Tris(2,2′-bipyridyl-κ²N,N′)nickel(II) β-octa­molybdate tetra­hydrate

The title compound, [Ni(C₁₀H₈N₂)₃]₂[Mo₈O₂₆]·4H₂O, was synthesized hydro­thermally as colorless crystalline blocks. The asymmetric unit consists of one cation, one half-anion and two water molecules; the anion is centrosymmetric.

Key indicators

• Single-crystal X-ray study
• T = 273 K
• Mean [sigma](C-C) = 0.005 Å
• H-atom completeness 86%
• R factor = 0.024
• wR factor = 0.072
• Data-to-parameter ratio = 18.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O14

Author Response: Hydrogen atoms from crystallization water molecule were not located in difference Fourier maps and were disregarded in the final model. H-atoms were not located.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O15

Author Response: Hydrogen atoms from crystallization water molecule were not located in difference Fourier maps and were disregarded in the final model. H-atoms were not located.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       2.00 Ratio
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.99
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT432_ALERT_2_C Short Inter X...Y Contact  O11    ..  C4      ..       2.95 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:C60 H56 Mo8 N12 Ni2 O30
            Atom count from the _atom_site data:  C60 H48 Mo8 N12 Ni2 O30
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    2
           From the CIF: _chemical_formula_sum  C60 H56 Mo8 N12 Ni2 O30
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        120.00    120.00    0.00
           H        112.00     96.00   16.00
           Mo        16.00     16.00    0.00
           N         24.00     24.00    0.00
           Ni         4.00      4.00    0.00
           O         60.00     60.00    0.00

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

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

---

Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); 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, 2000); software used to prepare material for publication: SHELXTL.

Tris(2,2'-bipyridyl-κ²N,N')nickel(II) β-octamolybdate tetrahydrate

Crystal data

[Ni(C10H8N2)3]2[Mo8O26]·4H2O	F(000) = 2264
Mr = 2310.10	Dx = 2.089 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 7772 reflections
a = 12.2823 (4) Å	θ = 2.4–28.3°
b = 13.7818 (4) Å	µ = 1.91 mm^−1
c = 21.6970 (6) Å	T = 273 K
β = 90.8703 (7)°	Block, colorless
V = 3672.28 (19) Å^3	0.24 × 0.20 × 0.14 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer	9119 independent reflections
Radiation source: fine-focus sealed tube	7347 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.045
φ and ω scans	θmax = 28.3°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −16→16
Tmin = 0.657, Tmax = 0.776	k = −18→18
36452 measured reflections	l = −28→28

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.072	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0361P)^2 + 0.5038P] where P = (Fo^2 + 2Fc^2)/3
9119 reflections	(Δ/σ)max = 0.005
505 parameters	Δρmax = 0.69 e Å^−3
24 restraints	Δρmin = −0.48 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.

