Crystal structure of an organic–inorganic hybrid compound based on morpholinium cations and a β-type Anderson polyanion

Lukianova, T.J.; Kinzhybalo, V.; Pietraszko, A.

doi:10.1107/S2056989015019246

Crystal structure of an organic–inorganic hybrid compound based on morpholinium cations and a β-type Anderson polyanion

T. J. Lukianova, V. Kinzhybalo and A. Pietraszko

The crystal structure of the novel organic–inorganic hybrid compound is based on a β-type Anderson polyoxidomolybdate anion containing a central Fe^III ion. In the crystal, intermolecular N—H

O and O—H

O hydrogen bonds link the components into a three-dimensional network structure.

Keywords: crystal structure; polyoxidomolybdate; Anderson-type anion; organic–inorganic hybrid.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989015019246/wm5221sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989015019246/wm5221Isup2.hkl Contains datablock I

CCDC reference: 1430684

checkCIF report

Key indicators

Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.006 Å
Disorder in solvent or counterion
R factor = 0.042
wR factor = 0.112
Data-to-parameter ratio = 16.4

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT223_ALERT_4_A Large Solvent/Anion H    Ueq(max)/Ueq(min) .....        5.1 Ratio

Author Response: Hydrogen atoms thermal parameters were restricted to 1.5 Ueq(O) for solvent water molecules. While most of water molecules are characterized by intermediate values of thermal vibration parameters, one of them (O1W) possesses considerably elongated thermal ellipsoid in one of the directions. This results in considerably higher values of Ueq for this water molecule H atoms in comparison with the remaining ones.


Alert level C
PLAT041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
PLAT221_ALERT_2_C Large Solv./Anion  C     Ueq(max)/Ueq(min) Range        5.0 Ratio
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.1 Note
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.7 Note
PLAT395_ALERT_2_C Deviating  X-O-Y  Angle from 120 Deg for    *O1W      140.1 Degree
PLAT417_ALERT_2_C Short Inter D-H..H-D       H2H    ..  H2WB    ..       2.11 Ang.
PLAT906_ALERT_3_C Large K value in the Analysis of Variance ......      2.058 Check
PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Th(Min) ...          6 Report
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          5 Report
PLAT971_ALERT_2_C Check Calcd Residual Density  0.78A From     Mo2       1.81 eA-3
PLAT971_ALERT_2_C Check Calcd Residual Density  0.84A From     Mo4       1.64 eA-3
PLAT971_ALERT_2_C Check Calcd Residual Density  0.79A From     Mo5       1.52 eA-3

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         12 Note
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         30 Report
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT045_ALERT_1_G Calculated and Reported Z Differ by ............       0.50 Ratio
PLAT154_ALERT_1_G The su's on the Cell Angles are Equal ..........    0.03000 Degree
PLAT175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records          1 Report
PLAT300_ALERT_4_G Atom Site Occupancy of *O1W    is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H1WA   is Constrained at      0.500 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H1WB   is Constrained at      0.500 Check
PLAT302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =         48 Note
PLAT304_ALERT_4_G Non-Integer Number of Atoms (  13.71) in Resd. #          4 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms (  11.25) in Resd. #          5 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms (  13.71) in Resd. #          6 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms (   2.29) in Resd. #          7 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms (   4.75) in Resd. #          8 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms (   2.29) in Resd. #          9 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms (   1.50) in Resd. #         11 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  O4     ..  C5B     ..       2.96 Ang.
PLAT432_ALERT_2_G Short Inter X...Y Contact  O4S    ..  C3D     ..       2.96 Ang.
PLAT432_ALERT_2_G Short Inter X...Y Contact  O13    ..  C3C     ..       2.98 Ang.
PLAT432_ALERT_2_G Short Inter X...Y Contact  O14    ..  C6B     ..       3.00 Ang.
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........         58 Note
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          3 Note
              C4 H10 N O
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          4 Note
              C4 H10 N O
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          5 Note
              C4 H10 N O
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          8 Note
              C4 H10 N O
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          9 Note
              C4 H10 N O
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #         10 Note
              O4 S
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #         14 Note
              H2 O
PLAT811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms ....          ! Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         12 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600       1780 Note

   1 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
  13 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  32 ALERT level G = General information/check it is not something unexpected

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  14 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
  22 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

Computing details top

Data collection: CrysAlis PRO (Rigaku Oxford Diffraction, 2015); cell refinement: CrysAlis PRO (Rigaku Oxford Diffraction, 2015); data reduction: CrysAlis PRO (Rigaku Oxford Diffraction, 2015); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 1997); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Pentamorpholinium hexahydrogen hexamolybdoferrate(III) sulfate 3.5-hydrate top

Crystal data top

(C₄H₁₀NO)₅[Fe(OH)₆Mo₆O₁₈](SO₄)·3.5H₂O	Z = 2
M_r = 1621.30	F(000) = 1608
Triclinic, P1	D_x = 2.243 Mg m⁻³
a = 8.900 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 13.143 (4) Å	Cell parameters from 15587 reflections
c = 20.778 (6) Å	θ = 2.4–29.3°
α = 84.92 (3)°	µ = 1.97 mm⁻¹
β = 85.37 (3)°	T = 100 K
γ = 83.70 (3)°	Block, light brown
V = 2400.1 (13) Å³	0.27 × 0.20 × 0.12 mm

Data collection top

Rigaku Oxford Diffraction Xcalibur Atlas diffractometer	11708 independent reflections
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source	9288 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.038
Detector resolution: 10.6249 pixels mm^-1	θ_max = 29.6°, θ_min = 2.4°
ω scans	h = −12→11
Absorption correction: analytical (CrysAlisPro; Rigaku Oxford Diffraction, 2015)	k = −18→17
T_min = 0.708, T_max = 0.819	l = −28→28
37127 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.042	H-atom parameters constrained
wR(F²) = 0.112	w = 1/[σ²(F_o²) + (0.0601P)² + 2.7906P] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.001
11708 reflections	Δρ_max = 1.98 e Å⁻³
714 parameters	Δρ_min = −1.29 e Å⁻³
12 restraints

