μ-Oxido-bis-[chlorido(4,4'-di-tert-butyl-2,2'-bipyridine-κN,N')dioxido-molybdenum(VI)] 0.2-hydrate.

The title hydrate, [Mo(2)Cl(2)O(5)(C(18)H(24)N(2))(2)]·0.2H(2)O, has been isolated as the oxidation product of [Mo(η(3)-C(3)H(5))Cl(CO)(2)(di-t-Bu-bipy)] (where di-t-Bu-bipy is 4,4'-di-tert-butyl-2,2'-bipyridine). A μ-oxide ligand bridges two similar MoCl(di-t-Bu-bipy)O(2) units, having the terminal oxide ligands mutually cis, and the chloride and μ-oxide trans to each other. In the binuclear complex, the coordination geometries of the metal atoms can be described as highly distorted octa-hedra. Individual complexes co-crystallize with a partially occupied water mol-ecule of crystallization (occupancy factor = 0.20; H atoms not located), with the crystal packing being mediated by the need to effectively fill the available space. A number of weak C-H⋯O and C-H⋯Cl inter-actions are present.

Related literature

For general background to dioxidomolybdenum(VI) com­plexes, see: Arzoumanian et al. (2006 ▶); Jeyakumar & Chand (2009 ▶); Kühn et al. (2002 ▶); Rodrigues et al. (2004 ▶). For studies on molybdenum complexes from our research groups, see: Coelho et al. (2011 ▶); Fernandes et al. (2011a ▶,b ▶, 2011 ▶); Gago et al. (2009 ▶); Nunes et al. (2003 ▶); Pereira et al. (2007 ▶).

Experimental

Crystal data

[Mo2Cl2O5(C18H24N2)2]·0.2H2O

M = 883.17

Monoclinic,

a = 16.9997 (7) Å

b = 12.7444 (6) Å

c = 18.4609 (8) Å

β = 99.582 (2)°

V = 3943.8 (3) Å3

Z = 4

Mo Kα radiation

μ = 0.82 mm−1

T = 150 K

0.08 × 0.06 × 0.03 mm

Data collection

Bruker X8 KappaCCD APEXII diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1997 ▶) T min = 0.938, T max = 0.976

54239 measured reflections

10578 independent reflections

7469 reflections with I > 2σ(I)

R int = 0.050

Refinement

R[F 2 > 2σ(F 2)] = 0.040

wR(F 2) = 0.086

S = 1.02

10578 reflections

463 parameters

18 restraints

H-atom parameters constrained

Δρmax = 0.96 e Å−3

Δρmin = −0.67 e Å−3

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT-Plus (Bruker, 2005 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 2009 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811046952/tk5013sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811046952/tk5013Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Mo2Cl2O5(C18H24N2)2]·0.2H2O	F(000) = 1808
Mr = 883.17	Dx = 1.487 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 9903 reflections
a = 16.9997 (7) Å	θ = 2.8–29.1°
b = 12.7444 (6) Å	µ = 0.82 mm−1
c = 18.4609 (8) Å	T = 150 K
β = 99.582 (2)°	Block, yellow
V = 3943.8 (3) Å3	0.08 × 0.06 × 0.03 mm
Z = 4

Bruker X8 KappaCCD APEXII diffractometer	10578 independent reflections
Radiation source: fine-focus sealed tube	7469 reflections with I > 2σ(I)
graphite	Rint = 0.050
ω and φ scans	θmax = 29.1°, θmin = 3.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −23→23
Tmin = 0.938, Tmax = 0.976	k = −16→17
54239 measured reflections	l = −24→25

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)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.086	H-atom parameters constrained
S = 1.02	w = 1/[σ2(Fo2) + (0.0315P)2 + 3.406P] where P = (Fo2 + 2Fc2)/3
10578 reflections	(Δ/σ)max = 0.001
463 parameters	Δρmax = 0.96 e Å−3
18 restraints	Δρmin = −0.67 e Å−3

