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The low-spin iron(II) ion in the title compound, [Fe(C12H12N2)3](ClO4)2·C12H12N2, possesses an octahedral geometry formed by three bidentate 5,5′-dimethyl-2,2′-bipyridyl ligands. An uncoordinated ligand and two perchlorate anions are also present in the crystal structure.
Supporting information
CCDC reference: 277770
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.006 Å
- Disorder in main residue
- R factor = 0.078
- wR factor = 0.238
- Data-to-parameter ratio = 16.9
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O23
| Author Response: the A alert (and also some B alerts) come
from the treatment of the disordered perchlorate
anion
|
Alert level B
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O22
| Author Response: the A alert (and also some B alerts) come
from the treatment of the disordered perchlorate
anion
|
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O34
| Author Response: the A alert (and also some B alerts) come
from the treatment of the disordered perchlorate
anion
|
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Cl3
Alert level C
RINTA01_ALERT_3_C The value of Rint is greater than 0.10
Rint given 0.108
PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT215_ALERT_3_C Disordered O32 has ADP max/min Ratio ....... 3.30
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.26 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O21
| Author Response: the A alert (and also some B alerts) come
from the treatment of the disordered perchlorate
anion
|
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cl2
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O33
PLAT301_ALERT_3_C Main Residue Disorder ......................... 7.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O22
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O24
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O32
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O34
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C17
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C27
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C37
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C57
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C67
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C77
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C87
PLAT413_ALERT_2_C Short Inter XH3 .. XHn H27A .. H33A .. 2.14 Ang.
PLAT413_ALERT_2_C Short Inter XH3 .. XHn H47A .. H73A .. 2.10 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
C12 H12 N2
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4
Cl O4
1 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
24 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 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
9 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 2002); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1990); software used to prepare material for publication: SHELXTL.
Tris(5,5'-dimethyl-2,2'-bipyridyl-
κ2N,
N')iron(II)
bis(perchlorate) 5,5'-dimethyl-2,2'-bipyridyl solvate
top
Crystal data top
[Fe(C12H12N2)3](ClO4)2·C12H12N2 | Z = 2 |
