Bis(guanidinium) hexa­hydroxo­octa­deca­oxodisodiohexa­molybdonickelate deca­hydrate

The title compound, (CH₆N₃)₂[Na₂Ni(OH)₆Mo₆O₁₈]·10H₂O, features inversion-generated hexa­molybdonickelate anions (Ni site symmetry ). The anions are linked by octa­hedrally coordinated Na⁺ cations into extended sheets. The guanidinium cations and uncoordinated water mol­ecules link the sheets together via O—H...O and N—H...O hydrogen bonds to form a three-dimensional network. Two water mol­ecule O atoms have site symmetry 2.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](N-C) = 0.005 Å
• R factor = 0.023
• wR factor = 0.060
• Data-to-parameter ratio = 15.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.09 Ratio
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.11 Ratio
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3B    ..  O11     ..       2.81 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........         14

Alert level G
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
   0 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 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

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Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.

Bis(guanidinium) hexahydroxooctadecaoxodisodiohexamolybdonickelate decahydrate

Crystal data

(CH6N3)2[Na2Ni(OH)6Mo6O18]·10H2O	F(000) = 2664
Mr = 1370.69	Dx = 2.480 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 5347 reflections
a = 25.2247 (9) Å	θ = 1.8–26.1°
b = 11.6583 (4) Å	µ = 2.62 mm^−1
c = 13.7668 (5) Å	T = 293 K
β = 114.918 (4)°	Prism, green
V = 3671.6 (3) Å^3	0.28 × 0.24 × 0.18 mm
Z = 4

Data collection

Bruker SMART APEXII CCD area-detector diffractometer	3557 independent reflections
Radiation source: fine-focus sealed tube	3275 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.017
ω and φ scans	θmax = 26.0°, θmin = 2.8°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −31→30
Tmin = 0.475, Tmax = 0.630	k = −14→11
9516 measured reflections	l = −16→16

