Triguanidinium hexa­hydrogenhexamolybdocobaltate(III) tetrahydrate

Crystals of the title compound, (CH₆N₃)₃[H₆CoMo₆O₂₄]·4H₂O, containing the well known B-type Anderson-Evans heteropolyoxometalate structure, were obtained by recrystallization of powder (CH₆N₃)₃[H₆CoMo₆O₂₄]·nH₂O. The anion has a Co^III atom at an inversion center and has approximate symmetry, with Co-O bond lengths in the range 1.905 (3)-1.918 (3) Å and Mo-O bond lengths in the ranges 1.704 (3)-1.722 (3) (Ot), 1.915 (3)-1.949 (3) (Ob), and 2.266 (3)-2.312 (3) Å (Oc), respectively.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](N-C) = 0.009 Å
• H-atom completeness 57%
• Disorder in solvent or counterion
• R factor = 0.031
• wR factor = 0.084
• Data-to-parameter ratio = 15.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_302  Alert C Anion/Solvent Disorder .......................      23.00 Perc.

PLAT_420  Alert C D-H Without Acceptor       N2     -   H2A               ?

General Notes



FORMU_01  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:C3 H32 Co1 Mo6 N9 O28
          Atom count from the _atom_site data:  C3 H18 Co1 Mo6 N9 O28

ABSTM_02  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
          Tmin and Tmax reported:      0.603     0.678
          Tmin and Tmax expected:      0.423     0.570
          RR =      1.199
          Please check that your absorption correction is appropriate.

CELLZ_01
         From the CIF: _cell_formula_units_Z    1
         From the CIF: _chemical_formula_sum  C3 H32 Co Mo6 N9 O28
         TEST: Compare cell contents of formula and atom_site data

         atom    Z*formula  cif sites diff
         C          3.00      3.00    0.00
         H         32.00     18.00   14.00
         Co         1.00      1.00    0.00
         Mo         6.00      6.00    0.00
         N          9.00      9.00    0.00
         O         28.00     28.00    0.00
          Difference between formula and atom_site contents detected.
          WARNING: H atoms missing from atom site list. Is this intentional?

CHEMW_03
         From the CIF: _cell_formula_units_Z                    1
         From the CIF: _chemical_formula_weight          1276.95
         TEST: Calculate formula weight from _atom_site_*
         atom     mass    num     sum
         C        12.01    3.00   36.03
         H         1.01   18.00   18.14
         N        14.01    9.00  126.06
         Mo       95.94    6.00  575.64
         O        16.00   28.00  447.97
         Co       58.93    1.00   58.93
         Calculated formula weight             1262.79
          The ratio of given/expected molecular weight as calculated
          from the _atom_site* data lies outside
          the range 0.99 <> 1.01


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

---

S1. Comment

We have recently reported the crystal structures of two guanidinium salts of polyoxometalates, viz. (CH₆N₃)₈[PtW₆O₂₄] (Lee, Jang et al., 2003). and (CH₆N₃)₈[SiPt₂W₁₀O₄₀]·6H₂O (Lee, Joo et al., 2003). Also, (CH₆N₃)₄[GeMo₁₂O₄₀] (Strandberg & Hedman, 1982), (CH₆N₃)₂[MoO₄] (Ozeki et al., 1987), (CH₆N₃)₄[SiMo₁₂O₄₀]·H₂O (Ichida et al., 1980), (CH₆N₃)₄[As₂Mo₁₈O₆₂]·9H₂O (Ichida & Sasaki, 1983), and (CH₆N₃)₆[V₁₀O₂₈]·6H₂O (Wang et al., 1993) have been reported by others. Good crystals of guanidinium polyoxometalates can not always be obtained, but sometimes very stable single crystals are obtained by recrystallization. And, these salts were shown to be arresting crystal packing by hydrogen bonds and thermal behavior of crystalline water molecules.

