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The crystal structure of the title compound, [Fe(C11H10N2O2)2]NO3·2H2O, is the first reported iron(III) complex containing the hydrated form of di-2-pyridyl ketone (dpk-hydrate) as a ligand. Fe atoms reside on inversion centers in the triclinic cell and each cation has a distorted octahedral environment, which is typical of bis­(dpk-hydrate)–transition metal complexes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802017798/om6111sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802017798/om6111Isup2.hkl
Contains datablock I

CCDC reference: 200717

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.042
  • wR factor = 0.108
  • Data-to-parameter ratio = 14.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 28.30 From the CIF: _reflns_number_total 5174 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 5777 Completeness (_total/calc) 89.56% Alert B: < 90% complete (theta max?)
Author response: Data on several crystals were attempted since many diffracted poorly. Other labs were given crystals and one data set was collected on a supercell and refined to only 20%... the reason turned out to be possible twinning (horrible E2-1 stats). Needless to say, we tried to get higher resolution and stopped barely below 90.00 (Its 89.56%! Please round up!
General Notes

ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.925 Tmax scaled 0.925 Tmin scaled 0.831
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
0 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXTL (Bruker, 1997).

bis(bis(2-Pyridyl)(hydroxy)methanolato-O,N,N')-iron(III) nitrate dihydrate top
Crystal data top
[Fe(C11H10N2O2)2]NO3·2H2OF(000) = 566
Mr = 556.30Dx = 1.579 Mg m3
Triclinic, P1Melting point: not measured K
a = 8.7813 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.8586 (10) ÅCell parameters from 7293 reflections
c = 16.1136 (18) Åθ = 2.4–28.2°
α = 103.703 (2)°µ = 0.71 mm1
β = 105.009 (2)°T = 153 K
γ = 94.870 (2)°Parallelepiped, orange–yellow
V = 1161.9 (2) Å30.35 × 0.13 × 0.11 mm
Z = 2
Data collection top
Bruker SMART APEX CCD
diffractometer
5174 independent reflections
Radiation source: fine-focus sealed tube4609 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
ω scansθmax = 28.3°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS, Bruker, 1997)
h = 1111
Tmin = 0.899, Tmax = 1.000k = 1111
9820 measured reflectionsl = 2020
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H atoms treated by a mixture of independent and constrained refinement
S = 1.02 w = 1/[σ2(Fo2) + (0.0557P)2 + 0.7918P]
where P = (Fo2 + 2Fc2)/3
5174 reflections(Δ/σ)max = 0.041
353 parametersΔρmax = 0.64 e Å3
0 restraintsΔρmin = 0.36 e Å3
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
Fe10.00000.50000.00000.01265 (11)
O10.21972 (17)0.55349 (17)0.02537 (10)0.0163 (3)