Mr = 991.69 | F(000) = 1032 |
Triclinic, P1 | Dx = 1.431 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.670 (2) Å | Cell parameters from 32869 reflections |
b = 13.466 (3) Å | θ = 2.7–27.5° |
c = 14.792 (3) Å | µ = 0.51 mm−1 |
α = 94.77 (3)° | T = 173 K |
β = 90.82 (3)° | Plate, red |
γ = 96.26 (3)° | 0.35 × 0.10 × 0.02 mm |
V = 2302.0 (8) Å3 | |
Data collection top
Nonius KappaCCD diffractometer | 10528 independent reflections |
Radiation source: fine-focus sealed tube | 6461 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.108 |
ω scans | θmax = 27.5°, θmin = 2.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→15 |
Tmin = 0.842, Tmax = 0.990 | k = −17→17 |
32869 measured reflections | l = −19→19 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.078 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.238 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.130P)2 + 0.9561P] where P = (Fo2 + 2Fc2)/3 |
10528 reflections | (Δ/σ)max = 0.001 |
622 parameters | Δρmax = 0.98 e Å−3 |
18 restraints | Δρmin = −0.94 e Å−3 |
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 | 0.72986 (4) | 0.14446 (4) | 0.25751 (4) | 0.02072 (18) | |
N11 | 0.8357 (3) | 0.2596 (2) | 0.3139 (2) | 0.0217 (7) | |
C12 | 0.8028 (3) | 0.3512 (3) | 0.3022 (3) | 0.0232 (9) | |
C13 | 0.8652 (3) | 0.4398 (3) | 0.3397 (3) | 0.0276 (9) | |
H13A | 0.8402 | 0.5031 | 0.3305 | 0.033* | |
C14 | 0.9643 (4) | 0.4335 (3) | 0.3909 (3) | 0.0299 (10) | |
H14A | 1.0080 | 0.4931 | 0.4165 | 0.036* | |
C15 | 1.0001 (3) | 0.3418 (3) | 0.4049 (3) | 0.0298 (10) | |
C16 | 0.9331 (3) | 0.2566 (3) | 0.3644 (3) | 0.0276 (9) | |
H16A | 0.9573 | 0.1928 | 0.3729 | 0.033* | |
C17 | 1.1072 (4) | 0.3324 (4) | 0.4609 (4) | 0.0435 (13) | |
H17A | 1.1425 | 0.3993 | 0.4836 | 0.065* | |
H17B | 1.1621 | 0.2987 | 0.4231 | 0.065* | |
H17C | 1.0864 | 0.2930 | 0.5122 | 0.065* | |
N21 | 0.6542 (3) | 0.2550 (2) | 0.2098 (2) | 0.0203 (7) | |
C22 | 0.6979 (3) | 0.3483 (3) | 0.2449 (3) | 0.0228 (9) | |
C23 | 0.6447 (3) | 0.4326 (3) | 0.2285 (3) | 0.0285 (10) | |
H23A | 0.6758 | 0.4969 | 0.2545 | 0.034* | |
C24 | 0.5455 (4) | 0.4220 (3) | 0.1738 (3) | 0.0296 (10) | |
H24A | 0.5076 | 0.4790 | 0.1628 | 0.035* | |
C25 | 0.5020 (3) | 0.3268 (3) | 0.1350 (3) | 0.0274 (9) | |
C26 | 0.5584 (3) | 0.2462 (3) | 0.1561 (3) | 0.0251 (9) | |
H26A | 0.5281 | 0.1811 | 0.1314 | 0.030* | |
C27 | 0.3958 (4) | 0.3109 (4) | 0.0727 (3) | 0.0340 (11) | |
H27A | 0.3790 | 0.2394 | 0.0531 | 0.051* | |
H27B | 0.4100 | 0.3488 | 0.0195 | 0.051* | |
H27C | 0.3299 | 0.3342 | 0.1053 | 0.051* | |
N31 | 0.6223 (3) | 0.0359 (2) | 0.1921 (2) | 0.0220 (7) | |
C32 | 0.6533 (3) | 0.0091 (3) | 0.1066 (3) | 0.0235 (9) | |
C33 | 0.5886 (4) | −0.0673 (3) | 0.0517 (3) | 0.0309 (10) | |
H33A | 0.6114 | −0.0852 | −0.0083 | 0.037* | |
C34 | 0.4905 (4) | −0.1162 (3) | 0.0867 (3) | 0.0324 (10) | |
H34A | 0.4452 | −0.1676 | 0.0501 | 0.039* | |
C35 | 0.4581 (3) | −0.0911 (3) | 0.1743 (3) | 0.0292 (10) | |
C36 | 0.5264 (3) | −0.0125 (3) | 0.2239 (3) | 0.0271 (9) | |
H36A | 0.5035 | 0.0077 | 0.2835 | 0.033* | |
C37 | 0.3556 (4) | −0.1474 (4) | 0.2158 (4) | 0.0396 (12) | |