Several heteropolyoxometalates containing the [H₆CoMo₆O₂₄]³⁻ polyanion, such as (18-crown-6.K⁺)₂·K[H₆CoMo₆O₂₄].12H₂O (Nagano et al., 1990), [Ga(H₂O)₆]₃[H₆CoMo₆O₂₄].10H₂O (Panneerselvam et al., 1996), Na₃[H₆CoMo₆O₂₄]·8H₂O (Nolan et al., 1998), K₃[H₆CoMo₆O₂₄]·KNO₃·4H₂O (Lee & Joo, 2000), and K₃[H₆CoMo₆O₂₄]·4H₂O (Lee et al., 2001), have been reported. The [H₆CoMo₆O₂₄]³⁻ anion is a typical B-type Anderson–Evans heteropolyanion structure (Anderson, 1937; Evans, 1948; Tsigdinos, 1978). Detailed discussions related to the position of six H atoms in the [H₆CoMo₆O₂₄]³⁻ have been given by Nolan et al. (1998). Six non-acidic H atoms are bound to six central O_c atoms surrounding the Co^III atom. As expected, they were not substituted by guanidinium ion. The crystal structure of (I) is a good example of the packing and the hydrogen bonding found in the B-type Anderson–Evans heteropolyoxometalate structure and thermal behavior of crystalline water molecules. Here we report on the crystal structure of (I), in which the replaceable cations were completely exchanged by guanidinium ions.

Fig. 1 shows the structure of the [H₆CoMo₆O₂₄]³⁻ polyanion. The labeling of the O atoms in the polyanion is the same as the labeling in the previous structure (Lee et al., 2001). The distance ranges of Co—Mo and Mo—Mo are 3.2999 (9)–3.3319 (9) and 3.3081 (9)–3.328 (1) Å, respectively. The bond-length range of Co—O is 1.905 (3)–1.918 (3) Å, and the three types of Mo—O bond-length ranges are 1.704 (3)–1.722 (3) (O_t), 1.915 (3)–1.949 (3) (O_b), and 2.266 (3)–2.312 (3) Å (O_c). The bond lengths and angles of (I) have shown a similar trend to what is found in the literatures, and the guanidinium ions also agree well with those in CH₆N₃Cl (Hass et al., 1965) and CH₆N₃(NO₃) (Katrusiak& Szafrański, 1994). There are one and a half crystallographically independent guanidinium (CH₆N₃)⁺ ions in the asymmetric unit, one of which lies on an inversion center.

Fig. 2 shows the hydrogen-bonding interaction of (CH₆N₃)⁺ ions with O atoms of the anions and crystalline water molecules. The list of all probable hydrogen bonds with N···O and O···O distances within 3.1 Å is given in Tables 1 and 2.An iInter-anion hydrogen bond is formed by O_c3—H···O_t11 [2.831 (4) Å]. All O atoms in the polyanion except O_c3 form strong N—H····O and O—H····O hydrogen bonds, with all N atoms of the guanidinium ions and all the crystalline water molecules. Each crystalline water molecule forms strong hydrogen bonds. As a result, the degradation temperature was very high (543 K) and those were decomposed with (CH₆N₃)⁺ ions. All probable N—O_{poly anion} hydrogen-bond distances fall into the range 2.78–3.10 Å, with the range of N—H···O angles varying between 119 and 177°. The crystal structure of (I) is stabilized by the formation of extensive N—H···O and O—H···O hydrogen-bond interactions with the guanidinium ions and the waters of crystallization. Fig. 3 shows the unit-cell packing and probable hydrogen-bonding interactions in the lattice.

S2. Experimental

A blue powder of (I) was obtained by adding a small excess stoichiometric amount of CH₆N₃Cl to a K₃[H₆CoMo₆O₂₄].nH₂O solution (Lee et al., 2001). Single crystals of (I) were obtained by recrystallizing the powdered crude sample from a boiling aqueous solution.

S3. Refinement

The guanidiniun ion that lies on an inversion center was fixed on (1/2, 1/2, 0) and refined under the restraint of FLAT, SAME conditions, and H atoms were generated by PART. All H atoms were placed in calculated positions with N—H distances of 0.86 Å and H—N—H angles of 120°. They were included in the refinement in riding-motion approximation with, U_iso = 1.2U_eq(N). The highest peak in the difference map is 0.43 Å from N5, and the largest hole is 0.42 Å from N5.

Computing details

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998).

