21530 (6)	0.98157 (4)	0.87316 (4)	0.01868 (16)
Mo5	0.48893 (6)	0.84778 (5)	0.83035 (5)	0.02006 (16)
Mo6	0.42035 (6)	0.66229 (5)	1.00122 (5)	0.02285 (17)
Mo7	0.26115 (6)	0.54757 (4)	0.74165 (5)	0.02084 (16)
Mo8	0.16745 (6)	0.58461 (4)	0.97831 (4)	0.02034 (16)
Mo9	−0.05994 (6)	0.90638 (5)	0.84667 (5)	0.02584 (17)
Mo10	0.32930 (7)	0.72022 (5)	0.59470 (5)	0.02517 (17)
Mo11	0.29486 (6)	0.94812 (4)	0.65889 (4)	0.01996 (16)
Mo12	0.51229 (6)	0.61656 (5)	0.77541 (5)	0.02623 (18)
P1	0.23023 (15)	0.76320 (11)	0.81313 (12)	0.0114 (4)
O1	0.2379 (4)	0.7195 (3)	0.9123 (3)	0.0145 (10)
O2	0.3000 (4)	0.6919 (3)	0.7571 (3)	0.0145 (10)
O3	0.0399 (5)	0.3870 (4)	0.6585 (4)	0.0248 (12)
O4	0.2839 (4)	0.8466 (3)	0.7991 (3)	0.0151 (10)
O5	0.0991 (4)	0.7942 (3)	0.7844 (3)	0.0171 (11)
O6	0.0362 (5)	0.6397 (3)	0.9014 (3)	0.0209 (12)
O7	0.4553 (5)	0.9141 (3)	0.7140 (3)	0.0210 (12)
O8	0.2837 (5)	0.6040 (3)	0.6256 (3)	0.0217 (12)
O9	0.4653 (4)	0.7637 (3)	0.9367 (3)	0.0196 (11)
O10	0.3892 (5)	0.9452 (3)	0.8799 (3)	0.0210 (12)
O11	0.1861 (5)	1.0824 (3)	0.9109 (4)	0.0251 (13)
O12	0.5288 (4)	0.7341 (3)	0.7792 (4)	0.0224 (12)
O13	0.3162 (5)	1.0242 (4)	0.5704 (4)	0.0311 (14)
O14	0.0132 (4)	0.8455 (3)	0.9559 (3)	0.0196 (11)
O15	0.2064 (4)	0.8959 (3)	0.9738 (3)	0.0180 (11)
O16	0.4781 (5)	0.6025 (3)	0.8966 (4)	0.0235 (12)
O17	0.2443 (5)	1.0240 (3)	0.7457 (3)	0.0203 (11)
O18	0.2518 (5)	0.4431 (4)	0.7231 (4)	0.0272 (13)
O19	0.0989 (5)	0.6147 (4)	0.7389 (3)	0.0251 (12)
O20	0.6244 (5)	0.8607 (4)	0.8495 (4)	0.0284 (13)
O21	0.4808 (5)	0.6541 (4)	0.6466 (4)	0.0246 (12)
O22	0.1440 (5)	0.9356 (3)	0.6420 (3)	0.0211 (12)
O23	0.1276 (5)	0.4956 (4)	1.0385 (4)	0.0311 (14)
O24	0.0892 (5)	0.8319 (4)	1.1298 (3)	0.0258 (13)
O25	−0.0697 (5)	0.9407 (4)	0.7151 (4)	0.0246 (12)
O26	0.1125 (4)	0.6757 (3)	1.0528 (3)	0.0182 (11)
O27	0.0638 (5)	0.9754 (3)	0.8367 (4)	0.0224 (12)
O28	0.1624 (5)	0.7788 (4)	0.5960 (3)	0.0253 (12)
O29	0.2471 (5)	0.5333 (3)	0.8736 (4)	0.0236 (12)
O31	0.5355 (5)	0.6149 (4)	1.0727 (4)	0.0327 (14)
O32	−0.0528 (5)	0.7729 (4)	0.6717 (4)	0.0256 (12)
O33	−0.1203 (4)	0.8052 (4)	0.8350 (4)	0.0244 (12)
O34	0.2366 (5)	0.2858 (4)	0.4944 (4)	0.0268 (13)
O35	−0.1483 (5)	0.6443 (4)	0.7843 (4)	0.0327 (14)
O36	0.4282 (5)	0.5230 (3)	0.7630 (4)	0.0236 (12)
O37	0.3568 (6)	0.7210 (4)	0.4855 (4)	0.0339 (14)
O38	−0.0425 (6)	0.9152 (4)	0.5364 (4)	0.0384 (16)
O41	0.3097 (4)	0.7311 (3)	1.0701 (3)	0.0209 (12)
O43	0.3291 (5)	0.5670 (3)	1.0238 (3)	0.0211 (12)
O45	0.3545 (5)	0.8328 (4)	0.6126 (3)	0.0249 (12)
O47	−0.1811 (5)	0.9824 (4)	0.8767 (4)	0.0346 (15)
O50	0.6525 (5)	0.5523 (4)	0.7729 (4)	0.0365 (15)
