The title compound, [Fe3O(C2H2ClO2)6(H2O)3]NO3·3H2O, contains an FeIII trimeric cation in which the three FeIII ions are at the corners of a slightly distorted triangle with an O atom in the centre. Two monochloroacetate ligands bridge each pair of FeIII ions and a water molecule coordinates each FeIII ion at the apex, opposite to the central O atom. Hence, the FeIII ions are surrounded by distorted oxygen octahedra. The distances between the FeIII ions and the central O atoms are considerably shorter than those between the FeIII ions and the other coordinated O atoms. The trimeric cations form a three-dimensional connected network via hydrogen-bonding interactions to extra-cluster water molecules and nitrate anions.
Supporting information
CCDC reference: 231804
Key indicators
- Single-crystal X-ray study
- T = 293 K
- R factor = 0.035
- wR factor = 0.099
- Data-to-parameter ratio = 13.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O4W - H4WB ... ?
PLAT420_ALERT_2_B D-H Without Acceptor >O6W - >H6WA ... ?
PLAT420_ALERT_2_B D-H Without Acceptor >O6W - >H6WB ... ?
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C2
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C10
PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... N1
PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 12.00 Perc.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 14
PLAT757_ALERT_4_C D...A Calc 3.08458, Rep 3.085(3) ...... Senseless su
O5W -O10 1.555 2.645
PLAT757_ALERT_4_C D...A Calc 3.08402, Rep 3.084(5) ...... Senseless su
O5W -O102 1.555 1.555
PLAT757_ALERT_4_C D...A Calc 3.21290, Rep 3.214(6) ...... Senseless su
O5W -O103 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 25.70 Deg.
CL1 -C2 -CL1' 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 22.20 Deg.
CL3' -C6 -CL3 1.555 1.555 1.555
0 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
14 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
7 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
6 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS (Stoe & Cie, 1998); cell refinement: IPDS; data reduction: X-RED (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
Triaqua-1
κO,2
κO,3
κO-hexakis-µ-monochloroacetato-
1:2
κ4O:
O';2:3
κ4O:
O';1:3
κ4O:
O'-µ
3-oxo-triiron(III) nitrate trihydrate
top
Crystal data top
[Fe3O(C2H2ClO2)6(H2O)3]NO3·3H2O | F(000) = 1836 |
Mr = 914.57 | Dx = 1.878 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 24332 reflections |
a = 12.523 (3) Å | θ = 1.8–32.2° |
b = 14.768 (3) Å | µ = 1.91 mm−1 |
