Tris(propane-1,3-diammonium) di-μ₅-phosphato-penta­molybdate(VI) tetra­hydrate

The anions of the title compound, (C₃H₁₂N₂)[Mo₅O₁₅(PO₄)₂]·4H₂O, consist of five MoO₆ octa­hedra and two PO₄ tetra­hedra. The octa­hedra form a ring. The PO₄ tetra­hedra are located above and below the ring and connected to it by three O atoms. Anions and cations are connected through an extensive network of hydrogen bonds

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.033
• wR factor = 0.092
• Data-to-parameter ratio = 17.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.98
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT731_ALERT_1_C Bond    Calc     0.83(4), Rep   0.829(19) ......       2.11 su-Rat
              O24  -H1      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(5), Rep   0.841(19) ......       2.63 su-Rat
              O24  -H2      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.83(5), Rep   0.833(19) ......       2.63 su-Rat
              O26  -H5      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.86(5), Rep   0.858(19) ......       2.63 su-Rat
              O27  -H8      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.83(4), Rep   0.829(19) ......       2.11 su-Rat
              O24  -H1      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(5), Rep   0.841(19) ......       2.63 su-Rat
              O24  -H2      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.83(5), Rep   0.833(19) ......       2.63 su-Rat
              O26  -H5      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.86(5), Rep   0.858(19) ......       2.63 su-Rat
              O27  -H8      1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.86(5), Rep   1.865(19) ......       2.63 su-Rat
              H2   -O9      1.555   4.575
PLAT736_ALERT_1_C H...A   Calc     1.99(5), Rep     1.99(2) ......       2.50 su-Rat
              H8   -O20     1.555   4.576

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

  11 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 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

---

Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Tris(propane-1,3-diammonium) di-µ₅-phosphato-pentamolybdate(VI) tetrahydrate

Crystal data

(C3H12N2)3[Mo5O15(PO4)2]·4H2O	F(000) = 2384
Mr = 1210.14	Dx = 2.396 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 12.971 (3) Å	Cell parameters from 13972 reflections
b = 15.608 (3) Å	θ = 2.3–28.3°
c = 16.750 (3) Å	µ = 2.02 mm^−1
β = 98.398 (3)°	T = 298 K
V = 3354.5 (12) Å^3	Block, colourless
Z = 4	0.34 × 0.17 × 0.15 mm

Data collection

Bruker SMART CCD area-detector diffractometer	8130 independent reflections
Radiation source: fine-focus sealed tube	7286 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.024
φ and ω scans	θmax = 28.3°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −17→16
Tmin = 0.547, Tmax = 0.751	k = −10→20
21375 measured reflections	l = −21→22

