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In the title dinuclear complex, [Mo2(C6H8N3O2)2O4]·3H2O, the Mo atoms, bridged by two μ-oxo atoms, have a distorted octa­hedral coordination environment. Besides the two bridging O atoms, the coordination of each Mo atom is completed by a terminal oxo atom and a tridentate histidinate ligand. The short Mo...Mo distance of 2.5458 (4) Å may indicate the existence of an Mo—Mo metal bond. Inter­molecular hydrogen bonding between the uncoordinated carboxyl­ate O atoms and amino groups leads to a layer-like arrangement of the mol­ecules. The uncoordinated water mol­ecules link these layers via O—H...O hydrogen bonds and help to stabilize the crystal packing.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805021732/cv6543sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805021732/cv6543Isup2.hkl
Contains datablock I

CCDC reference: 282307

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.020
  • wR factor = 0.049
  • Data-to-parameter ratio = 12.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 27.00 From the CIF: _reflns_number_total 3372 Count of symmetry unique reflns 2370 Completeness (_total/calc) 142.28% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1002 Fraction of Friedel pairs measured 0.423 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2003); software used to prepare material for publication: SHELXTL.

Di-µ-oxo-bis[(histidinato-κ3N,N,O)oxomolybdenum(V)] trihydrate top
Crystal data top
[Mo2(C6H8N3O2)2O4]·3H2OF(000) = 616
Mr = 618.24Dx = 2.017 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 5483 reflections
a = 10.9594 (12) Åθ = 3.0–28.3°
b = 8.7222 (9) ŵ = 1.30 mm1
c = 11.5783 (12) ÅT = 292 K
β = 113.136 (2)°Block, yellow
V = 1017.76 (19) Å30.3 × 0.2 × 0.2 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
3372 independent reflections
Radiation source: fine-focus sealed tube3343 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
φ and ω scansθmax = 27.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1313
Tmin = 0.696, Tmax = 0.781k = 511
5964 measured reflectionsl = 1214
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.020H-atom parameters constrained
wR(F2) = 0.049 w = 1/[σ2(Fo2) + (0.0218P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max = 0.001
3372 reflectionsΔρmax = 0.33 e Å3
280 parametersΔρmin = 0.69 e Å3
1 restraintAbsolute structure: Flack (1983), with 1006 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.03 (3)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.84113 (2)0.47077 (3)0.58675 (2)0.02049 (7)