c = 17.601 (4) Å | T = 293 K |
β = 96.35 (3)° | Block, red |
V = 3235.1 (11) Å3 | 0.4 × 0.4 × 0.3 mm |
Z = 4 | |
Data collection top
Stoe IPDS II diffractometer | 5682 independent reflections |
Radiation source: fine-focus sealed tube | 4634 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
φ scans | θmax = 25.0°, θmin = 2.1° |
Absorption correction: numerical (IPDS; Stoe & Cie, 1998) | h = −14→14 |
Tmin = 0.598, Tmax = 0.677 | k = −17→17 |
20401 measured reflections | l = −20→20 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.035 | H-atom parameters constrained |
wR(F2) = 0.099 | w = 1/[σ2(Fo2) + (0.065P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
5682 reflections | Δρmax = 0.81 e Å−3 |
425 parameters | Δρmin = −0.62 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997a), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0037 (4) |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Fe1 | 0.16289 (3) | 0.53507 (3) | 0.26795 (3) | 0.02671 (14) | |
Fe2 | 0.15971 (3) | 0.69874 (3) | 0.39758 (3) | 0.02638 (13) | |
Fe3 | 0.38400 (3) | 0.58768 (3) | 0.37855 (3) | 0.02703 (13) | |
Cl1 | 0.3721 (8) | 0.6029 (10) | 0.0531 (2) | 0.087 (3) | 0.58 (2) |
Cl1' | 0.3901 (6) | 0.5518 (15) | 0.0564 (3) | 0.098 (3) | 0.42 (2) |
Cl2 | 0.40111 (10) | 0.26626 (8) | 0.45033 (7) | 0.0651 (3) | |
Cl3 | −0.0748 (13) | 0.723 (2) | 0.0951 (3) | 0.082 (4) | 0.54 (4) |
Cl3' | −0.0353 (17) | 0.7569 (7) | 0.0936 (3) | 0.058 (3) | 0.46 (4) |
Cl4 | −0.16233 (7) | 0.55964 (7) | 0.47384 (6) | 0.0480 (2) | |
Cl5 | 0.54314 (10) | 0.86320 (9) | 0.31807 (11) | 0.0871 (5) | |
Cl6 | 0.27184 (8) | 0.70058 (8) | 0.67022 (6) | 0.0532 (3) | |
O1 | 0.23500 (16) | 0.60744 (14) | 0.34763 (12) | 0.0265 (5) | |
O2 | 0.42305 (19) | 0.5769 (2) | 0.27254 (15) | 0.0467 (6) | |
O3 | 0.27375 (19) | 0.55714 (18) | 0.19306 (14) | 0.0385 (6) | |
O4 | 0.37267 (19) | 0.45131 (16) | 0.39057 (16) | 0.0414 (6) | |
O5 | 0.23616 (19) | 0.41828 (16) | 0.30239 (15) | 0.0394 (6) | |
O6 | 0.07765 (19) | 0.63709 (17) | 0.21230 (14) | 0.0375 (5) | |
O7 | 0.0731 (2) | 0.74207 (17) | 0.30216 (15) | 0.0437 (6) | |
O8 | 0.04009 (18) | 0.50689 (16) | 0.32835 (14) | 0.0365 (5) | |
O9 | 0.03890 (18) | 0.61447 (16) | 0.41758 (15) | 0.0367 (5) | |
O10 | 0.26591 (18) | 0.79940 (15) | 0.37992 (15) | 0.0374 (6) | |
O11 | 0.41725 (18) | 0.72095 (16) | 0.37511 (17) | 0.0430 (6) | |
O12 | 0.37796 (18) | 0.59348 (18) | 0.49122 (14) | 0.0379 (6) | |
O13 | 0.23212 (18) | 0.67743 (17) | 0.50410 (14) | 0.0368 (5) | |