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)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.092	H atoms treated by a mixture of independent and constrained refinement
S = 1.01	w = 1/[σ^2(Fo^2) + (0.064P)^2 + 2.6086P] where P = (Fo^2 + 2Fc^2)/3
8130 reflections	(Δ/σ)max = 0.001
466 parameters	Δρmax = 0.72 e Å^−3
13 restraints	Δρmin = −2.47 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	0.94322 (2)	0.831621 (18)	0.394089 (16)	0.01625 (7)
Mo2	1.08455 (2)	0.649617 (18)	0.412108 (16)	0.01531 (7)
Mo3	1.12745 (2)	0.588057 (18)	0.227447 (16)	0.01562 (7)
Mo4	0.99401 (2)	0.714039 (18)	0.087232 (16)	0.01610 (7)
Mo5	0.84299 (2)	0.846657 (18)	0.177606 (17)	0.01679 (7)
N1	0.7517 (3)	0.5646 (2)	−0.0759 (2)	0.0308 (7)
H1A	0.6993	0.5810	−0.1131	0.046*
H1B	0.8109	0.5659	−0.0968	0.046*
H1C	0.7565	0.6000	−0.0338	0.046*
N2	0.8820 (2)	0.4445 (2)	0.16406 (19)	0.0265 (7)
H2A	0.8708	0.4682	0.2103	0.040*
H2B	0.9465	0.4563	0.1554	0.040*
H2C	0.8739	0.3879	0.1667	0.040*
N3	0.3877 (2)	0.7718 (2)	0.2341 (2)	0.0316 (7)
H3A	0.3258	0.7956	0.2362	0.047*
H3B	0.4355	0.8127	0.2342	0.047*
H3C	0.4047	0.7381	0.2768	0.047*
N4	0.6141 (3)	0.5634 (2)	0.1915 (2)	0.0347 (8)
H4A	0.6312	0.5204	0.2258	0.052*
H4B	0.6651	0.6021	0.1970	0.052*
H4C	0.6047	0.5434	0.1412	0.052*
N5	0.8100 (2)	0.5232 (2)	0.43172 (17)	0.0234 (6)
H5A	0.8248	0.5367	0.3830	0.035*
H5B	0.7637	0.4807	0.4273	0.035*
H5C	0.8679	0.5065	0.4630	0.035*
N6	0.6103 (2)	0.5238 (2)	0.63182 (18)	0.0254 (6)
H6A	0.5507	0.4950	0.6302	0.038*
H6B	0.6033	0.5756	0.6525	0.038*
H6C	0.6610	0.4956	0.6625	0.038*
O1	1.07591 (18)	0.86166 (15)	0.32927 (14)	0.0179 (5)
O2	1.13682 (17)	0.71418 (14)	0.29794 (14)	0.0167 (5)
O3	1.01401 (17)	0.79884 (15)	0.19509 (14)	0.0172 (5)
O4	1.20079 (19)	0.84521 (16)	0.23048 (16)	0.0228 (5)
O5	0.94128 (17)	0.69198 (15)	0.33634 (13)	0.0153 (4)
O6	0.95592 (17)	0.63188 (15)	0.19752 (13)	0.0160 (4)
O7	0.80030 (17)	0.71930 (15)	0.22328 (14)	0.0187 (5)
O8	0.82453 (19)	0.56961 (16)	0.27749 (14)	0.0202 (5)
O9	1.05278 (18)	0.76051 (16)	0.45166 (13)	0.0195 (5)
O10	1.08211 (19)	0.56244 (15)	0.32820 (14)	0.0181 (5)
O11	1.12311 (18)	0.66545 (15)	0.13965 (14)	0.0187 (5)
O12	0.86285 (18)	0.77282 (16)	0.09068 (14)	0.0206 (5)
O13	0.86880 (19)	0.86828 (16)	0.29149 (14)	0.0202 (5)
O14	0.9679 (2)	0.92812 (17)	0.44008 (16)	0.0281 (6)
O15	0.8391 (2)	0.79525 (17)	0.43723 (16)	0.0264 (6)
O16	1.0267 (2)	0.58576 (17)	0.47605 (16)	0.0284 (6)
O17	1.2142 (2)	0.64440 (17)	0.45035 (16)	0.0266 (6)
O18	1.09275 (19)	0.49329 (16)	0.17670 (15)	0.0232 (5)
O19	1.25987 (19)	0.57837 (17)	0.25180 (16)	0.0251 (5)
O20	1.0470 (2)	0.78131 (18)	0.02358 (16)	0.0286 (6)
O21	0.9443 (2)	0.63196 (17)	0.02592 (15)	0.0252 (5)
O22	0.8909 (2)	0.94282 (16)	0.14534 (16)	0.0252 (5)
