The title compound (systematic name: μ-oxo-bis{[4,15-bis(ethoxycarbonyl)-5,14-dimethyl-2,7,13,17-tetraazatricyclo[16.4.0.07,12]docosa-3,5,7,9,11,13,15,18(1),19,21-decaene-2,17-diido]iron(III)} sesquihydrate), [Fe2(C26H26N4O4)O]·1.5H2O, crystallizes in the monoclinic space group C2/c and has two iron centres which are coordinated by macrocyclic ligands with an N4 donor set. These iron centres are bridged by a μ-oxo ligand, resulting in the formation of a dinuclear complex unit. The μ-oxo ligand interacts with a water molecule via strong hydrogen bonds. These solvent molecules aggregate by additional hydrogen bonds, producing a tetranuclear aggregate. Towards the outer rim of the cavity formed by the carboxyethyl substituents attached to the tetraaza-annulene systems there are additional solvent molecules. Due to much weaker hydrogen-bond interactions, the latter are disordered and have site-occupancy factors less than 1.
Supporting information
CCDC reference: 601793
Key indicators
- Single-crystal X-ray study
- T = 213 K
- Mean (C-C) = 0.006 Å
- Disorder in main residue
- R factor = 0.047
- wR factor = 0.131
- Data-to-parameter ratio = 13.2
checkCIF/PLATON results
No syntax errors found
Datablock: I
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.72 Ratio
| Author Response: All atoms are correctly assigned, the composition of the compound is
clear from other analytical data. The reason for this problem are disordered
methyl groups which nevertheless could not be resolved.
|
PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.17 Ratio
| Author Response: All atoms are correctly assigned, the composition of the compound is
clear from other analytical data. The reason for this problem are disordered
methyl groups which nevertheless could not be resolved.
|
PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C17
| Author Response: The methyl group C18 is disordered. Unfortunately this disorder could
not be resolved.
|
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O10
| Author Response: This is indeed one of the solvate water molecules. H-atoms could not
be resolved from Difference Fourier Analysis.
|
PLAT430_ALERT_2_A Short Inter D...A Contact O11X .. O11X .. 2.45 Ang.
| Author Response: This is caused by the highly disordered water molecule O11 which is
only weakly bound and in addition to being disordered thus shows an site
occupation factor below 1.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C32X .. C32X .. 2.75 Ang.
| Author Response: This effect again is due to disorder of the ethyl group which
unfortunately could not be resolved.
|
Alert level B
PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............ 24.98 Deg.
| Author Response: Since the criterion for MoKa is 25.24 deg and the data parameter
ratio for I looks alright, I hope this is not a real problem.
|
PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 4
| Author Response: Again this is due to the disorder of some of the ethyl substituents
which could not be resolved.
|
PLAT430_ALERT_2_B Short Inter D...A Contact O10 .. O11 .. 2.65 Ang.
| Author Response: This is caused by the highly disordered water molecule O11 which is
only weakly bound and in addition to being disordered thus shows an site
occupation factor below 1.
|
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.01 Ratio
| Author Response: All atoms are correctly assigned, the composition of the compound is
clear from other analytical data. The reason for this problem are disordered
methyl groups which nevertheless could not be resolved.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C17X
| Author Response: The methyl group C18 is disordered. Unfortunately this disorder could
not be resolved.
|
PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 17.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O11
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O11X
PLAT430_ALERT_2_C Short Inter D...A Contact O1 .. O10 .. 2.89 Ang.
| Author Response: This is caused by the highly disordered water molecule O11 which is
