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The title compound, (C16H36N)2[W2Br4(C2O4)O4], has a centrosymmetric dinuclear anion in which two tungsten(VI) centres, with distorted octa­hedral coordination, are bridged by an oxalate dianion, forming two five-membered chelate rings. All atoms of the complex anion, except for the Br atoms, lie essentially in a plane.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807017102/sg2155sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807017102/sg2155Isup2.hkl
Contains datablock I

CCDC reference: 648087

Key indicators

  • Single-crystal X-ray study
  • T = 160 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.026
  • wR factor = 0.063
  • Data-to-parameter ratio = 20.3

checkCIF/PLATON results

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Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.83 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.95 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.76 Ratio PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C1 - C1_a ... 1.55 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C16 H36 N
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: local programs; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

Bis(tetrabutylammonium) µ-oxalato-bis[dibromidodioxidotungstate(VI)] top
Crystal data top
(C16H36N)2[W2Br4(C2O4)O4]F(000) = 1284
Mr = 1324.28Dx = 1.850 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 9.8891 (9) ÅCell parameters from 10570 reflections
b = 18.0806 (15) Åθ = 1.1–26.3°
c = 13.2945 (11) ŵ = 8.24 mm1
β = 90.905 (2)°T = 160 K
V = 2376.8 (4) Å3Block, colourless
Z = 20.32 × 0.32 × 0.16 mm
Data collection top
Bruker SMART 1K CCD
diffractometer
4689 independent reflections
Radiation source: sealed tube4435 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
Detector resolution: 8.192 pixels mm-1θmax = 26.3°, θmin = 1.9°
thin–slice ω scansh = 612
Absorption correction: multi-scan
(XPREP in SHELXTL; Sheldrick, 2001)
k = 2120
Tmin = 0.075, Tmax = 0.270l = 1516
12764 measured reflections
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)] = 0.026H-atom parameters constrained
wR(F2) = 0.063 w = 1/[σ2(Fo2) + (0.0214P)2 + 4.8146P]
where P = (Fo2 + 2Fc2)/3
S = 1.17(Δ/σ)max = 0.001
4689 reflectionsΔρmax = 1.21 e Å3
231 parametersΔρmin = 1.18 e Å3
0 restraintsExtinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00108 (9)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
W10.399964 (14)0.076456 (8)0.677516 (11)0.02061 (7)