O23	0.71168 (19)	0.86363 (17)	0.15633 (16)	0.0255 (5)
O24	0.6928 (2)	0.65571 (18)	0.05909 (18)	0.0313 (6)
O25	0.5015 (2)	0.8998 (2)	0.1723 (2)	0.0384 (7)
O26	0.8493 (2)	0.2627 (2)	0.1756 (2)	0.0394 (7)
O27	0.4069 (3)	0.6743 (2)	0.38290 (19)	0.0423 (8)
P1	1.10962 (6)	0.80475 (5)	0.26312 (5)	0.01376 (16)
P2	0.87970 (6)	0.65162 (5)	0.25865 (5)	0.01339 (16)
C1	0.7324 (3)	0.4761 (3)	−0.0491 (2)	0.0287 (8)
H1D	0.7259	0.4381	−0.0954	0.034*
H1E	0.6668	0.4749	−0.0277	0.034*
C2	0.8177 (3)	0.4434 (2)	0.0143 (2)	0.0246 (7)
H2D	0.8849	0.4599	0.0003	0.030*
H2E	0.8150	0.3814	0.0161	0.030*
C3	0.8061 (3)	0.4795 (2)	0.09673 (19)	0.0206 (7)
H3D	0.8143	0.5413	0.0953	0.025*
H3E	0.7361	0.4677	0.1077	0.025*
C4	0.3829 (3)	0.7206 (3)	0.1597 (3)	0.0313 (8)
H4D	0.3630	0.7577	0.1135	0.038*
H4E	0.3293	0.6773	0.1594	0.038*
C5	0.4853 (3)	0.6772 (3)	0.1510 (2)	0.0309 (8)
H5D	0.4811	0.6552	0.0964	0.037*
H5E	0.5403	0.7198	0.1584	0.037*
C6	0.5148 (3)	0.6046 (3)	0.2093 (2)	0.0342 (9)
H6D	0.4593	0.5625	0.2043	0.041*
H6E	0.5247	0.6263	0.2642	0.041*
C7	0.7662 (3)	0.5989 (2)	0.4679 (2)	0.0290 (8)
H7A	0.7042	0.6176	0.4327	0.035*
H7B	0.8166	0.6451	0.4717	0.035*
C8	0.7381 (3)	0.5813 (3)	0.5509 (2)	0.0275 (8)
H8A	0.7325	0.6354	0.5785	0.033*
H8B	0.7939	0.5487	0.5818	0.033*
C9	0.6365 (3)	0.5322 (2)	0.5489 (2)	0.0237 (7)
H9A	0.5809	0.5623	0.5151	0.028*
H9B	0.6434	0.4758	0.5259	0.028*
H1	0.710 (4)	0.682 (4)	0.102 (2)	0.080*
H2	0.648 (4)	0.685 (3)	0.029 (3)	0.080*
H3	0.492 (4)	0.9511 (18)	0.158 (4)	0.080*
H4	0.565 (2)	0.888 (4)	0.163 (4)	0.080*
H5	0.814 (4)	0.242 (4)	0.208 (2)	0.080*
H6	0.813 (4)	0.258 (4)	0.1295 (16)	0.080*
H7	0.348 (2)	0.676 (4)	0.399 (3)	0.080*
H8	0.450 (3)	0.693 (4)	0.423 (3)	0.080*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.01711 (14)	0.01543 (14)	0.01651 (14)	0.00151 (10)	0.00343 (10)	−0.00252 (10)
Mo2	0.01646 (14)	0.01465 (14)	0.01420 (13)	0.00109 (10)	0.00016 (10)	0.00057 (10)
Mo3	0.01435 (14)	0.01587 (14)	0.01664 (14)	0.00193 (10)	0.00231 (10)	−0.00112 (10)
Mo4	0.01587 (14)	0.01843 (15)	0.01363 (13)	−0.00105 (10)	0.00096 (10)	−0.00018 (10)
Mo5	0.01441 (14)	0.01584 (14)	0.01950 (14)	0.00261 (10)	0.00035 (10)	0.00248 (10)
N1	0.0290 (17)	0.0354 (19)	0.0264 (16)	0.0056 (14)	−0.0015 (13)	0.0031 (14)
N2	0.0257 (16)	0.0228 (16)	0.0291 (16)	−0.0014 (13)	−0.0029 (13)	−0.0015 (13)
N3	0.0217 (16)	0.0310 (18)	0.044 (2)	0.0071 (13)	0.0117 (14)	0.0013 (15)
N4	0.0283 (18)	0.0347 (19)	0.040 (2)	0.0073 (15)	0.0021 (15)	−0.0056 (16)
N5	0.0282 (15)	0.0242 (16)	0.0184 (14)	−0.0044 (13)	0.0055 (12)	−0.0008 (12)
N6	0.0253 (15)	0.0257 (16)	0.0268 (15)	0.0036 (13)	0.0095 (12)	−0.0012 (13)
O1	0.0173 (11)	0.0160 (11)	0.0207 (11)	−0.0016 (9)	0.0041 (9)	−0.0048 (9)
O2	0.0173 (11)	0.0144 (11)	0.0184 (11)	0.0014 (9)	0.0023 (9)	0.0001 (9)
