Literature DB >> 21587767

Tripyridinium cis-tetra-chlorido-dioxido-molybdate(VI) chloride.

José A Fernandes, Ana C Gomes, Sónia Figueiredo, Sandra Gago, Paulo J A Ribeiro-Claro, Isabel S Gonçalves, Filipe A Almeida Paz.   

Abstract

In the title compound, (C(5)H(6)N)(3)[MoCl(4)O(2)]Cl, the pyridinium cations are N-H⋯Cl hydrogen bonded to the anionic [MoCl(4)O(2)](2-) complexes and to the two crystallographically independent chloride anions (located on C2 axes). The Mo(6+) centre adopts a highly distorted octa-hedral geometry, being surrounded by four chloride and two terminal oxide groups. The oxide ligands are mutually cis.

Entities:  

Year:  2010        PMID： 21587767      PMCID： PMC3006702          DOI： 10.1107/S1600536810023950

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For a related structure, see: Luan et al. (2008 ▶). For previous studies by our group on dioxidomolybdenum complexes, see: Monteiro et al. (2010 ▶); Gago et al. (2009 ▶); Pereira et al. (2007 ▶); Cunha-Silva et al. (2007 ▶); Bruno et al. (2007 ▶). For graph-set notation for hydrogen-bonded aggregates, see: Grell et al. (1999 ▶). For a description of the Cambridge Structural Database, see: Allen (2002 ▶).

Experimental

Crystal data

(C5H6N)3[MoCl4O2]Cl M = 545.51 Trigonal, a = 11.3972 (2) Å c = 29.4265 (9) Å V = 3310.28 (13) Å3 Z = 6 Mo Kα radiation μ = 1.21 mm−1 T = 150 K 0.18 × 0.12 × 0.10 mm

Data collection

Bruker X8 Kappa CCD APEXII diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1998 ▶) T min = 0.811, T max = 0.888 33230 measured reflections 10395 independent reflections 8105 reflections with I > 2σ(I) R int = 0.047

