A hydrated co-crystal of bis­(μ-oxo-κ2O:O)bis[aquaoxodichloro­molybdenum(VI)] with cucurbit[6]uril

Lin, R.-G.; Long, L.-S.; Huang, R.-B.; Zheng, L.-S.; Ng, S.W.

doi:10.1107/S1600536805010858

A hydrated co-crystal of bis(μ-oxo-κ²O:O)bis[aquaoxodichloromolybdenum(VI)] with cucurbit[6]uril

R.-G. Lin, L.-S. Long, R.-B. Huang, L.-S. Zheng and S. W. Ng

Cucurbit[6]uril crystallizes with bis(μ-oxo-κ²O:O)bis[aquaoxodichloromolybdenum(VI)] as the 10.5-hydrate, with the formula [Mo₂O₄Cl₄(H₂O)₂]·(C₃₆H₃₆N₂₄O₁₂)·10.5H₂O. The molybdenum-bearing component interacts indirectly with two cryptands through the two coordinated water molecules, each outer-sphere-coordination cryptand forming only one hydrogen bond with each water molecule. The asymmetric unit has two cryptands, both of which lie on special positions of $\overline{1}$ site symmetry. One of them encapsulates a water molecule that is disordered over two general positions, whereas the other encapsulates one that lies on a centre of inversion. The solvent water molecules interact with the dinuclear complex and with both cucurbituril molecules to form a three-dimensional network structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805010858/bt6642sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805010858/bt6642Isup2.hkl Contains datablock I

CCDC reference: 271819

checkCIF report

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.005 Å
H-atom completeness 99%
Disorder in solvent or counterion
R factor = 0.046
wR factor = 0.139
Data-to-parameter ratio = 14.4

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT430_ALERT_2_A Short Inter D...A Contact  O13'   ..  O13W    ..       1.98 Ang.

Author Response: The two atoms are disordered with respect to each other.

PLAT430_ALERT_2_A Short Inter D...A Contact  O13W   ..  O13W    ..       2.47 Ang.

Author Response: The two atoms are disordered with respect to each other.


Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.96
PLAT417_ALERT_2_B Short Inter D-H..H-D       H22    ..  H62     ..       2.05 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D       H61    ..  H72     ..       2.05 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D       H81    ..  H102    ..       2.05 Ang.
PLAT420_ALERT_2_B D-H Without Acceptor       O6W    -   H62    ...          ?
PLAT430_ALERT_2_B Short Inter D...A Contact  O13'   ..  O13'    ..       2.69 Ang.

Author Response: The two atoms are disordered with respect to each other.


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)...          ?
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      18.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) .....      <O12'
PLAT417_ALERT_2_C Short Inter D-H..H-D       H41    ..  H52     ..       2.12 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H102   ..  H112    ..       2.12 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O9     ..  C5      ..       2.93 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O12W   ..  C7      ..       2.99 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O13    ..  C22     ..       2.96 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          9
              H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         10
              H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         11
              H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         12
              H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         13
              H2 O0.70
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         15
              O

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C36 H61 Cl4 Mo2 N24 O28.5
            Atom count from _chemical_formula_moiety:C36 H97 Cl80 N24 O122.5
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:C36 H61 Cl4 Mo2 N24 O28.5
            Atom count from the _atom_site data:  C36 H60 Cl4 Mo2 N24 O28.5
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  C36 H61 Cl4 Mo2 N24 O28.50
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         72.00     72.00    0.00
           H        122.00    120.00    2.00
           Cl         8.00      8.00    0.00
           Mo         4.00      4.00    0.00
           N         48.00     48.00    0.00
           O         57.00     57.00    0.00

   2 ALERT level A = In general: serious problem
   6 ALERT level B = Potentially serious problem
  17 ALERT level C = Check and explain
   4 ALERT level G = General alerts; check

   7 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
   1 ALERT type 3 Indicator that the structure quality may be low
   7 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Bis[µ-oxoaquadichloromolybdenum(VI)]–cucurbit[6]uril 10.5-hydrate top

Crystal data top

[Mo₂O₄Cl₄(H2O)₂]·(C₃₆H₃₆N₂₄O₁₂)·10.5H₂O	Z = 2
M_r = 1619.77	F(000) = 1650
Triclinic, P1	D_x = 1.866 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 12.4125 (5) Å	Cell parameters from 8301 reflections
b = 15.4864 (6) Å	θ = 2.8–28.3°
c = 17.5542 (7) Å	µ = 0.73 mm⁻¹
α = 106.082 (1)°	T = 173 K
β = 105.386 (1)°	Rod, brown
γ = 106.520 (1)°	0.41 × 0.40 × 0.10 mm
V = 2883.5 (2) Å³

