Tris[bis­(μ-1,10-phenanthrolin-2-olato)dicopper(I)] monosodium trihydrogen β-octa­molybdate hemihydrate

Li, M.-X.; Ma, P.-T.; Wang, J.-P.

doi:10.1107/S1600536806037433

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Tris[bis(μ-1,10-phenanthrolin-2-olato)dicopper(I)] monosodium trihydrogen β-octamolybdate hemihydrate

M.-X. Li, P.-T. Ma and J.-P. Wang

The title compound, Na[H₃Mo₈O₂₆][Cu₂(C₁₂H₇N₂O)₂]₃·0.5H₂O, contains neutral dinuclear copper(I) complexes and infinite chain-like polyoxoanions comprising β-[Mo₈O₂₆]⁴⁻ units linked by Na⁺ cations which lie on centres of inversion. The polyoxoanion chains are protonated, rendering them neutral.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806037433/bi2061sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806037433/bi2061Isup2.hkl Contains datablock I

CCDC reference: 623997

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.015 Å
H-atom completeness 92%
Disorder in solvent or counterion
R factor = 0.058
wR factor = 0.159
Data-to-parameter ratio = 11.4

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.95
PLAT430_ALERT_2_B Short Inter D...A Contact  O2     ..  O2W     ..       2.72 Ang.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.31
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.75 Ratio
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      12.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) .....       <O1W
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) .....       <O2W
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         15
PLAT432_ALERT_2_C Short Inter X...Y Contact  C5     ..  C35     ..       3.16 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C16    ..  C34     ..       3.18 Ang.

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C72 H46 Cu6 Mo8 N12 Na1 O32.5
            Atom count from the _atom_site data:  C72 H42 Cu6 Mo8 N12 Na1 O32.5
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    1
           From the CIF: _chemical_formula_sum  C72 H46 Cu6 Mo8 N12 Na O32.50
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         72.00     72.00    0.00
           H         46.00     42.00    4.00
           Cu         6.00      6.00    0.00
           Mo         8.00      8.00    0.00
           N         12.00     12.00    0.00
           Na         1.00      1.00    0.00
           O         32.50     32.50    0.00
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
  12 ALERT level C = Check and explain
   5 ALERT level G = General alerts; check

   7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   8 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

Tris[bis(µ-1,10-phenanthroline-2-olato)dicopper(I)] monosodium trihydrogen β-octamolybdate hemihydrate top

Crystal data top

Na[H₃Mo₈O₂₆][Cu₂(C₁₂H₇N₂O)₂]₃·0.5H₂O	Z = 1
M_r = 2770.98	F(000) = 1340
Triclinic, P1	D_x = 2.259 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.640 (4) Å	Cell parameters from 250 reflections
b = 13.651 (4) Å	θ = 2.5–25°
c = 15.952 (5) Å	µ = 2.82 mm⁻¹
α = 84.309 (4)°	T = 293 K
β = 78.972 (4)°	Block, green
γ = 82.091 (2)°	0.18 × 0.16 × 0.15 mm
V = 2035.1 (11) Å³

Data collection top

Bruker SMART APEX CCD diffractometer	6828 independent reflections
Radiation source: sealed tube	4626 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.031
φ and ω scans	θ_max = 25.0°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→11
T_min = 0.612, T_max = 0.657	k = −16→16
10029 measured reflections	l = −15→18

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.059	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.159	H-atom parameters constrained
S = 1.00	w = 1/[σ²(F_o²) + (0.0899P)²] where P = (F_o² + 2F_c²)/3
6828 reflections	(Δ/σ)_max < 0.001
600 parameters	Δρ_max = 2.28 e Å⁻³
0 restraints	Δρ_min = −0.99 e Å⁻³