H37A | 0.3186 | −0.1990 | 0.1708 | 0.059* | |
H37B | 0.3002 | −0.1006 | 0.2349 | 0.059* | |
H37C | 0.3815 | −0.1792 | 0.2686 | 0.059* | |
N41 | 0.8186 (3) | 0.1266 (2) | 0.1448 (2) | 0.0224 (7) | |
C42 | 0.7622 (3) | 0.0618 (3) | 0.0783 (3) | 0.0231 (9) | |
C43 | 0.8088 (4) | 0.0459 (3) | −0.0066 (3) | 0.0297 (10) | |
H43A | 0.7667 | 0.0034 | −0.0529 | 0.036* | |
C44 | 0.9175 (4) | 0.0925 (3) | −0.0234 (3) | 0.0323 (10) | |
H44A | 0.9506 | 0.0815 | −0.0812 | 0.039* | |
C45 | 0.9777 (3) | 0.1556 (3) | 0.0449 (3) | 0.0271 (9) | |
C46 | 0.9247 (3) | 0.1711 (3) | 0.1274 (3) | 0.0230 (9) | |
H46A | 0.9647 | 0.2150 | 0.1739 | 0.028* | |
C47 | 1.0981 (4) | 0.2070 (4) | 0.0303 (3) | 0.0340 (11) | |
H47A | 1.1264 | 0.2469 | 0.0862 | 0.051* | |
H47B | 1.0951 | 0.2510 | −0.0190 | 0.051* | |
H47C | 1.1502 | 0.1563 | 0.0144 | 0.051* | |
N51 | 0.6401 (3) | 0.1492 (2) | 0.3694 (2) | 0.0223 (7) | |
C52 | 0.6762 (3) | 0.0941 (3) | 0.4354 (3) | 0.0247 (9) | |
C53 | 0.6256 (4) | 0.0938 (3) | 0.5196 (3) | 0.0306 (10) | |
H53A | 0.6533 | 0.0555 | 0.5647 | 0.037* | |
C54 | 0.5345 (4) | 0.1497 (4) | 0.5377 (3) | 0.0352 (11) | |
H54A | 0.4989 | 0.1490 | 0.5951 | 0.042* | |
C55 | 0.4946 (3) | 0.2070 (3) | 0.4720 (3) | 0.0271 (9) | |
C56 | 0.5510 (3) | 0.2039 (3) | 0.3887 (3) | 0.0243 (9) | |
H56A | 0.5252 | 0.2425 | 0.3430 | 0.029* | |
C57 | 0.3981 (4) | 0.2699 (4) | 0.4867 (3) | 0.0391 (12) | |
H57A | 0.3690 | 0.2639 | 0.5480 | 0.059* | |
H57B | 0.3359 | 0.2470 | 0.4421 | 0.059* | |
H57C | 0.4259 | 0.3401 | 0.4796 | 0.059* | |
N61 | 0.8039 (3) | 0.0436 (2) | 0.3202 (2) | 0.0219 (7) | |
C62 | 0.7698 (3) | 0.0341 (3) | 0.4067 (3) | 0.0229 (9) | |
C63 | 0.8187 (4) | −0.0284 (3) | 0.4623 (3) | 0.0328 (10) | |
H63A | 0.7947 | −0.0327 | 0.5230 | 0.039* | |
C64 | 0.9035 (4) | −0.0850 (4) | 0.4278 (4) | 0.0377 (11) | |
H64A | 0.9393 | −0.1270 | 0.4655 | 0.045* | |
C65 | 0.9357 (4) | −0.0800 (3) | 0.3381 (3) | 0.0311 (10) | |
C66 | 0.8842 (3) | −0.0134 (3) | 0.2873 (3) | 0.0267 (9) | |
H66A | 0.9070 | −0.0081 | 0.2264 | 0.032* | |
C67 | 1.02254 (19) | −0.14333 (17) | 0.29802 (17) | 0.0500 (14) | |
H67A | 1.0485 | −0.1850 | 0.3438 | 0.075* | |
H67B | 1.0886 | −0.1001 | 0.2778 | 0.075* | |
H67C | 0.9875 | −0.1865 | 0.2461 | 0.075* | |
N71 | 1.09456 (19) | −0.39381 (17) | 0.23883 (17) | 0.0402 (10) | |
C72 | 1.07515 (19) | −0.48679 (17) | 0.19626 (17) | 0.0308 (10) | |
C73 | 1.14403 (19) | −0.56191 (17) | 0.20998 (17) | 0.0360 (11) | |
H73A | 1.1265 | −0.6269 | 0.1796 | 0.043* | |
C74 | 1.2390 (4) | −0.5410 (4) | 0.2687 (4) | 0.0407 (12) | |
H74A | 1.2876 | −0.5915 | 0.2783 | 0.049* | |
C75 | 1.2625 (4) | −0.4463 (4) | 0.3130 (4) | 0.0405 (12) | |
C76 | 1.1873 (5) | −0.3770 (4) | 0.2967 (4) | 0.0498 (14) | |
H76A | 1.2017 | −0.3125 | 0.3285 | 0.060* | |
C77 | 1.3644 (5) | −0.4196 (5) | 0.3798 (5) | 0.0677 (19) | |
H77A | 1.3662 | −0.3495 | 0.4039 | 0.102* | |
H77B | 1.4363 | −0.4292 | 0.3485 | 0.102* | |
H77C | 1.3561 | −0.4631 | 0.4298 | 0.102* | |
N81 | 0.9518 (3) | −0.5978 (3) | 0.0893 (3) | 0.0365 (9) | |
C82 | 0.9701 (4) | −0.5062 (3) | 0.1337 (3) | 0.0312 (10) | |
C83 | 0.8965 (4) | −0.4336 (4) | 0.1231 (3) | 0.0375 (11) | |