Mo20.60843 (2)0.52951 (3)0.42698 (2)0.02015 (6)
O10.9534 (2)0.0052 (3)0.6463 (2)0.0343 (5)
O20.83566 (18)0.2183 (3)0.57700 (18)0.0262 (5)
O30.3375 (2)0.2042 (3)0.2237 (2)0.0363 (5)
O40.52055 (19)0.3008 (3)0.37024 (19)0.0262 (5)
O50.76353 (18)0.4547 (3)0.40437 (17)0.0248 (5)
O60.67035 (19)0.4624 (3)0.59928 (17)0.0264 (4)
O70.6098 (2)0.7245 (3)0.4264 (2)0.0321 (5)
O80.9057 (2)0.6498 (3)0.6190 (2)0.0339 (5)
O90.8483 (2)0.3550 (4)0.1685 (2)0.0449 (7)
H9A0.90850.38770.23600.054*
H9B0.83390.26120.17870.054*
O100.7517 (2)0.1325 (3)0.2968 (2)0.0411 (6)
H10C0.68230.07830.27950.049*
H10D0.75710.19350.35590.049*
O110.5041 (2)0.9766 (4)0.2157 (2)0.0454 (6)
H11A0.45931.04130.23770.055*
H11B0.50100.89070.24910.055*
N10.9250 (2)0.4029 (3)0.7868 (2)0.0251 (5)
N20.9300 (3)0.3579 (4)0.9738 (2)0.0321 (6)
H20.90730.35751.03690.039*
N31.0342 (2)0.3858 (3)0.5867 (2)0.0268 (6)
H3A1.02650.37150.50710.032*
H3B1.09800.45610.62270.032*
N40.5089 (2)0.5407 (4)0.2183 (2)0.0264 (5)
N50.4759 (3)0.5350 (5)0.0202 (2)0.0434 (7)
H50.49140.53150.04700.052*
N60.4094 (2)0.5204 (4)0.4346 (2)0.0263 (5)
H6A0.41400.47050.50430.032*
H6B0.37940.61600.43670.032*
C10.8636 (3)0.4229 (4)0.8639 (3)0.0290 (7)
H10.78420.47580.84330.035*
C21.0414 (3)0.2910 (4)0.9695 (3)0.0334 (7)
H2A1.10590.23641.03350.040*
C31.0390 (3)0.3203 (4)0.8534 (3)0.0265 (6)
C41.1346 (3)0.2688 (4)0.7981 (3)0.0305 (7)
H4A1.17710.17520.83980.037*
H4B1.20300.34620.81510.037*
C51.0715 (3)0.2398 (4)0.6567 (3)0.0260 (6)
H5A1.13460.18470.63090.031*
C60.9450 (3)0.1432 (4)0.6242 (3)0.0249 (6)
C70.5670 (3)0.5272 (5)0.1374 (3)0.0355 (7)
H70.65760.51420.15930.043*
C80.3538 (3)0.5496 (5)0.0250 (3)0.0381 (8)
H80.27260.55620.04290.046*
C90.3746 (3)0.5526 (4)0.1477 (3)0.0274 (7)
C100.2760 (3)0.5476 (4)0.2090 (3)0.0319 (7)
H10A0.19050.51530.14750.038*
H10B0.26580.64990.23680.038*
C110.3183 (3)0.4387 (4)0.3211 (3)0.0274 (7)
H110.24000.40320.33450.033*
C120.3944 (3)0.3018 (4)0.3023 (3)0.0248 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01965 (11)0.01993 (12)0.02006 (11)0.00022 (10)0.00585 (9)0.00066 (10)
Mo20.01999 (11)0.02074 (12)0.01889 (11)0.00110 (10)0.00673 (8)0.00040 (10)
O10.0365 (12)0.0246 (15)0.0453 (12)0.0047 (10)0.0198 (10)0.0017 (10)
O20.0222 (10)0.0228 (12)0.0302 (11)0.0003 (9)0.0068 (8)0.0017 (9)
O30.0312 (11)0.0285 (13)0.0423 (13)0.0079 (11)0.0070 (10)0.0033 (11)
O40.0209 (10)0.0234 (12)0.0327 (11)0.0004 (9)0.0088 (8)0.0006 (10)
O50.0221 (9)0.0331 (13)0.0200 (9)0.0021 (10)0.0091 (7)0.0006 (10)
O60.0256 (10)0.0332 (11)0.0208 (9)0.0033 (11)0.0095 (8)0.0014 (10)
O70.0372 (13)0.0214 (12)0.0343 (12)0.0012 (10)0.0104 (10)0.0002 (9)
