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The Na atom of the title complex, [Na2(ClO4)2(C10H8N2O2)2(H2O)4], is six-coordinate in a distorted octa­hedron. The N,N′-bis­(furan-2-ylmethyl­ene)hydrazine ligand is approximately planar, with a transoid configuration. Two coordinated water mol­ecules bridge two Na atoms, with an Na...Na separation of 3.542 (2) Å. The mol­ecule lies on an inversion centre. Inter­molecular π–π stacking inter­actions and O—H...O, O—H...N and C—H...O hydrogen bonds link the mol­ecules together to form a three-dimensional structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806034167/ng2084sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806034167/ng2084Isup2.hkl
Contains datablock I

CCDC reference: 624929

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • Disorder in main residue
  • R factor = 0.041
  • wR factor = 0.120
  • Data-to-parameter ratio = 11.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cl1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 15.00 Perc. PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Di-µ-aqua-bis{aqua[N,N'-bis(furan-2-ylmethylene)hydrazine- κ2N,O](perchlorato-κO)sodium} top
Crystal data top
[Na2(ClO4)2(C10H8N2O2)2(H2O)4]Z = 1
Mr = 693.31F(000) = 356
Triclinic, P1Dx = 1.542 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.5565 (1) ÅCell parameters from 856 reflections
b = 9.9647 (2) Åθ = 2.8–20.2°
c = 12.4108 (2) ŵ = 0.33 mm1
α = 73.882 (1)°T = 293 K
β = 81.473 (1)°Block, yellow
γ = 74.058 (1)°0.20 × 0.15 × 0.15 mm
V = 746.73 (2) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
2407 reflections with I > 2σ(I)
Radiation source: sealed tubeRint = 0.020
Graphite monochromatorθmax = 25.0°, θmin = 1.7°
φ/ω scansh = 77
8844 measured reflectionsk = 1111
2621 independent reflectionsl = 1414
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)] = 0.041H-atom parameters constrained
wR(F2) = 0.120 w = 1/[σ2(Fo2) + (0.072P)2 + 0.3846P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max < 0.001
2621 reflectionsΔρmax = 0.56 e Å3
237 parametersΔρmin = 0.36 e Å3
48 restraintsExtinction correction: SHELXTL (Bruker, 2000), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.095 (10)
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*/UeqOcc. (<1)
Na10.71743 (16)0.34806 (11)0.00085 (9)0.0415 (3)
O10.6572 (3)0.3102 (2)0.18161 (16)0.0451 (5)
O20.7817 (3)0.2482 (2)0.30456 (16)0.0457 (5)
N10.7186 (3)0.0909 (2)0.01327 (18)0.0351 (5)
N20.7450 (3)0.0317 (2)0.10467 (18)0.0354 (5)
C10.6488 (5)0.3887 (4)0.2914 (3)0.0533 (8)
H10.61120.48880.31420.064*
C20.7020 (5)0.3019 (4)0.3615 (3)0.0519 (8)
H20.70900.33000.43970.062*