H83A | 0.9118 | −0.3689 | 0.1545 | 0.045* | |
C84 | 0.8010 (4) | −0.4566 (4) | 0.0665 (3) | 0.0360 (11) | |
H84A | 0.7488 | −0.4081 | 0.0601 | 0.043* | |
C85 | 0.7802 (4) | −0.5505 (4) | 0.0184 (3) | 0.0327 (10) | |
C86 | 0.8593 (4) | −0.6179 (4) | 0.0339 (3) | 0.0399 (12) | |
H86A | 0.8465 | −0.6828 | 0.0028 | 0.048* | |
C87 | 0.6780 (4) | −0.5809 (4) | −0.0460 (4) | 0.0416 (12) | |
H87A | 0.6808 | −0.6499 | −0.0720 | 0.062* | |
H87B | 0.6806 | −0.5358 | −0.0948 | 0.062* | |
H87C | 0.6063 | −0.5766 | −0.0129 | 0.062* | |
Cl1 | 0.68163 (10) | −0.26625 (8) | 0.24199 (9) | 0.0368 (3) | |
O11 | 0.5830 (4) | −0.3282 (3) | 0.2013 (4) | 0.0729 (14) | |
O12 | 0.7531 (3) | −0.2278 (3) | 0.1723 (3) | 0.0574 (10) | |
O13 | 0.6447 (3) | −0.1838 (3) | 0.2977 (3) | 0.0472 (9) | |
O14 | 0.7471 (3) | −0.3244 (3) | 0.2961 (3) | 0.0503 (10) | |
Cl2 | 0.2480 (5) | 0.1252 (4) | 0.2634 (4) | 0.0473 (18) | 0.50 |
O21 | 0.2833 (8) | 0.2308 (4) | 0.2782 (6) | 0.076 (3) | 0.50 |
O22 | 0.2914 (9) | 0.0874 (8) | 0.1786 (6) | 0.084 (4) | 0.50 |
O23 | 0.1245 (5) | 0.1080 (8) | 0.2611 (8) | 0.137 (5) | 0.50 |
O24 | 0.2930 (10) | 0.0749 (7) | 0.3356 (6) | 0.043 (3) | 0.50 |
Cl3 | 0.2337 (4) | 0.1160 (3) | 0.2539 (3) | 0.0280 (12) | 0.50 |
O31 | 0.2066 (7) | 0.2161 (4) | 0.2772 (6) | 0.079 (4) | 0.50 |
O32 | 0.3256 (5) | 0.1182 (7) | 0.1906 (6) | 0.059 (3) | 0.50 |
O33 | 0.1338 (5) | 0.0562 (4) | 0.2137 (4) | 0.0450 (19) | 0.50 |
O34 | 0.2688 (8) | 0.0736 (7) | 0.3343 (5) | 0.072 (6) | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0169 (3) | 0.0200 (3) | 0.0260 (3) | 0.0083 (2) | 0.0033 (2) | −0.0021 (2) |
N11 | 0.0154 (15) | 0.0229 (18) | 0.0275 (19) | 0.0069 (13) | 0.0048 (13) | −0.0006 (14) |
C12 | 0.0189 (18) | 0.023 (2) | 0.028 (2) | 0.0068 (16) | 0.0067 (16) | −0.0029 (17) |
C13 | 0.027 (2) | 0.026 (2) | 0.031 (2) | 0.0083 (18) | 0.0035 (17) | −0.0002 (19) |
C14 | 0.025 (2) | 0.031 (2) | 0.033 (2) | 0.0039 (18) | 0.0032 (18) | −0.0022 (19) |
C15 | 0.020 (2) | 0.036 (3) | 0.034 (3) | 0.0063 (18) | −0.0020 (17) | 0.001 (2) |
C16 | 0.024 (2) | 0.029 (2) | 0.031 (2) | 0.0101 (18) | 0.0009 (17) | 0.0032 (19) |
C17 | 0.026 (2) | 0.047 (3) | 0.057 (3) | 0.003 (2) | −0.012 (2) | 0.004 (3) |
N21 | 0.0167 (15) | 0.0228 (18) | 0.0223 (18) | 0.0083 (13) | 0.0047 (13) | −0.0016 (14) |
C22 | 0.0210 (19) | 0.023 (2) | 0.025 (2) | 0.0078 (16) | 0.0044 (16) | −0.0024 (17) |
C23 | 0.023 (2) | 0.020 (2) | 0.042 (3) | 0.0068 (17) | 0.0005 (18) | −0.0029 (19) |
C24 | 0.027 (2) | 0.021 (2) | 0.042 (3) | 0.0114 (17) | 0.0010 (19) | 0.0025 (19) |
C25 | 0.0194 (19) | 0.024 (2) | 0.040 (3) | 0.0064 (17) | 0.0030 (17) | 0.0028 (19) |
C26 | 0.0203 (19) | 0.024 (2) | 0.031 (2) | 0.0078 (17) | 0.0027 (17) | 0.0001 (18) |
C27 | 0.024 (2) | 0.033 (3) | 0.047 (3) | 0.0124 (19) | −0.0065 (19) | 0.002 (2) |
N31 | 0.0221 (16) | 0.0174 (17) | 0.0274 (19) | 0.0077 (14) | 0.0036 (14) | −0.0021 (14) |
C32 | 0.0190 (18) | 0.021 (2) | 0.031 (2) | 0.0067 (16) | 0.0021 (16) | −0.0021 (17) |
C33 | 0.031 (2) | 0.029 (2) | 0.031 (2) | 0.0072 (19) | 0.0013 (18) | −0.0083 (19) |
C34 | 0.030 (2) | 0.027 (2) | 0.037 (3) | −0.0020 (19) | −0.0026 (19) | −0.009 (2) |