O80.0318 (12)0.0236 (12)0.0394 (13)0.0027 (10)0.0064 (10)0.0019 (11)
O90.0499 (15)0.0533 (18)0.0353 (13)0.0127 (15)0.0209 (11)0.0090 (13)
O100.0369 (12)0.0483 (16)0.0402 (13)0.0018 (13)0.0175 (10)0.0116 (13)
O110.0542 (15)0.0463 (16)0.0445 (13)0.0002 (14)0.0288 (12)0.0005 (14)
N10.0243 (12)0.0263 (13)0.0226 (11)0.0045 (11)0.0069 (10)0.0007 (11)
N20.0377 (14)0.0373 (16)0.0224 (12)0.0042 (13)0.0129 (11)0.0019 (12)
N30.0254 (12)0.0271 (16)0.0284 (13)0.0015 (11)0.0111 (10)0.0000 (11)
N40.0262 (12)0.0291 (14)0.0222 (11)0.0014 (13)0.0075 (9)0.0032 (12)
N50.0480 (16)0.063 (2)0.0233 (12)0.0087 (18)0.0180 (12)0.0009 (16)
N60.0254 (11)0.0302 (14)0.0248 (11)0.0065 (13)0.0116 (9)0.0011 (12)
C10.0287 (15)0.0300 (16)0.0268 (14)0.0054 (13)0.0093 (12)0.0030 (13)
C20.0337 (16)0.0338 (19)0.0273 (15)0.0055 (15)0.0062 (13)0.0016 (14)
C30.0257 (14)0.0262 (16)0.0227 (13)0.0016 (13)0.0044 (11)0.0023 (12)
C40.0223 (14)0.0338 (18)0.0310 (16)0.0021 (14)0.0058 (12)0.0024 (14)
C50.0248 (14)0.0247 (16)0.0278 (14)0.0016 (12)0.0097 (12)0.0033 (12)
C60.0291 (14)0.0260 (16)0.0220 (13)0.0033 (13)0.0127 (11)0.0025 (12)
C70.0313 (15)0.0478 (19)0.0296 (15)0.0045 (18)0.0143 (12)0.0010 (18)
C80.0351 (16)0.047 (2)0.0269 (15)0.0031 (17)0.0064 (13)0.0011 (16)
C90.0275 (14)0.0258 (18)0.0254 (13)0.0029 (13)0.0066 (11)0.0051 (13)
C100.0233 (14)0.036 (2)0.0305 (15)0.0082 (15)0.0040 (12)0.0051 (15)
C110.0194 (13)0.033 (2)0.0313 (15)0.0005 (12)0.0114 (11)0.0023 (13)
C120.0234 (13)0.0248 (16)0.0267 (14)0.0025 (13)0.0104 (11)0.0059 (12)
Geometric parameters (Å, º) top
Mo1—O81.695 (2)N3—H3A0.9000
Mo1—O61.9347 (19)N3—H3B0.9000
Mo1—O51.9470 (19)N4—C71.329 (4)
Mo1—O22.205 (2)N4—C91.378 (4)
Mo1—N12.210 (2)N5—C71.334 (4)
Mo1—N32.242 (2)N5—C81.367 (4)
Mo1—Mo22.5458 (4)N5—H50.8600
Mo2—O71.701 (3)N6—C111.483 (4)
Mo2—O61.9286 (19)N6—H6A0.9000
Mo2—O51.932 (2)N6—H6B0.9000
Mo2—O42.201 (2)C1—H10.9300
Mo2—N62.219 (2)C2—C31.359 (4)
Mo2—N42.228 (2)C2—H2A0.9300
O1—C61.226 (4)C3—C41.495 (4)
O2—C61.284 (4)C4—C51.528 (4)
O3—C121.223 (4)C4—H4A0.9700
O4—C121.295 (3)C4—H4B0.9700
O9—H9A0.8500C5—C61.538 (4)
O9—H9B0.8499C5—H5A0.9800
O10—H10C0.8500C7—H70.9300
O10—H10D0.8500C8—C91.348 (4)
O11—H11A0.8501C8—H80.9300
O11—H11B0.8500C9—C101.508 (4)
N1—C11.324 (4)C10—C111.526 (4)
N1—C31.384 (4)C10—H10A0.9700
N2—C11.320 (4)C10—H10B0.9700
N2—C21.371 (4)C11—C121.520 (4)
N2—H20.8600C11—H110.9800
N3—C51.478 (4)
O8—Mo1—O6110.53 (11)C7—N4—C9106.5 (2)
O8—Mo1—O5105.78 (11)C7—N4—Mo2126.4 (2)
O6—Mo1—O593.18 (8)C9—N4—Mo2126.89 (19)
O8—Mo1—O2158.82 (9)C7—N5—C8108.5 (2)
O6—Mo1—O287.62 (10)C7—N5—H5125.8
O5—Mo1—O283.17 (9)C8—N5—H5125.8
