Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801016919/cf6112sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801016919/cf6112Isup2.hkl |
CCDC reference: 175974
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.050
- wR factor = 0.124
- Data-to-parameter ratio = 19.4
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_360 Alert C Short C(sp3)-C(sp3) Bond C6 - C7 = 1.41 Ang.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
A solution of H2MoO4 (4.86 g, 30 mmol) in 20 ml concentrated HCl and 20 ml water was stirred with N2H4·2HCl (0.75 g, 7.14 mmol) for about 1 h, resulting in a green mixture. [(C4H9)4N]Cl (2.77 g, 10 mmol) was added and the solution was filtered. Green crystals of the title compound formed after a few days.
H atoms on C atoms were generated geometrically. Aqua H atoms were clearly visible in different maps and were positioned geometrically and included in the structure-factor calculations as riding atoms with fixed isotropic displacement parameters.
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXLTL (Siemens, 1994); software used to prepare material for publication: SHELXL97.
Fig. 1. The cation and anion of (I) shown with 30% probability ellipsoids. | |
Fig. 2. Packing diagram of (I), viewed down the a axis. |
(C16H36N)[MoOCl4(H2O)] | F(000) = 1068 |
Mr = 514.21 | Dx = 1.374 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 9.401 (1) Å | Cell parameters from 3968 reflections |
b = 15.770 (1) Å | θ = 1.8–25.1° |
c = 16.845 (1) Å | µ = 0.97 mm−1 |
β = 95.581 (1)° | T = 293 K |
V = 2485.6 (2) Å3 | Prism, green |
Z = 4 | 0.45 × 0.20 × 0.10 mm |
SMART CCD diffractometer | 4368 independent reflections |
Radiation source: fine-focus sealed tube | 3157 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ϕ and ω scans | θmax = 25.1°, θmin = 1.8° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.644, Tmax = 0.908 | k = −13→18 |
8905 measured reflections | l = −20→13 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.050 | H-atom parameters constrained |
wR(F2) = 0.124 | w = 1/[σ2(Fo2) + (0.0375P)2 + 3.4179P] where P = (Fo2 + 2Fc2)/3 |
S = 1.15 | (Δ/σ)max < 0.001 |
4368 reflections | Δρmax = 0.54 e Å−3 |
225 parameters | Δρmin = −0.45 e Å−3 |
3 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0010 (3) |
(C16H36N)[MoOCl4(H2O)] | V = 2485.6 (2) Å3 |
Mr = 514.21 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 9.401 (1) Å | µ = 0.97 mm−1 |
b = 15.770 (1) Å | T = 293 K |
c = 16.845 (1) Å | 0.45 × 0.20 × 0.10 mm |
β = 95.581 (1)° |