Br10.55009 (4)0.17320 (2)0.59921 (3)0.03541 (11)
Br20.27883 (4)0.04418 (2)0.70104 (3)0.03561 (11)
O10.2597 (3)0.13192 (16)0.6808 (2)0.0327 (6)
O20.4712 (3)0.08290 (15)0.7952 (2)0.0318 (6)
O30.5636 (2)0.00313 (15)0.62216 (19)0.0231 (5)
C10.5609 (3)0.01447 (19)0.5314 (3)0.0198 (7)
O40.6449 (2)0.05281 (15)0.4857 (2)0.0230 (5)
N10.4453 (3)0.28446 (16)1.0635 (2)0.0205 (6)
C20.4015 (4)0.2921 (2)1.1720 (3)0.0241 (8)
H2A0.38540.24191.19910.029*
H2B0.47750.31391.21130.029*
C30.2756 (4)0.3387 (2)1.1903 (3)0.0280 (8)
H3A0.19610.31551.15690.034*
H3B0.28760.38871.16140.034*
C40.2522 (5)0.3446 (3)1.3031 (3)0.0360 (10)
H4A0.33450.36511.33600.043*
H4B0.23760.29441.33060.043*
C50.1322 (5)0.3929 (3)1.3291 (4)0.0401 (11)
H5A0.12660.39771.40240.060*
H5B0.14350.44201.29920.060*
H5C0.04890.37031.30270.060*
C60.5677 (4)0.2341 (2)1.0609 (3)0.0228 (7)
H6A0.54260.18601.09090.027*
H6B0.59020.22490.98970.027*
C70.6938 (4)0.2622 (2)1.1149 (3)0.0280 (8)
H7A0.71890.31121.08740.034*
H7B0.67530.26831.18740.034*
C80.8105 (4)0.2084 (2)1.1017 (3)0.0295 (9)
H8A0.78500.15931.12850.035*
H8B0.82940.20271.02920.035*
C90.9377 (4)0.2362 (3)1.1569 (4)0.0403 (11)
H9A1.01050.19991.15000.060*
H9B0.96590.28351.12770.060*
H9C0.91820.24321.22830.060*
C100.4780 (4)0.3609 (2)1.0221 (3)0.0210 (7)
H10A0.53820.38651.07110.025*
H10B0.39290.38971.01720.025*
C110.5448 (4)0.3620 (2)0.9200 (3)0.0237 (8)
H11A0.63300.33620.92440.028*
H11B0.48700.33570.87020.028*
C120.5662 (4)0.4413 (2)0.8860 (3)0.0284 (8)
H12A0.63580.46480.92980.034*
H12B0.48080.46930.89370.034*
C130.6102 (5)0.4459 (3)0.7777 (3)0.0423 (11)
H13A0.62410.49780.75930.063*
H13B0.69500.41860.76980.063*
H13C0.54010.42440.73380.063*
C140.3329 (4)0.2505 (2)0.9990 (3)0.0244 (8)
H14A0.36430.24830.92870.029*
H14B0.25410.28421.00010.029*
C150.2849 (4)0.1738 (2)1.0283 (3)0.0309 (9)
H15A0.36280.13951.03140.037*
H15B0.24400.17561.09570.037*
C160.1813 (5)0.1461 (3)0.9517 (4)0.0398 (10)
H16A0.22240.14610.88420.048*
H16B0.10350.18060.94970.048*
C170.1309 (7)0.0691 (3)0.9751 (5)0.0624 (17)
H17A0.05890.05560.92700.094*
H17B0.20570.03380.96990.094*
H17C0.09550.06791.04350.094*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.02427 (9)0.02173 (10)0.01584 (10)0.00202 (5)0.00063 (6)0.00254 (5)
Br10.0420 (2)0.0298 (2)0.0345 (2)0.01094 (17)0.00287 (18)0.00072 (17)
Br20.0350 (2)0.0313 (2)0.0406 (3)0.00694 (17)0.00136 (18)0.00578 (18)
O10.0365 (15)0.0335 (16)0.0281 (15)0.0096 (12)0.0037 (12)0.0016 (12)
O20.0409 (16)0.0325 (16)0.0220 (15)0.0020 (12)0.0030 (12)0.0043 (12)