O3	0.0152 (11)	0.0176 (11)	0.0178 (11)	0.0012 (9)	−0.0010 (8)	0.0004 (9)
O4	0.0160 (12)	0.0239 (13)	0.0296 (13)	−0.0011 (9)	0.0068 (10)	0.0046 (10)
O5	0.0143 (10)	0.0169 (11)	0.0142 (10)	0.0015 (9)	0.0004 (8)	−0.0026 (9)
O6	0.0132 (10)	0.0179 (11)	0.0173 (11)	−0.0009 (9)	0.0036 (8)	−0.0020 (9)
O7	0.0133 (11)	0.0185 (12)	0.0238 (12)	0.0015 (9)	0.0005 (9)	0.0018 (9)
O8	0.0216 (12)	0.0190 (12)	0.0208 (11)	−0.0060 (9)	0.0062 (9)	0.0015 (9)
O9	0.0224 (12)	0.0182 (12)	0.0165 (11)	0.0020 (9)	−0.0015 (9)	−0.0046 (9)
O10	0.0241 (12)	0.0127 (11)	0.0174 (11)	0.0005 (9)	0.0026 (9)	0.0016 (9)
O11	0.0157 (11)	0.0217 (12)	0.0189 (11)	0.0015 (9)	0.0032 (9)	0.0000 (9)
O12	0.0204 (12)	0.0231 (12)	0.0164 (11)	0.0034 (10)	−0.0035 (9)	−0.0015 (10)
O13	0.0194 (11)	0.0213 (12)	0.0197 (11)	0.0059 (9)	0.0016 (9)	0.0006 (10)
O14	0.0298 (14)	0.0246 (13)	0.0304 (14)	−0.0015 (11)	0.0069 (11)	−0.0105 (11)
O15	0.0263 (13)	0.0241 (13)	0.0308 (14)	0.0016 (10)	0.0110 (11)	0.0007 (11)
O16	0.0333 (15)	0.0271 (14)	0.0252 (13)	−0.0022 (11)	0.0055 (11)	0.0080 (11)
O17	0.0209 (13)	0.0304 (15)	0.0267 (13)	0.0023 (10)	−0.0028 (10)	−0.0010 (11)
O18	0.0240 (12)	0.0198 (12)	0.0264 (13)	−0.0005 (10)	0.0057 (10)	−0.0081 (10)
O19	0.0182 (12)	0.0268 (13)	0.0293 (13)	0.0021 (10)	0.0002 (10)	0.0013 (11)
O20	0.0291 (14)	0.0323 (15)	0.0243 (13)	−0.0058 (11)	0.0034 (11)	0.0086 (11)
O21	0.0236 (13)	0.0280 (14)	0.0235 (12)	−0.0017 (11)	0.0017 (10)	−0.0072 (11)
O22	0.0227 (12)	0.0212 (13)	0.0314 (14)	0.0003 (10)	0.0032 (10)	0.0049 (11)
O23	0.0174 (12)	0.0254 (13)	0.0324 (14)	0.0037 (10)	−0.0004 (10)	0.0043 (11)
O24	0.0283 (14)	0.0277 (15)	0.0337 (15)	0.0057 (11)	−0.0090 (12)	−0.0012 (12)
O25	0.0323 (16)	0.0276 (15)	0.059 (2)	0.0019 (12)	0.0181 (15)	0.0018 (15)
O26	0.0379 (17)	0.0371 (17)	0.0440 (18)	−0.0018 (14)	0.0085 (14)	0.0014 (15)
O27	0.0391 (18)	0.056 (2)	0.0315 (16)	−0.0115 (16)	0.0046 (13)	−0.0083 (15)
P1	0.0123 (4)	0.0137 (4)	0.0151 (4)	−0.0013 (3)	0.0012 (3)	−0.0002 (3)
P2	0.0125 (4)	0.0136 (4)	0.0141 (4)	−0.0008 (3)	0.0020 (3)	−0.0007 (3)
C1	0.0269 (19)	0.034 (2)	0.0248 (18)	−0.0100 (16)	0.0022 (14)	−0.0105 (16)
C2	0.0284 (18)	0.0201 (17)	0.0273 (18)	−0.0003 (14)	0.0106 (15)	−0.0025 (14)
C3	0.0205 (16)	0.0228 (17)	0.0180 (15)	0.0015 (13)	0.0016 (12)	−0.0006 (13)
C4	0.0266 (19)	0.029 (2)	0.038 (2)	0.0022 (16)	0.0043 (16)	0.0001 (17)
C5	0.031 (2)	0.032 (2)	0.032 (2)	0.0067 (17)	0.0131 (16)	−0.0001 (17)
C6	0.031 (2)	0.042 (2)	0.031 (2)	0.0115 (18)	0.0072 (16)	−0.0015 (18)
C7	0.037 (2)	0.0195 (18)	0.034 (2)	0.0009 (15)	0.0150 (17)	0.0010 (15)
C8	0.0256 (18)	0.030 (2)	0.0281 (19)	−0.0032 (15)	0.0069 (15)	−0.0079 (16)
C9	0.0253 (18)	0.0251 (18)	0.0209 (16)	−0.0011 (14)	0.0037 (14)	−0.0022 (14)

