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The title compound, [Fe(C10H8N2)3]Br2·4.5H2O, contains discrete tris­(2,2′-bipyrid­yl)iron(II) cations, bromide anions and water mol­ecules. The Fe atom (site symmetry 3) is octa­hedrally coordinated by six N atoms of the three bidentate bipyridyl ligands. One bromide ion occupies a site of symmetry m; the other one is located on a site of symmetry 32. All the water O atoms are also located on special positions of site symmetries 3, m (×2) and \overline6.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806020903/hb2074sup1.cif
Contains datablocks IV, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806020903/hb2074IVsup2.hkl
Contains datablock IV

CCDC reference: 615286

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.017 Å
  • H-atom completeness 73%
  • Disorder in solvent or counterion
  • R factor = 0.101
  • wR factor = 0.283
  • Data-to-parameter ratio = 14.9

checkCIF/PLATON results

No syntax errors found




Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O1
Author Response: The water H atom could not be found and were excluded from refinement.
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......         O2
Author Response: The water H atom could not be found and were excluded from refinement.
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......         O3
Author Response: The water H atom could not be found and were excluded from refinement.
PLAT430_ALERT_2_A Short Inter D...A Contact  O2     ..  O4'     ..       1.97 Ang.
Author Response: O4' is one site of a disordered water O atom.

Alert level B PLAT341_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 17 PLAT431_ALERT_2_B Short Inter HL..A Contact Br2 .. O1 .. 2.98 Ang. PLAT431_ALERT_2_B Short Inter HL..A Contact Br2 .. O1 .. 2.98 Ang.
Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 765.29 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 30.00 360.33 H 1.01 24.00 24.19 Br 79.90 2.00 159.81 Fe 55.85 1.00 55.85 N 14.01 6.00 84.04 O 16.00 4.50 72.00 Calculated formula weight 756.21 RFACG01_ALERT_3_C The value of the R factor is > 0.10 R factor given 0.101 RFACR01_ALERT_3_C The value of the weighted R factor is > 0.25 Weighted R factor given 0.283 STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.560 From the CIF: _refine_ls_abs_structure_Flack_su 0.050 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.56 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 765.29 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT084_ALERT_2_C High R2 Value .................................. 0.28 PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 1 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.16 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 14.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O4' PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O4 PLAT431_ALERT_2_C Short Inter HL..A Contact Br1 .. O3 .. 3.22 Ang.
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C30 H33 Br2 Fe1 N6 O4.5 Atom count from the _atom_site data: C30 H24 Br2 Fe1 N6 O4.5 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C30 H33 Br2 Fe N6 O4.50 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 120.00 120.00 0.00 H 132.00 96.00 36.00 Br 8.00 8.00 0.00 Fe 4.00 4.00 0.00 N 24.00 24.00 0.00 O 18.00 18.00 0.00 REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.57 From the CIF: _reflns_number_total 2071 Count of symmetry unique reflns 1193 Completeness (_total/calc) 173.60% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 878 Fraction of Friedel pairs measured 0.736 Are heavy atom types Z>Si present yes
4 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 18 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 14 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

; top
Crystal data top
[Fe(C10H8N2)3]Br2·4.5H2ODx = 1.572 Mg m3
Mr = 765.29Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P62cCell parameters from 12085 reflections
Hall symbol: P -6c -2cθ = 2.6–25.7°
a = 13.1386 (12) ŵ = 2.98 mm1
c = 21.630 (3) ÅT = 173 K
V = 3233.6 (6) Å3Plate, red
Z = 40.26 × 0.24 × 0.08 mm
F(000) = 1548
Data collection top
STOE IPDSII two-circle
diffractometer
2071 independent reflections
Radiation source: fine-focus sealed tube1569 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.097
ω scansθmax = 25.6°, θmin = 2.6°
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
h = 1515
Tmin = 0.511, Tmax = 0.796k = 1515
25866 measured reflectionsl = 2526
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)] = 0.101H-atom parameters constrained
wR(F2) = 0.283 w = 1/[σ2(Fo2) + (0.188P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max = 0.033
2071 reflectionsΔρmax = 2.19 e Å3
139 parametersΔρmin = 1.17 e Å3
6 restraintsAbsolute structure: Flack (1983), 892 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.56 (5)
Special details top

Experimental. ;