Data collection top

Bruker APEX CCD area-detector diffractometer	12659 independent reflections
Radiation source: fine-focus sealed tube	11649 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.016
φ and ω scans	θ_max = 27.5°, θ_min = 1.3°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −16→16
T_min = 0.701, T_max = 0.930	k = −20→20
24428 measured reflections	l = −22→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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.139	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0814P)² + 8.1614P] where P = (F_o² + 2F_c²)/3
12659 reflections	(Δ/σ)_max = 0.001
879 parameters	Δρ_max = 1.75 e Å⁻³
75 restraints	Δρ_min = −1.70 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mo1	0.60746 (2)	0.334298 (19)	0.844003 (17)	0.01660 (8)
Mo2	0.45234 (2)	0.179157 (19)	0.716433 (17)	0.01717 (8)
Cl1	0.59089 (15)	0.47195 (10)	0.93595 (9)	0.0593 (3)
Cl2	0.83062 (8)	0.42171 (6)	0.89688 (6)	0.02733 (18)
Cl3	0.22912 (8)	0.10991 (6)	0.63950 (6)	0.02900 (19)
Cl4	0.47979 (10)	0.06971 (7)	0.59802 (7)	0.0390 (2)
O1	0.9720 (2)	0.5054 (2)	0.74476 (18)	0.0336 (6)
O2	0.5981 (3)	0.4594 (2)	0.41654 (17)	0.0332 (6)
O3	1.1486 (2)	0.7330 (2)	0.76140 (18)	0.0308 (6)
O4	0.7872 (3)	0.6859 (2)	0.43772 (18)	0.0410 (7)
O5	1.3632 (2)	0.76091 (19)	0.69062 (15)	0.0249 (5)
O6	0.9999 (2)	0.7096 (2)	0.35269 (17)	0.0302 (6)
O7	0.6779 (2)	0.77056 (19)	0.75935 (17)	0.0275 (5)
O8	0.6833 (3)	1.06307 (19)	1.08288 (16)	0.0289 (6)
O9	0.7813 (2)	0.64015 (18)	0.86873 (16)	0.0246 (5)
O10	0.8346 (2)	0.95723 (18)	1.18661 (17)	0.0283 (6)
O11	1.0998 (2)	0.7571 (2)	0.95076 (17)	0.0337 (6)
O12	1.1398 (2)	1.03028 (19)	1.29138 (17)	0.0297 (6)
O13	0.6217 (2)	0.28867 (18)	0.92072 (16)	0.0273 (5)
O14	0.4414 (2)	0.10072 (18)	0.76637 (16)	0.0248 (5)
O15	0.6244 (2)	0.24796 (16)	0.74973 (15)	0.0196 (5)
O16	0.4351 (2)	0.29330 (17)	0.78371 (15)	0.0207 (5)
O1W	0.6288 (2)	0.44041 (17)	0.77717 (15)	0.0228 (5)
H11	0.6861	0.4942	0.8074	0.050*
H12	0.5664	0.4520	0.7608	0.050*
O2W	0.4299 (2)	0.25623 (19)	0.61839 (16)	0.0256 (5)
H21	0.3967	0.2960	0.6243	0.050*
H22	0.4060	0.2226	0.5666	0.050*
O3W	0.4309 (3)	0.4608 (3)	0.7047 (2)	0.0421 (7)
H31	0.4125	0.4832	0.6672	0.050*
H32	0.3731	0.4477	0.7212	0.050*
O4W	0.2475 (3)	0.3547 (2)	0.7529 (2)	0.0371 (6)
H41	0.2892	0.3208	0.7480	0.050*
H42	0.1798	0.3234	0.7132	0.050*
O5W	0.4050 (6)	0.5109 (4)	0.8859 (4)	0.036 (2)	0.537 (14)
H51	0.3707	0.5267	0.9201	0.050*
H52	0.3515	0.4605	0.8446	0.050*
O5'	0.3453 (10)	0.5272 (6)	0.9108 (5)	0.055 (3)	0.463 (14)
O6W	0.3312 (4)	0.1247 (3)	0.4535 (2)	0.0704 (13)
H61	0.3173	0.0810	0.4076	0.050*
H62	0.2657	0.1116	0.4627	0.050*
O7W	0.3257 (11)	−0.0436 (9)	0.4110 (8)	0.206 (5)
H71	0.3220	−0.0928	0.3696	0.050*
H72	0.2498	−0.0580	0.4036	0.050*
O8W	1.1187 (4)	0.4680 (3)	0.6336 (3)	0.0751 (13)
H81	1.1411	0.4450	0.5934	0.050*
H82	1.0633	0.4204	0.6323	0.050*
O9W	1.1348 (3)	0.5295 (3)	0.9029 (2)	0.0572 (10)
H91	1.1299	0.5490	0.9512	0.050*
H92	1.0698	0.5240	0.8672	0.050*
O10W	1.3020 (3)	0.6148 (2)	0.7409 (2)	0.0399 (7)
H101	1.3199	0.6500	0.7140	0.050*
H102	1.2502	0.5607	0.7061	0.050*
O11W	1.2667 (3)	0.6789 (3)	0.8744 (2)	0.0451 (8)
H111	1.2159	0.7008	0.8546	0.050*
H112	1.2747	0.6432	0.8321	0.050*
O12W	0.9333 (5)	1.0992 (4)	1.1297 (4)	0.0593 (18)	0.705 (11)
H121	0.9544	1.0704	1.0917	0.050*
H122	0.8805	1.1165	1.1064	0.050*
O12'	1.0770 (15)	1.1282 (14)	1.0802 (12)	0.085 (6)	0.295 (11)
O13W	0.946 (3)	0.538 (2)	0.5397 (15)	0.121 (7)	0.25
O13'	1.076 (3)	0.594 (2)	0.5325 (15)	0.121 (7)	0.25
N1	0.7798 (3)	0.4069 (2)	0.64596 (18)	0.0220 (6)
N2	0.6295 (3)	0.3891 (2)	0.51503 (18)	0.0215 (6)
N3	0.8304 (3)	0.5663 (2)	0.69580 (19)	0.0232 (6)
N4	0.6856 (3)	0.5492 (2)	0.56199 (19)	0.0230 (6)
N5	0.9530 (3)	0.7228 (2)	0.7040 (2)	0.0254 (6)
N6	0.8045 (3)	0.7119 (2)	0.5768 (2)	0.0268 (6)
N7	1.0997 (3)	0.8239 (2)	0.68472 (19)	0.0228 (6)
N8	0.9516 (3)	0.8060 (2)	0.55287 (19)	0.0239 (6)
N9	1.2607 (3)	0.8423 (2)	0.62929 (18)	0.0225 (6)
N10	1.1079 (3)	0.8140 (2)	0.49380 (19)	0.0229 (6)
N11	1.3405 (3)	0.7564 (2)	0.55489 (18)	0.0220 (6)
N12	1.2015 (3)	0.7446 (2)	0.42053 (18)	0.0245 (6)
N13	0.6291 (3)	0.9026 (2)	0.81093 (18)	0.0198 (5)
N14	0.6244 (3)	1.0164 (2)	0.93701 (18)	0.0204 (6)
N15	0.5905 (3)	0.7851 (2)	0.86106 (18)	0.0201 (6)
N16	0.5960 (3)	0.9021 (2)	0.98990 (18)	0.0230 (6)
N17	0.6719 (3)	0.6988 (2)	0.94186 (18)	0.0202 (6)
N18	0.6895 (3)	0.8220 (2)	1.07105 (19)	0.0215 (6)
N19	0.8389 (3)	0.6877 (2)	1.01472 (18)	0.0216 (6)
N20	0.8566 (3)	0.8101 (2)	1.14469 (18)	0.0219 (6)
N21	1.0575 (2)	0.7584 (2)	1.07165 (18)	0.0202 (6)
N22	1.0753 (3)	0.8675 (2)	1.20886 (19)	0.0220 (6)
N23	1.2367 (2)	0.8589 (2)	1.08683 (18)	0.0197 (5)
N24	1.2505 (3)	0.9695 (2)	1.22090 (18)	0.0210 (6)
C1	0.8712 (3)	0.4947 (3)	0.7002 (2)	0.0231 (7)
C2	0.6687 (3)	0.4177 (2)	0.6065 (2)	0.0189 (6)
H2	0.6050	0.3866	0.6229	0.023*
C3	0.7051 (3)	0.5295 (2)	0.6396 (2)	0.0207 (6)
H3	0.6563	0.5493	0.6694	0.025*
C4	0.6352 (3)	0.4653 (3)	0.4898 (2)	0.0220 (7)
C5	0.9011 (3)	0.6678 (3)	0.7489 (2)	0.0248 (7)
