The title compound, [Fe2Yb2(CN)12(C4H9NO)5(H2O)6]·2H2O, is a tetranuclear complex, where the four metal centres are connected through three cyano bridges, the iron centres making one and two bridges, respectively. Each Fe atom is surrounded by six cyano ligands, forming almost ideal octahedra. The two Yb atoms have different ligand environments; both are coordinated by seven ligands, consisting of water molecules, dimethylacetamide (DMA) solvent and cyano groups, but not in the same ratio. Four of the five DMA molecules show various degrees of common structural disorder. The asymmetric unit also includes two solvent water molecules, which take part in hydrogen bonding, forming an extended network of tetramers.
Supporting information
CCDC reference: 605145
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.003 Å
- Disorder in main residue
- R factor = 0.027
- wR factor = 0.054
- Data-to-parameter ratio = 62.3
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 15
| Author Response: In order to refine the disorder in the DMA molecules it was
necessary to describe them isotropically.
|
PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.63 Ratio
| Author Response: C54 and C70A has the largest and smallest Ueq value, respectively
compared to the other carbon atoms.
C54 is a methyl atom and C70A is a carbonyl atom - both belonging to separate
disordered DMA molecules. In an isotropic model the disorder may not be
described accurately enough potentially leading to larger differences
between Ueq values.
|
PLAT220_ALERT_2_A Large Non-Solvent N Ueq(max)/Ueq(min) ... 5.14 Ratio
| Author Response: C54 and C70A has the largest and smallest Ueq value, respectively
compared to the other carbon atoms.
C54 is a methyl atom and C70A is a carbonyl atom - both belonging to separate
disordered DMA molecules. In an isotropic model the disorder may not be
described accurately enough potentially leading to larger differences
between Ueq values.
|
PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.72 Ratio
| Author Response: The hydrogen atoms on the water molecule with O2 have the smallest
Ueq value, whereas the hydrogens on C54 (a methyl atom in a DMA molecule)
have the largest value compared to other hydrogen atoms. The disorder in the
DMA molecules leads to C54 having the largest Ueq value. Because
the displacement parameters of the hydrogen atoms depend on the displacement
of the parent C atom the H atoms on C54 also get the largest Ueq values.
|
Alert level B
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C12
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C13A
PLAT417_ALERT_2_B Short Inter D-H..H-D H2B .. H98A .. 2.06 Ang.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT213_ALERT_2_C Atom O60 has ADP max/min Ratio ............. 3.20 prolat
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.50 Ratio
| Author Response: C54 and C70A has the largest and smallest Ueq value, respectively
compared to the other carbon atoms.
C54 is a methyl atom and C70A is a carbonyl atom - both belonging to separate
disordered DMA molecules. In an isotropic model the disorder may not be
described accurately enough potentially leading to larger differences
between Ueq values.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O60
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C11A
PLAT301_ALERT_3_C Main Residue Disorder ......................... 24.00 Perc.
PLAT416_ALERT_2_C Short Intra D-H..H-D H1B .. H2B .. 1.97 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact N2 .. C70 .. 3.03 Ang.
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 43.31
From the CIF: _reflns_number_total 37796
Count of symmetry unique reflns 20103
Completeness (_total/calc) 188.01%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 17693
Fraction of Friedel pairs measured 0.880
Are heavy atom types Z>Si present yes
4 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