O1W | 0.08128 (19) | 0.45735 (17) | 0.18504 (14) | 0.0394 (6) | |
H1WA | 0.1129 | 0.4064 | 0.1856 | 0.047* | |
H1WB | 0.0889 | 0.4820 | 0.1423 | 0.047* | |
O2W | 0.07216 (19) | 0.79589 (17) | 0.44474 (16) | 0.0421 (6) | |
H2WA | 0.0160 | 0.7721 | 0.4592 | 0.063* | |
H2WB | 0.0542 | 0.8365 | 0.4115 | 0.063* | |
O3W | 0.54858 (17) | 0.57309 (17) | 0.40605 (15) | 0.0389 (6) | |
H3WB | 0.5636 | 0.6020 | 0.4476 | 0.047* | |
H3WA | 0.5844 | 0.5987 | 0.3737 | 0.047* | |
C1 | 0.3718 (3) | 0.5750 (2) | 0.2081 (2) | 0.0367 (8) | |
C2 | 0.4394 (3) | 0.6004 (3) | 0.1461 (2) | 0.0529 (10) | |
H2A | 0.5126 | 0.5802 | 0.1603 | 0.063* | |
H2B | 0.4405 | 0.6658 | 0.1412 | 0.063* | |
C3 | 0.3107 (3) | 0.3977 (2) | 0.3531 (2) | 0.0346 (8) | |
C4 | 0.3251 (4) | 0.2973 (3) | 0.3646 (3) | 0.0569 (12) | |
H4A | 0.3596 | 0.2730 | 0.3223 | 0.068* | |
H4B | 0.2547 | 0.2695 | 0.3630 | 0.068* | |
C5 | 0.0503 (2) | 0.7123 (2) | 0.2364 (2) | 0.0321 (7) | |
C6 | −0.0180 (3) | 0.7771 (3) | 0.1863 (2) | 0.0487 (10) | |
H6A | 0.0134 | 0.8370 | 0.1937 | 0.058* | |
H6B | −0.0883 | 0.7793 | 0.2044 | 0.058* | |
C7 | 0.0034 (2) | 0.5450 (2) | 0.38399 (19) | 0.0285 (7) | |
C8 | −0.0915 (3) | 0.4962 (2) | 0.4113 (2) | 0.0359 (8) | |
H8A | −0.0660 | 0.4409 | 0.4369 | 0.043* | |
H8B | −0.1406 | 0.4792 | 0.3671 | 0.043* | |
C9 | 0.3635 (2) | 0.7916 (2) | 0.36991 (19) | 0.0303 (7) | |
C10 | 0.4178 (3) | 0.8787 (2) | 0.3520 (2) | 0.0406 (8) | |
H10A | 0.4274 | 0.9156 | 0.3978 | 0.049* | |
H10B | 0.3712 | 0.9117 | 0.3138 | 0.049* | |
C11 | 0.3152 (2) | 0.6358 (2) | 0.52996 (19) | 0.0307 (7) | |
C12 | 0.3476 (3) | 0.6314 (3) | 0.6148 (2) | 0.0389 (8) | |
H12A | 0.4226 | 0.6486 | 0.6247 | 0.047* | |
H12B | 0.3415 | 0.5691 | 0.6313 | 0.047* | |
N1 | 0.7387 (3) | 0.6175 (2) | 0.2832 (2) | 0.0493 (8) | |
O101 | 0.6878 (3) | 0.6670 (2) | 0.3224 (2) | 0.0739 (10) | |
O102 | 0.7062 (3) | 0.5407 (3) | 0.2676 (3) | 0.0844 (11) | |
O103 | 0.8243 (3) | 0.6441 (3) | 0.2641 (3) | 0.1067 (17) | |
O4W | 0.85242 (18) | 0.80864 (17) | 0.38804 (16) | 0.0678 (9) | |
H4WA | 0.8210 | 0.7695 | 0.3580 | 0.081* | |
H4WB | 0.8176 | 0.8112 | 0.4268 | 0.081* | |
O5W | 0.86887 (18) | 0.47066 (17) | 0.16201 (16) | 0.0841 (12) | |
H5WA | 0.8586 | 0.4227 | 0.1875 | 0.101* | |
H5WB | 0.8347 | 0.5169 | 0.1749 | 0.101* | |
O6W | 0.1044 (5) | 0.9270 (4) | 0.5427 (3) | 0.094 (2) | 0.670 (8) |
H6WA | 0.1574 | 0.8951 | 0.5615 | 0.112* | 0.670 (8) |
H6WB | 0.1283 | 0.9721 | 0.5198 | 0.112* | 0.670 (8) |
O7W | 0.7833 (13) | 0.9143 (8) | 0.5050 (7) | 0.098 (5) | 0.330 (8) |
H7WA | 0.7174 | 0.9279 | 0.5058 | 0.118* | 0.330 (8) |