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)] = 0.024	Hydrogen site location: difference Fourier map
wR(F^2) = 0.060	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0316P)^2 + 13.3478P] where P = (Fo^2 + 2Fc^2)/3
3557 reflections	(Δ/σ)max < 0.001
233 parameters	Δρmax = 0.65 e Å^−3
0 restraints	Δρmin = −0.63 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
Ni	0.7500	0.7500	0.0000	0.01399 (12)
Mo1	0.875219 (11)	0.65271 (2)	0.18571 (2)	0.01685 (8)
Mo2	0.627324 (11)	0.71958 (2)	0.03086 (2)	0.01634 (8)
Mo3	0.752803 (11)	0.62372 (2)	0.21791 (2)	0.01563 (8)
Na	0.83122 (6)	0.34440 (12)	0.19303 (11)	0.0304 (3)
O1	0.78101 (9)	0.60580 (18)	0.08711 (16)	0.0160 (4)
H1	0.7719	0.5389	0.0561	0.019*
O2	0.72033 (9)	0.78138 (17)	0.11499 (16)	0.0151 (4)
H2	0.7252	0.8473	0.1452	0.018*
O3	0.83390 (9)	0.80500 (18)	0.08610 (17)	0.0168 (4)
H3	0.8382	0.8667	0.1147	0.020*
O4	0.88537 (10)	0.64101 (18)	0.05404 (18)	0.0200 (5)
O5	0.82963 (10)	0.69438 (19)	0.26683 (17)	0.0191 (4)
O6	0.77292 (11)	0.4850 (2)	0.25988 (19)	0.0258 (5)
O7	0.61116 (10)	0.7807 (2)	0.12909 (18)	0.0254 (5)
O8	0.67600 (9)	0.59067 (18)	0.10722 (18)	0.0195 (4)
O9	0.89049 (11)	0.5110 (2)	0.22220 (19)	0.0270 (5)
O10	0.93650 (10)	0.7243 (2)	0.26786 (19)	0.0317 (6)
O11	0.56614 (11)	0.6427 (2)	−0.0445 (2)	0.0301 (6)
O12	0.73482 (10)	0.6854 (2)	0.31356 (18)	0.0248 (5)
OW1	0.75490 (12)	0.3860 (2)	0.0220 (2)	0.0315 (6)
H1WA	0.7245	0.3661	0.0292	0.038*
H1WB	0.7474	0.3601	−0.0385	0.038*
OW2	0.65516 (15)	0.3564 (2)	0.0716 (2)	0.0471 (8)
H2WA	0.6636	0.4281	0.0964	0.057*
H2WB	0.6682	0.3233	0.1355	0.057*
OW3	0.63482 (16)	0.4915 (3)	0.2827 (3)	0.0581 (9)
H3WA	0.6255	0.5451	0.3154	0.070*
H3WB	0.6511	0.5313	0.2470	0.070*
OW4	0.5000	0.4497 (7)	0.2500	0.113 (5)
H4W	0.5300	0.4079	0.2624	0.135*
OW5	0.5000	0.6753 (7)	0.2500	0.142 (4)
H5W	0.4920	0.6310	0.2969	0.171*
OW6	0.88282 (14)	0.2150 (3)	0.1377 (2)	0.0466 (7)
H6WA	0.9182	0.2218	0.1812	0.056*
H6WB	0.8772	0.1987	0.0761	0.056*
N1	0.90291 (13)	0.5722 (3)	0.4734 (2)	0.0337 (7)
H1A	0.8817	0.6152	0.4205	0.040*
H1B	0.8887	0.5098	0.4860	0.040*
N2	0.98862 (15)	0.5344 (3)	0.6167 (3)	0.0459 (9)
H2A	0.9738	0.4725	0.6286	0.055*
H2B	1.0241	0.5528	0.6577	0.055*