only weakly bound and in addition to being disordered thus shows an site
occupation factor below 1.
|
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 31.00 A 3
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 27.30 Deg.
C6X -C5 -C6 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 41.23 Deg.
N2 -C8 -FE1 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 41.47 Deg.
N3 -C13 -FE1 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 30.40 Deg.
C17 -O4 -C17X 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 41.38 Deg.
N6 -C34 -FE2 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 41.09 Deg.
N7 -C39 -FE2 1.555 1.555 1.555
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
O
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C52 H52 Fe2 N8 O10.5
Atom count from _chemical_formula_moiety:C52 H55 Fe2 N8 O10.5
6 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
20 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
20 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: SET4 (Boer et al., 1984); data reduction: MolEN (Nonius, 1990); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1990); software used to prepare material for publication: XP.
µ-oxo-bis{[4,15-bis(ethoxycarbonyl)-5,14-dimethyl-2,7,13,17-
tetraazatricyclo[16.4.0.0
7,12]docosa-3,5,7,9,11,13,15,18 (1),19,21-decaene-
2,17-diido]iron(III)} sesquihydrate
top
Crystal data top
[Fe2(C26H26N4O4)O]·1.5H2O | F(000) = 4448 |
Mr = 1071.72 | Dx = 1.385 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 25 reflections |
a = 27.322 (6) Å | θ = 20.1–27.8° |
b = 13.494 (4) Å | µ = 0.63 mm−1 |
c = 29.838 (5) Å | T = 213 K |
β = 111.26 (2)° | Cube, red |
V = 10252 (4) Å3 | 0.6 × 0.4 × 0.3 mm |
Z = 8 | |
Data collection top
Enraf–Nonius CAD-4 diffractometer | 6718 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.024 |
Graphite monochromator | θmax = 25.0°, θmin = 2.5° |
ω/2θ scans | h = 0→32 |
Absorption correction: ψ scan (North et al., 1968) | k = −16→0 |
Tmin = 0.776, Tmax = 0.830 | l = −35→33 |
9161 measured reflections | 3 standard reflections every 600 min |
8963 independent reflections | intensity decay: 3.6% |
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)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0507P)2 + 35.0302P] where P = (Fo2 + 2Fc2)/3 |
8963 reflections | (Δ/σ)max = 0.004 |
681 parameters | Δρmax = 0.74 e Å−3 |
0 restraints | Δρmin = −0.52 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 | 0.455878 (18) | 0.11981 (4) | 0.363464 (18) | 0.02613 (14) | |
Fe2 | 0.345151 (18) | 0.04404 (4) | 0.282503 (17) | 0.02348 (13) | |
O1 | 0.40880 (9) | 0.10002 (18) | 0.30446 (8) | 0.0287 (5) | |
N1 | 0.47942 (11) | −0.0180 (2) | 0.39148 (10) | 0.0299 (7) | |
C1 | 0.47211 (14) | −0.0668 (3) | 0.42675 (12) | 0.0320 (8) | |
C2 | 0.50456 (16) | −0.1576 (3) | 0.44782 (15) | 0.0418 (10) | |
H2A | 0.4858 | −0.2158 | 0.4323 | 0.050 (5)* | |
H2B | 0.5112 | −0.1609 | 0.4817 | 0.050 (5)* | |
H2C | 0.5373 | −0.1539 | 0.4429 | 0.050 (5)* | |
C3 | 0.43734 (14) | −0.0282 (3) | 0.44852 (12) | 0.0317 (8) | |
C4 | 0.42105 (16) | −0.0860 (3) | 0.48288 (14) | 0.0393 (9) | |
O2 | 0.40931 (14) | −0.0512 (2) | 0.51489 (11) | 0.0558 (8) | |
O3 | 0.41855 (12) | −0.1836 (2) | 0.47378 (10) | 0.0491 (8) | |
C5 | 0.4070 (2) | −0.2457 (4) | 0.50843 (19) | 0.0659 (15) | |
H5A | 0.3696 | −0.2462 | 0.5021 | 0.15 (2)* | |
H5B | 0.4253 | −0.2217 | 0.5409 | 0.15 (2)* | |
C6 | 0.4269 (8) | −0.3538 (9) | 0.5018 (5) | 0.060 (5)* | 0.46 (3) |
H6A | 0.4205 | −0.3985 | 0.5241 | 0.063 (12)* | 0.46 (3) |
H6B | 0.4639 | −0.3517 | 0.5077 | 0.063 (12)* | 0.46 (3) |
H6C | 0.4083 | −0.3763 | 0.4696 | 0.063 (12)* | 0.46 (3) |
C6X | 0.3989 (8) | −0.3424 (8) | 0.4914 (4) | 0.066 (4)* | 0.54 (3) |
H6D | 0.3681 | −0.3450 | 0.4625 | 0.063 (12)* | 0.54 (3) |
H6E | 0.3941 | −0.3848 | 0.5153 | 0.063 (12)* | 0.54 (3) |
H6F | 0.4288 | −0.3643 | 0.4845 | 0.063 (12)* | 0.54 (3) |
C7 | 0.41673 (13) | 0.0674 (3) | 0.44219 (13) | 0.0320 (8) | |
H7 | 0.3970 | 0.0845 | 0.4607 | 0.035 (7)* | |
N2 | 0.42203 (11) | 0.1358 (2) | 0.41314 (10) | 0.0298 (7) | |