13 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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: Please provide missing details and reference; cell refinement: SAINT-Plus; data reduction: SAINT-Plus (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XSHELL (Bruker, 2000); software used to prepare material for publication: enCIFer (Version 1.1; Allen et al., 2004) and WinGX (Farrugia, 1999).
Hexaaqua-1
κ3O,3
κ3O-tri-µ-cyano-1:2
κ2N:
C;2:3
κ2C:
N;3:4
κ2N:
C-
nonacyano-2
κ4C,4
κ5C-pentakis(
N,
N-dimethylacetamide)-1
κ3O,3
κ2O- diiron(III)diytterbium(III)
dihydrate
top
Crystal data top
[Fe2Yb2(CN)12(C4H9NO)5(H2O)6]·2H2O | F(000) = 2672 |
Mr = 1349.76 | Dx = 1.725 Mg m−3 |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 9695 reflections |
a = 25.2387 (9) Å | θ = 5.7–85.4° |
b = 14.4943 (6) Å | µ = 4.18 mm−1 |
c = 14.2058 (5) Å | T = 100 K |
V = 5196.7 (3) Å3 | Block, yellow |
Z = 4 | 0.20 × 0.15 × 0.10 mm |
Data collection top
Bruker X8 APEXII diffractometer | 37796 independent reflections |
Radiation source: fine-focus sealed tube | 32727 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
Detector resolution: 83.33 pixels mm-1 | θmax = 43.3°, θmin = 1.6° |
φ and ω scans | h = −37→48 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −27→27 |
Tmin = 0.45, Tmax = 0.66 | l = −27→27 |
271064 measured reflections | |
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)] = 0.027 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.054 | w = 1/[σ2(Fo2) + (0.0221P)2 + 1.3004P] where P = (Fo2 + 2Fc2)/3 |
S = 1.17 | (Δ/σ)max = 0.011 |
37796 reflections | Δρmax = 2.36 e Å−3 |
607 parameters | Δρmin = −1.51 e Å−3 |
25 restraints | Absolute structure: Flack (1983), with 17930 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.007 (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) |
Fe3 | −0.006526 (7) | 0.698941 (13) | 0.44633 (2) | 0.00870 (3) | |
Fe4 | 0.256330 (8) | 0.303175 (16) | 0.431182 (15) | 0.00790 (4) | |
Yb1 | 0.206811 (2) | 0.667222 (4) | 0.447156 (6) | 0.00839 (1) | |
Yb2 | 0.047075 (2) | 0.204152 (4) | 0.452747 (5) | 0.00999 (1) | |
C1 | −0.08253 (5) | 0.69562 (10) | 0.44650 (17) | 0.0135 (2) | |
C1A | 0.24021 (5) | 0.43272 (10) | 0.44113 (14) | 0.0119 (3) | |
C2 | −0.00903 (8) | 0.68828 (17) | 0.31024 (14) | 0.0139 (3) | |
C2A | 0.26033 (7) | 0.29269 (12) | 0.56727 (12) | 0.0133 (3) | |
C3 | −0.00294 (5) | 0.56506 (10) | 0.44909 (18) | 0.0141 (2) | |
C3A | 0.33094 (6) | 0.33289 (12) | 0.42678 (11) | 0.0130 (3) | |
C4 | −0.00755 (8) | 0.69927 (17) | 0.58317 (14) | 0.0149 (3) | |
C4A | 0.25240 (7) | 0.31147 (13) | 0.29527 (12) | 0.0126 (3) | |
C6 | 0.06987 (5) | 0.70365 (9) | 0.44865 (15) | 0.0118 (2) | |
C6A | 0.18094 (6) | 0.27605 (11) | 0.43574 (11) | 0.0124 (3) | |
C5 | −0.01132 (6) | 0.83282 (12) | 0.43639 (15) | 0.0159 (3) | |
C5A | 0.27547 (7) | 0.17457 (12) | 0.41935 (13) | 0.0147 (3) | |
C21 | 0.15301 (6) | 0.61926 (13) | 0.65846 (12) | 0.0151 (3) | |
C22 | 0.10039 (8) | 0.53172 (19) | 0.77270 (17) | 0.0288 (5) | |
H22A | 0.1077 | 0.5769 | 0.8204 | 0.043* | |
H22B | 0.1022 | 0.4711 | 0.7997 | 0.043* | |
H22C | 0.0656 | 0.5419 | 0.7476 | 0.043* | |
C23 | 0.16309 (9) | 0.45365 (15) | 0.66348 (17) | 0.0257 (4) | |
H23A | 0.1901 | 0.4671 | 0.6179 | 0.039* | |
H23B | 0.1361 | 0.4162 | 0.6350 | 0.039* | |
H23C | 0.1784 | 0.4210 | 0.7156 | 0.039* | |
N1 | −0.12836 (5) | 0.69524 (10) | 0.44684 (19) | 0.0218 (3) | |
N1A | 0.23131 (5) | 0.51055 (9) | 0.44746 (16) | 0.0167 (2) | |
N2 | −0.01323 (9) | 0.67942 (16) | 0.22977 (13) | 0.0207 (4) | |
N2A | 0.26313 (7) | 0.28571 (13) | 0.64822 (12) | 0.0206 (3) | |
N3 | −0.00014 (6) | 0.48563 (10) | 0.44660 (18) | 0.0221 (3) | |
N3A | 0.37526 (6) | 0.35284 (12) | 0.42379 (12) | 0.0206 (3) | |
N4 | −0.00874 (8) | 0.69576 (17) | 0.66406 (13) | 0.0227 (4) | |
N4A | 0.25084 (7) | 0.31478 (14) | 0.21390 (12) | 0.0201 (3) | |
N6 | 0.11588 (4) | 0.70442 (9) | 0.45014 (16) | 0.0153 (2) | |
N6A | 0.13601 (5) | 0.26147 (11) | 0.43810 (12) | 0.0160 (3) | |