N3	0.97935 (16)	0.6976 (3)	0.5166 (3)	0.0491 (10)
H3A	0.9586	0.7413	0.4640	0.059*
H3B	1.0148	0.7161	0.5576	0.059*
C1	0.95669 (15)	0.6017 (3)	0.5347 (3)	0.0281 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni	0.0136 (3)	0.0149 (3)	0.0125 (3)	0.0014 (2)	0.0045 (2)	0.0013 (2)
Mo1	0.01433 (14)	0.01939 (14)	0.01446 (14)	0.00183 (10)	0.00376 (10)	0.00253 (10)
Mo2	0.01388 (14)	0.01949 (15)	0.01508 (14)	0.00034 (10)	0.00553 (10)	0.00090 (10)
Mo3	0.01756 (14)	0.01569 (14)	0.01377 (14)	0.00222 (10)	0.00672 (11)	0.00250 (10)
Na	0.0325 (8)	0.0282 (7)	0.0264 (7)	−0.0019 (6)	0.0084 (6)	0.0016 (6)
O1	0.0175 (10)	0.0141 (10)	0.0152 (10)	0.0003 (8)	0.0058 (8)	−0.0017 (8)
O2	0.0172 (11)	0.0126 (10)	0.0154 (10)	−0.0005 (8)	0.0067 (9)	−0.0005 (8)
O3	0.0184 (11)	0.0142 (10)	0.0173 (11)	−0.0003 (8)	0.0070 (9)	−0.0021 (8)
O4	0.0217 (11)	0.0200 (11)	0.0196 (11)	0.0070 (9)	0.0100 (9)	0.0030 (9)
O5	0.0207 (11)	0.0219 (11)	0.0133 (10)	−0.0001 (9)	0.0058 (9)	−0.0012 (9)
O6	0.0285 (13)	0.0205 (12)	0.0287 (13)	0.0032 (10)	0.0124 (11)	0.0078 (10)
O7	0.0236 (12)	0.0325 (14)	0.0225 (12)	0.0035 (10)	0.0122 (10)	0.0013 (10)
O8	0.0191 (11)	0.0167 (11)	0.0213 (11)	−0.0020 (9)	0.0072 (9)	0.0015 (9)
O9	0.0256 (12)	0.0277 (13)	0.0268 (12)	0.0074 (10)	0.0102 (10)	0.0085 (10)
O10	0.0217 (13)	0.0430 (16)	0.0248 (13)	−0.0074 (11)	0.0043 (11)	−0.0016 (11)
O11	0.0212 (12)	0.0355 (14)	0.0287 (13)	−0.0068 (10)	0.0055 (10)	−0.0018 (11)
O12	0.0266 (12)	0.0309 (13)	0.0191 (12)	0.0012 (10)	0.0118 (10)	−0.0006 (10)
OW1	0.0422 (15)	0.0270 (13)	0.0240 (13)	−0.0046 (11)	0.0126 (12)	−0.0063 (10)
OW2	0.072 (2)	0.0280 (15)	0.0297 (15)	−0.0036 (14)	0.0095 (14)	−0.0001 (12)
OW3	0.079 (3)	0.0401 (18)	0.065 (2)	−0.0005 (17)	0.041 (2)	0.0114 (16)
OW4	0.118 (9)	0.025 (4)	0.082 (7)	0.000	−0.068 (6)	0.000
OW5	0.066 (5)	0.101 (6)	0.171 (8)	0.000	−0.038 (5)	0.000
OW6	0.0470 (18)	0.056 (2)	0.0362 (16)	0.0046 (15)	0.0169 (14)	−0.0035 (14)
N1	0.0254 (16)	0.0385 (18)	0.0276 (16)	−0.0082 (13)	0.0019 (13)	0.0100 (14)
N2	0.0307 (18)	0.062 (2)	0.0360 (19)	0.0033 (17)	0.0055 (15)	0.0176 (18)
N3	0.036 (2)	0.052 (2)	0.051 (2)	−0.0205 (17)	0.0101 (17)	0.0080 (18)
C1	0.0232 (17)	0.040 (2)	0.0226 (17)	−0.0016 (15)	0.0110 (14)	−0.0006 (15)