Figures

	Fig. 1. The anion structure in (CH6N3)3[H6CoMo6O24]·4H2O. Displacement ellipsoids are drawn at the 50% probability level. H atoms was not shown. [Symmetry code: (i) 1 − x, −y, 1 − z.]
	Fig. 2. Formation of hydrogen bonds by guanidinium ions and crystalline water molecules. [Symmetry cods: (i) −1 + x, y, z; (ii) 1 − x, −y, 2 − z; (iii) 1 − x, 1 − y, 1 − z; (iv) −1 + x, y, −1 + z; (v) 1 − x, −y, 1 − z; (vi) 2 − x, −y, 1 − z; (vii) 2 − x, 1 − y, 1 − z; (viii) 1 − x, 1 − y, −z; (ix) x, y, −1 + z.]
	Fig. 3. The crystal packing of (CH6N3)3[H6CoMo6O24]·4H2O in the unit cell shown as a polyhedral model. Violet and cyan octahedra are [CoO6] and [MoO6], respectively. Probable hydrogen bonds are shown in blue (N···O), and red (O···O) broken lines. [Symmetry code: (i) 1 − x, −y, 1 − z.]

(I)

Crystal data

(CH6N3)3[H6CoMo6O24]·4H2O	Z = 1
Mr = 1276.95	F(000) = 616
Triclinic, P1	Dx = 2.707 Mg m^−3
Hall symbol: -p_1	Mo Kα radiation, λ = 0.7107 Å
a = 8.821 (1) Å	Cell parameters from 27 reflections
b = 11.603 (3) Å	θ = 9.5–10.4°
c = 8.013 (1) Å	µ = 2.96 mm^−1
α = 93.93 (3)°	T = 298 K
β = 105.95 (1)°	Polyhedron, blue
γ = 83.77 (1)°	0.38 × 0.25 × 0.19 mm
V = 783.3 (2) Å^3

Data collection

Stoe Stadi-4 diffractometer	3309 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.000
Graphite monochromator	θmax = 27.5°, θmin = 1.8°
ω/2–θ scans	h = −11→11
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996)	k = −15→15
Tmin = 0.603, Tmax = 0.678	l = 0→10
3588 measured reflections	3 standard reflections every 60 min
3588 independent reflections	intensity decay: 2.0%