Geometric parameters (Å, º)

Mo1—O14	1.701 (3)	N5—H5A	0.8900
Mo1—O15	1.719 (3)	N5—H5B	0.8900
Mo1—O13	1.931 (2)	N5—H5C	0.8900
Mo1—O9	1.944 (2)	N6—C9	1.484 (4)
Mo1—O1	2.215 (2)	N6—H6A	0.8900
Mo1—O5	2.383 (2)	N6—H6B	0.8900
Mo2—O17	1.712 (3)	N6—H6C	0.8900
Mo2—O16	1.714 (3)	O1—P1	1.533 (2)
Mo2—O9	1.919 (2)	O2—P1	1.550 (2)
Mo2—O10	1.953 (2)	O3—P1	1.560 (2)
Mo2—O5	2.194 (2)	O4—P1	1.512 (2)
Mo2—O2	2.347 (2)	O5—P2	1.557 (2)
Mo3—O19	1.713 (2)	O6—P2	1.554 (2)
Mo3—O18	1.732 (2)	O7—P2	1.533 (2)
Mo3—O11	1.897 (2)	O8—P2	1.522 (2)
Mo3—O10	1.909 (2)	O24—H1	0.829 (19)
Mo3—O2	2.290 (2)	O24—H2	0.841 (19)
Mo3—O6	2.312 (2)	O25—H3	0.838 (19)
Mo4—O21	1.708 (3)	O25—H4	0.880 (15)
Mo4—O20	1.711 (3)	O26—H5	0.833 (19)
Mo4—O11	1.929 (2)	O26—H6	0.849 (19)
Mo4—O12	1.941 (2)	O27—H7	0.852 (19)
Mo4—O3	2.224 (2)	O27—H8	0.858 (19)
Mo4—O6	2.360 (2)	C1—C2	1.507 (5)
Mo5—O23	1.709 (2)	C1—H1D	0.9700
Mo5—O22	1.740 (3)	C1—H1E	0.9700
Mo5—O12	1.904 (2)	C2—C3	1.519 (5)
Mo5—O13	1.918 (2)	C2—H2D	0.9700
Mo5—O7	2.229 (2)	C2—H2E	0.9700
Mo5—O3	2.318 (2)	C3—H3D	0.9700
N1—C1	1.485 (5)	C3—H3E	0.9700
N1—H1A	0.8900	C4—C5	1.517 (5)
N1—H1B	0.8900	C4—H4D	0.9700
N1—H1C	0.8900	C4—H4E	0.9700
N2—C3	1.488 (4)	C5—C6	1.508 (6)
N2—H2A	0.8900	C5—H5D	0.9700
N2—H2B	0.8900	C5—H5E	0.9700
N2—H2C	0.8900	C6—H6D	0.9700
N3—C4	1.474 (5)	C6—H6E	0.9700
N3—H3A	0.8900	C7—C8	1.513 (5)
N3—H3B	0.8900	C7—H7A	0.9700
N3—H3C	0.8900	C7—H7B	0.9700
N4—C6	1.508 (5)	C8—C9	1.520 (5)
N4—H4A	0.8900	C8—H8A	0.9700
N4—H4B	0.8900	C8—H8B	0.9700
N4—H4C	0.8900	C9—H9A	0.9700
N5—C7	1.479 (5)	C9—H9B	0.9700
O14—Mo1—O15	102.10 (13)	C7—N5—H5B	109.5
O14—Mo1—O13	100.21 (12)	H5A—N5—H5B	109.5
O15—Mo1—O13	98.66 (12)	C7—N5—H5C	109.5
O14—Mo1—O9	101.84 (12)	H5A—N5—H5C	109.5
O15—Mo1—O9	99.51 (12)	H5B—N5—H5C	109.5
O13—Mo1—O9	147.64 (10)	C9—N6—H6A	109.5
O14—Mo1—O1	85.77 (11)	C9—N6—H6B	109.5