N1	−0.1241 (6)	0.4351 (6)	0.7403 (5)	0.046 (2)
H1A	−0.1681	0.4601	0.6940	0.055*
H1B	−0.1544	0.4374	0.7926	0.055*
N2	0.0541 (6)	0.3566 (4)	0.8088 (4)	0.0257 (15)
H2A	0.0241	0.3663	0.8599	0.031*
N3	0.1684 (5)	0.3038 (4)	0.7994 (4)	0.0202 (14)
N4	0.3796 (5)	0.2074 (4)	0.7629 (4)	0.0188 (14)
N5	0.4167 (6)	0.1887 (4)	0.5969 (4)	0.0200 (14)
N6	0.4194 (6)	0.1853 (4)	0.5080 (4)	0.0206 (14)
H6B	0.4810	0.1538	0.4835	0.025*
N7	0.3209 (6)	0.2209 (5)	0.3762 (5)	0.0356 (18)
H7A	0.2603	0.2498	0.3426	0.043*
H7B	0.3810	0.1841	0.3553	0.043*
C1	−0.0091 (7)	0.3928 (5)	0.7311 (6)	0.0272 (19)
C2	0.2359 (7)	0.2699 (5)	0.8687 (5)	0.0206 (17)
C3	0.3527 (7)	0.2097 (5)	0.8495 (5)	0.0185 (16)
C4	0.4290 (8)	0.1570 (6)	0.9169 (5)	0.030 (2)
H4A	0.4083	0.1595	0.9762	0.036*
C5	0.5369 (8)	0.1002 (6)	0.8950 (6)	0.034 (2)
H5A	0.5913	0.0666	0.9393	0.041*
C6	0.5621 (7)	0.0944 (6)	0.8081 (5)	0.0269 (19)
H6A	0.6327	0.0548	0.7926	0.032*
C7	0.4816 (7)	0.1480 (5)	0.7424 (5)	0.0223 (17)
C8	0.5004 (7)	0.1385 (5)	0.6476 (5)	0.0176 (16)
C9	0.3217 (7)	0.2332 (5)	0.4610 (5)	0.0217 (17)
C10	0.1976 (7)	0.2854 (6)	0.9609 (5)	0.0270 (19)
H10A	0.2617	0.2539	1.0018	0.040*
H10B	0.1777	0.3502	0.9630	0.040*
H10C	0.1288	0.2619	0.9770	0.040*
C11	0.6100 (8)	0.0731 (6)	0.6185 (6)	0.032 (2)
H11A	0.6600	0.0430	0.6692	0.048*
H11B	0.5869	0.0277	0.5914	0.048*
H11C	0.6533	0.1067	0.5762	0.048*
O1W	0.1516 (5)	0.1971 (3)	0.6600 (4)	0.0315 (14)
H1WA	0.1073	0.1885	0.6202	0.047*
H1WB	0.1715	0.1482	0.6987	0.047*
O2W	0.1775 (6)	0.4579 (4)	0.5350 (4)	0.0360 (15)
H2WA	0.2149	0.4994	0.5351	0.054*
H2WB	0.1023	0.4831	0.5318	0.054*
O3W	0.4153 (6)	0.3715 (4)	0.5998 (5)	0.0501 (18)
H3WA	0.4855	0.3424	0.6149	0.075*
H3WB	0.4115	0.4239	0.5688	0.075*
O4W	0.0158	0.6205	0.5536	0.057 (2)
H4WA	0.0545	0.6565	0.5751	0.085*
H4WB	0.0015	0.5873	0.6055	0.085*
O5W	0.0660 (8)	0.7631 (7)	1.4214 (5)	0.086 (3)
H5WA	0.0410	0.8046	1.4588	0.129*
H5WB	0.1319	0.7294	1.4531	0.129*
O6W	0.5984 (9)	0.3541 (6)	0.7184 (6)	0.107 (4)
H6WA	0.5292	0.3625	0.7473	0.161*
H6WB	0.6050	0.4129	0.7091	0.161*
O7W	0.3509 (9)	0.4984 (6)	0.4200 (7)	0.109 (4)
H7WA	0.3392	0.4719	0.3746	0.163*
H7WB	0.4310	0.4884	0.4162	0.163*
O8W	0.2335	0.7984	1.2867	0.061 (3)	0.630 (12)
H8WA	0.2034	0.7620	1.3243	0.092*	0.630 (12)
H8WB	0.1833	0.8273	1.2459	0.092*	0.630 (12)
O8WA	0.1255	0.8717	1.3049	0.072 (5)	0.370 (12)
H8WC	0.0500	0.8837	1.3111	0.108*	0.370 (12)
H8WD	0.1611	0.8465	1.3539	0.108*	0.370 (12)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Dy1	0.0187 (2)	0.01724 (18)	0.01712 (19)	−0.00538 (15)	0.00789 (14)	−0.00589 (14)
Mo1	0.0239 (4)	0.0361 (4)	0.0196 (4)	−0.0097 (3)	−0.0035 (3)	0.0021 (3)
