metal-organic compounds
Low-temperature phase of hexaguanidinium heptamolybdate monohydrate
aSchool of Engineering and Science, Jacobs University Bremen, PO Box 750561, 28725 Bremen, Germany
*Correspondence e-mail: m.dickman@jacobs-university.de
The 2)3]6[Mo7O24]·H2O, previously determined at room temperature in the monoclinic C2/c from Weissenberg techniques [Don & Weakley (1981). Acta Cryst. B37, 451–453], has been redetermined from low-temperature single-crystal data in the monoclinic P21/c. The contains one heptamolybdate anion, six guanidinium cations and one water molecule of hydration. The anions and cations are linked by an extensive network of N—H⋯O hydrogen bonds.
of the title compound, [C(NHRelated literature
For the previous determination of the title compound in the monoclinic C2/c, see: Don & Weakley (1981). For an example of a structurally characterized [Mo7O24]6− anion, see: Kortz & Pope (1995). For more information about isopolymolybdates and polyoxometalates in general, see: Pope (1983).
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2005); cell APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and WINGX Farrugia (1999)..
Supporting information
10.1107/S1600536808008234/mg2049sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808008234/mg2049Isup2.hkl
To an aqueous solution (30 ml) of Na2MoO4.2H2O (0.726 g) and Na2HPO4 (0.071 g) was added solid (CH3)SnCl2 (0.220 g). After stirring for 30 min at room temperature, few drops of aqueous 1M [C(NH2)3]Cl were added, and the resulting solution was left to slowly evaporate at room temperature, colorless block-like single crystals of the title compound forming in a few days.
The H atoms of the guanidinium cations were positioned geometrically and refined as riding. The positional parameters of the H atoms of the water molecule were calculated using the CALCOH tool of WinGX (Farrugia, 1999) and fixed during the refinment. All H atoms were refined with isotropic displacement parameters fixed at 1.2 times Ueq of their parent atoms.
Data collection: APEX2 (Bruker, 2005); cell
APEX2 (Bruker, 2005); data reduction: APEX2 (Bruker, 2005); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).(CH6N3)6[Mo7O24]·H2O | F(000) = 2776 |
Mr = 1434.12 | Dx = 2.531 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 7762 reflections |
a = 11.9402 (6) Å | θ = 2.3–29.7° |
b = 15.9131 (9) Å | µ = 2.37 mm−1 |
c = 19.8223 (13) Å | T = 173 K |
β = 92.312 (4)° | Prism, colourless |
V = 3763.3 (4) Å3 | 0.17 × 0.17 × 0.08 mm |
Z = 4 |
Bruker X8 APEXII CCD area-detector diffractometer | 15842 independent reflections |
Radiation source: sealed tube | 9689 reflections with I > 2s(I) |
Graphite monochromator | Rint = 0.150 |
ϕ and ω scans | θmax = 34.4°, θmin = 1.7° |
Absorption correction: multi-scan APEXII (Bruker, 2005) | h = −18→18 |
Tmin = 0.689, Tmax = 0.833 | k = −25→25 |
153838 measured reflections | l = −31→31 |
Refinement on F2 | H-atom parameters constrained |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.065P)2 + 1.0536P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.053 | (Δ/σ)max = 0.001 |
wR(F2) = 0.164 | Δρmax = 1.77 e Å−3 |
S = 1.06 | Δρmin = −2.33 e Å−3 |
15842 reflections | Extinction correction: SHELXL |
506 parameters | Extinction coefficient: 0.00102 (9) |
0 restraints |
(CH6N3)6[Mo7O24]·H2O | V = 3763.3 (4) Å3 |
Mr = 1434.12 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.9402 (6) Å | µ = 2.37 mm−1 |
b = 15.9131 (9) Å | T = 173 K |
c = 19.8223 (13) Å | 0.17 × 0.17 × 0.08 mm |
β = 92.312 (4)° |
Bruker X8 APEXII CCD area-detector diffractometer | 15842 independent reflections |
Absorption correction: multi-scan APEXII (Bruker, 2005) | 9689 reflections with I > 2s(I) |
Tmin = 0.689, Tmax = 0.833 | Rint = 0.150 |
153838 measured reflections |
R[F2 > 2σ(F2)] = 0.053 | 0 restraints |
wR(F2) = 0.164 | H-atom parameters constrained |