N5 | −0.01555 (7) | 0.91181 (12) | 0.42768 (13) | 0.0246 (4) | |
N5A | 0.28814 (7) | 0.09847 (12) | 0.41233 (15) | 0.0250 (4) | |
N20 | 0.13971 (6) | 0.53976 (13) | 0.69689 (12) | 0.0183 (3) | |
O1 | 0.22730 (6) | 0.77855 (10) | 0.33939 (9) | 0.0159 (2) | |
H1A | 0.2255 (9) | 0.7784 (16) | 0.2715 (2) | 0.019* | |
H1B | 0.2498 (8) | 0.8287 (12) | 0.3603 (13) | 0.019* | |
O2 | 0.22021 (5) | 0.80284 (10) | 0.52979 (9) | 0.0147 (2) | |
H2A | 0.2346 (8) | 0.7898 (16) | 0.5917 (8) | 0.018* | |
H2B | 0.2437 (7) | 0.8454 (14) | 0.4976 (13) | 0.018* | |
O3 | 0.29702 (4) | 0.66422 (9) | 0.46166 (16) | 0.0252 (4) | |
H3A | 0.3114 (9) | 0.6155 (10) | 0.5005 (16) | 0.030* | |
H3B | 0.3184 (8) | 0.7192 (8) | 0.4701 (19) | 0.030* | |
O4 | −0.01636 (5) | 0.10780 (10) | 0.38197 (11) | 0.0181 (3) | |
H4A | −0.0124 (8) | 0.0420 (4) | 0.3915 (18) | 0.022* | |
H4B | −0.0534 (3) | 0.1244 (13) | 0.3867 (19) | 0.022* | |
O5 | 0.05126 (5) | 0.33740 (10) | 0.54731 (9) | 0.0166 (2) | |
H5A | 0.0395 (9) | 0.3968 (8) | 0.5234 (14) | 0.020* | |
H5B | 0.0424 (10) | 0.3337 (15) | 0.6137 (5) | 0.020* | |
O6 | 0.01503 (6) | 0.31275 (10) | 0.35417 (9) | 0.0170 (2) | |
H6A | 0.0128 (10) | 0.3098 (15) | 0.2859 (3) | 0.020* | |
H6B | −0.0007 (9) | 0.3705 (9) | 0.3746 (13) | 0.020* | |
O98 | 0.28225 (5) | 0.91301 (9) | 0.42138 (10) | 0.0165 (2) | |
H98A | 0.3152 (4) | 0.8844 (11) | 0.441 (2) | 0.020* | |
H98B | 0.2879 (7) | 0.9783 (4) | 0.4122 (18) | 0.020* | |
O20 | 0.18601 (6) | 0.62270 (12) | 0.59169 (10) | 0.0149 (3) | |
C24 | 0.12900 (7) | 0.70600 (14) | 0.69564 (15) | 0.0207 (4) | |
H24A | 0.1459 | 0.7582 | 0.6669 | 0.031* | |
H24B | 0.1338 | 0.7087 | 0.7626 | 0.031* | |
H24C | 0.0918 | 0.7069 | 0.6813 | 0.031* | |
O99 | 0.37355 (6) | 0.54030 (12) | 0.50654 (13) | 0.0277 (3) | |
H99A | 0.3761 (9) | 0.4822 (9) | 0.4736 (17) | 0.033* | |
H99B | 0.4041 (6) | 0.5783 (13) | 0.4924 (18) | 0.033* | |
O10 | 0.18233 (7) | 0.61067 (12) | 0.30785 (11) | 0.0182 (3) | |
N10 | 0.14137 (9) | 0.50361 (18) | 0.22049 (17) | 0.0166 (5)* | 0.667 (5) |
C10 | 0.18218 (10) | 0.55841 (19) | 0.23655 (18) | 0.0142 (5)* | 0.667 (5) |
C11 | 0.13814 (9) | 0.44220 (17) | 0.13759 (17) | 0.0273 (4)* | 0.667 (5) |
H11A | 0.1404 | 0.4784 | 0.0811 | 0.041* | 0.667 (5) |
H11B | 0.1051 | 0.4095 | 0.1386 | 0.041* | 0.667 (5) |
H11C | 0.1669 | 0.3989 | 0.1392 | 0.041* | 0.667 (5) |
C12 | 0.09920 (13) | 0.5018 (3) | 0.2945 (2) | 0.0501 (8)* | 0.667 (5) |
H12A | 0.1023 | 0.4461 | 0.3307 | 0.075* | 0.667 (5) |
H12B | 0.0650 | 0.5040 | 0.2651 | 0.075* | 0.667 (5) |
H12C | 0.1033 | 0.5542 | 0.3353 | 0.075* | 0.667 (5) |
C13 | 0.22585 (11) | 0.5530 (2) | 0.1635 (2) | 0.0369 (6)* | 0.667 (5) |
H13A | 0.2506 | 0.6023 | 0.1736 | 0.055* | 0.667 (5) |
H13B | 0.2108 | 0.5585 | 0.1017 | 0.055* | 0.667 (5) |
H13C | 0.2438 | 0.4949 | 0.1689 | 0.055* | 0.667 (5) |
N10A | 0.17024 (19) | 0.5109 (4) | 0.1910 (3) | 0.0168 (10)* | 0.333 (5) |
C10A | 0.15679 (18) | 0.5426 (4) | 0.2750 (3) | 0.0125 (9)* | 0.333 (5) |
C12A | 0.13814 (9) | 0.44220 (17) | 0.13759 (17) | 0.0273 (4)* | 0.333 (5) |
H12D | 0.1109 | 0.4177 | 0.1777 | 0.041* | 0.333 (5) |
H12E | 0.1607 | 0.3930 | 0.1166 | 0.041* | 0.333 (5) |
H12F | 0.1222 | 0.4717 | 0.0841 | 0.041* | 0.333 (5) |
C13A | 0.09920 (13) | 0.5018 (3) | 0.2945 (2) | 0.0501 (8)* | 0.333 (5) |
H13D | 0.0906 | 0.5091 | 0.3599 | 0.075* | 0.333 (5) |
H13E | 0.0986 | 0.4375 | 0.2785 | 0.075* | 0.333 (5) |
H13F | 0.0737 | 0.5343 | 0.2569 | 0.075* | 0.333 (5) |
C11A | 0.22585 (11) | 0.5530 (2) | 0.1635 (2) | 0.0369 (6)* | 0.333 (5) |
H11D | 0.2376 | 0.5938 | 0.2125 | 0.055* | 0.333 (5) |
H11E | 0.2226 | 0.5868 | 0.1056 | 0.055* | 0.333 (5) |
H11F | 0.2511 | 0.5041 | 0.1556 | 0.055* | 0.333 (5) |
O60 | 0.08617 (7) | 0.11926 (18) | 0.34371 (15) | 0.0368 (6) | |
N60 | 0.15366 (11) | 0.1048 (2) | 0.2498 (2) | 0.0166 (6)* | 0.554 (5) |
C61 | 0.13126 (12) | 0.0773 (2) | 0.3294 (2) | 0.0147 (6)* | 0.554 (5) |
C62 | 0.12683 (10) | 0.1798 (2) | 0.19222 (19) | 0.0273 (5)* | 0.554 (5) |