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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.084	H-atom parameters constrained
S = 1.15	w = 1/[σ^2(Fo^2) + (0.0366P)^2 + 2.8997P] where P = (Fo^2 + 2Fc^2)/3
3588 reflections	(Δ/σ)max = 0.001
229 parameters	Δρmax = 1.42 e Å^−3
7 restraints	Δρmin = −1.64 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	Occ. (<1)
Co	0.5000	0.0000	0.5000	0.01253 (15)
Mo1	0.54492 (4)	0.27422 (3)	0.45785 (5)	0.01909 (10)
Mo2	0.75405 (4)	0.13827 (3)	0.81265 (5)	0.01957 (10)
Mo3	0.69975 (4)	−0.13468 (3)	0.86017 (4)	0.01856 (10)
Oc1	0.3702 (3)	0.1413 (2)	0.4394 (4)	0.0160 (5)
Oc2	0.6723 (3)	0.0911 (2)	0.5200 (4)	0.0167 (6)
Oc3	0.5409 (3)	0.0282 (2)	0.7463 (3)	0.0150 (5)
Ob4	0.4941 (4)	0.2072 (3)	0.2236 (4)	0.0223 (6)
Ob5	0.5889 (4)	0.2565 (3)	0.7037 (4)	0.0229 (6)
Ob6	0.8349 (4)	−0.0218 (3)	0.8280 (4)	0.0235 (6)
Ot7	0.4006 (5)	0.3876 (3)	0.4360 (5)	0.0333 (8)
Ot8	0.7122 (5)	0.3319 (3)	0.4465 (5)	0.0341 (8)
Ot9	0.9163 (4)	0.1958 (3)	0.7878 (5)	0.0375 (9)
Ot10	0.7456 (4)	0.1745 (3)	1.0201 (4)	0.0315 (8)
Ot11	0.6861 (4)	−0.0991 (3)	1.0681 (4)	0.0278 (7)
Ot12	0.8312 (4)	−0.2549 (3)	0.8737 (5)	0.0329 (8)
C1	0.9309 (7)	0.4957 (5)	0.2659 (8)	0.0387 (12)
N1	0.8336 (7)	0.5577 (4)	0.3460 (8)	0.0509 (13)
H1a	0.8386	0.6313	0.3637	0.061*
H1b	0.7657	0.5241	0.3801	0.061*
N2	1.0340 (8)	0.5444 (5)	0.2136 (9)	0.0632 (17)
H2a	1.0949	0.5035	0.1603	0.076*
H2b	1.0416	0.6177	0.2320	0.076*
N3	0.9172 (7)	0.3831 (4)	0.2390 (9)	0.0593 (17)
H3a	0.9773	0.3410	0.1859	0.071*
H3b	0.8482	0.3520	0.2746	0.071*
C2	0.5000	0.5000	0.0000	0.091 (6)
N4	0.4269 (15)	0.5214 (8)	0.1453 (12)	0.061 (4)	0.50
H4a	0.3976	0.5912	0.1746	0.073*	0.50
H4b	0.4136	0.4641	0.2008	0.073*	0.50
N5	0.5239 (14)	0.5628 (10)	−0.0806 (15)	0.079 (5)	0.50
H5a	0.5543	0.5400	−0.1716	0.095*	0.50
H5b	0.5126	0.6357	−0.0537	0.095*	0.50
N6	0.5084 (13)	0.3763 (7)	−0.0123 (13)	0.045 (3)	0.50
H6a	0.5372	0.3391	−0.0968	0.054*	0.50
H6b	0.4848	0.3390	0.0647	0.054*	0.50
Ow1	−0.0959 (4)	0.0823 (4)	0.3372 (5)	0.0389 (9)