Special details top

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

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0.5000	0.0000	0.5000	0.0492 (15)
Mo1	0.12760 (8)	−0.06625 (5)	0.64755 (5)	0.0264 (2)
Mo2	0.26405 (8)	−0.21494 (5)	0.49942 (5)	0.0278 (2)
Mo3	0.21953 (8)	−0.03747 (5)	0.35330 (5)	0.0267 (2)
Mo4	0.08165 (7)	0.10838 (5)	0.50154 (4)	0.01874 (19)
Cu1	0.15672 (12)	−0.47962 (8)	1.03995 (7)	0.0337 (3)
Cu2	0.20685 (13)	−0.63161 (8)	0.96552 (8)	0.0364 (3)
Cu3	0.49671 (12)	−0.57473 (8)	0.04740 (7)	0.0336 (3)
O1	0.2918 (7)	−0.0291 (5)	0.6346 (4)	0.0404 (16)
O2	0.0687 (8)	−0.0817 (5)	0.7543 (4)	0.0483 (18)
O3	0.3047 (7)	−0.3399 (5)	0.4988 (4)	0.0456 (17)
O4	0.4204 (7)	−0.1706 (4)	0.5000 (4)	0.0367 (15)
O5	0.3763 (6)	−0.0037 (4)	0.3686 (4)	0.0398 (16)
O6	0.2279 (8)	−0.0330 (5)	0.2462 (4)	0.0502 (19)
O7	0.2490 (6)	0.1365 (5)	0.5025 (4)	0.0376 (16)
O8	−0.0271 (6)	0.2221 (4)	0.5021 (4)	0.0307 (14)
O9	0.0206 (6)	0.0652 (4)	0.6226 (4)	0.0267 (13)
O10	0.1763 (6)	−0.1988 (4)	0.6176 (4)	0.0302 (14)
O11	0.2484 (6)	−0.1758 (4)	0.3828 (4)	0.0320 (14)
O12	0.0970 (6)	0.0894 (4)	0.3802 (3)	0.0230 (13)
O13	0.1348 (6)	−0.0507 (4)	0.5008 (3)	0.0247 (13)
O1A	0.1798 (8)	−0.4021 (5)	0.9368 (4)	0.0467 (18)
O2A	0.1838 (7)	−0.7097 (5)	1.0691 (4)	0.0439 (17)
O3A	0.4700 (7)	−0.3441 (4)	0.0441 (4)	0.0402 (16)
N1	0.2523 (9)	−0.7366 (6)	0.8788 (5)	0.039 (2)
N2	0.2166 (8)	−0.5415 (6)	0.8673 (5)	0.0302 (17)
N3	0.1066 (8)	−0.3712 (6)	1.1254 (5)	0.0354 (19)
N4	0.1379 (8)	−0.5696 (6)	1.1384 (5)	0.0321 (18)
N5	0.4860 (8)	−0.6790 (5)	0.1481 (5)	0.0368 (19)
N6	0.4535 (7)	−0.4817 (5)	0.1339 (5)	0.0301 (17)
C1	0.2751 (13)	−0.8348 (8)	0.8871 (9)	0.062 (3)
H1A	0.2665	−0.8660	0.9421	0.075*
C2	0.3111 (15)	−0.8930 (10)	0.8185 (11)	0.077 (4)
H2A	0.3215	−0.9618	0.8279	0.093*
C3	0.3312 (13)	−0.8508 (9)	0.7378 (11)	0.069 (4)
H3A	0.3595	−0.8897	0.6915	0.083*
C4	0.3085 (11)	−0.7456 (8)	0.7246 (8)	0.051 (3)
C5	0.2710 (9)	−0.6932 (7)	0.7982 (6)	0.035 (2)
C6	0.3266 (11)	−0.6882 (11)	0.6415 (8)	0.058 (3)
H6A	0.3544	−0.7212	0.5916	0.070*
C7	0.3040 (11)	−0.5898 (9)	0.6362 (6)	0.046 (3)
H7A	0.3142	−0.5553	0.5825	0.055*
C8	0.2640 (9)	−0.5349 (8)	0.7120 (6)	0.041 (3)
C9	0.2493 (10)	−0.5865 (7)	0.7914 (6)	0.033 (2)
C10	0.2425 (10)	−0.4308 (8)	0.7103 (6)	0.041 (3)
H10A	0.2485	−0.3932	0.6581	0.049*
C11	0.2127 (10)	−0.3848 (8)	0.7848 (7)	0.041 (3)
H11A	0.1989	−0.3159	0.7838	0.049*
C12	0.2031 (9)	−0.4437 (6)	0.8648 (6)	0.030 (2)
C13	0.0947 (10)	−0.2732 (7)	1.1154 (7)	0.038 (2)
H13A	0.1096	−0.2423	1.0603	0.046*
C14	0.0603 (11)	−0.2144 (7)	1.1857 (8)	0.049 (3)
H14A	0.0513	−0.1456	1.1774	0.059*
C15	0.0399 (11)	−0.2605 (8)	1.2675 (8)	0.051 (3)
H15A	0.0159	−0.2217	1.3140	0.061*
C16	0.0542 (9)	−0.3629 (8)	1.2823 (6)	0.039 (2)
C17	0.0907 (9)	−0.4184 (7)	1.2052 (6)	0.031 (2)
C18	0.0391 (10)	−0.4182 (9)	1.3615 (7)	0.045 (3)
H18A	0.0189	−0.3848	1.4113	0.054*
C19	0.0529 (10)	−0.5184 (8)	1.3682 (6)	0.039 (2)
H19A	0.0406	−0.5523	1.4221	0.047*
C20	0.0866 (10)	−0.5738 (7)	1.2923 (6)	0.038 (2)
C21	0.1043 (9)	−0.5210 (6)	1.2136 (6)	0.028 (2)
C22	0.1044 (10)	−0.6793 (7)	1.2941 (6)	0.039 (2)
H22A	0.0958	−0.7167	1.3464	0.047*
C23	0.1332 (10)	−0.7252 (7)	1.2213 (7)	0.044 (3)
H23A	0.1425	−0.7940	1.2226	0.052*
C24	0.1495 (10)	−0.6657 (7)	1.1406 (6)	0.034 (2)
C25	0.5067 (12)	−0.7772 (7)	0.1523 (7)	0.052 (3)
H25A	0.5296	−0.8091	0.1017	0.062*
C26	0.4950 (13)	−0.8344 (7)	0.2307 (8)	0.055 (3)
H26A	0.5037	−0.9032	0.2317	0.066*
C27	0.4705 (11)	−0.7881 (7)	0.3072 (8)	0.050 (3)
H27A	0.4707	−0.8251	0.3594	0.060*
C28	0.4455 (9)	−0.6843 (7)	0.3033 (6)	0.034 (2)
C29	0.4571 (9)	−0.6326 (6)	0.2231 (5)	0.027 (2)
C30	0.4143 (10)	−0.6281 (8)	0.3773 (6)	0.042 (3)
H30A	0.4078	−0.6613	0.4314	0.051*
C31	0.3944 (10)	−0.5295 (8)	0.3701 (6)	0.040 (2)
H31A	0.3734	−0.4957	0.4197	0.049*
C32	0.4043 (9)	−0.4730 (7)	0.2882 (6)	0.029 (2)
C33	0.4387 (9)	−0.5280 (7)	0.2157 (6)	0.029 (2)
C34	0.3880 (9)	−0.3721 (7)	0.2745 (6)	0.038 (2)
H34A	0.3620	−0.3338	0.3213	0.045*
C35	0.4087 (9)	−0.3259 (7)	0.1936 (6)	0.032 (2)
H35A	0.3991	−0.2570	0.1857	0.038*
C36	0.4458 (9)	−0.3853 (7)	0.1206 (6)	0.028 (2)
O1W	0.371 (8)	−0.038 (5)	0.040 (5)	0.08 (2)*	0.125
O2W	0.028 (6)	−0.138 (4)	0.925 (3)	0.046 (14)*	0.125