H62A | 0.0995 | 0.1529 | 0.1541 | 0.041* | 0.554 (5) |
H62B | 0.1525 | 0.2091 | 0.1524 | 0.041* | 0.554 (5) |
H62C | 0.1116 | 0.2247 | 0.2338 | 0.041* | 0.554 (5) |
C63 | 0.20506 (10) | 0.0625 (2) | 0.21932 (19) | 0.0329 (5)* | 0.554 (5) |
H63A | 0.2168 | 0.0193 | 0.2662 | 0.049* | 0.554 (5) |
H63B | 0.2312 | 0.1100 | 0.2117 | 0.049* | 0.554 (5) |
H63C | 0.2001 | 0.0310 | 0.1605 | 0.049* | 0.554 (5) |
C64 | 0.15882 (9) | 0.00915 (18) | 0.38757 (17) | 0.0283 (4)* | 0.554 (5) |
H64A | 0.1865 | 0.0390 | 0.4225 | 0.042* | 0.554 (5) |
H64B | 0.1739 | −0.0376 | 0.3479 | 0.042* | 0.554 (5) |
H64C | 0.1341 | −0.0187 | 0.4304 | 0.042* | 0.554 (5) |
N60A | 0.16084 (15) | 0.0639 (3) | 0.2918 (3) | 0.0204 (8)* | 0.446 (5) |
C61A | 0.12333 (15) | 0.1259 (3) | 0.2764 (3) | 0.0148 (8)* | 0.446 (5) |
C64A | 0.12683 (10) | 0.1798 (2) | 0.19222 (19) | 0.0273 (5)* | 0.446 (5) |
H64D | 0.1580 | 0.2176 | 0.1946 | 0.041* | 0.446 (5) |
H64E | 0.0961 | 0.2183 | 0.1869 | 0.041* | 0.446 (5) |
H64F | 0.1288 | 0.1395 | 0.1387 | 0.041* | 0.446 (5) |
C62A | 0.20506 (10) | 0.0625 (2) | 0.21932 (19) | 0.0329 (5)* | 0.446 (5) |
H62D | 0.1930 | 0.0314 | 0.1636 | 0.049* | 0.446 (5) |
H62E | 0.2351 | 0.0305 | 0.2447 | 0.049* | 0.446 (5) |
H62F | 0.2149 | 0.1246 | 0.2039 | 0.049* | 0.446 (5) |
C63A | 0.15882 (9) | 0.00915 (18) | 0.38757 (17) | 0.0283 (4)* | 0.446 (5) |
H63D | 0.1774 | 0.0432 | 0.4352 | 0.042* | 0.446 (5) |
H63E | 0.1752 | −0.0501 | 0.3795 | 0.042* | 0.446 (5) |
H63F | 0.1226 | 0.0009 | 0.4064 | 0.042* | 0.446 (5) |
O50 | 0.08175 (7) | 0.11465 (15) | 0.55938 (13) | 0.0273 (4) | |
N50 | 0.11019 (16) | 0.0176 (3) | 0.6672 (3) | 0.0360 (10)* | 0.582 (6) |
C51 | 0.10565 (14) | 0.1047 (3) | 0.6374 (3) | 0.0213 (8)* | 0.582 (6) |
C52 | 0.13149 (13) | 0.1855 (3) | 0.6957 (2) | 0.0399 (7)* | 0.582 (6) |
H52A | 0.1367 | 0.2380 | 0.6556 | 0.060* | 0.582 (6) |
H52B | 0.1650 | 0.1657 | 0.7203 | 0.060* | 0.582 (6) |
H52C | 0.1085 | 0.2021 | 0.7468 | 0.060* | 0.582 (6) |
C53 | 0.08662 (15) | −0.0553 (3) | 0.6133 (3) | 0.0540 (8)* | 0.582 (6) |
H53A | 0.0674 | −0.0295 | 0.5613 | 0.081* | 0.582 (6) |
H53B | 0.0628 | −0.0898 | 0.6525 | 0.081* | 0.582 (6) |
H53C | 0.1139 | −0.0955 | 0.5900 | 0.081* | 0.582 (6) |
C54 | 0.14007 (18) | 0.0096 (3) | 0.7637 (3) | 0.0687 (11)* | 0.582 (6) |
H54A | 0.1630 | 0.0619 | 0.7716 | 0.103* | 0.582 (6) |
H54B | 0.1608 | −0.0460 | 0.7645 | 0.103* | 0.582 (6) |
H54C | 0.1148 | 0.0080 | 0.8141 | 0.103* | 0.582 (6) |
N50A | 0.12534 (19) | 0.0832 (4) | 0.6930 (4) | 0.0288 (12)* | 0.418 (6) |
C51A | 0.09864 (19) | 0.0542 (4) | 0.6194 (4) | 0.0220 (11)* | 0.418 (6) |
C54A | 0.13149 (13) | 0.1855 (3) | 0.6957 (2) | 0.0399 (7)* | 0.418 (6) |
H54D | 0.1505 | 0.2057 | 0.6409 | 0.060* | 0.418 (6) |
H54E | 0.1508 | 0.2027 | 0.7512 | 0.060* | 0.418 (6) |
H54F | 0.0971 | 0.2139 | 0.6968 | 0.060* | 0.418 (6) |
C52A | 0.08662 (15) | −0.0553 (3) | 0.6133 (3) | 0.0540 (8)* | 0.418 (6) |
H52D | 0.0592 | −0.0663 | 0.5679 | 0.081* | 0.418 (6) |
H52E | 0.0754 | −0.0773 | 0.6738 | 0.081* | 0.418 (6) |
H52F | 0.1182 | −0.0874 | 0.5946 | 0.081* | 0.418 (6) |
C53A | 0.14007 (18) | 0.0096 (3) | 0.7637 (3) | 0.0687 (11)* | 0.418 (6) |
H53D | 0.1085 | −0.0141 | 0.7927 | 0.103* | 0.418 (6) |
H53E | 0.1627 | 0.0358 | 0.8111 | 0.103* | 0.418 (6) |
H53F | 0.1584 | −0.0396 | 0.7323 | 0.103* | 0.418 (6) |
O70 | −0.02283 (6) | 0.19947 (13) | 0.54452 (11) | 0.0287 (4) | |
N70 | −0.07197 (7) | 0.15684 (15) | 0.66686 (13) | 0.0226 (5) | 0.937 (5) |
C70 | −0.06098 (8) | 0.21686 (17) | 0.59945 (15) | 0.0219 (5) | 0.937 (5) |
C71 | −0.03964 (10) | 0.07341 (19) | 0.6778 (2) | 0.0339 (11) | 0.937 (5) |
H71A | −0.0238 | 0.0578 | 0.6185 | 0.051* | 0.937 (5) |
H71B | −0.0617 | 0.0234 | 0.6986 | 0.051* | 0.937 (5) |
H71C | −0.0123 | 0.0845 | 0.7234 | 0.051* | 0.937 (5) |
C72 | −0.11259 (10) | 0.1742 (2) | 0.73816 (18) | 0.0386 (11) | 0.937 (5) |
H72A | −0.1241 | 0.2372 | 0.7341 | 0.058* | 0.937 (5) |