O15—Mo1—O1	172.13 (11)	H6A—N6—H6B	109.5
O13—Mo1—O1	79.88 (10)	C9—N6—H6C	109.5
O9—Mo1—O1	78.47 (10)	H6A—N6—H6C	109.5
O14—Mo1—O5	169.71 (11)	H6B—N6—H6C	109.5
O15—Mo1—O5	84.62 (10)	P1—O1—Mo1	123.77 (13)
O13—Mo1—O5	86.30 (9)	P1—O2—Mo3	126.72 (13)
O9—Mo1—O5	69.08 (9)	P1—O2—Mo2	128.39 (13)
O1—Mo1—O5	87.57 (8)	Mo3—O2—Mo2	92.93 (8)
O17—Mo2—O16	103.55 (13)	P1—O3—Mo4	127.93 (13)
O17—Mo2—O9	99.35 (11)	P1—O3—Mo5	135.85 (14)
O16—Mo2—O9	99.96 (12)	Mo4—O3—Mo5	95.34 (8)
O17—Mo2—O10	98.50 (12)	P2—O5—Mo2	130.49 (13)
O16—Mo2—O10	94.70 (12)	P2—O5—Mo1	133.08 (13)
O9—Mo2—O10	153.49 (10)	Mo2—O5—Mo1	94.76 (8)
O17—Mo2—O5	159.01 (11)	P2—O6—Mo3	126.89 (13)
O16—Mo2—O5	97.23 (11)	P2—O6—Mo4	129.35 (13)
O9—Mo2—O5	73.83 (9)	Mo3—O6—Mo4	91.47 (8)
O10—Mo2—O5	82.55 (9)	P2—O7—Mo5	124.11 (13)
O17—Mo2—O2	86.57 (11)	Mo2—O9—Mo1	121.45 (11)
O16—Mo2—O2	164.47 (11)	Mo3—O10—Mo2	121.04 (12)
O9—Mo2—O2	89.79 (9)	Mo3—O11—Mo4	121.91 (12)
O10—Mo2—O2	71.89 (9)	Mo5—O12—Mo4	121.73 (12)
O5—Mo2—O2	73.76 (8)	Mo5—O13—Mo1	145.60 (14)
O19—Mo3—O18	102.78 (12)	H1—O24—H2	109 (3)
O19—Mo3—O11	98.97 (11)	H3—O25—H4	105 (3)
O18—Mo3—O11	100.78 (11)	H5—O26—H6	106 (3)
O19—Mo3—O10	101.46 (11)	H7—O27—H8	104 (3)
O18—Mo3—O10	99.41 (11)	O4—P1—O1	109.89 (14)
O11—Mo3—O10	147.18 (10)	O4—P1—O2	111.72 (14)
O19—Mo3—O2	88.69 (11)	O1—P1—O2	109.25 (13)
O18—Mo3—O2	167.83 (10)	O4—P1—O3	109.95 (14)
O11—Mo3—O2	81.13 (9)	O1—P1—O3	106.38 (13)
O10—Mo3—O2	73.98 (9)	O2—P1—O3	109.51 (13)
O19—Mo3—O6	167.83 (11)	O8—P2—O7	110.49 (14)
O18—Mo3—O6	88.47 (10)	O8—P2—O6	109.48 (13)
O11—Mo3—O6	74.03 (9)	O7—P2—O6	109.76 (13)
O10—Mo3—O6	80.95 (9)	O8—P2—O5	111.49 (14)
O2—Mo3—O6	80.47 (8)	O7—P2—O5	106.13 (13)
O21—Mo4—O20	103.68 (13)	O6—P2—O5	109.44 (13)
O21—Mo4—O11	101.85 (11)	N1—C1—C2	112.9 (3)
O20—Mo4—O11	97.11 (12)	N1—C1—H1D	109.0
O21—Mo4—O12	96.69 (11)	C2—C1—H1D	109.0
O20—Mo4—O12	99.34 (12)	N1—C1—H1E	109.0