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mo1	0.07030 (4)	0.98765 (2)	0.70745 (2)	0.01685 (8)
Mo2	0.08559 (5)	0.86149 (3)	0.85537 (2)	0.02715 (10)
Mo3	0.16217 (4)	0.60317 (3)	0.86796 (2)	0.02082 (9)
Mo4	0.22287 (4)	0.47443 (2)	0.73545 (2)	0.01670 (8)
Mo5	0.23106 (4)	0.60189 (2)	0.58822 (2)	0.01558 (8)
Mo6	0.15245 (3)	0.85979 (2)	0.57545 (2)	0.01468 (8)
O1	0.1659 (3)	0.9593 (2)	0.78943 (12)	0.0246 (6)
O2	0.0207 (3)	0.7260 (2)	0.87992 (13)	0.0268 (7)
O3	0.2976 (3)	0.5184 (2)	0.81276 (12)	0.0185 (5)
O4	0.1380 (3)	0.5093 (2)	0.65144 (12)	0.0192 (6)
O5	0.2965 (3)	0.7388 (2)	0.56585 (12)	0.0180 (5)
O6	0.0066 (3)	0.9393 (2)	0.62919 (12)	0.0169 (5)
O7	0.1890 (3)	1.0768 (2)	0.67652 (13)	0.0245 (6)
O8	−0.0969 (3)	1.0558 (2)	0.73014 (13)	0.0274 (7)
O9	0.2118 (5)	0.8721 (3)	0.91123 (14)	0.0443 (9)
O1W	0.2590 (12)	0.9809 (15)	1.0154 (8)	0.184 (9)	0.5
H1WA	0.2462	0.9492	0.9832	0.276*	0.5
H1WB	0.2094	1.0047	1.0482	0.276*	0.5
O10	−0.0799 (4)	0.9283 (3)	0.88176 (15)	0.0438 (9)
O11	0.2876 (4)	0.6120 (2)	0.92487 (14)	0.0346 (8)
O12	0.0389 (4)	0.5191 (2)	0.90187 (14)	0.0314 (7)
O13	0.0944 (3)	0.3921 (2)	0.76519 (14)	0.0299 (7)
O14	0.3796 (3)	0.3960 (2)	0.71415 (14)	0.0274 (6)
O15	0.1131 (3)	0.5942 (2)	0.52742 (13)	0.0230 (6)
O16	0.3973 (3)	0.5344 (2)	0.56528 (13)	0.0226 (6)
O17	0.2801 (3)	0.9456 (2)	0.54611 (12)	0.0206 (6)
O18	0.0397 (3)	0.8525 (2)	0.51406 (12)	0.0215 (6)
Fe1	0.16272 (5)	0.73185 (4)	0.72223 (2)	0.01210 (11)
O1H	0.2536 (3)	0.7399 (2)	0.80532 (12)	0.0185 (6)
H1H	0.3645	0.7472	0.8042	0.022*
O2H	0.2464 (3)	0.85564 (19)	0.67550 (11)	0.0147 (5)
H2H	0.3564	0.8633	0.6777	0.018*
O3H	0.3128 (3)	0.62367 (19)	0.68738 (12)	0.0147 (5)
H3H	0.4227	0.6314	0.6898	0.018*
O4H	0.0625 (3)	0.7268 (2)	0.63805 (11)	0.0151 (5)
H4H	−0.0486	0.7198	0.6402	0.018*
O5H	0.0654 (3)	0.6135 (2)	0.76894 (12)	0.0161 (5)
H5H	−0.0464	0.6125	0.7673	0.019*
O6H	0.0001 (3)	0.8368 (2)	0.75643 (12)	0.0166 (5)
H6H	−0.1079	0.8232	0.7553	0.020*
S1	−0.33015 (11)	0.68657 (8)	0.74350 (5)	0.0269 (2)
O1S	−0.2351 (3)	0.6113 (2)	0.78520 (15)	0.0332 (7)
O2S	−0.2325 (3)	0.7606 (2)	0.70866 (15)	0.0349 (8)
O3S	−0.3991 (3)	0.6318 (2)	0.69703 (15)	0.0312 (7)
O4S	−0.4464 (3)	0.7430 (3)	0.78508 (17)	0.0405 (8)
O1A	0.7444 (3)	0.6640 (2)	0.44577 (13)	0.0257 (6)
C2A	0.7298 (5)	0.6408 (4)	0.5141 (2)	0.0291 (10)
H2AA	0.8212	0.5969	0.5278	0.035*
H2AB	0.6410	0.6018	0.5255	0.035*
C3A	0.7109 (5)	0.7361 (4)	0.5492 (2)	0.0342 (11)
H3AA	0.8029	0.7726	0.5407	0.041*
H3AB	0.6962	0.7182	0.5964	0.041*
N4A	0.5764 (4)	0.8037 (3)	0.52633 (17)	0.0291 (8)
H4AA	0.5711	0.8649	0.5442	0.035*
H4AB	0.4907	0.7738	0.5401	0.035*
C5A	0.5837 (5)	0.8224 (3)	0.4542 (2)	0.0289 (9)
H5AA	0.6676	0.8642	0.4391	0.035*
H5AB	0.4877	0.8601	0.4404	0.035*
C6A	0.6097 (5)	0.7196 (4)	0.4258 (2)	0.0295 (10)
H6AA	0.5231	0.6796	0.4397	0.035*
H6AB	0.6156	0.7302	0.3779	0.035*
O1B	−0.3116 (3)	0.2911 (2)	0.65919 (15)	0.0287 (7)
C2B	−0.2048 (4)	0.2376 (3)	0.6169 (2)	0.0257 (9)
H2BA	−0.2334	0.2535	0.5718	0.031*
H2BB	−0.2059	0.1627	0.6276	0.031*
C3B	−0.0465 (4)	0.2670 (3)	0.6222 (2)	0.0222 (8)
H3BA	−0.0151	0.2484	0.6667	0.027*
H3BB	0.0263	0.2296	0.5918	0.027*
N4B	−0.0472 (4)	0.3801 (2)	0.60629 (15)	0.0206 (7)
H4BA	0.0454	0.3994	0.6124	0.025*
H4BB	−0.0653	0.3957	0.5639	0.025*
C5B	−0.1655 (4)	0.4378 (3)	0.6478 (2)	0.0246 (9)
H5BA	−0.1708	0.5121	0.6340	0.030*
H5BB	−0.1395	0.4280	0.6935	0.030*
C6B	−0.3155 (5)	0.3992 (3)	0.6417 (2)	0.0311 (10)
H6BA	−0.3938	0.4361	0.6701	0.037*
H6BB	−0.3439	0.4138	0.5965	0.037*
O1C	0.0475 (5)	0.1916 (5)	0.8976 (2)	0.0507 (14)	0.857 (6)
C2C	−0.0299 (8)	0.1850 (5)	0.8422 (3)	0.0418 (16)	0.857 (6)
H2CA	−0.0784	0.1203	0.8465	0.050*	0.857 (6)
H2CB	0.0437	0.1832	0.8038	0.050*	0.857 (6)
C3C	−0.1492 (6)	0.2742 (7)	0.8318 (3)	0.0405 (16)	0.857 (6)
H3CA	−0.1004	0.3386	0.8222	0.049*	0.857 (6)
H3CB	−0.2065	0.2643	0.7943	0.049*	0.857 (6)
N4C	−0.2543 (6)	0.2821 (5)	0.8907 (3)	0.030 (3)	0.857 (6)
H4CA	−0.3116	0.2284	0.8951	0.036*	0.857 (6)
H4CB	−0.3178	0.3411	0.8864	0.036*	0.857 (6)
C5C	−0.1696 (7)	0.2820 (6)	0.9505 (3)	0.0441 (17)	0.857 (6)
H5CA	−0.1188	0.3455	0.9493	0.053*	0.857 (6)
H5CB	−0.2406	0.2788	0.9896	0.053*	0.857 (6)
C6C	−0.0539 (8)	0.1896 (7)	0.9524 (3)	0.058 (2)	0.857 (6)
H6CA	0.0028	0.1877	0.9917	0.070*	0.857 (6)
H6CB	−0.1061	0.1264	0.9551	0.070*	0.857 (6)
O11C	−0.043 (3)	0.271 (2)	0.9549 (11)	0.057 (8)*	0.143 (6)
C21C	0.063 (3)	0.234 (3)	0.9067 (18)	0.061 (19)*	0.143 (6)
H21A	0.1521	0.1960	0.9271	0.074*	0.143 (6)
H21B	0.0988	0.2921	0.8782	0.074*	0.143 (6)
C31C	−0.007 (5)	0.163 (3)	0.867 (2)	0.10 (3)*	0.143 (6)
H31A	0.0682	0.1359	0.8336	0.122*	0.143 (6)
H31B	−0.0428	0.1046	0.8953	0.122*	0.143 (6)