SMART CCD diffractometer | 4368 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 3157 reflections with I > 2σ(I) |
Tmin = 0.644, Tmax = 0.908 | Rint = 0.033 |
8905 measured reflections |
R[F2 > 2σ(F2)] = 0.050 | 3 restraints |
wR(F2) = 0.124 | H-atom parameters constrained |
S = 1.15 | Δρmax = 0.54 e Å−3 |
4368 reflections | Δρmin = −0.45 e Å−3 |
225 parameters |
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 | ||
Mo | 0.90088 (5) | 0.37397 (3) | 0.87363 (3) | 0.05693 (18) | |
Cl1 | 0.80082 (17) | 0.38097 (10) | 0.99793 (9) | 0.0809 (4) | |
Cl2 | 0.99286 (18) | 0.23966 (9) | 0.91145 (10) | 0.0829 (5) | |
Cl3 | 0.86824 (16) | 0.52455 (8) | 0.86015 (8) | 0.0702 (4) | |
Cl4 | 1.06195 (17) | 0.38032 (9) | 0.77485 (8) | 0.0771 (4) | |
O | 0.7560 (4) | 0.3452 (3) | 0.8173 (2) | 0.0838 (12) | |
OW | 1.1030 (4) | 0.4205 (2) | 0.9538 (2) | 0.0684 (10) | |
HW1 | 1.1310 | 0.4697 | 0.9434 | 0.103* | |
HW2 | 1.1034 | 0.4155 | 1.0038 | 0.103* | |
C1 | 0.4262 (6) | 0.2423 (3) | 0.8743 (3) | 0.0658 (14) | |
H1A | 0.5223 | 0.2653 | 0.8792 | 0.079* | |
H1B | 0.3613 | 0.2884 | 0.8585 | 0.079* | |
C2 | 0.4693 (6) | 0.2167 (3) | 0.7339 (3) | 0.0668 (14) | |
H2A | 0.5651 | 0.2379 | 0.7484 | 0.080* | |
H2B | 0.4759 | 0.1731 | 0.6938 | 0.080* | |
C3 | 0.3621 (10) | 0.2617 (5) | 1.0945 (4) | 0.126 (3) | |
H3A | 0.3741 | 0.3099 | 1.1294 | 0.189* | |
H3B | 0.4204 | 0.2158 | 1.1163 | 0.189* | |
H3C | 0.2636 | 0.2446 | 1.0892 | 0.189* | |
C4 | 0.3593 (12) | 0.3941 (6) | 0.5871 (5) | 0.159 (4) | |
H4A | 0.4096 | 0.4171 | 0.5450 | 0.239* | |
H4B | 0.3400 | 0.4385 | 0.6235 | 0.239* | |
H4C | 0.2708 | 0.3697 | 0.5647 | 0.239* | |
C5 | 0.4479 (9) | 0.3279 (5) | 0.6301 (4) | 0.113 (3) | |
H5A | 0.5382 | 0.3529 | 0.6510 | 0.135* | |
H5B | 0.4686 | 0.2841 | 0.5925 | 0.135* | |
C6 | 0.6940 (9) | −0.0227 (5) | 0.9255 (5) | 0.122 (3) | |
H6A | 0.7537 | −0.0722 | 0.9310 | 0.183* | |
H6B | 0.5983 | −0.0391 | 0.9066 | 0.183* | |
H6C | 0.6936 | 0.0047 | 0.9764 | 0.183* | |
C7 | 0.7476 (8) | 0.0338 (4) | 0.8704 (4) | 0.100 (2) | |
H7A | 0.7503 | 0.0046 | 0.8199 | 0.120* | |
H7B | 0.8450 | 0.0486 | 0.8896 | 0.120* | |
C8 | 0.4057 (8) | 0.2849 (4) | 1.0146 (3) | 0.0867 (19) | |
H8A | 0.5039 | 0.3047 | 1.0209 | 0.104* | |
H8B | 0.3463 | 0.3314 | 0.9931 | 0.104* | |
C9 | 0.0455 (7) | 0.0004 (5) | 0.6413 (4) | 0.100 (2) | |
H9A | −0.0511 | −0.0192 | 0.6411 | 0.150* | |
H9B | 0.1092 | −0.0473 | 0.6434 | 0.150* | |
H9C | 0.0552 | 0.0324 | 0.5936 | 0.150* | |
C10 | 0.3798 (7) | 0.2883 (4) | 0.6968 (3) | 0.0833 (18) | |
H10A | 0.2862 | 0.2668 | 0.6771 | 0.100* | |
H10B | 0.3667 | 0.3308 | 0.7371 | 0.100* | |