H5A	0.9652	0.6728	0.7969	0.030*
H5B	0.8505	0.6960	0.7706	0.030*
C6	0.6869 (3)	0.6420 (3)	0.5598 (3)	0.0269 (7)
H6A	0.6328	0.6312	0.5044	0.032*
H6B	0.6562	0.6696	0.6011	0.032*
C7	1.0746 (3)	0.7569 (3)	0.7203 (2)	0.0229 (7)
C8	0.8927 (3)	0.7736 (2)	0.6619 (2)	0.0222 (7)
H8	0.8596	0.8093	0.6966	0.027*
C9	0.9954 (3)	0.8420 (2)	0.6452 (2)	0.0210 (6)
H9	1.0071	0.9091	0.6699	0.025*
C10	0.8424 (3)	0.7294 (3)	0.5143 (2)	0.0269 (7)
C11	1.0142 (3)	0.8488 (3)	0.5060 (2)	0.0233 (7)
H11A	1.0504	0.9182	0.5359	0.028*
H11B	0.9564	0.8348	0.4510	0.028*
C12	1.2230 (3)	0.8812 (3)	0.6985 (2)	0.0229 (7)
H12A	1.2767	0.8843	0.7508	0.027*
H12B	1.2302	0.9465	0.7051	0.027*
C13	1.3231 (3)	0.7829 (2)	0.6304 (2)	0.0205 (6)
C14	1.2344 (3)	0.8610 (2)	0.5519 (2)	0.0210 (6)
H14	1.2662	0.9295	0.5637	0.025*
C15	1.2974 (3)	0.8070 (2)	0.5023 (2)	0.0212 (7)
H15	1.3631	0.8517	0.4963	0.025*
C16	1.0932 (3)	0.7513 (3)	0.4164 (2)	0.0226 (7)
C17	1.2180 (3)	0.6841 (3)	0.3490 (2)	0.0237 (7)
H17A	1.1534	0.6704	0.2973	0.028*
H17B	1.2927	0.7198	0.3458	0.028*
C18	1.4256 (3)	0.7116 (2)	0.5448 (2)	0.0221 (7)
H18A	1.4714	0.7145	0.5996	0.027*
H18B	1.4812	0.7488	0.5258	0.027*
C19	0.6368 (3)	0.8142 (2)	0.8055 (2)	0.0199 (6)
C20	0.6434 (3)	0.9417 (2)	0.7467 (2)	0.0218 (7)
H20A	0.6485	0.8936	0.7011	0.026*
H20B	0.5729	0.9542	0.7233	0.026*
C21	0.5595 (3)	0.9278 (2)	0.8615 (2)	0.0181 (6)
H21A	0.4850	0.9276	0.8270	0.022*
C22	0.6582 (3)	1.1120 (2)	0.9351 (2)	0.0199 (6)
H22A	0.6740	1.1581	0.9903	0.024*
H22B	0.5911	1.1145	0.8945	0.024*
C23	0.5359 (3)	0.8473 (2)	0.8985 (2)	0.0184 (6)
H23	0.4508	0.8124	0.8827	0.022*
C24	0.6402 (3)	1.0003 (2)	1.0108 (2)	0.0210 (6)
C25	0.5967 (3)	0.8602 (3)	1.0539 (2)	0.0205 (6)
H25A	0.6077	0.9092	1.1060	0.025*
H25B	0.5192	0.8087	1.0354	0.025*
C26	0.5773 (3)	0.6923 (2)	0.8686 (2)	0.0199 (6)
H26A	0.5774	0.6488	0.8176	0.024*
H26B	0.5003	0.6649	0.8727	0.024*
C27	0.6705 (3)	0.7217 (2)	1.0272 (2)	0.0176 (6)
H27	0.5993	0.6772	1.0280	0.021*
C28	0.7877 (3)	0.7134 (2)	1.0786 (2)	0.0195 (6)
H28	0.7700	0.6646	1.1023	0.023*
C29	0.7975 (3)	0.8719 (2)	1.1391 (2)	0.0206 (6)
C30	0.7665 (3)	0.6733 (2)	0.9353 (2)	0.0194 (6)
C31	0.9493 (3)	0.6698 (2)	1.0304 (2)	0.0222 (7)
H31A	0.9494	0.6319	0.9769	0.027*
H31B	0.9508	0.6323	1.0656	0.027*
C32	1.1283 (3)	0.7879 (2)	1.0286 (2)	0.0215 (7)
C33	1.1221 (3)	0.8038 (2)	1.1632 (2)	0.0196 (6)
H33	1.1309	0.7565	1.1875	0.024*
C34	0.9614 (3)	0.8343 (3)	1.2191 (2)	0.0221 (7)
H34A	0.9621	0.8841	1.2664	0.027*
H34B	0.9536	0.7777	1.2332	0.027*
C35	1.1535 (3)	0.9632 (2)	1.2445 (2)	0.0211 (6)
C36	1.2463 (3)	0.8747 (2)	1.1734 (2)	0.0188 (6)
H36	1.3120	0.8611	1.2037	0.023*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.01957 (14)	0.01388 (14)	0.01605 (14)	0.00537 (10)	0.00654 (10)	0.00651 (10)
Mo2	0.01846 (14)	0.01453 (14)	0.01714 (14)	0.00418 (10)	0.00697 (10)	0.00602 (11)
Cl1	0.0757 (9)	0.0469 (7)	0.0522 (7)	0.0164 (6)	0.0287 (7)	0.0173 (6)
Cl2	0.0204 (4)	0.0222 (4)	0.0324 (4)	0.0062 (3)	0.0050 (3)	0.0072 (3)
Cl3	0.0195 (4)	0.0260 (4)	0.0355 (5)	0.0040 (3)	0.0060 (3)	0.0122 (4)
Cl4	0.0402 (5)	0.0308 (5)	0.0329 (5)	0.0043 (4)	0.0160 (4)	0.0006 (4)
O1	0.0217 (13)	0.0370 (15)	0.0320 (14)	0.0056 (11)	0.0011 (11)	0.0135 (12)
O2	0.0346 (15)	0.0339 (15)	0.0204 (13)	0.0044 (12)	0.0019 (11)	0.0122 (11)
O3	0.0260 (13)	0.0334 (14)	0.0333 (14)	0.0102 (11)	0.0103 (11)	0.0152 (12)
O4	0.0425 (17)	0.0320 (15)	0.0244 (14)	−0.0078 (13)	0.0044 (12)	0.0066 (12)
O5	0.0214 (12)	0.0289 (13)	0.0191 (12)	0.0071 (10)	0.0063 (9)	0.0055 (10)
O6	0.0266 (13)	0.0361 (15)	0.0231 (13)	0.0132 (11)	0.0045 (10)	0.0079 (11)
O7	0.0331 (14)	0.0284 (13)	0.0278 (13)	0.0161 (11)	0.0183 (11)	0.0095 (11)
O8	0.0384 (15)	0.0220 (12)	0.0185 (12)	0.0098 (11)	0.0083 (11)	0.0008 (10)
O9	0.0268 (12)	0.0263 (13)	0.0249 (12)	0.0114 (10)	0.0153 (10)	0.0093 (10)
O10	0.0311 (14)	0.0186 (12)	0.0253 (13)	0.0076 (10)	0.0075 (11)	−0.0008 (10)
O11	0.0257 (13)	0.0396 (16)	0.0181 (12)	0.0033 (12)	0.0053 (10)	−0.0016 (11)
O12	0.0283 (13)	0.0218 (12)	0.0294 (14)	0.0055 (10)	0.0133 (11)	−0.0020 (10)
O13	0.0333 (14)	0.0223 (12)	0.0229 (12)	0.0062 (11)	0.0067 (10)	0.0119 (10)
O14	0.0258 (12)	0.0187 (12)	0.0282 (13)	0.0044 (10)	0.0092 (10)	0.0119 (10)
O15	0.0198 (11)	0.0167 (11)	0.0224 (11)	0.0062 (9)	0.0090 (9)	0.0073 (9)
O16	0.0201 (11)	0.0187 (11)	0.0231 (12)	0.0076 (9)	0.0086 (9)	0.0071 (9)
O1W	0.0251 (12)	0.0184 (11)	0.0224 (12)	0.0045 (9)	0.0070 (10)	0.0099 (10)
O2W	0.0253 (12)	0.0289 (13)	0.0209 (12)	0.0079 (10)	0.0071 (10)	0.0110 (10)
O3W	0.0329 (15)	0.0544 (19)	0.0450 (17)	0.0136 (14)	0.0109 (13)	0.0343 (16)
O4W	0.0366 (15)	0.0437 (17)	0.0385 (16)	0.0233 (13)	0.0154 (13)	0.0170 (13)
O5W	0.034 (3)	0.032 (3)	0.034 (3)	0.005 (2)	0.010 (2)	0.013 (2)
O5'	0.082 (6)	0.052 (4)	0.031 (4)	0.028 (4)	0.019 (4)	0.017 (3)
O6W	0.068 (3)	0.071 (3)	0.0259 (17)	−0.015 (2)	0.0071 (16)	0.0050 (17)
O7W	0.203 (8)	0.214 (8)	0.212 (8)	0.126 (7)	0.086 (6)	0.040 (6)
O8W	0.074 (3)	0.047 (2)	0.080 (3)	0.001 (2)	0.022 (2)	0.020 (2)
O9W	0.0447 (19)	0.069 (2)	0.0372 (18)	0.0007 (17)	0.0044 (15)	0.0235 (17)