Ow2	0.1414 (5)	0.1924 (3)	0.5934 (5)	0.0379 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co	0.0136 (3)	0.0128 (3)	0.0127 (3)	−0.0021 (3)	0.0057 (3)	0.0004 (3)
Mo1	0.0261 (2)	0.01388 (17)	0.02034 (19)	−0.00479 (13)	0.01006 (14)	0.00137 (13)
Mo2	0.02118 (19)	0.02327 (19)	0.01604 (18)	−0.00880 (14)	0.00616 (13)	−0.00232 (13)
Mo3	0.02037 (18)	0.01963 (18)	0.01537 (17)	0.00139 (13)	0.00518 (13)	0.00228 (13)
Oc1	0.0189 (13)	0.0145 (13)	0.0167 (13)	−0.0003 (11)	0.0085 (11)	0.0022 (10)
Oc2	0.0189 (14)	0.0161 (13)	0.0175 (13)	−0.0049 (11)	0.0078 (11)	0.0001 (11)
Oc3	0.0156 (13)	0.0173 (13)	0.0135 (13)	−0.0035 (10)	0.0058 (10)	−0.0001 (10)
Ob4	0.0301 (16)	0.0220 (15)	0.0183 (14)	−0.0063 (12)	0.0105 (12)	0.0035 (11)
Ob5	0.0329 (17)	0.0179 (14)	0.0204 (15)	−0.0045 (12)	0.0112 (13)	−0.0026 (11)
Ob6	0.0170 (14)	0.0288 (16)	0.0240 (15)	−0.0032 (12)	0.0039 (12)	0.0013 (12)
Ot7	0.044 (2)	0.0196 (16)	0.038 (2)	0.0038 (14)	0.0159 (16)	0.0031 (14)
Ot8	0.041 (2)	0.0322 (18)	0.0355 (19)	−0.0175 (16)	0.0160 (16)	0.0011 (15)
Ot9	0.0329 (19)	0.048 (2)	0.035 (2)	−0.0192 (17)	0.0100 (16)	−0.0006 (17)
Ot10	0.042 (2)	0.0348 (19)	0.0182 (16)	−0.0069 (15)	0.0092 (14)	−0.0034 (13)
Ot11	0.0315 (17)	0.0322 (18)	0.0197 (15)	−0.0021 (14)	0.0070 (13)	0.0011 (13)
Ot12	0.0308 (18)	0.0296 (18)	0.0344 (19)	0.0084 (14)	0.0064 (15)	0.0028 (14)
C1	0.041 (3)	0.034 (3)	0.048 (3)	−0.009 (2)	0.023 (3)	−0.007 (2)
N1	0.057 (3)	0.035 (3)	0.071 (4)	−0.002 (2)	0.038 (3)	−0.009 (2)
N2	0.076 (4)	0.049 (3)	0.086 (5)	−0.029 (3)	0.052 (4)	−0.011 (3)
N3	0.062 (4)	0.034 (3)	0.103 (5)	−0.014 (2)	0.059 (4)	−0.016 (3)
C2	0.141 (13)	0.056 (7)	0.033 (5)	0.053 (8)	−0.022 (6)	−0.010 (5)
N4	0.137 (12)	0.021 (5)	0.026 (5)	0.003 (6)	0.027 (6)	0.003 (4)
N5	0.153 (16)	0.036 (7)	0.049 (8)	−0.012 (8)	0.027 (9)	0.005 (6)
N6	0.079 (8)	0.024 (4)	0.045 (6)	0.011 (4)	0.044 (6)	0.011 (4)
Ow1	0.037 (2)	0.048 (2)	0.0308 (19)	0.0020 (17)	0.0103 (16)	0.0044 (17)
Ow2	0.039 (2)	0.040 (2)	0.043 (2)	−0.0017 (17)	0.0257 (17)	0.0029 (17)