H7WB | 0.8071 | 0.8872 | 0.5460 | 0.118* | 0.330 (8) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0260 (2) | 0.0252 (2) | 0.0292 (3) | 0.00076 (17) | 0.00446 (17) | 0.00020 (19) |
Fe2 | 0.0226 (2) | 0.0226 (2) | 0.0346 (3) | 0.00037 (16) | 0.00585 (17) | −0.00076 (19) |
Fe3 | 0.0213 (2) | 0.0235 (2) | 0.0369 (3) | 0.00034 (16) | 0.00618 (17) | 0.00037 (19) |
Cl1 | 0.087 (4) | 0.139 (6) | 0.0375 (13) | −0.034 (3) | 0.0191 (14) | 0.010 (2) |
Cl1' | 0.101 (3) | 0.154 (8) | 0.047 (2) | 0.042 (4) | 0.0321 (19) | 0.020 (3) |
Cl2 | 0.0728 (7) | 0.0418 (6) | 0.0756 (8) | 0.0042 (5) | −0.0139 (6) | 0.0149 (5) |
Cl3 | 0.072 (4) | 0.133 (10) | 0.0389 (14) | 0.046 (6) | −0.0048 (17) | −0.002 (2) |
Cl3' | 0.078 (6) | 0.063 (4) | 0.0303 (14) | 0.028 (3) | −0.0020 (18) | 0.0014 (14) |
Cl4 | 0.0349 (4) | 0.0535 (6) | 0.0586 (6) | −0.0027 (4) | 0.0189 (4) | −0.0026 (5) |
Cl5 | 0.0594 (7) | 0.0531 (7) | 0.1596 (15) | −0.0036 (5) | 0.0608 (8) | 0.0183 (8) |
Cl6 | 0.0556 (6) | 0.0613 (7) | 0.0436 (5) | 0.0082 (5) | 0.0086 (4) | −0.0122 (5) |
O1 | 0.0234 (10) | 0.0239 (11) | 0.0327 (12) | 0.0000 (8) | 0.0052 (8) | 0.0006 (9) |
O2 | 0.0306 (12) | 0.0676 (18) | 0.0434 (15) | 0.0006 (12) | 0.0111 (11) | −0.0080 (14) |
O3 | 0.0349 (13) | 0.0474 (15) | 0.0350 (13) | 0.0008 (10) | 0.0114 (10) | −0.0001 (11) |
O4 | 0.0325 (12) | 0.0226 (12) | 0.0669 (18) | −0.0013 (9) | −0.0050 (11) | 0.0027 (12) |
O5 | 0.0416 (13) | 0.0256 (12) | 0.0490 (15) | 0.0035 (10) | −0.0043 (11) | 0.0012 (11) |
O6 | 0.0402 (13) | 0.0343 (13) | 0.0368 (13) | 0.0099 (10) | −0.0005 (10) | 0.0023 (11) |
O7 | 0.0469 (14) | 0.0382 (14) | 0.0437 (15) | 0.0139 (11) | −0.0056 (11) | −0.0038 (12) |
O8 | 0.0351 (12) | 0.0370 (13) | 0.0389 (14) | −0.0092 (10) | 0.0109 (10) | −0.0030 (11) |
O9 | 0.0305 (11) | 0.0330 (13) | 0.0483 (14) | −0.0047 (10) | 0.0130 (10) | −0.0065 (11) |
O10 | 0.0324 (12) | 0.0282 (12) | 0.0533 (15) | −0.0033 (9) | 0.0122 (10) | −0.0010 (11) |
O11 | 0.0275 (11) | 0.0274 (13) | 0.0738 (19) | −0.0032 (10) | 0.0047 (11) | 0.0047 (12) |
O12 | 0.0296 (12) | 0.0497 (15) | 0.0353 (13) | 0.0065 (10) | 0.0071 (10) | −0.0018 (11) |
O13 | 0.0332 (12) | 0.0398 (13) | 0.0370 (13) | 0.0072 (10) | 0.0025 (10) | −0.0003 (11) |
O1W | 0.0418 (13) | 0.0365 (13) | 0.0392 (14) | 0.0018 (10) | 0.0013 (10) | −0.0057 (11) |
O2W | 0.0354 (12) | 0.0390 (14) | 0.0532 (16) | 0.0064 (10) | 0.0106 (11) | −0.0064 (12) |
O3W | 0.0266 (11) | 0.0415 (14) | 0.0494 (15) | 0.0012 (10) | 0.0077 (10) | 0.0024 (12) |