C35 | 0.024 (2) | 0.024 (2) | 0.039 (3) | 0.0060 (17) | 0.0016 (18) | −0.0023 (19) |
C36 | 0.025 (2) | 0.027 (2) | 0.030 (2) | 0.0068 (18) | 0.0032 (17) | −0.0009 (19) |
C37 | 0.029 (2) | 0.038 (3) | 0.049 (3) | −0.006 (2) | 0.006 (2) | −0.004 (2) |
N41 | 0.0213 (16) | 0.0166 (17) | 0.0298 (19) | 0.0063 (13) | 0.0022 (14) | −0.0005 (14) |
C42 | 0.0239 (19) | 0.019 (2) | 0.028 (2) | 0.0074 (16) | 0.0048 (16) | −0.0012 (17) |
C43 | 0.028 (2) | 0.032 (2) | 0.029 (2) | 0.0075 (19) | 0.0030 (18) | −0.0039 (19) |
C44 | 0.035 (2) | 0.034 (3) | 0.029 (2) | 0.012 (2) | 0.0115 (19) | −0.002 (2) |
C45 | 0.023 (2) | 0.027 (2) | 0.032 (2) | 0.0075 (17) | 0.0062 (17) | 0.0009 (19) |
C46 | 0.0181 (18) | 0.025 (2) | 0.027 (2) | 0.0076 (16) | 0.0045 (16) | −0.0005 (17) |
C47 | 0.024 (2) | 0.040 (3) | 0.039 (3) | 0.0082 (19) | 0.0118 (19) | 0.003 (2) |
N51 | 0.0186 (16) | 0.0197 (17) | 0.0286 (19) | 0.0073 (13) | 0.0038 (13) | −0.0045 (14) |
C52 | 0.025 (2) | 0.020 (2) | 0.029 (2) | 0.0053 (17) | 0.0031 (17) | −0.0013 (17) |
C53 | 0.034 (2) | 0.032 (2) | 0.028 (2) | 0.013 (2) | 0.0054 (18) | 0.0027 (19) |
C54 | 0.033 (2) | 0.041 (3) | 0.033 (3) | 0.014 (2) | 0.0136 (19) | −0.002 (2) |
C55 | 0.022 (2) | 0.027 (2) | 0.032 (2) | 0.0058 (17) | 0.0045 (17) | −0.0040 (19) |
C56 | 0.0211 (19) | 0.024 (2) | 0.028 (2) | 0.0103 (17) | 0.0039 (16) | −0.0023 (18) |
C57 | 0.031 (2) | 0.049 (3) | 0.040 (3) | 0.022 (2) | 0.009 (2) | −0.002 (2) |
N61 | 0.0191 (16) | 0.0189 (17) | 0.0275 (19) | 0.0053 (13) | 0.0021 (13) | −0.0044 (14) |
C62 | 0.025 (2) | 0.019 (2) | 0.025 (2) | 0.0064 (16) | 0.0037 (16) | −0.0023 (17) |
C63 | 0.035 (2) | 0.033 (3) | 0.033 (3) | 0.013 (2) | 0.0042 (19) | 0.004 (2) |
C64 | 0.034 (2) | 0.034 (3) | 0.049 (3) | 0.016 (2) | 0.002 (2) | 0.008 (2) |
C65 | 0.031 (2) | 0.025 (2) | 0.041 (3) | 0.0150 (19) | 0.0054 (19) | 0.002 (2) |
C66 | 0.025 (2) | 0.019 (2) | 0.037 (3) | 0.0091 (17) | 0.0070 (18) | −0.0012 (18) |
C67 | 0.048 (3) | 0.047 (3) | 0.062 (4) | 0.033 (3) | 0.012 (3) | 0.007 (3) |
N71 | 0.038 (2) | 0.028 (2) | 0.055 (3) | 0.0060 (18) | −0.0007 (19) | −0.0028 (19) |
C72 | 0.028 (2) | 0.028 (2) | 0.038 (3) | 0.0061 (18) | 0.0113 (19) | 0.004 (2) |
C73 | 0.033 (2) | 0.032 (3) | 0.044 (3) | 0.010 (2) | 0.002 (2) | −0.003 (2) |
C74 | 0.031 (2) | 0.043 (3) | 0.050 (3) | 0.011 (2) | 0.005 (2) | 0.003 (2) |
C75 | 0.034 (2) | 0.032 (3) | 0.055 (3) | 0.004 (2) | −0.005 (2) | 0.002 (2) |
C76 | 0.050 (3) | 0.028 (3) | 0.070 (4) | 0.003 (2) | −0.003 (3) | −0.002 (3) |
C77 | 0.054 (4) | 0.053 (4) | 0.093 (5) | 0.004 (3) | −0.022 (3) | −0.003 (3) |
N81 | 0.036 (2) | 0.031 (2) | 0.044 (2) | 0.0158 (17) | 0.0007 (18) | −0.0042 (18) |
C82 | 0.029 (2) | 0.030 (2) | 0.036 (3) | 0.0076 (19) | 0.0139 (19) | 0.004 (2) |
C83 | 0.035 (2) | 0.030 (3) | 0.048 (3) | 0.013 (2) | 0.009 (2) | 0.000 (2) |
C84 | 0.029 (2) | 0.032 (3) | 0.050 (3) | 0.016 (2) | 0.003 (2) | 0.007 (2) |
C85 | 0.028 (2) | 0.034 (3) | 0.037 (3) | 0.008 (2) | 0.0090 (19) | 0.006 (2) |
C86 | 0.045 (3) | 0.030 (3) | 0.045 (3) | 0.012 (2) | 0.000 (2) | −0.004 (2) |
C87 | 0.035 (2) | 0.039 (3) | 0.053 (3) | 0.009 (2) | 0.001 (2) | 0.010 (2) |