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
Mo1	0.901617 (18)	0.534383 (15)	1.054832 (10)	0.02709 (6)
Mo2	0.913304 (18)	0.617884 (16)	0.902001 (10)	0.03113 (6)
Mo3	0.727849 (19)	0.459218 (17)	0.936603 (11)	0.03420 (6)
Mo4	1.082596 (19)	0.693407 (16)	1.018682 (11)	0.03262 (6)
Ni1	0.38567 (3)	0.96955 (2)	0.831308 (15)	0.02978 (8)
O1	0.92724 (16)	0.56760 (15)	0.83120 (9)	0.0418 (5)
O2	0.90859 (17)	0.73960 (14)	0.88863 (9)	0.0443 (5)
O3	1.08672 (18)	0.79604 (14)	0.97591 (10)	0.0506 (5)
O4	1.23086 (14)	0.65619 (13)	1.01866 (9)	0.0361 (4)
O5	1.06703 (16)	0.73233 (15)	1.09232 (9)	0.0462 (5)
O6	1.07475 (13)	0.52811 (11)	1.04517 (8)	0.0273 (4)
O7	0.89636 (16)	0.57937 (15)	1.12731 (8)	0.0391 (4)
O8	0.93059 (14)	0.39781 (12)	1.07143 (8)	0.0299 (4)
O9	0.92751 (14)	0.65145 (12)	1.00711 (8)	0.0291 (4)
O10	0.76564 (14)	0.59177 (13)	0.91943 (9)	0.0361 (4)
O11	0.73853 (17)	0.41367 (16)	0.86448 (9)	0.0478 (5)
O12	0.59163 (16)	0.46480 (16)	0.94854 (11)	0.0494 (5)
O13	0.76458 (14)	0.51910 (13)	1.03375 (8)	0.0341 (4)
O14	0.9120 (4)	0.0117 (4)	0.7657 (3)	0.1648 (19)
O15	0.0027 (5)	0.0604 (4)	0.1165 (3)	0.200 (2)
C1	0.4666 (2)	0.8791 (2)	0.71198 (13)	0.0378 (6)
H1	0.4023	0.8434	0.7124	0.045*
C2	0.6018 (2)	1.0525 (2)	0.81344 (14)	0.0379 (6)
C3	0.5834 (2)	0.9884 (2)	0.75967 (13)	0.0353 (6)
C4	0.1816 (2)	0.9000 (2)	0.76256 (14)	0.0455 (7)
H4	0.1827	0.9604	0.7434	0.055*
C5	0.2593 (3)	0.7912 (2)	0.83106 (13)	0.0429 (7)
C6	0.5355 (3)	0.8695 (2)	0.66233 (14)	0.0448 (7)
H6	0.5171	0.8290	0.6295	0.054*
C7	0.2515 (2)	1.1448 (2)	0.82641 (13)	0.0378 (6)
C8	0.3379 (2)	1.1269 (2)	0.73334 (14)	0.0423 (7)
H8	0.3850	1.0921	0.7085	0.051*
C9	0.6562 (3)	0.9787 (3)	0.71162 (15)	0.0512 (8)
H9	0.7221	1.0118	0.7128	0.061*
C10	0.5345 (3)	1.1089 (2)	0.90569 (14)	0.0453 (7)
H10	0.4809	1.1072	0.9355	0.054*
C11	0.2763 (3)	0.9827 (2)	0.95747 (15)	0.0517 (8)
H11	0.3105	0.9239	0.9659	0.062*
C12	0.2900 (3)	1.2096 (2)	0.70952 (15)	0.0484 (8)
H12	0.3053	1.2306	0.6699	0.058*
C13	0.3539 (3)	0.7707 (2)	0.87177 (14)	0.0444 (7)
C14	0.2386 (2)	1.1071 (2)	0.88926 (14)	0.0424 (7)
C15	0.2193 (3)	1.2598 (2)	0.74576 (17)	0.0572 (9)
H15	0.1849	1.3153	0.7307	0.069*
C16	0.1993 (3)	1.2277 (2)	0.80490 (16)	0.0544 (9)
H16	0.1514	1.2612	0.8300	0.065*
C17	0.5195 (3)	0.8273 (3)	0.90990 (15)	0.0550 (9)
H17	0.5703	0.8770	0.9137	0.066*
C18	0.6305 (3)	0.9201 (3)	0.66242 (15)	0.0529 (8)
H18	0.6776	0.9150	0.6294	0.064*
C19	0.6214 (3)	1.1714 (2)	0.91405 (16)	0.0527 (8)
H19	0.6261	1.2110	0.9487	0.063*
C20	0.6918 (3)	1.1137 (2)	0.81999 (17)	0.0555 (9)
H20	0.7458	1.1138	0.7904	0.067*
C21	0.7000 (3)	1.1736 (2)	0.87039 (18)	0.0597 (9)
H21	0.7590	1.2155	0.8747	0.072*