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mo1	0.161140 (13)	0.78289 (2)	0.101763 (13)	0.02009 (7)
Mo2	0.153567 (14)	0.63578 (2)	−0.067460 (14)	0.02215 (7)
Cl1	0.16494 (4)	0.87386 (6)	0.22163 (4)	0.02652 (16)
Cl2	0.21012 (5)	0.51282 (7)	−0.14517 (4)	0.03473 (19)
N1	0.11178 (12)	0.65491 (18)	0.17242 (13)	0.0210 (5)
N2	0.02749 (13)	0.81233 (19)	0.10764 (13)	0.0213 (5)
N3	0.27507 (13)	0.59963 (19)	0.00696 (13)	0.0223 (5)
N4	0.14638 (12)	0.48235 (19)	−0.00290 (12)	0.0211 (5)
O1	0.12571 (10)	0.69242 (15)	0.02171 (10)	0.0224 (4)
O2	0.25605 (11)	0.73982 (17)	0.12818 (11)	0.0276 (5)
O3	0.16755 (12)	0.89784 (16)	0.05679 (12)	0.0311 (5)
O4	0.06091 (11)	0.61851 (17)	−0.11680 (11)	0.0297 (5)
O5	0.19330 (13)	0.74344 (18)	−0.10133 (12)	0.0360 (5)
C1	0.15948 (16)	0.5835 (2)	0.21063 (16)	0.0238 (6)
H1	0.2115	0.5743	0.1992	0.029*
C2	0.13739 (16)	0.5228 (2)	0.26543 (17)	0.0245 (6)
H2	0.1739	0.4736	0.2910	0.029*
C3	0.06192 (16)	0.5334 (2)	0.28335 (16)	0.0263 (7)
C4	0.01067 (16)	0.6030 (3)	0.23986 (17)	0.0297 (7)
H4	−0.0432	0.6088	0.2472	0.036*
C5	0.03666 (15)	0.6629 (2)	0.18700 (16)	0.0235 (6)
C6	−0.01214 (16)	0.7471 (2)	0.14631 (16)	0.0232 (6)
C7	−0.09241 (16)	0.7619 (3)	0.14974 (17)	0.0292 (7)
H7	−0.1198	0.7126	0.1751	0.035*
C8	−0.13296 (16)	0.8487 (3)	0.11624 (17)	0.0298 (7)
C9	−0.09027 (17)	0.9162 (3)	0.07927 (17)	0.0295 (7)
H9	−0.1152	0.9770	0.0561	0.035*
C10	−0.01101 (17)	0.8954 (2)	0.07589 (16)	0.0245 (6)
H10	0.0171	0.9427	0.0497	0.029*
C11	0.03393 (19)	0.4783 (3)	0.34808 (19)	0.0385 (8)
C12	0.0029 (3)	0.5616 (4)	0.3962 (2)	0.0777 (16)
H12A	0.0464	0.6095	0.4158	0.117*
H12B	−0.0172	0.5273	0.4370	0.117*
H12C	−0.0403	0.6013	0.3666	0.117*
C13	−0.0336 (2)	0.4023 (4)	0.3180 (2)	0.0666 (14)
H13A	−0.0763	0.4408	0.2868	0.100*
H13B	−0.0547	0.3701	0.3590	0.100*
H13C	−0.0129	0.3474	0.2890	0.100*
C14	0.1016 (2)	0.4186 (3)	0.3952 (2)	0.0461 (10)
H14A	0.1204	0.3627	0.3659	0.069*
H14B	0.0822	0.3878	0.4376	0.069*
H14C	0.1456	0.4669	0.4123	0.069*
C15	−0.22161 (17)	0.8645 (3)	0.1206 (2)	0.0397 (9)
C16	−0.2495 (2)	0.9713 (4)	0.0924 (4)	0.0971 (19)
H16A	−0.3076	0.9757	0.0886	0.146*
H16B	−0.2348	0.9824	0.0438	0.146*
H16C	−0.2243	1.0252	0.1264	0.146*
C17	−0.2693 (2)	0.7825 (4)	0.0698 (3)	0.0681 (13)
H17A	−0.2527	0.7118	0.0870	0.102*
H17B	−0.2590	0.7920	0.0195	0.102*
H17C	−0.3264	0.7914	0.0706	0.102*
C18	−0.2369 (3)	0.8407 (6)	0.1960 (3)	0.106 (2)
H18A	−0.2121	0.8948	0.2301	0.159*
H18B	−0.2142	0.7720	0.2115	0.159*
H18C	−0.2946	0.8397	0.1960	0.159*
C19	0.33976 (16)	0.6593 (2)	0.00679 (17)	0.0274 (7)
H19	0.3352	0.7203	−0.0232	0.033*
C20	0.41289 (16)	0.6358 (3)	0.04836 (17)	0.0279 (7)
H20	0.4572	0.6806	0.0465	0.033*
C21	0.42233 (15)	0.5476 (2)	0.09269 (16)	0.0241 (6)
C22	0.35406 (15)	0.4888 (2)	0.09491 (16)	0.0243 (6)
H22	0.3568	0.4295	0.1265	0.029*
C23	0.28184 (15)	0.5150 (2)	0.05182 (15)	0.0206 (6)
C24	0.20800 (15)	0.4519 (2)	0.04866 (15)	0.0209 (6)
C25	0.20205 (15)	0.3673 (2)	0.09379 (15)	0.0213 (6)
H25	0.2459	0.3494	0.1307	0.026*
C26	0.13233 (16)	0.3073 (2)	0.08606 (15)	0.0211 (6)
C27	0.07065 (16)	0.3385 (2)	0.03097 (16)	0.0234 (6)
H27	0.0223	0.2995	0.0223	0.028*
C28	0.07950 (15)	0.4252 (2)	−0.01084 (16)	0.0232 (6)
H28	0.0360	0.4457	−0.0473	0.028*
C29	0.50289 (16)	0.5150 (3)	0.13790 (18)	0.0304 (7)
C30	0.50366 (18)	0.5490 (3)	0.21771 (19)	0.0435 (9)
H30A	0.5534	0.5256	0.2481	0.065*
H30B	0.4582	0.5174	0.2359	0.065*
H30C	0.4999	0.6256	0.2201	0.065*
C31	0.57226 (17)	0.5677 (3)	0.1089 (2)	0.0420 (9)
H31A	0.5688	0.6439	0.1147	0.063*
H31B	0.5696	0.5505	0.0568	0.063*
H31C	0.6229	0.5423	0.1367	0.063*
C32	0.51307 (18)	0.3958 (3)	0.1352 (2)	0.0428 (9)
H32A	0.5029	0.3722	0.0840	0.064*
H32B	0.4752	0.3619	0.1624	0.064*
H32C	0.5676	0.3770	0.1575	0.064*
C33	0.12703 (17)	0.2135 (2)	0.13614 (16)	0.0260 (6)
C34	0.1347 (2)	0.2522 (3)	0.21501 (17)	0.0394 (9)
H34A	0.1857	0.2888	0.2288	0.059*
H34B	0.1325	0.1923	0.2479	0.059*
H34C	0.0908	0.3006	0.2192	0.059*
C35	0.04774 (18)	0.1555 (3)	0.11683 (17)	0.0319 (7)
H35A	0.0043	0.2012	0.1265	0.048*
H35B	0.0490	0.0919	0.1469	0.048*
H35C	0.0391	0.1362	0.0647	0.048*
C36	0.1950 (2)	0.1374 (3)	0.1283 (2)	0.0459 (9)
H36A	0.1899	0.1143	0.0771	0.069*
H36B	0.1922	0.0763	0.1601	0.069*
H36C	0.2464	0.1729	0.1428	0.069*
O1W	−0.1847 (9)	0.6639 (13)	0.2975 (10)	0.078 (5)	0.20