O10W	0.0354 (15)	0.0442 (17)	0.0408 (17)	0.0137 (13)	0.0131 (13)	0.0201 (14)
O11W	0.0421 (17)	0.061 (2)	0.0366 (16)	0.0224 (16)	0.0153 (14)	0.0228 (15)
O12W	0.049 (3)	0.038 (3)	0.067 (4)	0.008 (2)	0.005 (2)	0.011 (2)
O12'	0.068 (8)	0.088 (9)	0.096 (9)	0.012 (6)	0.049 (7)	0.032 (7)
O13W	0.152 (18)	0.144 (17)	0.071 (10)	0.065 (15)	0.014 (12)	0.066 (11)
O13'	0.152 (18)	0.144 (17)	0.071 (10)	0.065 (15)	0.014 (12)	0.066 (11)
N1	0.0217 (14)	0.0218 (14)	0.0198 (14)	0.0066 (11)	0.0066 (11)	0.0071 (11)
N2	0.0229 (14)	0.0223 (14)	0.0154 (13)	0.0064 (11)	0.0073 (11)	0.0036 (11)
N3	0.0203 (14)	0.0202 (14)	0.0215 (14)	0.0026 (11)	0.0050 (11)	0.0051 (11)
N4	0.0215 (14)	0.0220 (14)	0.0202 (14)	0.0032 (11)	0.0060 (11)	0.0078 (11)
N5	0.0199 (14)	0.0278 (15)	0.0274 (15)	0.0048 (12)	0.0099 (12)	0.0123 (13)
N6	0.0226 (15)	0.0224 (15)	0.0268 (15)	−0.0004 (12)	0.0063 (12)	0.0092 (12)
N7	0.0178 (13)	0.0218 (14)	0.0260 (15)	0.0051 (11)	0.0100 (11)	0.0062 (12)
N8	0.0221 (14)	0.0232 (14)	0.0232 (15)	0.0041 (12)	0.0104 (12)	0.0071 (12)
N9	0.0217 (14)	0.0245 (14)	0.0199 (14)	0.0079 (12)	0.0106 (11)	0.0050 (11)
N10	0.0201 (14)	0.0239 (14)	0.0228 (14)	0.0073 (12)	0.0089 (11)	0.0062 (12)
N11	0.0212 (14)	0.0260 (15)	0.0181 (13)	0.0090 (12)	0.0095 (11)	0.0054 (11)
N12	0.0253 (15)	0.0293 (16)	0.0170 (13)	0.0109 (12)	0.0085 (11)	0.0051 (12)
N13	0.0232 (14)	0.0162 (13)	0.0185 (13)	0.0056 (11)	0.0094 (11)	0.0050 (11)
N14	0.0240 (14)	0.0136 (13)	0.0179 (13)	0.0043 (11)	0.0065 (11)	0.0022 (10)
N15	0.0251 (14)	0.0163 (13)	0.0198 (13)	0.0083 (11)	0.0109 (11)	0.0054 (11)
N16	0.0314 (15)	0.0185 (14)	0.0167 (13)	0.0085 (12)	0.0091 (12)	0.0046 (11)
N17	0.0218 (14)	0.0208 (14)	0.0185 (13)	0.0097 (11)	0.0085 (11)	0.0057 (11)
N18	0.0205 (14)	0.0175 (13)	0.0229 (14)	0.0077 (11)	0.0067 (11)	0.0035 (11)
N19	0.0189 (13)	0.0219 (14)	0.0215 (14)	0.0082 (11)	0.0076 (11)	0.0043 (11)
N20	0.0201 (13)	0.0186 (14)	0.0201 (14)	0.0050 (11)	0.0038 (11)	0.0037 (11)
N21	0.0175 (13)	0.0148 (13)	0.0203 (14)	0.0029 (10)	0.0044 (11)	0.0012 (11)
N22	0.0195 (13)	0.0168 (13)	0.0232 (14)	0.0039 (11)	0.0083 (11)	0.0010 (11)
N23	0.0182 (13)	0.0174 (13)	0.0192 (13)	0.0056 (11)	0.0071 (11)	0.0022 (11)
N24	0.0219 (14)	0.0152 (13)	0.0197 (13)	0.0021 (11)	0.0092 (11)	0.0017 (11)
C1	0.0219 (16)	0.0267 (17)	0.0179 (15)	0.0054 (14)	0.0085 (13)	0.0075 (13)
C2	0.0184 (15)	0.0201 (15)	0.0163 (15)	0.0050 (12)	0.0087 (12)	0.0047 (12)
C3	0.0182 (15)	0.0203 (16)	0.0206 (16)	0.0032 (12)	0.0091 (12)	0.0063 (13)
C4	0.0153 (14)	0.0249 (17)	0.0224 (16)	0.0032 (13)	0.0078 (12)	0.0081 (13)
C5	0.0254 (17)	0.0235 (17)	0.0170 (15)	0.0009 (14)	0.0076 (13)	0.0048 (13)
C6	0.0160 (15)	0.0250 (17)	0.036 (2)	0.0033 (13)	0.0063 (14)	0.0134 (15)
C7	0.0210 (16)	0.0210 (16)	0.0201 (16)	0.0041 (13)	0.0080 (13)	0.0023 (13)
C8	0.0180 (15)	0.0207 (16)	0.0254 (17)	0.0039 (13)	0.0111 (13)	0.0059 (13)
C9	0.0191 (15)	0.0167 (15)	0.0245 (17)	0.0041 (12)	0.0114 (13)	0.0039 (13)
C10	0.0281 (18)	0.0195 (16)	0.0280 (18)	0.0042 (14)	0.0099 (15)	0.0072 (14)
C11	0.0255 (17)	0.0222 (16)	0.0291 (18)	0.0111 (14)	0.0152 (14)	0.0129 (14)
C12	0.0191 (15)	0.0205 (16)	0.0208 (16)	0.0016 (13)	0.0091 (13)	0.0007 (13)
C13	0.0135 (14)	0.0208 (15)	0.0172 (15)	0.0001 (12)	0.0047 (12)	0.0006 (12)
C14	0.0197 (15)	0.0177 (15)	0.0228 (16)	0.0041 (12)	0.0103 (13)	0.0048 (13)
C15	0.0197 (15)	0.0217 (16)	0.0198 (16)	0.0043 (13)	0.0103 (13)	0.0056 (13)
C16	0.0273 (17)	0.0222 (16)	0.0217 (16)	0.0094 (14)	0.0115 (13)	0.0114 (13)
C17	0.0314 (18)	0.0261 (17)	0.0176 (15)	0.0125 (14)	0.0124 (14)	0.0095 (13)
C18	0.0166 (15)	0.0228 (16)	0.0202 (16)	0.0051 (13)	0.0062 (12)	0.0018 (13)
C19	0.0180 (15)	0.0181 (15)	0.0180 (15)	0.0044 (12)	0.0039 (12)	0.0042 (12)
C20	0.0238 (16)	0.0178 (15)	0.0146 (15)	0.0015 (13)	0.0037 (12)	0.0031 (12)
C21	0.0173 (14)	0.0154 (14)	0.0174 (15)	0.0048 (12)	0.0044 (12)	0.0038 (12)
C22	0.0201 (15)	0.0162 (15)	0.0234 (16)	0.0073 (12)	0.0106 (13)	0.0049 (12)
C23	0.0179 (14)	0.0156 (14)	0.0189 (15)	0.0051 (12)	0.0066 (12)	0.0044 (12)
C24	0.0197 (15)	0.0199 (16)	0.0218 (16)	0.0081 (13)	0.0082 (13)	0.0051 (13)
C25	0.0229 (16)	0.0236 (16)	0.0196 (15)	0.0112 (13)	0.0124 (13)	0.0084 (13)
C26	0.0209 (15)	0.0131 (14)	0.0192 (15)	0.0035 (12)	0.0046 (12)	0.0028 (12)
C27	0.0178 (14)	0.0133 (14)	0.0198 (15)	0.0030 (11)	0.0081 (12)	0.0058 (12)
C28	0.0191 (15)	0.0155 (15)	0.0211 (15)	0.0034 (12)	0.0082 (12)	0.0059 (12)
C29	0.0203 (15)	0.0211 (16)	0.0198 (15)	0.0064 (13)	0.0102 (13)	0.0060 (13)
C30	0.0182 (15)	0.0118 (14)	0.0250 (16)	0.0020 (11)	0.0077 (12)	0.0067 (12)
C31	0.0164 (15)	0.0129 (14)	0.0309 (18)	0.0043 (12)	0.0062 (13)	0.0032 (13)
C32	0.0187 (15)	0.0185 (15)	0.0243 (17)	0.0079 (13)	0.0069 (13)	0.0043 (13)
C33	0.0194 (15)	0.0168 (15)	0.0223 (16)	0.0075 (12)	0.0061 (12)	0.0080 (12)
C34	0.0194 (15)	0.0245 (17)	0.0189 (15)	0.0051 (13)	0.0067 (12)	0.0070 (13)
C35	0.0208 (15)	0.0198 (16)	0.0168 (15)	0.0053 (13)	0.0040 (12)	0.0041 (12)
C36	0.0177 (15)	0.0167 (15)	0.0212 (16)	0.0080 (12)	0.0047 (12)	0.0071 (12)