Geometric parameters (Å, º)

Ni—O1	2.021 (2)	Na—O9	2.379 (3)
Ni—O3	2.045 (2)	Na—OW1	2.380 (3)
Ni—O2	2.049 (2)	Na—O12^ii	2.468 (3)
Ni—O1^i	2.021 (2)	Na—O6	2.615 (3)
Ni—O3^i	2.045 (2)	O1—H1	0.8723
Ni—O2^i	2.049 (2)	O2—H2	0.8574
Mo1—O10	1.701 (2)	O3—H3	0.8049
Mo1—O9	1.723 (2)	OW1—H1WA	0.8460
Mo1—O4	1.939 (2)	OW1—H1WB	0.8295
Mo1—O5	1.972 (2)	OW2—H2WA	0.8948
Mo1—O3	2.217 (2)	OW2—H2WB	0.8877
Mo1—O1	2.252 (2)	OW3—H3WA	0.8583
Mo2—O11	1.707 (2)	OW3—H3WB	0.8918
Mo2—O7	1.723 (2)	OW4—H4W	0.8542
Mo2—O8	1.945 (2)	OW5—H5W	0.9141
Mo2—O4^i	1.948 (2)	OW6—H6WA	0.8430
Mo2—O3^i	2.227 (2)	OW6—H6WB	0.8211
Mo2—O2	2.253 (2)	N1—C1	1.306 (5)
Mo3—O6	1.720 (2)	N1—H1A	0.8600
Mo3—O12	1.721 (2)	N1—H1B	0.8600
Mo3—O8	1.933 (2)	N2—C1	1.331 (5)
Mo3—O5	1.946 (2)	N2—H2A	0.8600
Mo3—O1	2.207 (2)	N2—H2B	0.8600
Mo3—O2	2.254 (2)	N3—C1	1.327 (5)
Na—OW6	2.321 (3)	N3—H3A	0.8600
Na—O7^ii	2.379 (3)	N3—H3B	0.8600
O1^i—Ni—O1	180.0	OW6—Na—O7^ii	87.20 (11)
O1^i—Ni—O3^i	82.51 (8)	OW6—Na—O9	100.76 (11)
O1—Ni—O3^i	97.49 (8)	O7^ii—Na—O9	90.75 (9)
O1^i—Ni—O3	97.49 (8)	OW6—Na—OW1	98.03 (11)
O1—Ni—O3	82.51 (8)	O7^ii—Na—OW1	166.02 (11)
O3^i—Ni—O3	180.0	O9—Na—OW1	100.92 (10)
O1^i—Ni—O2^i	82.31 (8)	OW6—Na—O12^ii	87.87 (11)
O1—Ni—O2^i	97.69 (8)	O7^ii—Na—O12^ii	85.05 (9)
O3^i—Ni—O2^i	97.00 (8)	O9—Na—O12^ii	170.22 (10)
O3—Ni—O2^i	83.00 (8)	OW1—Na—O12^ii	82.21 (9)
O1^i—Ni—O2	97.69 (8)	OW6—Na—O6	178.07 (11)
O1—Ni—O2	82.31 (8)	O7^ii—Na—O6	91.35 (9)
O3^i—Ni—O2	83.00 (8)	O9—Na—O6	80.53 (9)
O3—Ni—O2	97.00 (8)	OW1—Na—O6	83.09 (9)
O2^i—Ni—O2	180.0	O12^ii—Na—O6	90.73 (9)
O10—Mo1—O9	104.36 (12)	Ni—O1—Mo3	103.18 (9)
O10—Mo1—O4	102.42 (11)	Ni—O1—Mo1	101.65 (9)
O9—Mo1—O4	95.95 (10)	Mo3—O1—Mo1	96.10 (8)
O10—Mo1—O5	94.94 (11)	Ni—O1—H1	119.8
O9—Mo1—O5	100.56 (10)	Mo3—O1—H1	112.1
O4—Mo1—O5	152.24 (9)	Mo1—O1—H1	120.3
O10—Mo1—O3	94.42 (11)	Ni—O2—Mo2	100.72 (8)
O9—Mo1—O3	159.65 (10)	Ni—O2—Mo3	100.70 (8)
O4—Mo1—O3	72.00 (8)	Mo2—O2—Mo3	94.95 (8)
O5—Mo1—O3	85.34 (8)	Ni—O2—H2	120.7
O10—Mo1—O1	162.32 (11)	Mo2—O2—H2	116.2
O9—Mo1—O1	89.56 (10)	Mo3—O2—H2	119.1
O4—Mo1—O1	86.61 (9)	Ni—O3—Mo1	102.09 (9)
O5—Mo1—O1	71.46 (8)	Ni—O3—Mo2^i	101.72 (9)
O3—Mo1—O1	73.73 (8)	Mo1—O3—Mo2^i	96.26 (8)
O11—Mo2—O7	104.01 (12)	Ni—O3—H3	117.2
O11—Mo2—O8	97.25 (11)	Mo1—O3—H3	118.8