H72B | −0.0981 | 0.1628 | 0.7996 | 0.058* | 0.937 (5) |
H72C | −0.1422 | 0.1340 | 0.7276 | 0.058* | 0.937 (5) |
C73 | −0.09324 (8) | 0.30308 (16) | 0.58858 (17) | 0.0258 (8) | 0.937 (5) |
H73A | −0.0808 | 0.3489 | 0.6321 | 0.039* | 0.937 (5) |
H73B | −0.1298 | 0.2896 | 0.6013 | 0.039* | 0.937 (5) |
H73C | −0.0898 | 0.3259 | 0.5254 | 0.039* | 0.937 (5) |
N70A | −0.0839 (8) | 0.2074 (16) | 0.6484 (14) | 0.007 (4)* | 0.063 (5) |
C70A | −0.0444 (9) | 0.1529 (18) | 0.6214 (17) | 0.009 (4)* | 0.063 (5) |
C73A | −0.03964 (10) | 0.07341 (19) | 0.6778 (2) | 0.033 (13)* | 0.063 (5) |
H73D | −0.0225 | 0.0891 | 0.7359 | 0.049* | 0.063 (5) |
H73E | −0.0190 | 0.0279 | 0.6452 | 0.049* | 0.063 (5) |
H73F | −0.0742 | 0.0490 | 0.6907 | 0.049* | 0.063 (5) |
C71A | −0.11259 (10) | 0.1742 (2) | 0.73816 (18) | 0.028 (10)* | 0.063 (5) |
H71D | −0.1372 | 0.1263 | 0.7221 | 0.042* | 0.063 (5) |
H71E | −0.1313 | 0.2250 | 0.7660 | 0.042* | 0.063 (5) |
H71F | −0.0871 | 0.1508 | 0.7822 | 0.042* | 0.063 (5) |
C72A | −0.09324 (8) | 0.30308 (16) | 0.58858 (17) | 0.023 (9)* | 0.063 (5) |
H72D | −0.0668 | 0.3476 | 0.6060 | 0.035* | 0.063 (5) |
H72E | −0.1278 | 0.3273 | 0.6024 | 0.035* | 0.063 (5) |
H72F | −0.0906 | 0.2903 | 0.5224 | 0.035* | 0.063 (5) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe3 | 0.00779 (6) | 0.00993 (7) | 0.00838 (8) | 0.00066 (5) | −0.00005 (9) | 0.00045 (12) |
Fe4 | 0.00786 (7) | 0.00766 (8) | 0.00817 (9) | −0.00007 (6) | 0.00031 (6) | −0.00004 (6) |
Yb1 | 0.00773 (2) | 0.00794 (2) | 0.00950 (2) | −0.00058 (1) | −0.00043 (3) | −0.00033 (3) |
Yb2 | 0.00752 (2) | 0.01259 (2) | 0.00987 (2) | −0.00048 (2) | 0.00077 (3) | −0.00003 (3) |
C1 | 0.0111 (4) | 0.0125 (5) | 0.0169 (7) | 0.0010 (4) | 0.0011 (7) | −0.0024 (9) |
C1A | 0.0118 (4) | 0.0121 (5) | 0.0117 (7) | −0.0003 (4) | 0.0017 (5) | −0.0003 (6) |
C2 | 0.0131 (7) | 0.0154 (9) | 0.0132 (7) | −0.0002 (6) | 0.0000 (5) | 0.0025 (6) |
C2A | 0.0153 (6) | 0.0119 (7) | 0.0126 (6) | 0.0012 (5) | 0.0001 (5) | 0.0001 (6) |
C3 | 0.0145 (5) | 0.0141 (6) | 0.0138 (5) | 0.0012 (4) | −0.0003 (8) | 0.0006 (9) |
C3A | 0.0116 (5) | 0.0124 (6) | 0.0150 (7) | 0.0002 (5) | −0.0003 (4) | 0.0004 (5) |
C4 | 0.0135 (7) | 0.0176 (10) | 0.0135 (7) | 0.0007 (7) | 0.0005 (5) | −0.0009 (7) |
C4A | 0.0134 (6) | 0.0124 (7) | 0.0121 (6) | 0.0026 (5) | 0.0015 (5) | −0.0006 (6) |
C6 | 0.0112 (4) | 0.0129 (5) | 0.0115 (5) | 0.0008 (4) | −0.0009 (6) | 0.0003 (9) |
C6A | 0.0116 (5) | 0.0122 (6) | 0.0135 (8) | −0.0017 (4) | 0.0016 (5) | −0.0013 (5) |
C5 | 0.0128 (5) | 0.0150 (6) | 0.0200 (10) | −0.0001 (5) | 0.0007 (6) | −0.0002 (6) |
C5A | 0.0141 (6) | 0.0117 (7) | 0.0183 (7) | −0.0008 (5) | 0.0005 (5) | −0.0008 (6) |
C21 | 0.0125 (6) | 0.0181 (8) | 0.0145 (7) | −0.0013 (5) | −0.0017 (5) | 0.0013 (6) |
C22 | 0.0223 (9) | 0.0348 (13) | 0.0294 (11) | −0.0038 (8) | 0.0116 (8) | 0.0074 (9) |
C23 | 0.0305 (10) | 0.0168 (9) | 0.0299 (10) | 0.0010 (8) | 0.0045 (8) | 0.0027 (8) |
N1 | 0.0107 (4) | 0.0192 (6) | 0.0355 (8) | 0.0007 (4) | −0.0010 (8) | 0.0051 (11) |
N1A | 0.0183 (5) | 0.0119 (5) | 0.0198 (6) | 0.0010 (4) | 0.0019 (7) | 0.0004 (8) |
N2 | 0.0237 (8) | 0.0271 (10) | 0.0114 (6) | −0.0030 (7) | −0.0007 (6) | 0.0016 (6) |
N2A | 0.0262 (8) | 0.0223 (9) | 0.0133 (6) | 0.0048 (6) | −0.0007 (6) | 0.0007 (6) |
N3 | 0.0280 (6) | 0.0146 (6) | 0.0239 (7) | 0.0027 (5) | 0.0011 (9) | 0.0012 (9) |
N3A | 0.0128 (5) | 0.0183 (7) | 0.0307 (9) | −0.0010 (5) | −0.0009 (5) | 0.0038 (6) |
N4 | 0.0227 (8) | 0.0316 (11) | 0.0138 (7) | 0.0005 (8) | 0.0018 (6) | −0.0005 (7) |
N4A | 0.0219 (7) | 0.0256 (9) | 0.0126 (6) | 0.0045 (6) | 0.0014 (5) | −0.0005 (6) |
N6 | 0.0110 (4) | 0.0183 (6) | 0.0167 (5) | 0.0007 (4) | −0.0003 (7) | −0.0027 (9) |
N6A | 0.0122 (4) | 0.0186 (6) | 0.0171 (8) | −0.0034 (4) | 0.0027 (5) | −0.0020 (6) |
N5 | 0.0230 (7) | 0.0161 (7) | 0.0346 (11) | 0.0011 (5) | −0.0013 (6) | 0.0018 (7) |
N5A | 0.0263 (8) | 0.0126 (7) | 0.0361 (10) | 0.0013 (6) | 0.0010 (7) | −0.0005 (7) |
