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The title compound, (C10H9N2)4[Mo8O26]·C10H8N2·1.5H2O or [4,4′-Hbipy]4[Mo8O26]·4,4′-bipy·1.5H2O (4,4′-bipy is 4,4′-bipyridine), has been prepared under hydro­thermal conditions. The anions are held together in an extended one-dimensional chain via O—H...O hydrogen bonds and the 4,4′-bipyridine groups are packed together through π–π stacking inter­actions. Through these hydrogen-bond contacts and π–π inter­actions, an extended three-dimensional supramolecular architecture is formed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807003479/mg2016sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807003479/mg2016Isup2.hkl
Contains datablock I

CCDC reference: 636752

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.015 Å
  • H-atom completeness 92%
  • Disorder in solvent or counterion
  • R factor = 0.045
  • wR factor = 0.102
  • Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact N1 .. N3 .. 2.70 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact N2 .. N4' .. 2.66 Ang.
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 ............ 0.50 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N5 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C23 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.03 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.39 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.40 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15 PLAT480_ALERT_4_C Long H...A H-Bond Reported H1WA .. O13 .. 2.63 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 11 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C10 H8 N2 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C10 H8 N2 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5 C10 H8 N2 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7 C10 H8 N2 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 8 H2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 9 H2 O
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:C50 H47 Mo8 N10 O27.5 Atom count from the _atom_site data: C50 H43 Mo8 N10 O27.5 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 C50 H47 Mo8 N10 O27.50 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 100.00 100.00 0.00 H 94.00 86.00 8.00 Mo 16.00 16.00 0.00 N 20.00 20.00 0.00 O 55.00 55.00 0.00 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 2 ALERT level B = Potentially serious problem 21 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 9 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); 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.

Tetrakis(4,4'-bipyridinium) octamolybdate 4,4'-bipyridine solvate sesquihydrate top
Crystal data top
(C10H9N2)4[Mo8O26]·C10H8N2·1.5H2OZ = 2
Mr = 1995.50F(000) = 1946
Triclinic, P1Dx = 2.162 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.2290 (18) ÅCell parameters from 250 reflections
b = 17.016 (3) Åθ = 2.5–25.0°
c = 18.874 (3) ŵ = 1.68 mm1
α = 86.296 (2)°T = 293 K
β = 78.076 (2)°Block, colourless
γ = 72.520 (2)°0.26 × 0.18 × 0.15 mm
V = 3065.9 (9) Å3
Data collection top
Bruker APEXII CCD area-detector