C8 | 0.40418 (14) | 0.2339 (3) | 0.41391 (13) | 0.0323 (8) | |
C9 | 0.36520 (15) | 0.2631 (3) | 0.43082 (14) | 0.0413 (10) | |
H9 | 0.3481 | 0.2163 | 0.4428 | 0.044 (4)* | |
C10 | 0.35202 (17) | 0.3624 (3) | 0.42971 (16) | 0.0495 (11) | |
H10 | 0.3269 | 0.3828 | 0.4420 | 0.044 (4)* | |
C11 | 0.37628 (17) | 0.4312 (3) | 0.41032 (17) | 0.0515 (12) | |
H11 | 0.3669 | 0.4976 | 0.4093 | 0.044 (4)* | |
C12 | 0.41401 (16) | 0.4029 (3) | 0.39252 (16) | 0.0450 (10) | |
H12 | 0.4296 | 0.4498 | 0.3791 | 0.044 (4)* | |
C13 | 0.42877 (14) | 0.3046 (3) | 0.39460 (14) | 0.0344 (8) | |
N3 | 0.46826 (11) | 0.2654 (2) | 0.37936 (11) | 0.0310 (7) | |
C14 | 0.50674 (14) | 0.3208 (3) | 0.37633 (13) | 0.0339 (8) | |
H14 | 0.5040 | 0.3887 | 0.3802 | 0.035 (7)* | |
C15 | 0.55094 (14) | 0.2887 (3) | 0.36793 (13) | 0.0337 (8) | |
C16 | 0.58724 (18) | 0.3652 (3) | 0.36345 (18) | 0.0528 (12) | |
O4 | 0.57978 (16) | 0.4520 (3) | 0.38086 (18) | 0.0863 (13) | |
O5 | 0.62041 (15) | 0.3554 (3) | 0.34659 (17) | 0.0843 (13) | |
C17 | 0.6168 (7) | 0.5338 (13) | 0.3897 (7) | 0.064 (4)* | 0.33 |
H17A | 0.6519 | 0.5063 | 0.3989 | 0.055 (13)* | 0.33 |
H17B | 0.6096 | 0.5693 | 0.3598 | 0.055 (13)* | 0.33 |
C18 | 0.6166 (18) | 0.600 (3) | 0.4239 (14) | 0.20 (2)* | 0.33 |
H18A | 0.5818 | 0.6259 | 0.4162 | 0.15 (3)* | 0.33 |
H18B | 0.6403 | 0.6535 | 0.4249 | 0.15 (3)* | 0.33 |
H18C | 0.6277 | 0.5679 | 0.4547 | 0.15 (3)* | 0.33 |
C17X | 0.6038 (4) | 0.5365 (7) | 0.3616 (4) | 0.085 (3)* | 0.67 |
H17C | 0.6405 | 0.5235 | 0.3672 | 0.055 (13)* | 0.67 |
H17D | 0.5850 | 0.5460 | 0.3274 | 0.055 (13)* | 0.67 |
C18X | 0.5987 (7) | 0.6169 (12) | 0.3870 (6) | 0.142 (5)* | 0.67 |
H18D | 0.5621 | 0.6320 | 0.3786 | 0.15 (3)* | 0.67 |
H18E | 0.6162 | 0.6726 | 0.3795 | 0.15 (3)* | 0.67 |
H18F | 0.6141 | 0.6029 | 0.4208 | 0.15 (3)* | 0.67 |
C19 | 0.56351 (14) | 0.1871 (3) | 0.36384 (13) | 0.0325 (8) | |
C20 | 0.61972 (15) | 0.1584 (3) | 0.37214 (16) | 0.0475 (11) | |
H20A | 0.6432 | 0.2019 | 0.3956 | 0.050 (5)* | |
H20B | 0.6258 | 0.1637 | 0.3425 | 0.050 (5)* | |
H20C | 0.6258 | 0.0913 | 0.3836 | 0.050 (5)* | |
N4 | 0.52804 (11) | 0.1178 (2) | 0.35791 (10) | 0.0294 (7) | |
C21 | 0.53450 (13) | 0.0183 (3) | 0.34651 (13) | 0.0328 (8) | |
C22 | 0.55615 (15) | −0.0084 (3) | 0.31257 (15) | 0.0418 (10) | |
H22 | 0.5725 | 0.0393 | 0.3003 | 0.044 (4)* | |
C23 | 0.55339 (16) | −0.1051 (3) | 0.29719 (17) | 0.0512 (12) | |
H23 | 0.5682 | −0.1228 | 0.2748 | 0.044 (4)* | |
C24 | 0.52890 (16) | −0.1755 (3) | 0.31477 (17) | 0.0497 (11) | |
H24 | 0.5277 | −0.2408 | 0.3045 | 0.044 (4)* | |
C25 | 0.50607 (15) | −0.1505 (3) | 0.34748 (15) | 0.0399 (9) | |
H25 | 0.4887 | −0.1985 | 0.3585 | 0.044 (4)* | |
C26 | 0.50887 (13) | −0.0540 (3) | 0.36408 (13) | 0.0317 (8) | |
N5 | 0.29887 (11) | 0.1301 (2) | 0.30736 (10) | 0.0280 (6) | |
C27 | 0.27784 (13) | 0.1125 (3) | 0.34000 (12) | 0.0292 (8) | |
C28 | 0.23440 (15) | 0.1776 (3) | 0.34246 (15) | 0.0418 (10) | |
H28A | 0.2484 | 0.2248 | 0.3680 | 0.051 (5)* | |
H28B | 0.2084 | 0.1376 | 0.3485 | 0.051 (5)* | |
H28C | 0.2186 | 0.2120 | 0.3125 | 0.051 (5)* | |
C29 | 0.29145 (13) | 0.0259 (3) | 0.36951 (12) | 0.0277 (8) | |
C30 | 0.27606 (14) | 0.0208 (3) | 0.41182 (13) | 0.0345 (9) | |
O6 | 0.26572 (13) | 0.0907 (2) | 0.43203 (10) | 0.0530 (8) | |
O7 | 0.27648 (13) | −0.0720 (2) | 0.42814 (10) | 0.0481 (7) | |
C31 | 0.2684 (2) | −0.0826 (4) | 0.47340 (16) | 0.0542 (12) | |
H31A | 0.2829 | −0.0254 | 0.4935 | 0.080 (9)* | |
H31B | 0.2870 | −0.1410 | 0.4901 | 0.080 (9)* | |
C32 | 0.2125 (4) | −0.0918 (9) | 0.4660 (4) | 0.071 (4)* | 0.539 (14) |
H32A | 0.1976 | −0.1459 | 0.4445 | 0.092 (14)* | 0.539 (14) |
H32B | 0.1947 | −0.0315 | 0.4524 | 0.092 (14)* | 0.539 (14) |
H32C | 0.2088 | −0.1040 | 0.4963 | 0.092 (14)* | 0.539 (14) |
C32X | 0.2382 (6) | −0.1653 (12) | 0.4724 (5) | 0.087 (5)* | 0.461 (14) |
H32D | 0.2354 | −0.1742 | 0.5033 | 0.092 (14)* | 0.461 (14) |
H32E | 0.2543 | −0.2227 | 0.4647 | 0.092 (14)* | 0.461 (14) |
H32F | 0.2037 | −0.1565 | 0.4485 | 0.092 (14)* | 0.461 (14) |
C33 | 0.31809 (13) | −0.0560 (3) | 0.36091 (12) | 0.0286 (8) | |