Cl1 | 0.0362 (6) | 0.0280 (6) | 0.0476 (7) | 0.0125 (5) | 0.0107 (5) | −0.0009 (5) |
O11 | 0.057 (2) | 0.045 (2) | 0.113 (4) | −0.003 (2) | −0.017 (3) | −0.001 (2) |
O12 | 0.064 (2) | 0.055 (2) | 0.057 (3) | 0.018 (2) | 0.028 (2) | 0.007 (2) |
O13 | 0.054 (2) | 0.037 (2) | 0.054 (2) | 0.0242 (17) | 0.0200 (17) | −0.0034 (17) |
O14 | 0.061 (2) | 0.043 (2) | 0.053 (2) | 0.0271 (18) | 0.0073 (18) | 0.0068 (18) |
Cl2 | 0.042 (3) | 0.047 (3) | 0.051 (3) | 0.016 (2) | −0.010 (2) | −0.013 (2) |
O21 | 0.134 (10) | 0.038 (5) | 0.060 (6) | 0.029 (6) | 0.010 (7) | 0.012 (4) |
O22 | 0.123 (8) | 0.080 (7) | 0.047 (6) | 0.040 (6) | −0.010 (6) | −0.035 (5) |
O23 | 0.073 (7) | 0.147 (9) | 0.196 (10) | 0.012 (7) | 0.000 (7) | 0.054 (8) |
O24 | 0.047 (5) | 0.045 (8) | 0.041 (8) | 0.026 (4) | 0.012 (4) | 0.010 (6) |
Cl3 | 0.0253 (17) | 0.0249 (19) | 0.036 (2) | 0.0088 (14) | 0.0041 (15) | 0.0068 (16) |
O31 | 0.105 (7) | 0.052 (5) | 0.081 (6) | 0.047 (5) | −0.029 (6) | −0.031 (4) |
O32 | 0.019 (3) | 0.109 (9) | 0.057 (6) | 0.006 (5) | 0.016 (4) | 0.044 (6) |
O33 | 0.048 (4) | 0.043 (4) | 0.039 (4) | −0.010 (4) | −0.012 (3) | −0.006 (3) |
O34 | 0.102 (11) | 0.074 (11) | 0.039 (9) | 0.001 (7) | −0.020 (7) | 0.018 (8) |
Geometric parameters (Å, º) top
Fe1—N51 | 1.972 (4) | C52—C62 | 1.474 (6) |
Fe1—N61 | 1.973 (3) | C53—C54 | 1.385 (6) |
Fe1—N21 | 1.983 (3) | C53—H53A | 0.9500 |
Fe1—N41 | 1.987 (4) | C54—C55 | 1.395 (6) |
Fe1—N11 | 1.991 (3) | C54—H54A | 0.9500 |
Fe1—N31 | 1.995 (3) | C55—C56 | 1.404 (6) |
N11—C12 | 1.355 (5) | C55—C57 | 1.489 (6) |
N11—C16 | 1.358 (5) | C56—H56A | 0.9500 |
C12—C13 | 1.397 (6) | C57—H57A | 0.9800 |
C12—C22 | 1.474 (5) | C57—H57B | 0.9800 |
C13—C14 | 1.387 (6) | C57—H57C | 0.9800 |
C13—H13A | 0.9500 | N61—C66 | 1.347 (5) |
C14—C15 | 1.377 (6) | N61—C62 | 1.358 (5) |
C14—H14A | 0.9500 | C62—C63 | 1.385 (6) |
C15—C16 | 1.401 (6) | C63—C64 | 1.390 (6) |
C15—C17 | 1.512 (6) | C63—H63A | 0.9500 |
C16—H16A | 0.9500 | C64—C65 | 1.389 (7) |
C17—H17A | 0.9800 | C64—H64A | 0.9500 |
C17—H17B | 0.9800 | C65—C66 | 1.394 (6) |
C17—H17C | 0.9800 | C65—C67 | 1.493 (5) |
N21—C26 | 1.351 (5) | C66—H66A | 0.9500 |
N21—C22 | 1.361 (5) | C67—H67A | 0.9800 |
C22—C23 | 1.388 (6) | C67—H67B | 0.9800 |
C23—C24 | 1.391 (6) | C67—H67C | 0.9800 |
C23—H23A | 0.9500 | N71—C72 | 1.349 (3) |
C24—C25 | 1.399 (6) | N71—C76 | 1.358 (6) |
C24—H24A | 0.9500 | C72—C73 | 1.384 (3) |
C25—C26 | 1.384 (6) | C72—C82 | 1.512 (5) |
C25—C27 | 1.519 (6) | C73—C74 | 1.387 (5) |
C26—H26A | 0.9500 | C73—H73A | 0.9500 |
C27—H27A | 0.9800 | C74—C75 | 1.383 (7) |
C27—H27B | 0.9800 | C74—H74A | 0.9500 |
C27—H27C | 0.9800 | C75—C76 | 1.382 (7) |
N31—C36 | 1.344 (5) | C75—C77 | 1.527 (7) |
N31—C32 | 1.352 (5) | C76—H76A | 0.9500 |
C32—C33 | 1.401 (6) | C77—H77A | 0.9800 |
C32—C42 | 1.470 (6) | C77—H77B | 0.9800 |
C33—C34 | 1.386 (6) | C77—H77C | 0.9800 |
C33—H33A | 0.9500 | N81—C86 | 1.335 (6) |
C34—C35 | 1.380 (6) | N81—C82 | 1.343 (6) |
C34—H34A | 0.9500 | C82—C83 | 1.387 (6) |
C35—C36 | 1.402 (6) | C83—C84 | 1.377 (7) |
C35—C37 | 1.511 (6) | C83—H83A | 0.9500 |
C36—H36A | 0.9500 | C84—C85 | 1.393 (7) |
C37—H37A | 0.9800 | C84—H84A | 0.9500 |