O30.0253 (12)0.0286 (14)0.0153 (12)0.0038 (11)0.0035 (10)0.0046 (11)
C10.0212 (17)0.0165 (17)0.0216 (18)0.0010 (13)0.0001 (14)0.0006 (14)
O40.0222 (12)0.0266 (13)0.0202 (13)0.0035 (10)0.0025 (10)0.0046 (11)
N10.0219 (14)0.0201 (15)0.0195 (16)0.0007 (12)0.0016 (12)0.0000 (12)
C20.0292 (19)0.028 (2)0.0154 (18)0.0009 (15)0.0006 (15)0.0042 (15)
C30.0250 (18)0.032 (2)0.027 (2)0.0030 (16)0.0024 (15)0.0038 (17)
C40.044 (2)0.039 (2)0.025 (2)0.011 (2)0.0087 (18)0.0084 (18)
C50.041 (2)0.045 (3)0.034 (2)0.012 (2)0.0104 (19)0.010 (2)
C60.0255 (18)0.0204 (18)0.0225 (19)0.0018 (14)0.0004 (14)0.0016 (15)
C70.0252 (18)0.030 (2)0.028 (2)0.0022 (16)0.0013 (15)0.0003 (17)
C80.0261 (19)0.031 (2)0.031 (2)0.0045 (16)0.0057 (16)0.0080 (17)
C90.029 (2)0.047 (3)0.045 (3)0.0041 (19)0.0029 (19)0.011 (2)
C100.0217 (16)0.0192 (17)0.0221 (18)0.0000 (14)0.0018 (14)0.0021 (15)
C110.0247 (18)0.0226 (19)0.0238 (19)0.0029 (14)0.0015 (14)0.0009 (15)
C120.032 (2)0.025 (2)0.028 (2)0.0064 (16)0.0005 (16)0.0042 (17)
C130.059 (3)0.039 (3)0.029 (2)0.018 (2)0.005 (2)0.006 (2)
C140.0277 (18)0.0248 (19)0.0205 (19)0.0055 (15)0.0038 (15)0.0003 (15)
C150.031 (2)0.030 (2)0.032 (2)0.0080 (17)0.0033 (17)0.0020 (18)
C160.044 (2)0.039 (2)0.037 (3)0.015 (2)0.000 (2)0.003 (2)
C170.077 (4)0.053 (3)0.057 (4)0.042 (3)0.004 (3)0.006 (3)
Geometric parameters (Å, º) top
W1—Br12.5291 (4)C7—C81.522 (5)
W1—Br22.5103 (5)C8—H8A0.990
W1—O11.712 (3)C8—H8B0.990
W1—O21.710 (3)C8—C91.532 (6)
W1—O32.226 (2)C9—H9A0.980
W1—O4i2.249 (3)C9—H9B0.980
C1—O31.247 (4)C9—H9C0.980
C1—O41.247 (4)C10—H10A0.990
C1—C1i1.547 (7)C10—H10B0.990
O4—W1i2.249 (3)C10—C111.519 (5)
N1—C21.520 (4)C11—H11A0.990
N1—C61.516 (4)C11—H11B0.990
N1—C101.524 (5)C11—C121.519 (5)
N1—C141.523 (5)C12—H12A0.990
C2—H2A0.990C12—H12B0.990
C2—H2B0.990C12—C131.514 (6)
C2—C31.526 (5)C13—H13A0.980
C3—H3A0.990C13—H13B0.980
C3—H3B0.990C13—H13C0.980
C3—C41.525 (6)C14—H14A0.990
C4—H4A0.990C14—H14B0.990
C4—H4B0.990C14—C151.517 (5)
C4—C51.519 (6)C15—H15A0.990
C5—H5A0.980C15—H15B0.990
C5—H5B0.980C15—C161.518 (6)
C5—H5C0.980C16—H16A0.990
C6—H6A0.990C16—H16B0.990
C6—H6B0.990C16—C171.514 (7)
C6—C71.517 (5)C17—H17A0.980
C7—H7A0.990C17—H17B0.980
C7—H7B0.990C17—H17C0.980
Br1—W1—Br2159.484 (16)H7B—C7—C8109.6
Br1—W1—O194.96 (10)C7—C8—H8A109.5
Br1—W1—O295.35 (10)C7—C8—H8B109.5
Br1—W1—O380.87 (7)C7—C8—C9110.7 (4)
Br1—W1—O4i80.94 (7)H8A—C8—H8B108.1
Br2—W1—O196.74 (10)H8A—C8—C9109.5
Br2—W1—O297.81 (10)H8B—C8—C9109.5
Br2—W1—O382.80 (7)C8—C9—H9A109.5