H33 | 0.3215 | −0.1108 | 0.3807 | 0.029 (7)* | |
N6 | 0.33886 (10) | −0.0633 (2) | 0.32762 (9) | 0.0245 (6) | |
C34 | 0.35855 (13) | −0.1543 (3) | 0.31836 (12) | 0.0259 (7) | |
C35 | 0.37697 (14) | −0.2313 (3) | 0.35113 (13) | 0.0315 (8) | |
H35 | 0.3775 | −0.2248 | 0.3823 | 0.038 (4)* | |
C36 | 0.39440 (15) | −0.3174 (3) | 0.33706 (14) | 0.0360 (9) | |
H36 | 0.4061 | −0.3693 | 0.3588 | 0.038 (4)* | |
C37 | 0.39470 (15) | −0.3277 (3) | 0.29101 (14) | 0.0367 (9) | |
H37 | 0.4062 | −0.3864 | 0.2819 | 0.038 (4)* | |
C38 | 0.37778 (14) | −0.2504 (3) | 0.25874 (13) | 0.0310 (8) | |
H38 | 0.3787 | −0.2567 | 0.2280 | 0.038 (4)* | |
C39 | 0.35946 (13) | −0.1634 (3) | 0.27180 (12) | 0.0261 (7) | |
N7 | 0.34043 (10) | −0.0792 (2) | 0.24262 (10) | 0.0249 (6) | |
C40 | 0.32261 (13) | −0.0847 (3) | 0.19529 (12) | 0.0262 (7) | |
H40 | 0.3279 | −0.1447 | 0.1823 | 0.029 (7)* | |
C41 | 0.29677 (13) | −0.0110 (3) | 0.16235 (12) | 0.0265 (7) | |
C42 | 0.28416 (14) | −0.0345 (3) | 0.11098 (12) | 0.0311 (8) | |
O8 | 0.26757 (12) | 0.0217 (2) | 0.07774 (9) | 0.0477 (7) | |
O9 | 0.29414 (12) | −0.1307 (2) | 0.10434 (9) | 0.0422 (7) | |
C43 | 0.29166 (18) | −0.1593 (3) | 0.05698 (14) | 0.0466 (11) | |
H43A | 0.2644 | −0.1216 | 0.0329 | 0.080 (9)* | |
H43B | 0.2828 | −0.2291 | 0.0518 | 0.080 (9)* | |
C44 | 0.3433 (2) | −0.1409 (4) | 0.05182 (18) | 0.0657 (14) | |
H44A | 0.3503 | −0.0710 | 0.0536 | 0.109 (13)* | |
H44B | 0.3422 | −0.1657 | 0.0213 | 0.109 (13)* | |
H44C | 0.3706 | −0.1742 | 0.0772 | 0.109 (13)* | |
C45 | 0.28257 (13) | 0.0840 (3) | 0.17507 (12) | 0.0282 (8) | |
C46 | 0.24108 (15) | 0.1450 (3) | 0.13775 (13) | 0.0384 (9) | |
H46A | 0.2144 | 0.1019 | 0.1172 | 0.051 (5)* | |
H46B | 0.2569 | 0.1813 | 0.1189 | 0.051 (5)* | |
H46C | 0.2256 | 0.1905 | 0.1535 | 0.051 (5)* | |
N8 | 0.30255 (11) | 0.1152 (2) | 0.22006 (10) | 0.0263 (6) | |
C47 | 0.29520 (13) | 0.2122 (3) | 0.23481 (13) | 0.0299 (8) | |
C48 | 0.29926 (14) | 0.2980 (3) | 0.21042 (14) | 0.0346 (8) | |
H48 | 0.3020 | 0.2935 | 0.1803 | 0.038 (4)* | |
C49 | 0.29919 (15) | 0.3895 (3) | 0.23075 (15) | 0.0403 (9) | |
H49 | 0.3013 | 0.4465 | 0.2140 | 0.038 (4)* | |
C50 | 0.29606 (16) | 0.3974 (3) | 0.27569 (16) | 0.0435 (10) | |
H50 | 0.2953 | 0.4596 | 0.2889 | 0.038 (4)* | |
C51 | 0.29405 (15) | 0.3134 (3) | 0.30102 (14) | 0.0370 (9) | |
H51 | 0.2933 | 0.3193 | 0.3318 | 0.038 (4)* | |
C52 | 0.29306 (13) | 0.2198 (3) | 0.28127 (12) | 0.0284 (8) | |
O10 | 0.44529 (18) | 0.2355 (4) | 0.24846 (15) | 0.1080 (17) | |
O11 | 0.4385 (7) | −0.5757 (12) | 0.2695 (6) | 0.096 (5)* | 0.30 |
O11X | 0.4666 (8) | −0.5359 (16) | 0.2685 (7) | 0.078 (5)* | 0.20 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0197 (2) | 0.0288 (3) | 0.0291 (3) | −0.0002 (2) | 0.0080 (2) | −0.0037 (2) |
Fe2 | 0.0200 (2) | 0.0271 (3) | 0.0226 (2) | 0.0013 (2) | 0.00675 (19) | 0.0003 (2) |
O1 | 0.0220 (12) | 0.0342 (14) | 0.0286 (12) | −0.0030 (10) | 0.0079 (10) | −0.0022 (11) |
N1 | 0.0233 (15) | 0.0332 (17) | 0.0319 (16) | 0.0000 (13) | 0.0084 (13) | −0.0027 (13) |
C1 | 0.0252 (18) | 0.035 (2) | 0.0267 (18) | −0.0034 (16) | −0.0012 (15) | −0.0046 (16) |
C2 | 0.035 (2) | 0.037 (2) | 0.044 (2) | 0.0038 (18) | 0.0024 (18) | 0.0026 (18) |
C3 | 0.0258 (18) | 0.040 (2) | 0.0255 (18) | −0.0029 (16) | 0.0044 (15) | 0.0032 (16) |
C4 | 0.037 (2) | 0.046 (2) | 0.029 (2) | −0.0017 (19) | 0.0049 (17) | 0.0036 (18) |
O2 | 0.075 (2) | 0.060 (2) | 0.0438 (17) | −0.0021 (17) | 0.0357 (17) | −0.0012 (15) |
O3 | 0.069 (2) | 0.0469 (18) | 0.0321 (15) | −0.0167 (15) | 0.0188 (14) | 0.0007 (13) |
C5 | 0.089 (4) | 0.056 (3) | 0.058 (3) | −0.009 (3) | 0.033 (3) | 0.020 (3) |
C7 | 0.0203 (17) | 0.042 (2) | 0.0300 (19) | −0.0020 (16) | 0.0044 (15) | −0.0054 (17) |
N2 | 0.0272 (16) | 0.0299 (17) | 0.0316 (16) | 0.0008 (13) | 0.0098 (13) | −0.0019 (13) |
C8 | 0.0256 (18) | 0.038 (2) | 0.0295 (19) | 0.0024 (16) | 0.0056 (15) | −0.0093 (16) |
C9 | 0.032 (2) | 0.051 (3) | 0.041 (2) | 0.0042 (19) | 0.0141 (18) | −0.0090 (19) |
C10 | 0.038 (2) | 0.059 (3) | 0.053 (3) | 0.013 (2) | 0.017 (2) | −0.017 (2) |