S = 1.06 | Δρmax = 1.77 e Å−3 |
15842 reflections | Δρmin = −2.33 e Å−3 |
506 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 | ||
Mo1 | 0.02068 (3) | 0.06939 (2) | 0.221800 (17) | 0.01551 (8) | |
Mo2 | 0.22006 (3) | 0.06307 (2) | 0.115322 (17) | 0.01597 (8) | |
Mo3 | 0.04258 (3) | 0.17323 (2) | 0.359758 (18) | 0.01829 (9) | |
Mo4 | 0.24555 (3) | 0.20215 (2) | 0.245700 (16) | 0.01436 (8) | |
Mo5 | 0.44752 (3) | 0.16970 (2) | 0.131721 (18) | 0.01815 (9) | |
Mo6 | 0.26730 (3) | 0.06331 (2) | 0.377162 (17) | 0.01662 (8) | |
Mo7 | 0.46759 (3) | 0.06731 (2) | 0.270582 (18) | 0.01634 (8) | |
O1B | −0.0700 (3) | 0.0900 (2) | 0.15428 (15) | 0.0235 (7) | |
O1A | −0.0382 (3) | −0.0105 (2) | 0.26587 (16) | 0.0249 (7) | |
O2B | 0.1171 (3) | 0.0798 (2) | 0.05310 (15) | 0.0238 (7) | |
O2A | 0.2968 (3) | −0.0190 (2) | 0.08550 (16) | 0.0246 (7) | |
O3B | −0.0348 (3) | 0.1000 (2) | 0.40054 (16) | 0.0270 (7) | |
O3A | −0.0090 (3) | 0.2697 (2) | 0.38553 (16) | 0.0266 (7) | |
O5B | 0.5214 (3) | 0.0936 (2) | 0.09095 (16) | 0.0256 (7) | |
O5A | 0.5025 (3) | 0.2644 (2) | 0.10420 (17) | 0.0271 (7) | |
O6B | 0.3707 (3) | 0.0785 (2) | 0.43900 (15) | 0.0241 (7) | |
O6A | 0.1877 (3) | −0.0173 (2) | 0.40575 (16) | 0.0269 (7) | |
O7B | 0.5567 (3) | 0.0861 (2) | 0.33821 (16) | 0.0248 (7) | |
O7A | 0.5255 (3) | −0.0139 (2) | 0.22726 (17) | 0.0256 (7) | |
O12 | 0.1370 (2) | 0.00412 (18) | 0.18077 (14) | 0.0186 (6) | |
O13 | −0.0327 (2) | 0.16739 (19) | 0.27278 (15) | 0.0201 (6) | |
O1M4 | 0.1493 (2) | 0.10064 (18) | 0.29826 (13) | 0.0156 (5) | |
O2M4 | 0.3391 (2) | 0.09888 (18) | 0.19337 (13) | 0.0152 (5) | |
O25 | 0.3103 (2) | 0.16081 (19) | 0.08014 (14) | 0.0203 (6) | |
O34 | 0.1626 (3) | 0.26978 (19) | 0.29144 (15) | 0.0215 (6) | |
O36 | 0.1794 (2) | 0.16226 (19) | 0.41150 (14) | 0.0208 (6) | |
O45 | 0.3298 (3) | 0.26854 (19) | 0.19892 (15) | 0.0216 (6) | |
O57 | 0.5234 (2) | 0.16324 (19) | 0.21861 (15) | 0.0205 (6) | |
O67 | 0.3490 (2) | 0.00393 (18) | 0.31125 (14) | 0.0184 (6) | |
O124 | 0.1415 (2) | 0.16496 (18) | 0.17796 (14) | 0.0160 (5) | |
O467 | 0.3486 (2) | 0.16389 (18) | 0.31372 (14) | 0.0175 (6) | |
C1 | −0.1887 (4) | 0.2916 (3) | 0.5167 (3) | 0.0331 (11) | |
C2 | 0.4571 (4) | 0.1742 (3) | −0.0860 (2) | 0.0231 (9) | |
C3 | 0.0480 (4) | 0.1669 (3) | 0.5786 (2) | 0.0227 (9) | |
C4 | −0.2559 (3) | 0.2966 (3) | 0.24617 (19) | 0.0216 (9) | |
C5 | −0.2245 (4) | −0.0488 (3) | 0.1085 (2) | 0.0199 (8) | |
C6 | 0.2837 (4) | 0.0415 (3) | 0.6044 (2) | 0.0225 (9) | |
N11 | −0.2273 (4) | 0.2477 (3) | 0.4624 (3) | 0.0513 (14) | |
H11A | −0.2897 | 0.2186 | 0.4643 | 0.062* | |
H11B | −0.1900 | 0.2481 | 0.4250 | 0.062* | |
N12 | 0.5055 (3) | 0.1087 (3) | −0.0551 (2) | 0.0288 (9) | |
H12A | 0.5597 | 0.0814 | −0.0744 | 0.035* | |
H12B | 0.4833 | 0.0927 | −0.0153 | 0.035* | |
N13 | 0.0031 (4) | 0.1011 (3) | 0.5475 (2) | 0.0308 (9) | |
H13A | −0.0506 | 0.0726 | 0.5663 | 0.037* | |
H13B | 0.0267 | 0.0857 | 0.5079 | 0.037* | |
N14 | −0.2542 (3) | 0.2142 (3) | 0.24754 (19) | 0.0298 (10) | |
H14A | −0.3154 | 0.1856 | 0.2369 | 0.036* | |
H14B | −0.1917 | 0.1875 | 0.2591 | 0.036* | |
N15 | −0.1334 (3) | −0.0878 (3) | 0.0894 (2) | 0.0275 (9) | |
H15A | −0.1071 | −0.0776 | 0.0494 | 0.033* | |
H15B | −0.0990 | −0.1238 | 0.1168 | 0.033* | |
N16 | 0.2399 (3) | 0.0624 (3) | 0.66201 (18) | 0.0269 (9) | |
H16A | 0.2705 | 0.1028 | 0.6869 | 0.032* | |
H16B | 0.1801 | 0.0361 | 0.6756 | 0.032* | |
N21 | −0.0947 (3) | 0.3375 (3) | 0.5144 (2) | 0.0349 (11) | |
H21A | −0.0712 | 0.3667 | 0.5500 | 0.042* | |
H21B | −0.0566 | 0.3385 | 0.4773 | 0.042* | |
N22 | 0.3746 (3) | 0.2148 (2) | −0.05681 (19) | 0.0274 (9) | |
H22A | 0.3420 | 0.2579 | −0.0773 | 0.033* | |
H22B | 0.3526 | 0.1986 | −0.0170 | 0.033* | |
N23 | 0.1296 (3) | 0.2099 (2) | 0.55026 (19) | 0.0253 (8) | |
H23A | 0.1536 | 0.1944 | 0.5108 | 0.030* | |
H23B | 0.1596 | 0.2538 | 0.5711 | 0.030* | |
N24 | −0.1629 (3) | 0.3397 (2) | 0.2631 (2) | 0.0299 (9) | |