C37—H37B | 0.9800 | C85—C86 | 1.392 (6) |
C37—H37C | 0.9800 | C85—C87 | 1.515 (6) |
N41—C46 | 1.353 (5) | C86—H86A | 0.9500 |
N41—C42 | 1.369 (5) | C87—H87A | 0.9800 |
C42—C43 | 1.385 (6) | C87—H87B | 0.9800 |
C43—C44 | 1.388 (6) | C87—H87C | 0.9800 |
C43—H43A | 0.9500 | Cl1—O12 | 1.431 (4) |
C44—C45 | 1.393 (6) | Cl1—O14 | 1.433 (4) |
C44—H44A | 0.9500 | Cl1—O13 | 1.435 (3) |
C45—C46 | 1.387 (6) | Cl1—O11 | 1.439 (4) |
C45—C47 | 1.523 (6) | Cl2—O22 | 1.4339 |
C46—H46A | 0.9500 | Cl2—O23 | 1.4340 |
C47—H47A | 0.9800 | Cl2—O21 | 1.4340 |
C47—H47B | 0.9800 | Cl2—O24 | 1.4340 |
C47—H47C | 0.9800 | Cl3—O32 | 1.4339 |
N51—C56 | 1.360 (5) | Cl3—O31 | 1.4340 |
N51—C52 | 1.363 (5) | Cl3—O33 | 1.4340 |
C52—C53 | 1.385 (6) | Cl3—O34 | 1.4340 |
| | | |
N51—Fe1—N61 | 81.75 (14) | C56—N51—C52 | 117.5 (4) |
N51—Fe1—N21 | 92.40 (14) | C56—N51—Fe1 | 127.3 (3) |
N61—Fe1—N21 | 172.76 (14) | C52—N51—Fe1 | 115.1 (3) |
N51—Fe1—N41 | 174.93 (13) | N51—C52—C53 | 122.0 (4) |
N61—Fe1—N41 | 94.54 (14) | N51—C52—C62 | 113.3 (4) |
N21—Fe1—N41 | 91.55 (14) | C53—C52—C62 | 124.7 (4) |
N51—Fe1—N11 | 88.26 (14) | C52—C53—C54 | 119.7 (4) |
N61—Fe1—N11 | 94.09 (13) | C52—C53—H53A | 120.2 |
N21—Fe1—N11 | 81.42 (13) | C54—C53—H53A | 120.2 |
N41—Fe1—N11 | 95.48 (14) | C53—C54—C55 | 120.2 (4) |
N51—Fe1—N31 | 94.61 (14) | C53—C54—H54A | 119.9 |
N61—Fe1—N31 | 90.17 (13) | C55—C54—H54A | 119.9 |
N21—Fe1—N31 | 94.56 (13) | C54—C55—C56 | 116.7 (4) |
N41—Fe1—N31 | 81.90 (14) | C54—C55—C57 | 123.4 (4) |
N11—Fe1—N31 | 175.17 (14) | C56—C55—C57 | 119.9 (4) |
C12—N11—C16 | 117.2 (4) | N51—C56—C55 | 124.0 (4) |
C12—N11—Fe1 | 114.9 (3) | N51—C56—H56A | 118.0 |
C16—N11—Fe1 | 127.8 (3) | C55—C56—H56A | 118.0 |
N11—C12—C13 | 122.4 (4) | C55—C57—H57A | 109.5 |
N11—C12—C22 | 113.9 (3) | C55—C57—H57B | 109.5 |
C13—C12—C22 | 123.7 (4) | H57A—C57—H57B | 109.5 |
C14—C13—C12 | 118.7 (4) | C55—C57—H57C | 109.5 |
C14—C13—H13A | 120.7 | H57A—C57—H57C | 109.5 |
C12—C13—H13A | 120.7 | H57B—C57—H57C | 109.5 |
C15—C14—C13 | 120.7 (4) | C66—N61—C62 | 118.1 (4) |
C15—C14—H14A | 119.7 | C66—N61—Fe1 | 127.4 (3) |
C13—C14—H14A | 119.7 | C62—N61—Fe1 | 114.5 (3) |
C14—C15—C16 | 117.1 (4) | N61—C62—C63 | 122.0 (4) |
C14—C15—C17 | 121.9 (4) | N61—C62—C52 | 114.7 (3) |
C16—C15—C17 | 121.0 (4) | C63—C62—C52 | 123.3 (4) |
N11—C16—C15 | 124.0 (4) | C62—C63—C64 | 119.1 (4) |
N11—C16—H16A | 118.0 | C62—C63—H63A | 120.5 |
C15—C16—H16A | 118.0 | C64—C63—H63A | 120.5 |
C15—C17—H17A | 109.5 | C65—C64—C63 | 119.8 (4) |
C15—C17—H17B | 109.5 | C65—C64—H64A | 120.1 |
H17A—C17—H17B | 109.5 | C63—C64—H64A | 120.1 |
C15—C17—H17C | 109.5 | C64—C65—C66 | 117.5 (4) |
H17A—C17—H17C | 109.5 | C64—C65—C67 | 121.1 (4) |
H17B—C17—H17C | 109.5 | C66—C65—C67 | 121.4 (4) |
C26—N21—C22 | 118.1 (3) | N61—C66—C65 | 123.4 (4) |
C26—N21—Fe1 | 127.0 (3) | N61—C66—H66A | 118.3 |
C22—N21—Fe1 | 114.4 (2) | C65—C66—H66A | 118.3 |
N21—C22—C23 | 121.6 (4) | C65—C67—H67A | 109.5 |
N21—C22—C12 | 114.7 (3) | C65—C67—H67B | 109.5 |
C23—C22—C12 | 123.7 (4) | H67A—C67—H67B | 109.5 |
C22—C23—C24 | 119.5 (4) | C65—C67—H67C | 109.5 |
C22—C23—H23A | 120.3 | H67A—C67—H67C | 109.5 |