C11 | 0.6622 (6) | 0.1152 (4) | 0.8558 (4) | 0.0796 (17) | |
H11A | 0.6707 | 0.1488 | 0.9043 | 0.096* | |
H11B | 0.7026 | 0.1479 | 0.8147 | 0.096* | |
C12 | 0.0822 (7) | 0.0560 (4) | 0.7130 (4) | 0.0887 (19) | |
H12A | 0.0149 | 0.1028 | 0.7112 | 0.106* | |
H12B | 0.0702 | 0.0234 | 0.7607 | 0.106* | |
C13 | 0.5070 (6) | 0.0993 (3) | 0.8308 (3) | 0.0670 (14) | |
H13A | 0.4662 | 0.0709 | 0.8744 | 0.080* | |
H13B | 0.5005 | 0.0604 | 0.7860 | 0.080* | |
C14 | 0.3937 (7) | 0.2116 (3) | 0.9551 (3) | 0.0725 (15) | |
H14A | 0.4604 | 0.1671 | 0.9732 | 0.087* | |
H14B | 0.2979 | 0.1882 | 0.9516 | 0.087* | |
C15 | 0.2296 (6) | 0.0912 (4) | 0.7196 (3) | 0.0731 (15) | |
H15A | 0.2426 | 0.1234 | 0.6718 | 0.088* | |
H15B | 0.2974 | 0.0447 | 0.7227 | 0.088* | |
C16 | 0.2616 (5) | 0.1479 (3) | 0.7915 (3) | 0.0635 (14) | |
H16A | 0.2016 | 0.1979 | 0.7846 | 0.076* | |
H16B | 0.2352 | 0.1180 | 0.8382 | 0.076* | |
N | 0.4152 (5) | 0.1761 (2) | 0.8072 (2) | 0.0591 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo | 0.0563 (3) | 0.0515 (3) | 0.0646 (3) | −0.0045 (2) | 0.0144 (2) | −0.0043 (2) |
Cl1 | 0.0827 (10) | 0.0806 (10) | 0.0857 (10) | −0.0039 (8) | 0.0402 (8) | 0.0027 (8) |
Cl2 | 0.0916 (11) | 0.0562 (8) | 0.1048 (11) | 0.0037 (7) | 0.0290 (9) | 0.0058 (7) |
Cl3 | 0.0821 (10) | 0.0561 (7) | 0.0743 (9) | 0.0041 (7) | 0.0167 (7) | 0.0020 (6) |
Cl4 | 0.0912 (10) | 0.0713 (9) | 0.0746 (9) | 0.0025 (8) | 0.0371 (8) | −0.0044 (7) |
O | 0.078 (3) | 0.080 (3) | 0.091 (3) | −0.011 (2) | −0.004 (2) | −0.011 (2) |
OW | 0.067 (2) | 0.068 (2) | 0.071 (2) | −0.003 (2) | 0.009 (2) | −0.0078 (19) |
C1 | 0.080 (4) | 0.051 (3) | 0.069 (3) | 0.004 (3) | 0.017 (3) | −0.008 (3) |
C2 | 0.074 (4) | 0.057 (3) | 0.072 (3) | −0.003 (3) | 0.023 (3) | −0.002 (3) |
C3 | 0.187 (9) | 0.109 (6) | 0.084 (5) | −0.013 (6) | 0.028 (5) | −0.025 (4) |
C4 | 0.258 (13) | 0.119 (7) | 0.097 (6) | 0.031 (8) | −0.008 (7) | 0.038 (5) |
C5 | 0.157 (8) | 0.098 (5) | 0.086 (5) | 0.012 (5) | 0.030 (5) | 0.020 (4) |
C6 | 0.126 (7) | 0.098 (6) | 0.141 (7) | 0.000 (5) | 0.004 (6) | 0.008 (5) |
C7 | 0.111 (6) | 0.082 (5) | 0.103 (5) | 0.012 (4) | −0.004 (4) | 0.002 (4) |
C8 | 0.109 (5) | 0.074 (4) | 0.078 (4) | 0.001 (4) | 0.012 (4) | −0.018 (3) |
C9 | 0.084 (5) | 0.097 (5) | 0.116 (6) | −0.018 (4) | −0.006 (4) | −0.002 (4) |
C10 | 0.111 (5) | 0.066 (4) | 0.075 (4) | 0.010 (4) | 0.018 (4) | 0.007 (3) |
C11 | 0.072 (4) | 0.071 (4) | 0.097 (4) | 0.006 (3) | 0.010 (3) | 0.004 (3) |
C12 | 0.068 (4) | 0.104 (5) | 0.095 (5) | −0.011 (4) | 0.012 (3) | 0.003 (4) |
C13 | 0.078 (4) | 0.048 (3) | 0.075 (4) | 0.003 (3) | 0.007 (3) | −0.006 (2) |