H24A | −0.1009 | 0.3128 | 0.2751 | 0.036* | |
H24B | −0.1638 | 0.3950 | 0.2622 | 0.036* | |
N25 | −0.2628 (3) | −0.0643 (3) | 0.16922 (19) | 0.0266 (8) | |
H25A | −0.2275 | −0.1002 | 0.1963 | 0.032* | |
H25B | −0.3234 | −0.0386 | 0.1824 | 0.032* | |
N26 | 0.2384 (3) | −0.0186 (2) | 0.5654 (2) | 0.0273 (8) | |
H26A | 0.1780 | −0.0451 | 0.5779 | 0.033* | |
H26B | 0.2687 | −0.0317 | 0.5270 | 0.033* | |
N31 | −0.2477 (4) | 0.2892 (3) | 0.5725 (2) | 0.0454 (12) | |
H31A | −0.2252 | 0.3180 | 0.6084 | 0.054* | |
H31B | −0.3092 | 0.2588 | 0.5734 | 0.054* | |
N32 | 0.4905 (4) | 0.1984 (3) | −0.1459 (2) | 0.0301 (9) | |
H32A | 0.5447 | 0.1712 | −0.1652 | 0.036* | |
H32B | 0.4584 | 0.2418 | −0.1663 | 0.036* | |
N33 | 0.0121 (4) | 0.1901 (3) | 0.63845 (19) | 0.0292 (9) | |
H33A | −0.0416 | 0.1616 | 0.6572 | 0.035* | |
H33B | 0.0420 | 0.2340 | 0.6593 | 0.035* | |
N34 | −0.3495 (3) | 0.3368 (2) | 0.2289 (2) | 0.0281 (9) | |
H34A | −0.4108 | 0.3083 | 0.2183 | 0.034* | |
H34B | −0.3504 | 0.3921 | 0.2280 | 0.034* | |
N35 | −0.2762 (3) | 0.0054 (2) | 0.06749 (19) | 0.0268 (8) | |
H35A | −0.2500 | 0.0155 | 0.0274 | 0.032* | |
H35B | −0.3369 | 0.0313 | 0.0802 | 0.032* | |
N36 | 0.3742 (3) | 0.0814 (3) | 0.58373 (19) | 0.0269 (9) | |
H36A | 0.4049 | 0.1217 | 0.6086 | 0.032* | |
H36B | 0.4034 | 0.0673 | 0.5452 | 0.032* | |
O1W | −0.4098 (3) | 0.1463 (3) | 0.4856 (2) | 0.0446 (10) | |
H1OW | −0.4589 | 0.1330 | 0.4545 | 0.054* | |
H2OW | −0.4419 | 0.1380 | 0.5233 | 0.054* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.01223 (16) | 0.01668 (17) | 0.01772 (15) | −0.00120 (12) | 0.00174 (12) | −0.00124 (12) |
Mo2 | 0.01468 (17) | 0.01756 (17) | 0.01579 (15) | 0.00145 (13) | 0.00233 (12) | −0.00065 (12) |
Mo3 | 0.01455 (17) | 0.02142 (19) | 0.01925 (16) | −0.00144 (13) | 0.00494 (13) | −0.00450 (13) |
Mo4 | 0.01179 (16) | 0.01357 (16) | 0.01786 (15) | 0.00013 (12) | 0.00221 (12) | 0.00014 (12) |
Mo5 | 0.01378 (17) | 0.01978 (19) | 0.02126 (17) | 0.00092 (13) | 0.00547 (13) | 0.00439 (13) |
Mo6 | 0.01591 (17) | 0.01855 (18) | 0.01550 (15) | −0.00138 (13) | 0.00215 (12) | 0.00095 (12) |
Mo7 | 0.01257 (16) | 0.01696 (17) | 0.01955 (16) | 0.00162 (12) | 0.00167 (12) | 0.00165 (12) |
O1B | 0.0211 (16) | 0.0266 (17) | 0.0224 (14) | 0.0034 (13) | −0.0041 (12) | 0.0003 (12) |
O1A | 0.0231 (16) | 0.0247 (17) | 0.0272 (16) | −0.0041 (13) | 0.0043 (13) | 0.0016 (13) |
O2B | 0.0231 (16) | 0.0286 (17) | 0.0196 (14) | −0.0017 (13) | −0.0012 (12) | 0.0002 (12) |
O2A | 0.0238 (16) | 0.0236 (16) | 0.0269 (16) | 0.0061 (13) | 0.0066 (13) | −0.0020 (13) |
O3B | 0.0231 (17) | 0.0334 (19) | 0.0250 (15) | −0.0062 (14) | 0.0072 (13) | −0.0005 (14) |
O3A | 0.0227 (16) | 0.0247 (17) | 0.0326 (17) | −0.0006 (13) | 0.0054 (13) | −0.0126 (13) |
O5B | 0.0198 (16) | 0.0301 (18) | 0.0274 (16) | 0.0055 (13) | 0.0089 (13) | 0.0005 (13) |
O5A | 0.0251 (17) | 0.0239 (17) | 0.0328 (17) | −0.0002 (14) | 0.0080 (14) | 0.0125 (13) |
O6B | 0.0224 (16) | 0.0309 (18) | 0.0191 (14) | 0.0006 (13) | 0.0009 (12) | −0.0004 (12) |
O6A | 0.0265 (17) | 0.0263 (17) | 0.0281 (16) | −0.0050 (14) | 0.0054 (14) | 0.0031 (13) |
O7B | 0.0205 (16) | 0.0263 (17) | 0.0274 (16) | 0.0008 (13) | −0.0036 (13) | 0.0049 (13) |
O7A | 0.0224 (16) | 0.0227 (16) | 0.0323 (17) | 0.0052 (13) | 0.0074 (13) | 0.0033 (13) |
O12 | 0.0198 (15) | 0.0160 (14) | 0.0201 (13) | 0.0007 (11) | 0.0021 (11) | −0.0017 (11) |
O13 | 0.0118 (13) | 0.0249 (16) | 0.0239 (14) | 0.0013 (12) | 0.0040 (11) | −0.0038 (12) |
O1M4 | 0.0137 (14) | 0.0170 (14) | 0.0163 (12) | −0.0003 (11) | 0.0018 (10) | −0.0002 (10) |
O2M4 | 0.0135 (13) | 0.0157 (13) | 0.0169 (12) | 0.0014 (11) | 0.0048 (10) | 0.0018 (10) |
O25 | 0.0175 (15) | 0.0258 (16) | 0.0179 (13) | 0.0009 (12) | 0.0045 (11) | 0.0038 (11) |
O34 | 0.0189 (15) | 0.0204 (15) | 0.0254 (15) | 0.0003 (12) | 0.0025 (12) | −0.0039 (12) |