diffractometer
10700 independent reflections
Radiation source: fine-focus sealed tube7820 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
ω scansθmax = 25.0°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 1212
Tmin = 0.670, Tmax = 0.787k = 2020
22446 measured reflectionsl = 2222
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.102H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0186P)2 + 24.0938P]
where P = (Fo2 + 2Fc2)/3
10700 reflections(Δ/σ)max = 0.001
859 parametersΔρmax = 0.95 e Å3
0 restraintsΔρmin = 0.79 e Å3
Special details top

Experimental. Spectroscopic analysis: IR (KBr disk, ν, cm-1): 1629, 1596, 1488, 1209, 945, 903, 841, 719, 672, 555.

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
xyzUiso*/UeqOcc. (<1)
Mo10.61145 (6)0.94098 (3)0.79170 (3)0.02447 (14)
Mo20.58683 (6)0.79966 (4)0.91509 (3)0.02963 (15)
Mo30.75021 (6)0.65864 (4)0.79151 (3)0.02702 (14)
Mo41.08717 (6)0.65881 (3)0.71234 (3)0.02661 (14)
Mo51.11082 (6)0.79869 (4)0.58779 (3)0.02818 (14)
Mo60.94456 (6)0.94131 (3)0.70878 (3)0.02369 (14)
Mo70.77516 (6)0.79947 (3)0.67218 (3)0.02432 (14)
Mo80.92145 (6)0.80047 (3)0.82946 (3)0.02415 (14)
O10.4644 (5)0.9328 (3)0.7673 (3)0.0341 (11)
O20.5863 (5)1.0447 (3)0.7957 (3)0.0363 (12)
O30.4351 (5)0.8013 (3)0.8889 (3)0.0406 (13)
O40.5488 (6)0.7995 (4)1.0074 (3)0.0471 (14)
O50.5965 (5)0.6643 (3)0.7672 (3)0.0369 (12)
O60.8306 (5)0.5559 (3)0.7960 (3)0.0405 (13)
O71.2349 (5)0.6666 (3)0.7371 (3)0.0363 (12)
O81.1094 (5)0.5561 (3)0.7106 (3)0.0393 (13)
O91.1507 (6)0.7978 (3)0.4962 (3)0.0441 (13)
O101.2602 (5)0.7993 (3)0.6143 (3)0.0381 (12)
O111.0984 (5)0.9338 (3)0.7343 (3)0.0336 (11)
O120.8654 (5)1.0443 (3)0.7045 (3)0.0353 (12)
O130.6212 (5)0.8000 (3)0.6513 (3)0.0324 (11)
O141.0739 (5)0.8018 (3)0.8501 (3)0.0332 (11)
O150.5804 (5)0.9127 (3)0.8912 (2)0.0306 (11)
O160.6914 (5)0.6868 (3)0.8916 (3)0.0332 (11)
O171.1189 (5)0.6857 (3)0.6120 (3)0.0318 (11)
O181.0041 (5)0.9121 (3)0.6099 (2)0.0299 (11)
O190.8093 (5)0.8012 (3)0.9135 (2)0.0294 (11)
O200.8873 (5)0.7990 (3)0.5885 (2)0.0308 (11)
O210.8411 (4)0.9165 (3)0.8061 (2)0.0239 (10)
O220.9581 (4)0.6846 (3)0.8083 (2)0.0253 (10)
O230.7380 (4)0.9157 (3)0.6944 (2)0.0237 (10)
O240.8532 (5)0.6839 (3)0.6955 (2)0.0252 (10)
O250.7156 (4)0.7997 (3)0.7883 (2)0.0242 (10)
O260.9807 (4)0.7998 (3)0.7138 (2)0.0246 (10)
N11.4995 (9)0.7854 (6)0.3678 (5)0.078 (3)
N1'1.1972 (10)1.0937 (6)0.6352 (6)0.080 (3)
N2'1.7809 (8)0.8884 (5)1.1608 (5)0.062 (2)
N21.8226 (9)1.1773 (6)0.8775 (4)0.072 (3)
N3'0.3045 (9)0.6064 (6)1.0294 (5)0.074 (3)
N30.4287 (10)0.3218 (7)0.7427 (5)0.091 (3)
N4'1.8101 (10)0.2807 (6)0.7654 (4)0.071 (2)
N41.5947 (11)0.5813 (7)0.4976 (6)0.090 (3)
N51.0865 (11)0.3280 (7)0.8832 (7)0.098 (4)
N61.8958 (10)0.6652 (6)0.3794 (5)0.077 (3)
C1'1.3154 (11)1.0325 (7)0.6393 (6)0.071 (3)
H1'A1.35521.03180.67950.086*
C11.5298 (11)0.7701 (8)0.4349 (6)0.090 (4)
H1A1.58730.71870.44530.107*
C2'1.3802 (11)0.9726 (7)0.5900 (6)0.068 (3)
H2'A1.46310.93350.59590.082*
C21.4764 (10)0.8296 (7)0.4878 (6)0.075 (3)
H2A1.50110.81860.53290.090*
C3'1.3216 (9)0.9693 (6)0.5295 (5)0.055 (3)
C31.3849 (9)0.9071 (7)0.4746 (6)0.060 (3)