C60.2350 (2)0.6899 (2)0.00505 (14)0.0152 (4)
O20.38930 (17)0.75839 (18)0.00981 (10)0.0190 (3)
H2A0.43200.70100.02420.029*
N10.0129 (2)0.7257 (2)0.04898 (11)0.0154 (4)
C10.0814 (3)0.8030 (3)0.09190 (15)0.0204 (4)
H1A0.17780.74770.09340.024*
C20.0399 (3)0.9619 (3)0.13390 (16)0.0254 (5)
H2B0.10671.01550.16480.030*
C30.0992 (3)1.0424 (3)0.13077 (16)0.0251 (5)
H3A0.12941.15160.15990.030*
C40.1952 (3)0.9626 (3)0.08458 (15)0.0211 (5)
H4A0.29051.01600.08060.025*
C50.1476 (2)0.8040 (2)0.04484 (14)0.0156 (4)
N20.0005 (2)0.5440 (2)0.11285 (11)0.0142 (3)
C70.1356 (2)0.6381 (2)0.10328 (14)0.0151 (4)
C80.1721 (3)0.6746 (3)0.17544 (15)0.0179 (4)
H8A0.26850.74070.16780.022*
C90.0641 (3)0.6123 (3)0.25912 (15)0.0205 (5)
H9A0.08620.63450.31010.025*
C100.0762 (3)0.5175 (3)0.26814 (15)0.0209 (5)
H10A0.15160.47500.32520.025*
C110.1055 (3)0.4851 (3)0.19330 (14)0.0178 (4)
H11A0.20170.42050.19910.021*
Fe20.00000.00000.50000.01261 (11)
O30.01782 (17)0.18958 (17)0.53020 (10)0.0153 (3)
C170.1848 (2)0.1809 (2)0.56511 (14)0.0148 (4)
O40.23057 (18)0.30616 (18)0.59671 (10)0.0187 (3)
H4B0.21870.38540.55360.028*
N30.1606 (2)0.0853 (2)0.61532 (12)0.0152 (4)
C120.1935 (3)0.2305 (3)0.66982 (15)0.0196 (4)
H12A0.14060.31110.65110.024*
C130.3038 (3)0.2657 (3)0.75346 (15)0.0230 (5)
H13A0.32690.36960.79170.028*
C140.3794 (3)0.1474 (3)0.78026 (15)0.0227 (5)
H14A0.45310.16900.83790.027*
C150.3476 (3)0.0033 (3)0.72266 (14)0.0193 (4)
H15A0.40010.08560.73950.023*
C160.2372 (2)0.0294 (2)0.64029 (14)0.0152 (4)
N40.1748 (2)0.0549 (2)0.45089 (11)0.0144 (3)
C180.2547 (2)0.1530 (2)0.49140 (14)0.0143 (4)
C190.3799 (2)0.2144 (2)0.46627 (15)0.0173 (4)
H19A0.43660.28170.49640.021*
C200.4208 (3)0.1750 (3)0.39562 (15)0.0201 (5)
H20A0.50530.21700.37590.024*
C210.3379 (3)0.0743 (3)0.35396 (15)0.0210 (5)
H21A0.36500.04650.30550.025*
C220.2155 (3)0.0147 (3)0.38364 (14)0.0181 (4)
H22A0.15940.05580.35590.022*
N50.4219 (2)0.3514 (2)0.29685 (14)0.0235 (4)
O50.4654 (3)0.4937 (2)0.32015 (15)0.0437 (5)
O60.3647 (2)0.2817 (2)0.34301 (13)0.0376 (5)
O70.4314 (2)0.2714 (2)0.22236 (12)0.0328 (4)
O80.5282 (2)0.5852 (2)0.09369 (13)0.0288 (4)
H8B0.551 (4)0.620 (4)0.128 (2)0.035 (9)*
H8C0.608 (4)0.540 (4)0.073 (2)0.042 (9)*
O90.2008 (2)0.5686 (2)0.46872 (13)0.0304 (4)
H9B0.261 (4)0.609 (4)0.440 (2)0.039 (9)*
H9C0.141 (4)0.642 (4)0.472 (2)0.040 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0152 (2)0.0130 (2)0.0105 (2)0.00328 (15)0.00487 (16)0.00282 (16)
O10.0176 (7)0.0187 (8)0.0142 (7)0.0049 (6)0.0053 (6)0.0057 (6)
C60.0161 (10)0.0152 (10)0.0139 (10)0.0015 (8)0.0049 (8)0.0030 (8)
O20.0169 (7)0.0202 (8)0.0183 (8)0.0005 (6)0.0063 (6)0.0016 (6)
N10.0190 (9)0.0149 (9)0.0122 (8)0.0033 (7)0.0051 (7)0.0030 (7)
C10.0226 (11)0.0216 (11)0.0222 (11)0.0083 (9)0.0125 (9)0.0075 (9)
C20.0309 (13)0.0224 (12)0.0265 (12)0.0110 (10)0.0148 (10)0.0038 (10)