C24—C23—H23A | 120.3 | H67B—C67—H67C | 109.5 |
C23—C24—C25 | 119.4 (4) | C72—N71—C76 | 115.9 (2) |
C23—C24—H24A | 120.3 | N71—C72—C73 | 123.0 (2) |
C25—C24—H24A | 120.3 | N71—C72—C82 | 115.89 (19) |
C26—C25—C24 | 117.7 (4) | C73—C72—C82 | 121.07 (19) |
C26—C25—C27 | 120.4 (4) | C72—C73—C74 | 119.1 (2) |
C24—C25—C27 | 121.9 (4) | C72—C73—H73A | 120.4 |
N21—C26—C25 | 123.7 (4) | C74—C73—H73A | 120.4 |
N21—C26—H26A | 118.2 | C75—C74—C73 | 119.6 (4) |
C25—C26—H26A | 118.2 | C75—C74—H74A | 120.2 |
C25—C27—H27A | 109.5 | C73—C74—H74A | 120.2 |
C25—C27—H27B | 109.5 | C76—C75—C74 | 117.0 (4) |
H27A—C27—H27B | 109.5 | C76—C75—C77 | 121.0 (5) |
C25—C27—H27C | 109.5 | C74—C75—C77 | 121.9 (5) |
H27A—C27—H27C | 109.5 | N71—C76—C75 | 125.2 (5) |
H27B—C27—H27C | 109.5 | N71—C76—H76A | 117.4 |
C36—N31—C32 | 118.3 (3) | C75—C76—H76A | 117.4 |
C36—N31—Fe1 | 127.5 (3) | C75—C77—H77A | 109.5 |
C32—N31—Fe1 | 114.2 (3) | C75—C77—H77B | 109.5 |
N31—C32—C33 | 121.6 (4) | H77A—C77—H77B | 109.5 |
N31—C32—C42 | 115.1 (3) | C75—C77—H77C | 109.5 |
C33—C32—C42 | 123.2 (4) | H77A—C77—H77C | 109.5 |
C34—C33—C32 | 118.6 (4) | H77B—C77—H77C | 109.5 |
C34—C33—H33A | 120.7 | C86—N81—C82 | 117.9 (4) |
C32—C33—H33A | 120.7 | N81—C82—C83 | 121.9 (4) |
C35—C34—C33 | 120.7 (4) | N81—C82—C72 | 116.3 (4) |
C35—C34—H34A | 119.6 | C83—C82—C72 | 121.8 (4) |
C33—C34—H34A | 119.6 | C84—C83—C82 | 119.0 (5) |
C34—C35—C36 | 117.0 (4) | C84—C83—H83A | 120.5 |
C34—C35—C37 | 121.7 (4) | C82—C83—H83A | 120.5 |
C36—C35—C37 | 121.4 (4) | C83—C84—C85 | 120.6 (4) |
N31—C36—C35 | 123.7 (4) | C83—C84—H84A | 119.7 |
N31—C36—H36A | 118.2 | C85—C84—H84A | 119.7 |
C35—C36—H36A | 118.2 | C86—C85—C84 | 115.8 (4) |
C35—C37—H37A | 109.5 | C86—C85—C87 | 120.6 (4) |
C35—C37—H37B | 109.5 | C84—C85—C87 | 123.6 (4) |
H37A—C37—H37B | 109.5 | N81—C86—C85 | 124.8 (4) |
C35—C37—H37C | 109.5 | N81—C86—H86A | 117.6 |
H37A—C37—H37C | 109.5 | C85—C86—H86A | 117.6 |
H37B—C37—H37C | 109.5 | C85—C87—H87A | 109.5 |
C46—N41—C42 | 118.3 (4) | C85—C87—H87B | 109.5 |
C46—N41—Fe1 | 127.7 (3) | H87A—C87—H87B | 109.5 |
C42—N41—Fe1 | 114.0 (3) | C85—C87—H87C | 109.5 |
N41—C42—C43 | 121.4 (4) | H87A—C87—H87C | 109.5 |
N41—C42—C32 | 114.4 (4) | H87B—C87—H87C | 109.5 |
C43—C42—C32 | 124.2 (4) | O12—Cl1—O14 | 108.9 (2) |
C42—C43—C44 | 119.5 (4) | O12—Cl1—O13 | 109.0 (2) |
C42—C43—H43A | 120.3 | O14—Cl1—O13 | 109.7 (2) |
C44—C43—H43A | 120.3 | O12—Cl1—O11 | 109.5 (3) |
C43—C44—C45 | 119.7 (4) | O14—Cl1—O11 | 109.8 (2) |
C43—C44—H44A | 120.2 | O13—Cl1—O11 | 109.9 (2) |
C45—C44—H44A | 120.2 | O22—Cl2—O23 | 109.5 |
C46—C45—C44 | 118.0 (4) | O22—Cl2—O21 | 109.4 |
C46—C45—C47 | 120.3 (4) | O23—Cl2—O21 | 109.4 |
C44—C45—C47 | 121.7 (4) | O22—Cl2—O24 | 109.5 |
N41—C46—C45 | 123.0 (4) | O23—Cl2—O24 | 109.5 |
N41—C46—H46A | 118.5 | O21—Cl2—O24 | 109.4 |
C45—C46—H46A | 118.5 | O32—Cl3—O31 | 109.4 |
C45—C47—H47A | 109.5 | O32—Cl3—O33 | 109.5 |
C45—C47—H47B | 109.5 | O31—Cl3—O33 | 109.4 |
H47A—C47—H47B | 109.5 | O32—Cl3—O34 | 109.5 |
C45—C47—H47C | 109.5 | O31—Cl3—O34 | 109.4 |
H47A—C47—H47C | 109.5 | O33—Cl3—O34 | 109.5 |
H47B—C47—H47C | 109.5 | | |
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