C1 | 0.0371 (19) | 0.0300 (17) | 0.046 (2) | 0.0049 (14) | 0.0190 (16) | 0.0012 (16) |
C2 | 0.052 (2) | 0.060 (3) | 0.052 (2) | 0.0057 (19) | 0.0274 (19) | 0.010 (2) |
C3 | 0.0280 (16) | 0.0266 (17) | 0.050 (2) | −0.0006 (13) | 0.0094 (15) | −0.0007 (16) |
C4 | 0.053 (2) | 0.029 (2) | 0.083 (3) | −0.0038 (17) | −0.021 (2) | 0.006 (2) |
C5 | 0.0243 (15) | 0.0304 (18) | 0.042 (2) | 0.0024 (13) | 0.0067 (13) | 0.0100 (16) |
C6 | 0.048 (2) | 0.043 (2) | 0.054 (2) | 0.0087 (17) | −0.0017 (18) | 0.0147 (19) |
C7 | 0.0254 (15) | 0.0268 (16) | 0.0329 (17) | −0.0017 (12) | 0.0017 (13) | 0.0046 (14) |
C8 | 0.0306 (16) | 0.0389 (19) | 0.0392 (19) | −0.0080 (14) | 0.0092 (14) | 0.0009 (16) |
C9 | 0.0315 (17) | 0.0259 (17) | 0.0335 (17) | −0.0050 (13) | 0.0041 (13) | −0.0011 (14) |
C10 | 0.0365 (18) | 0.0298 (18) | 0.057 (2) | −0.0049 (14) | 0.0125 (16) | 0.0029 (17) |
C11 | 0.0267 (15) | 0.0285 (16) | 0.0376 (18) | −0.0064 (13) | 0.0063 (13) | 0.0021 (15) |
C12 | 0.0366 (18) | 0.045 (2) | 0.0357 (19) | 0.0033 (15) | 0.0049 (14) | −0.0001 (17) |
N1 | 0.0403 (17) | 0.050 (2) | 0.060 (2) | 0.0063 (15) | 0.0130 (16) | 0.0121 (18) |
O101 | 0.075 (2) | 0.060 (2) | 0.092 (3) | 0.0108 (17) | 0.031 (2) | −0.0043 (19) |
O102 | 0.091 (3) | 0.061 (2) | 0.101 (3) | −0.0123 (19) | 0.006 (2) | −0.015 (2) |
O103 | 0.063 (2) | 0.102 (3) | 0.165 (5) | 0.001 (2) | 0.062 (3) | 0.041 (3) |
O4W | 0.0586 (19) | 0.061 (2) | 0.082 (2) | −0.0081 (15) | 0.0015 (16) | 0.0166 (18) |
O5W | 0.0531 (19) | 0.073 (2) | 0.127 (3) | −0.0043 (16) | 0.016 (2) | −0.043 (2) |
O6W | 0.103 (4) | 0.104 (5) | 0.080 (4) | −0.047 (4) | 0.035 (3) | −0.071 (4) |
O7W | 0.158 (13) | 0.066 (8) | 0.076 (8) | 0.042 (8) | 0.042 (8) | 0.023 (6) |
Geometric parameters (Å, º) top
Fe1—O1 | 1.909 (2) | O13—C11 | 1.250 (4) |
Fe1—O8 | 2.007 (2) | O1W—H1WA | 0.8501 |
Fe1—O5 | 2.015 (2) | O1W—H1WB | 0.8500 |
Fe1—O6 | 2.034 (2) | O2W—H2WA | 0.8500 |
Fe1—O1W | 2.040 (2) | O2W—H2WB | 0.8501 |
Fe1—O3 | 2.043 (2) | O3W—H3WB | 0.8501 |
Fe2—O1 | 1.914 (2) | O3W—H3WA | 0.8510 |
Fe2—O7 | 2.001 (3) | C1—C2 | 1.501 (5) |
Fe2—O13 | 2.015 (2) | C2—H2A | 0.9700 |
Fe2—O9 | 2.020 (2) | C2—H2B | 0.9700 |
Fe2—O2W | 2.037 (2) | C3—C4 | 1.505 (5) |
Fe2—O10 | 2.041 (2) | C4—H4A | 0.9700 |
Fe3—O1 | 1.907 (2) | C4—H4B | 0.9700 |
Fe3—O2 | 1.987 (3) | C5—C6 | 1.502 (5) |
Fe3—O12 | 1.995 (2) | C6—H6A | 0.9700 |
Fe3—O11 | 2.014 (2) | C6—H6B | 0.9700 |
Fe3—O4 | 2.032 (2) | C7—C8 | 1.513 (4) |
Fe3—O3W | 2.076 (2) | C8—H8A | 0.9700 |
Cl1—C2 | 1.757 (7) | C8—H8B | 0.9700 |
Cl1'—C2 | 1.783 (12) | C9—C10 | 1.505 (5) |