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)
Fe10.33330.66670.51370 (11)0.0237 (6)
N10.3245 (7)0.5370 (8)0.5638 (5)0.030 (2)
C20.2488 (8)0.4271 (8)0.5411 (5)0.027 (2)
C30.2273 (10)0.3254 (9)0.5734 (6)0.035 (3)
H30.17190.24990.55810.042*
C40.2888 (12)0.3367 (11)0.6284 (7)0.041 (3)
H40.27830.26940.65030.050*
C50.3638 (9)0.4468 (10)0.6493 (6)0.032 (3)
H50.40420.45670.68720.039*
C60.3821 (9)0.5442 (10)0.6165 (5)0.032 (2)
H60.43780.61970.63160.038*
N110.2157 (7)0.5332 (8)0.4630 (4)0.0276 (19)
C120.1896 (8)0.4246 (10)0.4825 (5)0.029 (2)
C130.1150 (10)0.3242 (9)0.4515 (6)0.037 (3)
H130.09600.24950.46760.045*
C140.0669 (10)0.3330 (10)0.3956 (6)0.041 (3)
H140.01650.26440.37250.050*
C150.0931 (9)0.4413 (10)0.3743 (6)0.037 (3)
H150.06450.45010.33550.044*
C160.1657 (9)0.5421 (10)0.4126 (7)0.040 (3)
H160.17750.61690.40080.048*
Br10.2892 (3)0.8867 (2)0.75000.0750 (9)
Br20.00000.00000.50000.0702 (14)
O10.00000.00000.3621 (5)0.028 (2)
O20.5290 (13)0.3246 (9)0.75000.041 (3)
O30.33330.66670.75000.072 (7)
O40.264 (4)0.138 (4)0.75000.062 (14)*0.39 (5)
O4'0.369 (6)0.187 (6)0.75000.16 (2)*0.61 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0175 (7)0.0175 (7)0.0359 (13)0.0088 (4)0.0000.000
N10.020 (4)0.022 (4)0.050 (6)0.013 (4)0.003 (4)0.001 (4)
C20.017 (4)0.013 (4)0.044 (6)0.003 (4)0.000 (4)0.004 (4)
C30.037 (6)0.012 (5)0.058 (8)0.013 (5)0.008 (5)0.008 (4)
C40.046 (7)0.032 (7)0.056 (8)0.027 (6)0.003 (6)0.004 (6)
C50.022 (5)0.033 (6)0.047 (7)0.018 (5)0.000 (4)0.009 (5)
C60.027 (5)0.032 (6)0.041 (6)0.019 (5)0.003 (4)0.010 (5)
N110.026 (4)0.034 (5)0.033 (5)0.022 (4)0.001 (4)0.003 (4)
C120.018 (5)0.024 (5)0.045 (6)0.012 (4)0.011 (4)0.011 (5)
C130.024 (5)0.019 (5)0.052 (8)0.002 (4)0.006 (5)0.014 (5)
C140.026 (6)0.026 (6)0.066 (9)0.009 (5)0.001 (5)0.013 (5)
C150.023 (5)0.035 (6)0.058 (8)0.017 (5)0.011 (5)0.014 (5)
C160.018 (5)0.022 (5)0.078 (9)0.007 (4)0.008 (5)0.001 (5)
Br10.093 (2)0.0573 (14)0.0598 (13)0.0265 (13)0.0000.000
Br20.0203 (8)0.0203 (8)0.170 (4)0.0102 (4)0.0000.000
O10.033 (4)0.033 (4)0.018 (6)0.0164 (18)0.0000.000
O20.105 (8)0.026 (5)0.009 (4)0.044 (5)0.0000.000
O30.054 (9)0.054 (9)0.11 (2)0.027 (5)0.0000.000
Geometric parameters (Å, º) top
Fe1—N11.973 (9)C5—C61.376 (16)
Fe1—N1i1.973 (9)C5—H50.9500
Fe1—N1ii1.973 (9)C6—H60.9500
Fe1—N11i1.989 (9)N11—C161.308 (16)