Mo2	0.0238 (4)	0.0165 (3)	0.0149 (3)	−0.0035 (3)	0.0081 (3)	−0.0053 (3)
Mo3	0.0158 (4)	0.0260 (4)	0.0272 (4)	−0.0090 (3)	0.0034 (3)	−0.0074 (3)
Mo4	0.0231 (4)	0.0140 (3)	0.0197 (4)	−0.0045 (3)	0.0090 (3)	−0.0072 (3)
Mo5	0.0164 (4)	0.0214 (3)	0.0236 (4)	−0.0058 (3)	0.0059 (3)	−0.0070 (3)
Mo6	0.0172 (4)	0.0244 (4)	0.0237 (4)	−0.0026 (3)	−0.0019 (3)	0.0013 (3)
Mo7	0.0224 (4)	0.0160 (3)	0.0277 (4)	−0.0088 (3)	0.0112 (3)	−0.0103 (3)
Mo8	0.0282 (4)	0.0172 (3)	0.0177 (4)	−0.0103 (3)	0.0074 (3)	−0.0034 (3)
Mo9	0.0135 (4)	0.0292 (4)	0.0334 (4)	0.0037 (3)	0.0003 (3)	−0.0156 (3)
Mo10	0.0382 (4)	0.0221 (3)	0.0194 (4)	−0.0138 (3)	0.0138 (3)	−0.0091 (3)
Mo11	0.0289 (4)	0.0166 (3)	0.0159 (3)	−0.0094 (3)	0.0067 (3)	−0.0030 (3)
Mo12	0.0134 (4)	0.0236 (4)	0.0439 (5)	−0.0010 (3)	0.0070 (3)	−0.0189 (3)
P1	0.0096 (9)	0.0111 (8)	0.0135 (9)	−0.0019 (7)	0.0042 (7)	−0.0045 (7)
O1	0.015 (3)	0.015 (2)	0.013 (3)	−0.001 (2)	0.006 (2)	−0.004 (2)
O2	0.014 (3)	0.017 (2)	0.015 (3)	−0.005 (2)	0.006 (2)	−0.008 (2)
O3	0.021 (3)	0.029 (3)	0.021 (3)	0.001 (2)	0.010 (2)	−0.006 (2)
O4	0.018 (3)	0.016 (2)	0.012 (3)	−0.003 (2)	0.002 (2)	−0.006 (2)
O5	0.015 (3)	0.019 (3)	0.018 (3)	−0.004 (2)	0.005 (2)	−0.005 (2)
O6	0.021 (3)	0.025 (3)	0.020 (3)	−0.007 (2)	0.007 (2)	−0.010 (2)
O7	0.026 (3)	0.020 (3)	0.020 (3)	−0.011 (2)	0.009 (2)	−0.007 (2)
O8	0.021 (3)	0.022 (3)	0.025 (3)	−0.011 (2)	0.007 (2)	−0.007 (2)
O9	0.018 (3)	0.018 (3)	0.020 (3)	0.001 (2)	0.005 (2)	−0.006 (2)
O10	0.021 (3)	0.021 (3)	0.024 (3)	−0.012 (2)	0.008 (2)	−0.006 (2)
O11	0.028 (3)	0.019 (3)	0.031 (3)	−0.005 (2)	0.013 (2)	−0.015 (2)
O12	0.013 (3)	0.025 (3)	0.030 (3)	−0.003 (2)	0.012 (2)	−0.011 (2)
O13	0.051 (4)	0.022 (3)	0.024 (3)	−0.019 (3)	0.008 (3)	0.000 (2)
O14	0.020 (3)	0.023 (3)	0.019 (3)	−0.007 (2)	0.007 (2)	−0.009 (2)
O15	0.017 (3)	0.019 (3)	0.019 (3)	−0.005 (2)	0.006 (2)	−0.008 (2)
O16	0.021 (3)	0.014 (2)	0.033 (3)	0.001 (2)	0.002 (2)	−0.005 (2)
O17	0.028 (3)	0.016 (2)	0.016 (3)	−0.005 (2)	0.007 (2)	−0.003 (2)
O18	0.037 (3)	0.024 (3)	0.026 (3)	−0.015 (3)	0.016 (3)	−0.012 (2)
O19	0.027 (3)	0.026 (3)	0.028 (3)	−0.012 (2)	0.009 (2)	−0.013 (2)
O20	0.021 (3)	0.030 (3)	0.036 (3)	−0.008 (2)	0.007 (3)	−0.009 (3)
O21	0.023 (3)	0.027 (3)	0.028 (3)	−0.011 (2)	0.020 (2)	−0.016 (2)
O22	0.025 (3)	0.023 (3)	0.017 (3)	−0.008 (2)	0.000 (2)	−0.004 (2)
O23	0.043 (4)	0.022 (3)	0.030 (3)	−0.015 (3)	0.011 (3)	0.000 (2)
O24	0.035 (3)	0.024 (3)	0.018 (3)	−0.005 (2)	0.009 (2)	−0.009 (2)
O25	0.021 (3)	0.028 (3)	0.022 (3)	−0.004 (2)	−0.005 (2)	0.003 (2)
O26	0.017 (3)	0.018 (3)	0.018 (3)	−0.001 (2)	0.007 (2)	−0.004 (2)