Cl2—C4 | 1.754 (4) | C10—H10A | 0.9700 |
Cl3—C6 | 1.863 (17) | C10—H10B | 0.9700 |
Cl3'—C6 | 1.649 (7) | C11—C12 | 1.504 (5) |
Cl4—C8 | 1.759 (4) | C12—H12A | 0.9700 |
Cl5—C10 | 1.755 (4) | C12—H12B | 0.9700 |
Cl6—C12 | 1.762 (4) | N1—O103 | 1.223 (5) |
O2—C1 | 1.240 (5) | N1—O102 | 1.226 (5) |
O3—C1 | 1.255 (4) | N1—O101 | 1.230 (5) |
O4—C3 | 1.245 (4) | O4W—H4WA | 0.8497 |
O5—C3 | 1.256 (4) | O4W—H4WB | 0.8500 |
O6—C5 | 1.250 (4) | O5W—H5WA | 0.8551 |
O7—C5 | 1.242 (4) | O5W—H5WB | 0.8503 |
O8—C7 | 1.260 (4) | O6W—H6WA | 0.8500 |
O9—C7 | 1.241 (4) | O6W—H6WB | 0.8500 |
O10—C9 | 1.259 (4) | O7W—H7WA | 0.8500 |
O11—C9 | 1.240 (4) | O7W—H7WB | 0.8500 |
O12—C11 | 1.261 (4) | | |
| | | |
O1—Fe1—O8 | 93.14 (9) | O2—C1—O3 | 126.4 (3) |
O1—Fe1—O5 | 95.48 (10) | O2—C1—C2 | 112.5 (3) |
O8—Fe1—O5 | 90.76 (11) | O3—C1—C2 | 121.1 (4) |
O1—Fe1—O6 | 96.87 (10) | C1—C2—Cl1 | 115.5 (4) |
O8—Fe1—O6 | 90.95 (10) | C1—C2—Cl1' | 112.1 (5) |
O5—Fe1—O6 | 167.42 (10) | Cl1—C2—Cl1' | 25.7 (2) |
O1—Fe1—O1W | 177.95 (10) | C1—C2—H2A | 109.2 |
O8—Fe1—O1W | 84.81 (10) | Cl1—C2—H2A | 126.1 |
O5—Fe1—O1W | 84.78 (10) | Cl1'—C2—H2A | 109.2 |
O6—Fe1—O1W | 82.96 (10) | C1—C2—H2B | 109.2 |
O1—Fe1—O3 | 94.86 (10) | Cl1—C2—H2B | 84.6 |
O8—Fe1—O3 | 171.70 (10) | Cl1'—C2—H2B | 109.2 |
O5—Fe1—O3 | 90.66 (11) | H2A—C2—H2B | 107.9 |
O6—Fe1—O3 | 85.93 (10) | O4—C3—O5 | 126.4 (3) |
O1W—Fe1—O3 | 87.17 (10) | O4—C3—C4 | 119.8 (3) |
O1—Fe2—O7 | 95.09 (10) | O5—C3—C4 | 113.7 (3) |
O1—Fe2—O13 | 97.09 (9) | C3—C4—Cl2 | 114.7 (3) |
O7—Fe2—O13 | 167.77 (10) | C3—C4—H4A | 108.6 |
O1—Fe2—O9 | 93.58 (9) | Cl2—C4—H4A | 108.6 |
O7—Fe2—O9 | 89.78 (11) | C3—C4—H4B | 108.6 |
O13—Fe2—O9 | 90.59 (10) | Cl2—C4—H4B | 108.6 |
O1—Fe2—O2W | 176.27 (10) | H4A—C4—H4B | 107.6 |
O7—Fe2—O2W | 81.40 (11) | O7—C5—O6 | 126.0 (3) |
O13—Fe2—O2W | 86.45 (10) | O7—C5—C6 | 112.2 (3) |
O9—Fe2—O2W | 85.17 (10) | O6—C5—C6 | 121.8 (3) |
O1—Fe2—O10 | 94.63 (9) | C5—C6—Cl3' | 118.0 (4) |
O7—Fe2—O10 | 86.64 (11) | C5—C6—Cl3 | 111.7 (6) |
O13—Fe2—O10 | 91.24 (11) | Cl3'—C6—Cl3 | 22.2 (2) |
O9—Fe2—O10 | 171.30 (10) | C5—C6—H6A | 107.8 |
O2W—Fe2—O10 | 86.46 (10) | Cl3'—C6—H6A | 107.8 |
O1—Fe3—O2 | 94.53 (10) | Cl3—C6—H6A | 128.2 |
O1—Fe3—O12 | 97.68 (10) | C5—C6—H6B | 107.8 |
O2—Fe3—O12 | 167.79 (10) | Cl3'—C6—H6B | 107.8 |
O1—Fe3—O11 | 92.34 (9) | Cl3—C6—H6B | 91.3 |
O2—Fe3—O11 | 88.70 (12) | H6A—C6—H6B | 107.2 |
O12—Fe3—O11 | 91.07 (11) | O9—C7—O8 | 126.7 (3) |
O1—Fe3—O4 | 95.97 (9) | O9—C7—C8 | 119.7 (3) |
O2—Fe3—O4 | 92.59 (12) | O8—C7—C8 | 113.6 (3) |