N41C	−0.137 (4)	0.223 (3)	0.8359 (14)	0.053 (12)*	0.143 (6)
H41A	−0.1878	0.1801	0.8158	0.064*	0.143 (6)
H41B	−0.1014	0.2701	0.8053	0.064*	0.143 (6)
C51C	−0.245 (3)	0.278 (4)	0.884 (2)	0.07 (4)*	0.143 (6)
H51A	−0.3003	0.2272	0.9119	0.087*	0.143 (6)
H51B	−0.3194	0.3259	0.8609	0.087*	0.143 (6)
C61C	−0.158 (3)	0.3357 (19)	0.9249 (12)	0.020 (6)*	0.143 (6)
H61A	−0.1118	0.3913	0.8975	0.024*	0.143 (6)
H61B	−0.2282	0.3678	0.9585	0.024*	0.143 (6)
O1E	0.5358 (5)	1.1453 (3)	0.8694 (2)	0.0366 (10)	0.857 (6)
C2E	0.4163 (7)	1.1963 (5)	0.8317 (3)	0.0443 (16)	0.857 (6)
H2EA	0.4200	1.2716	0.8297	0.053*	0.857 (6)
H2EB	0.3168	1.1807	0.8528	0.053*	0.857 (6)
C3E	0.4328 (8)	1.1618 (4)	0.7643 (3)	0.0389 (15)	0.857 (6)
H3EA	0.5270	1.1840	0.7414	0.047*	0.857 (6)
H3EB	0.3461	1.1935	0.7399	0.047*	0.857 (6)
N4E	0.4379 (5)	1.0468 (4)	0.7675 (2)	0.0304 (11)	0.857 (6)
H4EA	0.3454	1.0277	0.7825	0.037*	0.857 (6)
H4EB	0.4586	1.0256	0.7268	0.037*	0.857 (6)
C5E	0.5540 (8)	0.9958 (5)	0.8100 (3)	0.0457 (17)	0.857 (6)
H5EA	0.6565	1.0085	0.7909	0.055*	0.857 (6)
H5EB	0.5476	0.9208	0.8146	0.055*	0.857 (6)
C6E	0.5269 (9)	1.0381 (5)	0.8748 (3)	0.0510 (19)	0.857 (6)
H6EA	0.4254	1.0235	0.8941	0.061*	0.857 (6)
H6EB	0.6033	1.0040	0.9039	0.061*	0.857 (6)
O11E	0.610 (3)	1.148 (2)	0.8423 (15)	0.048 (7)*	0.143 (6)
C21E	0.528 (4)	1.200 (3)	0.7879 (18)	0.044 (9)*	0.143 (6)
H21C	0.5806	1.1787	0.7466	0.053*	0.143 (6)
H21D	0.5273	1.2749	0.7883	0.053*	0.143 (6)
C31E	0.363 (4)	1.170 (3)	0.7931 (18)	0.029 (7)*	0.143 (6)
H31C	0.3099	1.1906	0.8344	0.035*	0.143 (6)
H31D	0.3071	1.2063	0.7570	0.035*	0.143 (6)
N41E	0.371 (3)	1.058 (2)	0.7901 (13)	0.026 (6)*	0.143 (6)
H41C	0.4108	1.0406	0.7504	0.032*	0.143 (6)
H41D	0.2757	1.0376	0.7961	0.032*	0.143 (6)
C51E	0.470 (3)	1.002 (2)	0.8430 (13)	0.016 (6)*	0.143 (6)
H51C	0.4192	1.0122	0.8864	0.019*	0.143 (6)
H51D	0.4835	0.9270	0.8376	0.019*	0.143 (6)
C61E	0.617 (4)	1.041 (3)	0.8376 (18)	0.038 (8)*	0.143 (6)
H61C	0.6784	1.0058	0.8721	0.046*	0.143 (6)
H61D	0.6700	1.0251	0.7954	0.046*	0.143 (6)
O1D	−0.4396 (8)	0.7161 (5)	1.0345 (3)	0.0377 (15)	0.703 (9)
C2D	−0.3989 (9)	0.7971 (5)	0.9881 (3)	0.039 (2)	0.703 (9)
H2DA	−0.3004	0.8185	0.9977	0.047*	0.703 (9)
H2DB	−0.4761	0.8570	0.9914	0.047*	0.703 (9)
C3D	−0.3873 (8)	0.7643 (6)	0.9214 (3)	0.0361 (19)	0.703 (9)
H3DA	−0.3537	0.8205	0.8906	0.043*	0.703 (9)
H3DB	−0.4882	0.7495	0.9101	0.043*	0.703 (9)
N4D	−0.2762 (9)	0.6697 (6)	0.9156 (3)	0.0303 (15)	0.703 (9)
H4DA	−0.2822	0.6448	0.8765	0.036*	0.703 (9)
H4DB	−0.1805	0.6869	0.9175	0.036*	0.703 (9)
C5D	−0.3069 (11)	0.5889 (6)	0.9678 (4)	0.041 (2)	0.703 (9)
H5DA	−0.2219	0.5336	0.9674	0.049*	0.703 (9)
H5DB	−0.4002	0.5587	0.9600	0.049*	0.703 (9)
C6D	−0.3255 (10)	0.6321 (6)	1.0326 (3)	0.046 (2)	0.703 (9)
H6DA	−0.3522	0.5776	1.0663	0.056*	0.703 (9)
H6DB	−0.2281	0.6549	1.0425	0.056*	0.703 (9)
O11D	−0.4846 (16)	0.7037 (12)	1.0209 (7)	0.027 (4)*	0.297 (9)
C21D	−0.4828 (19)	0.7728 (13)	0.9674 (8)	0.032 (4)*	0.297 (9)
H21E	−0.5345	0.8400	0.9789	0.038*	0.297 (9)
H21F	−0.5382	0.7483	0.9333	0.038*	0.297 (9)
C31D	−0.3180 (18)	0.7855 (11)	0.9415 (7)	0.025 (3)*	0.297 (9)
H31E	−0.3177	0.8357	0.9030	0.030*	0.297 (9)
H31F	−0.2638	0.8122	0.9751	0.030*	0.297 (9)
N41D	−0.241 (2)	0.6885 (15)	0.9241 (9)	0.027 (5)*	0.297 (9)
H41E	−0.1424	0.6955	0.9115	0.032*	0.297 (9)
H41F	−0.2853	0.6664	0.8906	0.032*	0.297 (9)
C51D	−0.252 (2)	0.6104 (15)	0.9834 (9)	0.033 (4)*	0.297 (9)
H51E	−0.2039	0.5422	0.9720	0.040*	0.297 (9)
H51F	−0.1978	0.6322	1.0188	0.040*	0.297 (9)
C61D	−0.4176 (16)	0.6035 (11)	1.0057 (7)	0.025 (4)*	0.297 (9)
H61E	−0.4711	0.5790	0.9710	0.030*	0.297 (9)
H61F	−0.4259	0.5543	1.0444	0.030*	0.297 (9)
O2W	0.5313 (3)	0.9178 (3)	0.67269 (17)	0.0394 (8)
H2WA	0.5813	0.9500	0.6425	0.059*
H2WB	0.5885	0.8684	0.6897	0.059*
O3W	0.5901 (4)	0.4619 (3)	0.8460 (2)	0.0525 (11)
H3WA	0.6398	0.4979	0.8176	0.079*
H3WB	0.4967	0.4702	0.8386	0.079*
O4W	−0.2744 (3)	0.9785 (3)	0.57958 (14)	0.0327 (7)
H4WA	−0.2595	1.0042	0.5408	0.049*
H4WB	−0.1942	0.9791	0.5993	0.049*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.02266 (17)	0.01483 (17)	0.01282 (15)	0.00194 (12)	−0.00431 (12)	−0.00177 (12)
Mo2	0.0502 (2)	0.01917 (19)	0.01084 (16)	0.00373 (16)	−0.00339 (15)	−0.00225 (14)
Mo3	0.03058 (19)	0.01924 (18)	0.01175 (15)	0.00277 (14)	−0.00552 (13)	0.00067 (13)
Mo4	0.02022 (17)	0.01442 (17)	0.01648 (16)	−0.00286 (12)	−0.00614 (12)	−0.00127 (13)
Mo5	0.01895 (16)	0.01605 (17)	0.01302 (15)	−0.00288 (12)	−0.00493 (12)	−0.00354 (12)
Mo6	0.01686 (16)	0.01677 (17)	0.01099 (14)	−0.00214 (12)	−0.00403 (11)	−0.00110 (12)
O1	0.0416 (17)	0.0191 (15)	0.0147 (13)	−0.0020 (12)	−0.0111 (11)	−0.0027 (11)