O27	0.020 (3)	0.017 (3)	0.029 (3)	−0.002 (2)	0.004 (2)	−0.005 (2)
O28	0.031 (3)	0.025 (3)	0.022 (3)	−0.011 (2)	0.002 (2)	−0.002 (2)
O29	0.028 (3)	0.022 (3)	0.025 (3)	−0.012 (2)	0.010 (2)	−0.011 (2)
O31	0.026 (3)	0.035 (3)	0.032 (3)	−0.007 (3)	−0.005 (3)	0.008 (3)
O32	0.023 (3)	0.028 (3)	0.025 (3)	−0.003 (2)	−0.004 (2)	−0.008 (2)
O33	0.013 (3)	0.030 (3)	0.027 (3)	0.001 (2)	0.005 (2)	−0.005 (2)
O34	0.027 (3)	0.029 (3)	0.023 (3)	−0.001 (3)	0.002 (2)	−0.010 (2)
O35	0.026 (3)	0.043 (4)	0.036 (4)	−0.019 (3)	0.000 (3)	−0.007 (3)
O36	0.024 (3)	0.017 (3)	0.032 (3)	−0.007 (2)	0.012 (2)	−0.009 (2)
O37	0.051 (4)	0.033 (3)	0.025 (3)	−0.022 (3)	0.020 (3)	−0.013 (3)
O38	0.039 (4)	0.050 (4)	0.028 (3)	−0.018 (3)	−0.011 (3)	0.002 (3)
O41	0.019 (3)	0.023 (3)	0.021 (3)	−0.006 (2)	0.003 (2)	−0.006 (2)
O43	0.026 (3)	0.019 (3)	0.015 (3)	−0.004 (2)	0.002 (2)	0.002 (2)
O45	0.034 (3)	0.026 (3)	0.018 (3)	−0.014 (3)	0.012 (2)	−0.007 (2)
O47	0.021 (3)	0.036 (3)	0.045 (4)	0.004 (3)	0.002 (3)	−0.020 (3)
O50	0.020 (3)	0.027 (3)	0.063 (4)	0.002 (3)	0.007 (3)	−0.023 (3)
N1	0.022 (4)	0.064 (5)	0.037 (5)	0.012 (4)	0.011 (3)	−0.005 (4)
N2	0.026 (3)	0.026 (3)	0.021 (3)	0.000 (3)	0.013 (3)	−0.006 (3)
N3	0.015 (3)	0.022 (3)	0.024 (3)	−0.003 (2)	0.010 (2)	−0.007 (2)
N4	0.014 (3)	0.024 (3)	0.017 (3)	−0.003 (3)	0.002 (3)	−0.002 (3)
N5	0.022 (4)	0.023 (3)	0.015 (3)	−0.006 (3)	0.008 (3)	−0.007 (3)
N6	0.025 (3)	0.027 (3)	0.012 (3)	−0.005 (3)	0.009 (3)	−0.012 (3)
N7	0.027 (4)	0.057 (5)	0.021 (4)	0.000 (3)	0.001 (3)	−0.018 (3)
C1	0.019 (4)	0.019 (4)	0.036 (5)	0.003 (3)	0.006 (4)	0.004 (4)
C2	0.026 (3)	0.024 (3)	0.020 (3)	−0.020 (3)	0.007 (3)	−0.005 (3)
C3	0.021 (3)	0.018 (3)	0.022 (3)	−0.013 (3)	−0.002 (3)	−0.004 (3)
C4	0.041 (5)	0.040 (5)	0.013 (4)	−0.016 (4)	0.004 (4)	−0.007 (4)
C5	0.024 (5)	0.044 (5)	0.032 (5)	−0.004 (4)	−0.009 (4)	−0.004 (4)
C6	0.019 (4)	0.035 (5)	0.026 (5)	−0.003 (4)	−0.003 (3)	−0.011 (4)
C7	0.014 (4)	0.023 (4)	0.030 (5)	−0.007 (3)	−0.004 (3)	−0.001 (3)
C8	0.022 (4)	0.021 (4)	0.015 (4)	−0.012 (3)	0.006 (3)	−0.009 (3)
C9	0.022 (3)	0.027 (3)	0.019 (3)	−0.010 (3)	0.007 (3)	−0.007 (3)
C10	0.027 (5)	0.037 (5)	0.015 (4)	−0.002 (4)	0.002 (3)	−0.009 (4)
C11	0.032 (5)	0.029 (4)	0.029 (5)	0.002 (4)	0.005 (4)	−0.006 (4)
O1W	0.037 (4)	0.016 (3)	0.042 (4)	−0.011 (3)	−0.004 (3)	0.000 (3)
O2W	0.043 (4)	0.020 (3)	0.037 (4)	−0.001 (3)	0.009 (3)	0.005 (3)
O3W	0.040 (4)	0.039 (4)	0.078 (5)	−0.021 (3)	0.025 (3)	−0.019 (3)
O4W	0.054 (5)	0.064 (5)	0.042 (4)	0.016 (4)	−0.024 (4)	−0.024 (4)
O5W	0.081 (6)	0.126 (7)	0.070 (5)	−0.049 (5)	−0.007 (4)	−0.033 (5)