	U11	U22	U33	U12	U13	U23
Mo1	0.01580 (10)	0.02716 (14)	0.01656 (13)	−0.00222 (10)	0.00054 (8)	−0.00064 (11)
Mo2	0.02064 (11)	0.02864 (15)	0.01613 (13)	0.00094 (10)	0.00001 (9)	0.00249 (11)
Cl1	0.0231 (3)	0.0348 (4)	0.0201 (4)	−0.0005 (3)	−0.0010 (3)	−0.0053 (3)
Cl2	0.0354 (4)	0.0461 (5)	0.0232 (4)	0.0068 (4)	0.0064 (3)	−0.0019 (4)
N1	0.0157 (10)	0.0261 (14)	0.0201 (13)	−0.0015 (9)	0.0001 (9)	−0.0008 (10)
N2	0.0193 (11)	0.0258 (14)	0.0169 (13)	0.0015 (9)	−0.0026 (9)	−0.0009 (10)
N3	0.0197 (11)	0.0278 (14)	0.0197 (13)	−0.0008 (10)	0.0042 (9)	−0.0008 (10)
N4	0.0175 (10)	0.0289 (14)	0.0150 (12)	−0.0024 (9)	−0.0030 (9)	0.0006 (10)
O1	0.0183 (9)	0.0286 (12)	0.0188 (11)	0.0011 (8)	−0.0015 (8)	−0.0022 (8)
O2	0.0177 (9)	0.0421 (13)	0.0222 (11)	−0.0017 (9)	0.0009 (8)	−0.0067 (9)
O3	0.0377 (12)	0.0301 (12)	0.0259 (12)	−0.0038 (9)	0.0067 (10)	0.0005 (9)
O4	0.0260 (10)	0.0400 (13)	0.0199 (11)	0.0023 (9)	−0.0052 (8)	−0.0001 (9)
O5	0.0374 (12)	0.0373 (14)	0.0332 (13)	−0.0015 (10)	0.0059 (10)	0.0100 (11)
C1	0.0184 (12)	0.0276 (17)	0.0244 (16)	0.0005 (11)	0.0008 (11)	−0.0013 (13)
C2	0.0202 (13)	0.0260 (16)	0.0257 (17)	0.0038 (11)	−0.0011 (12)	0.0026 (13)
C3	0.0223 (13)	0.0332 (18)	0.0221 (16)	0.0011 (12)	0.0001 (12)	0.0064 (13)
C4	0.0164 (13)	0.043 (2)	0.0296 (18)	0.0021 (12)	0.0049 (12)	0.0090 (14)
C5	0.0167 (12)	0.0327 (17)	0.0204 (15)	−0.0003 (11)	0.0008 (11)	0.0024 (13)
C6	0.0195 (13)	0.0300 (17)	0.0189 (15)	0.0008 (11)	−0.0007 (11)	0.0022 (12)
C7	0.0168 (13)	0.044 (2)	0.0259 (17)	0.0010 (13)	0.0016 (12)	0.0048 (14)
C8	0.0201 (13)	0.043 (2)	0.0248 (17)	0.0051 (13)	−0.0012 (12)	−0.0036 (14)
C9	0.0282 (15)	0.0311 (18)	0.0256 (17)	0.0071 (13)	−0.0059 (13)	0.0003 (14)
C10	0.0277 (14)	0.0245 (16)	0.0189 (16)	−0.0003 (12)	−0.0032 (12)	−0.0014 (12)
C11	0.0338 (17)	0.051 (2)	0.033 (2)	0.0093 (16)	0.0107 (14)	0.0173 (17)
C12	0.107 (4)	0.090 (4)	0.047 (3)	0.053 (3)	0.043 (3)	0.033 (3)
C13	0.0322 (19)	0.099 (4)	0.070 (3)	−0.011 (2)	0.0104 (19)	0.048 (3)
C14	0.0408 (19)	0.058 (3)	0.040 (2)	0.0081 (17)	0.0077 (16)	0.0235 (19)
C15	0.0185 (14)	0.059 (2)	0.040 (2)	0.0117 (15)	0.0008 (13)	0.0013 (18)
C16	0.037 (2)	0.072 (3)	0.186 (6)	0.021 (2)	0.029 (3)	0.006 (4)
C17	0.0261 (17)	0.096 (4)	0.083 (3)	−0.005 (2)	0.0089 (19)	−0.006 (3)
C18	0.048 (2)	0.219 (6)	0.056 (3)	0.055 (3)	0.023 (2)	0.010 (4)
C19	0.0246 (14)	0.0271 (17)	0.0318 (18)	0.0008 (12)	0.0084 (13)	0.0010 (14)
C20	0.0179 (13)	0.0360 (18)	0.0302 (18)	−0.0029 (12)	0.0057 (12)	−0.0050 (14)
C21	0.0188 (13)	0.0330 (18)	0.0198 (16)	0.0008 (12)	0.0013 (11)	−0.0062 (13)
C22	0.0201 (13)	0.0294 (17)	0.0230 (16)	0.0016 (12)	0.0025 (11)	−0.0003 (13)
C23	0.0175 (12)	0.0281 (16)	0.0160 (15)	0.0000 (11)	0.0020 (10)	−0.0008 (12)
C24	0.0186 (12)	0.0260 (16)	0.0163 (15)	−0.0006 (11)	−0.0024 (10)	−0.0034 (12)
C25	0.0201 (12)	0.0250 (16)	0.0166 (14)	−0.0008 (11)	−0.0033 (11)	0.0003 (12)
C26	0.0221 (13)	0.0240 (16)	0.0161 (15)	−0.0014 (11)	0.0000 (11)	−0.0022 (12)
C27	0.0204 (13)	0.0268 (17)	0.0212 (16)	−0.0040 (11)	−0.0018 (11)	−0.0022 (12)
C28	0.0189 (12)	0.0306 (17)	0.0178 (15)	−0.0008 (11)	−0.0039 (11)	−0.0023 (13)
C29	0.0168 (13)	0.045 (2)	0.0282 (18)	0.0030 (13)	0.0011 (12)	−0.0047 (15)
C30	0.0240 (15)	0.072 (3)	0.031 (2)	0.0066 (16)	−0.0046 (14)	−0.0089 (18)
C31	0.0182 (14)	0.064 (3)	0.043 (2)	0.0004 (15)	0.0031 (14)	0.0020 (19)
C32	0.0232 (15)	0.052 (2)	0.051 (2)	0.0094 (15)	−0.0012 (15)	−0.0005 (18)
C33	0.0273 (14)	0.0306 (17)	0.0182 (15)	−0.0062 (13)	−0.0013 (11)	0.0023 (13)
C34	0.0481 (19)	0.046 (2)	0.0210 (18)	−0.0263 (16)	−0.0025 (15)	−0.0002 (15)
C35	0.0388 (17)	0.0327 (19)	0.0199 (17)	−0.0130 (14)	−0.0075 (13)	0.0037 (14)
C36	0.0426 (19)	0.034 (2)	0.060 (3)	0.0063 (16)	0.0040 (18)	0.0164 (18)
O1W	0.055 (9)	0.079 (12)	0.105 (14)	−0.006 (8)	0.029 (9)	0.015 (10)