O36 | 0.0191 (15) | 0.0235 (16) | 0.0201 (14) | −0.0012 (12) | 0.0029 (11) | −0.0057 (11) |
O45 | 0.0215 (15) | 0.0178 (15) | 0.0255 (15) | −0.0038 (12) | 0.0019 (12) | 0.0044 (12) |
O57 | 0.0118 (13) | 0.0215 (16) | 0.0283 (15) | −0.0008 (11) | 0.0027 (12) | 0.0050 (12) |
O67 | 0.0171 (14) | 0.0159 (14) | 0.0225 (14) | −0.0009 (11) | 0.0041 (11) | 0.0016 (11) |
O124 | 0.0144 (13) | 0.0164 (14) | 0.0174 (12) | −0.0009 (11) | 0.0006 (10) | 0.0004 (10) |
O467 | 0.0151 (14) | 0.0194 (15) | 0.0179 (13) | −0.0005 (11) | 0.0017 (11) | 0.0017 (11) |
C1 | 0.030 (3) | 0.037 (3) | 0.032 (2) | 0.005 (2) | −0.001 (2) | −0.007 (2) |
C2 | 0.021 (2) | 0.022 (2) | 0.027 (2) | 0.0038 (17) | −0.0003 (17) | −0.0043 (17) |
C3 | 0.021 (2) | 0.021 (2) | 0.026 (2) | 0.0001 (17) | 0.0010 (17) | 0.0003 (16) |
C4 | 0.023 (2) | 0.020 (2) | 0.0227 (19) | −0.0002 (17) | 0.0064 (17) | −0.0016 (16) |
C5 | 0.020 (2) | 0.019 (2) | 0.0199 (18) | 0.0045 (16) | −0.0018 (16) | −0.0040 (15) |
C6 | 0.027 (2) | 0.020 (2) | 0.0203 (18) | −0.0015 (18) | −0.0011 (17) | 0.0021 (16) |
N11 | 0.044 (3) | 0.066 (4) | 0.044 (3) | −0.018 (3) | 0.004 (2) | −0.017 (3) |
N12 | 0.029 (2) | 0.029 (2) | 0.0289 (19) | 0.0158 (17) | 0.0043 (17) | 0.0043 (16) |
N13 | 0.037 (2) | 0.025 (2) | 0.031 (2) | −0.0157 (18) | 0.0049 (18) | −0.0070 (16) |
N14 | 0.0161 (19) | 0.0166 (19) | 0.056 (3) | −0.0017 (14) | −0.0017 (19) | 0.0027 (17) |
N15 | 0.027 (2) | 0.030 (2) | 0.0255 (18) | 0.0131 (17) | 0.0029 (16) | −0.0001 (16) |
N16 | 0.029 (2) | 0.032 (2) | 0.0203 (17) | −0.0072 (17) | 0.0101 (15) | −0.0042 (15) |
N21 | 0.0174 (19) | 0.050 (3) | 0.038 (2) | −0.0126 (19) | 0.0076 (17) | −0.016 (2) |
N22 | 0.029 (2) | 0.027 (2) | 0.0259 (18) | 0.0129 (17) | 0.0019 (16) | 0.0031 (15) |
N23 | 0.028 (2) | 0.0222 (19) | 0.0256 (18) | −0.0116 (16) | 0.0055 (16) | −0.0008 (15) |
N24 | 0.025 (2) | 0.0193 (19) | 0.045 (2) | −0.0076 (16) | 0.0025 (18) | −0.0027 (17) |
N25 | 0.023 (2) | 0.034 (2) | 0.0229 (18) | 0.0077 (17) | 0.0041 (15) | 0.0004 (15) |
N26 | 0.0222 (19) | 0.032 (2) | 0.0276 (19) | −0.0117 (17) | 0.0050 (15) | −0.0039 (16) |
N31 | 0.043 (3) | 0.059 (3) | 0.036 (2) | −0.009 (2) | 0.014 (2) | −0.011 (2) |
N32 | 0.031 (2) | 0.032 (2) | 0.0278 (19) | 0.0099 (18) | 0.0049 (17) | 0.0057 (17) |
N33 | 0.031 (2) | 0.033 (2) | 0.0240 (18) | −0.0061 (18) | 0.0097 (16) | −0.0054 (16) |
N34 | 0.025 (2) | 0.0180 (19) | 0.042 (2) | 0.0055 (15) | 0.0019 (17) | 0.0034 (16) |
N35 | 0.025 (2) | 0.030 (2) | 0.0249 (18) | 0.0118 (17) | 0.0001 (15) | −0.0004 (16) |
N36 | 0.030 (2) | 0.028 (2) | 0.0230 (18) | −0.0130 (17) | 0.0045 (16) | −0.0012 (15) |
O1W | 0.027 (2) | 0.058 (3) | 0.049 (2) | −0.0094 (19) | 0.0001 (17) | −0.016 (2) |
Mo1—O1A | 1.710 (3) | C3—N13 | 1.317 (6) |
Mo1—O1B | 1.719 (3) | C3—N33 | 1.330 (6) |
Mo1—O12 | 1.939 (3) | C3—N23 | 1.334 (6) |
Mo1—O13 | 1.978 (3) | C4—N14 | 1.311 (6) |
Mo1—O1M4 | 2.171 (3) | C4—N34 | 1.321 (6) |
Mo1—O124 | 2.291 (3) | C4—N24 | 1.336 (6) |
Mo1—Mo3 | 3.1968 (5) | C5—N15 | 1.320 (5) |
Mo2—O2A | 1.714 (3) | C5—N35 | 1.321 (5) |
Mo2—O2B | 1.726 (3) | C5—N25 | 1.328 (5) |
Mo2—O12 | 1.910 (3) | C6—N16 | 1.318 (5) |
Mo2—O25 | 2.032 (3) | C6—N36 | 1.332 (6) |
Mo2—O2M4 | 2.136 (3) | C6—N26 | 1.331 (6) |
Mo2—O124 | 2.268 (3) | N11—H11A | 0.8800 |
Mo2—Mo5 | 3.2078 (5) | N11—H11B | 0.8800 |
Mo3—O3B | 1.711 (3) | N12—H12A | 0.8800 |
Mo3—O3A | 1.738 (3) | N12—H12B | 0.8800 |
Mo3—O36 | 1.902 (3) | N13—H13A | 0.8800 |
Mo3—O13 | 1.914 (3) | N13—H13B | 0.8800 |
Mo3—O1M4 | 2.138 (3) | N14—H14A | 0.8800 |
Mo3—Mo6 | 3.2099 (5) | N14—H14B | 0.8800 |
Mo4—O34 | 1.742 (3) | N15—H15A | 0.8800 |
Mo4—O45 | 1.751 (3) | N15—H15B | 0.8800 |
Mo4—O124 | 1.887 (3) | N16—H16A | 0.8800 |
Mo4—O467 | 1.889 (3) | N16—H16B | 0.8800 |
Mo4—O1M4 | 2.261 (3) | N21—H21A | 0.8800 |
Mo4—O2M4 | 2.262 (3) | N21—H21B | 0.8800 |
Mo5—O5B | 1.719 (3) | N22—H22A | 0.8800 |
Mo5—O5A | 1.740 (3) | N22—H22B | 0.8800 |
Mo5—O25 | 1.901 (3) | N23—H23A | 0.8800 |