O6W	0.095 (6)	0.089 (6)	0.160 (8)	−0.050 (5)	0.001 (6)	−0.040 (6)
O7W	0.128 (7)	0.102 (6)	0.107 (7)	−0.042 (6)	0.064 (6)	−0.042 (5)
O8W	0.072 (9)	0.076 (8)	0.041 (6)	−0.034 (6)	−0.006 (6)	0.000 (6)
O8WA	0.097 (11)	0.076 (10)	0.044 (9)	−0.023 (9)	−0.012 (9)	−0.010 (8)

Geometric parameters (Å, º)

Dy1—O1W	2.315 (5)	Mo11—O13	1.674 (5)
Dy1—O3	2.352 (5)	Mo11—O22	1.837 (5)
Dy1—O3W	2.359 (6)	Mo11—O17	1.881 (5)
Dy1—O34	2.384 (6)	Mo11—O45	1.954 (5)
Dy1—O2W	2.425 (5)	Mo11—O7	1.975 (5)
Dy1—O18	2.481 (5)	Mo11—O4	2.433 (5)
Dy1—N3	2.523 (6)	Mo12—O50	1.666 (6)
Dy1—N4	2.548 (6)	Mo12—O12	1.857 (5)
Dy1—N5	2.567 (6)	Mo12—O16	1.864 (6)
Mo1—O38	1.673 (6)	Mo12—O36	1.958 (5)
Mo1—O32	1.851 (6)	Mo12—O21	1.969 (6)
Mo1—O28	1.922 (6)	Mo12—O2	2.433 (5)
Mo1—O25	1.945 (6)	P1—O5	1.527 (5)
Mo1—O22	1.976 (5)	P1—O4	1.532 (5)
Mo1—O5	2.452 (5)	P1—O2	1.537 (5)
Mo2—O24	1.669 (5)	P1—O1	1.543 (5)
Mo2—O14	1.883 (5)	O3—C1	1.231 (10)
Mo2—O26	1.922 (5)	O34—C9	1.246 (9)
Mo2—O15	1.942 (5)	N1—C1	1.334 (11)
Mo2—O41	1.973 (5)	N1—H1A	0.8600
Mo2—O1	2.449 (5)	N1—H1B	0.8600
Mo3—O35	1.676 (6)	N2—C1	1.371 (10)
Mo3—O6	1.874 (5)	N2—N3	1.373 (9)
Mo3—O33	1.900 (5)	N2—H2A	0.8600
Mo3—O19	1.982 (6)	N3—C2	1.290 (10)
Mo3—O32	1.991 (6)	N4—C7	1.349 (10)
Mo3—O5	2.439 (5)	N4—C3	1.350 (10)
Mo4—O11	1.677 (5)	N5—C8	1.263 (10)
Mo4—O15	1.854 (5)	N5—N6	1.367 (8)
Mo4—O27	1.890 (5)	N6—C9	1.339 (10)
Mo4—O10	1.944 (5)	N6—H6B	0.8600
Mo4—O17	1.984 (5)	N7—C9	1.338 (10)
Mo4—O4	2.450 (5)	N7—H7A	0.8600
Mo5—O20	1.674 (6)	N7—H7B	0.8600
Mo5—O10	1.880 (5)	C2—C3	1.476 (11)
Mo5—O7	1.887 (5)	C2—C10	1.494 (11)
Mo5—O9	1.941 (5)	C3—C4	1.380 (11)
Mo5—O12	1.960 (5)	C4—C5	1.388 (12)
Mo5—O4	2.443 (5)	C4—H4A	0.9300
Mo6—O31	1.685 (6)	C5—C6	1.356 (12)
Mo6—O41	1.848 (5)	C5—H5A	0.9300
Mo6—O9	1.864 (5)	C6—C7	1.395 (11)
Mo6—O16	1.978 (6)	C6—H6A	0.9300
Mo6—O43	1.981 (5)	C7—C8	1.479 (11)
Mo6—O1	2.435 (5)	C8—C11	1.503 (11)
Mo7—O18	1.691 (5)	C10—H10A	0.9600
Mo7—O8	1.871 (5)	C10—H10B	0.9600
Mo7—O19	1.890 (6)	C10—H10C	0.9600
Mo7—O36	1.900 (6)	C11—H11A	0.9600
Mo7—O29	1.991 (6)	C11—H11B	0.9600
Mo7—O2	2.407 (5)	C11—H11C	0.9600
Mo8—O23	1.659 (5)	O1W—H1WA	0.8587
Mo8—O6	1.880 (5)	O1W—H1WB	0.8535
Mo8—O26	1.909 (5)	O2W—H2WA	0.8522
Mo8—O43	1.959 (5)	O2W—H2WB	0.8540
Mo8—O29	1.985 (5)	O3W—H3WA	0.8382
Mo8—O1	2.441 (5)	O3W—H3WB	0.8468
Mo9—O47	1.673 (6)	O4W—H4WA	0.8992
Mo9—O14	1.879 (5)	O4W—H4WB	0.8975
Mo9—O33	1.884 (6)	O5W—H5WA	0.9076
Mo9—O27	1.970 (5)	O5W—H5WB	0.9056
Mo9—O25	1.986 (6)	O6W—H6WA	0.8876
Mo9—O5	2.447 (5)	O6W—H6WB	0.9041
Mo10—O37	1.681 (6)	O7W—H7WA	0.8906
Mo10—O45	1.875 (5)	O7W—H7WB	0.9000
Mo10—O28	1.907 (6)	O8W—H8WA	0.8550
Mo10—O21	1.910 (6)	O8W—H8WB	0.8501