C14 | 0.090 (4) | 0.061 (3) | 0.067 (3) | 0.002 (3) | 0.015 (3) | −0.004 (3) |
C15 | 0.066 (4) | 0.072 (4) | 0.082 (4) | −0.003 (3) | 0.015 (3) | −0.006 (3) |
C16 | 0.061 (3) | 0.061 (3) | 0.071 (3) | 0.001 (3) | 0.020 (3) | 0.000 (3) |
N | 0.067 (3) | 0.042 (2) | 0.071 (3) | 0.003 (2) | 0.016 (2) | −0.0017 (19) |
Mo—O | 1.647 (4) | C6—H6C | 0.960 |
Mo—OW | 2.340 (4) | C7—C11 | 1.521 (8) |
Mo—Cl2 | 2.352 (2) | C7—H7A | 0.970 |
Mo—Cl4 | 2.358 (1) | C7—H7B | 0.970 |
Mo—Cl1 | 2.380 (1) | C8—C14 | 1.528 (7) |
Mo—Cl3 | 2.402 (1) | C8—H8A | 0.970 |
OW—HW1 | 0.843 | C8—H8B | 0.970 |
OW—HW2 | 0.846 | C9—C12 | 1.506 (9) |
C1—C14 | 1.504 (7) | C9—H9A | 0.960 |
C1—N | 1.534 (6) | C9—H9B | 0.960 |
C1—H1A | 0.970 | C9—H9C | 0.960 |
C1—H1B | 0.970 | C10—H10A | 0.970 |
C2—C10 | 1.506 (7) | C10—H10B | 0.970 |
C2—N | 1.523 (6) | C11—C13 | 1.500 (7) |
C2—H2A | 0.970 | C11—H11A | 0.970 |
C2—H2B | 0.970 | C11—H11B | 0.970 |
C3—C8 | 1.490 (8) | C12—C15 | 1.486 (8) |
C3—H3A | 0.960 | C12—H12A | 0.970 |
C3—H3B | 0.960 | C12—H12B | 0.970 |
C3—H3C | 0.960 | C13—N | 1.517 (6) |
C4—C5 | 1.481 (10) | C13—H13A | 0.970 |
C4—H4A | 0.960 | C13—H13B | 0.970 |
C4—H4B | 0.960 | C14—H14A | 0.970 |
C4—H4C | 0.960 | C14—H14B | 0.970 |
C5—C10 | 1.485 (8) | C15—C16 | 1.511 (7) |
C5—H5A | 0.970 | C15—H15A | 0.970 |
C5—H5B | 0.970 | C15—H15B | 0.970 |
C6—C7 | 1.414 (10) | C16—N | 1.510 (6) |
C6—H6A | 0.960 | C16—H16A | 0.970 |
C6—H6B | 0.960 | C16—H16B | 0.970 |
O—Mo—OW | 177.7 (2) | C3—C8—C14 | 113.4 (5) |
O—Mo—Cl2 | 99.8 (2) | C3—C8—H8A | 108.9 |
OW—Mo—Cl2 | 82.48 (11) | C14—C8—H8A | 108.9 |
O—Mo—Cl4 | 99.0 (2) | C3—C8—H8B | 108.9 |
OW—Mo—Cl4 | 81.5 (1) | C14—C8—H8B | 108.9 |
Cl2—Mo—Cl4 | 89.1 (1) | H8A—C8—H8B | 107.7 |
O—Mo—Cl1 | 98.3 (2) | C12—C9—H9A | 109.5 |
OW—Mo—Cl1 | 81.1 (1) | C12—C9—H9B | 109.5 |
Cl2—Mo—Cl1 | 88.3 (1) | H9A—C9—H9B | 109.5 |
Cl4—Mo—Cl1 | 162.7 (1) | C12—C9—H9C | 109.5 |
O—Mo—Cl3 | 97.3 (2) | H9A—C9—H9C | 109.5 |
OW—Mo—Cl3 | 80.4 (1) | H9B—C9—H9C | 109.5 |
Cl2—Mo—Cl3 | 162.9 (1) | C5—C10—C2 | 111.3 (6) |
Cl4—Mo—Cl3 | 88.6 (1) | C5—C10—H10A | 109.4 |
Cl1—Mo—Cl3 | 88.8 (1) | C2—C10—H10A | 109.4 |
Mo—OW—HW1 | 115 | C5—C10—H10B | 109.4 |
Mo—OW—HW2 | 118 | C2—C10—H10B | 109.4 |
HW1—OW—HW2 | 109 | H10A—C10—H10B | 108.0 |
C14—C1—N | 116.3 (4) | C13—C11—C7 | 112.8 (5) |
C14—C1—H1A | 108.2 | C13—C11—H11A | 109.0 |
N—C1—H1A | 108.2 | C7—C11—H11A | 109.0 |
C14—C1—H1B | 108.2 | C13—C11—H11B | 109.0 |
N—C1—H1B | 108.2 | C7—C11—H11B | 109.0 |
H1A—C1—H1B | 107.4 | H11A—C11—H11B | 107.8 |
C10—C2—N | 115.8 (4) | C15—C12—C9 | 114.6 (6) |