O2	0.0430 (18)	0.0202 (15)	0.0137 (13)	0.0069 (13)	0.0033 (12)	0.0001 (11)
O3	0.0209 (13)	0.0187 (14)	0.0166 (12)	0.0005 (10)	−0.0082 (10)	−0.0019 (11)
O4	0.0245 (14)	0.0193 (14)	0.0157 (12)	−0.0051 (11)	−0.0072 (10)	−0.0030 (11)
O5	0.0194 (13)	0.0176 (14)	0.0170 (12)	−0.0020 (10)	0.0006 (10)	−0.0037 (11)
O6	0.0175 (13)	0.0188 (14)	0.0140 (12)	0.0016 (10)	−0.0040 (10)	−0.0014 (10)
O7	0.0348 (16)	0.0180 (15)	0.0213 (14)	−0.0024 (12)	−0.0085 (12)	−0.0005 (12)
O8	0.0317 (16)	0.0245 (16)	0.0231 (14)	0.0089 (12)	0.0011 (12)	−0.0028 (12)
O9	0.088 (3)	0.0299 (19)	0.0172 (15)	−0.0044 (18)	−0.0195 (16)	−0.0034 (13)
O1W	0.047 (6)	0.34 (2)	0.204 (15)	−0.034 (10)	0.009 (8)	−0.222 (16)
O10	0.073 (3)	0.0252 (18)	0.0257 (16)	0.0091 (16)	0.0178 (16)	0.0002 (14)
O11	0.056 (2)	0.0290 (17)	0.0201 (14)	0.0045 (15)	−0.0213 (14)	−0.0012 (13)
O12	0.0392 (18)	0.0264 (17)	0.0249 (15)	0.0032 (13)	0.0026 (13)	0.0052 (13)
O13	0.0352 (17)	0.0300 (17)	0.0277 (15)	−0.0146 (13)	−0.0124 (13)	0.0038 (13)
O14	0.0336 (16)	0.0221 (16)	0.0258 (15)	0.0034 (12)	−0.0055 (12)	−0.0035 (12)
O15	0.0272 (15)	0.0242 (15)	0.0198 (13)	−0.0051 (12)	−0.0099 (11)	−0.0040 (12)
O16	0.0241 (14)	0.0223 (15)	0.0219 (14)	−0.0012 (11)	−0.0027 (11)	−0.0060 (12)
O17	0.0211 (14)	0.0205 (15)	0.0195 (13)	−0.0003 (11)	−0.0007 (10)	−0.0001 (11)
O18	0.0253 (15)	0.0234 (15)	0.0163 (13)	−0.0007 (11)	−0.0062 (11)	−0.0028 (11)
Fe1	0.0122 (2)	0.0141 (3)	0.0106 (2)	−0.00148 (19)	−0.00381 (18)	−0.0014 (2)
O1H	0.0199 (13)	0.0204 (14)	0.0167 (12)	−0.0009 (11)	−0.0091 (10)	−0.0042 (11)
O2H	0.0148 (12)	0.0162 (13)	0.0139 (12)	−0.0024 (10)	−0.0046 (9)	−0.0015 (10)
O3H	0.0130 (12)	0.0162 (13)	0.0154 (12)	0.0002 (9)	−0.0038 (9)	−0.0041 (10)
O4H	0.0139 (12)	0.0194 (14)	0.0129 (12)	−0.0034 (10)	−0.0058 (9)	−0.0005 (10)
O5H	0.0134 (12)	0.0171 (14)	0.0183 (12)	−0.0038 (10)	−0.0063 (10)	0.0027 (11)
O6H	0.0148 (12)	0.0197 (14)	0.0145 (12)	0.0024 (10)	−0.0025 (9)	−0.0003 (11)
S1	0.0144 (5)	0.0299 (6)	0.0369 (6)	−0.0038 (4)	−0.0080 (4)	0.0019 (5)
O1S	0.0202 (15)	0.0391 (19)	0.0395 (18)	−0.0083 (13)	−0.0063 (13)	0.0112 (15)
O2S	0.0244 (15)	0.0367 (19)	0.0445 (19)	−0.0103 (13)	−0.0176 (13)	0.0150 (15)
O3S	0.0184 (14)	0.0361 (18)	0.0401 (18)	−0.0065 (12)	−0.0052 (12)	−0.0003 (14)
O4S	0.0203 (16)	0.046 (2)	0.060 (2)	−0.0082 (14)	−0.0074 (15)	−0.0161 (17)
O1A	0.0239 (15)	0.0290 (16)	0.0239 (14)	0.0007 (12)	−0.0022 (11)	−0.0054 (12)
C2A	0.026 (2)	0.035 (3)	0.026 (2)	−0.0006 (18)	−0.0054 (17)	0.0016 (19)
C3A	0.029 (2)	0.052 (3)	0.025 (2)	−0.011 (2)	−0.0061 (17)	−0.007 (2)
N4A	0.0265 (19)	0.031 (2)	0.0321 (19)	−0.0077 (15)	0.0075 (15)	−0.0162 (16)
C5A	0.026 (2)	0.025 (2)	0.034 (2)	0.0018 (17)	0.0024 (17)	0.0009 (19)
C6A	0.030 (2)	0.038 (3)	0.022 (2)	0.0001 (19)	−0.0096 (17)	−0.0072 (19)
O1B	0.0245 (15)	0.0247 (16)	0.0373 (17)	−0.0046 (12)	0.0005 (12)	−0.0047 (13)
C2B	0.023 (2)	0.023 (2)	0.031 (2)	−0.0014 (16)	−0.0095 (17)	−0.0026 (18)
C3B	0.023 (2)	0.019 (2)	0.025 (2)	−0.0010 (15)	−0.0053 (15)	−0.0004 (16)
N4B	0.0208 (16)	0.0244 (18)	0.0179 (15)	−0.0031 (13)	−0.0077 (12)	−0.0024 (14)
C5B	0.026 (2)	0.022 (2)	0.026 (2)	−0.0014 (16)	−0.0028 (16)	−0.0049 (17)
C6B	0.025 (2)	0.022 (2)	0.047 (3)	−0.0005 (17)	−0.0061 (19)	−0.007 (2)
O1C	0.036 (2)	0.072 (4)	0.040 (3)	0.013 (2)	−0.008 (2)	−0.002 (3)
C2C	0.054 (4)	0.035 (3)	0.031 (3)	0.011 (3)	0.011 (3)	−0.005 (3)
C3C	0.032 (3)	0.056 (5)	0.026 (3)	0.004 (3)	0.006 (2)	0.015 (3)
N4C	0.025 (3)	0.036 (4)	0.029 (3)	−0.0039 (18)	0.0011 (18)	−0.005 (2)
C5C	0.037 (3)	0.064 (5)	0.036 (3)	−0.009 (3)	0.001 (2)	−0.034 (3)
C6C	0.055 (4)	0.089 (6)	0.029 (3)	0.010 (4)	−0.016 (3)	−0.007 (3)
O1E	0.048 (3)	0.030 (2)	0.034 (2)	−0.0058 (18)	−0.019 (2)	−0.0044 (17)
C2E	0.049 (4)	0.033 (3)	0.054 (4)	−0.001 (3)	−0.021 (3)	−0.009 (3)
C3E	0.050 (4)	0.035 (3)	0.036 (3)	−0.021 (3)	−0.025 (3)	0.011 (3)
N4E	0.025 (2)	0.039 (3)	0.030 (2)	−0.009 (2)	−0.007 (2)	−0.006 (2)
C5E	0.050 (4)	0.033 (3)	0.058 (4)	0.002 (3)	−0.031 (3)	−0.008 (3)
C6E	0.085 (5)	0.034 (4)	0.038 (3)	−0.018 (3)	−0.030 (3)	0.010 (3)
O1D	0.041 (4)	0.044 (3)	0.022 (3)	0.012 (3)	0.002 (3)	0.006 (2)
C2D	0.048 (5)	0.030 (4)	0.036 (4)	0.007 (3)	0.001 (3)	−0.002 (3)
C3D	0.034 (4)	0.043 (4)	0.026 (3)	0.009 (3)	−0.002 (3)	0.010 (3)
N4D	0.035 (4)	0.037 (4)	0.019 (3)	−0.008 (3)	0.001 (3)	−0.005 (3)
C5D	0.063 (6)	0.024 (4)	0.033 (4)	0.003 (4)	0.002 (4)	0.001 (3)
C6D	0.059 (5)	0.044 (5)	0.029 (4)	0.017 (4)	−0.001 (3)	0.008 (3)
O2W	0.0255 (16)	0.044 (2)	0.049 (2)	−0.0111 (14)	−0.0154 (14)	0.0164 (17)
O3W	0.0206 (16)	0.064 (3)	0.068 (3)	−0.0085 (17)	−0.0126 (16)	0.032 (2)
O4W	0.0242 (15)	0.048 (2)	0.0244 (15)	−0.0006 (14)	−0.0078 (12)	0.0055 (15)