C11 | 0.041 (2) | 0.039 (2) | 0.072 (3) | 0.005 (2) | 0.017 (2) | −0.016 (2) |
C12 | 0.038 (2) | 0.032 (2) | 0.064 (3) | 0.0031 (18) | 0.019 (2) | −0.009 (2) |
C13 | 0.0274 (19) | 0.036 (2) | 0.039 (2) | −0.0003 (16) | 0.0105 (16) | −0.0082 (17) |
N3 | 0.0246 (15) | 0.0328 (17) | 0.0349 (16) | 0.0008 (13) | 0.0098 (13) | −0.0043 (13) |
C14 | 0.035 (2) | 0.027 (2) | 0.037 (2) | −0.0012 (16) | 0.0106 (17) | 0.0004 (16) |
C15 | 0.0286 (19) | 0.037 (2) | 0.037 (2) | −0.0077 (16) | 0.0128 (16) | −0.0027 (17) |
C16 | 0.047 (3) | 0.042 (3) | 0.073 (3) | −0.010 (2) | 0.026 (2) | −0.001 (2) |
O4 | 0.079 (3) | 0.039 (2) | 0.157 (4) | −0.0224 (19) | 0.063 (3) | −0.011 (2) |
O5 | 0.068 (2) | 0.074 (3) | 0.141 (4) | −0.009 (2) | 0.075 (3) | 0.010 (2) |
C19 | 0.0270 (19) | 0.040 (2) | 0.0303 (19) | −0.0024 (17) | 0.0099 (15) | −0.0074 (16) |
C20 | 0.027 (2) | 0.055 (3) | 0.059 (3) | −0.0045 (19) | 0.0147 (19) | −0.016 (2) |
N4 | 0.0220 (15) | 0.0320 (16) | 0.0330 (16) | −0.0011 (13) | 0.0085 (13) | −0.0069 (13) |
C21 | 0.0179 (17) | 0.039 (2) | 0.039 (2) | 0.0013 (15) | 0.0072 (15) | −0.0097 (17) |
C22 | 0.027 (2) | 0.050 (3) | 0.053 (2) | −0.0086 (18) | 0.0212 (18) | −0.018 (2) |
C23 | 0.034 (2) | 0.060 (3) | 0.066 (3) | −0.006 (2) | 0.027 (2) | −0.028 (2) |
C24 | 0.036 (2) | 0.042 (2) | 0.072 (3) | −0.0024 (19) | 0.022 (2) | −0.028 (2) |
C25 | 0.029 (2) | 0.036 (2) | 0.053 (2) | −0.0006 (17) | 0.0128 (19) | −0.0104 (19) |
C26 | 0.0202 (17) | 0.035 (2) | 0.037 (2) | 0.0026 (15) | 0.0076 (15) | −0.0063 (16) |
N5 | 0.0259 (15) | 0.0301 (16) | 0.0270 (15) | 0.0026 (13) | 0.0085 (12) | 0.0002 (12) |
C27 | 0.0211 (17) | 0.041 (2) | 0.0249 (17) | −0.0013 (16) | 0.0073 (14) | −0.0058 (16) |
C28 | 0.034 (2) | 0.054 (3) | 0.040 (2) | 0.0118 (19) | 0.0171 (18) | 0.0002 (19) |
C29 | 0.0239 (17) | 0.037 (2) | 0.0233 (17) | −0.0025 (15) | 0.0098 (14) | −0.0026 (15) |
C30 | 0.0294 (19) | 0.047 (2) | 0.0284 (19) | −0.0012 (17) | 0.0121 (16) | −0.0011 (18) |
O6 | 0.073 (2) | 0.0555 (19) | 0.0424 (17) | 0.0108 (17) | 0.0347 (16) | −0.0043 (15) |
O7 | 0.072 (2) | 0.0490 (18) | 0.0364 (15) | −0.0080 (15) | 0.0359 (15) | −0.0015 (13) |
C31 | 0.071 (3) | 0.061 (3) | 0.042 (2) | −0.013 (3) | 0.035 (2) | 0.000 (2) |
C33 | 0.0241 (17) | 0.036 (2) | 0.0236 (17) | −0.0025 (15) | 0.0064 (14) | 0.0017 (15) |
N6 | 0.0213 (14) | 0.0298 (16) | 0.0215 (14) | 0.0002 (12) | 0.0065 (12) | −0.0012 (12) |
C34 | 0.0217 (17) | 0.0291 (18) | 0.0267 (17) | −0.0027 (14) | 0.0086 (14) | −0.0009 (15) |
C35 | 0.033 (2) | 0.034 (2) | 0.0284 (19) | −0.0014 (16) | 0.0122 (16) | 0.0037 (16) |
C36 | 0.040 (2) | 0.028 (2) | 0.038 (2) | 0.0013 (17) | 0.0130 (18) | 0.0078 (17) |
C37 | 0.040 (2) | 0.026 (2) | 0.045 (2) | 0.0015 (17) | 0.0160 (18) | −0.0008 (17) |
C38 | 0.0305 (19) | 0.0302 (19) | 0.0337 (19) | −0.0025 (16) | 0.0134 (16) | −0.0062 (16) |
C39 | 0.0202 (17) | 0.0278 (18) | 0.0279 (18) | −0.0045 (14) | 0.0056 (14) | 0.0026 (15) |
N7 | 0.0210 (14) | 0.0298 (15) | 0.0243 (14) | −0.0021 (12) | 0.0088 (12) | 0.0001 (12) |
C40 | 0.0225 (17) | 0.0316 (19) | 0.0260 (17) | −0.0076 (15) | 0.0107 (14) | −0.0035 (15) |
C41 | 0.0226 (17) | 0.0325 (19) | 0.0238 (17) | −0.0054 (15) | 0.0076 (14) | −0.0017 (14) |
C42 | 0.0268 (18) | 0.039 (2) | 0.0272 (19) | −0.0075 (16) | 0.0096 (15) | 0.0000 (17) |
O8 | 0.064 (2) | 0.0514 (18) | 0.0240 (14) | 0.0069 (15) | 0.0120 (13) | 0.0062 (13) |
O9 | 0.0629 (19) | 0.0409 (16) | 0.0247 (13) | −0.0040 (14) | 0.0183 (13) | −0.0036 (12) |
C43 | 0.066 (3) | 0.047 (3) | 0.028 (2) | −0.005 (2) | 0.019 (2) | −0.0066 (18) |
C44 | 0.066 (3) | 0.085 (4) | 0.053 (3) | 0.007 (3) | 0.030 (3) | 0.002 (3) |
C45 | 0.0193 (17) | 0.038 (2) | 0.0279 (18) | −0.0033 (15) | 0.0095 (14) | 0.0063 (16) |
C46 | 0.031 (2) | 0.048 (2) | 0.031 (2) | 0.0038 (18) | 0.0042 (16) | 0.0021 (18) |
N8 | 0.0230 (14) | 0.0287 (16) | 0.0261 (15) | 0.0011 (12) | 0.0077 (12) | −0.0002 (12) |
C47 | 0.0201 (17) | 0.033 (2) | 0.034 (2) | 0.0044 (15) | 0.0069 (15) | 0.0014 (16) |
C48 | 0.0288 (19) | 0.037 (2) | 0.036 (2) | 0.0071 (17) | 0.0101 (16) | 0.0050 (17) |