C30.0320 (13)0.0146 (11)0.0250 (12)0.0036 (9)0.0076 (10)0.0010 (9)
C40.0228 (11)0.0180 (11)0.0207 (11)0.0011 (8)0.0057 (9)0.0033 (9)
C50.0178 (10)0.0176 (10)0.0126 (10)0.0039 (8)0.0048 (8)0.0058 (8)
N20.0190 (9)0.0137 (8)0.0108 (8)0.0039 (7)0.0052 (7)0.0034 (7)
C70.0183 (10)0.0140 (10)0.0146 (10)0.0052 (8)0.0068 (8)0.0033 (8)
C80.0207 (10)0.0171 (10)0.0203 (11)0.0060 (8)0.0103 (9)0.0074 (9)
C90.0291 (12)0.0214 (11)0.0157 (10)0.0096 (9)0.0105 (9)0.0077 (9)
C100.0272 (12)0.0222 (11)0.0137 (10)0.0077 (9)0.0047 (9)0.0057 (9)
C110.0196 (10)0.0182 (10)0.0150 (10)0.0032 (8)0.0046 (8)0.0037 (8)
Fe20.0132 (2)0.0125 (2)0.0123 (2)0.00184 (15)0.00522 (16)0.00204 (16)
O30.0144 (7)0.0159 (7)0.0173 (7)0.0029 (6)0.0063 (6)0.0051 (6)
C170.0151 (10)0.0146 (10)0.0157 (10)0.0029 (8)0.0056 (8)0.0043 (8)
O40.0238 (8)0.0161 (7)0.0186 (8)0.0057 (6)0.0082 (6)0.0062 (6)
N30.0139 (8)0.0172 (9)0.0149 (9)0.0018 (7)0.0062 (7)0.0028 (7)
C120.0186 (10)0.0193 (11)0.0215 (11)0.0025 (8)0.0102 (9)0.0019 (9)
C130.0237 (11)0.0212 (11)0.0192 (11)0.0019 (9)0.0088 (9)0.0045 (9)
C140.0171 (10)0.0325 (13)0.0144 (10)0.0001 (9)0.0032 (8)0.0016 (9)
C150.0177 (10)0.0256 (12)0.0174 (10)0.0042 (9)0.0079 (9)0.0075 (9)
C160.0144 (9)0.0191 (10)0.0147 (10)0.0030 (8)0.0079 (8)0.0048 (8)
N40.0155 (8)0.0125 (8)0.0137 (8)0.0001 (6)0.0049 (7)0.0005 (7)
C180.0150 (9)0.0121 (9)0.0133 (10)0.0007 (7)0.0038 (8)0.0002 (8)
C190.0168 (10)0.0140 (10)0.0201 (11)0.0027 (8)0.0063 (8)0.0016 (8)
C200.0175 (10)0.0189 (11)0.0237 (11)0.0022 (8)0.0108 (9)0.0003 (9)
C210.0237 (11)0.0225 (11)0.0191 (11)0.0011 (9)0.0110 (9)0.0052 (9)
C220.0193 (10)0.0181 (10)0.0179 (10)0.0017 (8)0.0069 (8)0.0058 (9)
N50.0241 (10)0.0217 (10)0.0264 (10)0.0069 (8)0.0078 (8)0.0077 (8)
O50.0525 (13)0.0184 (9)0.0577 (14)0.0020 (8)0.0184 (11)0.0041 (9)
O60.0452 (11)0.0375 (11)0.0421 (11)0.0104 (9)0.0231 (10)0.0203 (9)
O70.0396 (10)0.0306 (10)0.0269 (9)0.0080 (8)0.0098 (8)0.0037 (8)
O80.0291 (10)0.0402 (11)0.0240 (9)0.0189 (8)0.0112 (8)0.0129 (8)
O90.0385 (11)0.0208 (9)0.0306 (10)0.0069 (8)0.0176 (9)0.0002 (8)
Geometric parameters (Å, º) top
Fe1—O1i1.8598 (15)Fe2—N3ii1.9517 (18)
Fe1—O11.8598 (15)Fe2—N31.9517 (18)
Fe1—N21.9491 (17)O3—C171.416 (2)
Fe1—N2i1.9491 (17)C17—O41.374 (2)
Fe1—N1i1.9499 (17)C17—C161.523 (3)
Fe1—N11.9499 (17)C17—C181.530 (3)
O1—C61.417 (2)O4—H4B0.8400
C6—O21.373 (2)N3—C121.334 (3)
C6—C51.524 (3)N3—C161.347 (3)
C6—C71.533 (3)C12—C131.388 (3)
O2—H2A0.8400C12—H12A0.9500
N1—C11.342 (3)C13—C141.382 (3)
N1—C51.345 (3)C13—H13A0.9500
C1—C21.381 (3)C14—C151.392 (3)
C1—H1A0.9500C14—H14A0.9500
C2—C31.380 (3)C15—C161.380 (3)
C2—H2B0.9500C15—H15A0.9500
C3—C41.393 (3)N4—C221.338 (3)
C3—H3A0.9500N4—C181.346 (3)
C4—C51.376 (3)C18—C191.377 (3)
C4—H4A0.9500C19—C201.387 (3)
N2—C111.338 (3)C19—H19A0.9500
N2—C71.342 (3)C20—C211.385 (3)
C7—C81.383 (3)C20—H20A0.9500
C8—C91.385 (3)C21—C221.381 (3)