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.053 (4)	0.049 (4)	0.049 (4)	−0.014 (3)	−0.015 (3)	−0.002 (3)
Mo1	0.0278 (4)	0.0238 (4)	0.0285 (5)	−0.0002 (3)	−0.0089 (3)	−0.0034 (3)
Mo2	0.0269 (4)	0.0227 (4)	0.0326 (5)	0.0028 (3)	−0.0056 (3)	−0.0042 (3)
Mo3	0.0247 (4)	0.0257 (4)	0.0274 (5)	−0.0009 (3)	0.0001 (3)	−0.0026 (3)
Mo4	0.0180 (4)	0.0164 (4)	0.0223 (4)	−0.0038 (3)	−0.0027 (3)	−0.0031 (3)
Cu1	0.0398 (7)	0.0324 (7)	0.0297 (7)	−0.0082 (5)	−0.0038 (5)	−0.0056 (5)
Cu2	0.0421 (7)	0.0276 (6)	0.0389 (7)	−0.0044 (5)	−0.0044 (6)	−0.0047 (5)
Cu3	0.0392 (7)	0.0313 (7)	0.0298 (7)	−0.0058 (5)	−0.0034 (5)	−0.0029 (5)
O1	0.032 (4)	0.040 (4)	0.051 (4)	0.000 (3)	−0.012 (3)	−0.007 (3)
O2	0.059 (5)	0.047 (4)	0.039 (4)	−0.006 (4)	−0.010 (4)	−0.005 (3)
O3	0.046 (4)	0.041 (4)	0.045 (4)	0.010 (3)	−0.007 (3)	−0.005 (3)
O4	0.037 (4)	0.037 (4)	0.036 (4)	−0.002 (3)	−0.008 (3)	−0.005 (3)
O5	0.028 (4)	0.035 (4)	0.055 (4)	−0.007 (3)	0.002 (3)	−0.010 (3)
O6	0.065 (5)	0.044 (4)	0.038 (4)	0.002 (4)	−0.004 (4)	−0.008 (3)
O7	0.030 (4)	0.039 (4)	0.046 (4)	−0.007 (3)	−0.009 (3)	−0.008 (3)
O8	0.035 (4)	0.021 (3)	0.035 (4)	−0.003 (3)	−0.004 (3)	−0.005 (2)
O9	0.027 (3)	0.026 (3)	0.026 (3)	−0.002 (3)	−0.002 (3)	−0.008 (2)
O10	0.035 (4)	0.022 (3)	0.031 (4)	0.004 (3)	−0.005 (3)	−0.003 (2)
O11	0.034 (4)	0.030 (3)	0.030 (4)	−0.005 (3)	0.002 (3)	−0.005 (3)
O12	0.031 (3)	0.015 (3)	0.021 (3)	0.001 (2)	−0.005 (3)	0.000 (2)
O13	0.018 (3)	0.024 (3)	0.034 (4)	−0.007 (2)	−0.006 (3)	−0.002 (3)
O1A	0.070 (5)	0.031 (4)	0.041 (4)	−0.016 (4)	−0.009 (4)	−0.001 (3)
O2A	0.056 (5)	0.029 (4)	0.046 (5)	−0.004 (3)	−0.009 (4)	−0.002 (3)
O3A	0.063 (5)	0.030 (4)	0.030 (4)	−0.008 (3)	−0.009 (3)	−0.007 (3)
N1	0.042 (5)	0.027 (4)	0.049 (6)	0.000 (4)	−0.013 (4)	−0.005 (4)
N2	0.028 (4)	0.040 (5)	0.022 (4)	−0.006 (3)	−0.001 (3)	−0.004 (3)
N3	0.034 (5)	0.035 (5)	0.040 (5)	−0.006 (4)	−0.007 (4)	−0.010 (4)
N4	0.034 (4)	0.034 (5)	0.029 (4)	−0.008 (4)	−0.006 (3)	−0.002 (3)
N5	0.036 (5)	0.028 (4)	0.042 (5)	0.001 (4)	0.000 (4)	−0.004 (4)
N6	0.023 (4)	0.030 (4)	0.034 (5)	0.002 (3)	0.003 (3)	−0.011 (3)
C1	0.069 (8)	0.033 (6)	0.084 (10)	0.009 (6)	−0.023 (7)	−0.002 (6)
C2	0.080 (10)	0.038 (7)	0.115 (13)	−0.004 (7)	−0.006 (9)	−0.039 (8)