Mo5—O57 | 1.916 (3) | N23—H23B | 0.8800 |
Mo5—O2M4 | 2.137 (3) | N24—H24A | 0.8800 |
Mo5—Mo7 | 3.1993 (5) | N24—H24B | 0.8800 |
Mo6—O6A | 1.708 (3) | N25—H25A | 0.8800 |
Mo6—O6B | 1.721 (3) | N25—H25B | 0.8800 |
Mo6—O67 | 1.911 (3) | N26—H26A | 0.8800 |
Mo6—O36 | 2.025 (3) | N26—H26B | 0.8800 |
Mo6—O1M4 | 2.146 (3) | N31—H31A | 0.8800 |
Mo6—O467 | 2.277 (3) | N31—H31B | 0.8800 |
Mo7—O7B | 1.704 (3) | N32—H32A | 0.8800 |
Mo7—O7A | 1.713 (3) | N32—H32B | 0.8800 |
Mo7—O67 | 1.941 (3) | N33—H33A | 0.8800 |
Mo7—O57 | 1.973 (3) | N33—H33B | 0.8800 |
Mo7—O2M4 | 2.181 (3) | N34—H34A | 0.8800 |
Mo7—O467 | 2.282 (3) | N34—H34B | 0.8800 |
C1—N31 | 1.336 (6) | N35—H35A | 0.8800 |
C1—N21 | 1.342 (6) | N35—H35B | 0.8800 |
C1—N11 | 1.350 (7) | N36—H36A | 0.8800 |
C2—N32 | 1.326 (6) | N36—H36B | 0.8800 |
C2—N12 | 1.328 (5) | O1W—H1OW | 0.8600 |
C2—N22 | 1.330 (6) | O1W—H2OW | 0.8620 |
O1A—Mo1—O1B | 106.28 (16) | O467—Mo6—Mo3 | 86.03 (7) |
O1A—Mo1—O12 | 97.62 (14) | O7B—Mo7—O7A | 105.95 (16) |
O1B—Mo1—O12 | 102.41 (14) | O7B—Mo7—O67 | 101.99 (14) |
O1A—Mo1—O13 | 100.22 (14) | O7A—Mo7—O67 | 97.60 (14) |
O1B—Mo1—O13 | 92.39 (14) | O7B—Mo7—O57 | 93.52 (14) |
O12—Mo1—O13 | 152.57 (12) | O7A—Mo7—O57 | 99.81 (14) |
O1A—Mo1—O1M4 | 96.18 (13) | O67—Mo7—O57 | 152.48 (12) |
O1B—Mo1—O1M4 | 154.88 (14) | O7B—Mo7—O2M4 | 155.59 (14) |
O12—Mo1—O1M4 | 85.24 (11) | O7A—Mo7—O2M4 | 96.25 (13) |
O13—Mo1—O1M4 | 72.31 (11) | O67—Mo7—O2M4 | 84.65 (11) |
O1A—Mo1—O124 | 164.91 (13) | O57—Mo7—O2M4 | 72.44 (11) |
O1B—Mo1—O124 | 87.97 (13) | O7B—Mo7—O467 | 88.02 (13) |
O12—Mo1—O124 | 73.97 (11) | O7A—Mo7—O467 | 164.99 (14) |
O13—Mo1—O124 | 83.74 (11) | O67—Mo7—O467 | 73.65 (11) |
O1M4—Mo1—O124 | 70.99 (10) | O57—Mo7—O467 | 84.44 (11) |
O1A—Mo1—Mo3 | 88.18 (11) | O2M4—Mo7—O467 | 71.16 (10) |
O1B—Mo1—Mo3 | 126.50 (11) | O7B—Mo7—Mo5 | 127.59 (11) |
O12—Mo1—Mo3 | 126.89 (9) | O7A—Mo7—Mo5 | 88.33 (11) |
O13—Mo1—Mo3 | 34.13 (9) | O67—Mo7—Mo5 | 126.26 (9) |
O1M4—Mo1—Mo3 | 41.71 (7) | O57—Mo7—Mo5 | 34.08 (9) |
O124—Mo1—Mo3 | 87.15 (7) | O2M4—Mo7—Mo5 | 41.66 (7) |
O2A—Mo2—O2B | 104.26 (15) | O467—Mo7—Mo5 | 87.32 (7) |
O2A—Mo2—O12 | 99.18 (14) | Mo2—O12—Mo1 | 114.96 (15) |
O2B—Mo2—O12 | 100.77 (14) | Mo3—O13—Mo1 | 110.45 (14) |
O2A—Mo2—O25 | 99.57 (14) | Mo3—O1M4—Mo6 | 97.06 (11) |
O2B—Mo2—O25 | 90.51 (14) | Mo3—O1M4—Mo1 | 95.78 (11) |
O12—Mo2—O25 | 154.96 (12) | Mo6—O1M4—Mo1 | 150.49 (15) |
O2A—Mo2—O2M4 | 95.94 (13) | Mo3—O1M4—Mo4 | 101.69 (12) |
O2B—Mo2—O2M4 | 155.53 (13) | Mo6—O1M4—Mo4 | 101.69 (11) |
O12—Mo2—O2M4 | 89.29 (11) | Mo1—O1M4—Mo4 | 101.56 (11) |
O25—Mo2—O2M4 | 72.40 (11) | Mo2—O2M4—Mo5 | 97.31 (11) |
O2A—Mo2—O124 | 166.43 (13) | Mo2—O2M4—Mo7 | 151.10 (15) |
O2B—Mo2—O124 | 89.00 (13) | Mo5—O2M4—Mo7 | 95.61 (11) |
O12—Mo2—O124 | 75.04 (11) | Mo2—O2M4—Mo4 | 101.50 (11) |
O25—Mo2—O124 | 82.96 (11) | Mo5—O2M4—Mo4 | 101.59 (11) |
O2M4—Mo2—O124 | 71.98 (10) | Mo7—O2M4—Mo4 | 101.07 (11) |
O2A—Mo2—Mo5 | 88.60 (11) | Mo5—O25—Mo2 | 109.26 (14) |
O2B—Mo2—Mo5 | 124.49 (11) | Mo3—O36—Mo6 | 109.60 (14) |
O12—Mo2—Mo5 | 130.65 (9) | Mo5—O57—Mo7 | 110.69 (14) |
O25—Mo2—Mo5 | 34.02 (8) | Mo6—O67—Mo7 | 115.34 (15) |
O2M4—Mo2—Mo5 | 41.36 (7) | Mo4—O124—Mo2 | 109.78 (13) |
O124—Mo2—Mo5 | 86.20 (7) | Mo4—O124—Mo1 | 110.17 (12) |
O3B—Mo3—O3A | 104.96 (16) | Mo2—O124—Mo1 | 90.79 (10) |
O3B—Mo3—O36 | 98.70 (15) | Mo4—O467—Mo6 | 109.92 (13) |
O3A—Mo3—O36 | 103.26 (14) | Mo4—O467—Mo7 | 110.30 (13) |
O3B—Mo3—O13 | 98.61 (14) | Mo6—O467—Mo7 | 91.11 (10) |
O3A—Mo3—O13 | 98.55 (14) | N31—C1—N21 | 120.9 (5) |
O36—Mo3—O13 | 147.48 (12) | N31—C1—N11 | 118.1 (5) |
O3B—Mo3—O1M4 | 104.31 (14) | N21—C1—N11 | 120.9 (5) |
O3A—Mo3—O1M4 | 150.60 (13) | N32—C2—N12 | 120.0 (4) |
O36—Mo3—O1M4 | 74.87 (11) | N32—C2—N22 | 120.1 (4) |
O13—Mo3—O1M4 | 74.28 (11) | N12—C2—N22 | 119.8 (4) |
O3B—Mo3—Mo1 | 91.43 (11) | N13—C3—N33 | 119.9 (4) |
O3A—Mo3—Mo1 | 133.64 (11) | N13—C3—N23 | 120.1 (4) |