C4'1.1951 (11)1.0306 (7)0.5250 (6)0.070 (3)
H4'A1.15141.03170.48620.084*
C41.3554 (12)0.9187 (7)0.4043 (6)0.074 (3)
H4A1.29440.96830.39280.088*
C5'1.1381 (12)1.0883 (7)0.5783 (7)0.077 (3)
H5'A1.05271.12660.57550.093*
C51.4138 (12)0.8594 (7)0.3530 (6)0.073 (3)
H5A1.39450.86990.30670.088*
C6'1.7195 (11)0.8897 (7)1.1054 (6)0.070 (3)
H6'A1.67240.85111.10370.084*
C61.7773 (10)1.1118 (7)0.8735 (5)0.068 (3)
H6A1.75441.10270.83010.081*
C7'1.7230 (9)0.9450 (6)1.0516 (5)0.060 (3)
H7'A1.68280.94221.01220.072*
C71.7631 (11)1.0584 (7)0.9283 (5)0.067 (3)
H7A1.72971.01470.92180.080*
C81.7971 (8)1.0670 (6)0.9941 (5)0.051 (2)
C8'1.7872 (9)1.0075 (6)1.0540 (5)0.052 (2)
C9'1.8457 (9)1.0068 (6)1.1146 (5)0.054 (2)
H9'A1.88841.04671.11950.064*
C91.8443 (11)1.1348 (7)0.9992 (5)0.065 (3)
H9A1.86951.14391.04190.077*
C10'1.8407 (10)0.9475 (6)1.1671 (6)0.065 (3)
H10A1.87900.94811.20760.078*
C101.8539 (12)1.1875 (7)0.9429 (6)0.073 (3)
H10B1.88321.23290.94890.088*
C110.3818 (10)0.4067 (8)0.7359 (6)0.076 (3)
H11A0.36400.42750.69100.091*
C11'0.3279 (12)0.6279 (7)0.9602 (7)0.077 (3)
H11B0.32450.68270.95050.092*
C12'0.3562 (11)0.5786 (7)0.9027 (6)0.074 (3)
H12A0.37080.59870.85570.089*
C120.3591 (12)0.4632 (7)0.7895 (6)0.078 (3)
H12B0.32450.51920.78030.093*
C130.3882 (9)0.4362 (6)0.8587 (5)0.062 (3)
C13'0.3627 (9)0.4950 (7)0.9164 (5)0.060 (3)
C140.4374 (10)0.3515 (7)0.8657 (6)0.072 (3)
H14A0.45980.32970.90960.086*
C14'0.3414 (8)0.4702 (7)0.9888 (5)0.059 (3)
H14B0.34690.41561.00090.071*
C15'0.3122 (10)0.5280 (7)1.0415 (6)0.063 (3)
H15A0.29670.51071.08940.076*
C150.4542 (12)0.2992 (8)0.8113 (6)0.081 (3)
H15B0.48560.24310.82090.097*
C16'1.7673 (12)0.3601 (8)0.7800 (6)0.082 (3)
H16A1.76640.37580.82640.099*
C161.5636 (13)0.5971 (8)0.5699 (8)0.091 (4)
H16B1.51250.65050.58460.109*
C17'1.7246 (11)0.4203 (7)0.7322 (6)0.068 (3)
H17A1.69590.47540.74570.081*
C171.6015 (14)0.5404 (8)0.6230 (7)0.087 (4)
H17B1.57610.55730.67110.104*
C181.6757 (10)0.4599 (6)0.6069 (6)0.062 (3)
C18'1.7244 (10)0.3978 (6)0.6609 (5)0.060 (3)
C19'1.7673 (11)0.3129 (6)0.6471 (6)0.069 (3)
H19A1.76710.29420.60190.083*
C191.7065 (10)0.4431 (7)0.5322 (5)0.062 (3)
H19B1.75470.38950.51680.074*
C20'1.8089 (12)0.2580 (7)0.6991 (6)0.075 (3)
H20A1.83780.20210.68830.090*
C201.6693 (10)0.5011 (7)0.4819 (7)0.072 (3)
H20B1.69620.48540.43350.086*
C211.0594 (11)0.4056 (8)0.8594 (6)0.075 (3)
H21A1.06450.41420.80990.090*
C221.0242 (9)0.4743 (6)0.9028 (5)0.054 (2)
H22A1.00370.52680.88270.065*
C231.0197 (8)0.4640 (5)0.9760 (4)0.0400 (18)
C241.0486 (10)0.3839 (6)1.0012 (6)0.061 (3)
H24A1.04540.37351.05040.073*
C251.0821 (13)0.3192 (7)0.9540 (7)0.081 (3)
H25A1.10290.26610.97290.098*
C261.9430 (13)0.5865 (8)0.3584 (6)0.079 (3)
H26A1.94520.57510.31060.095*
C271.9881 (10)0.5218 (6)0.4026 (5)0.058 (2)
H27A2.02520.46870.38380.069*
C281.9790 (8)0.5349 (5)0.4750 (4)0.044 (2)
C291.9296 (10)0.6179 (6)0.4974 (5)0.057 (2)
H29A1.92430.63090.54530.069*
C301.8891 (5)0.6801 (3)0.4484 (3)0.073 (3)
H30A1.85590.73440.46440.088*
O1W1.3485 (5)0.8001 (3)0.7517 (3)0.0533 (15)
H1WA1.42520.76180.74820.080*
H1WB1.32880.81160.70990.080*
O2W0.1785 (5)1.2188 (3)0.7343 (3)0.094 (6)0.50