C22	0.5404 (3)	0.7383 (3)	0.93838 (17)	0.0700 (12)
H22	0.6055	0.7279	0.9598	0.084*
C23	0.4646 (4)	0.6675 (3)	0.93440 (19)	0.0767 (13)
H23	0.4766	0.6085	0.9541	0.092*
C24	0.3702 (4)	0.6824 (3)	0.90140 (17)	0.0664 (11)
H24	0.3176	0.6339	0.8988	0.080*
C25	0.1747 (3)	0.7257 (2)	0.82001 (18)	0.0610 (10)
H25	0.1724	0.6669	0.8409	0.073*
C26	0.0940 (3)	0.7499 (3)	0.77720 (19)	0.0699 (11)
H26	0.0375	0.7067	0.7688	0.084*
C27	0.0977 (3)	0.8367 (3)	0.74765 (17)	0.0602 (9)
H27	0.0453	0.8533	0.7181	0.072*
C28	0.2146 (3)	1.0244 (3)	1.00283 (16)	0.0668 (11)
H28	0.2061	0.9941	1.0407	0.080*
C29	0.1661 (4)	1.1116 (3)	0.99045 (19)	0.0837 (14)
H29	0.1256	1.1427	1.0205	0.100*
C30	0.1775 (4)	1.1529 (3)	0.93363 (18)	0.0756 (13)
H30	0.1440	1.2119	0.9248	0.091*
N1	0.48971 (17)	0.93841 (16)	0.75929 (10)	0.0314 (5)
N2	0.32034 (19)	1.09430 (16)	0.79022 (10)	0.0348 (5)
N3	0.26045 (19)	0.87866 (16)	0.80288 (10)	0.0362 (5)
N4	0.52400 (19)	1.05084 (16)	0.85664 (11)	0.0356 (5)
N5	0.4278 (2)	0.84235 (17)	0.87725 (11)	0.0405 (6)
N6	0.28958 (19)	1.02235 (16)	0.90219 (11)	0.0373 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.02702 (11)	0.02610 (11)	0.02826 (11)	0.00128 (8)	0.00449 (9)	−0.00450 (8)
Mo2	0.03251 (12)	0.03002 (12)	0.03080 (12)	0.00028 (9)	−0.00145 (9)	0.00129 (9)
Mo3	0.02794 (12)	0.03619 (13)	0.03841 (13)	−0.00186 (9)	−0.00167 (10)	−0.00352 (10)
Mo4	0.03134 (12)	0.02527 (11)	0.04119 (13)	−0.00216 (9)	−0.00156 (10)	−0.00635 (10)
Ni1	0.03229 (18)	0.02604 (16)	0.03110 (17)	0.00256 (13)	0.00320 (14)	−0.00033 (13)
O1	0.0470 (12)	0.0453 (11)	0.0329 (10)	−0.0009 (10)	−0.0026 (9)	−0.0019 (9)
O2	0.0520 (13)	0.0340 (11)	0.0467 (11)	0.0003 (9)	−0.0060 (10)	0.0047 (9)
O3	0.0544 (13)	0.0312 (10)	0.0661 (14)	−0.0059 (10)	−0.0039 (11)	0.0035 (10)
O4	0.0295 (9)	0.0334 (10)	0.0455 (11)	−0.0067 (8)	0.0009 (8)	−0.0038 (9)
O5	0.0417 (11)	0.0459 (12)	0.0508 (12)	−0.0019 (10)	−0.0036 (10)	−0.0208 (10)
O6	0.0279 (9)	0.0249 (9)	0.0292 (9)	0.0009 (7)	0.0017 (7)	−0.0026 (7)
O7	0.0414 (11)	0.0418 (11)	0.0342 (10)	0.0044 (9)	0.0053 (8)	−0.0094 (9)
O8	0.0320 (9)	0.0265 (9)	0.0313 (9)	−0.0020 (7)	0.0032 (7)	0.0000 (7)
O9	0.0289 (9)	0.0236 (8)	0.0349 (9)	0.0024 (7)	0.0003 (7)	−0.0034 (7)
O10	0.0310 (9)	0.0356 (10)	0.0416 (11)	0.0041 (8)	−0.0037 (8)	0.0009 (8)
O11	0.0496 (12)	0.0530 (13)	0.0408 (11)	−0.0053 (10)	−0.0032 (10)	−0.0100 (10)
O12	0.0298 (11)	0.0560 (14)	0.0621 (14)	0.0000 (9)	−0.0013 (10)	−0.0007 (11)
O13	0.0286 (9)	0.0369 (10)	0.0369 (10)	0.0010 (8)	0.0042 (8)	−0.0046 (8)
O14	0.139 (4)	0.192 (4)	0.164 (4)	0.031 (3)	0.028 (3)	0.023 (4)
O15	0.271 (6)	0.179 (4)	0.149 (4)	−0.005 (4)	0.037 (4)	0.028 (4)