N20 | 0.0174 (6) | 0.0191 (8) | 0.0183 (7) | −0.0012 (6) | 0.0048 (5) | 0.0029 (6) |
O1 | 0.0224 (6) | 0.0165 (7) | 0.0089 (5) | −0.0069 (5) | −0.0011 (4) | 0.0006 (4) |
O2 | 0.0211 (6) | 0.0125 (6) | 0.0106 (5) | −0.0042 (5) | −0.0010 (4) | −0.0011 (4) |
O3 | 0.0098 (4) | 0.0152 (5) | 0.0505 (12) | −0.0016 (4) | −0.0057 (6) | 0.0054 (8) |
O4 | 0.0091 (4) | 0.0151 (6) | 0.0302 (7) | −0.0017 (4) | 0.0013 (4) | −0.0062 (5) |
O5 | 0.0213 (6) | 0.0173 (6) | 0.0111 (5) | 0.0025 (5) | 0.0025 (4) | −0.0014 (5) |
O6 | 0.0262 (6) | 0.0146 (6) | 0.0102 (5) | 0.0025 (5) | −0.0025 (5) | 0.0010 (4) |
O98 | 0.0140 (4) | 0.0105 (5) | 0.0249 (6) | −0.0001 (4) | −0.0021 (4) | 0.0013 (5) |
O20 | 0.0143 (6) | 0.0164 (7) | 0.0139 (6) | 0.0002 (5) | 0.0024 (4) | 0.0039 (5) |
C24 | 0.0175 (7) | 0.0183 (9) | 0.0262 (9) | 0.0005 (6) | 0.0024 (6) | −0.0057 (7) |
O99 | 0.0172 (6) | 0.0217 (7) | 0.0444 (10) | 0.0020 (5) | −0.0007 (6) | −0.0083 (7) |
O10 | 0.0250 (7) | 0.0145 (7) | 0.0151 (6) | −0.0028 (6) | −0.0057 (5) | −0.0048 (5) |
O60 | 0.0109 (6) | 0.0520 (14) | 0.0476 (11) | −0.0041 (8) | 0.0066 (6) | −0.0378 (10) |
O50 | 0.0237 (8) | 0.0299 (10) | 0.0282 (8) | −0.0004 (7) | −0.0067 (6) | 0.0140 (7) |
O70 | 0.0171 (6) | 0.0501 (11) | 0.0188 (6) | −0.0098 (6) | 0.0092 (5) | −0.0085 (7) |
N70 | 0.0183 (7) | 0.0313 (12) | 0.0182 (8) | −0.0078 (7) | 0.0069 (6) | −0.0061 (7) |
C70 | 0.0144 (7) | 0.0335 (12) | 0.0180 (9) | −0.0080 (7) | 0.0044 (6) | −0.0106 (8) |
C71 | 0.0327 (16) | 0.0329 (16) | 0.0360 (16) | −0.0045 (10) | 0.0035 (10) | 0.0019 (11) |
C72 | 0.0297 (13) | 0.062 (3) | 0.0243 (12) | −0.0119 (12) | 0.0166 (10) | −0.0098 (12) |
C73 | 0.0199 (10) | 0.0293 (14) | 0.0283 (13) | 0.0006 (8) | 0.0001 (8) | −0.0063 (9) |
Geometric parameters (Å, º) top
Fe3—C1 | 1.9187 (13) | O99—H99A | 0.965 (15) |
Fe3—C6 | 1.9296 (12) | O99—H99B | 0.969 (16) |
Fe3—C2 | 1.941 (2) | O10—C10 | 1.265 (3) |
Fe3—C3 | 1.9430 (15) | O10—C10A | 1.268 (5) |
Fe3—C4 | 1.944 (2) | N10—C10 | 1.321 (4) |
Fe3—C5 | 1.9494 (17) | N10—C11 | 1.478 (3) |
Fe4—C1A | 1.9265 (15) | N10—C12 | 1.497 (4) |
Fe4—C3A | 1.9326 (16) | C10—C13 | 1.516 (4) |
Fe4—C5A | 1.9329 (18) | C11—H11A | 0.9600 |
Fe4—C4A | 1.9370 (18) | C11—H11B | 0.9600 |
Fe4—C2A | 1.9418 (17) | C11—H11C | 0.9600 |
Fe4—C6A | 1.9440 (14) | C12—H12A | 0.9600 |
Yb1—O20 | 2.2154 (14) | C12—H12B | 0.9600 |
Yb1—O10 | 2.2293 (15) | C12—H12C | 0.9600 |
Yb1—O1 | 2.2836 (13) | C13—H13A | 0.9600 |
Yb1—O3 | 2.2866 (11) | C13—H13B | 0.9600 |
Yb1—O2 | 2.3143 (14) | C13—H13C | 0.9600 |
Yb1—N1A | 2.3535 (13) | N10A—C10A | 1.322 (7) |
Yb1—N6 | 2.3578 (11) | O60—C61 | 1.307 (4) |
Yb2—O50 | 2.1779 (18) | O60—C61A | 1.343 (4) |
Yb2—O70 | 2.1947 (14) | N60—C61 | 1.326 (4) |
Yb2—O60 | 2.2106 (18) | N60—C63 | 1.499 (4) |
Yb2—O6 | 2.2567 (13) | N60—C62 | 1.519 (4) |
Yb2—O4 | 2.3504 (13) | C61—C64 | 1.463 (4) |
Yb2—O5 | 2.3549 (14) | C62—H62A | 0.9600 |
Yb2—N6A | 2.4026 (13) | C62—H62B | 0.9600 |
C1—N1 | 1.1568 (18) | C62—H62C | 0.9600 |
C1A—N1A | 1.154 (2) | C63—H63A | 0.9600 |
C2—N2 | 1.155 (3) | C63—H63B | 0.9600 |
C2A—N2A | 1.157 (2) | C63—H63C | 0.9600 |
C3—N3 | 1.154 (2) | C64—H64A | 0.9600 |
C3A—N3A | 1.156 (2) | C64—H64B | 0.9600 |
C4—N4 | 1.151 (3) | C64—H64C | 0.9600 |
C4A—N4A | 1.158 (2) | N60A—C61A | 1.324 (6) |
C6—N6 | 1.1616 (17) | O50—C51 | 1.270 (4) |
C6A—N6A | 1.1538 (18) | O50—C51A | 1.294 (6) |
C5—N5 | 1.156 (2) | N50—C51 | 1.337 (6) |
C5A—N5A | 1.153 (2) | N50—C53 | 1.434 (5) |
C21—O20 | 1.263 (2) | N50—C54 | 1.569 (6) |
C21—N20 | 1.319 (3) | C51—C52 | 1.576 (5) |
C21—C24 | 1.492 (3) | C52—H52A | 0.9600 |
C22—N20 | 1.469 (3) | C52—H52B | 0.9600 |
C22—H22A | 0.9600 | C52—H52C | 0.9600 |
C22—H22B | 0.9600 | C53—H53A | 0.9600 |
C22—H22C | 0.9600 | C53—H53B | 0.9600 |
C23—N20 | 1.460 (3) | C53—H53C | 0.9600 |
C23—H23A | 0.9600 | C54—H54A | 0.9600 |
C23—H23B | 0.9600 | C54—H54B | 0.9600 |
C23—H23C | 0.9600 | C54—H54C | 0.9600 |
O1—H1A | 0.966 (3) | N50A—C51A | 1.313 (7) |
O1—H1B | 0.969 (13) | O70—C70 | 1.265 (2) |