C3	0.046 (7)	0.042 (7)	0.120 (13)	0.012 (6)	−0.008 (8)	−0.046 (8)
C4	0.026 (6)	0.058 (7)	0.073 (9)	0.003 (5)	−0.009 (5)	−0.032 (6)
C5	0.022 (5)	0.042 (6)	0.043 (6)	−0.010 (4)	0.004 (4)	−0.018 (5)
C6	0.033 (6)	0.102 (11)	0.045 (7)	−0.001 (6)	−0.008 (5)	−0.033 (7)
C7	0.041 (6)	0.062 (8)	0.030 (6)	−0.002 (5)	0.000 (5)	−0.001 (5)
C8	0.017 (5)	0.070 (8)	0.035 (6)	−0.008 (5)	0.002 (4)	−0.007 (5)
C9	0.031 (5)	0.027 (5)	0.040 (6)	0.008 (4)	−0.010 (4)	−0.006 (4)
C10	0.031 (6)	0.057 (7)	0.034 (6)	−0.013 (5)	−0.006 (4)	0.010 (5)
C11	0.034 (6)	0.048 (6)	0.041 (6)	−0.010 (5)	−0.012 (5)	0.013 (5)
C12	0.024 (5)	0.027 (5)	0.040 (6)	0.003 (4)	−0.006 (4)	−0.013 (4)
C13	0.037 (6)	0.034 (6)	0.047 (6)	−0.007 (4)	−0.012 (5)	−0.008 (5)
C14	0.043 (6)	0.025 (6)	0.083 (9)	0.006 (5)	−0.017 (6)	−0.021 (6)
C15	0.038 (6)	0.041 (6)	0.080 (9)	−0.001 (5)	−0.013 (6)	−0.033 (6)
C16	0.013 (5)	0.062 (7)	0.040 (6)	−0.004 (4)	0.006 (4)	−0.022 (5)
C17	0.019 (5)	0.042 (6)	0.036 (6)	−0.001 (4)	−0.006 (4)	−0.016 (4)
C18	0.032 (6)	0.067 (8)	0.038 (6)	−0.005 (5)	0.001 (5)	−0.020 (5)
C19	0.031 (6)	0.058 (7)	0.024 (5)	−0.005 (5)	0.005 (4)	−0.004 (5)
C20	0.022 (5)	0.047 (6)	0.040 (6)	−0.004 (4)	0.000 (4)	0.000 (5)
C21	0.024 (5)	0.023 (5)	0.034 (5)	0.001 (4)	−0.002 (4)	−0.002 (4)
C22	0.037 (6)	0.047 (6)	0.029 (6)	−0.016 (5)	0.005 (4)	0.012 (5)
C23	0.038 (6)	0.030 (6)	0.062 (8)	0.002 (4)	−0.011 (5)	−0.003 (5)
C24	0.038 (6)	0.028 (5)	0.034 (6)	−0.005 (4)	0.000 (4)	−0.006 (4)
C25	0.069 (8)	0.036 (6)	0.045 (7)	−0.004 (5)	0.006 (6)	−0.006 (5)
C26	0.069 (8)	0.022 (5)	0.068 (8)	0.007 (5)	−0.013 (6)	0.006 (5)
C27	0.041 (6)	0.033 (6)	0.067 (8)	0.006 (5)	−0.007 (6)	0.015 (5)
C28	0.024 (5)	0.031 (5)	0.044 (6)	0.005 (4)	−0.011 (4)	0.004 (4)
C29	0.024 (5)	0.032 (5)	0.021 (5)	0.002 (4)	0.002 (4)	0.000 (4)
C30	0.039 (6)	0.056 (7)	0.028 (6)	0.002 (5)	−0.004 (4)	0.003 (5)
C31	0.040 (6)	0.049 (7)	0.031 (6)	0.009 (5)	−0.010 (5)	−0.011 (5)
C32	0.020 (5)	0.039 (6)	0.027 (5)	−0.006 (4)	−0.002 (4)	−0.001 (4)
C33	0.020 (5)	0.036 (5)	0.027 (5)	0.008 (4)	−0.003 (4)	−0.001 (4)
C34	0.023 (5)	0.046 (6)	0.042 (6)	0.000 (4)	−0.002 (4)	−0.005 (5)
C35	0.029 (5)	0.021 (5)	0.047 (6)	0.005 (4)	−0.008 (4)	−0.019 (4)
C36	0.024 (5)	0.034 (5)	0.027 (5)	−0.002 (4)	−0.001 (4)	−0.010 (4)