Geometric parameters (Å, º) top

Mo1—O1	1.954 (3)	N4C—H4CA	0.9100
Mo1—O6	1.944 (3)	N4C—H4CB	0.9100
Mo1—O7	1.712 (3)	N4C—C5C	1.503 (8)
Mo1—O8	1.705 (3)	C5C—H5CA	0.9900
Mo1—O2H	2.312 (3)	C5C—H5CB	0.9900
Mo1—O6H	2.273 (3)	C5C—C6C	1.503 (10)
Mo2—O1	1.942 (3)	C6C—H6CA	0.9900
Mo2—O2	1.944 (3)	C6C—H6CB	0.9900
Mo2—O9	1.703 (3)	O11C—C21C	1.404 (14)
Mo2—O10	1.706 (3)	O11C—C61C	1.403 (12)
Mo2—O1H	2.322 (3)	C21C—H21A	0.9900
Mo2—O6H	2.309 (3)	C21C—H21B	0.9900
Mo3—O2	1.957 (3)	C21C—C31C	1.511 (13)
Mo3—O3	1.928 (3)	C31C—H31A	0.9900
Mo3—O11	1.710 (3)	C31C—H31B	0.9900
Mo3—O12	1.710 (3)	C31C—N41C	1.484 (13)
Mo3—O1H	2.307 (3)	N41C—H41A	0.9100
Mo3—O5H	2.281 (3)	N41C—H41B	0.9100
Mo4—O3	1.944 (3)	N41C—C51C	1.500 (13)
Mo4—O4	1.955 (3)	C51C—H51A	0.9900
Mo4—O13	1.703 (3)	C51C—H51B	0.9900
Mo4—O14	1.694 (3)	C51C—C61C	1.501 (14)
Mo4—O3H	2.314 (3)	C61C—H61A	0.9900
Mo4—O5H	2.302 (3)	C61C—H61B	0.9900
Mo5—O4	1.912 (3)	O1E—C2E	1.442 (7)
Mo5—O5	1.957 (3)	O1E—C6E	1.413 (7)
Mo5—O15	1.723 (3)	C2E—H2EA	0.9900
Mo5—O16	1.696 (3)	C2E—H2EB	0.9900
Mo5—O3H	2.291 (3)	C2E—C3E	1.500 (9)
Mo5—O4H	2.351 (3)	C3E—H3EA	0.9900
Mo6—O5	1.944 (3)	C3E—H3EB	0.9900
Mo6—O6	1.923 (3)	C3E—N4E	1.504 (7)
Mo6—O17	1.727 (3)	N4E—H4EA	0.9100
Mo6—O18	1.701 (3)	N4E—H4EB	0.9100
Mo6—O2H	2.297 (2)	N4E—C5E	1.480 (7)
Mo6—O4H	2.264 (3)	C5E—H5EA	0.9900
O1W—H1WA	0.8397	C5E—H5EB	0.9900
O1W—H1WB	0.8468	C5E—C6E	1.493 (10)
Fe1—O1H	1.981 (3)	C6E—H6EA	0.9900
Fe1—O2H	2.003 (3)	C6E—H6EB	0.9900
Fe1—O3H	1.985 (3)	O11E—C21E	1.47 (4)
Fe1—O4H	2.036 (3)	O11E—C61E	1.41 (5)
Fe1—O5H	2.001 (3)	C21E—H21C	0.9900
Fe1—O6H	2.018 (3)	C21E—H21D	0.9900
O1H—H1H	1.0000	C21E—C31E	1.55 (5)
O2H—H2H	1.0000	C31E—H31C	0.9900
O3H—H3H	1.0000	C31E—H31D	0.9900
O4H—H4H	1.0000	C31E—N41E	1.48 (4)
O5H—H5H	1.0000	N41E—H41C	0.9100
O6H—H6H	1.0000	N41E—H41D	0.9100
S1—O1S	1.493 (3)	N41E—C51E	1.55 (4)
S1—O2S	1.478 (3)	C51E—H51C	0.9900
S1—O3S	1.464 (3)	C51E—H51D	0.9900
S1—O4S	1.473 (4)	C51E—C61E	1.45 (4)
O1A—C2A	1.423 (5)	C61E—H61C	0.9900
O1A—C6A	1.406 (5)	C61E—H61D	0.9900
C2A—H2AA	0.9900	O1D—C2D	1.430 (9)
C2A—H2AB	0.9900	O1D—C6D	1.417 (9)
C2A—C3A	1.492 (7)	C2D—H2DA	0.9900
C3A—H3AA	0.9900	C2D—H2DB	0.9900
C3A—H3AB	0.9900	C2D—C3D	1.479 (10)
C3A—N4A	1.494 (6)	C3D—H3DA	0.9900
N4A—H4AA	0.9100	C3D—H3DB	0.9900
N4A—H4AB	0.9100	C3D—N4D	1.508 (10)
N4A—C5A	1.494 (5)	N4D—H4DA	0.9100
C5A—H5AA	0.9900	N4D—H4DB	0.9100
C5A—H5AB	0.9900	N4D—C5D	1.480 (10)
C5A—C6A	1.510 (6)	C5D—H5DA	0.9900
C6A—H6AA	0.9900	C5D—H5DB	0.9900
C6A—H6AB	0.9900	C5D—C6D	1.496 (11)
O1B—C2B	1.413 (5)	C6D—H6DA	0.9900
O1B—C6B	1.432 (5)	C6D—H6DB	0.9900
C2B—H2BA	0.9900	O11D—C21D	1.37 (2)
C2B—H2BB	0.9900	O11D—C61D	1.44 (2)
C2B—C3B	1.516 (5)	C21D—H21E	0.9900
C3B—H3BA	0.9900	C21D—H21F	0.9900
C3B—H3BB	0.9900	C21D—C31D	1.54 (2)
C3B—N4B	1.494 (5)	C31D—H31E	0.9900
N4B—H4BA	0.9100	C31D—H31F	0.9900
N4B—H4BB	0.9100	C31D—N41D	1.44 (2)
N4B—C5B	1.491 (5)	N41D—H41E	0.9100
C5B—H5BA	0.9900	N41D—H41F	0.9100
C5B—H5BB	0.9900	N41D—C51D	1.54 (3)
C5B—C6B	1.497 (6)	C51D—H51E	0.9900
C6B—H6BA	0.9900	C51D—H51F	0.9900
C6B—H6BB	0.9900	C51D—C61D	1.52 (2)
O1C—C2C	1.403 (9)	C61D—H61E	0.9900
O1C—C6C	1.395 (8)	C61D—H61F	0.9900
C2C—H2CA	0.9900	O2W—H2WA	0.8486
C2C—H2CB	0.9900	O2W—H2WB	0.8488
C2C—C3C	1.505 (9)	O3W—H3WA	0.8504
C3C—H3CA	0.9900	O3W—H3WB	0.8517
C3C—H3CB	0.9900	O4W—H4WA	0.8512
C3C—N4C	1.484 (8)	O4W—H4WB	0.8530