Mo1—O1	1.8920 (19)	C15—C17	1.541 (5)
Mo1—O2	1.6972 (19)	C16—H16A	0.9800
Mo1—O3	1.696 (2)	C16—H16B	0.9800
Mo1—N1	2.330 (2)	C16—H16C	0.9800
Mo1—N2	2.323 (2)	C17—H17A	0.9800
Mo1—Cl1	2.4895 (8)	C17—H17B	0.9800
Mo2—O1	1.9274 (19)	C17—H17C	0.9800
Mo2—O4	1.6975 (19)	C18—H18A	0.9800
Mo2—O5	1.694 (2)	C18—H18B	0.9800
Mo2—N3	2.328 (2)	C18—H18C	0.9800
Mo2—N4	2.304 (2)	C19—C20	1.381 (4)
Mo2—Cl2	2.4283 (8)	C19—H19	0.9500
N1—C1	1.339 (3)	C20—C21	1.384 (4)
N1—C5	1.352 (3)	C20—H20	0.9500
N2—C10	1.329 (4)	C21—C22	1.388 (4)
N2—C6	1.347 (4)	C21—C29	1.537 (4)
N3—C19	1.337 (4)	C22—C23	1.388 (4)
N3—C23	1.353 (4)	C22—H22	0.9500
N4—C28	1.338 (3)	C23—C24	1.484 (4)
N4—C24	1.350 (3)	C24—C25	1.377 (4)
C1—C2	1.375 (4)	C25—C26	1.397 (4)
C1—H1	0.9500	C25—H25	0.9500
C2—C3	1.384 (4)	C26—C27	1.391 (4)
C2—H2	0.9500	C26—C33	1.523 (4)
C3—C4	1.399 (4)	C27—C28	1.371 (4)
C3—C11	1.529 (4)	C27—H27	0.9500
C4—C5	1.369 (4)	C28—H28	0.9500
C4—H4	0.9500	C29—C31	1.529 (4)
C5—C6	1.482 (4)	C29—C32	1.531 (5)
C6—C7	1.389 (4)	C29—C30	1.534 (5)
C7—C8	1.393 (4)	C30—H30A	0.9800
C7—H7	0.9500	C30—H30B	0.9800
C8—C9	1.378 (4)	C30—H30C	0.9800
C8—C15	1.536 (4)	C31—H31A	0.9800
C9—C10	1.385 (4)	C31—H31B	0.9800
C9—H9	0.9500	C31—H31C	0.9800
C10—H10	0.9500	C32—H32A	0.9800
C11—C14	1.524 (4)	C32—H32B	0.9800
C11—C13	1.533 (5)	C32—H32C	0.9800
C11—C12	1.534 (6)	C33—C34	1.522 (4)
C12—H12A	0.9800	C33—C35	1.526 (4)
C12—H12B	0.9800	C33—C36	1.534 (4)
C12—H12C	0.9800	C34—H34A	0.9800
C13—H13A	0.9800	C34—H34B	0.9800
C13—H13B	0.9800	C34—H34C	0.9800
C13—H13C	0.9800	C35—H35A	0.9800
C14—H14A	0.9800	C35—H35B	0.9800
C14—H14B	0.9800	C35—H35C	0.9800
C14—H14C	0.9800	C36—H36A	0.9800
C15—C18	1.490 (6)	C36—H36B	0.9800
C15—C16	1.504 (6)	C36—H36C	0.9800
O3—Mo1—O2	106.53 (10)	C18—C15—C17	105.9 (4)
O3—Mo1—O1	100.49 (9)	C16—C15—C17	107.4 (4)
O2—Mo1—O1	101.02 (9)	C8—C15—C17	107.5 (3)
O3—Mo1—N2	91.51 (9)	C15—C16—H16A	109.5
O2—Mo1—N2	158.31 (9)	C15—C16—H16B	109.5
O1—Mo1—N2	87.03 (8)	H16A—C16—H16B	109.5
O3—Mo1—N1	159.54 (9)	C15—C16—H16C	109.5
O2—Mo1—N1	91.52 (9)	H16A—C16—H16C	109.5
O1—Mo1—N1	85.02 (8)	H16B—C16—H16C	109.5
N2—Mo1—N1	68.95 (8)	C15—C17—H17A	109.5
O3—Mo1—Cl1	92.21 (8)	C15—C17—H17B	109.5
O2—Mo1—Cl1	90.71 (7)	H17A—C17—H17B	109.5
O1—Mo1—Cl1	159.37 (6)	C15—C17—H17C	109.5