C49 | 0.036 (2) | 0.031 (2) | 0.048 (2) | 0.0061 (17) | 0.0085 (19) | 0.0076 (18) |
C50 | 0.041 (2) | 0.031 (2) | 0.054 (3) | 0.0108 (18) | 0.013 (2) | 0.0007 (19) |
C51 | 0.033 (2) | 0.037 (2) | 0.039 (2) | 0.0071 (17) | 0.0110 (17) | −0.0031 (18) |
C52 | 0.0206 (17) | 0.035 (2) | 0.0279 (18) | 0.0069 (15) | 0.0067 (14) | 0.0025 (15) |
O10 | 0.084 (3) | 0.162 (5) | 0.078 (3) | −0.017 (3) | 0.029 (2) | 0.033 (3) |
Geometric parameters (Å, º) top
Fe1—O1 | 1.784 (2) | C20—H20C | 0.9600 |
Fe1—N3 | 2.020 (3) | N4—C21 | 1.412 (5) |
Fe1—N2 | 2.023 (3) | C21—C22 | 1.393 (5) |
Fe1—N4 | 2.038 (3) | C21—C26 | 1.407 (5) |
Fe1—N1 | 2.045 (3) | C22—C23 | 1.377 (6) |
Fe1—C21 | 2.745 (3) | C22—H22 | 0.9300 |
Fe1—C26 | 2.753 (4) | C23—C24 | 1.371 (6) |
Fe1—C13 | 2.851 (4) | C23—H23 | 0.9300 |
Fe1—C8 | 2.859 (4) | C24—C25 | 1.377 (6) |
Fe1—Fe2 | 3.2762 (11) | C24—H24 | 0.9300 |
Fe2—O1 | 1.788 (2) | C25—C26 | 1.385 (5) |
Fe2—N7 | 2.022 (3) | C25—H25 | 0.9300 |
Fe2—N6 | 2.026 (3) | N5—C27 | 1.320 (4) |
Fe2—N8 | 2.043 (3) | N5—C52 | 1.416 (4) |
Fe2—N5 | 2.044 (3) | C27—C29 | 1.429 (5) |
Fe2—C52 | 2.759 (4) | C27—C28 | 1.499 (5) |
Fe2—C47 | 2.762 (4) | C28—H28A | 0.9600 |
Fe2—C34 | 2.857 (4) | C28—H28B | 0.9600 |
Fe2—C39 | 2.860 (4) | C28—H28C | 0.9600 |
N1—C1 | 1.317 (5) | C29—C33 | 1.397 (5) |
N1—C26 | 1.424 (4) | C29—C30 | 1.470 (5) |
C1—C3 | 1.429 (5) | C30—O6 | 1.207 (5) |
C1—C2 | 1.509 (5) | C30—O7 | 1.342 (5) |
C2—H2A | 0.9600 | O7—C31 | 1.452 (5) |
C2—H2B | 0.9600 | C31—C32X | 1.382 (14) |
C2—H2C | 0.9600 | C31—C32 | 1.466 (11) |
C3—C7 | 1.392 (5) | C31—H31A | 0.9700 |
C3—C4 | 1.480 (5) | C31—H31B | 0.9700 |
C4—O2 | 1.207 (5) | C32—H32A | 0.9600 |
C4—O3 | 1.342 (5) | C32—H32B | 0.9600 |
O3—C5 | 1.452 (5) | C32—H32C | 0.9600 |
C5—C6X | 1.390 (11) | C32X—H32D | 0.9600 |
C5—C6 | 1.595 (15) | C32X—H32E | 0.9600 |
C5—H5A | 0.9700 | C32X—H32F | 0.9600 |
C5—H5B | 0.9700 | C33—N6 | 1.314 (4) |
C6—H6A | 0.9600 | C33—H33 | 0.9300 |
C6—H6B | 0.9600 | N6—C34 | 1.409 (4) |
C6—H6C | 0.9600 | C34—C35 | 1.390 (5) |
C6X—H6D | 0.9600 | C34—C39 | 1.404 (5) |
C6X—H6E | 0.9600 | C35—C36 | 1.377 (5) |
C6X—H6F | 0.9600 | C35—H35 | 0.9300 |
C7—N2 | 1.311 (5) | C36—C37 | 1.384 (5) |
C7—H7 | 0.9300 | C36—H36 | 0.9300 |
N2—C8 | 1.413 (5) | C37—C38 | 1.381 (5) |
C8—C9 | 1.391 (5) | C37—H37 | 0.9300 |
C8—C13 | 1.405 (5) | C38—C39 | 1.386 (5) |
C9—C10 | 1.385 (6) | C38—H38 | 0.9300 |
C9—H9 | 0.9300 | C39—N7 | 1.411 (4) |
C10—C11 | 1.384 (6) | N7—C40 | 1.318 (4) |
C10—H10 | 0.9300 | C40—C41 | 1.397 (5) |
C11—C12 | 1.374 (6) | C40—H40 | 0.9300 |
C11—H11 | 0.9300 | C41—C45 | 1.429 (5) |
C12—C13 | 1.381 (5) | C41—C42 | 1.478 (5) |
C12—H12 | 0.9300 | C42—O8 | 1.199 (4) |
C13—N3 | 1.416 (5) | C42—O9 | 1.356 (5) |
N3—C14 | 1.320 (5) | O9—C43 | 1.443 (4) |
C14—C15 | 1.388 (5) | C43—C44 | 1.495 (6) |
C14—H14 | 0.9300 | C43—H43A | 0.9700 |
C15—C19 | 1.430 (5) | C43—H43B | 0.9700 |
C15—C16 | 1.470 (6) | C44—H44A | 0.9600 |
C16—O5 | 1.192 (5) | C44—H44B | 0.9600 |
C16—O4 | 1.327 (6) | C44—H44C | 0.9600 |
O4—C17 | 1.455 (17) | C45—N8 | 1.322 (4) |
O4—C17X | 1.530 (11) | C45—C46 | 1.512 (5) |
C17—C18 | 1.36 (4) | C46—H46A | 0.9600 |
C17—H17A | 0.9700 | C46—H46B | 0.9600 |
C17—H17B | 0.9700 | C46—H46C | 0.9600 |
C18—H18A | 0.9600 | N8—C47 | 1.419 (5) |
C18—H18B | 0.9600 | C47—C48 | 1.393 (5) |
C18—H18C | 0.9600 | C47—C52 | 1.412 (5) |
C17X—C18X | 1.360 (17) | C48—C49 | 1.375 (5) |
C17X—H17C | 0.9700 | C48—H48 | 0.9300 |
C17X—H17D | 0.9700 | C49—C50 | 1.378 (6) |
C18X—H18D | 0.9600 | C49—H49 | 0.9300 |
C18X—H18E | 0.9600 | C50—C51 | 1.374 (6) |
C18X—H18F | 0.9600 | C50—H50 | 0.9300 |
C19—N4 | 1.311 (5) | C51—C52 | 1.391 (5) |
C19—C20 | 1.515 (5) | C51—H51 | 0.9300 |
C20—H20A | 0.9600 | O11—O11X | 0.95 (2) |
C20—H20B | 0.9600 | | |
| | | |
O1—Fe1—N3 | 112.13 (12) | C18—C17—O4 | 116 (2) |
O1—Fe1—N2 | 112.42 (11) | C18—C17—H17A | 108.2 |
N3—Fe1—N2 | 78.82 (12) | O4—C17—H17A | 108.2 |
O1—Fe1—N4 | 106.88 (11) | C18—C17—H17B | 108.2 |
N3—Fe1—N4 | 87.00 (12) | O4—C17—H17B | 108.2 |
N2—Fe1—N4 | 140.70 (12) | H17A—C17—H17B | 107.3 |
O1—Fe1—N1 | 105.93 (12) | C18X—C17X—O4 | 103.8 (10) |