Geometric parameters (Å, º) top

Mo1—O13	1.678 (2)	N12—C17	1.445 (4)
Mo1—O15	1.921 (2)	N13—C19	1.378 (4)
Mo1—O16	1.937 (2)	N13—C21	1.447 (4)
Mo1—O1W	2.266 (2)	N13—C20	1.447 (4)
Mo1—Cl1	2.390 (2)	N14—C24	1.361 (4)
Mo1—Cl2	2.485 (1)	N14—C22	1.432 (4)
Mo1—Mo2	2.5680 (4)	N14—C21	1.444 (4)
Mo2—O14	1.680 (2)	N15—C19	1.370 (4)
Mo2—O15	1.933 (2)	N15—C23	1.441 (4)
Mo2—O16	1.938 (2)	N15—C26	1.446 (4)
Mo2—O2W	2.353 (2)	N16—C24	1.363 (4)
Mo2—Cl3	2.485 (1)	N16—C25	1.443 (4)
Mo2—Cl4	2.462 (1)	N16—C23	1.450 (4)
O1—C1	1.223 (4)	N17—C30	1.365 (4)
O2—C4	1.213 (4)	N17—C27	1.447 (4)
O3—C7	1.220 (5)	N17—C26	1.450 (4)
O4—C10	1.216 (5)	N18—C29	1.368 (4)
O5—C13	1.224 (4)	N18—C25	1.439 (4)
O6—C16	1.223 (4)	N18—C27	1.446 (4)
O7—C19	1.219 (4)	N19—C30	1.361 (4)
O8—C24	1.222 (4)	N19—C31	1.444 (4)
O9—C30	1.223 (4)	N19—C28	1.448 (4)
O10—C29	1.222 (4)	N20—C29	1.370 (4)
O11—C32	1.226 (4)	N20—C34	1.445 (4)
O12—C35	1.220 (4)	N20—C28	1.450 (4)
O1W—H11	0.84	N21—C32	1.367 (5)
O1W—H12	0.84	N21—C33	1.446 (4)
O2W—H21	0.83	N21—C31	1.448 (4)
O2W—H22	0.83	N22—C35	1.369 (4)
O3W—H31	0.84	N22—C34	1.438 (4)
O3W—H32	0.84	N22—C33	1.446 (4)
O4W—H41	0.84	N23—C32	1.368 (4)
O4W—H42	0.84	N23—C36	1.438 (4)
O5W—H51	0.85	N23—C22ⁱⁱ	1.443 (4)
O5W—H52	0.84	N24—C35	1.360 (4)
O6W—H61	0.84	N24—C20ⁱⁱ	1.445 (4)
O6W—H62	0.85	N24—C36	1.452 (4)
O7W—H71	0.88	C2—C3	1.548 (5)
O7W—H72	0.87	C2—H2	0.9600
O8W—H81	0.85	C3—H3	0.9600
O8W—H82	0.84	C5—H5A	0.9600
O9W—H91	0.84	C5—H5B	0.9600
O9W—H92	0.84	C6—H6A	0.9600
O10W—H101	0.84	C6—H6B	0.9600
O10W—H102	0.83	C8—C9	1.561 (5)
O11W—H111	0.84	C8—H8	0.9600
O11W—H112	0.84	C9—H9	0.9600
O12W—H121	0.84	C11—H11A	0.9600
O12W—H122	0.83	C11—H11B	0.9600
N1—C1	1.370 (4)	C12—H12A	0.9600
N1—C17ⁱ	1.444 (4)	C12—H12B	0.9600
N1—C2	1.449 (4)	C14—C15	1.549 (5)
N2—C4	1.361 (5)	C14—H14	0.9600
N2—C2	1.442 (4)	C15—H15	0.9600
N2—C18ⁱ	1.452 (4)	C17—N1ⁱ	1.444 (4)
N3—C1	1.355 (5)	C17—H17A	0.9600
N3—C5	1.443 (4)	C17—H17B	0.9600
N3—C3	1.444 (4)	C18—N2ⁱ	1.452 (4)
N4—C4	1.375 (4)	C18—H18A	0.9600
N4—C6	1.445 (5)	C18—H18B	0.9600
N4—C3	1.450 (4)	C20—N24ⁱⁱ	1.445 (4)
N5—C7	1.368 (4)	C20—H20A	0.9600
N5—C8	1.444 (5)	C20—H20B	0.9600
N5—C5	1.447 (4)	C21—C23	1.551 (4)
N6—C10	1.365 (5)	C21—H21A	0.9600
N6—C6	1.443 (4)	C22—N23ⁱⁱ	1.443 (4)
N6—C8	1.446 (5)	C22—H22A	0.9600
N7—C7	1.358 (5)	C22—H22B	0.9600
N7—C9	1.440 (4)	C23—H23	0.9600
N7—C12	1.449 (4)	C25—H25A	0.9600
N8—C10	1.363 (5)	C25—H25B	0.9600
N8—C11	1.438 (4)	C26—H26A	0.9600
N8—C9	1.446 (4)	C26—H26B	0.9600
N9—C13	1.361 (5)	C27—C28	1.555 (5)
N9—C14	1.439 (5)	C27—H27	0.9600
N9—C12	1.455 (4)	C28—H28	0.9600
N10—C16	1.364 (4)	C31—H31A	0.9600
N10—C11	1.453 (4)	C31—H31B	0.9600
N10—C14	1.457 (4)	C33—C36	1.548 (5)
N11—C13	1.369 (4)	C33—H33	0.9600
N11—C18	1.442 (4)	C34—H34A	0.9600
N11—C15	1.459 (5)	C34—H34B	0.9600
N12—C16	1.362 (5)	C36—H36	0.9600
N12—C15	1.443 (4)