O11—Mo4—O12	151.48 (10)	C2—C1—H1E	109.0
O21—Mo4—O3	157.45 (11)	H1D—C1—H1E	107.8
O20—Mo4—O3	97.54 (11)	C1—C2—C3	110.8 (3)
O11—Mo4—O3	82.75 (9)	C1—C2—H2D	109.5
O12—Mo4—O3	72.14 (9)	C3—C2—H2D	109.5
O21—Mo4—O6	87.66 (11)	C1—C2—H2E	109.5
O20—Mo4—O6	166.10 (10)	C3—C2—H2E	109.5
O11—Mo4—O6	72.36 (9)	H2D—C2—H2E	108.1
O12—Mo4—O6	87.07 (9)	N2—C3—C2	114.2 (3)
O3—Mo4—O6	72.56 (8)	N2—C3—H3D	108.7
O23—Mo5—O22	101.05 (12)	C2—C3—H3D	108.7
O23—Mo5—O12	100.16 (12)	N2—C3—H3E	108.7
O22—Mo5—O12	100.96 (12)	C2—C3—H3E	108.7
O23—Mo5—O13	101.77 (12)	H3D—C3—H3E	107.6
O22—Mo5—O13	97.98 (12)	N3—C4—C5	113.2 (3)
O12—Mo5—O13	147.54 (10)	N3—C4—H4D	108.9
O23—Mo5—O7	85.40 (11)	C5—C4—H4D	108.9
O22—Mo5—O7	173.54 (10)	N3—C4—H4E	108.9
O12—Mo5—O7	77.93 (10)	C5—C4—H4E	108.9
O13—Mo5—O7	80.30 (10)	H4D—C4—H4E	107.7
O23—Mo5—O3	169.23 (11)	C6—C5—C4	114.6 (3)
O22—Mo5—O3	86.47 (10)	C6—C5—H5D	108.6
O12—Mo5—O3	70.60 (9)	C4—C5—H5D	108.6
O13—Mo5—O3	84.62 (9)	C6—C5—H5E	108.6
O7—Mo5—O3	87.17 (8)	C4—C5—H5E	108.6
C1—N1—H1A	109.5	H5D—C5—H5E	107.6
C1—N1—H1B	109.5	C5—C6—N4	109.6 (3)
H1A—N1—H1B	109.5	C5—C6—H6D	109.7
C1—N1—H1C	109.5	N4—C6—H6D	109.7
H1A—N1—H1C	109.5	C5—C6—H6E	109.7
H1B—N1—H1C	109.5	N4—C6—H6E	109.7
C3—N2—H2A	109.5	H6D—C6—H6E	108.2
C3—N2—H2B	109.5	N5—C7—C8	113.0 (3)
H2A—N2—H2B	109.5	N5—C7—H7A	109.0
C3—N2—H2C	109.5	C8—C7—H7A	109.0
H2A—N2—H2C	109.5	N5—C7—H7B	109.0
H2B—N2—H2C	109.5	C8—C7—H7B	109.0
C4—N3—H3A	109.5	H7A—C7—H7B	107.8
C4—N3—H3B	109.5	C7—C8—C9	113.2 (3)
H3A—N3—H3B	109.5	C7—C8—H8A	108.9
C4—N3—H3C	109.5	C9—C8—H8A	108.9
H3A—N3—H3C	109.5	C7—C8—H8B	108.9
H3B—N3—H3C	109.5	C9—C8—H8B	108.9
C6—N4—H4A	109.5	H8A—C8—H8B	107.7
C6—N4—H4B	109.5	N6—C9—C8	109.9 (3)
H4A—N4—H4B	109.5	N6—C9—H9A	109.7
C6—N4—H4C	109.5	C8—C9—H9A	109.7
H4A—N4—H4C	109.5	N6—C9—H9B	109.7
H4B—N4—H4C	109.5	C8—C9—H9B	109.7
C7—N5—H5A	109.5	H9A—C9—H9B	108.2