O2—H2A | 0.970 (18) | O70—C70A | 1.39 (2) |
O2—H2B | 0.970 (18) | N70—C70 | 1.323 (3) |
O3—H3A | 0.968 (19) | N70—C72 | 1.463 (3) |
O3—H3B | 0.970 (14) | N70—C71 | 1.467 (4) |
O4—H4A | 0.968 (8) | C70—C73 | 1.499 (3) |
O4—H4B | 0.967 (9) | C71—H71A | 0.9600 |
O5—H5A | 0.971 (13) | C71—H71B | 0.9600 |
O5—H5B | 0.971 (7) | C71—H71C | 0.9600 |
O6—H6A | 0.972 (3) | C72—H72A | 0.9600 |
O6—H6B | 0.971 (15) | C72—H72B | 0.9600 |
O98—H98A | 0.969 (13) | C72—H72C | 0.9600 |
O98—H98B | 0.966 (7) | C73—H73A | 0.9600 |
C24—H24A | 0.9600 | C73—H73B | 0.9600 |
C24—H24B | 0.9600 | C73—H73C | 0.9600 |
C24—H24C | 0.9600 | N70A—C70A | 1.33 (3) |
| | | |
C1—Fe3—C6 | 178.80 (9) | Yb2—O6—H6B | 124.2 (12) |
C1—Fe3—C2 | 88.09 (9) | H6A—O6—H6B | 108.2 (16) |
C6—Fe3—C2 | 93.00 (9) | H98A—O98—H98B | 109.3 (14) |
C1—Fe3—C3 | 91.23 (6) | C21—O20—Yb1 | 149.72 (13) |
C6—Fe3—C3 | 89.33 (6) | C21—C24—H24A | 109.5 |
C2—Fe3—C3 | 86.68 (11) | C21—C24—H24B | 109.5 |
C1—Fe3—C4 | 89.17 (10) | H24A—C24—H24B | 109.5 |
C6—Fe3—C4 | 89.78 (9) | C21—C24—H24C | 109.5 |
C2—Fe3—C4 | 174.85 (7) | H24A—C24—H24C | 109.5 |
C3—Fe3—C4 | 89.02 (11) | H24B—C24—H24C | 109.5 |
C1—Fe3—C5 | 87.88 (6) | H99A—O99—H99B | 110.0 (16) |
C6—Fe3—C5 | 91.61 (6) | C10—O10—Yb1 | 158.73 (17) |
C2—Fe3—C5 | 90.29 (10) | C10A—O10—Yb1 | 138.9 (3) |
C3—Fe3—C5 | 176.87 (9) | C10—N10—C11 | 122.9 (2) |
C4—Fe3—C5 | 93.97 (10) | C10—N10—C12 | 116.3 (3) |
C1A—Fe4—C3A | 89.48 (6) | C11—N10—C12 | 120.7 (2) |
C1A—Fe4—C5A | 177.57 (7) | O10—C10—N10 | 120.1 (2) |
C3A—Fe4—C5A | 88.20 (7) | O10—C10—C13 | 125.2 (2) |
C1A—Fe4—C4A | 90.10 (8) | N10—C10—C13 | 114.7 (2) |
C3A—Fe4—C4A | 90.22 (7) | N10—C11—H11A | 109.5 |
C5A—Fe4—C4A | 89.19 (8) | N10—C11—H11B | 109.5 |
C1A—Fe4—C2A | 90.82 (8) | H11A—C11—H11B | 109.5 |
C3A—Fe4—C2A | 89.94 (7) | N10—C11—H11C | 109.5 |
C5A—Fe4—C2A | 89.89 (8) | H11A—C11—H11C | 109.5 |
C4A—Fe4—C2A | 179.07 (8) | H11B—C11—H11C | 109.5 |
C1A—Fe4—C6A | 89.31 (6) | N10—C12—H12A | 109.5 |
C3A—Fe4—C6A | 178.79 (7) | N10—C12—H12B | 109.5 |
C5A—Fe4—C6A | 93.01 (7) | H12A—C12—H12B | 109.5 |
C4A—Fe4—C6A | 89.75 (7) | N10—C12—H12C | 109.5 |
C2A—Fe4—C6A | 90.11 (7) | H12A—C12—H12C | 109.5 |
O20—Yb1—O10 | 130.54 (5) | H12B—C12—H12C | 109.5 |
O20—Yb1—O1 | 151.74 (6) | C10—C13—H13A | 109.5 |
O10—Yb1—O1 | 74.18 (6) | C10—C13—H13B | 109.5 |
O20—Yb1—O3 | 98.45 (7) | H13A—C13—H13B | 109.5 |
O10—Yb1—O3 | 110.43 (7) | C10—C13—H13C | 109.5 |
O1—Yb1—O3 | 81.28 (6) | H13A—C13—H13C | 109.5 |
O20—Yb1—O2 | 79.16 (6) | H13B—C13—H13C | 109.5 |
O10—Yb1—O2 | 143.42 (6) | O10—C10A—N10A | 118.1 (4) |
O1—Yb1—O2 | 72.95 (5) | C61—O60—C61A | 46.7 (2) |
O3—Yb1—O2 | 79.92 (5) | C61—O60—Yb2 | 139.21 (19) |
O20—Yb1—N1A | 77.26 (7) | C61A—O60—Yb2 | 140.4 (2) |
O10—Yb1—N1A | 73.72 (7) | C61—N60—C63 | 119.5 (3) |
O1—Yb1—N1A | 128.57 (6) | C61—N60—C62 | 119.0 (3) |
O3—Yb1—N1A | 73.73 (4) | C63—N60—C62 | 121.5 (2) |
O2—Yb1—N1A | 141.27 (6) | O60—C61—N60 | 111.3 (3) |
O20—Yb1—N6 | 79.59 (7) | O60—C61—C64 | 129.8 (3) |
O10—Yb1—N6 | 80.23 (7) | N60—C61—C64 | 118.8 (3) |
O1—Yb1—N6 | 94.07 (6) | N60—C62—H62A | 109.5 |
O3—Yb1—N6 | 166.39 (5) | N60—C62—H62B | 109.5 |
O2—Yb1—N6 | 86.50 (5) | H62A—C62—H62B | 109.5 |
N1A—Yb1—N6 | 118.45 (4) | N60—C62—H62C | 109.5 |
O50—Yb2—O70 | 83.77 (7) | H62A—C62—H62C | 109.5 |
O50—Yb2—O60 | 88.65 (7) | H62B—C62—H62C | 109.5 |
O70—Yb2—O60 | 139.27 (7) | N60—C63—H63A | 109.5 |
O50—Yb2—O6 | 172.33 (7) | N60—C63—H63B | 109.5 |
O70—Yb2—O6 | 95.85 (6) | H63A—C63—H63B | 109.5 |
O60—Yb2—O6 | 96.51 (8) | N60—C63—H63C | 109.5 |
O50—Yb2—O4 | 102.55 (7) | H63A—C63—H63C | 109.5 |
O70—Yb2—O4 | 71.83 (5) | H63B—C63—H63C | 109.5 |
O60—Yb2—O4 | 70.94 (6) | C61—C64—H64A | 109.5 |
O6—Yb2—O4 | 84.54 (5) | C61—C64—H64B | 109.5 |
O50—Yb2—O5 | 94.23 (7) | H64A—C64—H64B | 109.5 |
O70—Yb2—O5 | 73.89 (6) | C61—C64—H64C | 109.5 |
O60—Yb2—O5 | 146.74 (6) | H64A—C64—H64C | 109.5 |
O6—Yb2—O5 | 78.35 (5) | H64B—C64—H64C | 109.5 |
O4—Yb2—O5 | 139.63 (5) | N60A—C61A—O60 | 109.4 (4) |
O50—Yb2—N6A | 83.73 (6) | C51—O50—Yb2 | 149.9 (2) |