O13—Mo1—O15	107.3 (1)	N6—C6—N4	114.7 (3)
O13—Mo1—O16	106.3 (1)	N6—C6—H6A	108.6
O13—Mo1—O1W	161.5 (1)	N4—C6—H6A	108.6
O13—Mo1—Cl1	90.0 (1)	N6—C6—H6B	108.6
O13—Mo1—Cl2	91.2 (1)	N4—C6—H6B	108.6
O15—Mo1—O16	92.9 (1)	H6A—C6—H6B	107.6
O15—Mo1—O1W	86.0 (1)	O3—C7—N7	125.6 (3)
O15—Mo1—Cl1	162.4 (1)	O3—C7—N5	126.1 (3)
O15—Mo1—Cl2	85.9 (1)	N7—C7—N5	108.3 (3)
O16—Mo1—O1W	85.3 (1)	N5—C8—N6	113.5 (3)
O16—Mo1—Cl1	85.0 (1)	N5—C8—C9	103.0 (3)
O16—Mo1—Cl2	162.0 (1)	N6—C8—C9	103.1 (3)
O1W—Mo1—Cl1	76.42 (7)	N5—C8—H8	112.2
O1W—Mo1—Cl2	76.78 (7)	N6—C8—H8	112.2
Cl1—Mo1—Cl2	90.72 (4)	C9—C8—H8	112.2
O13—Mo1—Mo2	99.00 (9)	N7—C9—N8	114.8 (3)
O15—Mo1—Mo2	48.42 (7)	N7—C9—C8	102.9 (3)
O16—Mo1—Mo2	48.52 (7)	N8—C9—C8	102.7 (3)
O1W—Mo1—Mo2	99.44 (6)	N7—C9—H9	111.9
Cl1—Mo1—Mo2	133.37 (4)	N8—C9—H9	111.9
Cl2—Mo1—Mo2	134.26 (2)	C8—C9—H9	111.9
O14—Mo2—O15	104.8 (1)	O4—C10—N8	126.0 (4)
O14—Mo2—O16	108.4 (1)	O4—C10—N6	126.1 (3)
O14—Mo2—O2W	166.1 (1)	N8—C10—N6	107.9 (3)
O14—Mo2—Cl3	91.4 (1)	N8—C11—N10	113.6 (3)
O14—Mo2—Cl4	92.8 (1)	N8—C11—H11A	108.9
O15—Mo2—O16	92.5 (1)	N10—C11—H11A	108.9
O15—Mo2—O2W	85.4 (1)	N8—C11—H11B	108.9
O15—Mo2—Cl3	163.0 (1)	N10—C11—H11B	108.9
O15—Mo2—Cl4	82.2 (1)	H11A—C11—H11B	107.7
O16—Mo2—O2W	80.0 (1)	N7—C12—N9	113.3 (3)
O16—Mo2—Cl3	87.2 (1)	N7—C12—H12A	108.9
O16—Mo2—Cl4	158.8 (1)	N9—C12—H12A	108.9
O2W—Mo2—Cl3	77.8 (1)	N7—C12—H12B	108.9
O2W—Mo2—Cl4	79.1 (1)	N9—C12—H12B	108.9
Cl3—Mo2—Cl4	91.95 (4)	H12A—C12—H12B	107.7
O14—Mo2—Mo1	98.75 (9)	O5—C13—N9	125.9 (3)
O15—Mo2—Mo1	48.01 (7)	O5—C13—N11	125.2 (3)
O16—Mo2—Mo1	48.48 (7)	N9—C13—N11	108.8 (3)
O2W—Mo2—Mo1	95.09 (6)	N9—C14—N10	115.5 (3)
Cl4—Mo2—Mo1	130.21 (3)	N9—C14—C15	103.1 (3)
Cl3—Mo2—Mo1	135.56 (3)	N10—C14—C15	102.9 (3)
Mo1—O15—Mo2	83.57 (9)	N9—C14—H14	111.5
Mo1—O16—Mo2	83.00 (9)	N10—C14—H14	111.5
Mo1—O1W—H11	113.4	C15—C14—H14	111.5
Mo1—O1W—H12	113.0	N12—C15—N11	115.0 (3)
H11—O1W—H12	106.8	N12—C15—C14	103.4 (3)
Mo2—O2W—H21	118.6	N11—C15—C14	103.5 (3)
Mo2—O2W—H22	118.5	N12—C15—H15	111.5
H21—O2W—H22	108.8	N11—C15—H15	111.5
H31—O3W—H32	107.7	C14—C15—H15	111.5
H41—O4W—H42	107.6	O6—C16—N12	125.0 (3)
H51—O5W—H52	105.3	O6—C16—N10	126.4 (3)
H61—O6W—H62	106.4	N12—C16—N10	108.6 (3)
H71—O7W—H72	101.8	N1ⁱ—C17—N12	113.7 (3)
H81—O8W—H82	106.0	N1ⁱ—C17—H17A	108.8
H91—O9W—H92	106.0	N12—C17—H17A	108.8
H101—O10W—H102	108.5	N1ⁱ—C17—H17B	108.8
H111—O11W—H112	106.4	N12—C17—H17B	108.8
H121—O12W—H122	107.5	H17A—C17—H17B	107.7
C1—N1—C17ⁱ	122.1 (3)	N11—C18—N2ⁱ	114.4 (3)
C1—N1—C2	112.0 (3)	N11—C18—H18A	108.7
C17ⁱ—N1—C2	122.6 (3)	N2ⁱ—C18—H18A	108.7
C4—N2—C2	113.1 (3)	N11—C18—H18B	108.7
C4—N2—C18ⁱ	122.8 (3)	N2ⁱ—C18—H18B	108.7
C2—N2—C18ⁱ	123.6 (3)	H18A—C18—H18B	107.6
C1—N3—C5	123.0 (3)	O7—C19—N15	126.6 (3)
C1—N3—C3	113.1 (3)	O7—C19—N13	125.6 (3)
C5—N3—C3	123.5 (3)	N15—C19—N13	107.8 (3)
C4—N4—C6	122.9 (3)	N24ⁱⁱ—C20—N13	113.4 (3)
C4—N4—C3	112.2 (3)	N24ⁱⁱ—C20—H20A	108.9
C6—N4—C3	122.8 (3)	N13—C20—H20A	108.9
C7—N5—C8	112.4 (3)	N24ⁱⁱ—C20—H20B	108.9
C7—N5—C5	122.0 (3)	N13—C20—H20B	108.9
C8—N5—C5	122.5 (3)	H20A—C20—H20B	107.7
C10—N6—C6	123.6 (3)	N14—C21—N13	115.4 (3)
C10—N6—C8	112.9 (3)	N14—C21—C23	103.2 (3)
C6—N6—C8	123.5 (3)	N13—C21—C23	103.5 (2)
C7—N7—C9	113.2 (3)	N14—C21—H21A	111.4
C7—N7—C12	121.7 (3)	N13—C21—H21A	111.4
C9—N7—C12	124.4 (3)	C23—C21—H21A	111.4
C10—N8—C11	123.0 (3)	N14—C22—N23ⁱⁱ	114.0 (3)
C10—N8—C9	113.3 (3)	N14—C22—H22A	108.8
C11—N8—C9	123.7 (3)	N23ⁱⁱ—C22—H22A	108.8
C13—N9—C14	112.9 (3)	N14—C22—H22B	108.8
C13—N9—C12	123.4 (3)	N23ⁱⁱ—C22—H22B	108.8
C14—N9—C12	123.7 (3)	H22A—C22—H22B	107.7
C16—N10—C11	121.8 (3)	N15—C23—N16	115.5 (3)
C16—N10—C14	112.0 (3)	N15—C23—C21	103.3 (3)
C11—N10—C14	124.0 (3)	N16—C23—C21	102.8 (3)
C13—N11—C18	121.1 (3)	N15—C23—H23	111.5
C13—N11—C15	111.3 (3)	N16—C23—H23	111.5
C18—N11—C15	124.5 (3)	C21—C23—H23	111.5
C16—N12—C15	112.6 (3)	O8—C24—N14	125.8 (3)
C16—N12—C17	123.0 (3)	O8—C24—N16	126.3 (3)
C15—N12—C17	124.3 (3)	N14—C24—N16	107.9 (3)
C19—N13—C21	112.0 (3)	N18—C25—N16	113.9 (3)
C19—N13—C20	121.1 (3)	N18—C25—H25A	108.8
C21—N13—C20	122.3 (3)	N16—C25—H25A	108.8
C24—N14—C22	122.9 (3)	N18—C25—H25B	108.8
C24—N14—C21	113.0 (3)	N16—C25—H25B	108.8
C22—N14—C21	123.8 (3)	H25A—C25—H25B	107.7
C19—N15—C23	112.7 (3)	N15—C26—N17	113.6 (3)
C19—N15—C26	123.1 (3)	N15—C26—H26A	108.8
C23—N15—C26	123.1 (3)	N17—C26—H26A	108.8
C24—N16—C25	122.0 (3)	N15—C26—H26B	108.8
C24—N16—C23	112.8 (3)	N17—C26—H26B	108.8
C25—N16—C23	124.7 (3)	H26A—C26—H26B	107.7
C30—N17—C27	112.2 (3)	N18—C27—N17	114.6 (3)
C30—N17—C26	122.7 (3)	N18—C27—C28	103.1 (3)
C27—N17—C26	124.8 (3)	N17—C27—C28	103.5 (3)
C29—N18—C25	123.2 (3)	N18—C27—H27	111.7
C29—N18—C27	112.7 (3)	N17—C27—H27	111.7
C25—N18—C27	123.3 (3)	C28—C27—H27	111.7
C30—N19—C31	122.4 (3)	N19—C28—N20	114.6 (3)
C30—N19—C28	112.9 (3)	N19—C28—C27	102.6 (3)
C31—N19—C28	124.5 (3)	N20—C28—C27	103.5 (3)
C29—N20—C34	122.0 (3)	N19—C28—H28	111.8
C29—N20—C28	112.2 (3)	N20—C28—H28	111.8
C34—N20—C28	124.4 (3)	C27—C28—H28	111.8
C32—N21—C33	112.0 (3)	O10—C29—N18	125.5 (3)
C32—N21—C31	121.6 (3)	O10—C29—N20	126.0 (3)
C33—N21—C31	123.2 (3)	N18—C29—N20	108.5 (3)
C35—N22—C34	123.4 (3)	O9—C30—N19	126.0 (3)
C35—N22—C33	112.6 (3)	O9—C30—N17	125.6 (3)
C34—N22—C33	124.0 (3)	N19—C30—N17	108.4 (3)
C32—N23—C36	112.3 (3)	N19—C31—N21	113.2 (3)
C32—N23—C22ⁱⁱ	122.1 (3)	N19—C31—H31A	108.9
C36—N23—C22ⁱⁱ	122.2 (3)	N21—C31—H31A	108.9
C35—N24—C20ⁱⁱ	123.4 (3)	N19—C31—H31B	108.9
C35—N24—C36	112.5 (3)	N21—C31—H31B	108.9
C20ⁱⁱ—N24—C36	123.1 (3)	H31A—C31—H31B	107.8
O1—C1—N3	126.6 (3)	O11—C32—N21	126.2 (3)
O1—C1—N1	125.1 (3)	O11—C32—N23	125.3 (3)
N3—C1—N1	108.3 (3)	N21—C32—N23	108.5 (3)
N2—C2—N1	114.6 (3)	N22—C33—N21	115.1 (3)
N2—C2—C3	103.3 (3)	N22—C33—C36	103.2 (3)
N1—C2—C3	103.5 (3)	N21—C33—C36	103.4 (3)
N2—C2—H2	111.6	N22—C33—H33	111.5
N1—C2—H2	111.6	N21—C33—H33	111.5
C3—C2—H2	111.6	C36—C33—H33	111.5
N3—C3—N4	115.0 (3)	N22—C34—N20	114.4 (3)
N3—C3—C2	102.9 (3)	N22—C34—H34A	108.7
N4—C3—C2	103.2 (3)	N20—C34—H34A	108.7
N3—C3—H3	111.7	N22—C34—H34B	108.7
N4—C3—H3	111.7	N20—C34—H34B	108.7
C2—C3—H3	111.7	H34A—C34—H34B	107.6
O2—C4—N2	125.7 (3)	O12—C35—N24	126.2 (3)
O2—C4—N4	126.3 (3)	O12—C35—N22	125.5 (3)
N2—C4—N4	107.9 (3)	N24—C35—N22	108.2 (3)
N3—C5—N5	113.0 (3)	N23—C36—N24	114.2 (3)
N3—C5—H5A	109.0	N23—C36—C33	103.6 (3)
N5—C5—H5A	109.0	N24—C36—C33	103.2 (3)
N3—C5—H5B	109.0	N23—C36—H36	111.7
N5—C5—H5B	109.0	N24—C36—H36	111.7
H5A—C5—H5B	107.8	C33—C36—H36	111.7