O1—Mo1—O2H	82.96 (11)	C5B—N4B—H4BB	109.5
O1—Mo1—O6H	71.17 (11)	N4B—C5B—H5BA	109.9
O6—Mo1—O1	149.82 (11)	N4B—C5B—H5BB	109.9
O6—Mo1—O2H	71.81 (10)	N4B—C5B—C6B	109.1 (3)
O6—Mo1—O6H	84.95 (10)	H5BA—C5B—H5BB	108.3
O7—Mo1—O1	94.58 (13)	C6B—C5B—H5BA	109.9
O7—Mo1—O6	101.90 (12)	C6B—C5B—H5BB	109.9
O7—Mo1—O2H	90.82 (12)	O1B—C6B—C5B	111.8 (3)
O7—Mo1—O6H	158.02 (11)	O1B—C6B—H6BA	109.3
O8—Mo1—O1	102.23 (13)	O1B—C6B—H6BB	109.3
O8—Mo1—O6	97.36 (13)	C5B—C6B—H6BA	109.3
O8—Mo1—O7	105.90 (14)	C5B—C6B—H6BB	109.3
O8—Mo1—O2H	161.86 (13)	H6BA—C6B—H6BB	107.9
O8—Mo1—O6H	93.71 (12)	C6C—O1C—C2C	109.8 (5)
O6H—Mo1—O2H	71.30 (9)	O1C—C2C—H2CA	109.2
O1—Mo2—O2	149.50 (12)	O1C—C2C—H2CB	109.2
O1—Mo2—O1H	85.23 (11)	O1C—C2C—C3C	112.0 (5)
O1—Mo2—O6H	70.54 (11)	H2CA—C2C—H2CB	107.9
O2—Mo2—O1H	71.10 (11)	C3C—C2C—H2CA	109.2
O2—Mo2—O6H	83.48 (11)	C3C—C2C—H2CB	109.2
O9—Mo2—O1	96.60 (15)	C2C—C3C—H3CA	109.7
O9—Mo2—O2	102.52 (15)	C2C—C3C—H3CB	109.7
O9—Mo2—O10	105.99 (18)	H3CA—C3C—H3CB	108.2
O9—Mo2—O1H	90.80 (14)	N4C—C3C—C2C	109.7 (5)
O9—Mo2—O6H	158.22 (14)	N4C—C3C—H3CA	109.7
O10—Mo2—O1	101.56 (14)	N4C—C3C—H3CB	109.7
O10—Mo2—O2	95.77 (15)	C3C—N4C—H4CA	109.3
O10—Mo2—O1H	160.83 (15)	C3C—N4C—H4CB	109.3
O10—Mo2—O6H	94.04 (15)	C3C—N4C—C5C	111.5 (5)
O6H—Mo2—O1H	71.13 (9)	H4CA—N4C—H4CB	108.0
O2—Mo3—O1H	71.25 (11)	C5C—N4C—H4CA	109.3
O2—Mo3—O5H	83.28 (11)	C5C—N4C—H4CB	109.3
O3—Mo3—O2	150.44 (11)	N4C—C5C—H5CA	110.1
O3—Mo3—O1H	85.43 (11)	N4C—C5C—H5CB	110.1
O3—Mo3—O5H	71.97 (10)	H5CA—C5C—H5CB	108.4
O11—Mo3—O2	101.54 (14)	C6C—C5C—N4C	108.1 (5)
O11—Mo3—O3	96.56 (14)	C6C—C5C—H5CA	110.1
O11—Mo3—O1H	90.81 (13)	C6C—C5C—H5CB	110.1
O11—Mo3—O5H	159.23 (13)	O1C—C6C—C5C	111.3 (6)
O12—Mo3—O2	94.92 (14)	O1C—C6C—H6CA	109.4
O12—Mo3—O3	102.24 (13)	O1C—C6C—H6CB	109.4
O12—Mo3—O11	106.25 (15)	C5C—C6C—H6CA	109.4
O12—Mo3—O1H	160.13 (12)	C5C—C6C—H6CB	109.4
O12—Mo3—O5H	93.31 (13)	H6CA—C6C—H6CB	108.0
O5H—Mo3—O1H	71.43 (9)	C61C—O11C—C21C	108.7 (15)
O3—Mo4—O4	149.43 (11)	O11C—C21C—H21A	109.7
O3—Mo4—O3H	83.18 (10)	O11C—C21C—H21B	109.7
O3—Mo4—O5H	71.25 (10)	O11C—C21C—C31C	109.8 (16)
O4—Mo4—O3H	70.39 (10)	H21A—C21C—H21B	108.2
O4—Mo4—O5H	85.41 (11)	C31C—C21C—H21A	109.7
O13—Mo4—O3	103.68 (13)	C31C—C21C—H21B	109.7
O13—Mo4—O4	96.24 (13)	C21C—C31C—H31A	110.1
O13—Mo4—O3H	158.31 (12)	C21C—C31C—H31B	110.1
O13—Mo4—O5H	91.61 (13)	H31A—C31C—H31B	108.4
O14—Mo4—O3	96.60 (13)	N41C—C31C—C21C	108.1 (15)
O14—Mo4—O4	100.88 (13)	N41C—C31C—H31A	110.1
O14—Mo4—O13	103.89 (15)	N41C—C31C—H31B	110.1
O14—Mo4—O3H	95.57 (12)	C31C—N41C—H41A	109.2
O14—Mo4—O5H	162.40 (12)	C31C—N41C—H41B	109.2
O5H—Mo4—O3H	70.87 (9)	C31C—N41C—C51C	112.1 (16)
O4—Mo5—O5	147.96 (11)	H41A—N41C—H41B	107.9
O4—Mo5—O3H	71.61 (10)	C51C—N41C—H41A	109.2
O4—Mo5—O4H	83.53 (11)	C51C—N41C—H41B	109.2
O5—Mo5—O3H	83.23 (10)	N41C—C51C—H51A	109.7
O5—Mo5—O4H	69.51 (10)	N41C—C51C—H51B	109.8
O15—Mo5—O4	97.32 (12)	N41C—C51C—C61C	109.6 (15)
O15—Mo5—O5	100.87 (12)	H51A—C51C—H51B	108.2
O15—Mo5—O3H	161.18 (11)	C61C—C51C—H51A	109.7
O15—Mo5—O4H	92.81 (12)	C61C—C51C—H51B	109.8
O16—Mo5—O4	103.40 (13)	O11C—C61C—C51C	111.3 (16)
O16—Mo5—O5	96.86 (12)	O11C—C61C—H61A	109.4
O16—Mo5—O15	105.52 (14)	O11C—C61C—H61B	109.4
O16—Mo5—O3H	92.07 (12)	C51C—C61C—H61A	109.4
O16—Mo5—O4H	159.17 (12)	C51C—C61C—H61B	109.4
O3H—Mo5—O4H	71.24 (9)	H61A—C61C—H61B	108.0
O5—Mo6—O2H	83.57 (10)	C6E—O1E—C2E	109.8 (5)
O5—Mo6—O4H	71.69 (10)	O1E—C2E—H2EA	109.5
O6—Mo6—O5	149.28 (10)	O1E—C2E—H2EB	109.5
O6—Mo6—O2H	72.51 (10)	O1E—C2E—C3E	110.5 (5)
O6—Mo6—O4H	82.58 (11)	H2EA—C2E—H2EB	108.1
O17—Mo6—O5	94.63 (12)	C3E—C2E—H2EA	109.5
O17—Mo6—O6	103.69 (12)	C3E—C2E—H2EB	109.5
O17—Mo6—O2H	88.87 (11)	C2E—C3E—H3EA	109.8
O17—Mo6—O4H	157.37 (11)	C2E—C3E—H3EB	109.8
O18—Mo6—O5	101.37 (12)	C2E—C3E—N4E	109.5 (5)
O18—Mo6—O6	97.17 (12)	H3EA—C3E—H3EB	108.2
O18—Mo6—O17	105.74 (13)	N4E—C3E—H3EA	109.8
O18—Mo6—O2H	163.99 (11)	N4E—C3E—H3EB	109.8
O18—Mo6—O4H	94.82 (12)	C3E—N4E—H4EA	109.2
O4H—Mo6—O2H	72.08 (9)	C3E—N4E—H4EB	109.2
Mo2—O1—Mo1	119.53 (15)	H4EA—N4E—H4EB	107.9
Mo2—O2—Mo3	120.08 (15)	C5E—N4E—C3E	111.9 (4)
Mo3—O3—Mo4	118.91 (13)	C5E—N4E—H4EA	109.2
Mo5—O4—Mo4	120.31 (14)	C5E—N4E—H4EB	109.2
Mo6—O5—Mo5	119.87 (13)	N4E—C5E—H5EA	110.0
Mo6—O6—Mo1	118.99 (13)	N4E—C5E—H5EB	110.0
H1WA—O1W—H1WB	140.1	N4E—C5E—C6E	108.7 (5)
O1H—Fe1—O2H	96.79 (11)	H5EA—C5E—H5EB	108.3
O1H—Fe1—O3H	97.53 (11)	C6E—C5E—H5EA	110.0
O1H—Fe1—O4H	177.91 (10)	C6E—C5E—H5EB	110.0