O12—Fe3—O4 | 85.89 (11) | C7—C8—Cl4 | 114.4 (3) |
O11—Fe3—O4 | 171.46 (10) | C7—C8—H8A | 108.7 |
O1—Fe3—O3W | 175.75 (10) | Cl4—C8—H8A | 108.7 |
O2—Fe3—O3W | 82.50 (11) | C7—C8—H8B | 108.7 |
O12—Fe3—O3W | 85.32 (10) | Cl4—C8—H8B | 108.7 |
O11—Fe3—O3W | 84.56 (10) | H8A—C8—H8B | 107.6 |
O4—Fe3—O3W | 87.23 (10) | O11—C9—O10 | 126.5 (3) |
Fe3—O1—Fe1 | 119.49 (11) | O11—C9—C10 | 118.7 (3) |
Fe3—O1—Fe2 | 119.52 (11) | O10—C9—C10 | 114.8 (3) |
Fe1—O1—Fe2 | 120.99 (11) | C9—C10—Cl5 | 113.7 (3) |
C1—O2—Fe3 | 134.7 (2) | C9—C10—H10A | 108.8 |
C1—O3—Fe1 | 128.0 (2) | Cl5—C10—H10A | 108.8 |
C3—O4—Fe3 | 128.4 (2) | C9—C10—H10B | 108.8 |
C3—O5—Fe1 | 134.4 (2) | Cl5—C10—H10B | 108.8 |
C5—O6—Fe1 | 130.1 (2) | H10A—C10—H10B | 107.7 |
C5—O7—Fe2 | 135.8 (2) | O13—C11—O12 | 126.1 (3) |
C7—O8—Fe1 | 133.3 (2) | O13—C11—C12 | 120.3 (3) |
C7—O9—Fe2 | 131.4 (2) | O12—C11—C12 | 113.5 (3) |
C9—O10—Fe2 | 127.8 (2) | C11—C12—Cl6 | 115.0 (3) |
C9—O11—Fe3 | 135.4 (2) | C11—C12—H12A | 108.5 |
C11—O12—Fe3 | 130.8 (2) | Cl6—C12—H12A | 108.5 |
C11—O13—Fe2 | 133.3 (2) | C11—C12—H12B | 108.5 |
Fe1—O1W—H1WA | 107.0 | Cl6—C12—H12B | 108.5 |
Fe1—O1W—H1WB | 107.2 | H12A—C12—H12B | 107.5 |
H1WA—O1W—H1WB | 106.9 | O103—N1—O102 | 121.0 (4) |
Fe2—O2W—H2WA | 109.4 | O103—N1—O101 | 119.2 (4) |
Fe2—O2W—H2WB | 109.2 | O102—N1—O101 | 119.7 (4) |
H2WA—O2W—H2WB | 109.5 | H4WA—O4W—H4WB | 106.6 |
Fe3—O3W—H3WB | 105.6 | H5WA—O5W—H5WB | 114.5 |
Fe3—O3W—H3WA | 112.4 | H6WA—O6W—H6WB | 108.6 |
H3WB—O3W—H3WA | 105.6 | H7WA—O7W—H7WB | 110.4 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O4Wi | 0.85 | 2.02 | 2.721 (4) | 139 |
O1W—H1WB···O6Wii | 0.85 | 2.23 | 3.071 (5) | 168 |
O2W—H2WA···O4Wiii | 0.85 | 2.34 | 2.828 (3) | 117 |
O2W—H2WA···Cl3′iv | 0.85 | 2.55 | 3.172 (10) | 130 |
O3W—H3WA···O101 | 0.85 | 1.94 | 2.774 (4) | 166 |
O6W—H6WB···O7Wv | 0.85 | 2.08 | 2.904 (15) | 162 |
O4W—H4WA···O101 | 0.85 | 2.29 | 3.071 (5) | 153 |
O4W—H4WA···O103 | 0.85 | 2.49 | 3.258 (6) | 152 |
O4W—H4WB···O7W | 0.85 | 2.13 | 2.796 (12) | 135 |
O5W—H5WA···O10i | 0.86 | 2.60 | 3.085 (3) | 117 |
O5W—H5WB···O102 | 0.85 | 2.44 | 3.084 (5) | 133 |
O5W—H5WB···O103 | 0.85 | 2.46 | 3.214 (6) | 148 |
O7W—H7WA···Cl1′vi | 0.85 | 2.46 | 3.08 (2) | 131 |
O7W—H7WB···Cl3vii | 0.85 | 2.30 | 3.03 (3) | 143 |
O6W—H6WA···Cl1iv | 0.85 | 2.71 | 3.365 (10) | 135 |
O6W—H6WB···O7Wv | 0.85 | 2.08 | 2.904 (15) | 162 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) x, −y+3/2, z−1/2; (iii) x−1, y, z; (iv) x, −y+3/2, z+1/2; (v) −x+1, −y+2, −z+1; (vi) −x+1, y+1/2, −z+1/2; (vii) x+1, −y+3/2, z+1/2. |