C1	0.0339 (14)	0.0402 (15)	0.0392 (15)	−0.0002 (12)	0.0010 (12)	−0.0077 (12)
C2	0.0353 (15)	0.0342 (14)	0.0442 (16)	−0.0052 (12)	−0.0050 (12)	0.0016 (12)
C3	0.0287 (13)	0.0361 (14)	0.0411 (15)	−0.0005 (11)	−0.0012 (12)	0.0027 (12)
C4	0.0423 (17)	0.0511 (18)	0.0431 (16)	−0.0081 (14)	0.0045 (14)	−0.0013 (14)
C5	0.0544 (18)	0.0353 (15)	0.0397 (15)	−0.0037 (13)	0.0202 (14)	−0.0005 (13)
C6	0.0467 (17)	0.0525 (18)	0.0353 (15)	0.0070 (14)	0.0038 (13)	−0.0075 (14)
C7	0.0408 (15)	0.0295 (13)	0.0430 (15)	0.0042 (12)	−0.0038 (13)	−0.0036 (12)
C8	0.0462 (17)	0.0388 (16)	0.0419 (16)	−0.0004 (13)	0.0015 (13)	0.0030 (13)
C9	0.0380 (17)	0.063 (2)	0.0532 (19)	−0.0124 (15)	0.0118 (15)	−0.0026 (16)
C10	0.0511 (18)	0.0430 (17)	0.0416 (16)	0.0004 (14)	−0.0065 (14)	−0.0070 (14)
C11	0.064 (2)	0.0499 (19)	0.0415 (17)	0.0159 (16)	0.0115 (16)	0.0041 (15)
C12	0.057 (2)	0.0402 (17)	0.0472 (17)	−0.0095 (15)	−0.0121 (15)	0.0105 (14)
C13	0.065 (2)	0.0278 (13)	0.0416 (16)	0.0078 (14)	0.0257 (15)	0.0044 (12)
C14	0.0460 (17)	0.0371 (15)	0.0441 (16)	0.0088 (13)	0.0048 (13)	−0.0070 (13)
C15	0.074 (2)	0.0327 (16)	0.064 (2)	0.0084 (16)	−0.0207 (19)	0.0050 (15)
C16	0.065 (2)	0.0381 (16)	0.059 (2)	0.0198 (16)	−0.0085 (17)	−0.0083 (15)
C17	0.059 (2)	0.058 (2)	0.0485 (18)	0.0208 (17)	0.0095 (16)	0.0120 (16)
C18	0.0453 (18)	0.069 (2)	0.0449 (18)	−0.0012 (17)	0.0171 (15)	−0.0071 (17)
C19	0.062 (2)	0.0420 (17)	0.0540 (19)	−0.0026 (16)	−0.0171 (17)	−0.0085 (15)
C20	0.0422 (18)	0.058 (2)	0.066 (2)	−0.0155 (16)	−0.0003 (16)	−0.0042 (17)
C21	0.057 (2)	0.049 (2)	0.073 (2)	−0.0197 (17)	−0.0166 (19)	−0.0081 (18)
C22	0.074 (3)	0.082 (3)	0.054 (2)	0.044 (2)	0.0123 (19)	0.022 (2)
C23	0.111 (4)	0.053 (2)	0.068 (3)	0.033 (2)	0.031 (3)	0.026 (2)
C24	0.096 (3)	0.0428 (19)	0.061 (2)	0.011 (2)	0.028 (2)	0.0166 (17)
C25	0.072 (2)	0.0429 (18)	0.069 (2)	−0.0181 (18)	0.030 (2)	0.0003 (17)
C26	0.060 (2)	0.075 (3)	0.075 (3)	−0.030 (2)	0.018 (2)	−0.014 (2)
C27	0.0456 (19)	0.078 (3)	0.057 (2)	−0.0203 (18)	0.0035 (16)	−0.0054 (19)
C28	0.083 (3)	0.076 (3)	0.0426 (19)	0.022 (2)	0.0214 (18)	0.0013 (18)
C29	0.107 (4)	0.087 (3)	0.058 (2)	0.048 (3)	0.032 (2)	−0.007 (2)
C30	0.098 (3)	0.066 (2)	0.064 (2)	0.046 (2)	0.025 (2)	−0.002 (2)
N1	0.0290 (11)	0.0333 (11)	0.0321 (11)	0.0003 (9)	0.0021 (9)	−0.0021 (9)
N2	0.0381 (12)	0.0305 (11)	0.0357 (12)	0.0024 (10)	−0.0002 (10)	0.0016 (10)
N3	0.0393 (13)	0.0340 (12)	0.0357 (12)	−0.0037 (10)	0.0115 (10)	−0.0032 (10)
N4	0.0375 (12)	0.0326 (12)	0.0367 (12)	0.0000 (10)	−0.0035 (10)	−0.0024 (10)
N5	0.0488 (14)	0.0351 (12)	0.0380 (13)	0.0131 (11)	0.0107 (11)	0.0059 (11)
N6	0.0425 (13)	0.0339 (12)	0.0357 (12)	0.0064 (10)	0.0056 (10)	−0.0018 (10)