O1H—Fe1—O5H	84.54 (11)	O1E—C6E—C5E	110.9 (5)
O1H—Fe1—O6H	84.69 (11)	O1E—C6E—H6EA	109.5
O2H—Fe1—O4H	83.25 (10)	O1E—C6E—H6EB	109.5
O2H—Fe1—O6H	83.30 (11)	C5E—C6E—H6EA	109.5
O3H—Fe1—O2H	99.02 (11)	C5E—C6E—H6EB	109.5
O3H—Fe1—O4H	84.52 (11)	H6EA—C6E—H6EB	108.0
O3H—Fe1—O5H	84.35 (11)	C61E—O11E—C21E	108 (3)
O3H—Fe1—O6H	176.55 (10)	O11E—C21E—H21C	109.6
O5H—Fe1—O2H	176.15 (10)	O11E—C21E—H21D	109.6
O5H—Fe1—O4H	95.29 (11)	O11E—C21E—C31E	110 (3)
O5H—Fe1—O6H	93.25 (11)	H21C—C21E—H21D	108.1
O6H—Fe1—O4H	93.25 (11)	C31E—C21E—H21C	109.6
Mo2—O1H—H1H	118.2	C31E—C21E—H21D	109.6
Mo3—O1H—Mo2	93.80 (10)	C21E—C31E—H31C	110.2
Mo3—O1H—H1H	118.2	C21E—C31E—H31D	110.2
Fe1—O1H—Mo2	102.45 (11)	H31C—C31E—H31D	108.5
Fe1—O1H—Mo3	101.86 (11)	N41E—C31E—C21E	107 (3)
Fe1—O1H—H1H	118.2	N41E—C31E—H31C	110.2
Mo1—O2H—H2H	118.5	N41E—C31E—H31D	110.2
Mo6—O2H—Mo1	92.61 (9)	C31E—N41E—H41C	109.6
Mo6—O2H—H2H	118.5	C31E—N41E—H41D	109.6
Fe1—O2H—Mo1	102.24 (10)	C31E—N41E—C51E	110 (2)
Fe1—O2H—Mo6	102.24 (11)	H41C—N41E—H41D	108.1
Fe1—O2H—H2H	118.5	C51E—N41E—H41C	109.6
Mo4—O3H—H3H	117.7	C51E—N41E—H41D	109.6
Mo5—O3H—Mo4	93.52 (10)	N41E—C51E—H51C	109.7
Mo5—O3H—H3H	117.7	N41E—C51E—H51D	109.7
Fe1—O3H—Mo4	102.43 (10)	H51C—C51E—H51D	108.2
Fe1—O3H—Mo5	103.95 (11)	C61E—C51E—N41E	110 (2)
Fe1—O3H—H3H	117.7	C61E—C51E—H51C	109.7
Mo5—O4H—H4H	118.6	C61E—C51E—H51D	109.7
Mo6—O4H—Mo5	94.02 (9)	O11E—C61E—C51E	114 (3)
Mo6—O4H—H4H	118.6	O11E—C61E—H61C	108.7
Fe1—O4H—Mo5	100.27 (10)	O11E—C61E—H61D	108.7
Fe1—O4H—Mo6	102.34 (11)	C51E—C61E—H61C	108.7
Fe1—O4H—H4H	118.6	C51E—C61E—H61D	108.7
Mo3—O5H—Mo4	93.37 (9)	H61C—C61E—H61D	107.6
Mo3—O5H—H5H	118.3	C6D—O1D—C2D	109.7 (6)
Mo4—O5H—H5H	118.3	O1D—C2D—H2DA	109.4
Fe1—O5H—Mo3	102.11 (11)	O1D—C2D—H2DB	109.4
Fe1—O5H—Mo4	102.35 (11)	O1D—C2D—C3D	111.3 (6)
Fe1—O5H—H5H	118.3	H2DA—C2D—H2DB	108.0
Mo1—O6H—Mo2	94.54 (10)	C3D—C2D—H2DA	109.4
Mo1—O6H—H6H	117.9	C3D—C2D—H2DB	109.4
Mo2—O6H—H6H	117.9	C2D—C3D—H3DA	109.5
Fe1—O6H—Mo1	103.15 (11)	C2D—C3D—H3DB	109.5
Fe1—O6H—Mo2	101.72 (11)	C2D—C3D—N4D	110.8 (6)
Fe1—O6H—H6H	117.9	H3DA—C3D—H3DB	108.1
O2S—S1—O1S	108.74 (16)	N4D—C3D—H3DA	109.5
O3S—S1—O1S	109.32 (19)	N4D—C3D—H3DB	109.5
O3S—S1—O2S	109.95 (19)	C3D—N4D—H4DA	109.3
O3S—S1—O4S	111.28 (18)	C3D—N4D—H4DB	109.3
O4S—S1—O1S	108.9 (2)	H4DA—N4D—H4DB	108.0
O4S—S1—O2S	108.6 (2)	C5D—N4D—C3D	111.6 (6)
C6A—O1A—C2A	109.2 (3)	C5D—N4D—H4DA	109.3
O1A—C2A—H2AA	109.4	C5D—N4D—H4DB	109.3
O1A—C2A—H2AB	109.4	N4D—C5D—H5DA	109.5
O1A—C2A—C3A	111.3 (4)	N4D—C5D—H5DB	109.5
H2AA—C2A—H2AB	108.0	N4D—C5D—C6D	110.8 (7)
C3A—C2A—H2AA	109.4	H5DA—C5D—H5DB	108.1
C3A—C2A—H2AB	109.4	C6D—C5D—H5DA	109.5
C2A—C3A—H3AA	109.9	C6D—C5D—H5DB	109.5
C2A—C3A—H3AB	109.9	O1D—C6D—C5D	111.9 (6)
C2A—C3A—N4A	109.1 (3)	O1D—C6D—H6DA	109.2
H3AA—C3A—H3AB	108.3	O1D—C6D—H6DB	109.2
N4A—C3A—H3AA	109.9	C5D—C6D—H6DA	109.2
N4A—C3A—H3AB	109.9	C5D—C6D—H6DB	109.2
C3A—N4A—H4AA	109.2	H6DA—C6D—H6DB	107.9
C3A—N4A—H4AB	109.2	C21D—O11D—C61D	111.7 (13)
C3A—N4A—C5A	112.1 (3)	O11D—C21D—H21E	109.6
H4AA—N4A—H4AB	107.9	O11D—C21D—H21F	109.6
C5A—N4A—H4AA	109.2	O11D—C21D—C31D	110.1 (13)
C5A—N4A—H4AB	109.2	H21E—C21D—H21F	108.2
N4A—C5A—H5AA	110.1	C31D—C21D—H21E	109.6
N4A—C5A—H5AB	110.1	C31D—C21D—H21F	109.6
N4A—C5A—C6A	108.1 (3)	C21D—C31D—H31E	109.6
H5AA—C5A—H5AB	108.4	C21D—C31D—H31F	109.6
C6A—C5A—H5AA	110.1	H31E—C31D—H31F	108.1
C6A—C5A—H5AB	110.1	N41D—C31D—C21D	110.4 (14)
O1A—C6A—C5A	111.0 (3)	N41D—C31D—H31E	109.6
O1A—C6A—H6AA	109.4	N41D—C31D—H31F	109.6
O1A—C6A—H6AB	109.4	C31D—N41D—H41E	110.0
C5A—C6A—H6AA	109.4	C31D—N41D—H41F	110.0
C5A—C6A—H6AB	109.4	C31D—N41D—C51D	108.4 (16)
H6AA—C6A—H6AB	108.0	H41E—N41D—H41F	108.4
C2B—O1B—C6B	109.5 (3)	C51D—N41D—H41E	110.0
O1B—C2B—H2BA	109.4	C51D—N41D—H41F	110.0
O1B—C2B—H2BB	109.4	N41D—C51D—H51E	109.8
O1B—C2B—C3B	111.1 (3)	N41D—C51D—H51F	109.8
H2BA—C2B—H2BB	108.0	H51E—C51D—H51F	108.3
C3B—C2B—H2BA	109.4	C61D—C51D—N41D	109.2 (15)
C3B—C2B—H2BB	109.4	C61D—C51D—H51E	109.8
C2B—C3B—H3BA	110.0	C61D—C51D—H51F	109.8
C2B—C3B—H3BB	110.0	O11D—C61D—C51D	108.5 (13)
H3BA—C3B—H3BB	108.3	O11D—C61D—H61E	110.0
N4B—C3B—C2B	108.7 (3)	O11D—C61D—H61F	110.0
N4B—C3B—H3BA	110.0	C51D—C61D—H61E	110.0
N4B—C3B—H3BB	110.0	C51D—C61D—H61F	110.0
C3B—N4B—H4BA	109.5	H61E—C61D—H61F	108.4
C3B—N4B—H4BB	109.5	H2WA—O2W—H2WB	109.7
H4BA—N4B—H4BB	108.0	H3WA—O3W—H3WB	109.3
C5B—N4B—C3B	110.9 (3)	H4WA—O4W—H4WB	109.1
C5B—N4B—H4BA	109.5