Geometric parameters (Å, º) top

Na1—O4	2.550 (6)	N5—C25	1.324 (12)
Na1—O4ⁱ	2.550 (6)	N5—C29	1.372 (11)
Na1—O5ⁱ	2.610 (6)	N6—C36	1.306 (11)
Na1—O5	2.610 (6)	N6—C33	1.384 (11)
Na1—O1	2.682 (6)	C1—C2	1.380 (17)
Na1—O1ⁱ	2.682 (6)	C1—H1A	0.930
Na1—O7ⁱ	2.840 (6)	C2—C3	1.346 (19)
Na1—O7	2.840 (6)	C2—H2A	0.930
Mo1—O2	1.690 (7)	C3—C4	1.423 (16)
Mo1—O1	1.698 (6)	C3—H3A	0.930
Mo1—O10	1.891 (6)	C4—C5	1.398 (14)
Mo1—O9	1.987 (6)	C4—C6	1.465 (17)
Mo1—O13	2.319 (5)	C5—C9	1.439 (13)
Mo1—O12ⁱⁱ	2.359 (6)	C6—C7	1.328 (15)
Mo1—Mo4	3.2104 (12)	C6—H6A	0.930
Mo2—O3	1.698 (6)	C7—C8	1.447 (14)
Mo2—O4	1.702 (6)	C7—H7A	0.930
Mo2—O11	1.912 (6)	C8—C9	1.379 (13)
Mo2—O10	1.934 (6)	C8—C10	1.406 (14)
Mo2—O8ⁱⁱ	2.304 (6)	C10—C11	1.363 (14)
Mo2—O13	2.410 (5)	C10—H10A	0.930
Mo3—O6	1.691 (7)	C11—C12	1.433 (13)
Mo3—O5	1.706 (6)	C11—H11A	0.930
Mo3—O11	1.895 (6)	C13—C14	1.406 (14)
Mo3—O12	1.992 (5)	C13—H13A	0.930
Mo3—O13	2.335 (6)	C14—C15	1.382 (16)
Mo3—O9ⁱⁱ	2.350 (6)	C14—H14A	0.930
Mo3—Mo4	3.2134 (12)	C15—C16	1.386 (14)
Mo4—O7	1.712 (6)	C15—H15A	0.930
Mo4—O8	1.749 (6)	C16—C18	1.399 (14)
Mo4—O12	1.953 (5)	C16—C17	1.469 (13)
Mo4—O9	1.965 (6)	C17—C21	1.384 (12)
Mo4—O13	2.162 (5)	C18—C19	1.352 (14)
Mo4—O13ⁱⁱ	2.337 (5)	C18—H18A	0.930
Cu1—O1A	1.860 (7)	C19—C20	1.450 (14)
Cu1—N4	1.892 (7)	C19—H19A	0.930
Cu1—N3	2.058 (8)	C20—C21	1.378 (13)
Cu1—Cu2	2.4374 (17)	C20—C22	1.425 (14)
Cu2—O2A	1.868 (6)	C22—C23	1.338 (14)
Cu2—N2	1.890 (7)	C22—H22A	0.930
Cu2—N1	2.037 (8)	C23—C24	1.446 (14)
Cu3—O3Aⁱⁱⁱ	1.873 (6)	C23—H23A	0.930
Cu3—N6	1.916 (7)	C25—C26	1.401 (14)
Cu3—N5	2.036 (7)	C25—H25A	0.930
Cu3—Cu3ⁱⁱⁱ	2.417 (2)	C26—C27	1.396 (15)
O8—Mo2ⁱⁱ	2.304 (6)	C26—H26A	0.930
O9—Mo3ⁱⁱ	2.350 (6)	C27—C28	1.402 (13)
O12—Mo1ⁱⁱ	2.359 (6)	C27—H27A	0.930
O13—Mo4ⁱⁱ	2.337 (5)	C28—C29	1.391 (12)
O1A—C12	1.299 (11)	C28—C30	1.433 (14)
O2A—C24	1.307 (11)	C29—C33	1.410 (12)
O3A—C36	1.284 (10)	C30—C31	1.330 (13)
O3A—Cu3ⁱⁱⁱ	1.873 (6)	C30—H30A	0.930
N1—C1	1.325 (13)	C31—C32	1.443 (13)
N1—C5	1.351 (12)	C31—H31A	0.930
N2—C12	1.321 (11)	C32—C34	1.365 (13)
N2—C9	1.375 (12)	C32—C33	1.403 (12)
N3—C13	1.324 (11)	C34—C35	1.372 (13)
N3—C17	1.359 (12)	C34—H34A	0.930
N4—C24	1.300 (11)	C35—C36	1.446 (12)
N4—C21	1.391 (11)	C35—H35A	0.930