O36—Mo3—Mo1 | 116.92 (9) | N33—C3—N23 | 120.0 (4) |
O13—Mo3—Mo1 | 35.43 (9) | N14—C4—N34 | 120.1 (4) |
O1M4—Mo3—Mo1 | 42.52 (7) | N14—C4—N24 | 119.8 (4) |
O3B—Mo3—Mo6 | 92.46 (12) | N34—C4—N24 | 120.1 (5) |
O3A—Mo3—Mo6 | 138.95 (11) | N15—C5—N35 | 120.1 (4) |
O36—Mo3—Mo6 | 36.46 (9) | N15—C5—N25 | 119.3 (4) |
O13—Mo3—Mo6 | 115.49 (9) | N35—C5—N25 | 120.6 (4) |
O1M4—Mo3—Mo6 | 41.57 (7) | N16—C6—N36 | 120.1 (4) |
Mo1—Mo3—Mo6 | 81.340 (13) | N16—C6—N26 | 121.2 (4) |
O34—Mo4—O45 | 104.71 (17) | N36—C6—N26 | 118.6 (4) |
O34—Mo4—O124 | 101.08 (13) | C1—N11—H11A | 120.0 |
O45—Mo4—O124 | 100.86 (13) | C1—N11—H11B | 120.0 |
O34—Mo4—O467 | 101.26 (13) | H11A—N11—H11B | 120.0 |
O45—Mo4—O467 | 101.58 (13) | C2—N12—H12A | 120.0 |
O124—Mo4—O467 | 142.93 (14) | C2—N12—H12B | 120.0 |
O34—Mo4—O1M4 | 83.76 (13) | H12A—N12—H12B | 120.0 |
O45—Mo4—O1M4 | 171.52 (13) | C3—N13—H13A | 120.0 |
O124—Mo4—O1M4 | 76.79 (11) | C3—N13—H13B | 120.0 |
O467—Mo4—O1M4 | 76.67 (11) | H13A—N13—H13B | 120.0 |
O34—Mo4—O2M4 | 171.58 (12) | C4—N14—H14A | 120.0 |
O45—Mo4—O2M4 | 83.71 (12) | C4—N14—H14B | 120.0 |
O124—Mo4—O2M4 | 76.66 (11) | H14A—N14—H14B | 120.0 |
O467—Mo4—O2M4 | 76.92 (11) | C5—N15—H15A | 120.0 |
O1M4—Mo4—O2M4 | 87.82 (11) | C5—N15—H15B | 120.0 |
O5B—Mo5—O5A | 104.80 (16) | H15A—N15—H15B | 120.0 |
O5B—Mo5—O25 | 98.17 (14) | C6—N16—H16A | 120.0 |
O5A—Mo5—O25 | 102.93 (14) | C6—N16—H16B | 120.0 |
O5B—Mo5—O57 | 98.72 (14) | H16A—N16—H16B | 120.0 |
O5A—Mo5—O57 | 99.06 (15) | C1—N21—H21A | 120.0 |
O25—Mo5—O57 | 147.72 (12) | C1—N21—H21B | 120.0 |
O5B—Mo5—O2M4 | 103.37 (13) | H21A—N21—H21B | 120.0 |
O5A—Mo5—O2M4 | 151.75 (13) | C2—N22—H22A | 120.0 |
O25—Mo5—O2M4 | 74.91 (11) | C2—N22—H22B | 120.0 |
O57—Mo5—O2M4 | 74.52 (11) | H22A—N22—H22B | 120.0 |
O5B—Mo5—Mo7 | 91.35 (11) | C3—N23—H23A | 120.0 |
O5A—Mo5—Mo7 | 134.00 (11) | C3—N23—H23B | 120.0 |
O25—Mo5—Mo7 | 117.25 (9) | H23A—N23—H23B | 120.0 |
O57—Mo5—Mo7 | 35.23 (9) | C4—N24—H24A | 120.0 |
O2M4—Mo5—Mo7 | 42.73 (7) | C4—N24—H24B | 120.0 |
O5B—Mo5—Mo2 | 91.60 (11) | H24A—N24—H24B | 120.0 |
O5A—Mo5—Mo2 | 139.02 (11) | C5—N25—H25A | 120.0 |
O25—Mo5—Mo2 | 36.72 (9) | C5—N25—H25B | 120.0 |
O57—Mo5—Mo2 | 115.50 (9) | H25A—N25—H25B | 120.0 |
O2M4—Mo5—Mo2 | 41.33 (7) | C6—N26—H26A | 120.0 |
Mo7—Mo5—Mo2 | 81.460 (12) | C6—N26—H26B | 120.0 |
O6A—Mo6—O6B | 105.22 (15) | H26A—N26—H26B | 120.0 |
O6A—Mo6—O67 | 99.29 (14) | C1—N31—H31A | 120.0 |
O6B—Mo6—O67 | 100.69 (14) | C1—N31—H31B | 120.0 |
O6A—Mo6—O36 | 99.78 (15) | H31A—N31—H31B | 120.0 |
O6B—Mo6—O36 | 91.00 (14) | C2—N32—H32A | 120.0 |
O67—Mo6—O36 | 154.12 (12) | C2—N32—H32B | 120.0 |
O6A—Mo6—O1M4 | 95.27 (14) | H32A—N32—H32B | 120.0 |
O6B—Mo6—O1M4 | 155.62 (14) | C3—N33—H33A | 120.0 |
O67—Mo6—O1M4 | 88.66 (12) | C3—N33—H33B | 120.0 |
O36—Mo6—O1M4 | 72.31 (11) | H33A—N33—H33B | 120.0 |
O6A—Mo6—O467 | 165.28 (13) | C4—N34—H34A | 120.0 |
O6B—Mo6—O467 | 89.13 (13) | C4—N34—H34B | 120.0 |
O67—Mo6—O467 | 74.30 (11) | H34A—N34—H34B | 120.0 |
O36—Mo6—O467 | 82.95 (11) | C5—N35—H35A | 120.0 |
O1M4—Mo6—O467 | 71.64 (10) | C5—N35—H35B | 120.0 |
O6A—Mo6—Mo3 | 88.34 (12) | H35A—N35—H35B | 120.0 |
O6B—Mo6—Mo3 | 124.90 (11) | C6—N36—H36A | 120.0 |
O67—Mo6—Mo3 | 130.03 (9) | C6—N36—H36B | 120.0 |
O36—Mo6—Mo3 | 33.93 (8) | H36A—N36—H36B | 120.0 |
O1M4—Mo6—Mo3 | 41.37 (7) | H1OW—O1W—H2OW | 105.7 |
D—H···A | D—H | H···A | D···A | D—H···A |
N11—H11A···O1W | 0.88 | 1.90 | 2.765 (6) | 168 |
N11—H11B···O3A | 0.88 | 2.35 | 3.091 (6) | 142 |
N12—H12A···O2Ai | 0.88 | 2.00 | 2.845 (5) | 160 |
N12—H12B···O5B | 0.88 | 2.14 | 2.903 (5) | 145 |
N13—H13A···O6Aii | 0.88 | 1.96 | 2.828 (5) | 169 |
N13—H13B···O3B | 0.88 | 2.23 | 2.930 (5) | 136 |
N14—H14B···O13 | 0.88 | 1.93 | 2.774 (4) | 159 |
N14—H14A···O57iii | 0.88 | 1.98 | 2.814 (4) | 159 |
N15—H15A···O2Biv | 0.88 | 2.03 | 2.843 (5) | 153 |
N15—H15B···O3Av | 0.88 | 2.13 | 2.866 (5) | 141 |
N15—H15B···O34v | 0.88 | 2.62 | 3.302 (5) | 135 |