O8—Mo1—N192.88 (11)C11—N6—Mo2108.16 (16)
O6—Mo1—N185.85 (9)C11—N6—H6A110.1
O5—Mo1—N1160.33 (11)Mo2—N6—H6A110.1
O2—Mo1—N177.16 (9)C11—N6—H6B110.1
O8—Mo1—N389.56 (11)Mo2—N6—H6B110.1
O6—Mo1—N3158.19 (10)H6A—N6—H6B108.4
O5—Mo1—N389.20 (9)N2—C1—N1111.1 (3)
O2—Mo1—N371.12 (9)N2—C1—H1124.5
N1—Mo1—N384.70 (9)N1—C1—H1124.5
O8—Mo1—Mo2100.78 (8)C3—C2—N2106.5 (3)
O6—Mo1—Mo248.67 (6)C3—C2—H2A126.7
O5—Mo1—Mo248.73 (6)N2—C2—H2A126.7
O2—Mo1—Mo299.47 (5)C2—C3—N1108.2 (3)
N1—Mo1—Mo2134.48 (6)C2—C3—C4128.5 (3)
N3—Mo1—Mo2137.94 (7)N1—C3—C4123.2 (3)
O7—Mo2—O6107.89 (11)C3—C4—C5114.3 (2)
O7—Mo2—O5109.13 (11)C3—C4—H4A108.7
O6—Mo2—O593.84 (8)C5—C4—H4A108.7
O7—Mo2—O4155.36 (9)C3—C4—H4B108.7
O6—Mo2—O488.20 (10)C5—C4—H4B108.7
O5—Mo2—O487.62 (9)H4A—C4—H4B107.6
O7—Mo2—N692.66 (12)N3—C5—C4110.9 (3)
O6—Mo2—N684.24 (9)N3—C5—C6108.0 (2)
O5—Mo2—N6157.55 (11)C4—C5—C6109.7 (2)
O4—Mo2—N669.98 (10)N3—C5—H5A109.4
O7—Mo2—N487.35 (12)C4—C5—H5A109.4
O6—Mo2—N4163.38 (11)C6—C5—H5A109.4
O5—Mo2—N487.13 (9)O1—C6—O2124.7 (3)
O4—Mo2—N475.25 (10)O1—C6—C5120.1 (3)
N6—Mo2—N488.54 (8)O2—C6—C5115.2 (3)
O7—Mo2—Mo1101.31 (7)N4—C7—N5109.8 (3)
O6—Mo2—Mo148.88 (6)N4—C7—H7125.1
O5—Mo2—Mo149.24 (6)N5—C7—H7125.1
O4—Mo2—Mo1103.32 (5)C9—C8—N5106.4 (3)
N6—Mo2—Mo1133.12 (6)C9—C8—H8126.8
N4—Mo2—Mo1136.11 (6)N5—C8—H8126.8
C6—O2—Mo1119.0 (2)C8—C9—N4108.8 (3)
C12—O4—Mo2114.4 (2)C8—C9—C10129.8 (3)
Mo2—O5—Mo182.03 (8)N4—C9—C10120.9 (2)
Mo2—O6—Mo182.44 (7)C9—C10—C11112.6 (2)
H9A—O9—H9B108.4C9—C10—H10A109.1
H10C—O10—H10D108.1C11—C10—H10A109.1
H11A—O11—H11B108.5C9—C10—H10B109.1
C1—N1—C3106.2 (3)C11—C10—H10B109.1
C1—N1—Mo1124.0 (2)H10A—C10—H10B107.8
C3—N1—Mo1129.49 (19)N6—C11—C12106.8 (2)
C1—N2—C2108.0 (3)N6—C11—C10109.2 (3)
C1—N2—H2126.0C12—C11—C10111.5 (2)
C2—N2—H2126.0N6—C11—H11109.8
C5—N3—Mo1110.04 (18)C12—C11—H11109.8
C5—N3—H3A109.7C10—C11—H11109.8
Mo1—N3—H3A109.7O3—C12—O4123.9 (3)
C5—N3—H3B109.7O3—C12—C11120.4 (3)
Mo1—N3—H3B109.7O4—C12—C11115.7 (3)
H3A—N3—H3B108.2
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9A···O1i0.851.892.716 (3)163
O9—H9B···O100.852.222.885 (4)136
O10—H10C···O11ii0.852.002.844 (4)170
O10—H10D···O50.852.343.056 (4)142
O11—H11A···O3iii0.851.912.724 (4)159
O11—H11B···O70.852.413.148 (4)145
N2—H2···O9iv0.861.882.735 (4)177
N3—H3A···O1i0.902.212.944 (3)139
N3—H3B···O10i0.902.183.077 (4)178
N5—H5···O11v0.862.032.869 (3)165
N6—H6A···O7vi0.902.343.091 (4)141
N6—H6B···O2vii0.902.473.150 (3)133
Symmetry codes: (i) x+2, y+1/2, z+1; (ii) x, y1, z; (iii) x, y+1, z; (iv) x, y, z+1; (v) x+1, y1/2, z; (vi) x+1, y1/2, z+1; (vii) x+1, y+1/2, z+1.
 

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