C30.7453 (4)0.1597 (3)0.2941 (2)0.0454 (7)
H30.78570.07590.31930.055*
C40.7171 (4)0.1678 (3)0.1857 (2)0.0371 (6)
C50.7398 (4)0.0595 (3)0.0817 (2)0.0361 (6)
H50.77100.03690.08310.043*
C60.7111 (4)0.0004 (3)0.1995 (2)0.0386 (6)
H60.67220.09720.20040.046*
C70.7305 (4)0.1060 (3)0.3044 (2)0.0424 (6)
C80.7082 (5)0.0922 (4)0.4116 (3)0.0585 (8)
H80.67480.00670.43430.070*
C90.7459 (6)0.2331 (5)0.4817 (3)0.0669 (10)
H90.74160.25870.55990.080*
C100.7889 (5)0.3229 (4)0.4145 (3)0.0585 (9)
H100.81960.42280.43930.070*
Cl10.90306 (13)0.30997 (8)0.26635 (6)0.0501 (3)
O30.7697 (10)0.3680 (7)0.1738 (5)0.0757 (11)0.705 (11)
O41.0027 (11)0.4217 (6)0.2617 (5)0.0700 (14)0.705 (11)
O50.7848 (11)0.2706 (9)0.3673 (4)0.0834 (15)0.705 (11)
O61.0497 (12)0.1969 (7)0.2344 (6)0.1007 (18)0.705 (11)
O3'0.718 (2)0.3404 (12)0.2035 (10)0.0575 (16)0.295 (11)
O4'0.920 (2)0.4356 (13)0.2927 (10)0.055 (2)0.295 (11)
O5'0.860 (2)0.2107 (14)0.3727 (10)0.064 (2)0.295 (11)
O6'1.128 (2)0.2250 (14)0.2444 (11)0.072 (3)0.295 (11)
O70.6613 (3)0.6034 (2)0.05352 (17)0.0454 (5)
H7A0.69130.63600.12330.054*
H7B0.72900.63490.01660.054*
O81.0858 (3)0.3200 (2)0.07367 (17)0.0458 (5)
H8B1.09210.38090.13670.055*
H8A1.13380.23620.08470.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0437 (6)0.0362 (6)0.0478 (7)0.0092 (4)0.0035 (5)0.0163 (5)
O10.0552 (12)0.0396 (10)0.0401 (11)0.0111 (9)0.0061 (9)0.0087 (8)
O20.0469 (11)0.0476 (11)0.0403 (11)0.0148 (9)0.0048 (8)0.0036 (8)
N10.0345 (11)0.0329 (11)0.0382 (12)0.0091 (8)0.0020 (9)0.0089 (9)
N20.0331 (11)0.0338 (11)0.0393 (12)0.0093 (8)0.0022 (9)0.0085 (9)
C10.0574 (18)0.0503 (17)0.0474 (17)0.0159 (14)0.0117 (14)0.0025 (14)
C20.0469 (16)0.074 (2)0.0361 (15)0.0232 (15)0.0048 (12)0.0064 (14)
C30.0398 (14)0.0600 (18)0.0420 (15)0.0152 (13)0.0017 (12)0.0195 (13)
C40.0325 (12)0.0403 (14)0.0414 (14)0.0105 (10)0.0035 (10)0.0127 (11)
C50.0321 (12)0.0366 (13)0.0420 (14)0.0094 (10)0.0029 (10)0.0128 (11)
C60.0355 (13)0.0398 (14)0.0426 (15)0.0114 (11)0.0007 (11)0.0134 (11)
C70.0366 (14)0.0526 (16)0.0406 (15)0.0164 (12)0.0007 (11)0.0126 (12)
C80.0556 (18)0.081 (2)0.0447 (17)0.0241 (17)0.0043 (14)0.0229 (16)
C90.064 (2)0.102 (3)0.0340 (16)0.036 (2)0.0040 (14)0.0001 (18)
C100.0540 (18)0.068 (2)0.0457 (18)0.0207 (16)0.0080 (14)0.0069 (16)
Cl10.0699 (5)0.0467 (5)0.0386 (4)0.0204 (4)0.0024 (3)0.0133 (3)
O30.085 (2)0.102 (2)0.0443 (19)0.0360 (19)0.0105 (16)0.0096 (17)
O40.092 (3)0.066 (2)0.062 (3)0.038 (2)0.008 (2)0.013 (2)
O50.092 (3)0.094 (3)0.052 (2)0.026 (3)0.009 (2)0.003 (2)
O60.094 (3)0.069 (3)0.134 (4)0.004 (3)0.007 (3)0.042 (3)
O3'0.072 (3)0.060 (2)0.043 (3)0.026 (2)0.003 (2)0.008 (2)
O4'0.075 (5)0.047 (4)0.050 (4)0.020 (4)0.004 (4)0.022 (3)