O70—Yb2—N6A | 144.41 (6) | C51A—O50—Yb2 | 173.4 (3) |
O60—Yb2—N6A | 73.43 (6) | C51—N50—C53 | 119.4 (4) |
O6—Yb2—N6A | 92.29 (5) | C51—N50—C54 | 112.8 (4) |
O4—Yb2—N6A | 143.59 (5) | C53—N50—C54 | 127.7 (4) |
O5—Yb2—N6A | 73.97 (5) | O50—C51—N50 | 115.1 (4) |
N1—C1—Fe3 | 178.82 (14) | O50—C51—C52 | 124.8 (3) |
N1A—C1A—Fe4 | 179.00 (15) | N50—C51—C52 | 120.0 (3) |
N2—C2—Fe3 | 176.1 (2) | C51—C52—H52A | 109.5 |
N2A—C2A—Fe4 | 179.26 (18) | C51—C52—H52B | 109.5 |
N3—C3—Fe3 | 177.0 (3) | H52A—C52—H52B | 109.5 |
N3A—C3A—Fe4 | 178.37 (16) | C51—C52—H52C | 109.5 |
N4—C4—Fe3 | 177.2 (2) | H52A—C52—H52C | 109.5 |
N4A—C4A—Fe4 | 178.46 (17) | H52B—C52—H52C | 109.5 |
N6—C6—Fe3 | 178.53 (13) | N50—C53—H53A | 109.5 |
N6A—C6A—Fe4 | 178.85 (15) | N50—C53—H53B | 109.5 |
N5—C5—Fe3 | 177.35 (18) | H53A—C53—H53B | 109.5 |
N5A—C5A—Fe4 | 178.37 (16) | N50—C53—H53C | 109.5 |
O20—C21—N20 | 120.88 (18) | H53A—C53—H53C | 109.5 |
O20—C21—C24 | 120.01 (18) | H53B—C53—H53C | 109.5 |
N20—C21—C24 | 119.11 (16) | N50—C54—H54A | 109.5 |
N20—C22—H22A | 109.5 | N50—C54—H54B | 109.5 |
N20—C22—H22B | 109.5 | H54A—C54—H54B | 109.5 |
H22A—C22—H22B | 109.5 | N50—C54—H54C | 109.5 |
N20—C22—H22C | 109.5 | H54A—C54—H54C | 109.5 |
H22A—C22—H22C | 109.5 | H54B—C54—H54C | 109.5 |
H22B—C22—H22C | 109.5 | O50—C51A—N50A | 118.5 (5) |
N20—C23—H23A | 109.5 | C70—O70—C70A | 46.9 (10) |
N20—C23—H23B | 109.5 | C70—O70—Yb2 | 166.50 (17) |
H23A—C23—H23B | 109.5 | C70A—O70—Yb2 | 142.5 (10) |
N20—C23—H23C | 109.5 | C70—N70—C72 | 122.3 (2) |
H23A—C23—H23C | 109.5 | C70—N70—C71 | 120.14 (19) |
H23B—C23—H23C | 109.5 | C72—N70—C71 | 117.3 (2) |
C1A—N1A—Yb1 | 173.94 (18) | O70—C70—N70 | 118.4 (2) |
C6—N6—Yb1 | 166.07 (12) | O70—C70—C73 | 121.1 (2) |
C6A—N6A—Yb2 | 169.72 (14) | N70—C70—C73 | 120.57 (19) |
C21—N20—C23 | 120.64 (16) | N70—C71—H71A | 109.5 |
C21—N20—C22 | 123.01 (19) | N70—C71—H71B | 109.5 |
C23—N20—C22 | 116.34 (18) | H71A—C71—H71B | 109.5 |
Yb1—O1—H1A | 131.1 (12) | N70—C71—H71C | 109.5 |
Yb1—O1—H1B | 117.2 (12) | H71A—C71—H71C | 109.5 |
H1A—O1—H1B | 109.6 (17) | H71B—C71—H71C | 109.5 |
Yb1—O2—H2A | 110.4 (15) | N70—C72—H72A | 109.5 |
Yb1—O2—H2B | 113.0 (14) | N70—C72—H72B | 109.5 |
H2A—O2—H2B | 108.8 (16) | H72A—C72—H72B | 109.5 |
Yb1—O3—H3A | 116.1 (14) | N70—C72—H72C | 109.5 |
Yb1—O3—H3B | 123.3 (13) | H72A—C72—H72C | 109.5 |
H3A—O3—H3B | 108.7 (16) | H72B—C72—H72C | 109.5 |
Yb2—O4—H4A | 117.0 (14) | C70—C73—H73A | 109.5 |
Yb2—O4—H4B | 118.7 (14) | C70—C73—H73B | 109.5 |
H4A—O4—H4B | 109.6 (16) | H73A—C73—H73B | 109.5 |
Yb2—O5—H5A | 120.9 (13) | C70—C73—H73C | 109.5 |
Yb2—O5—H5B | 119.9 (14) | H73A—C73—H73C | 109.5 |
H5A—O5—H5B | 108.5 (16) | H73B—C73—H73C | 109.5 |
Yb2—O6—H6A | 127.5 (12) | N70A—C70A—O70 | 103.3 (19) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1B···O98 | 0.97 (2) | 1.71 (2) | 2.6604 (19) | 167 (2) |
O1—H1A···N2Ai | 0.97 (1) | 1.78 (1) | 2.728 (2) | 168 (2) |
O2—H2B···O98 | 0.97 (2) | 1.76 (2) | 2.7154 (19) | 170 (2) |
O2—H2A···N4Aii | 0.97 (1) | 1.81 (1) | 2.721 (2) | 155 (2) |
O3—H3A···O99 | 0.97 (2) | 1.91 (2) | 2.714 (2) | 139 (2) |
O3—H3B···N1iii | 0.97 (2) | 1.86 (1) | 2.7821 (18) | 158 (2) |
O4—H4A···N5iv | 0.97 (1) | 1.96 (1) | 2.914 (2) | 169 (2) |
O4—H4B···N3Av | 0.97 (1) | 1.91 (1) | 2.8567 (19) | 167 (2) |
O5—H5B···N2vi | 0.97 (1) | 1.82 (1) | 2.775 (2) | 169 (2) |
O5—H5A···N3 | 0.97 (1) | 1.96 (1) | 2.889 (2) | 159 (2) |
O6—H6B···N3 | 0.97 (2) | 1.96 (1) | 2.855 (2) | 153 (2) |
O6—H6A···N4vii | 0.97 (1) | 1.74 (1) | 2.708 (2) | 180 (2) |
O98—H98B···N5Aviii | 0.97 (1) | 1.74 (1) | 2.695 (2) | 169 (2) |
O98—H98A···N1iii | 0.97 (1) | 1.84 (1) | 2.7718 (19) | 162 (2) |
O99—H99A···N3A | 0.97 (2) | 2.01 (2) | 2.961 (2) | 170 (2) |
O99—H99B···N5iii | 0.97 (2) | 2.23 (1) | 3.094 (2) | 148 (2) |
Symmetry codes: (i) −x+1/2, y+1/2, z−1/2; (ii) −x+1/2, y+1/2, z+1/2; (iii) x+1/2, −y+3/2, z; (iv) x, y−1, z; (v) x−1/2, −y+1/2, z; (vi) −x, −y+1, z+1/2; (vii) −x, −y+1, z−1/2; (viii) x, y+1, z. |