O13—Mo1—Mo2—O14	−3.10 (13)	C11—N10—C14—N9	77.9 (4)
O15—Mo1—Mo2—O14	102.11 (13)	C16—N10—C14—C15	−7.3 (4)
O16—Mo1—Mo2—O14	−106.88 (13)	C11—N10—C14—C15	−170.5 (3)
O1W—Mo1—Mo2—O14	178.12 (11)	C16—N12—C15—N11	109.7 (3)
Cl1—Mo1—Mo2—O14	−101.69 (10)	C17—N12—C15—N11	−72.7 (4)
Cl2—Mo1—Mo2—O14	97.43 (10)	C16—N12—C15—C14	−2.3 (4)
O13—Mo1—Mo2—O15	−105.22 (13)	C17—N12—C15—C14	175.3 (3)
O16—Mo1—Mo2—O15	151.01 (14)	C13—N11—C15—N12	−118.9 (3)
O1W—Mo1—Mo2—O15	76.01 (11)	C18—N11—C15—N12	80.9 (4)
Cl1—Mo1—Mo2—O15	156.20 (11)	C13—N11—C15—C14	−6.9 (3)
Cl2—Mo1—Mo2—O15	−4.68 (10)	C18—N11—C15—C14	−167.1 (3)
O13—Mo1—Mo2—O16	103.78 (14)	N9—C14—C15—N12	126.0 (3)
O15—Mo1—Mo2—O16	−151.01 (14)	N10—C14—C15—N12	5.5 (3)
O1W—Mo1—Mo2—O16	−75.00 (12)	N9—C14—C15—N11	5.7 (3)
Cl1—Mo1—Mo2—O16	5.19 (10)	N10—C14—C15—N11	−114.8 (3)
Cl2—Mo1—Mo2—O16	−155.69 (10)	C15—N12—C16—O6	176.0 (3)
O13—Mo1—Mo2—O2W	175.63 (12)	C17—N12—C16—O6	−1.6 (6)
O15—Mo1—Mo2—O2W	−79.15 (11)	C15—N12—C16—N10	−2.2 (4)
O16—Mo1—Mo2—O2W	71.86 (11)	C17—N12—C16—N10	−179.8 (3)
O1W—Mo1—Mo2—O2W	−3.14 (9)	C11—N10—C16—O6	−8.3 (5)
Cl1—Mo1—Mo2—O2W	77.05 (8)	C14—N10—C16—O6	−172.0 (3)
Cl2—Mo1—Mo2—O2W	−83.83 (7)	C11—N10—C16—N12	169.9 (3)
O13—Mo1—Mo2—Cl4	−104.29 (10)	C14—N10—C16—N12	6.2 (4)
O15—Mo1—Mo2—Cl4	0.93 (10)	C16—N12—C17—N1ⁱ	−101.4 (4)
O16—Mo1—Mo2—Cl4	151.93 (10)	C15—N12—C17—N1ⁱ	81.3 (4)
O1W—Mo1—Mo2—Cl4	76.93 (8)	C13—N11—C18—N2ⁱ	113.0 (3)
Cl1—Mo1—Mo2—Cl4	157.12 (6)	C15—N11—C18—N2ⁱ	−88.7 (4)
Cl2—Mo1—Mo2—Cl4	−3.76 (5)	C23—N15—C19—O7	−172.9 (3)
O13—Mo1—Mo2—Cl3	97.96 (10)	C26—N15—C19—O7	−4.0 (5)
O15—Mo1—Mo2—Cl3	−156.82 (10)	C23—N15—C19—N13	7.3 (4)
O16—Mo1—Mo2—Cl3	−5.81 (10)	C26—N15—C19—N13	176.1 (3)
O1W—Mo1—Mo2—Cl3	−80.81 (7)	C21—N13—C19—O7	171.2 (3)
Cl1—Mo1—Mo2—Cl3	−0.62 (6)	C20—N13—C19—O7	14.9 (5)
Cl2—Mo1—Mo2—Cl3	−161.50 (5)	C21—N13—C19—N15	−9.0 (4)
O13—Mo1—O15—Mo2	86.69 (12)	C20—N13—C19—N15	−165.2 (3)
O16—Mo1—O15—Mo2	−21.32 (10)	C19—N13—C20—N24ⁱⁱ	−114.8 (3)
O1W—Mo1—O15—Mo2	−106.36 (9)	C21—N13—C20—N24ⁱⁱ	91.4 (4)
Cl1—Mo1—O15—Mo2	−103.8 (3)	C24—N14—C21—N13	−113.1 (3)
Cl2—Mo1—O15—Mo2	176.64 (7)	C22—N14—C21—N13	72.9 (4)
O14—Mo2—O15—Mo1	−88.48 (11)	C24—N14—C21—C23	−1.0 (4)
O16—Mo2—O15—Mo1	21.30 (10)	C22—N14—C21—C23	−175.0 (3)
O2W—Mo2—O15—Mo1	101.07 (9)	C19—N13—C21—N14	118.9 (3)
Cl4—Mo2—O15—Mo1	−179.29 (8)	C20—N13—C21—N14	−85.2 (4)
Cl3—Mo2—O15—Mo1	110.0 (2)	C19—N13—C21—C23	6.9 (3)
O13—Mo1—O16—Mo2	−87.69 (12)	C20—N13—C21—C23	162.8 (3)
O15—Mo1—O16—Mo2	21.29 (10)	C24—N14—C22—N23ⁱⁱ	108.3 (4)
O1W—Mo1—O16—Mo2	107.04 (9)	C21—N14—C22—N23ⁱⁱ	−78.3 (4)
Cl1—Mo1—O16—Mo2	−176.21 (8)	C19—N15—C23—N16	−114.3 (3)
Cl2—Mo1—O16—Mo2	107.1 (2)	C26—N15—C23—N16	76.9 (4)
O14—Mo2—O16—Mo1	85.38 (11)	C19—N15—C23—C21	−2.9 (3)
O15—Mo2—O16—Mo1	−21.14 (10)	C26—N15—C23—C21	−171.7 (3)
O2W—Mo2—O16—Mo1	−106.03 (9)	C24—N16—C23—N15	117.1 (3)
Cl4—Mo2—O16—Mo1	−95.8 (2)	C25—N16—C23—N15	−70.6 (4)
Cl3—Mo2—O16—Mo1	175.93 (7)	C24—N16—C23—C21	5.3 (4)
C5—N3—C1—O1	−3.9 (6)	C25—N16—C23—C21	177.7 (3)
C3—N3—C1—O1	−177.7 (3)	N14—C21—C23—N15	−123.0 (3)
C5—N3—C1—N1	176.0 (3)	N13—C21—C23—N15	−2.4 (3)
C3—N3—C1—N1	2.3 (4)	N14—C21—C23—N16	−2.5 (3)
C17ⁱ—N1—C1—O1	16.0 (5)	N13—C21—C23—N16	118.2 (3)
C2—N1—C1—O1	176.1 (3)	C22—N14—C24—O8	0.3 (5)
C17ⁱ—N1—C1—N3	−164.0 (3)	C21—N14—C24—O8	−173.7 (3)
C2—N1—C1—N3	−3.9 (4)	C22—N14—C24—N16	178.4 (3)
C4—N2—C2—N1	−112.9 (3)	C21—N14—C24—N16	4.4 (4)
C18ⁱ—N2—C2—N1	74.9 (4)	C25—N16—C24—O8	−0.7 (6)
C4—N2—C2—C3	−1.1 (4)	C23—N16—C24—O8	171.9 (3)
C18ⁱ—N2—C2—C3	−173.3 (3)	C25—N16—C24—N14	−178.8 (3)
C1—N1—C2—N2	115.5 (3)	C23—N16—C24—N14	−6.2 (4)
C17ⁱ—N1—C2—N2	−84.5 (4)	C29—N18—C25—N16	98.8 (4)
C1—N1—C2—C3	3.8 (3)	C27—N18—C25—N16	−91.9 (4)
C17ⁱ—N1—C2—C3	163.7 (3)	C24—N16—C25—N18	−103.9 (4)
C1—N3—C3—N4	−111.4 (3)	C23—N16—C25—N18	84.5 (4)
C5—N3—C3—N4	75.0 (4)	C19—N15—C26—N17	101.1 (4)
C1—N3—C3—C2	0.1 (4)	C23—N15—C26—N17	−91.2 (4)
C5—N3—C3—C2	−173.6 (3)	C30—N17—C26—N15	−102.0 (4)
C4—N4—C3—N3	116.0 (3)	C27—N17—C26—N15	85.4 (4)
C6—N4—C3—N3	−80.2 (4)	C29—N18—C27—N17	−112.1 (3)
C4—N4—C3—C2	4.7 (4)	C25—N18—C27—N17	77.6 (4)
C6—N4—C3—C2	168.5 (3)	C29—N18—C27—C28	−0.4 (4)
N2—C2—C3—N3	−122.0 (3)	C25—N18—C27—C28	−170.7 (3)
N1—C2—C3—N3	−2.2 (3)	C30—N17—C27—N18	115.2 (3)
N2—C2—C3—N4	−2.0 (3)	C26—N17—C27—N18	−71.5 (4)
N1—C2—C3—N4	117.8 (3)	C30—N17—C27—C28	3.7 (3)
C2—N2—C4—O2	−173.6 (3)	C26—N17—C27—C28	177.0 (3)
C18ⁱ—N2—C4—O2	−1.3 (5)	C30—N19—C28—N20	−115.8 (3)
C2—N2—C4—N4	4.1 (4)	C31—N19—C28—N20	69.6 (4)
C18ⁱ—N2—C4—N4	176.3 (3)	C30—N19—C28—C27	−4.4 (3)
C6—N4—C4—O2	8.3 (6)	C31—N19—C28—C27	−179.0 (3)
C3—N4—C4—O2	172.1 (3)	C29—N20—C28—N19	111.0 (3)