Geometric parameters (Å, º)

Mo1—Mo2	3.328 (1)	Mo3—Ot12	1.704 (3)
Mo2—Mo3	3.317 (1)	Mo3—Ot11	1.722 (3)
Mo1—Mo3^i	3.3081 (9)	Mo3—Ob4^i	1.920 (3)
Co—Mo1	3.2999 (9)	Mo3—Ob6	1.938 (3)
Co—Mo2	3.3191 (9)	Mo3—Oc1^i	2.307 (3)
Co—Mo3	3.3319 (9)	Mo3—Oc3	2.308 (3)
Co—Oc1	1.905 (3)	Oc3—Ot11^ii	2.831 (4)
Co—Oc2	1.909 (3)	C1—N2	1.295 (7)
Co—Oc3	1.918 (3)	C1—N3	1.323 (7)
Mo1—Ot7	1.711 (3)	C1—N1	1.331 (7)
Mo1—Ot8	1.712 (3)	C2—N5	1.08 (1)
Mo1—Ob5	1.921 (3)	C2—N6	1.427 (8)
Mo1—Ob4	1.934 (3)	C2—N4	1.473 (9)
Mo1—Oc1	2.266 (3)	Ow1—Oc2^iii	2.814 (5)
Mo1—Oc2	2.312 (3)	Ow1—Ot10^iv	2.765 (5)
Mo2—Ot10	1.706 (3)	Ow1—Ob6^i	2.956 (5)
Mo2—Ot9	1.707 (3)	Ow1—Ow2	2.843 (6)
Mo2—Ob6	1.915 (3)	Ow2—Oc1	2.638 (4)
Mo2—Ob5	1.949 (3)	Ow2—Ot9^iii	2.837 (5)
Mo2—Oc2	2.302 (3)	Ow2—Ot11^ii	2.937 (5)
Mo2—Oc3	2.308 (3)	Ow2—N1^v	2.930 (7)
Mo3—Mo2—Mo1	119.78 (3)	Ot10—Mo2—Oc3	95.06 (14)
Mo3^i—Mo1—Mo2	120.63 (2)	Ot9—Mo2—Oc3	158.18 (15)
Oc1—Co—Oc2^i	95.10 (12)	Ob6—Mo2—Oc3	72.12 (12)
Oc1—Co—Oc2	84.90 (12)	Ob5—Mo2—Oc3	81.28 (12)
Oc2^i—Co—Oc2	180.0	Oc2—Mo2—Oc3	68.22 (10)
Oc1—Co—Oc3	95.56 (12)	Ot12—Mo3—Ot11	106.57 (17)
Oc1^i—Co—Oc3	84.44 (12)	Ot12—Mo3—Ob6	98.30 (16)
Oc2^i—Co—Oc3	95.00 (12)	Ot11—Mo3—Ob6	101.96 (15)
Oc2—Co—Oc3	85.00 (12)	Ot12—Mo3—Oc3	159.32 (14)
Ot7—Mo1—Ot8	106.05 (18)	Ot11—Mo3—Oc3	93.41 (13)
Ot7—Mo1—Ob5	98.69 (16)	Ob6—Mo3—Oc3	71.75 (11)
Ot8—Mo1—Ob5	101.04 (16)	N2—C1—N3	121.1 (5)
Ot7—Mo1—Ob4	100.43 (16)	N2—C1—N1	121.1 (5)
Ot8—Mo1—Ob4	95.84 (16)	N3—C1—N1	117.9 (5)
Ob5—Mo1—Ob4	149.82 (13)	N5—C2—N6	132.1 (8)
Ot7—Mo1—Oc1	92.65 (15)	N5—C2—N4	128.1 (8)
Ot8—Mo1—Oc1	159.47 (15)	N6—C2—N4	99.4 (5)
Ob5—Mo1—Oc1	84.02 (12)	Ot10^iv—Ow1—Oc2^iii	104.60 (15)
Ob4—Mo1—Oc1	72.01 (11)	Ot10^iv—Ow1—Ow2	124.06 (18)
Ot7—Mo1—Oc2	159.33 (14)	Oc2^iii—Ow1—Ow2	98.87 (15)
Ot8—Mo1—Oc2	94.01 (15)	Ot10^iv—Ow1—Ob6^i	84.11 (14)
Ob5—Mo1—Oc2	72.02 (12)	Oc2^iii—Ow1—Ob6^i	167.65 (18)
Ob4—Mo1—Oc2	82.07 (12)	Ow2—Ow1—Ob6^i	82.89 (14)
Oc1—Mo1—Oc2	68.41 (10)	Oc1—Ow2—Ot9^iii	166.92 (19)
Ot10—Mo2—Ot9	106.45 (18)	Oc1—Ow2—Ow1	96.44 (16)
Ot10—Mo2—Ob6	102.30 (16)	Ot9^iii—Ow2—Ow1	82.23 (15)
Ot9—Mo2—Ob6	99.15 (17)	Oc1—Ow2—N1^v	98.81 (17)
Ot10—Mo2—Ob5	95.67 (15)	Ot9^iii—Ow2—N1^v	92.29 (17)
Ot9—Mo2—Ob5	99.79 (17)	Ow1—Ow2—N1^v	126.9 (2)
OB6—Mo2—Ob5	148.91 (13)	Oc1—Ow2—Ot11^ii	96.96 (15)
Ot10—Mo2—Oc2	160.06 (15)	Ot9^iii—Ow2—Ot11^ii	73.68 (14)
Ot9—Mo2—Oc2	91.24 (15)	Ow1—Ow2—Ot11^ii	125.36 (17)
Ob6—Mo2—Oc2	83.38 (12)	N1^v—Ow2—Ot11^ii	102.79 (19)
Ob5—Mo2—Oc2	71.80 (11)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1b···Ot7^v	0.86	2.46	3.044 (6)	126
N2—H2b···Ot9^vi	0.86	2.26	3.094 (7)	164
N3—H3a···Ot12^vii	0.86	2.02	2.855 (6)	163
N3—H3b···Ot8	0.86	2.10	2.900 (6)	155
N4—H4a···Ob5^v	0.86	1.96	2.78 (1)	159
N4—H4b···Ot7	0.86	2.17	2.96 (1)	152
N5—H5b···Ob4^viii	0.86	2.34	2.95 (1)	128
N6—H6a···Ob5^ix	0.86	1.94	2.803 (9)	177
N6—H6b···Ob4	0.86	2.04	2.852 (9)	158
N6—H6a···Ot10^ix	0.86	2.54	2.941 (9)	110

Symmetry codes: (v) −x+1, −y+1, −z+1; (vi) −x+2, −y+1, −z+1; (vii) −x+2, −y, −z+1; (viii) −x+1, −y+1, −z; (ix) x, y, z−1.