C10—C2—H2A | 108.3 | C15—C12—H12A | 108.6 |
N—C2—H2A | 108.3 | C9—C12—H12A | 108.6 |
C10—C2—H2B | 108.3 | C15—C12—H12B | 108.6 |
N—C2—H2B | 108.3 | C9—C12—H12B | 108.6 |
H2A—C2—H2B | 107.4 | H12A—C12—H12B | 107.6 |
C8—C3—H3A | 109.5 | C11—C13—N | 116.9 (4) |
C8—C3—H3B | 109.5 | C11—C13—H13A | 108.1 |
H3A—C3—H3B | 109.5 | N—C13—H13A | 108.1 |
C8—C3—H3C | 109.5 | C11—C13—H13B | 108.1 |
H3A—C3—H3C | 109.5 | N—C13—H13B | 108.1 |
H3B—C3—H3C | 109.5 | H13A—C13—H13B | 107.3 |
C5—C4—H4A | 109.5 | C1—C14—C8 | 110.0 (5) |
C5—C4—H4B | 109.5 | C1—C14—H14A | 109.7 |
H4A—C4—H4B | 109.5 | C8—C14—H14A | 109.7 |
C5—C4—H4C | 109.5 | C1—C14—H14B | 109.7 |
H4A—C4—H4C | 109.5 | C8—C14—H14B | 109.7 |
H4B—C4—H4C | 109.5 | H14A—C14—H14B | 108.2 |
C4—C5—C10 | 113.8 (7) | C12—C15—C16 | 113.1 (5) |
C4—C5—H5A | 108.8 | C12—C15—H15A | 109.0 |
C10—C5—H5A | 108.8 | C16—C15—H15A | 109.0 |
C4—C5—H5B | 108.8 | C12—C15—H15B | 109.0 |
C10—C5—H5B | 108.8 | C16—C15—H15B | 109.0 |
H5A—C5—H5B | 107.7 | H15A—C15—H15B | 107.8 |
C7—C6—H6A | 109.5 | N—C16—C15 | 115.3 (4) |
C7—C6—H6B | 109.5 | N—C16—H16A | 108.5 |
H6A—C6—H6B | 109.5 | C15—C16—H16A | 108.5 |
C7—C6—H6C | 109.5 | N—C16—H16B | 108.5 |
H6A—C6—H6C | 109.5 | C15—C16—H16B | 108.5 |
H6B—C6—H6C | 109.5 | H16A—C16—H16B | 107.5 |
C6—C7—C11 | 115.0 (7) | C16—N—C13 | 108.7 (4) |
C6—C7—H7A | 108.5 | C16—N—C2 | 111.8 (4) |
C11—C7—H7A | 108.5 | C13—N—C2 | 108.8 (4) |
C6—C7—H7B | 108.5 | C16—N—C1 | 108.9 (4) |
C11—C7—H7B | 108.5 | C13—N—C1 | 110.8 (4) |
H7A—C7—H7B | 107.5 | C2—N—C1 | 107.9 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···Cl1i | 0.84 | 2.61 | 3.338 (4) | 145 |
OW—HW2···Cl3i | 0.85 | 2.47 | 3.238 (4) | 151 |
Symmetry code: (i) −x+2, −y+1, −z+2. |
Experimental details
Crystal data | |
Chemical formula | (C16H36N)[MoOCl4(H2O)] |
Mr | 514.21 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 9.401 (1), 15.770 (1), 16.845 (1) |
β (°) | 95.581 (1) |
V (Å3) | 2485.6 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.97 |
Crystal size (mm) | 0.45 × 0.20 × 0.10 |
Data collection | |
Diffractometer | SMART CCD diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.644, 0.908 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8905, 4368, 3157 |
Rint | 0.033 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.050, 0.124, 1.15 |
No. of reflections | 4368 |
No. of parameters | 225 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.54, −0.45 |
Computer programs: SMART (Siemens, 1996), SMART and SAINT (Siemens, 1994), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXLTL (Siemens, 1994), SHELXL97.