O4—Na1—O4ⁱ	180.00 (8)	Mo4—O12—Mo1ⁱⁱ	109.7 (2)
O4—Na1—O5ⁱ	109.41 (19)	Mo3—O12—Mo1ⁱⁱ	104.6 (2)
O4ⁱ—Na1—O5ⁱ	70.59 (19)	Mo4—O13—Mo1	91.5 (2)
O4—Na1—O5	70.59 (19)	Mo4—O13—Mo3	91.12 (19)
O4ⁱ—Na1—O5	109.41 (19)	Mo1—O13—Mo3	161.7 (3)
O5ⁱ—Na1—O5	180.0	Mo4—O13—Mo4ⁱⁱ	104.0 (2)
O4—Na1—O1	70.02 (19)	Mo1—O13—Mo4ⁱⁱ	98.7 (2)
O4ⁱ—Na1—O1	109.98 (19)	Mo3—O13—Mo4ⁱⁱ	98.26 (19)
O5ⁱ—Na1—O1	76.61 (19)	Mo4—O13—Mo2	162.8 (3)
O5—Na1—O1	103.39 (19)	Mo1—O13—Mo2	86.28 (18)
O4—Na1—O1ⁱ	109.98 (19)	Mo3—O13—Mo2	85.92 (19)
O4ⁱ—Na1—O1ⁱ	70.02 (19)	Mo4ⁱⁱ—O13—Mo2	93.20 (17)
O5ⁱ—Na1—O1ⁱ	103.39 (19)	C12—O1A—Cu1	120.0 (6)
O5—Na1—O1ⁱ	76.61 (19)	C24—O2A—Cu2	118.7 (6)
O1—Na1—O1ⁱ	180.0	C36—O3A—Cu3ⁱⁱⁱ	118.1 (6)
O4—Na1—O7ⁱ	74.64 (18)	C1—N1—C5	117.0 (9)
O4ⁱ—Na1—O7ⁱ	105.36 (18)	C1—N1—Cu2	132.6 (8)
O5ⁱ—Na1—O7ⁱ	66.19 (19)	C5—N1—Cu2	110.3 (6)
O5—Na1—O7ⁱ	113.81 (19)	C12—N2—C9	118.8 (8)
O1—Na1—O7ⁱ	114.88 (18)	C12—N2—Cu2	127.3 (6)
O1ⁱ—Na1—O7ⁱ	65.12 (18)	C9—N2—Cu2	113.8 (6)
O4—Na1—O7	105.36 (18)	C13—N3—C17	120.4 (8)
O4ⁱ—Na1—O7	74.64 (18)	C13—N3—Cu1	132.7 (7)
O5ⁱ—Na1—O7	113.81 (19)	C17—N3—Cu1	106.8 (6)
O5—Na1—O7	66.19 (19)	C24—N4—C21	120.9 (8)
O1—Na1—O7	65.12 (18)	C24—N4—Cu1	127.1 (6)
O1ⁱ—Na1—O7	114.88 (18)	C21—N4—Cu1	112.0 (6)
O7ⁱ—Na1—O7	180.0 (3)	C25—N5—C29	118.6 (8)
O2—Mo1—O1	106.5 (3)	C25—N5—Cu3	132.2 (7)
O2—Mo1—O10	101.9 (3)	C29—N5—Cu3	109.1 (6)
O1—Mo1—O10	100.6 (3)	C36—N6—C33	121.6 (8)
O2—Mo1—O9	99.6 (3)	C36—N6—Cu3	126.0 (6)
O1—Mo1—O9	97.8 (3)	C33—N6—Cu3	112.3 (6)
O10—Mo1—O9	146.3 (2)	N1—C1—C2	123.4 (13)
O2—Mo1—O13	162.0 (3)	N1—C1—H1A	118.3
O1—Mo1—O13	91.2 (3)	C2—C1—H1A	118.3
O10—Mo1—O13	77.4 (2)	C3—C2—C1	120.3 (13)
O9—Mo1—O13	74.2 (2)	C3—C2—H2A	119.9
O2—Mo1—O12ⁱⁱ	91.0 (3)	C1—C2—H2A	119.9
O1—Mo1—O12ⁱⁱ	160.7 (2)	C2—C3—C4	119.0 (12)
O10—Mo1—O12ⁱⁱ	83.1 (2)	C2—C3—H3A	120.5
O9—Mo1—O12ⁱⁱ	70.8 (2)	C4—C3—H3A	120.5
O13—Mo1—O12ⁱⁱ	71.00 (18)	C5—C4—C3	116.4 (12)
O2—Mo1—Mo4	134.9 (2)	C5—C4—C6	117.7 (10)
O1—Mo1—Mo4	83.4 (2)	C3—C4—C6	125.9 (12)
O10—Mo1—Mo4	119.73 (17)	N1—C5—C4	123.9 (10)
O9—Mo1—Mo4	35.44 (16)	N1—C5—C9	115.6 (8)
O13—Mo1—Mo4	42.32 (13)	C4—C5—C9	120.5 (10)
