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
Supporting information
CCDC reference: 277913
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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-µ
5-phosphato-pentamolybdate(VI) tetrahydrate
top
Crystal data top
(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) Å3 | Block, colourless |
Z = 4 | 0.34 × 0.17 × 0.15 mm |
Data collection top
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 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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.064P)2 + 2.6086P] where P = (Fo2 + 2Fc2)/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 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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
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) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O1i | 0.89 | 1.96 | 2.826 (4) | 164 |
N1—H1B···O18ii | 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···O4iii | 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···O13iv | 0.89 | 2.39 | 3.064 (5) | 132 |
N4—H4A···O22iv | 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···O14iv | 0.89 | 2.37 | 3.125 (5) | 143 |
N5—H5A···O8 | 0.89 | 1.84 | 2.716 (4) | 167 |
N5—H5B···O22iv | 0.89 | 2.27 | 3.008 (4) | 141 |
N5—H5B···O23iv | 0.89 | 2.35 | 2.887 (4) | 119 |
N5—H5C···O16v | 0.89 | 2.14 | 2.968 (4) | 155 |
N5—H5C···O16 | 0.89 | 2.38 | 2.966 (4) | 123 |
N6—H6A···O22vi | 0.89 | 2.34 | 2.934 (4) | 125 |
N6—H6B···O4vi | 0.89 | 2.09 | 2.780 (4) | 134 |
N6—H6B···O3vi | 0.89 | 2.44 | 3.276 (4) | 158 |
N6—H6C···O19v | 0.89 | 2.00 | 2.867 (4) | 163 |
O24—H1···O7 | 0.83 (2) | 2.27 (2) | 3.062 (4) | 161 (5) |
O24—H2···O9i | 0.84 (2) | 1.87 (2) | 2.700 (4) | 172 (6) |
O25—H3···O10vii | 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···O7iv | 0.83 (2) | 2.03 (3) | 2.837 (4) | 163 (6) |
O26—H6···O15iv | 0.85 (2) | 2.19 (4) | 2.907 (4) | 142 (6) |
O27—H7···O17iii | 0.85 (2) | 2.10 (3) | 2.926 (4) | 163 (7) |
O27—H8···O20vi | 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. |