C8—H8A0.9500C21—H21A0.9500
C9—C101.385 (3)C22—H22A0.9500
C9—H9A0.9500N5—O51.223 (3)
C10—C111.384 (3)N5—O61.243 (3)
C10—H10A0.9500N5—O71.269 (3)
C11—H11A0.9500O8—H8B0.75 (3)
Fe2—O3ii1.8639 (14)O8—H8C0.87 (4)
Fe2—O31.8639 (14)O9—H9B0.84 (3)
Fe2—N41.9470 (17)O9—H9C0.82 (3)
Fe2—N4ii1.9470 (17)
O1i—Fe1—O1180.00 (3)O3ii—Fe2—N4ii82.45 (7)
O1i—Fe1—N297.30 (7)O3—Fe2—N4ii97.55 (7)
O1—Fe1—N282.70 (7)N4—Fe2—N4ii180.000 (1)
O1i—Fe1—N2i82.70 (7)O3ii—Fe2—N3ii82.95 (7)
O1—Fe1—N2i97.30 (7)O3—Fe2—N3ii97.05 (7)
N2—Fe1—N2i180.00 (9)N4—Fe2—N3ii92.90 (7)
O1i—Fe1—N1i82.59 (7)N4ii—Fe2—N3ii87.10 (7)
O1—Fe1—N1i97.41 (7)O3ii—Fe2—N397.05 (7)
N2—Fe1—N1i92.74 (7)O3—Fe2—N382.95 (7)
N2i—Fe1—N1i87.26 (7)N4—Fe2—N387.10 (7)
O1i—Fe1—N197.41 (7)N4ii—Fe2—N392.90 (7)
O1—Fe1—N182.59 (7)N3ii—Fe2—N3180.0
N2—Fe1—N187.26 (7)C17—O3—Fe2102.92 (11)
N2i—Fe1—N192.74 (7)O4—C17—O3114.71 (16)
N1i—Fe1—N1180.00 (11)O4—C17—C16110.15 (17)
C6—O1—Fe1103.10 (11)O3—C17—C16105.08 (16)
O2—C6—O1114.85 (17)O4—C17—C18114.79 (16)
O2—C6—C5110.09 (17)O3—C17—C18105.16 (16)
O1—C6—C5104.85 (16)C16—C17—C18106.15 (16)
O2—C6—C7114.71 (17)C17—O4—H4B109.5
O1—C6—C7104.45 (16)C12—N3—C16120.12 (19)
C5—C6—C7107.13 (16)C12—N3—Fe2129.47 (15)
C6—O2—H2A109.5C16—N3—Fe2110.30 (14)
C1—N1—C5119.93 (19)N3—C12—C13121.0 (2)
C1—N1—Fe1129.03 (15)N3—C12—H12A119.5
C5—N1—Fe1110.59 (14)C13—C12—H12A119.5
N1—C1—C2120.7 (2)C14—C13—C12119.0 (2)
N1—C1—H1A119.6C14—C13—H13A120.5
C2—C1—H1A119.6C12—C13—H13A120.5
C3—C2—C1119.6 (2)C13—C14—C15120.0 (2)
C3—C2—H2B120.2C13—C14—H14A120.0
C1—C2—H2B120.2C15—C14—H14A120.0
C2—C3—C4119.6 (2)C16—C15—C14117.8 (2)
C2—C3—H3A120.2C16—C15—H15A121.1
C4—C3—H3A120.2C14—C15—H15A121.1
C5—C4—C3117.9 (2)N3—C16—C15122.1 (2)
C5—C4—H4A121.0N3—C16—C17109.93 (17)
C3—C4—H4A121.0C15—C16—C17127.97 (19)
N1—C5—C4122.26 (19)C22—N4—C18120.05 (18)
N1—C5—C6109.77 (18)C22—N4—Fe2129.24 (15)
C4—C5—C6127.92 (19)C18—N4—Fe2110.63 (13)
C11—N2—C7120.44 (18)N4—C18—C19122.02 (19)
C11—N2—Fe1128.93 (15)N4—C18—C17109.84 (17)
C7—N2—Fe1110.43 (14)C19—C18—C17128.14 (19)
N2—C7—C8121.75 (19)C18—C19—C20118.1 (2)
N2—C7—C6110.01 (17)C18—C19—H19A121.0
C8—C7—C6128.23 (19)C20—C19—H19A121.0
C7—C8—C9118.2 (2)C21—C20—C19119.72 (19)
C7—C8—H8A120.9C21—C20—H20A120.1
C9—C8—H8A120.9C19—C20—H20A120.1
C8—C9—C10119.6 (2)C22—C21—C20119.2 (2)
C8—C9—H9A120.2C22—C21—H21A120.4
C10—C9—H9A120.2C20—C21—H21A120.4
C11—C10—C9119.3 (2)N4—C22—C21120.9 (2)
C11—C10—H10A120.3N4—C22—H22A119.5
C9—C10—H10A120.3C21—C22—H22A119.5
N2—C11—C10120.6 (2)O5—N5—O6122.2 (2)
N2—C11—H11A119.7O5—N5—O7119.6 (2)
C10—C11—H11A119.7O6—N5—O7118.2 (2)
O3ii—Fe2—O3180.0H8B—O8—H8C106 (3)
O3ii—Fe2—N497.55 (7)H9B—O9—H9C106 (3)
O3—Fe2—N482.45 (7)
Symmetry codes: (i) x, y+1, z; (ii) x, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2A···O80.841.762.604 (2)178
O4—H4B···O90.841.822.660 (2)174
 

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