Fe1—N111.989 (10)N11—C121.357 (14)
Fe1—N11ii1.989 (9)C12—C131.363 (15)
N1—C61.344 (15)C13—C141.40 (2)
N1—C21.371 (13)C13—H130.9500
C2—C31.405 (14)C14—C151.366 (17)
C2—C121.480 (15)C14—H140.9500
C3—C41.40 (2)C15—C161.445 (16)
C3—H30.9500C15—H150.9500
C4—C51.357 (18)C16—H160.9500
C4—H40.9500
N1—Fe1—N1i92.7 (4)C3—C4—H4121.0
N1—Fe1—N1ii92.7 (4)C4—C5—C6121.0 (11)
N1i—Fe1—N1ii92.7 (4)C4—C5—H5119.5
N1—Fe1—N11i171.9 (3)C6—C5—H5119.5
N1i—Fe1—N11i81.8 (3)N1—C6—C5122.8 (10)
N1ii—Fe1—N11i93.5 (3)N1—C6—H6118.6
N1—Fe1—N1181.8 (3)C5—C6—H6118.6
N1i—Fe1—N1193.5 (3)C16—N11—C12118.6 (10)
N1ii—Fe1—N11171.9 (3)C16—N11—Fe1125.8 (7)
N11i—Fe1—N1192.6 (4)C12—N11—Fe1115.6 (7)
N1—Fe1—N11ii93.5 (3)N11—C12—C13123.2 (11)
N1i—Fe1—N11ii171.9 (3)N11—C12—C2112.9 (10)
N1ii—Fe1—N11ii81.8 (3)C13—C12—C2124.0 (10)
N11i—Fe1—N11ii92.6 (4)C12—C13—C14118.8 (11)
N11—Fe1—N11ii92.6 (4)C12—C13—H13120.6
C6—N1—C2117.7 (10)C14—C13—H13120.6
C6—N1—Fe1128.1 (8)C15—C14—C13119.3 (10)
C2—N1—Fe1114.3 (7)C15—C14—H14120.3
N1—C2—C3121.2 (10)C13—C14—H14120.3
N1—C2—C12115.3 (10)C14—C15—C16117.9 (11)
C3—C2—C12123.5 (10)C14—C15—H15121.0
C4—C3—C2119.3 (10)C16—C15—H15121.0
C4—C3—H3120.4N11—C16—C15121.8 (10)
C2—C3—H3120.4N11—C16—H16119.1
C5—C4—C3117.9 (11)C15—C16—H16119.1
C5—C4—H4121.0
N1i—Fe1—N1—C685.8 (7)N11i—Fe1—N11—C165.5 (10)
N1ii—Fe1—N1—C67.1 (9)N11ii—Fe1—N11—C1687.2 (8)
N11—Fe1—N1—C6178.9 (9)N1—Fe1—N11—C122.7 (7)
N11ii—Fe1—N1—C689.0 (9)N1i—Fe1—N11—C1295.0 (7)
N1i—Fe1—N1—C293.5 (9)N11i—Fe1—N11—C12176.9 (7)
N1ii—Fe1—N1—C2173.6 (7)N11ii—Fe1—N11—C1290.4 (9)
N11—Fe1—N1—C20.4 (7)C16—N11—C12—C130.9 (15)
N11ii—Fe1—N1—C291.6 (7)Fe1—N11—C12—C13176.9 (9)
C6—N1—C2—C33.2 (14)C16—N11—C12—C2178.0 (9)
Fe1—N1—C2—C3176.2 (8)Fe1—N11—C12—C24.3 (10)
C6—N1—C2—C12178.9 (8)N1—C2—C12—N113.9 (11)
Fe1—N1—C2—C121.7 (10)C3—C2—C12—N11174.0 (10)
N1—C2—C3—C42.9 (17)N1—C2—C12—C13177.3 (10)
C12—C2—C3—C4179.3 (11)C3—C2—C12—C134.8 (15)
C2—C3—C4—C52.4 (19)N11—C12—C13—C143.1 (17)
C3—C4—C5—C62.3 (19)C2—C12—C13—C14178.2 (10)
C2—N1—C6—C53.1 (15)C12—C13—C14—C151.8 (18)
Fe1—N1—C6—C5176.2 (8)C13—C14—C15—C162.9 (17)
C4—C5—C6—N12.7 (17)C12—N11—C16—C156.0 (16)
N1—Fe1—N11—C16179.7 (9)Fe1—N11—C16—C15171.6 (8)
N1i—Fe1—N11—C1687.4 (10)C14—C15—C16—N117.1 (17)
Symmetry codes: (i) x+y, x+1, z; (ii) y+1, xy+1, z.
 

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