N2—Mo1—Cl1	76.36 (6)	H17A—C17—H17C	109.5
N1—Mo1—Cl1	77.70 (6)	H17B—C17—H17C	109.5
O5—Mo2—O4	107.35 (10)	C15—C18—H18A	109.5
O5—Mo2—O1	100.46 (10)	C15—C18—H18B	109.5
O4—Mo2—O1	99.73 (9)	H18A—C18—H18B	109.5
O5—Mo2—N4	159.56 (9)	C15—C18—H18C	109.5
O4—Mo2—N4	92.48 (9)	H18A—C18—H18C	109.5
O1—Mo2—N4	80.46 (8)	H18B—C18—H18C	109.5
O5—Mo2—N3	90.52 (9)	N3—C19—C20	122.7 (3)
O4—Mo2—N3	160.69 (9)	N3—C19—H19	118.7
O1—Mo2—N3	83.69 (8)	C20—C19—H19	118.7
N4—Mo2—N3	69.21 (8)	C19—C20—C21	120.7 (3)
O5—Mo2—Cl2	94.77 (8)	C19—C20—H20	119.7
O4—Mo2—Cl2	91.29 (7)	C21—C20—H20	119.7
O1—Mo2—Cl2	157.51 (6)	C20—C21—C22	116.2 (3)
N4—Mo2—Cl2	79.53 (6)	C20—C21—C29	123.0 (3)
N3—Mo2—Cl2	79.71 (6)	C22—C21—C29	120.8 (3)
C1—N1—C5	117.1 (2)	C21—C22—C23	121.1 (3)
C1—N1—Mo1	121.85 (18)	C21—C22—H22	119.4
C5—N1—Mo1	119.91 (18)	C23—C22—H22	119.4
C10—N2—C6	118.2 (2)	N3—C23—C22	121.3 (3)
C10—N2—Mo1	121.46 (19)	N3—C23—C24	115.0 (2)
C6—N2—Mo1	120.28 (18)	C22—C23—C24	123.6 (3)
C19—N3—C23	117.9 (2)	N4—C24—C25	121.7 (2)
C19—N3—Mo2	122.4 (2)	N4—C24—C23	115.1 (2)
C23—N3—Mo2	119.71 (17)	C25—C24—C23	123.2 (2)
C28—N4—C24	117.8 (2)	C24—C25—C26	120.9 (2)
C28—N4—Mo2	121.53 (18)	C24—C25—H25	119.6
C24—N4—Mo2	120.46 (18)	C26—C25—H25	119.6
Mo1—O1—Mo2	143.50 (10)	C27—C26—C25	116.2 (3)
N1—C1—C2	123.7 (3)	C27—C26—C33	123.6 (2)
N1—C1—H1	118.2	C25—C26—C33	120.1 (2)
C2—C1—H1	118.2	C28—C27—C26	120.1 (3)
C1—C2—C3	119.9 (3)	C28—C27—H27	119.9
C1—C2—H2	120.0	C26—C27—H27	119.9
C3—C2—H2	120.0	N4—C28—C27	123.3 (3)
C2—C3—C4	116.0 (3)	N4—C28—H28	118.4
C2—C3—C11	124.3 (3)	C27—C28—H28	118.4
C4—C3—C11	119.6 (3)	C31—C29—C32	109.0 (3)
C5—C4—C3	121.2 (3)	C31—C29—C30	109.2 (3)
C5—C4—H4	119.4	C32—C29—C30	109.2 (3)
C3—C4—H4	119.4	C31—C29—C21	111.2 (3)
N1—C5—C4	121.8 (3)	C32—C29—C21	110.2 (3)
N1—C5—C6	114.9 (2)	C30—C29—C21	108.1 (2)
C4—C5—C6	123.0 (3)	C29—C30—H30A	109.5
N2—C6—C7	121.4 (3)	C29—C30—H30B	109.5
N2—C6—C5	115.4 (2)	H30A—C30—H30B	109.5
C7—C6—C5	123.1 (3)	C29—C30—H30C	109.5
C6—C7—C8	120.3 (3)	H30A—C30—H30C	109.5
C6—C7—H7	119.8	H30B—C30—H30C	109.5
C8—C7—H7	119.8	C29—C31—H31A	109.5
C9—C8—C7	117.0 (3)	C29—C31—H31B	109.5
C9—C8—C15	123.1 (3)	H31A—C31—H31B	109.5
C7—C8—C15	119.9 (3)	C29—C31—H31C	109.5
C8—C9—C10	120.0 (3)	H31A—C31—H31C	109.5
C8—C9—H9	120.0	H31B—C31—H31C	109.5