O7—Mo2—O8	101.53 (10)	Mo2^i—O3—H3	117.4
O11—Mo2—O4^i	101.26 (11)	Mo1—O4—Mo2^i	116.68 (11)
O7—Mo2—O4^i	95.29 (10)	Mo3—O5—Mo1	115.66 (10)
O8—Mo2—O4^i	151.12 (9)	Mo3—O6—Na	126.96 (12)
O11—Mo2—O3^i	93.03 (10)	Mo2—O7—Na^iii	133.87 (13)
O7—Mo2—O3^i	160.42 (10)	Mo3—O8—Mo2	117.83 (11)
O8—Mo2—O3^i	85.52 (9)	Mo1—O9—Na	133.33 (13)
O4^i—Mo2—O3^i	71.62 (8)	Mo3—O12—Na^iii	132.64 (13)
O11—Mo2—O2	163.68 (10)	Na—OW1—H1WA	103.0
O7—Mo2—O2	90.21 (10)	Na—OW1—H1WB	131.7
O8—Mo2—O2	71.68 (8)	H1WA—OW1—H1WB	100.6
O4^i—Mo2—O2	85.06 (9)	H2WA—OW2—H2WB	95.6
O3^i—Mo2—O2	74.53 (8)	H3WA—OW3—H3WB	101.5
O6—Mo3—O12	105.76 (11)	Na—OW6—H6WA	106.1
O6—Mo3—O8	97.66 (11)	Na—OW6—H6WB	127.7
O12—Mo3—O8	100.76 (10)	H6WA—OW6—H6WB	115.3
O6—Mo3—O5	99.89 (10)	C1—N1—H1A	120.0
O12—Mo3—O5	95.93 (10)	C1—N1—H1B	120.0
O8—Mo3—O5	151.44 (9)	H1A—N1—H1B	120.0
O6—Mo3—O1	91.96 (10)	C1—N2—H2A	120.0
O12—Mo3—O1	160.64 (10)	C1—N2—H2B	120.0
O8—Mo3—O1	84.18 (9)	H2A—N2—H2B	120.0
O5—Mo3—O1	72.91 (8)	C1—N3—H3A	120.0
O6—Mo3—O2	162.84 (10)	C1—N3—H3B	120.0
O12—Mo3—O2	89.82 (10)	H3A—N3—H3B	120.0
O8—Mo3—O2	71.87 (8)	N1—C1—N3	120.9 (4)
O5—Mo3—O2	85.27 (8)	N1—C1—N2	119.0 (4)
O1—Mo3—O2	73.80 (7)	N3—C1—N2	120.1 (4)
O3^i—Ni—O1—Mo3	−81.79 (9)	O10—Mo1—O3—Ni	−167.57 (11)
O3—Ni—O1—Mo3	98.21 (9)	O9—Mo1—O3—Ni	35.0 (3)
O2^i—Ni—O1—Mo3	−179.95 (8)	O4—Mo1—O3—Ni	90.79 (10)
O2—Ni—O1—Mo3	0.05 (8)	O5—Mo1—O3—Ni	−72.96 (9)
O3^i—Ni—O1—Mo1	179.02 (8)	O1—Mo1—O3—Ni	−0.93 (7)
O3—Ni—O1—Mo1	−0.98 (8)	O10—Mo1—O3—Mo2^i	88.99 (10)
O2^i—Ni—O1—Mo1	80.86 (9)	O9—Mo1—O3—Mo2^i	−68.4 (3)
O2—Ni—O1—Mo1	−99.14 (9)	O4—Mo1—O3—Mo2^i	−12.65 (8)
O6—Mo3—O1—Ni	170.23 (11)	O5—Mo1—O3—Mo2^i	−176.40 (9)
O12—Mo3—O1—Ni	−33.3 (3)	O1—Mo1—O3—Mo2^i	−104.37 (9)
O8—Mo3—O1—Ni	72.73 (10)	O10—Mo1—O4—Mo2^i	−74.48 (15)
O5—Mo3—O1—Ni	−90.02 (10)	O9—Mo1—O4—Mo2^i	179.37 (13)
O2—Mo3—O1—Ni	−0.05 (8)	O5—Mo1—O4—Mo2^i	52.9 (3)
O6—Mo3—O1—Mo1	−86.26 (10)	O3—Mo1—O4—Mo2^i	16.17 (11)
O12—Mo3—O1—Mo1	70.2 (3)	O1—Mo1—O4—Mo2^i	90.16 (12)
O8—Mo3—O1—Mo1	176.24 (9)	O6—Mo3—O5—Mo1	71.91 (13)
O5—Mo3—O1—Mo1	13.49 (8)	O12—Mo3—O5—Mo1	179.09 (12)
O2—Mo3—O1—Mo1	103.46 (8)	O8—Mo3—O5—Mo1	−55.2 (2)
O10—Mo1—O1—Ni	50.3 (4)	O1—Mo3—O5—Mo1	−17.09 (10)
O9—Mo1—O1—Ni	−167.28 (11)	O2—Mo3—O5—Mo1	−91.58 (12)
O4—Mo1—O1—Ni	−71.29 (9)	O10—Mo1—O5—Mo3	−174.68 (13)