Mo10—O8	1.951 (5)	O8WA—H8WC	0.8497
Mo10—O2	2.465 (5)	O8WA—H8WD	0.8493
O1W—Dy1—O3	75.0 (2)	O37—Mo10—O21	102.1 (3)
O1W—Dy1—O3W	148.9 (2)	O45—Mo10—O21	91.3 (2)
O3—Dy1—O3W	134.9 (2)	O28—Mo10—O21	155.2 (2)
O1W—Dy1—O34	76.5 (2)	O37—Mo10—O8	100.0 (2)
O3—Dy1—O34	98.46 (19)	O45—Mo10—O8	156.9 (2)
O3W—Dy1—O34	88.5 (2)	O28—Mo10—O8	86.3 (2)
O1W—Dy1—O2W	123.4 (2)	O21—Mo10—O8	86.0 (2)
O3—Dy1—O2W	68.3 (2)	O37—Mo10—O2	170.8 (2)
O3W—Dy1—O2W	73.4 (2)	O45—Mo10—O2	85.10 (19)
O34—Dy1—O2W	68.4 (2)	O28—Mo10—O2	82.25 (19)
O1W—Dy1—O18	136.5 (2)	O21—Mo10—O2	72.97 (19)
O3—Dy1—O18	78.14 (19)	O8—Mo10—O2	72.20 (19)
O3W—Dy1—O18	69.7 (2)	O13—Mo11—O22	104.1 (3)
O34—Dy1—O18	141.51 (19)	O13—Mo11—O17	102.0 (2)
O2W—Dy1—O18	75.0 (2)	O22—Mo11—O17	93.6 (2)
O1W—Dy1—N3	74.4 (2)	O13—Mo11—O45	100.5 (2)
O3—Dy1—N3	64.6 (2)	O22—Mo11—O45	86.5 (2)
O3W—Dy1—N3	121.9 (2)	O17—Mo11—O45	156.8 (2)
O34—Dy1—N3	149.3 (2)	O13—Mo11—O7	99.8 (3)
O2W—Dy1—N3	121.5 (2)	O22—Mo11—O7	155.4 (2)
O18—Dy1—N3	63.33 (19)	O17—Mo11—O7	87.0 (2)
O1W—Dy1—N4	81.4 (2)	O45—Mo11—O7	83.5 (2)
O3—Dy1—N4	125.2 (2)	O13—Mo11—O4	171.4 (2)
O3W—Dy1—N4	84.5 (2)	O22—Mo11—O4	83.42 (19)
O34—Dy1—N4	123.0 (2)	O17—Mo11—O4	73.05 (18)
O2W—Dy1—N4	155.2 (2)	O45—Mo11—O4	83.94 (19)
O18—Dy1—N4	87.1 (2)	O7—Mo11—O4	73.24 (18)
N3—Dy1—N4	61.6 (2)	O50—Mo12—O12	104.2 (3)
O1W—Dy1—N5	80.2 (2)	O50—Mo12—O16	102.6 (3)
O3—Dy1—N5	152.5 (2)	O12—Mo12—O16	89.4 (2)
O3W—Dy1—N5	68.7 (2)	O50—Mo12—O36	98.8 (2)
O34—Dy1—N5	63.74 (19)	O12—Mo12—O36	156.7 (2)
O2W—Dy1—N5	118.2 (2)	O16—Mo12—O36	89.7 (2)
O18—Dy1—N5	129.1 (2)	O50—Mo12—O21	99.6 (3)
N3—Dy1—N5	119.8 (2)	O12—Mo12—O21	88.7 (2)
N4—Dy1—N5	61.1 (2)	O16—Mo12—O21	157.5 (2)
O38—Mo1—O32	102.3 (3)	O36—Mo12—O21	83.3 (2)
O38—Mo1—O28	101.1 (3)	O50—Mo12—O2	168.3 (2)
O32—Mo1—O28	92.0 (2)	O12—Mo12—O2	84.86 (19)
O38—Mo1—O25	101.9 (3)	O16—Mo12—O2	84.7 (2)
O32—Mo1—O25	90.9 (2)	O36—Mo12—O2	71.84 (19)
O28—Mo1—O25	155.6 (2)	O21—Mo12—O2	72.81 (18)
O38—Mo1—O22	102.7 (2)	O5—P1—O4	109.5 (3)
O32—Mo1—O22	155.0 (2)	O5—P1—O2	109.5 (3)
O28—Mo1—O22	81.9 (2)	O4—P1—O2	109.3 (3)
O25—Mo1—O22	85.3 (2)	O5—P1—O1	109.0 (3)
O38—Mo1—O5	173.2 (3)	O4—P1—O1	109.8 (3)
O32—Mo1—O5	73.70 (19)	O2—P1—O1	109.7 (3)
O28—Mo1—O5	84.58 (19)	P1—O1—Mo6	125.7 (3)
O25—Mo1—O5	73.04 (18)	P1—O1—Mo8	126.0 (3)
O22—Mo1—O5	81.55 (18)	Mo6—O1—Mo8	90.88 (15)
O24—Mo2—O14	103.3 (2)	P1—O1—Mo2	125.8 (3)
O24—Mo2—O26	101.1 (2)	Mo6—O1—Mo2	88.15 (15)
O14—Mo2—O26	91.9 (2)	Mo8—O1—Mo2	88.39 (15)
O24—Mo2—O15	103.5 (2)	P1—O2—Mo7	127.8 (3)
O14—Mo2—O15	85.0 (2)	P1—O2—Mo12	124.1 (3)
O26—Mo2—O15	155.3 (2)	Mo7—O2—Mo12	89.98 (16)
O24—Mo2—O41	101.1 (2)	P1—O2—Mo10	125.9 (3)