O12ⁱⁱ—Mo1—Mo4	78.45 (12)	C7—C6—C4	121.1 (10)
O3—Mo2—O4	105.4 (3)	C7—C6—H6A	119.4
O3—Mo2—O11	102.7 (3)	C4—C6—H6A	119.4
O4—Mo2—O11	98.3 (3)	C6—C7—C8	121.5 (10)
O3—Mo2—O10	102.2 (3)	C6—C7—H7A	119.2
O4—Mo2—O10	98.6 (3)	C8—C7—H7A	119.2
O11—Mo2—O10	144.8 (3)	C9—C8—C10	117.0 (9)
O3—Mo2—O8ⁱⁱ	92.8 (3)	C9—C8—C7	118.9 (10)
O4—Mo2—O8ⁱⁱ	161.8 (2)	C10—C8—C7	124.0 (9)
O11—Mo2—O8ⁱⁱ	76.9 (2)	N2—C9—C8	123.6 (9)
O10—Mo2—O8ⁱⁱ	77.4 (2)	N2—C9—C5	116.2 (8)
O3—Mo2—O13	162.5 (3)	C8—C9—C5	120.2 (9)
O4—Mo2—O13	92.1 (2)	C11—C10—C8	120.3 (9)
O11—Mo2—O13	74.4 (2)	C11—C10—H10A	119.8
O10—Mo2—O13	74.4 (2)	C8—C10—H10A	119.8
O8ⁱⁱ—Mo2—O13	69.67 (18)	C10—C11—C12	119.3 (10)
O6—Mo3—O5	106.4 (3)	C10—C11—H11A	120.4
O6—Mo3—O11	102.2 (3)	C12—C11—H11A	120.4
O5—Mo3—O11	100.4 (3)	O1A—C12—N2	118.3 (8)
O6—Mo3—O12	100.5 (3)	O1A—C12—C11	120.8 (9)
O5—Mo3—O12	97.9 (3)	N2—C12—C11	120.9 (9)
O11—Mo3—O12	145.3 (2)	N3—C13—C14	121.8 (10)
O6—Mo3—O13	162.1 (3)	N3—C13—H13A	119.1
O5—Mo3—O13	91.3 (3)	C14—C13—H13A	119.1
O11—Mo3—O13	76.6 (2)	C15—C14—C13	118.9 (10)
O12—Mo3—O13	73.9 (2)	C15—C14—H14A	120.5
O6—Mo3—O9ⁱⁱ	90.9 (3)	C13—C14—H14A	120.5
O5—Mo3—O9ⁱⁱ	161.1 (3)	C14—C15—C16	122.1 (10)
O11—Mo3—O9ⁱⁱ	82.8 (2)	C14—C15—H15A	118.9
O12—Mo3—O9ⁱⁱ	71.0 (2)	C16—C15—H15A	118.9
O13—Mo3—O9ⁱⁱ	71.24 (19)	C15—C16—C18	127.6 (10)
O6—Mo3—Mo4	135.4 (2)	C15—C16—C17	115.3 (10)
O5—Mo3—Mo4	83.8 (2)	C18—C16—C17	117.2 (10)
O11—Mo3—Mo4	118.83 (18)	N3—C17—C21	119.1 (8)
O12—Mo3—Mo4	35.06 (15)	N3—C17—C16	121.5 (9)
O13—Mo3—Mo4	42.28 (13)	C21—C17—C16	119.4 (9)
O9ⁱⁱ—Mo3—Mo4	78.49 (14)	C19—C18—C16	122.4 (10)
O7—Mo4—O8	105.6 (3)	C19—C18—H18A	118.8
O7—Mo4—O12	100.5 (3)	C16—C18—H18A	118.8
O8—Mo4—O12	97.0 (2)	C18—C19—C20	120.8 (9)
O7—Mo4—O9	101.0 (3)	C18—C19—H19A	119.6
O8—Mo4—O9	96.9 (3)	C20—C19—H19A	119.6
O12—Mo4—O9	150.2 (2)	C21—C20—C22	117.9 (9)
O7—Mo4—O13	97.3 (3)	C21—C20—C19	117.9 (9)
O8—Mo4—O13	157.1 (2)	C22—C20—C19	124.2 (9)
O12—Mo4—O13	78.7 (2)	C20—C21—C17	122.3 (9)
O9—Mo4—O13	78.3 (2)	C20—C21—N4	120.7 (8)
O7—Mo4—O13ⁱⁱ	173.3 (2)	C17—C21—N4	116.9 (8)
O8—Mo4—O13ⁱⁱ	81.1 (2)	C23—C22—C20	120.8 (9)