O5—Mo1—O1—Ni	91.42 (10)	O9—Mo1—O5—Mo3	−69.06 (14)
O3—Mo1—O1—Ni	0.94 (7)	O4—Mo1—O5—Mo3	56.4 (2)
O10—Mo1—O1—Mo3	−54.6 (3)	O3—Mo1—O5—Mo3	91.28 (12)
O9—Mo1—O1—Mo3	87.87 (10)	O1—Mo1—O5—Mo3	16.88 (10)
O4—Mo1—O1—Mo3	−176.14 (9)	O12—Mo3—O6—Na	−163.37 (14)
O5—Mo1—O1—Mo3	−13.42 (8)	O8—Mo3—O6—Na	93.11 (15)
O3—Mo1—O1—Mo3	−103.91 (9)	O5—Mo3—O6—Na	−64.26 (16)
O1^i—Ni—O2—Mo2	82.76 (9)	O1—Mo3—O6—Na	8.73 (15)
O1—Ni—O2—Mo2	−97.24 (9)	O2—Mo3—O6—Na	42.1 (4)
O3^i—Ni—O2—Mo2	1.34 (8)	O7^ii—Na—O6—Mo3	137.67 (16)
O3—Ni—O2—Mo2	−178.66 (8)	O9—Na—O6—Mo3	47.14 (16)
O1^i—Ni—O2—Mo3	179.95 (8)	OW1—Na—O6—Mo3	−55.20 (16)
O1—Ni—O2—Mo3	−0.05 (8)	O12^ii—Na—O6—Mo3	−137.26 (16)
O3^i—Ni—O2—Mo3	98.53 (9)	O11—Mo2—O7—Na^iii	153.45 (17)
O3—Ni—O2—Mo3	−81.47 (9)	O8—Mo2—O7—Na^iii	52.86 (18)
O11—Mo2—O2—Ni	40.2 (4)	O4^i—Mo2—O7—Na^iii	−103.54 (17)
O7—Mo2—O2—Ni	−168.83 (10)	O3^i—Mo2—O7—Na^iii	−56.7 (4)
O8—Mo2—O2—Ni	89.09 (10)	O2—Mo2—O7—Na^iii	−18.48 (17)
O4^i—Mo2—O2—Ni	−73.54 (9)	O6—Mo3—O8—Mo2	177.07 (13)
O3^i—Mo2—O2—Ni	−1.26 (8)	O12—Mo3—O8—Mo2	69.34 (14)
O11—Mo2—O2—Mo3	−61.7 (4)	O5—Mo3—O8—Mo2	−55.4 (2)
O7—Mo2—O2—Mo3	89.27 (10)	O1—Mo3—O8—Mo2	−91.74 (12)
O8—Mo2—O2—Mo3	−12.81 (8)	O2—Mo3—O8—Mo2	−16.90 (10)
O4^i—Mo2—O2—Mo3	−175.44 (9)	O11—Mo2—O8—Mo3	−175.39 (13)
O3^i—Mo2—O2—Mo3	−103.16 (8)	O7—Mo2—O8—Mo3	−69.43 (14)
O6—Mo3—O2—Ni	−34.8 (4)	O4^i—Mo2—O8—Mo3	54.9 (2)
O12—Mo3—O2—Ni	169.58 (11)	O3^i—Mo2—O8—Mo3	92.11 (12)
O8—Mo3—O2—Ni	−89.03 (10)	O2—Mo2—O8—Mo3	16.93 (10)
O5—Mo3—O2—Ni	73.61 (9)	O10—Mo1—O9—Na	162.78 (17)
O1—Mo3—O2—Ni	0.05 (8)	O4—Mo1—O9—Na	−92.75 (18)
O6—Mo3—O2—Mo2	67.1 (3)	O5—Mo1—O9—Na	64.84 (18)
O12—Mo3—O2—Mo2	−88.52 (10)	O3—Mo1—O9—Na	−40.5 (4)
O8—Mo3—O2—Mo2	12.88 (8)	O1—Mo1—O9—Na	−6.20 (17)
O5—Mo3—O2—Mo2	175.52 (9)	OW6—Na—O9—Mo1	132.98 (18)
O1—Mo3—O2—Mo2	101.96 (8)	O7^ii—Na—O9—Mo1	−139.73 (18)
O1^i—Ni—O3—Mo1	−179.00 (8)	OW1—Na—O9—Mo1	32.5 (2)
O1—Ni—O3—Mo1	1.00 (8)	O6—Na—O9—Mo1	−48.48 (18)
O2^i—Ni—O3—Mo1	−97.75 (9)	O6—Mo3—O12—Na^iii	−153.45 (16)
O2—Ni—O3—Mo1	82.25 (9)	O8—Mo3—O12—Na^iii	−52.23 (18)
O1^i—Ni—O3—Mo2^i	−79.89 (9)	O5—Mo3—O12—Na^iii	104.50 (17)
O1—Ni—O3—Mo2^i	100.11 (9)	O1—Mo3—O12—Na^iii	51.0 (4)
O2^i—Ni—O3—Mo2^i	1.36 (8)	O2—Mo3—O12—Na^iii	19.27 (17)
O2—Ni—O3—Mo2^i	−178.64 (8)