C10—C9—H9	120.0	C29—C32—H32A	109.5
N2—C10—C9	123.0 (3)	C29—C32—H32B	109.5
N2—C10—H10	118.5	H32A—C32—H32B	109.5
C9—C10—H10	118.5	C29—C32—H32C	109.5
C14—C11—C3	111.8 (3)	H32A—C32—H32C	109.5
C14—C11—C13	109.9 (3)	H32B—C32—H32C	109.5
C3—C11—C13	108.6 (3)	C34—C33—C26	108.7 (3)
C14—C11—C12	108.4 (3)	C34—C33—C35	108.2 (3)
C3—C11—C12	108.5 (3)	C26—C33—C35	112.2 (2)
C13—C11—C12	109.8 (3)	C34—C33—C36	110.4 (3)
C11—C12—H12A	109.5	C26—C33—C36	108.5 (3)
C11—C12—H12B	109.5	C35—C33—C36	108.8 (3)
H12A—C12—H12B	109.5	C33—C34—H34A	109.5
C11—C12—H12C	109.5	C33—C34—H34B	109.5
H12A—C12—H12C	109.5	H34A—C34—H34B	109.5
H12B—C12—H12C	109.5	C33—C34—H34C	109.5
C11—C13—H13A	109.5	H34A—C34—H34C	109.5
C11—C13—H13B	109.5	H34B—C34—H34C	109.5
H13A—C13—H13B	109.5	C33—C35—H35A	109.5
C11—C13—H13C	109.5	C33—C35—H35B	109.5
H13A—C13—H13C	109.5	H35A—C35—H35B	109.5
H13B—C13—H13C	109.5	C33—C35—H35C	109.5
C11—C14—H14A	109.5	H35A—C35—H35C	109.5
C11—C14—H14B	109.5	H35B—C35—H35C	109.5
H14A—C14—H14B	109.5	C33—C36—H36A	109.5
C11—C14—H14C	109.5	C33—C36—H36B	109.5
H14A—C14—H14C	109.5	H36A—C36—H36B	109.5
H14B—C14—H14C	109.5	C33—C36—H36C	109.5
C18—C15—C16	114.4 (4)	H36A—C36—H36C	109.5
C18—C15—C8	110.3 (3)	H36B—C36—H36C	109.5
C16—C15—C8	110.9 (3)
O3—Mo1—N1—C1	−154.4 (3)	N1—C5—C6—N2	−8.0 (4)
O2—Mo1—N1—C1	−2.2 (2)	C4—C5—C6—N2	166.9 (3)
O1—Mo1—N1—C1	98.8 (2)	N1—C5—C6—C7	174.8 (3)
N2—Mo1—N1—C1	−172.5 (2)	C4—C5—C6—C7	−10.3 (5)
Cl1—Mo1—N1—C1	−92.6 (2)	N2—C6—C7—C8	−3.5 (5)
O3—Mo1—N1—C5	13.1 (4)	C5—C6—C7—C8	173.5 (3)
O2—Mo1—N1—C5	165.3 (2)	C6—C7—C8—C9	1.2 (5)
O1—Mo1—N1—C5	−93.7 (2)	C6—C7—C8—C15	−179.8 (3)
N2—Mo1—N1—C5	−5.0 (2)	C7—C8—C9—C10	0.8 (5)
Cl1—Mo1—N1—C5	74.9 (2)	C15—C8—C9—C10	−178.2 (3)
O3—Mo1—N2—C10	3.8 (2)	C6—N2—C10—C9	−1.7 (4)
O2—Mo1—N2—C10	150.5 (3)	Mo1—N2—C10—C9	−179.0 (2)
O1—Mo1—N2—C10	−96.7 (2)	C8—C9—C10—N2	−0.6 (5)
N1—Mo1—N2—C10	177.5 (2)	C2—C3—C11—C14	5.6 (5)
Cl1—Mo1—N2—C10	95.7 (2)	C4—C3—C11—C14	−171.7 (3)
O3—Mo1—N2—C6	−173.5 (2)	C2—C3—C11—C13	−115.8 (4)
O2—Mo1—N2—C6	−26.7 (4)	C4—C3—C11—C13	67.0 (4)
O1—Mo1—N2—C6	86.1 (2)	C2—C3—C11—C12	125.0 (4)
N1—Mo1—N2—C6	0.3 (2)	C4—C3—C11—C12	−52.2 (4)
Cl1—Mo1—N2—C6	−81.6 (2)	C9—C8—C15—C18	−138.6 (4)
O5—Mo2—N3—C19	−1.0 (2)	C7—C8—C15—C18	42.5 (5)