H2WA0.10131.22410.76370.141*0.50
H2WB0.21711.25300.74500.141*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0221 (3)0.0227 (3)0.0269 (3)0.0037 (2)0.0054 (2)0.0005 (2)
Mo20.0283 (3)0.0332 (3)0.0281 (3)0.0113 (3)0.0054 (3)0.0049 (3)
Mo30.0278 (3)0.0223 (3)0.0356 (3)0.0106 (2)0.0131 (3)0.0043 (2)
Mo40.0240 (3)0.0213 (3)0.0351 (3)0.0029 (2)0.0119 (3)0.0023 (2)
Mo50.0271 (3)0.0316 (3)0.0254 (3)0.0083 (3)0.0033 (2)0.0043 (3)
Mo60.0259 (3)0.0216 (3)0.0258 (3)0.0096 (2)0.0060 (2)0.0002 (2)
Mo70.0250 (3)0.0236 (3)0.0268 (3)0.0069 (2)0.0112 (2)0.0008 (2)
Mo80.0257 (3)0.0239 (3)0.0260 (3)0.0084 (2)0.0107 (2)0.0007 (2)
O10.026 (3)0.034 (3)0.042 (3)0.007 (2)0.010 (2)0.001 (2)
O20.047 (3)0.026 (3)0.035 (3)0.009 (2)0.008 (2)0.003 (2)
O30.032 (3)0.046 (3)0.045 (3)0.014 (2)0.007 (2)0.007 (2)
O40.048 (3)0.059 (4)0.032 (3)0.016 (3)0.004 (3)0.009 (3)
O50.031 (3)0.036 (3)0.051 (3)0.015 (2)0.018 (2)0.006 (2)
O60.046 (3)0.029 (3)0.051 (3)0.010 (2)0.022 (3)0.000 (2)
O70.029 (3)0.038 (3)0.045 (3)0.010 (2)0.014 (2)0.002 (2)
O80.033 (3)0.025 (3)0.059 (4)0.002 (2)0.016 (3)0.008 (2)
O90.046 (3)0.058 (4)0.026 (3)0.015 (3)0.000 (2)0.008 (2)
O100.028 (3)0.041 (3)0.043 (3)0.010 (2)0.003 (2)0.006 (2)
O110.033 (3)0.037 (3)0.035 (3)0.015 (2)0.009 (2)0.000 (2)
O120.042 (3)0.023 (3)0.041 (3)0.013 (2)0.005 (2)0.005 (2)
O130.030 (3)0.035 (3)0.038 (3)0.010 (2)0.017 (2)0.004 (2)
O140.032 (3)0.036 (3)0.037 (3)0.013 (2)0.015 (2)0.001 (2)
O150.031 (3)0.029 (3)0.028 (3)0.006 (2)0.002 (2)0.000 (2)
O160.037 (3)0.030 (3)0.036 (3)0.013 (2)0.015 (2)0.012 (2)
O170.031 (3)0.028 (3)0.033 (3)0.004 (2)0.004 (2)0.006 (2)
O180.033 (3)0.031 (3)0.025 (3)0.011 (2)0.004 (2)0.001 (2)
O190.032 (3)0.029 (3)0.030 (3)0.010 (2)0.010 (2)0.002 (2)
O200.035 (3)0.035 (3)0.025 (3)0.012 (2)0.009 (2)0.004 (2)
O210.023 (2)0.019 (2)0.032 (3)0.0084 (18)0.0066 (19)0.0019 (19)
O220.023 (2)0.020 (2)0.035 (3)0.0059 (19)0.013 (2)0.0037 (19)
O230.027 (2)0.020 (2)0.025 (2)0.0074 (19)0.0072 (19)0.0030 (18)
O240.030 (3)0.017 (2)0.032 (3)0.0060 (19)0.013 (2)0.0011 (19)
O250.023 (2)0.027 (2)0.026 (2)0.0092 (19)0.0080 (19)0.0028 (19)
O260.023 (2)0.023 (2)0.029 (3)0.0059 (19)0.0067 (19)0.0023 (19)
N10.056 (5)0.108 (8)0.057 (5)0.009 (5)0.011 (4)0.024 (5)
N1'0.079 (6)0.069 (6)0.102 (8)0.030 (5)0.038 (6)0.035 (5)
N2'0.057 (5)0.061 (5)0.071 (6)0.021 (4)0.008 (4)0.012 (4)
N20.074 (6)0.109 (7)0.045 (5)0.048 (6)0.002 (4)0.010 (5)
N3'0.064 (6)0.083 (7)0.080 (7)0.030 (5)0.019 (5)0.028 (5)
N30.066 (6)0.130 (9)0.050 (5)0.002 (6)0.000 (4)0.004 (6)
N4'0.087 (6)0.086 (7)0.051 (5)0.044 (5)0.004 (4)0.016 (5)
N40.078 (7)0.107 (9)0.093 (8)0.042 (6)0.010 (6)0.002 (7)
N50.082 (7)0.091 (8)0.111 (9)0.008 (6)0.035 (7)0.044 (7)
N60.096 (7)0.088 (7)0.064 (6)0.043 (6)0.035 (5)0.016 (5)
C1'0.067 (7)0.091 (8)0.067 (7)0.034 (6)0.033 (6)0.035 (6)
C10.047 (6)0.125 (11)0.056 (7)0.020 (6)0.004 (5)0.027 (7)
C2'0.058 (6)0.071 (7)0.078 (8)0.023 (5)0.026 (6)0.035 (6)
C20.041 (5)0.113 (9)0.052 (6)0.001 (6)0.011 (5)0.043 (6)
C3'0.047 (5)0.065 (6)0.070 (6)0.037 (5)0.030 (5)0.045 (5)
C30.042 (5)0.081 (7)0.065 (6)0.030 (5)0.017 (5)0.036 (6)
C4'0.064 (7)0.071 (7)0.081 (8)0.019 (6)0.034 (6)0.028 (6)