C6—N4—C4—N2	−169.3 (3)	C34—N20—C28—N19	−82.2 (4)
C3—N4—C4—N2	−5.5 (4)	C29—N20—C28—C27	0.0 (4)
C1—N3—C5—N5	103.3 (4)	C34—N20—C28—C27	166.8 (3)
C3—N3—C5—N5	−83.7 (4)	N18—C27—C28—N19	−119.3 (3)
C7—N5—C5—N3	−109.1 (4)	N17—C27—C28—N19	0.4 (3)
C8—N5—C5—N3	92.4 (4)	N18—C27—C28—N20	0.2 (3)
C10—N6—C6—N4	99.2 (4)	N17—C27—C28—N20	120.0 (3)
C8—N6—C6—N4	−83.4 (4)	C25—N18—C29—O10	−9.4 (6)
C4—N4—C6—N6	−108.8 (4)	C27—N18—C29—O10	−179.7 (3)
C3—N4—C6—N6	89.1 (4)	C25—N18—C29—N20	170.7 (3)
C9—N7—C7—O3	−175.9 (3)	C27—N18—C29—N20	0.4 (4)
C12—N7—C7—O3	−5.3 (5)	C34—N20—C29—O10	12.6 (5)
C9—N7—C7—N5	2.7 (4)	C28—N20—C29—O10	179.8 (3)
C12—N7—C7—N5	173.3 (3)	C34—N20—C29—N18	−167.5 (3)
C8—N5—C7—O3	173.4 (3)	C28—N20—C29—N18	−0.3 (4)
C5—N5—C7—O3	12.9 (6)	C31—N19—C30—O9	3.8 (5)
C8—N5—C7—N7	−5.1 (4)	C28—N19—C30—O9	−170.9 (3)
C5—N5—C7—N7	−165.6 (3)	C31—N19—C30—N17	−178.4 (3)
C7—N5—C8—N6	115.9 (3)	C28—N19—C30—N17	6.9 (4)
C5—N5—C8—N6	−83.7 (4)	C27—N17—C30—O9	171.3 (3)
C7—N5—C8—C9	5.2 (4)	C26—N17—C30—O9	−2.2 (5)
C5—N5—C8—C9	165.6 (3)	C27—N17—C30—N19	−6.5 (4)
C10—N6—C8—N5	−107.0 (3)	C26—N17—C30—N19	180.0 (3)
C6—N6—C8—N5	75.4 (4)	C30—N19—C31—N21	106.2 (4)
C10—N6—C8—C9	3.7 (4)	C28—N19—C31—N21	−79.7 (4)
C6—N6—C8—C9	−173.9 (3)	C32—N21—C31—N19	−107.8 (4)
C7—N7—C9—N8	−110.2 (3)	C33—N21—C31—N19	94.0 (4)
C12—N7—C9—N8	79.5 (4)	C33—N21—C32—O11	175.3 (3)
C7—N7—C9—C8	0.5 (4)	C31—N21—C32—O11	14.9 (5)
C12—N7—C9—C8	−169.8 (3)	C33—N21—C32—N23	−5.3 (4)
C10—N8—C9—N7	110.8 (3)	C31—N21—C32—N23	−165.8 (3)
C11—N8—C9—N7	−71.5 (4)	C36—N23—C32—O11	−176.1 (3)
C10—N8—C9—C8	0.0 (4)	C22ⁱⁱ—N23—C32—O11	−16.6 (5)
C11—N8—C9—C8	177.7 (3)	C36—N23—C32—N21	4.6 (4)
N5—C8—C9—N7	−3.3 (3)	C22ⁱⁱ—N23—C32—N21	164.1 (3)
N6—C8—C9—N7	−121.6 (3)	C35—N22—C33—N21	−112.8 (3)
N5—C8—C9—N8	116.2 (3)	C34—N22—C33—N21	69.7 (4)
N6—C8—C9—N8	−2.1 (3)	C35—N22—C33—C36	−0.9 (4)
C11—N8—C10—O4	2.9 (6)	C34—N22—C33—C36	−178.4 (3)
C9—N8—C10—O4	−179.3 (4)	C32—N21—C33—N22	115.7 (3)
C11—N8—C10—N6	−175.4 (3)	C31—N21—C33—N22	−84.2 (4)
C9—N8—C10—N6	2.3 (4)	C32—N21—C33—C36	3.9 (3)
C6—N6—C10—O4	−4.6 (6)	C31—N21—C33—C36	164.0 (3)
C8—N6—C10—O4	177.8 (4)	C35—N22—C34—N20	104.6 (4)
C6—N6—C10—N8	173.7 (3)	C33—N22—C34—N20	−78.2 (4)
C8—N6—C10—N8	−3.9 (4)	C29—N20—C34—N22	−101.7 (4)
C10—N8—C11—N10	−98.1 (4)	C28—N20—C34—N22	92.7 (4)
C9—N8—C11—N10	84.4 (4)	C20ⁱⁱ—N24—C35—O12	3.9 (6)
C16—N10—C11—N8	106.7 (4)	C36—N24—C35—O12	172.6 (3)
C14—N10—C11—N8	−91.7 (4)	C20ⁱⁱ—N24—C35—N22	−174.0 (3)
C7—N7—C12—N9	97.8 (4)	C36—N24—C35—N22	−5.2 (4)
C9—N7—C12—N9	−92.7 (4)	C34—N22—C35—O12	3.4 (6)
C13—N9—C12—N7	−95.6 (4)	C33—N22—C35—O12	−174.1 (3)
C14—N9—C12—N7	83.3 (4)	C34—N22—C35—N24	−178.8 (3)
C14—N9—C13—O5	175.1 (3)	C33—N22—C35—N24	3.7 (4)
C12—N9—C13—O5	−5.9 (5)	C32—N23—C36—N24	−113.5 (3)
C14—N9—C13—N11	−1.3 (4)	C22ⁱⁱ—N23—C36—N24	87.0 (4)
C12—N9—C13—N11	177.8 (3)	C32—N23—C36—C33	−2.0 (3)
C18—N11—C13—O5	−10.0 (5)	C22ⁱⁱ—N23—C36—C33	−161.5 (3)
C15—N11—C13—O5	−171.0 (3)	C35—N24—C36—N23	116.2 (3)
C18—N11—C13—N9	166.3 (3)	C20ⁱⁱ—N24—C36—N23	−75.0 (4)
C15—N11—C13—N9	5.4 (4)	C35—N24—C36—C33	4.5 (4)
C13—N9—C14—N10	108.5 (3)	C20ⁱⁱ—N24—C36—C33	173.3 (3)
C12—N9—C14—N10	−70.5 (4)	N22—C33—C36—N23	−121.4 (3)
C13—N9—C14—C15	−3.0 (4)	N21—C33—C36—N23	−1.1 (3)
C12—N9—C14—C15	178.0 (3)	N22—C33—C36—N24	−2.0 (3)
C16—N10—C14—N9	−118.9 (3)	N21—C33—C36—N24	118.3 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11···O9	0.84	2.03	2.835 (3)	161
O1W—H12···O3W	0.84	1.77	2.599 (4)	168
O2W—H21···O4ⁱⁱⁱ	0.83	2.39	3.080 (4)	142
O2W—H21···O3W	0.83	2.40	3.105 (4)	143
O2W—H22···O6W	0.83	1.91	2.731 (4)	168
O3W—H31···O2ⁱⁱⁱ	0.84	1.91	2.738 (4)	169
O3W—H32···O4W	0.84	2.11	2.874 (4)	152
O4W—H42···O6ⁱⁱⁱ	0.84	2.06	2.842 (4)	157
O4W—H41···O16	0.84	1.96	2.738 (4)	154
O5W—H51···Cl1^iv	0.85	2.44	3.050 (7)	130
O5W—H52···O4W	0.84	1.78	2.624 (6)	175
O6W—H61···O12^v	0.84	2.32	2.831 (4)	120
O7W—H71···Cl4^vi	0.88	2.27	2.60 (1)	102
O8W—H82···O6ⁱ	0.84	2.06	2.835 (5)	153
O8W—H81···O13Wⁱ	0.85	2.42	2.90 (2)	116
O9W—H91···Cl2^vii	0.84	2.46	3.264 (4)	159
O9W—H92···O1	0.84	2.06	2.819 (4)	149
O10W—H101···O5	0.84	1.84	2.638 (4)	159
O10W—H102···O8W	0.83	1.70	2.511 (5)	164
O11W—H112···O10W	0.84	1.69	2.485 (5)	156
O11W—H111···O3	0.84	1.89	2.619 (4)	144
O12W—H122···O11ⁱⁱ	0.83	2.42	3.012 (7)	129

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

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A hydrated co-crystal of bis­(μ-oxo-κ2O:O)bis[aquaoxodichloro­molybdenum(VI)] with cucurbit[6]uril

Supporting information

Key indicators

checkCIF/PLATON results

A hydrated co-crystal of bis(μ-oxo-κ²O:O)bis[aquaoxodichloromolybdenum(VI)] with cucurbit[6]uril