Refinement

R[F 2 > 2σ(F 2)] = 0.038 wR(F 2) = 0.074 S = 1.05 10395 reflections 237 parameters H-atom parameters constrained Δρmax = 0.46 e Å−3 Δρmin = −0.68 e Å−3 Absolute structure: Flack (1983 ▶), 4490 Friedel pairs Flack parameter: 0.03 (4) 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, 2006 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810023950/sj5018sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810023950/sj5018Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C5H6N)3[MoCl4O2]ClDx = 1.642 Mg m−3
Mr = 545.51Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3121Cell parameters from 6207 reflections
Hall symbol: P 31 2"θ = 5.5–33.1°
a = 11.3972 (2) ŵ = 1.21 mm−1
c = 29.4265 (9) ÅT = 150 K
V = 3310.28 (13) Å3Block, yellow
Z = 60.18 × 0.12 × 0.10 mm
F(000) = 1632
Bruker X8 Kappa CCD APEXII diffractometer10395 independent reflections
Radiation source: fine-focus sealed tube8105 reflections with I > 2σ(I)
graphiteRint = 0.047
ω & φ scansθmax = 36.3°, θmin = 5.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1998)h = −18→16
Tmin = 0.811, Tmax = 0.888k = −17→8
33230 measured reflectionsl = −48→49
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.038H-atom parameters constrained
wR(F2) = 0.074w = 1/[σ2(Fo2) + (0.0224P)2 + 0.183P] where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.003
10395 reflectionsΔρmax = 0.46 e Å−3
237 parametersΔρmin = −0.68 e Å−3
0 restraintsAbsolute structure: Flack (1983), 4490 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.03 (4)
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.
xyzUiso*/Ueq
Mo10.663054 (16)0.338004 (17)0.915715 (4)0.01643 (3)
O10.77729 (15)0.39544 (18)0.87246 (4)0.0238 (3)
O20.76505 (15)0.38526 (17)0.96219 (4)0.0233 (3)
Cl10.64140 (7)0.53687 (6)0.916423 (17)0.02869 (12)
Cl20.62465 (7)0.11310 (6)0.914936 (17)0.02893 (12)
Cl30.47182 (5)0.25297 (6)0.856354 (14)0.02601 (11)
Cl40.45883 (5)0.24295 (6)0.971200 (14)0.02623 (11)
Cl51.00836 (8)0.00000.83330.0421 (2)
Cl60.94835 (8)0.94835 (8)0.00000.0352 (2)
N10.6973 (2)0.8428 (2)0.94054 (6)0.0266 (4)
H1A0.77260.87650.95640.032*
N20.1156 (2)0.8720 (2)0.89938 (5)0.0306 (4)
H2A0.09890.91610.87820.037*
N30.2586 (2)0.3111 (2)0.91300 (7)0.0333 (5)
H3A0.32990.30290.91860.040*
C10.5793 (3)0.7649 (3)0.96154 (7)0.0289 (5)
H10.57820.74490.99290.035*
C20.4601 (3)0.7139 (3)0.93800 (7)0.0304 (5)
H20.37590.65720.95260.037*
C30.4649 (3)0.7467 (3)0.89223 (7)0.0321 (5)
H30.38320.71540.87560.039*
C40.5876 (3)0.8244 (3)0.87119 (7)0.0313 (6)
H40.59160.84540.83980.038*
C50.7049 (3)0.8714 (3)0.89623 (7)0.0295 (5)
H50.79070.92390.88210.035*
C60.2380 (3)0.9313 (3)0.91843 (8)0.0335 (6)
H60.30641.01830.90850.040*
C70.2645 (3)0.8657 (3)0.95249 (8)0.0327 (6)
H70.35010.90820.96730.039*
C80.1656 (3)0.7374 (3)0.96502 (8)0.0345 (6)
H80.18330.69020.98820.041*
C90.0411 (3)0.6777 (3)0.94404 (8)0.0367 (6)