O5'0.079 (5)0.055 (4)0.052 (4)0.020 (4)0.005 (4)0.000 (4)
O6'0.079 (5)0.064 (4)0.066 (4)0.015 (4)0.003 (4)0.011 (4)
O70.0443 (11)0.0440 (11)0.0508 (12)0.0138 (9)0.0022 (9)0.0146 (9)
O80.0510 (11)0.0359 (10)0.0513 (12)0.0104 (8)0.0013 (9)0.0138 (9)
Geometric parameters (Å, º) top
Na1—O32.292 (5)C6—C71.430 (4)
Na1—O72.381 (2)C6—H60.9300
Na1—O7i2.421 (2)C7—C81.358 (4)
Na1—O82.424 (2)C8—C91.409 (6)
Na1—O3'2.496 (12)C8—H80.9300
Na1—O12.499 (2)C9—C101.335 (6)
Na1—N12.522 (2)C9—H90.9300
O1—C11.371 (4)C10—H100.9300
O1—C41.377 (3)Cl1—O61.376 (6)
O2—C101.361 (4)Cl1—O51.390 (5)
O2—C71.362 (4)Cl1—O4'1.415 (12)
N1—C51.280 (3)Cl1—O41.422 (5)
N1—N21.408 (3)Cl1—O31.439 (5)
N2—C61.277 (3)Cl1—O5'1.455 (11)
C1—C21.337 (5)Cl1—O3'1.455 (11)
C1—H10.9300Cl1—O6'1.515 (13)
C2—C31.407 (5)O7—Na1i2.421 (2)
C2—H20.9300O7—H7A0.8501
C3—C41.353 (4)O7—H7B0.8499
C3—H30.9300O8—H8B0.8502
C4—C51.431 (4)O8—H8A0.8498
C5—H50.9300
O3—Na1—O784.99 (18)N1—C5—H5118.9
O3—Na1—O7i88.71 (17)C4—C5—H5118.9
O7—Na1—O7i84.99 (7)N2—C6—C7122.8 (3)
O3—Na1—O896.22 (17)N2—C6—H6118.6
O7—Na1—O890.51 (7)C7—C6—H6118.6
O7i—Na1—O8173.02 (9)C8—C7—O2109.9 (3)
O7—Na1—O3'92.2 (3)C8—C7—C6130.9 (3)
O7i—Na1—O3'80.0 (3)O2—C7—C6119.3 (2)
O8—Na1—O3'105.5 (3)C7—C8—C9106.3 (3)
O3—Na1—O1176.25 (19)C7—C8—H8126.8
O7—Na1—O198.60 (8)C9—C8—H8126.8
O7i—Na1—O190.52 (8)C10—C9—C8106.9 (3)
O8—Na1—O184.87 (7)C10—C9—H9126.6
O3'—Na1—O1165.0 (3)C8—C9—H9126.6
O3—Na1—N1109.44 (18)C9—C10—O2110.7 (3)
O7—Na1—N1164.34 (9)C9—C10—H10124.6
O7i—Na1—N189.16 (7)O2—C10—H10124.6
O8—Na1—N193.83 (7)O6—Cl1—O5114.4 (4)
O3'—Na1—N1101.1 (3)O6—Cl1—O4109.8 (4)
O1—Na1—N166.88 (7)O5—Cl1—O4114.0 (3)
C1—O1—C4105.7 (2)O6—Cl1—O3102.5 (4)
C1—O1—Na1136.46 (19)O5—Cl1—O3111.2 (3)
C4—O1—Na1113.55 (15)O4—Cl1—O3103.9 (4)
C10—O2—C7106.2 (3)O4'—Cl1—O5'106.6 (7)
C5—N1—N2112.8 (2)O4'—Cl1—O3'110.9 (7)
C5—N1—Na1114.72 (17)O5'—Cl1—O3'105.4 (6)
N2—N1—Na1130.99 (16)O4'—Cl1—O6'106.4 (7)
C6—N2—N1112.6 (2)O5'—Cl1—O6'95.4 (7)
C2—C1—O1110.9 (3)O3'—Cl1—O6'129.1 (8)
C2—C1—H1124.6Cl1—O3—Na1144.9 (4)
O1—C1—H1124.6Cl1—O3'—Na1127.1 (7)
C1—C2—C3106.7 (3)Na1—O7—Na1i95.01 (7)
C1—C2—H2126.6Na1—O7—H7A113.3
C3—C2—H2126.6Na1i—O7—H7A113.3
C4—C3—C2107.1 (3)Na1—O7—H7B113.3
C4—C3—H3126.4Na1i—O7—H7B113.3
C2—C3—H3126.4H7A—O7—H7B108.4
C3—C4—O1109.6 (2)Na1—O8—H8B109.0
C3—C4—C5132.2 (3)Na1—O8—H8A109.1
O1—C4—C5118.2 (2)H8B—O8—H8A107.9
N1—C5—C4122.1 (2)
Symmetry code: (i) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O4ii0.852.493.155 (8)136
O7—H7B···O8ii0.851.982.822 (3)172
O8—H8B···O4ii0.852.142.941 (6)157
O8—H8A···N2iii0.852.042.893 (3)178
C2—H2···O5iv0.932.573.415 (6)151
Symmetry codes: (ii) x+2, y+1, z; (iii) x+2, y, z; (iv) x, y, z1.
 

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