Geometric parameters (Å, º)

Mo1—O7	1.6925 (18)	C6—C18	1.359 (4)
Mo1—O13	1.7502 (18)	C6—H6	0.9300
Mo1—O9	1.9458 (17)	C7—N2	1.355 (3)
Mo1—O8	1.9481 (17)	C7—C16	1.387 (4)
Mo1—O6	2.1417 (17)	C7—C14	1.470 (4)
Mo1—O6^i	2.3565 (17)	C8—N2	1.334 (4)
Mo2—O1	1.6963 (19)	C8—C12	1.380 (4)
Mo2—O2	1.7032 (19)	C8—H8	0.9300
Mo2—O10	1.8928 (18)	C9—C18	1.371 (5)
Mo2—O8^i	2.0054 (18)	C9—H9	0.9300
Mo2—O6^i	2.3191 (16)	C10—N4	1.336 (4)
Mo2—O9	2.3310 (17)	C10—C19	1.381 (4)
Mo3—O11	1.693 (2)	C10—H10	0.9300
Mo3—O12	1.699 (2)	C11—N6	1.330 (4)
Mo3—O10	1.9227 (19)	C11—C28	1.377 (4)
Mo3—O4^i	1.9273 (19)	C11—H11	0.9300
Mo3—O13	2.3018 (18)	C12—C15	1.368 (5)
Mo3—O6^i	2.4568 (17)	C12—H12	0.9300
Mo4—O3	1.693 (2)	C13—N5	1.345 (4)
Mo4—O5	1.699 (2)	C13—C24	1.390 (4)
Mo4—O4	1.8919 (18)	C14—N6	1.353 (3)
Mo4—O9	2.0028 (17)	C14—C30	1.382 (4)
Mo4—O8^i	2.3280 (17)	C15—C16	1.383 (5)
Mo4—O6	2.3518 (16)	C15—H15	0.9300
Ni1—N3	2.070 (2)	C16—H16	0.9300
Ni1—N1	2.078 (2)	C17—N5	1.338 (4)
Ni1—N5	2.078 (2)	C17—C22	1.395 (5)
Ni1—N6	2.084 (2)	C17—H17	0.9300
Ni1—N2	2.091 (2)	C18—H18	0.9300
Ni1—N4	2.101 (2)	C19—C21	1.364 (5)
O4—Mo3^i	1.9273 (19)	C19—H19	0.9300
O6—Mo2^i	2.3191 (16)	C20—C21	1.373 (5)
O6—Mo1^i	2.3565 (17)	C20—H20	0.9300
O6—Mo3^i	2.4568 (17)	C21—H21	0.9300
O8—Mo2^i	2.0054 (17)	C22—C23	1.350 (6)
O8—Mo4^i	2.3280 (17)	C22—H22	0.9300
C1—N1	1.339 (3)	C23—C24	1.369 (6)
C1—C6	1.387 (4)	C23—H23	0.9300
C1—H1	0.9300	C24—H24	0.9300
C2—N4	1.349 (4)	C25—C26	1.389 (6)
C2—C20	1.396 (4)	C25—H25	0.9300
C2—C3	1.478 (4)	C26—C27	1.359 (5)
C3—N1	1.341 (3)	C26—H26	0.9300
C3—C9	1.390 (4)	C27—H27	0.9300
C4—N3	1.329 (4)	C28—C29	1.367 (5)
C4—C27	1.384 (4)	C28—H28	0.9300
C4—H4	0.9300	C29—C30	1.367 (5)
C5—N3	1.352 (3)	C29—H29	0.9300
C5—C25	1.395 (4)	C30—H30	0.9300
C5—C13	1.476 (5)
O7—Mo1—O13	103.70 (9)	N1—C3—C2	115.6 (2)
O7—Mo1—O9	101.51 (9)	C9—C3—C2	123.9 (3)
O13—Mo1—O9	97.18 (8)	N3—C4—C27	123.2 (3)
O7—Mo1—O8	101.04 (9)	N3—C4—H4	118.4
O13—Mo1—O8	95.98 (8)	C27—C4—H4	118.4
O9—Mo1—O8	150.30 (7)	N3—C5—C25	120.8 (3)