O14—Mo2—O41	155.4 (2)	Mo7—O2—Mo10	87.99 (15)
O26—Mo2—O41	86.3 (2)	Mo12—O2—Mo10	89.23 (15)
O15—Mo2—O41	86.5 (2)	C1—O3—Dy1	123.7 (5)
O24—Mo2—O1	170.7 (2)	P1—O4—Mo11	126.3 (3)
O14—Mo2—O1	84.07 (19)	P1—O4—Mo5	127.3 (3)
O26—Mo2—O1	72.63 (18)	Mo11—O4—Mo5	88.39 (16)
O15—Mo2—O1	82.65 (18)	P1—O4—Mo4	125.0 (3)
O41—Mo2—O1	71.95 (19)	Mo11—O4—Mo4	89.76 (15)
O35—Mo3—O6	105.2 (3)	Mo5—O4—Mo4	87.92 (15)
O35—Mo3—O33	102.5 (3)	P1—O5—Mo3	126.1 (3)
O6—Mo3—O33	93.6 (2)	P1—O5—Mo9	126.2 (3)
O35—Mo3—O19	102.2 (3)	Mo3—O5—Mo9	87.99 (16)
O6—Mo3—O19	85.5 (2)	P1—O5—Mo1	125.8 (3)
O33—Mo3—O19	154.6 (2)	Mo3—O5—Mo1	88.63 (16)
O35—Mo3—O32	99.0 (3)	Mo9—O5—Mo1	90.04 (16)
O6—Mo3—O32	155.1 (2)	Mo3—O6—Mo8	155.2 (3)
O33—Mo3—O32	86.6 (2)	Mo5—O7—Mo11	123.3 (3)
O19—Mo3—O32	83.8 (2)	Mo7—O8—Mo10	124.6 (3)
O35—Mo3—O5	169.5 (2)	Mo6—O9—Mo5	155.8 (3)
O6—Mo3—O5	84.47 (19)	Mo5—O10—Mo4	125.4 (3)
O33—Mo3—O5	72.23 (19)	Mo12—O12—Mo5	151.1 (3)
O19—Mo3—O5	82.42 (19)	Mo9—O14—Mo2	154.9 (3)
O32—Mo3—O5	71.87 (19)	Mo4—O15—Mo2	150.3 (3)
O11—Mo4—O15	104.1 (2)	Mo12—O16—Mo6	147.7 (3)
O11—Mo4—O27	103.7 (2)	Mo11—O17—Mo4	126.1 (3)
O15—Mo4—O27	89.5 (2)	Mo7—O18—Dy1	159.8 (3)
O11—Mo4—O10	100.7 (2)	Mo7—O19—Mo3	150.6 (3)
O15—Mo4—O10	90.5 (2)	Mo10—O21—Mo12	124.9 (3)
O27—Mo4—O10	154.9 (2)	Mo11—O22—Mo1	154.5 (3)
O11—Mo4—O17	100.0 (2)	Mo1—O25—Mo9	123.8 (3)
O15—Mo4—O17	155.9 (2)	Mo8—O26—Mo2	126.0 (3)
O27—Mo4—O17	86.4 (2)	Mo4—O27—Mo9	147.9 (3)
O10—Mo4—O17	83.5 (2)	Mo10—O28—Mo1	153.5 (3)
O11—Mo4—O4	169.2 (2)	Mo8—O29—Mo7	147.5 (3)
O15—Mo4—O4	84.78 (19)	Mo1—O32—Mo3	125.6 (3)
O27—Mo4—O4	82.26 (19)	Mo9—O33—Mo3	127.6 (3)
O10—Mo4—O4	72.74 (18)	C9—O34—Dy1	122.5 (5)
O17—Mo4—O4	71.10 (18)	Mo7—O36—Mo12	124.7 (3)
O20—Mo5—O10	101.4 (2)	Mo6—O41—Mo2	125.6 (3)
O20—Mo5—O7	102.3 (3)	Mo8—O43—Mo6	123.9 (2)
O10—Mo5—O7	91.6 (2)	Mo10—O45—Mo11	148.3 (3)
O20—Mo5—O9	101.5 (2)	C1—N1—H1A	120.0
O10—Mo5—O9	88.7 (2)	C1—N1—H1B	120.0
O7—Mo5—O9	155.8 (2)	H1A—N1—H1B	120.0
O20—Mo5—O12	102.0 (2)	C1—N2—N3	115.4 (6)
O10—Mo5—O12	156.2 (2)	C1—N2—H2A	122.3
O7—Mo5—O12	88.1 (2)	N3—N2—H2A	122.3
O9—Mo5—O12	82.1 (2)	C2—N3—N2	119.6 (7)
O20—Mo5—O4	174.0 (2)	C2—N3—Dy1	124.3 (5)
O10—Mo5—O4	73.92 (19)	N2—N3—Dy1	114.2 (4)
O7—Mo5—O4	74.41 (19)	C7—N4—C3	118.4 (6)
O9—Mo5—O4	82.40 (19)	C7—N4—Dy1	121.1 (5)
O12—Mo5—O4	83.05 (18)	C3—N4—Dy1	120.5 (5)
O31—Mo6—O41	102.0 (3)	C8—N5—N6	120.8 (6)
O31—Mo6—O9	102.5 (2)	C8—N5—Dy1	125.4 (5)
O41—Mo6—O9	94.6 (2)	N6—N5—Dy1	113.4 (4)
O31—Mo6—O16	101.5 (3)	C9—N6—N5	116.8 (6)
O41—Mo6—O16	156.0 (2)	C9—N6—H6B	121.6
O9—Mo6—O16	84.9 (2)	N5—N6—H6B	121.6
O31—Mo6—O43	100.9 (2)	C9—N7—H7A	120.0
O41—Mo6—O43	88.0 (2)	C9—N7—H7B	120.0
O9—Mo6—O43	155.3 (2)	H7A—N7—H7B	120.0