N3—Fe1—N1 | 141.93 (12) | C18X—C17X—H17C | 111.0 |
N2—Fe1—N1 | 87.56 (12) | O4—C17X—H17C | 111.0 |
N4—Fe1—N1 | 81.42 (12) | C18X—C17X—H17D | 111.0 |
O1—Fe1—C21 | 94.35 (11) | O4—C17X—H17D | 111.0 |
N3—Fe1—C21 | 116.94 (12) | H17C—C17X—H17D | 109.0 |
N2—Fe1—C21 | 141.67 (12) | N4—C19—C15 | 120.5 (3) |
N4—Fe1—C21 | 29.94 (11) | N4—C19—C20 | 119.7 (3) |
N1—Fe1—C21 | 58.00 (12) | C15—C19—C20 | 119.4 (3) |
O1—Fe1—C26 | 93.92 (11) | C19—C20—H20A | 109.5 |
N3—Fe1—C26 | 141.62 (11) | C19—C20—H20B | 109.5 |
N2—Fe1—C26 | 117.73 (12) | H20A—C20—H20B | 109.5 |
N4—Fe1—C26 | 57.79 (11) | C19—C20—H20C | 109.5 |
N1—Fe1—C26 | 30.19 (11) | H20A—C20—H20C | 109.5 |
C21—Fe1—C26 | 29.66 (11) | H20B—C20—H20C | 109.5 |
O1—Fe1—C13 | 105.84 (11) | C19—N4—C21 | 124.0 (3) |
N3—Fe1—C13 | 27.66 (11) | C19—N4—Fe1 | 132.0 (3) |
N2—Fe1—C13 | 54.97 (12) | C21—N4—Fe1 | 104.0 (2) |
N4—Fe1—C13 | 114.31 (11) | C22—C21—C26 | 119.5 (4) |
N1—Fe1—C13 | 137.96 (12) | C22—C21—N4 | 122.9 (4) |
C21—Fe1—C13 | 144.07 (11) | C26—C21—N4 | 116.5 (3) |
C26—Fe1—C13 | 160.24 (11) | C22—C21—Fe1 | 146.1 (3) |
O1—Fe1—C8 | 106.45 (10) | C26—C21—Fe1 | 75.5 (2) |
N3—Fe1—C8 | 54.93 (11) | N4—C21—Fe1 | 46.08 (15) |
N2—Fe1—C8 | 27.41 (11) | C23—C22—C21 | 120.0 (4) |
N4—Fe1—C8 | 136.68 (11) | C23—C22—H22 | 120.0 |
N1—Fe1—C8 | 114.63 (11) | C21—C22—H22 | 120.0 |
C21—Fe1—C8 | 159.20 (10) | C24—C23—C22 | 120.3 (4) |
C26—Fe1—C8 | 144.52 (11) | C24—C23—H23 | 119.8 |
C13—Fe1—C8 | 28.49 (11) | C22—C23—H23 | 119.8 |
O1—Fe1—Fe2 | 23.52 (7) | C23—C24—C25 | 120.7 (4) |
N3—Fe1—Fe2 | 120.52 (9) | C23—C24—H24 | 119.7 |
N2—Fe1—Fe2 | 91.63 (9) | C25—C24—H24 | 119.7 |
N4—Fe1—Fe2 | 126.71 (8) | C24—C25—C26 | 120.2 (4) |
N1—Fe1—Fe2 | 94.99 (8) | C24—C25—H25 | 119.9 |
C21—Fe1—Fe2 | 106.46 (8) | C26—C25—H25 | 119.9 |
C26—Fe1—Fe2 | 94.70 (8) | C25—C26—C21 | 119.2 (3) |
C13—Fe1—Fe2 | 103.51 (8) | C25—C26—N1 | 123.8 (3) |
C8—Fe1—Fe2 | 93.20 (7) | C21—C26—N1 | 116.0 (3) |
O1—Fe2—N7 | 114.15 (11) | C25—C26—Fe1 | 146.9 (3) |
O1—Fe2—N6 | 111.34 (11) | C21—C26—Fe1 | 74.9 (2) |
N7—Fe2—N6 | 78.50 (11) | N1—C26—Fe1 | 46.24 (16) |
O1—Fe2—N8 | 107.00 (11) | C27—N5—C52 | 124.6 (3) |
N7—Fe2—N8 | 87.49 (11) | C27—N5—Fe2 | 131.1 (3) |
N6—Fe2—N8 | 141.63 (11) | C52—N5—Fe2 | 104.3 (2) |
O1—Fe2—N5 | 105.92 (11) | N5—C27—C29 | 121.1 (3) |
N7—Fe2—N5 | 139.93 (11) | N5—C27—C28 | 119.7 (3) |
N6—Fe2—N5 | 87.27 (11) | C29—C27—C28 | 118.9 (3) |
N8—Fe2—N5 | 80.85 (11) | C27—C28—H28A | 109.5 |
O1—Fe2—C52 | 94.03 (11) | C27—C28—H28B | 109.5 |
N7—Fe2—C52 | 140.96 (11) | H28A—C28—H28B | 109.5 |
N6—Fe2—C52 | 117.09 (11) | C27—C28—H28C | 109.5 |
N8—Fe2—C52 | 57.54 (11) | H28A—C28—H28C | 109.5 |
N5—Fe2—C52 | 29.82 (11) | H28B—C28—H28C | 109.5 |
O1—Fe2—C47 | 94.29 (11) | C33—C29—C27 | 124.8 (3) |
N7—Fe2—C47 | 117.29 (11) | C33—C29—C30 | 116.8 (3) |
N6—Fe2—C47 | 141.65 (11) | C27—C29—C30 | 118.4 (3) |
N8—Fe2—C47 | 29.83 (11) | O6—C30—O7 | 121.4 (3) |
N5—Fe2—C47 | 57.65 (11) | O6—C30—C29 | 125.7 (4) |
C52—Fe2—C47 | 29.63 (10) | O7—C30—C29 | 112.8 (3) |
O1—Fe2—C34 | 106.45 (10) | C30—O7—C31 | 116.5 (3) |
N7—Fe2—C34 | 54.67 (10) | C32X—C31—O7 | 110.5 (7) |
N6—Fe2—C34 | 27.36 (10) | C32X—C31—C32 | 49.2 (7) |
N8—Fe2—C34 | 137.32 (11) | O7—C31—C32 | 111.7 (5) |
N5—Fe2—C34 | 114.13 (11) | C32X—C31—H31A | 139.8 |
C52—Fe2—C34 | 143.69 (10) | O7—C31—H31A | 109.3 |
C47—Fe2—C34 | 159.25 (10) | C32—C31—H31A | 109.3 |
O1—Fe2—C39 | 107.47 (10) | C32X—C31—H31B | 63.5 |
N7—Fe2—C39 | 27.30 (10) | O7—C31—H31B | 109.3 |
N6—Fe2—C39 | 54.75 (10) | C32—C31—H31B | 109.3 |
N8—Fe2—C39 | 114.45 (11) | H31A—C31—H31B | 107.9 |
N5—Fe2—C39 | 136.41 (11) | C31—C32—H32A | 109.5 |
C52—Fe2—C39 | 158.50 (10) | C31—C32—H32B | 109.5 |
C47—Fe2—C39 | 143.96 (10) | C31—C32—H32C | 109.5 |
C34—Fe2—C39 | 28.43 (9) | C31—C32X—H32D | 109.5 |
O1—Fe2—Fe1 | 23.46 (7) | C31—C32X—H32E | 109.5 |
N7—Fe2—Fe1 | 122.38 (8) | C31—C32X—H32F | 109.5 |
N6—Fe2—Fe1 | 90.65 (8) | N6—C33—C29 | 126.5 (3) |
N8—Fe2—Fe1 | 126.44 (8) | N6—C33—H33 | 116.8 |
N5—Fe2—Fe1 | 94.73 (8) | C29—C33—H33 | 116.8 |
C52—Fe2—Fe1 | 94.33 (8) | C33—N6—C34 | 120.9 (3) |
C47—Fe2—Fe1 | 105.97 (8) | C33—N6—Fe2 | 127.8 (2) |