H9−0.02720.58870.95220.044*
C100.0168 (3)0.7481 (3)0.91116 (8)0.0345 (6)
H10−0.06930.70940.89690.041*
C110.1483 (3)0.2387 (3)0.93686 (7)0.0339 (6)
H110.14640.17750.95920.041*
C120.0362 (3)0.2502 (3)0.92996 (8)0.0361 (6)
H12−0.04340.19890.94750.043*
C130.0413 (3)0.3393 (3)0.89645 (9)0.0395 (6)
H13−0.03560.34870.89080.047*
C140.1574 (3)0.4132 (3)0.87173 (9)0.0389 (7)
H140.16180.47430.84900.047*
C150.2673 (3)0.3979 (3)0.88024 (8)0.0351 (6)
H150.34850.44780.86330.042*
U11U22U33U12U13U23
Mo10.01527 (8)0.01530 (8)0.01882 (5)0.00773 (7)0.00036 (5)0.00003 (5)
O10.0216 (7)0.0270 (9)0.0249 (5)0.0137 (7)0.0046 (5)0.0054 (6)
O20.0215 (7)0.0220 (9)0.0248 (5)0.0096 (7)−0.0042 (5)−0.0012 (6)
Cl10.0361 (3)0.0210 (3)0.0348 (2)0.0187 (3)−0.0008 (2)−0.0004 (2)
Cl20.0381 (4)0.0186 (3)0.0334 (2)0.0167 (3)0.0018 (2)−0.0006 (2)
Cl30.0213 (2)0.0335 (3)0.02208 (16)0.0128 (2)−0.00321 (16)−0.00294 (19)
Cl40.0216 (2)0.0311 (3)0.02295 (17)0.0109 (2)0.00463 (16)0.00273 (19)
Cl50.0355 (3)0.0628 (7)0.0371 (3)0.0314 (3)0.01181 (18)0.0236 (4)
Cl60.0300 (3)0.0300 (3)0.0359 (3)0.0077 (4)−0.00797 (16)0.00797 (16)
N10.0273 (10)0.0259 (11)0.0312 (7)0.0169 (10)−0.0071 (7)−0.0074 (8)
N20.0337 (13)0.0350 (13)0.0280 (7)0.0208 (10)−0.0009 (8)0.0038 (8)
N30.0245 (12)0.0311 (13)0.0480 (11)0.0166 (10)0.0007 (9)0.0044 (9)
C10.0393 (14)0.0348 (14)0.0213 (7)0.0250 (12)0.0004 (8)−0.0004 (8)
C20.0297 (12)0.0334 (14)0.0304 (9)0.0174 (11)0.0053 (8)−0.0008 (9)
C30.0338 (13)0.0349 (15)0.0303 (9)0.0192 (12)−0.0104 (8)−0.0087 (9)
C40.0473 (16)0.0272 (13)0.0220 (8)0.0206 (12)−0.0018 (9)−0.0011 (8)
C50.0323 (13)0.0228 (13)0.0340 (9)0.0141 (11)0.0068 (9)0.0018 (9)
C60.0337 (15)0.0233 (13)0.0389 (11)0.0108 (12)0.0003 (10)0.0010 (10)
C70.0234 (13)0.0319 (14)0.0363 (10)0.0091 (11)−0.0074 (9)−0.0007 (10)
C80.0315 (14)0.0366 (16)0.0336 (10)0.0157 (13)0.0005 (10)0.0110 (10)
C90.0247 (13)0.0299 (14)0.0458 (12)0.0064 (11)0.0035 (10)0.0090 (11)
C100.0224 (13)0.0401 (16)0.0370 (11)0.0126 (12)−0.0048 (10)−0.0032 (10)
C110.0409 (16)0.0288 (13)0.0285 (9)0.0148 (12)0.0000 (9)0.0074 (9)
C120.0300 (14)0.0321 (15)0.0416 (11)0.0122 (12)0.0131 (11)0.0031 (10)
C130.0250 (14)0.0436 (18)0.0508 (13)0.0178 (14)−0.0058 (11)−0.0029 (12)
C140.0353 (15)0.0410 (18)0.0414 (12)0.0200 (14)−0.0006 (11)0.0158 (12)
C150.0325 (15)0.0338 (16)0.0395 (11)0.0169 (13)0.0130 (10)0.0128 (10)
Mo1—O21.6988 (13)C4—C51.379 (4)
Mo1—O11.7004 (13)C4—H40.9500
Mo1—Cl22.3750 (6)C5—H50.9500
Mo1—Cl12.3995 (6)C6—C71.372 (4)
Mo1—Cl32.5746 (5)C6—H60.9500
Mo1—Cl42.5953 (5)C7—C81.377 (4)
N1—C11.335 (3)C7—H70.9500
N1—C51.336 (3)C8—C91.375 (4)
N1—H1A0.8800C8—H80.9500
N2—C61.332 (4)C9—C101.371 (4)
N2—C101.338 (4)C9—H90.9500
N2—H2A0.8800C10—H100.9500
N3—C111.310 (3)C11—C121.363 (4)
N3—C151.349 (3)C11—H110.9500
N3—H3A0.8800C12—C131.395 (4)
C1—C21.369 (3)C12—H120.9500
C1—H10.9500C13—C141.369 (4)
C2—C31.392 (3)C13—H130.9500