C40.082 (8)0.074 (7)0.091 (8)0.043 (6)0.063 (7)0.057 (7)
C5'0.062 (7)0.071 (8)0.109 (10)0.024 (6)0.048 (7)0.046 (7)
C50.093 (9)0.081 (8)0.057 (7)0.037 (7)0.027 (6)0.023 (6)
C6'0.075 (7)0.071 (7)0.068 (7)0.034 (6)0.003 (6)0.015 (6)
C60.062 (6)0.102 (9)0.052 (6)0.034 (6)0.010 (5)0.042 (6)
C7'0.046 (5)0.085 (7)0.058 (6)0.028 (5)0.010 (5)0.024 (5)
C70.068 (7)0.086 (8)0.055 (6)0.033 (6)0.008 (5)0.023 (6)
C80.030 (4)0.071 (6)0.053 (5)0.014 (4)0.001 (4)0.042 (5)
C8'0.038 (5)0.063 (6)0.046 (5)0.006 (4)0.001 (4)0.019 (4)
C9'0.040 (5)0.067 (6)0.055 (6)0.011 (4)0.007 (4)0.030 (5)
C90.078 (7)0.094 (8)0.038 (5)0.049 (6)0.010 (5)0.012 (5)
C10'0.062 (6)0.069 (7)0.058 (6)0.006 (5)0.013 (5)0.020 (5)
C100.105 (9)0.075 (7)0.064 (7)0.049 (7)0.031 (6)0.007 (6)
C110.050 (6)0.090 (9)0.070 (8)0.003 (6)0.018 (5)0.036 (7)
C11'0.084 (8)0.072 (8)0.072 (8)0.023 (6)0.012 (6)0.012 (6)
C12'0.068 (7)0.072 (7)0.075 (8)0.018 (6)0.014 (6)0.040 (6)
C120.081 (8)0.074 (8)0.056 (7)0.008 (6)0.012 (6)0.008 (6)
C130.032 (5)0.074 (7)0.065 (6)0.003 (4)0.013 (4)0.038 (5)
C13'0.037 (5)0.081 (7)0.055 (6)0.011 (5)0.008 (4)0.017 (5)
C140.059 (6)0.094 (9)0.048 (6)0.010 (6)0.002 (5)0.024 (6)
C14'0.026 (4)0.084 (7)0.064 (6)0.019 (4)0.010 (4)0.043 (6)
C15'0.049 (6)0.094 (8)0.051 (6)0.032 (6)0.009 (5)0.015 (6)
C150.079 (8)0.084 (8)0.065 (7)0.006 (6)0.014 (6)0.022 (6)
C16'0.084 (8)0.103 (10)0.053 (7)0.032 (7)0.010 (6)0.014 (7)
C160.079 (8)0.064 (8)0.122 (12)0.023 (6)0.009 (8)0.040 (8)
C17'0.089 (8)0.065 (7)0.060 (7)0.042 (6)0.005 (6)0.025 (5)
C170.119 (11)0.075 (8)0.063 (7)0.034 (8)0.003 (7)0.011 (6)
C180.056 (6)0.063 (6)0.073 (7)0.031 (5)0.007 (5)0.032 (5)
C18'0.067 (6)0.067 (7)0.049 (6)0.030 (5)0.002 (5)0.007 (5)
C19'0.085 (8)0.066 (7)0.061 (7)0.035 (6)0.003 (6)0.032 (6)
C190.051 (6)0.074 (7)0.057 (6)0.018 (5)0.005 (5)0.008 (5)
C20'0.100 (9)0.069 (7)0.064 (7)0.043 (7)0.003 (6)0.007 (6)
C200.041 (6)0.084 (8)0.088 (8)0.022 (5)0.007 (5)0.032 (7)
C210.066 (7)0.105 (10)0.053 (6)0.020 (7)0.015 (5)0.014 (6)
C220.048 (5)0.076 (7)0.038 (5)0.011 (5)0.016 (4)0.002 (5)
C230.025 (4)0.054 (5)0.042 (5)0.010 (4)0.014 (3)0.005 (4)
C240.063 (6)0.057 (6)0.064 (6)0.012 (5)0.033 (5)0.016 (5)
C250.097 (9)0.060 (7)0.093 (9)0.015 (6)0.046 (8)0.002 (6)
C260.108 (9)0.106 (10)0.041 (6)0.062 (8)0.005 (6)0.000 (6)
C270.075 (7)0.064 (6)0.044 (5)0.031 (5)0.014 (5)0.007 (5)
C280.043 (5)0.067 (6)0.033 (4)0.031 (4)0.006 (4)0.008 (4)
C290.064 (6)0.065 (6)0.050 (6)0.021 (5)0.019 (5)0.015 (5)
C300.071 (7)0.071 (7)0.083 (8)0.023 (6)0.026 (6)0.002 (6)
O1W0.042 (3)0.061 (4)0.060 (4)0.012 (3)0.021 (3)0.002 (3)
O2W0.096 (11)0.050 (8)0.097 (12)0.009 (8)0.006 (9)0.049 (8)
Geometric parameters (Å, º) top
Mo1—O11.707 (5)C3—C41.410 (13)
Mo1—O21.710 (5)C4'—C5'1.362 (16)
Mo1—O151.894 (5)C4'—H4'A0.9300
Mo1—O232.005 (4)C4—C51.354 (15)
Mo1—O252.317 (4)C4—H4A0.9300
Mo1—O212.330 (4)C5'—H5'A0.9300
Mo2—O41.704 (5)C5—H5A0.9300
Mo2—O31.715 (5)C6'—C7'1.342 (14)
Mo2—O161.926 (5)C6'—H6'A0.9300
Mo2—O151.932 (5)C6—C71.347 (14)
Mo2—O192.278 (5)C6—H6A0.9300
Mo2—O252.482 (4)C7'—C8'1.416 (12)
Mo3—O61.699 (5)C7'—H7'A0.9300
Mo3—O51.701 (5)C7—C81.386 (12)