Mo—O | 1.647 (4) | Mo—Cl4 | 2.358 (1) |
Mo—OW | 2.340 (4) | Mo—Cl1 | 2.380 (1) |
Mo—Cl2 | 2.352 (2) | Mo—Cl3 | 2.402 (1) |
O—Mo—OW | 177.7 (2) | Cl2—Mo—Cl1 | 88.3 (1) |
O—Mo—Cl2 | 99.8 (2) | Cl4—Mo—Cl1 | 162.7 (1) |
OW—Mo—Cl2 | 82.48 (11) | O—Mo—Cl3 | 97.3 (2) |
O—Mo—Cl4 | 99.0 (2) | OW—Mo—Cl3 | 80.4 (1) |
OW—Mo—Cl4 | 81.5 (1) | Cl2—Mo—Cl3 | 162.9 (1) |
Cl2—Mo—Cl4 | 89.1 (1) | Cl4—Mo—Cl3 | 88.6 (1) |
O—Mo—Cl1 | 98.3 (2) | Cl1—Mo—Cl3 | 88.8 (1) |
OW—Mo—Cl1 | 81.1 (1) |
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···Cl1i | 0.84 | 2.61 | 3.338 (4) | 145 |
OW—HW2···Cl3i | 0.85 | 2.47 | 3.238 (4) | 151 |
Symmetry code: (i) −x+2, −y+1, −z+2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
Molybdenum in its higher oxidation states readily forms polynuclear anionic metal–oxygen clusters and many polymolybdates with a wide variety of geometrical and electronic structures have been reported (Pope & Müller, 1991; Müller et al., 1995, 1998; Müller & Serain, 2000). However, the synthesis of polymolybdates with bridging chlorine atoms is far less well developed. In the course of our work on the synthesis of chlorine-bridged polymolybdates, the title compound, (I), was unexpectedly obtained as single crystals.
The X-ray structure analysis of (I) reveals that the geometry of the [MoOCl4(H2O)]- anion is similar to those of its analogues (Bino & Cotton, 1979; Boorman et al., 1975; Cindric et al., 1996; Garner et al., 1977; Junk & Atwood, 1998; Kepert et al., 1997). As shown in Fig. 1, the coordination environment of the Mo atom is a distorted octahedron with the cis angles at Mo ranging from 80.4 (1) to 99.8 (2)°. The Mo═O bond length of 1.647 (4) Å and the Mo—Owater bond length of 2.340 (4) Å are of typical values for terminal oxygen and aqua bond lengths to Mo. The Mo—Cl bond lengths are in the range 2.352 (2)–2.402 (1) Å, the cis-Cl—Mo—Cl angles are 88.3 (1)–89.1 (1)°, and the O═ Mo—OH2 angle is 177.7 (2)°, so the [MoOCl4(H2O)]- anion deviates only slightly from C4v symmetry.
Anions are linked in pairs through O—H···Cl hydrogen bonds involving the aqua ligands (Table 2). As shown in the packing of the cations and anions in the crystal structure, there are no other significant interactions (Fig. 2).