C2—H20.9500C14—C151.370 (4)
C3—C41.373 (4)C14—H140.9500
C3—H30.9500C15—H150.9500
O2—Mo1—O1102.11 (7)C5—C4—H4120.4
O2—Mo1—Cl294.45 (6)N1—C5—C4119.6 (2)
O1—Mo1—Cl295.78 (6)N1—C5—H5120.2
O2—Mo1—Cl194.06 (6)C4—C5—H5120.2
O1—Mo1—Cl193.64 (6)N2—C6—C7119.4 (3)
Cl2—Mo1—Cl1165.71 (2)N2—C6—H6120.3
O2—Mo1—Cl3169.07 (5)C7—C6—H6120.3
O1—Mo1—Cl388.75 (5)C6—C7—C8119.2 (3)
Cl2—Mo1—Cl385.57 (2)C6—C7—H7120.4
Cl1—Mo1—Cl383.91 (2)C8—C7—H7120.4
O2—Mo1—Cl487.40 (5)C9—C8—C7120.0 (2)
O1—Mo1—Cl4170.36 (5)C9—C8—H8120.0
Cl2—Mo1—Cl484.99 (2)C7—C8—H8120.0
Cl1—Mo1—Cl483.94 (2)C10—C9—C8119.2 (3)
Cl3—Mo1—Cl481.717 (16)C10—C9—H9120.4
C1—N1—C5122.4 (2)C8—C9—H9120.4
C1—N1—H1A118.8N2—C10—C9119.4 (2)
C5—N1—H1A118.8N2—C10—H10120.3
C6—N2—C10122.8 (2)C9—C10—H10120.3
C6—N2—H2A118.6N3—C11—C12120.6 (2)
C10—N2—H2A118.6N3—C11—H11119.7
C11—N3—C15122.7 (2)C12—C11—H11119.7
C11—N3—H3A118.6C11—C12—C13118.4 (3)
C15—N3—H3A118.6C11—C12—H12120.8
N1—C1—C2120.24 (19)C13—C12—H12120.8
N1—C1—H1119.9C14—C13—C12119.9 (3)
C2—C1—H1119.9C14—C13—H13120.0
C1—C2—C3118.6 (2)C12—C13—H13120.0
C1—C2—H2120.7C13—C14—C15119.2 (3)
C3—C2—H2120.7C13—C14—H14120.4
C4—C3—C2120.0 (2)C15—C14—H14120.4
C4—C3—H3120.0N3—C15—C14119.1 (3)
C2—C3—H3120.0N3—C15—H15120.4
C3—C4—C5119.14 (19)C14—C15—H15120.4
C3—C4—H4120.4
C5—N1—C1—C2−1.7 (4)C7—C8—C9—C10−0.9 (4)
N1—C1—C2—C3−1.0 (4)C6—N2—C10—C9−0.3 (4)
C1—C2—C3—C42.5 (4)C8—C9—C10—N21.6 (4)
C2—C3—C4—C5−1.5 (4)C15—N3—C11—C12−1.3 (4)
C1—N1—C5—C42.8 (4)N3—C11—C12—C131.0 (4)
C3—C4—C5—N1−1.1 (4)C11—C12—C13—C14−0.5 (4)
C10—N2—C6—C7−1.9 (4)C12—C13—C14—C150.2 (5)
N2—C6—C7—C82.6 (4)C11—N3—C15—C141.0 (4)
C6—C7—C8—C9−1.2 (4)C13—C14—C15—N3−0.5 (5)
D—H···AD—HH···AD···AD—H···A
N1—H1A···Cl6i0.882.163.0424 (19)175
N2—H2A···Cl5ii0.882.173.0304 (19)166
N3—H3A···Cl40.882.453.243 (2)150
N3—H3A···Cl30.882.693.277 (2)126
Mo1—O21.6988 (13)
Mo1—O11.7004 (13)
Mo1—Cl22.3750 (6)
Mo1—Cl12.3995 (6)
Mo1—Cl32.5746 (5)
Mo1—Cl42.5953 (5)
O2—Mo1—O1102.11 (7)
O2—Mo1—Cl294.45 (6)
O1—Mo1—Cl295.78 (6)
O2—Mo1—Cl194.06 (6)
O1—Mo1—Cl193.64 (6)
Cl2—Mo1—Cl1165.71 (2)
O2—Mo1—Cl3169.07 (5)
O1—Mo1—Cl388.75 (5)
Cl2—Mo1—Cl385.57 (2)
Cl1—Mo1—Cl383.91 (2)
O2—Mo1—Cl487.40 (5)
O1—Mo1—Cl4170.36 (5)
Cl2—Mo1—Cl484.99 (2)
Cl1—Mo1—Cl483.94 (2)
Cl3—Mo1—Cl481.717 (16)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
N1—H1A⋯Cl6i0.882.163.0424 (19)175
N2—H2A⋯Cl5ii0.882.173.0304 (19)166
N3—H3A⋯Cl40.882.453.243 (2)150
N3—H3A⋯Cl30.882.693.277 (2)126

Symmetry codes: (i) ; (ii) .

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Authors:  Frank H Allen
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3.  Graph-set analysis of hydrogen-bond patterns: some mathematical concepts.

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

Authors:  Ana C Gomes; José A Fernandes; Carla A Gamelas; Isabel S Gonçalves; Filipe A Almeida Paz
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