Mo3—O161.906 (5)C7—H7A0.9300
Mo3—O241.991 (5)C8—C91.392 (12)
Mo3—O252.318 (4)C8—C8'1.477 (13)
Mo3—O222.383 (4)C8'—C9'1.393 (12)
Mo3—Mo73.2114 (9)C9'—C10'1.373 (14)
Mo4—O81.694 (5)C9'—H9'A0.9300
Mo4—O71.714 (5)C9—C101.353 (14)
Mo4—O171.903 (5)C9—H9A0.9300
Mo4—O221.996 (5)C10'—H10A0.9300
Mo4—O262.317 (4)C10—H10B0.9300
Mo4—O242.386 (4)C11—C121.377 (15)
Mo4—Mo83.2024 (9)C11—H11A0.9300
Mo5—O91.692 (5)C11'—C12'1.345 (15)
Mo5—O101.706 (5)C11'—H11B0.9300
Mo5—O171.928 (5)C12'—C13'1.413 (14)
Mo5—O181.934 (5)C12'—H12A0.9300
Mo5—O202.281 (5)C12—C131.415 (13)
Mo5—O262.472 (4)C12—H12B0.9300
Mo6—O121.699 (5)C13—C141.385 (14)
Mo6—O111.706 (5)C13—C13'1.457 (15)
Mo6—O181.889 (4)C13'—C14'1.396 (12)
Mo6—O212.008 (4)C14—C151.352 (15)
Mo6—O262.323 (4)C14—H14A0.9300
Mo6—O232.352 (4)C14'—C15'1.369 (14)
Mo7—O131.698 (4)C14'—H14B0.9300
Mo7—O201.748 (5)C15'—H15A0.9300
Mo7—O241.947 (4)C15—H15B0.9300
Mo7—O231.954 (4)C16'—C17'1.352 (15)
Mo7—O252.150 (4)C16'—H16A0.9300
Mo7—O262.393 (4)C16—C171.376 (17)
Mo8—O141.690 (4)C16—H16B0.9300
Mo8—O191.753 (5)C17'—C18'1.424 (13)
Mo8—O221.945 (4)C17'—H17A0.9300
Mo8—O211.957 (4)C17—C181.370 (15)
Mo8—O262.141 (4)C17—H17B0.9300
Mo8—O252.394 (4)C18—C191.409 (13)
N1—C51.351 (13)C18—C18'1.469 (14)
N1—C11.357 (13)C18'—C19'1.404 (13)
N1'—C1'1.351 (13)C19'—C20'1.353 (15)
N1'—C5'1.356 (14)C19'—H19A0.9300
N2'—C6'1.321 (13)C19—C201.349 (14)
N2'—C10'1.348 (12)C19—H19B0.9300
N2—C61.342 (12)C20'—H20A0.9300
N2—C101.371 (12)C20—H20B0.9300
N3'—C15'1.321 (13)C21—C221.384 (14)
N3'—C11'1.326 (13)C21—H21A0.9300
N3—C151.382 (13)C22—C231.373 (11)
N3—C111.385 (14)C22—H22A0.9300
N4'—C16'1.317 (14)C23—C241.381 (12)
N4'—C20'1.337 (13)C23—C23i1.476 (16)
N4—C161.361 (15)C24—C251.376 (14)
N4—C201.366 (14)C24—H24A0.9300
N5—C251.330 (15)C25—H25A0.9300
N5—C211.332 (15)C26—C271.361 (14)
N6—C301.326 (10)C26—H26A0.9300
N6—C261.336 (14)C27—C281.378 (11)
C1'—C2'1.343 (15)C27—H27A0.9300
C1'—H1'A0.9300C28—C291.411 (12)
C1—C21.376 (16)C28—C28ii1.485 (17)
C1—H1A0.9300C29—C301.385 (11)
C2'—C3'1.406 (13)C29—H29A0.9300
C2'—H2'A0.9300C30—H30A0.9300
C2—C31.410 (13)O1W—H1WA0.8501
C2—H2A0.9300O1W—H1WB0.8499
C3'—C4'1.412 (13)O2W—H2WA0.8499
C3'—C31.438 (14)O2W—H2WB0.8500
O1—Mo1—O2104.5 (2)Mo8—O26—Mo491.76 (16)
O1—Mo1—O15101.5 (2)Mo8—O26—Mo692.42 (16)
O2—Mo1—O15101.6 (2)Mo4—O26—Mo6162.5 (2)
O1—Mo1—O2397.1 (2)Mo8—O26—Mo7104.68 (17)
O2—Mo1—O23100.2 (2)Mo4—O26—Mo798.14 (15)
O15—Mo1—O23146.61 (18)Mo6—O26—Mo797.25 (15)
O1—Mo1—O2592.99 (19)Mo8—O26—Mo5164.3 (2)
O2—Mo1—O25162.1 (2)Mo4—O26—Mo585.78 (14)
O15—Mo1—O2578.16 (17)Mo6—O26—Mo585.60 (14)
O23—Mo1—O2573.41 (16)Mo7—O26—Mo590.97 (15)
O1—Mo1—O21163.29 (19)C5—N1—C1119.6 (11)
O2—Mo1—O2189.8 (2)C1'—N1'—C5'114.8 (11)
O15—Mo1—O2183.52 (18)C6'—N2'—C10'119.9 (9)
O23—Mo1—O2171.51 (16)C6—N2—C10115.1 (9)
O25—Mo1—O2172.27 (14)C15'—N3'—C11'115.2 (10)
O4—Mo2—O3105.3 (3)C15—N3—C11111.1 (10)
O4—Mo2—O16103.3 (2)C16'—N4'—C20'117.7 (11)
O3—Mo2—O1698.6 (2)C16—N4—C20112.5 (11)
O4—Mo2—O15103.4 (2)C25—N5—C21114.8 (10)
O3—Mo2—O1597.4 (2)C30—N6—C26117.1 (8)
O16—Mo2—O15143.8 (2)C2'—C1'—N1'125.3 (10)
O4—Mo2—O1991.8 (2)C2'—C1'—H1'A117.3
O3—Mo2—O19162.8 (2)N1'—C1'—H1'A117.3