C34—Fe2—Fe1 | 93.31 (7) | C34—N6—Fe2 | 111.3 (2) |
C39—Fe2—Fe1 | 105.11 (7) | C35—C34—C39 | 120.0 (3) |
Fe1—O1—Fe2 | 133.01 (14) | C35—C34—N6 | 125.5 (3) |
C1—N1—C26 | 124.7 (3) | C39—C34—N6 | 114.5 (3) |
C1—N1—Fe1 | 131.7 (3) | C35—C34—Fe2 | 158.2 (3) |
C26—N1—Fe1 | 103.6 (2) | C39—C34—Fe2 | 75.9 (2) |
N1—C1—C3 | 119.9 (3) | N6—C34—Fe2 | 41.38 (15) |
N1—C1—C2 | 120.2 (3) | C36—C35—C34 | 119.5 (3) |
C3—C1—C2 | 119.6 (3) | C36—C35—H35 | 120.2 |
C1—C2—H2A | 109.5 | C34—C35—H35 | 120.2 |
C1—C2—H2B | 109.5 | C35—C36—C37 | 121.0 (3) |
H2A—C2—H2B | 109.5 | C35—C36—H36 | 119.5 |
C1—C2—H2C | 109.5 | C37—C36—H36 | 119.5 |
H2A—C2—H2C | 109.5 | C38—C37—C36 | 119.7 (4) |
H2B—C2—H2C | 109.5 | C38—C37—H37 | 120.2 |
C7—C3—C1 | 125.4 (3) | C36—C37—H37 | 120.2 |
C7—C3—C4 | 112.0 (3) | C37—C38—C39 | 120.5 (3) |
C1—C3—C4 | 122.6 (3) | C37—C38—H38 | 119.8 |
O2—C4—O3 | 122.2 (4) | C39—C38—H38 | 119.8 |
O2—C4—C3 | 125.2 (4) | C38—C39—C34 | 119.3 (3) |
O3—C4—C3 | 112.6 (3) | C38—C39—N7 | 126.7 (3) |
C4—O3—C5 | 115.5 (3) | C34—C39—N7 | 114.0 (3) |
C6X—C5—O3 | 109.1 (6) | C38—C39—Fe2 | 159.7 (2) |
C6X—C5—C6 | 27.3 (6) | C34—C39—Fe2 | 75.7 (2) |
O3—C5—C6 | 105.5 (6) | N7—C39—Fe2 | 41.09 (15) |
C6X—C5—H5A | 84.6 | C40—N7—C39 | 121.7 (3) |
O3—C5—H5A | 110.6 | C40—N7—Fe2 | 126.6 (2) |
C6—C5—H5A | 110.6 | C39—N7—Fe2 | 111.6 (2) |
C6X—C5—H5B | 129.4 | N7—C40—C41 | 127.6 (3) |
O3—C5—H5B | 110.6 | N7—C40—H40 | 116.2 |
C6—C5—H5B | 110.6 | C41—C40—H40 | 116.2 |
H5A—C5—H5B | 108.8 | C40—C41—C45 | 124.6 (3) |
C5—C6—H6A | 109.5 | C40—C41—C42 | 116.4 (3) |
C5—C6—H6B | 109.5 | C45—C41—C42 | 118.9 (3) |
C5—C6—H6C | 109.5 | O8—C42—O9 | 121.3 (3) |
C5—C6X—H6D | 109.5 | O8—C42—C41 | 126.8 (4) |
C5—C6X—H6E | 109.5 | O9—C42—C41 | 111.9 (3) |
H6D—C6X—H6E | 109.5 | C42—O9—C43 | 117.3 (3) |
C5—C6X—H6F | 109.5 | O9—C43—C44 | 110.2 (4) |
H6D—C6X—H6F | 109.5 | O9—C43—H43A | 109.6 |
H6E—C6X—H6F | 109.5 | C44—C43—H43A | 109.6 |
N2—C7—C3 | 127.3 (3) | O9—C43—H43B | 109.6 |
N2—C7—H7 | 116.3 | C44—C43—H43B | 109.6 |
C3—C7—H7 | 116.3 | H43A—C43—H43B | 108.1 |
C7—N2—C8 | 121.8 (3) | C43—C44—H44A | 109.5 |
C7—N2—Fe1 | 126.8 (2) | C43—C44—H44B | 109.5 |
C8—N2—Fe1 | 111.4 (2) | H44A—C44—H44B | 109.5 |
C9—C8—C13 | 119.9 (4) | C43—C44—H44C | 109.5 |
C9—C8—N2 | 125.9 (4) | H44A—C44—H44C | 109.5 |
C13—C8—N2 | 114.2 (3) | H44B—C44—H44C | 109.5 |
C9—C8—Fe1 | 159.0 (3) | N8—C45—C41 | 120.3 (3) |
C13—C8—Fe1 | 75.4 (2) | N8—C45—C46 | 119.8 (3) |
N2—C8—Fe1 | 41.23 (16) | C41—C45—C46 | 119.7 (3) |
C10—C9—C8 | 119.5 (4) | C45—C46—H46A | 109.5 |
C10—C9—H9 | 120.2 | C45—C46—H46B | 109.5 |
C8—C9—H9 | 120.2 | H46A—C46—H46B | 109.5 |
C11—C10—C9 | 120.0 (4) | C45—C46—H46C | 109.5 |
C11—C10—H10 | 120.0 | H46A—C46—H46C | 109.5 |
C9—C10—H10 | 120.0 | H46B—C46—H46C | 109.5 |
C12—C11—C10 | 121.0 (4) | C45—N8—C47 | 123.8 (3) |
C12—C11—H11 | 119.5 | C45—N8—Fe2 | 131.7 (2) |
C10—C11—H11 | 119.5 | C47—N8—Fe2 | 104.4 (2) |
C11—C12—C13 | 119.8 (4) | C48—C47—C52 | 119.5 (3) |
C11—C12—H12 | 120.1 | C48—C47—N8 | 123.9 (3) |
C13—C12—H12 | 120.1 | C52—C47—N8 | 115.6 (3) |
C12—C13—C8 | 119.7 (4) | C48—C47—Fe2 | 146.5 (2) |
C12—C13—N3 | 126.0 (4) | C52—C47—Fe2 | 75.0 (2) |
C8—C13—N3 | 114.3 (3) | N8—C47—Fe2 | 45.76 (15) |
C12—C13—Fe1 | 158.7 (3) | C49—C48—C47 | 120.1 (4) |
C8—C13—Fe1 | 76.1 (2) | C49—C48—H48 | 119.9 |
N3—C13—Fe1 | 41.47 (16) | C47—C48—H48 | 119.9 |
C14—N3—C13 | 121.9 (3) | C48—C49—C50 | 120.6 (4) |
C14—N3—Fe1 | 127.2 (3) | C48—C49—H49 | 119.7 |
C13—N3—Fe1 | 110.9 (2) | C50—C49—H49 | 119.7 |
N3—C14—C15 | 127.1 (4) | C51—C50—C49 | 120.0 (4) |
N3—C14—H14 | 116.5 | C51—C50—H50 | 120.0 |
C15—C14—H14 | 116.5 | C49—C50—H50 | 120.0 |
C14—C15—C19 | 124.4 (3) | C50—C51—C52 | 121.0 (4) |
C14—C15—C16 | 117.2 (4) | C50—C51—H51 | 119.5 |
C19—C15—C16 | 118.3 (3) | C52—C51—H51 | 119.5 |
O5—C16—O4 | 120.7 (4) | C51—C52—C47 | 118.7 (3) |
O5—C16—C15 | 127.0 (4) | C51—C52—N5 | 124.2 (3) |
O4—C16—C15 | 112.3 (4) | C47—C52—N5 | 116.2 (3) |
C16—O4—C17 | 123.1 (8) | C51—C52—Fe2 | 147.7 (3) |
C16—O4—C17X | 111.3 (5) | C47—C52—Fe2 | 75.3 (2) |
C17—O4—C17X | 30.4 (7) | N5—C52—Fe2 | 45.89 (15) |