O1A—C2A—C3A—N4A	56.9 (4)	O1E—C2E—C3E—N4E	55.3 (7)
C2A—O1A—C6A—C5A	64.4 (4)	C2E—O1E—C6E—C5E	64.1 (7)
C2A—C3A—N4A—C5A	−52.4 (5)	C2E—C3E—N4E—C5E	−52.5 (7)
C3A—N4A—C5A—C6A	52.8 (5)	C3E—N4E—C5E—C6E	53.9 (7)
N4A—C5A—C6A—O1A	−58.7 (4)	N4E—C5E—C6E—O1E	−59.7 (7)
C6A—O1A—C2A—C3A	−63.6 (4)	C6E—O1E—C2E—C3E	−61.8 (7)
O1B—C2B—C3B—N4B	−58.7 (4)	O11E—C21E—C31E—N41E	−61 (4)
C2B—O1B—C6B—C5B	−61.6 (5)	C21E—O11E—C61E—C51E	−63 (4)
C2B—C3B—N4B—C5B	54.7 (4)	C21E—C31E—N41E—C51E	55 (3)
C3B—N4B—C5B—C6B	−54.4 (4)	C31E—N41E—C51E—C61E	−53 (3)
N4B—C5B—C6B—O1B	57.5 (5)	N41E—C51E—C61E—O11E	57 (4)
C6B—O1B—C2B—C3B	61.9 (4)	C61E—O11E—C21E—C31E	63 (4)
O1C—C2C—C3C—N4C	−55.1 (7)	O1D—C2D—C3D—N4D	−56.2 (9)
C2C—O1C—C6C—C5C	−64.2 (8)	C2D—O1D—C6D—C5D	−61.6 (9)
C2C—C3C—N4C—C5C	51.1 (8)	C2D—C3D—N4D—C5D	49.8 (10)
C3C—N4C—C5C—C6C	−52.9 (8)	C3D—N4D—C5D—C6D	−48.9 (10)
N4C—C5C—C6C—O1C	59.4 (8)	N4D—C5D—C6D—O1D	55.4 (10)
C6C—O1C—C2C—C3C	61.6 (8)	C6D—O1D—C2D—C3D	62.2 (8)
O11C—C21C—C31C—N41C	61 (3)	O11D—C21D—C31D—N41D	59.6 (19)
C21C—O11C—C61C—C51C	65 (3)	C21D—O11D—C61D—C51D	63.0 (17)
C21C—C31C—N41C—C51C	−52 (3)	C21D—C31D—N41D—C51D	−55.8 (18)
C31C—N41C—C51C—C61C	50 (4)	C31D—N41D—C51D—C61D	57.0 (19)
N41C—C51C—C61C—O11C	−55 (3)	N41D—C51D—C61D—O11D	−58.6 (18)
C61C—O11C—C21C—C31C	−67 (3)	C61D—O11D—C21D—C31D	−62.2 (17)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O9	0.84	1.94	2.781 (11)	178
O1W—H1WB···O10ⁱ	0.85	1.99	2.831 (11)	173
O2W—H2WA···O4Wⁱⁱ	0.85	1.80	2.619 (4)	161
O2W—H2WB···O2Sⁱⁱ	0.85	2.05	2.876 (4)	164
O2W—H2WB···O4Sⁱⁱ	0.85	2.48	3.129 (5)	133
O3W—H3WA···O1Sⁱⁱ	0.85	1.99	2.790 (5)	155
O3W—H3WB···O3	0.85	1.92	2.753 (4)	167
O4W—H4WA···O17ⁱⁱⁱ	0.85	1.88	2.714 (4)	165
O4W—H4WB···O6	0.85	1.94	2.761 (4)	161
O1H—H1H···O4Sⁱⁱ	1.00	1.69	2.673 (4)	165
O2H—H2H···O2W	1.00	1.78	2.743 (4)	162
O3H—H3H···O3Sⁱⁱ	1.00	1.61	2.602 (4)	174
O4H—H4H···O2S	1.00	2.13	2.911 (4)	133
O5H—H5H···O1S	1.00	1.69	2.672 (4)	165
O6H—H6H···O2S	1.00	1.83	2.691 (4)	142
N4A—H4AA···O4Wⁱⁱ	0.91	2.34	3.102 (5)	141
N4A—H4AB···O5	0.91	1.86	2.760 (4)	169
N4B—H4BA···O4	0.91	2.00	2.761 (4)	140
N4B—H4BA···O1A^iv	0.91	2.26	2.840 (4)	121
N4B—H4BB···O15^v	0.91	1.97	2.869 (4)	171
N4C—H4CA···O1E^vi	0.91	1.97	2.817 (7)	155
N41C—H41A···O11E^vi	0.91	1.92	2.54 (5)	124
N4E—H4EA···O1	0.91	1.91	2.780 (6)	160
N41E—H41D···O1	0.91	1.52	2.35 (3)	150
N4D—H4DA···O1S	0.91	1.99	2.866 (8)	162
N4D—H4DB···O2	0.91	2.00	2.846 (9)	155
N41D—H41E···O2	0.91	1.62	2.520 (19)	169

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

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