O16—Mo2—O1978.45 (18)N1—C1—C2120.7 (10)
O15—Mo2—O1976.68 (18)N1—C1—H1A119.6
O4—Mo2—O25161.7 (2)C2—C1—H1A119.6
O3—Mo2—O2593.0 (2)C1'—C2'—C3'119.5 (10)
O16—Mo2—O2573.52 (17)C1'—C2'—H2'A120.2
O15—Mo2—O2573.41 (16)C3'—C2'—H2'A120.2
O19—Mo2—O2569.91 (15)C1—C2—C3121.1 (10)
O6—Mo3—O5104.1 (2)C1—C2—H2A119.4
O6—Mo3—O16101.4 (2)C3—C2—H2A119.4
O5—Mo3—O16102.1 (2)C2'—C3'—C4'116.6 (11)
O6—Mo3—O2499.7 (2)C2'—C3'—C3122.7 (9)
O5—Mo3—O2498.3 (2)C4'—C3'—C3120.7 (9)
O16—Mo3—O24145.98 (18)C2—C3—C4115.4 (11)
O6—Mo3—O25160.5 (2)C2—C3—C3'122.7 (9)
O5—Mo3—O2595.02 (19)C4—C3—C3'121.9 (10)
O16—Mo3—O2577.93 (17)C5'—C4'—C3'119.0 (10)
O24—Mo3—O2573.39 (16)C5'—C4'—H4'A120.5
O6—Mo3—O2289.3 (2)C3'—C4'—H4'A120.5
O5—Mo3—O22164.66 (19)C5—C4—C3121.6 (10)
O16—Mo3—O2282.26 (18)C5—C4—H4A119.2
O24—Mo3—O2271.58 (16)C3—C4—H4A119.2
O25—Mo3—O2271.29 (14)N1'—C5'—C4'124.7 (11)
O6—Mo3—Mo7134.48 (19)N1'—C5'—H5'A117.7
O5—Mo3—Mo786.19 (17)C4'—C5'—H5'A117.7
O16—Mo3—Mo7119.92 (14)N1—C5—C4121.4 (10)
O24—Mo3—Mo734.90 (12)N1—C5—H5A119.3
O25—Mo3—Mo741.99 (11)C4—C5—H5A119.3
O22—Mo3—Mo778.98 (10)N2'—C6'—C7'122.2 (10)
O8—Mo4—O7104.5 (2)N2'—C6'—H6'A118.9
O8—Mo4—O17102.2 (2)C7'—C6'—H6'A118.9
O7—Mo4—O17101.9 (2)N2—C6—C7124.0 (9)
O8—Mo4—O2298.7 (2)N2—C6—H6A118.0
O7—Mo4—O2298.0 (2)C7—C6—H6A118.0
O17—Mo4—O22146.25 (18)C6'—C7'—C8'120.6 (9)
O8—Mo4—O26160.6 (2)C6'—C7'—H7'A119.7
O7—Mo4—O2694.22 (19)C8'—C7'—H7'A119.7
O17—Mo4—O2678.08 (17)C6—C7—C8121.5 (10)
O22—Mo4—O2673.51 (16)C6—C7—H7A119.3
O8—Mo4—O2489.40 (19)C8—C7—H7A119.3
O7—Mo4—O24163.88 (19)C7—C8—C9115.2 (10)
O17—Mo4—O2482.58 (18)C7—C8—C8'122.4 (8)
O22—Mo4—O2471.43 (16)C9—C8—C8'122.4 (8)
O26—Mo4—O2471.36 (14)C9'—C8'—C7'115.9 (9)
O8—Mo4—Mo8133.76 (19)C9'—C8'—C8122.4 (9)
O7—Mo4—Mo885.45 (17)C7'—C8'—C8121.6 (8)
O17—Mo4—Mo8120.00 (14)C10'—C9'—C8'120.4 (9)
O22—Mo4—Mo835.12 (12)C10'—C9'—H9'A119.8
O26—Mo4—Mo841.93 (11)C8'—C9'—H9'A119.8
O24—Mo4—Mo878.98 (10)C10—C9—C8120.9 (9)
O9—Mo5—O10105.1 (3)C10—C9—H9A119.6
O9—Mo5—O17103.1 (2)C8—C9—H9A119.6
O10—Mo5—O1798.0 (2)N2'—C10'—C9'120.8 (9)
O9—Mo5—O18103.2 (2)N2'—C10'—H10A119.6
O10—Mo5—O1898.3 (2)C9'—C10'—H10A119.6
O17—Mo5—O18144.12 (19)C9—C10—N2123.3 (9)
O9—Mo5—O2091.9 (2)C9—C10—H10B118.3
O10—Mo5—O20163.0 (2)N2—C10—H10B118.3
O17—Mo5—O2078.09 (18)C12—C11—N3126.2 (10)
O18—Mo5—O2077.07 (18)C12—C11—H11A116.9
O9—Mo5—O26161.8 (2)N3—C11—H11A116.9
O10—Mo5—O2693.1 (2)N3'—C11'—C12'126.7 (11)
O17—Mo5—O2673.77 (17)N3'—C11'—H11B116.7
O18—Mo5—O2673.59 (16)C12'—C11'—H11B116.7
O20—Mo5—O2669.93 (15)C11'—C12'—C13'117.5 (10)
O12—Mo6—O11104.6 (2)C11'—C12'—H12A121.2
O12—Mo6—O18102.2 (2)C13'—C12'—H12A121.2
O11—Mo6—O18102.2 (2)C11—C12—C13120.1 (10)
O12—Mo6—O2199.5 (2)C11—C12—H12B119.9
O11—Mo6—O2197.1 (2)C13—C12—H12B119.9
O18—Mo6—O21146.10 (18)C14—C13—C12114.2 (11)
O12—Mo6—O26161.6 (2)C14—C13—C13'124.8 (9)
O11—Mo6—O2693.24 (19)C12—C13—C13'120.9 (9)
O18—Mo6—O2678.09 (17)C14'—C13'—C12'117.1 (10)
O21—Mo6—O2673.18 (16)C14'—C13'—C13120.3 (10)
O12—Mo6—O2389.8 (2)C12'—C13'—C13122.6 (9)
O11—Mo6—O23162.85 (19)C15—C14—C13122.7 (10)
O18—Mo6—O2383.37 (18)C15—C14—H14A118.6
O21—Mo6—O2370.95 (16)C13—C14—H14A118.6
O26—Mo6—O2371.85 (15)C15'—C14'—C13'118.5 (10)
O13—Mo7—O20104.8 (2)C15'—C14'—H14B120.7