N16—H16B···O1Aii | 0.88 | 2.13 | 2.967 (5) | 159 |
N16—H16A···O45vi | 0.88 | 2.18 | 2.977 (5) | 151 |
N21—H21A···O1Bvi | 0.88 | 2.18 | 3.006 (5) | 156 |
N21—H21A···O2Bvi | 0.88 | 2.40 | 2.926 (5) | 118 |
N21—H21B···O3A | 0.88 | 2.22 | 2.992 (5) | 147 |
N22—H22A···O36vii | 0.88 | 2.32 | 3.087 (5) | 145 |
N22—H22A···O467vii | 0.88 | 2.50 | 3.216 (5) | 139 |
N22—H22A···O6Bvii | 0.88 | 2.64 | 3.290 (5) | 131 |
N22—H22B···O25 | 0.88 | 2.10 | 2.977 (5) | 177 |
N23—H23A···O36 | 0.88 | 2.07 | 2.937 (5) | 169 |
N23—H23B···O25vi | 0.88 | 2.26 | 3.023 (5) | 145 |
N23—H23B···O124vi | 0.88 | 2.50 | 3.219 (5) | 140 |
N24—H24A···O13 | 0.88 | 2.45 | 3.154 (5) | 137 |
N24—H24A···O3A | 0.88 | 2.50 | 3.186 (5) | 135 |
N24—H24B···O12viii | 0.88 | 2.09 | 2.855 (5) | 145 |
N25—H25A···O34v | 0.88 | 2.22 | 2.990 (5) | 146 |
N25—H25B···O7Aiii | 0.88 | 2.08 | 2.931 (5) | 162 |
N26—H26A···O3Bii | 0.88 | 1.98 | 2.859 (5) | 175 |
N26—H26B···O1Wii | 0.88 | 2.50 | 3.084 (6) | 124 |
N26—H26B···O6A | 0.88 | 2.57 | 3.197 (5) | 129 |
N31—H31A···O1Bvi | 0.88 | 2.50 | 3.248 (6) | 143 |
N31—H31B···O5Aix | 0.88 | 2.38 | 3.188 (6) | 152 |
N32—H32A···N34x | 0.88 | 2.50 | 3.242 (6) | 143 |
N32—H32B···O467vii | 0.88 | 2.02 | 2.864 (5) | 160 |
N33—H33A···N24vi | 0.88 | 2.60 | 3.334 (6) | 142 |
N33—H33B···O124vi | 0.88 | 2.02 | 2.867 (5) | 160 |
N34—H34B···O67viii | 0.88 | 1.94 | 2.776 (5) | 157 |
N34—H34A···O57iii | 0.88 | 2.44 | 3.154 (5) | 139 |
N34—H34A···O5Aiii | 0.88 | 2.55 | 3.195 (5) | 131 |
N35—H35A···O2Aiv | 0.88 | 2.29 | 3.040 (5) | 144 |
N35—H35B···O5Biii | 0.88 | 1.98 | 2.849 (5) | 170 |
N36—H36A···O5Avi | 0.88 | 2.16 | 2.913 (5) | 144 |
N36—H36B···O6B | 0.88 | 2.13 | 2.868 (5) | 141 |
O1W—H1OW···O6Biii | 0.86 | 2.22 | 2.948 (5) | 142.0 |
O1W—H1OW···O7Biii | 0.86 | 2.44 | 3.086 (5) | 132.8 |
O1W—H2OW···O5Aix | 0.86 | 2.35 | 2.973 (5) | 129.6 |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x, −y, −z+1; (iii) x−1, y, z; (iv) −x, −y, −z; (v) −x, y−1/2, −z+1/2; (vi) x, −y+1/2, z+1/2; (vii) x, −y+1/2, z−1/2; (viii) −x, y+1/2, −z+1/2; (ix) x−1, −y+1/2, z+1/2; (x) x+1, −y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | (CH6N3)6[Mo7O24]·H2O |
Mr | 1434.12 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 173 |
a, b, c (Å) | 11.9402 (6), 15.9131 (9), 19.8223 (13) |
β (°) | 92.312 (4) |
V (Å3) | 3763.3 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.37 |
Crystal size (mm) | 0.17 × 0.17 × 0.08 |
Data collection | |
Diffractometer | Bruker X8 APEXII CCD area-detector diffractometer |
Absorption correction | Multi-scan APEXII (Bruker, 2005) |
Tmin, Tmax | 0.689, 0.833 |
No. of measured, independent and observed [I > 2s(I)] reflections | 153838, 15842, 9689 |
Rint | 0.150 |
(sin θ/λ)max (Å−1) | 0.796 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.053, 0.164, 1.06 |
No. of reflections | 15842 |
No. of parameters | 506 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.77, −2.33 |
Computer programs: APEX2 (Bruker, 2005), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
N11—H11A···O1W | 0.88 | 1.90 | 2.765 (6) | 167.8 |
N11—H11B···O3A | 0.88 | 2.35 | 3.091 (6) | 141.6 |
N12—H12A···O2Ai | 0.88 | 2.00 | 2.845 (5) | 160.3 |
N12—H12B···O5B | 0.88 | 2.14 | 2.903 (5) | 145.2 |
N13—H13A···O6Aii | 0.88 | 1.96 | 2.828 (5) | 169.3 |
N13—H13B···O3B | 0.88 | 2.23 | 2.930 (5) | 135.7 |
N14—H14B···O13 | 0.88 | 1.93 | 2.774 (4) | 158.9 |
N14—H14A···O57iii | 0.88 | 1.98 | 2.814 (4) | 158.6 |
N15—H15A···O2Biv | 0.88 | 2.03 | 2.843 (5) | 152.9 |
N15—H15B···O3Av | 0.88 | 2.13 | 2.866 (5) | 140.7 |
N15—H15B···O34v | 0.88 | 2.62 | 3.302 (5) | 135.1 |
N16—H16B···O1Aii | 0.88 | 2.13 | 2.967 (5) | 158.5 |
N16—H16A···O45vi | 0.88 | 2.18 | 2.977 (5) | 150.9 |
N21—H21A···O1Bvi | 0.88 | 2.18 | 3.006 (5) | 156.4 |
N21—H21A···O2Bvi | 0.88 | 2.40 | 2.926 (5) | 118.4 |
N21—H21B···O3A | 0.88 | 2.22 | 2.992 (5) | 146.5 |
N22—H22A···O36vii | 0.88 | 2.32 | 3.087 (5) | 145.3 |