O7—Mo1—O6	99.07 (8)	N3—C5—C13	115.3 (3)
O13—Mo1—O6	157.21 (8)	C25—C5—C13	123.8 (3)
O9—Mo1—O6	79.10 (7)	C18—C6—C1	118.9 (3)
O8—Mo1—O6	78.48 (7)	C18—C6—H6	120.5
O7—Mo1—O6^i	175.11 (8)	C1—C6—H6	120.5
O13—Mo1—O6^i	81.18 (7)	N2—C7—C16	121.1 (3)
O9—Mo1—O6^i	77.86 (6)	N2—C7—C14	115.7 (2)
O8—Mo1—O6^i	78.02 (6)	C16—C7—C14	123.2 (3)
O6—Mo1—O6^i	76.05 (7)	N2—C8—C12	123.4 (3)
O1—Mo2—O2	104.58 (10)	N2—C8—H8	118.3
O1—Mo2—O10	102.32 (9)	C12—C8—H8	118.3
O2—Mo2—O10	101.02 (9)	C18—C9—C3	119.8 (3)
O1—Mo2—O8^i	96.15 (8)	C18—C9—H9	120.1
O2—Mo2—O8^i	100.67 (9)	C3—C9—H9	120.1
O10—Mo2—O8^i	146.81 (8)	N4—C10—C19	122.9 (3)
O1—Mo2—O6^i	94.97 (8)	N4—C10—H10	118.6
O2—Mo2—O6^i	160.12 (8)	C19—C10—H10	118.6
O10—Mo2—O6^i	77.87 (7)	N6—C11—C28	123.3 (3)
O8^i—Mo2—O6^i	73.22 (6)	N6—C11—H11	118.3
O1—Mo2—O9	163.75 (8)	C28—C11—H11	118.3
O2—Mo2—O9	88.45 (8)	C15—C12—C8	118.3 (3)
O10—Mo2—O9	84.26 (7)	C15—C12—H12	120.9
O8^i—Mo2—O9	71.52 (6)	C8—C12—H12	120.9
O6^i—Mo2—O9	71.66 (6)	N5—C13—C24	120.6 (3)
O11—Mo3—O12	104.36 (11)	N5—C13—C5	115.9 (2)
O11—Mo3—O10	98.68 (10)	C24—C13—C5	123.4 (3)
O12—Mo3—O10	103.17 (9)	N6—C14—C30	120.3 (3)
O11—Mo3—O4^i	97.82 (10)	N6—C14—C7	116.2 (2)
O12—Mo3—O4^i	102.29 (9)	C30—C14—C7	123.5 (3)
O10—Mo3—O4^i	145.01 (8)	C12—C15—C16	119.6 (3)
O11—Mo3—O13	164.25 (9)	C12—C15—H15	120.2
O12—Mo3—O13	91.37 (9)	C16—C15—H15	120.2
O10—Mo3—O13	78.01 (7)	C15—C16—C7	119.2 (3)
O4^i—Mo3—O13	77.77 (7)	C15—C16—H16	120.4
O11—Mo3—O6^i	94.88 (8)	C7—C16—H16	120.4
O12—Mo3—O6^i	160.75 (9)	N5—C17—C22	121.2 (4)
O10—Mo3—O6^i	73.92 (7)	N5—C17—H17	119.4
O4^i—Mo3—O6^i	74.11 (7)	C22—C17—H17	119.4
O13—Mo3—O6^i	69.38 (6)	C6—C18—C9	119.4 (3)
O3—Mo4—O5	104.86 (11)	C6—C18—H18	120.3
O3—Mo4—O4	100.93 (10)	C9—C18—H18	120.3
O5—Mo4—O4	102.00 (9)	C21—C19—C10	118.5 (3)
O3—Mo4—O9	102.05 (9)	C21—C19—H19	120.8
O5—Mo4—O9	95.09 (8)	C10—C19—H19	120.8
O4—Mo4—O9	146.65 (8)	C21—C20—C2	119.5 (3)
O3—Mo4—O8^i	89.60 (9)	C21—C20—H20	120.2
O5—Mo4—O8^i	162.35 (8)	C2—C20—H20	120.2
O4—Mo4—O8^i	84.73 (7)	C19—C21—C20	119.7 (3)