Br2—W1—O4i82.40 (7)C8—C9—H9B109.5
O1—W1—O2105.00 (14)C8—C9—H9C109.5
O1—W1—O3161.90 (12)H9A—C9—H9B109.5
O1—W1—O4i89.35 (12)H9A—C9—H9C109.5
O2—W1—O392.96 (12)H9B—C9—H9C109.5
O2—W1—O4i165.48 (12)N1—C10—H10A108.4
O3—W1—O4i72.62 (9)N1—C10—H10B108.4
W1—O3—C1117.8 (2)N1—C10—C11115.6 (3)
W1i—O4—C1116.9 (2)H10A—C10—H10B107.4
O3—C1—C1i116.1 (4)H10A—C10—C11108.4
O3—C1—O4127.5 (3)H10B—C10—C11108.4
C1i—C1—O4116.4 (4)C10—C11—H11A109.7
C2—N1—C6108.4 (3)C10—C11—H11B109.7
C2—N1—C10109.0 (3)C10—C11—C12110.0 (3)
C2—N1—C14110.8 (3)H11A—C11—H11B108.2
C6—N1—C10111.3 (3)H11A—C11—C12109.7
C6—N1—C14108.7 (3)H11B—C11—C12109.7
C10—N1—C14108.7 (3)C11—C12—H12A109.2
N1—C2—H2A108.2C11—C12—H12B109.2
N1—C2—H2B108.2C11—C12—C13112.2 (3)
N1—C2—C3116.5 (3)H12A—C12—H12B107.9
H2A—C2—H2B107.3H12A—C12—C13109.2
H2A—C2—C3108.2H12B—C12—C13109.2
H2B—C2—C3108.2C12—C13—H13A109.5
C2—C3—H3A109.8C12—C13—H13B109.5
C2—C3—H3B109.8C12—C13—H13C109.5
C2—C3—C4109.4 (3)H13A—C13—H13B109.5
H3A—C3—H3B108.2H13A—C13—H13C109.5
H3A—C3—C4109.8H13B—C13—H13C109.5
H3B—C3—C4109.8N1—C14—H14A108.1
C3—C4—H4A108.9N1—C14—H14B108.1
C3—C4—H4B108.9N1—C14—C15116.9 (3)
C3—C4—C5113.3 (4)H14A—C14—H14B107.3
H4A—C4—H4B107.7H14A—C14—C15108.1
H4A—C4—C5108.9H14B—C14—C15108.1
H4B—C4—C5108.9C14—C15—H15A109.7
C4—C5—H5A109.5C14—C15—H15B109.7
C4—C5—H5B109.5C14—C15—C16109.8 (4)
C4—C5—H5C109.5H15A—C15—H15B108.2
H5A—C5—H5B109.5H15A—C15—C16109.7
H5A—C5—H5C109.5H15B—C15—C16109.7
H5B—C5—H5C109.5C15—C16—H16A109.0
N1—C6—H6A108.3C15—C16—H16B109.0
N1—C6—H6B108.3C15—C16—C17112.7 (4)
N1—C6—C7116.0 (3)H16A—C16—H16B107.8
H6A—C6—H6B107.4H16A—C16—C17109.0
H6A—C6—C7108.3H16B—C16—C17109.0
H6B—C6—C7108.3C16—C17—H17A109.5
C6—C7—H7A109.6C16—C17—H17B109.5
C6—C7—H7B109.6C16—C17—H17C109.5
C6—C7—C8110.5 (3)H17A—C17—H17B109.5
H7A—C7—H7B108.1H17A—C17—H17C109.5
H7A—C7—C8109.6H17B—C17—H17C109.5
Br1—W1—O3—C180.5 (3)C10—N1—C6—C755.8 (4)
Br2—W1—O3—C187.0 (3)C14—N1—C6—C7175.5 (3)
O1—W1—O3—C12.6 (5)N1—C6—C7—C8177.0 (3)
O2—W1—O3—C1175.5 (3)C6—C7—C8—C9179.5 (3)
O4i—W1—O3—C12.8 (2)C2—N1—C10—C11170.6 (3)
W1—O3—C1—C1i2.6 (5)C6—N1—C10—C1151.1 (4)
W1—O3—C1—O4177.6 (3)C14—N1—C10—C1168.6 (4)
O3—C1—O4—W1i177.5 (3)N1—C10—C11—C12177.6 (3)
C1i—C1—O4—W1i2.3 (5)C10—C11—C12—C13170.3 (4)
C6—N1—C2—C3177.7 (3)C2—N1—C14—C1560.0 (4)
C10—N1—C2—C361.0 (4)C6—N1—C14—C1559.0 (4)
C14—N1—C2—C358.5 (4)C10—N1—C14—C15179.7 (3)
N1—C2—C3—C4176.3 (3)N1—C14—C15—C16175.5 (3)
C2—C3—C4—C5177.5 (4)C14—C15—C16—C17178.8 (4)
C2—N1—C6—C764.0 (4)
Symmetry code: (i) x+1, y, z+1.
 

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