N22—H22A···O467vii | 0.88 | 2.50 | 3.216 (5) | 139.4 |
N22—H22A···O6Bvii | 0.88 | 2.64 | 3.290 (5) | 131.2 |
N22—H22B···O25 | 0.88 | 2.10 | 2.977 (5) | 176.5 |
N23—H23A···O36 | 0.88 | 2.07 | 2.937 (5) | 169.3 |
N23—H23B···O25vi | 0.88 | 2.26 | 3.023 (5) | 145.4 |
N23—H23B···O124vi | 0.88 | 2.50 | 3.219 (5) | 139.6 |
N24—H24A···O13 | 0.88 | 2.45 | 3.154 (5) | 136.9 |
N24—H24A···O3A | 0.88 | 2.50 | 3.186 (5) | 134.8 |
N24—H24B···O12viii | 0.88 | 2.09 | 2.855 (5) | 145.0 |
N25—H25A···O34v | 0.88 | 2.22 | 2.990 (5) | 145.9 |
N25—H25B···O7Aiii | 0.88 | 2.08 | 2.931 (5) | 162.2 |
N26—H26A···O3Bii | 0.88 | 1.98 | 2.859 (5) | 175.0 |
N26—H26B···O1Wii | 0.88 | 2.50 | 3.084 (6) | 124.2 |
N26—H26B···O6A | 0.88 | 2.57 | 3.197 (5) | 129.4 |
N31—H31A···O1Bvi | 0.88 | 2.50 | 3.248 (6) | 142.8 |
N31—H31B···O5Aix | 0.88 | 2.38 | 3.188 (6) | 152.4 |
N32—H32A···N34x | 0.88 | 2.50 | 3.242 (6) | 142.9 |
N32—H32B···O467vii | 0.88 | 2.02 | 2.864 (5) | 159.9 |
N33—H33A···N24vi | 0.88 | 2.60 | 3.334 (6) | 141.7 |
N33—H33B···O124vi | 0.88 | 2.02 | 2.867 (5) | 160.2 |
N34—H34B···O67viii | 0.88 | 1.94 | 2.776 (5) | 157.4 |
N34—H34A···O57iii | 0.88 | 2.44 | 3.154 (5) | 138.8 |
N34—H34A···O5Aiii | 0.88 | 2.55 | 3.195 (5) | 131.2 |
N35—H35A···O2Aiv | 0.88 | 2.29 | 3.040 (5) | 143.7 |
N35—H35B···O5Biii | 0.88 | 1.98 | 2.849 (5) | 169.5 |
N36—H36A···O5Avi | 0.88 | 2.16 | 2.913 (5) | 143.5 |
N36—H36B···O6B | 0.88 | 2.13 | 2.868 (5) | 140.5 |
O1W—H1OW···O6Biii | 0.86 | 2.22 | 2.948 (5) | 142.0 |
O1W—H1OW···O7Biii | 0.86 | 2.44 | 3.086 (5) | 132.8 |
O1W—H2OW···O5Aix | 0.86 | 2.35 | 2.973 (5) | 129.6 |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x, −y, −z+1; (iii) x−1, y, z; (iv) −x, −y, −z; (v) −x, y−1/2, −z+1/2; (vi) x, −y+1/2, z+1/2; (vii) x, −y+1/2, z−1/2; (viii) −x, y+1/2, −z+1/2; (ix) x−1, −y+1/2, z+1/2; (x) x+1, −y+1/2, z−1/2. |
Acknowledgements
SR thanks Gobierno Vasco/Eusko Jaurlaritza for his postdoctoral fellowship.
References
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Acidification of aqueous molybdate solutions gives rise to the formation of different isopolymolybdate(VI) anions depending on the pH. The heptamolybdate anion, [Mo7O24]6-, is known to be the predominant species in neutral to moderately acidic solutions (Pope, 1983). Single crystals of the title compound, [C(NH2)3]6[Mo7O24].H2O (I), were obtained in an attempt to prepare a guanidinium salt of a dimethyltin-containing phosphomolybdate species.
Routine examination of (I) at low temperature resulted in the assignment of the monoclinic space group P21/c, with the C-centered reflections being systematically weak. However, a previous room-temperature study using Weissenberg techniques reported the structure of (I) in the monoclinic space group C2/c (Don & Weakley, 1981). Therefore, data were collected on a second crystal at room temperature, confirming the original assignment of C2/c; data were then collected on this same crystal cooled to 173 K, confirming the low-temperature assignment of P21/c. The value of Rint for the low-temperature data was 15.0%. We attribute this higher than usual value to the phase change; the value of Rint for the room-temperature data was less than 10%. The low-temperature structure consists of one [Mo7O24]6- anion, six [C(NH2)3]+ cations, and one molecule of water of hydration in the asymmetric unit (Fig. 1). The [Mo7O24]6- anion shows the well known bent arrangement of seven edge-sharing MoO6 distorted octahedra (Kortz & Pope, 1995), which can be formally derived from the parent {M10O28} decametalate framework by removal of three octahedra from the central level (Pope, 1983). The anions and the cations are linked by an extensive and intricate three-dimensional network of N—H···O hydrogen bonds involving all guanidinium –NH2 groups and all heptamolybdate terminal and bridging O atoms, with the exception of the terminal O7B and the bridging µ4-O atoms (O1M4 and O2M4).