Symmetry codes: (i) −x+3/2, −y+3/2, −z; (ii) −x+3/2, y−1/2, −z+1/2; (iii) −x+3/2, y+1/2, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···OW1	0.87	1.85	2.703 (3)	167
O2—H2···O6^iii	0.86	2.06	2.896 (3)	165
O3—H3···OW3^iii	0.80	1.94	2.722 (4)	164
OW1—H1WB···O12^iv	0.83	2.00	2.822 (3)	173
OW1—H1WA···OW2	0.85	2.07	2.892 (4)	165
OW2—H2WA···O8	0.89	1.92	2.786 (4)	164
OW2—H2WB···O5^ii	0.89	2.00	2.818 (3)	152
OW3—H3WA···OW6^iii	0.86	2.12	2.932 (4)	158
OW5—H5W···OW4	0.91	2.24	2.630 (11)	105
OW6—H6WA···OW5^ii	0.84	1.95	2.736 (4)	155
OW6—H6WB···OW2^v	0.82	1.95	2.754 (4)	165
OW6—H6WA···OW5^vi	0.84	1.95	2.736 (4)	155
N1—H1A···O5	0.86	2.17	3.017 (4)	168
N1—H1B···O4^vii	0.86	2.01	2.832 (4)	159
N2—H2B···O9^viii	0.86	2.22	2.966 (4)	145
N3—H3B···O7^ix	0.86	2.20	3.029 (4)	161
N3—H3B···O11^ix	0.86	2.81	3.243 (4)	113

Symmetry codes: (ii) −x+3/2, y−1/2, −z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x+3/2, −y+1/2, −z; (vi) x+1/2, y−1/2, z; (vii) x, −y+1, z+1/2; (viii) −x+2, −y+1, −z+1; (ix) x+1/2, −y+3/2, z+1/2.