O16—Mo6—O43	82.9 (2)	O3—C1—N1	123.4 (8)
O31—Mo6—O1	172.1 (2)	O3—C1—N2	120.9 (7)
O41—Mo6—O1	74.26 (19)	N1—C1—N2	115.6 (8)
O9—Mo6—O1	84.86 (19)	N3—C2—C3	113.6 (7)
O16—Mo6—O1	81.80 (19)	N3—C2—C10	123.7 (7)
O43—Mo6—O1	72.26 (18)	C3—C2—C10	122.6 (7)
O18—Mo7—O8	100.5 (2)	N4—C3—C4	122.0 (7)
O18—Mo7—O19	102.3 (2)	N4—C3—C2	116.4 (6)
O8—Mo7—O19	91.1 (2)	C4—C3—C2	121.5 (7)
O18—Mo7—O36	100.5 (2)	C3—C4—C5	119.1 (8)
O8—Mo7—O36	89.5 (2)	C3—C4—H4A	120.5
O19—Mo7—O36	156.7 (2)	C5—C4—H4A	120.5
O18—Mo7—O29	101.7 (2)	C6—C5—C4	119.2 (8)
O8—Mo7—O29	157.8 (2)	C6—C5—H5A	120.4
O19—Mo7—O29	86.1 (2)	C4—C5—H5A	120.4
O36—Mo7—O29	84.7 (2)	C5—C6—C7	119.7 (8)
O18—Mo7—O2	172.1 (2)	C5—C6—H6A	120.2
O8—Mo7—O2	74.96 (19)	C7—C6—H6A	120.2
O19—Mo7—O2	84.32 (19)	N4—C7—C6	121.5 (8)
O36—Mo7—O2	73.35 (18)	N4—C7—C8	116.8 (7)
O29—Mo7—O2	82.84 (18)	C6—C7—C8	121.6 (7)
O23—Mo8—O6	103.2 (3)	N5—C8—C7	113.9 (7)
O23—Mo8—O26	100.5 (3)	N5—C8—C11	125.3 (7)
O6—Mo8—O26	90.7 (2)	C7—C8—C11	120.8 (7)
O23—Mo8—O43	101.2 (3)	O34—C9—N6	121.8 (7)
O6—Mo8—O43	155.4 (2)	O34—C9—N7	122.4 (7)
O26—Mo8—O43	88.0 (2)	N6—C9—N7	115.7 (7)
O23—Mo8—O29	103.2 (3)	C2—C10—H10A	109.5
O6—Mo8—O29	85.2 (2)	C2—C10—H10B	109.5
O26—Mo8—O29	156.3 (2)	H10A—C10—H10B	109.5
O43—Mo8—O29	86.1 (2)	C2—C10—H10C	109.5
O23—Mo8—O1	170.7 (2)	H10A—C10—H10C	109.5
O6—Mo8—O1	83.77 (19)	H10B—C10—H10C	109.5
O26—Mo8—O1	73.00 (18)	C8—C11—H11A	109.5
O43—Mo8—O1	72.42 (18)	C8—C11—H11B	109.5
O29—Mo8—O1	83.37 (18)	H11A—C11—H11B	109.5
O47—Mo9—O14	103.4 (3)	C8—C11—H11C	109.5
O47—Mo9—O33	102.7 (3)	H11A—C11—H11C	109.5
O14—Mo9—O33	91.6 (2)	H11B—C11—H11C	109.5
O47—Mo9—O27	102.7 (3)	Dy1—O1W—H1WA	123.7
O14—Mo9—O27	85.5 (2)	Dy1—O1W—H1WB	124.9
O33—Mo9—O27	154.4 (2)	H1WA—O1W—H1WB	109.3
O47—Mo9—O25	100.8 (3)	Dy1—O2W—H2WA	116.5
O14—Mo9—O25	155.4 (2)	Dy1—O2W—H2WB	117.2
O33—Mo9—O25	87.6 (2)	H2WA—O2W—H2WB	109.3
O27—Mo9—O25	84.7 (2)	Dy1—O3W—H3WA	124.5
O47—Mo9—O5	171.5 (2)	Dy1—O3W—H3WB	122.8
O14—Mo9—O5	83.82 (19)	H3WA—O3W—H3WB	112.7
O33—Mo9—O5	72.23 (19)	H4WA—O4W—H4WB	98.1
O27—Mo9—O5	82.16 (19)	H5WA—O5W—H5WB	96.4
O25—Mo9—O5	72.51 (19)	H6WA—O6W—H6WB	98.6
O37—Mo10—O45	102.9 (2)	H7WA—O7W—H7WB	98.7
O37—Mo10—O28	102.4 (3)	H8WA—O8W—H8WB	110.7
O45—Mo10—O28	86.6 (2)	H8WC—O8WA—H8WD	111.3

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O26^i	0.86	2.18	2.864 (8)	137
N6—H6B···O45^ii	0.86	2.38	3.112 (9)	143
N7—H7A···O32^iii	0.86	2.54	3.189 (10)	133
N7—H7A···O35^iii	0.86	2.46	3.280 (10)	158
N7—H7B···O7^ii	0.86	2.42	3.277 (10)	176
C6—H6A···O47^iv	0.93	2.45	3.140 (11)	131
C10—H10B···O23	0.96	2.59	3.489 (11)	156

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