O12—Mo4—O13ⁱⁱ	78.0 (2)	C23—C22—H22A	119.6
O9—Mo4—O13ⁱⁱ	78.2 (2)	C20—C22—H22A	119.6
O13—Mo4—O13ⁱⁱ	76.0 (2)	C22—C23—C24	118.7 (9)
O7—Mo4—Mo1	88.6 (2)	C22—C23—H23A	120.6
O8—Mo4—Mo1	132.81 (19)	C24—C23—H23A	120.6
O12—Mo4—Mo1	124.92 (15)	N4—C24—O2A	119.6 (8)
O9—Mo4—Mo1	35.91 (17)	N4—C24—C23	120.9 (9)
O13—Mo4—Mo1	46.22 (14)	O2A—C24—C23	119.4 (8)
O13ⁱⁱ—Mo4—Mo1	86.96 (13)	N5—C25—C26	121.9 (10)
O7—Mo4—Mo3	88.4 (2)	N5—C25—H25A	119.0
O8—Mo4—Mo3	132.84 (19)	C26—C25—H25A	119.0
O12—Mo4—Mo3	35.87 (15)	C27—C26—C25	120.0 (10)
O9—Mo4—Mo3	124.88 (16)	C27—C26—H26A	120.0
O13—Mo4—Mo3	46.60 (14)	C25—C26—H26A	120.0
O13ⁱⁱ—Mo4—Mo3	86.68 (14)	C26—C27—C28	118.1 (9)
Mo1—Mo4—Mo3	91.33 (3)	C26—C27—H27A	120.9
O1A—Cu1—N4	174.3 (3)	C28—C27—H27A	120.9
O1A—Cu1—N3	100.5 (3)	C29—C28—C27	118.3 (9)
N4—Cu1—N3	85.1 (3)	C29—C28—C30	118.1 (9)
O1A—Cu1—Cu2	91.5 (2)	C27—C28—C30	123.6 (9)
N4—Cu1—Cu2	82.9 (2)	N5—C29—C28	122.8 (8)
N3—Cu1—Cu2	168.0 (2)	N5—C29—C33	116.8 (7)
O2A—Cu2—N2	173.7 (3)	C28—C29—C33	120.4 (8)
O2A—Cu2—N1	101.6 (3)	C31—C30—C28	121.3 (9)
N2—Cu2—N1	84.0 (3)	C31—C30—H30A	119.3
O2A—Cu2—Cu1	91.6 (2)	C28—C30—H30A	119.3
N2—Cu2—Cu1	82.8 (2)	C30—C31—C32	122.4 (9)
N1—Cu2—Cu1	166.8 (2)	C30—C31—H31A	118.8
O3Aⁱⁱⁱ—Cu3—N6	174.3 (3)	C32—C31—H31A	118.8
O3Aⁱⁱⁱ—Cu3—N5	100.5 (3)	C34—C32—C33	117.2 (8)
N6—Cu3—N5	84.6 (3)	C34—C32—C31	126.6 (9)
O3Aⁱⁱⁱ—Cu3—Cu3ⁱⁱⁱ	92.4 (2)	C33—C32—C31	116.2 (8)
N6—Cu3—Cu3ⁱⁱⁱ	82.6 (2)	N6—C33—C32	121.2 (8)
N5—Cu3—Cu3ⁱⁱⁱ	167.1 (2)	N6—C33—C29	117.2 (8)
Mo1—O1—Na1	134.7 (3)	C32—C33—C29	121.6 (8)
Mo2—O4—Na1	135.9 (3)	C32—C34—C35	121.8 (9)
Mo3—O5—Na1	135.6 (3)	C32—C34—H34A	119.1
Mo4—O7—Na1	126.5 (3)	C35—C34—H34A	119.1
Mo4—O8—Mo2ⁱⁱ	116.0 (3)	C34—C35—C36	119.2 (9)
Mo4—O9—Mo1	108.6 (3)	C34—C35—H35A	120.4
Mo4—O9—Mo3ⁱⁱ	109.6 (2)	C36—C35—H35A	120.4
Mo1—O9—Mo3ⁱⁱ	105.2 (2)	O3A—C36—N6	120.7 (8)
Mo1—O10—Mo2	115.5 (3)	O3A—C36—C35	120.6 (8)
Mo3—O11—Mo2	116.3 (3)	N6—C36—C35	118.7 (8)
Mo4—O12—Mo3	109.1 (2)

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

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