O13—Mo7—O24101.8 (2)C13'—C14'—H14B120.7
O20—Mo7—O2496.7 (2)N3'—C15'—C14'124.9 (10)
O13—Mo7—O23101.1 (2)N3'—C15'—H15A117.5
O20—Mo7—O2396.9 (2)C14'—C15'—H15A117.5
O24—Mo7—O23149.31 (18)C14—C15—N3125.6 (11)
O13—Mo7—O2599.0 (2)C14—C15—H15B117.2
O20—Mo7—O25156.21 (19)N3—C15—H15B117.2
O24—Mo7—O2578.18 (17)N4'—C16'—C17'124.6 (11)
O23—Mo7—O2578.30 (17)N4'—C16'—H16A117.7
O13—Mo7—O26174.4 (2)C17'—C16'—H16A117.7
O20—Mo7—O2680.80 (18)N4—C16—C17125.3 (11)
O24—Mo7—O2677.67 (16)N4—C16—H16B117.3
O23—Mo7—O2677.52 (16)C17—C16—H16B117.3
O25—Mo7—O2675.41 (15)C16'—C17'—C18'118.9 (10)
O13—Mo7—Mo390.26 (16)C16'—C17'—H17A120.6
O20—Mo7—Mo3132.53 (16)C18'—C17'—H17A120.6
O24—Mo7—Mo335.81 (13)C18—C17—C16121.9 (11)
O23—Mo7—Mo3124.45 (13)C18—C17—H17B119.1
O25—Mo7—Mo346.17 (11)C16—C17—H17B119.1
O26—Mo7—Mo386.10 (11)C17—C18—C19112.9 (11)
O14—Mo8—O19104.7 (2)C17—C18—C18'124.2 (10)
O14—Mo8—O22102.0 (2)C19—C18—C18'122.8 (9)
O19—Mo8—O2296.6 (2)C19'—C18'—C17'115.6 (10)
O14—Mo8—O21101.3 (2)C19'—C18'—C18122.7 (9)
O19—Mo8—O2196.33 (19)C17'—C18'—C18121.7 (9)
O22—Mo8—O21149.41 (18)C20'—C19'—C18'120.4 (10)
O14—Mo8—O2699.0 (2)C20'—C19'—H19A119.8
O19—Mo8—O26156.34 (19)C18'—C19'—H19A119.8
O22—Mo8—O2678.65 (17)C20—C19—C18123.1 (10)
O21—Mo8—O2678.40 (17)C20—C19—H19B118.4
O14—Mo8—O25174.5 (2)C18—C19—H19B118.4
O19—Mo8—O2580.80 (18)N4'—C20'—C19'122.8 (11)
O22—Mo8—O2577.55 (16)N4'—C20'—H20A118.6
O21—Mo8—O2577.33 (16)C19'—C20'—H20A118.6
O26—Mo8—O2575.54 (15)C19—C20—N4124.2 (11)
O14—Mo8—Mo490.28 (17)C19—C20—H20B117.9
O19—Mo8—Mo4132.80 (15)N4—C20—H20B117.9
O22—Mo8—Mo436.19 (13)N5—C21—C22125.0 (11)
O21—Mo8—Mo4124.70 (13)N5—C21—H21A117.5
O26—Mo8—Mo446.31 (11)C22—C21—H21A117.5
O25—Mo8—Mo486.19 (11)C23—C22—C21119.3 (10)
Mo1—O15—Mo2117.2 (2)C23—C22—H22A120.3
Mo3—O16—Mo2117.2 (2)C21—C22—H22A120.3
Mo4—O17—Mo5116.7 (2)C22—C23—C24116.2 (8)
Mo6—O18—Mo5117.0 (2)C22—C23—C23i120.8 (9)
Mo8—O19—Mo2118.4 (2)C24—C23—C23i123.0 (10)
Mo7—O20—Mo5118.3 (2)C25—C24—C23120.5 (10)
Mo8—O21—Mo6108.8 (2)C25—C24—H24A119.8
Mo8—O21—Mo1110.41 (18)C23—C24—H24A119.8
Mo6—O21—Mo1104.90 (18)N5—C25—C24124.1 (11)
Mo8—O22—Mo4108.7 (2)N5—C25—H25A118.0
Mo8—O22—Mo3110.36 (18)C24—C25—H25A118.0
Mo4—O22—Mo3104.15 (18)N6—C26—C27124.2 (10)
Mo7—O23—Mo1109.2 (2)N6—C26—H26A117.9
Mo7—O23—Mo6110.20 (19)C27—C26—H26A117.9
Mo1—O23—Mo6104.20 (18)C26—C27—C28120.1 (10)
Mo7—O24—Mo3109.3 (2)C26—C27—H27A119.9
Mo7—O24—Mo4110.04 (18)C28—C27—H27A119.9
Mo3—O24—Mo4104.22 (18)C27—C28—C29115.8 (8)
Mo7—O25—Mo192.41 (16)C27—C28—C28ii121.2 (10)
Mo7—O25—Mo391.84 (16)C29—C28—C28ii122.9 (9)
Mo1—O25—Mo3162.8 (2)C30—C29—C28120.1 (7)
Mo7—O25—Mo8104.37 (17)C30—C29—H29A120.0
Mo1—O25—Mo896.91 (15)C28—C29—H29A120.0
Mo3—O25—Mo898.20 (16)N6—C30—C29122.5 (7)
Mo7—O25—Mo2164.8 (2)N6—C30—H30A118.8
Mo1—O25—Mo285.70 (14)C29—C30—H30A118.8
Mo3—O25—Mo285.83 (14)H1WA—O1W—H1WB109.5
Mo8—O25—Mo290.84 (14)H2WA—O2W—H2WB109.5
Symmetry codes: (i) x+2, y+1, z+2; (ii) x+4, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O5iii0.852.092.925166
O1W—H1WA···O13iii0.852.633.031111
O1W—H1WB···O100.852.112.919159
Symmetry code: (iii) x+1, y, z.
 

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