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O1^i	0.89	1.96	2.826 (4)	164
N1—H1B···O18^ii	0.89	2.17	2.955 (4)	147
N1—H1C···O24	0.89	2.06	2.867 (5)	151
N1—H1C···O21	0.89	2.54	3.001 (4)	113
N2—H2A···O8	0.89	2.08	2.897 (4)	152
N2—H2B···O18	0.89	1.96	2.816 (4)	160
N2—H2C···O26	0.89	1.99	2.879 (5)	177
N3—H3A···O4^iii	0.89	1.79	2.674 (4)	175
N3—H3B···O25	0.89	1.98	2.773 (5)	148
N3—H3C···O27	0.89	2.03	2.900 (5)	164
N4—H4A···O13^iv	0.89	2.39	3.064 (5)	132
N4—H4A···O22^iv	0.89	2.53	3.327 (5)	150
N4—H4B···O8	0.89	2.35	2.895 (4)	119
N4—H4B···O7	0.89	2.53	3.414 (4)	174
N4—H4C···O14^iv	0.89	2.37	3.125 (5)	143
N5—H5A···O8	0.89	1.84	2.716 (4)	167
N5—H5B···O22^iv	0.89	2.27	3.008 (4)	141
N5—H5B···O23^iv	0.89	2.35	2.887 (4)	119
N5—H5C···O16^v	0.89	2.14	2.968 (4)	155
N5—H5C···O16	0.89	2.38	2.966 (4)	123
N6—H6A···O22^vi	0.89	2.34	2.934 (4)	125
N6—H6B···O4^vi	0.89	2.09	2.780 (4)	134
N6—H6B···O3^vi	0.89	2.44	3.276 (4)	158
N6—H6C···O19^v	0.89	2.00	2.867 (4)	163
O24—H1···O7	0.83 (2)	2.27 (2)	3.062 (4)	161 (5)
O24—H2···O9^i	0.84 (2)	1.87 (2)	2.700 (4)	172 (6)
O25—H3···O10^vii	0.84 (2)	2.01 (3)	2.760 (4)	148 (5)
O25—H4···O23	0.88 (2)	1.96 (2)	2.834 (4)	174 (6)
O26—H5···O7^iv	0.83 (2)	2.03 (3)	2.837 (4)	163 (6)
O26—H6···O15^iv	0.85 (2)	2.19 (4)	2.907 (4)	142 (6)
O27—H7···O17^iii	0.85 (2)	2.10 (3)	2.926 (4)	163 (7)
O27—H8···O20^vi	0.86 (2)	1.99 (2)	2.843 (4)	171 (7)

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