O9—Mo4—O8^i	71.63 (6)	C19—C21—H21	120.2
O3—Mo4—O6	160.91 (9)	C20—C21—H21	120.2
O5—Mo4—O6	94.04 (9)	C23—C22—C17	119.0 (4)
O4—Mo4—O6	77.32 (7)	C23—C22—H22	120.5
O9—Mo4—O6	73.06 (6)	C17—C22—H22	120.5
O8^i—Mo4—O6	71.31 (6)	C22—C23—C24	120.2 (4)
N3—Ni1—N1	96.52 (9)	C22—C23—H23	119.9
N3—Ni1—N5	79.11 (10)	C24—C23—H23	119.9
N1—Ni1—N5	92.00 (9)	C23—C24—C13	119.2 (4)
N3—Ni1—N6	90.27 (9)	C23—C24—H24	120.4
N1—Ni1—N6	171.31 (9)	C13—C24—H24	120.4
N5—Ni1—N6	94.61 (9)	C26—C25—C5	118.8 (3)
N3—Ni1—N2	95.27 (9)	C26—C25—H25	120.6
N1—Ni1—N2	94.91 (9)	C5—C25—H25	120.6
N5—Ni1—N2	171.56 (9)	C27—C26—C25	119.8 (3)
N6—Ni1—N2	79.02 (9)	C27—C26—H26	120.1
N3—Ni1—N4	174.02 (9)	C25—C26—H26	120.1
N1—Ni1—N4	78.63 (9)	C26—C27—C4	118.4 (4)
N5—Ni1—N4	97.45 (10)	C26—C27—H27	120.8
N6—Ni1—N4	94.90 (9)	C4—C27—H27	120.8
N2—Ni1—N4	88.66 (9)	C29—C28—C11	118.0 (3)
Mo4—O4—Mo3^i	118.00 (9)	C29—C28—H28	121.0
Mo1—O6—Mo2^i	92.41 (6)	C11—C28—H28	121.0
Mo1—O6—Mo4	91.67 (6)	C30—C29—C28	119.5 (3)
Mo2^i—O6—Mo4	163.47 (8)	C30—C29—H29	120.2
Mo1—O6—Mo1^i	103.95 (7)	C28—C29—H29	120.2
Mo2^i—O6—Mo1^i	97.48 (6)	C29—C30—C14	120.2 (3)
Mo4—O6—Mo1^i	97.06 (6)	C29—C30—H30	119.9
Mo1—O6—Mo3^i	163.79 (8)	C14—C30—H30	119.9
Mo2^i—O6—Mo3^i	85.83 (6)	C1—N1—C3	119.3 (2)
Mo4—O6—Mo3^i	85.79 (5)	C1—N1—Ni1	125.21 (18)
Mo1^i—O6—Mo3^i	92.24 (6)	C3—N1—Ni1	115.27 (18)
Mo1—O8—Mo2^i	109.18 (8)	C8—N2—C7	118.3 (2)
Mo1—O8—Mo4^i	110.87 (8)	C8—N2—Ni1	127.19 (19)
Mo2^i—O8—Mo4^i	103.72 (7)	C7—N2—Ni1	114.46 (18)
Mo1—O9—Mo4	109.60 (8)	C4—N3—C5	118.9 (3)
Mo1—O9—Mo2	110.22 (7)	C4—N3—Ni1	126.4 (2)
Mo4—O9—Mo2	103.70 (7)	C5—N3—Ni1	114.7 (2)
Mo2—O10—Mo3	117.01 (9)	C10—N4—C2	118.9 (3)
Mo1—O13—Mo3	117.18 (9)	C10—N4—Ni1	126.5 (2)
N1—C1—C6	121.9 (3)	C2—N4—Ni1	113.94 (18)
N1—C1—H1	119.0	C17—N5—C13	119.6 (3)
C6—C1—H1	119.0	C17—N5—Ni1	125.9 (2)
N4—C2—C20	120.5 (3)	C13—N5—Ni1	114.4 (2)
N4—C2—C3	115.9 (2)	C11—N6—C14	118.6 (3)
C20—C2—C3	123.5 (3)	C11—N6—Ni1	126.9 (2)
N1—C3—C9	120.5 (3)	C14—N6—Ni1	114.45 (18)

Symmetry code: (i) −x+2, −y+1, −z+2.