O4—Mo2—N3—C19	157.1 (3)	C9—C8—C15—C16	−10.8 (5)
O1—Mo2—N3—C19	−101.5 (2)	C7—C8—C15—C16	170.3 (4)
N4—Mo2—N3—C19	176.4 (2)	C9—C8—C15—C17	106.4 (4)
Cl2—Mo2—N3—C19	93.7 (2)	C7—C8—C15—C17	−72.6 (4)
O5—Mo2—N3—C23	179.7 (2)	C23—N3—C19—C20	2.2 (4)
O4—Mo2—N3—C23	−22.2 (4)	Mo2—N3—C19—C20	−177.1 (2)
O1—Mo2—N3—C23	79.2 (2)	N3—C19—C20—C21	0.1 (5)
N4—Mo2—N3—C23	−3.0 (2)	C19—C20—C21—C22	−2.8 (4)
Cl2—Mo2—N3—C23	−85.6 (2)	C19—C20—C21—C29	177.6 (3)
O5—Mo2—N4—C28	−171.6 (3)	C20—C21—C22—C23	3.2 (4)
O4—Mo2—N4—C28	−5.4 (2)	C29—C21—C22—C23	−177.2 (3)
O1—Mo2—N4—C28	94.0 (2)	C19—N3—C23—C22	−1.8 (4)
N3—Mo2—N4—C28	−179.2 (2)	Mo2—N3—C23—C22	177.6 (2)
Cl2—Mo2—N4—C28	−96.3 (2)	C19—N3—C23—C24	−179.5 (3)
O5—Mo2—N4—C24	13.8 (4)	Mo2—N3—C23—C24	−0.1 (3)
O4—Mo2—N4—C24	179.9 (2)	C21—C22—C23—N3	−1.0 (4)
O1—Mo2—N4—C24	−80.6 (2)	C21—C22—C23—C24	176.5 (3)
N3—Mo2—N4—C24	6.2 (2)	C28—N4—C24—C25	−2.3 (4)
Cl2—Mo2—N4—C24	89.1 (2)	Mo2—N4—C24—C25	172.5 (2)
O3—Mo1—O1—Mo2	60.75 (19)	C28—N4—C24—C23	176.7 (2)
O2—Mo1—O1—Mo2	−48.57 (19)	Mo2—N4—C24—C23	−8.5 (3)
N2—Mo1—O1—Mo2	151.74 (18)	N3—C23—C24—N4	5.4 (4)
N1—Mo1—O1—Mo2	−139.15 (18)	C22—C23—C24—N4	−172.2 (3)
Cl1—Mo1—O1—Mo2	−172.16 (6)	N3—C23—C24—C25	−175.6 (3)
O5—Mo2—O1—Mo1	−40.34 (19)	C22—C23—C24—C25	6.8 (4)
O4—Mo2—O1—Mo1	−150.18 (18)	N4—C24—C25—C26	2.1 (4)
N4—Mo2—O1—Mo1	118.93 (18)	C23—C24—C25—C26	−176.8 (3)
N3—Mo2—O1—Mo1	49.02 (18)	C24—C25—C26—C27	−0.1 (4)
Cl2—Mo2—O1—Mo1	91.5 (2)	C24—C25—C26—C33	179.6 (3)
C5—N1—C1—C2	−3.3 (4)	C25—C26—C27—C28	−1.7 (4)
Mo1—N1—C1—C2	164.5 (2)	C33—C26—C27—C28	178.7 (3)
N1—C1—C2—C3	0.4 (5)	C24—N4—C28—C27	0.5 (4)
C1—C2—C3—C4	3.8 (4)	Mo2—N4—C28—C27	−174.3 (2)
C1—C2—C3—C11	−173.6 (3)	C26—C27—C28—N4	1.5 (5)
C2—C3—C4—C5	−5.2 (5)	C20—C21—C29—C31	−18.8 (4)
C11—C3—C4—C5	172.3 (3)	C22—C21—C29—C31	161.6 (3)
C1—N1—C5—C4	1.8 (4)	C20—C21—C29—C32	−139.8 (3)
Mo1—N1—C5—C4	−166.3 (2)	C22—C21—C29—C32	40.6 (4)
C1—N1—C5—C6	176.7 (2)	C20—C21—C29—C30	101.0 (4)
Mo1—N1—C5—C6	8.6 (3)	C22—C21—C29—C30	−78.6 (4)
C3—C4—C5—N1	2.6 (5)	C27—C26—C33—C34	−117.4 (3)
C3—C4—C5—C6	−172.0 (3)	C25—C26—C33—C34	62.9 (3)
C10—N2—C6—C7	3.7 (4)	C27—C26—C33—C35	2.2 (4)
Mo1—N2—C6—C7	−178.9 (2)	C25—C26—C33—C35	−177.4 (3)
C10—N2—C6—C5	−173.5 (2)	C27—C26—C33—C36	122.4 (3)
Mo1—N2—C6—C5	3.8 (3)	C25—C26—C33—C36	−57.2 (4)

D—H···A	D—H	H···A	D···A	D—H···A
C27—H27···O1i	0.95	2.52	3.341 (3)	145
C34—H34A···Cl1ii	0.98	2.77	3.748 (4)	174
C35—H35A···O4i	0.98	2.54	3.421 (4)	149
C12—H12C···O1W	0.98	2.69	3.641 (16)	163
C18—H18B···O1W	0.98	2.10	2.970 (18)	147
O1W—···.Cl2i	.	.	3.573 (18)	.
O1W—···.O5iii	.	.	3.236 (17)	.

Table 1

Selected bond lengths (Å)

Mo1—O1	1.8920 (19)
Mo1—O2	1.6972 (19)
Mo1—O3	1.696 (2)
Mo1—N1	2.330 (2)
Mo1—N2	2.323 (2)
Mo1—Cl1	2.4895 (8)
Mo2—O1	1.9274 (19)
Mo2—O4	1.6975 (19)
Mo2—O5	1.694 (2)
Mo2—N3	2.328 (2)
Mo2—N4	2.304 (2)
Mo2—Cl2	2.4283 (8)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C27—H27⋯O1i	0.95	2.52	3.341 (3)	145
C34—H34A⋯Cl1ii	0.98	2.77	3.748 (4)	174
C35—H35A⋯O4i	0.98	2.54	3.421 (4)	149
C12—H12C⋯O1W	0.98	2.69	3.641 (16)	163
C18—H18B⋯O1W	0.98	2.10	2.970 (18)	147
O1W⋯Cl2i			3.573 (18)
O1W⋯O5iii			3.236 (17)

Symmetry codes: (i) ; (ii) ; (iii) .