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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680600883X/om2005sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680600883X/om2005Isup2.hkl
Contains datablock I

CCDC reference: 605145

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](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

Computing details top

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-1κ3O,3κ3O-tri-µ-cyano-1:2κ2N:C;2:3κ2C:N;3:4κ2N:C- nonacyano-2κ4C,4κ5C-pentakis(N,N-dimethylacetamide)-1κ3O,3κ2O- diiron(III)diytterbium(III) dihydrate top
Crystal data top
[Fe2Yb2(CN)12(C4H9NO)5(H2O)6]·2H2OF(000) = 2672
Mr = 1349.76Dx = 1.725 Mg m3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2nCell parameters from 9695 reflections
a = 25.2387 (9) Åθ = 5.7–85.4°
b = 14.4943 (6) ŵ = 4.18 mm1
c = 14.2058 (5) ÅT = 100 K
V = 5196.7 (3) Å3Block, yellow
Z = 40.20 × 0.15 × 0.10 mm
Data collection top
Bruker X8 APEXII
diffractometer
37796 independent reflections
Radiation source: fine-focus sealed tube32727 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
Detector resolution: 83.33 pixels mm-1θmax = 43.3°, θmin = 1.6°
φ and ω scansh = 3748
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 2727
Tmin = 0.45, Tmax = 0.66l = 2727
271064 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H 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 reflectionsΔρmax = 2.36 e Å3
607 parametersΔρmin = 1.51 e Å3
25 restraintsAbsolute structure: Flack (1983), with 17930 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute 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
xyzUiso*/UeqOcc. (<1)
Fe30.006526 (7)0.698941 (13)0.44633 (2)0.00870 (3)
Fe40.256330 (8)0.303175 (16)0.431182 (15)0.00790 (4)
Yb10.206811 (2)0.667222 (4)0.447156 (6)0.00839 (1)
Yb20.047075 (2)0.204152 (4)0.452747 (5)0.00999 (1)
C10.08253 (5)0.69562 (10)0.44650 (17)0.0135 (2)
C1A0.24021 (5)0.43272 (10)0.44113 (14)0.0119 (3)
C20.00903 (8)0.68828 (17)0.31024 (14)0.0139 (3)
C2A0.26033 (7)0.29269 (12)0.56727 (12)0.0133 (3)
C30.00294 (5)0.56506 (10)0.44909 (18)0.0141 (2)
C3A0.33094 (6)0.33289 (12)0.42678 (11)0.0130 (3)
C40.00755 (8)0.69927 (17)0.58317 (14)0.0149 (3)
C4A0.25240 (7)0.31147 (13)0.29527 (12)0.0126 (3)
C60.06987 (5)0.70365 (9)0.44865 (15)0.0118 (2)
C6A0.18094 (6)0.27605 (11)0.43574 (11)0.0124 (3)
C50.01132 (6)0.83282 (12)0.43639 (15)0.0159 (3)
C5A0.27547 (7)0.17457 (12)0.41935 (13)0.0147 (3)
C210.15301 (6)0.61926 (13)0.65846 (12)0.0151 (3)
C220.10039 (8)0.53172 (19)0.77270 (17)0.0288 (5)
H22A0.10770.57690.82040.043*
H22B0.10220.47110.79970.043*
H22C0.06560.54190.74760.043*
C230.16309 (9)0.45365 (15)0.66348 (17)0.0257 (4)
H23A0.19010.46710.61790.039*
H23B0.13610.41620.63500.039*
H23C0.17840.42100.71560.039*
N10.12836 (5)0.69524 (10)0.44684 (19)0.0218 (3)
N1A0.23131 (5)0.51055 (9)0.44746 (16)0.0167 (2)
N20.01323 (9)0.67942 (16)0.22977 (13)0.0207 (4)
N2A0.26313 (7)0.28571 (13)0.64822 (12)0.0206 (3)
N30.00014 (6)0.48563 (10)0.44660 (18)0.0221 (3)
N3A0.37526 (6)0.35284 (12)0.42379 (12)0.0206 (3)
N40.00874 (8)0.69576 (17)0.66406 (13)0.0227 (4)
N4A0.25084 (7)0.31478 (14)0.21390 (12)0.0201 (3)
N60.11588 (4)0.70442 (9)0.45014 (16)0.0153 (2)
N6A0.13601 (5)0.26147 (11)0.43810 (12)0.0160 (3)
N50.01555 (7)0.91181 (12)0.42768 (13)0.0246 (4)
N5A0.28814 (7)0.09847 (12)0.41233 (15)0.0250 (4)
N200.13971 (6)0.53976 (13)0.69689 (12)0.0183 (3)
O10.22730 (6)0.77855 (10)0.33939 (9)0.0159 (2)
H1A0.2255 (9)0.7784 (16)0.2715 (2)0.019*
H1B0.2498 (8)0.8287 (12)0.3603 (13)0.019*
O20.22021 (5)0.80284 (10)0.52979 (9)0.0147 (2)
H2A0.2346 (8)0.7898 (16)0.5917 (8)0.018*
H2B0.2437 (7)0.8454 (14)0.4976 (13)0.018*
O30.29702 (4)0.66422 (9)0.46166 (16)0.0252 (4)
H3A0.3114 (9)0.6155 (10)0.5005 (16)0.030*
H3B0.3184 (8)0.7192 (8)0.4701 (19)0.030*
O40.01636 (5)0.10780 (10)0.38197 (11)0.0181 (3)
H4A0.0124 (8)0.0420 (4)0.3915 (18)0.022*
H4B0.0534 (3)0.1244 (13)0.3867 (19)0.022*
O50.05126 (5)0.33740 (10)0.54731 (9)0.0166 (2)
H5A0.0395 (9)0.3968 (8)0.5234 (14)0.020*
H5B0.0424 (10)0.3337 (15)0.6137 (5)0.020*
O60.01503 (6)0.31275 (10)0.35417 (9)0.0170 (2)
H6A0.0128 (10)0.3098 (15)0.2859 (3)0.020*
H6B0.0007 (9)0.3705 (9)0.3746 (13)0.020*
O980.28225 (5)0.91301 (9)0.42138 (10)0.0165 (2)
H98A0.3152 (4)0.8844 (11)0.441 (2)0.020*
H98B0.2879 (7)0.9783 (4)0.4122 (18)0.020*
O200.18601 (6)0.62270 (12)0.59169 (10)0.0149 (3)
C240.12900 (7)0.70600 (14)0.69564 (15)0.0207 (4)
H24A0.14590.75820.66690.031*
H24B0.13380.70870.76260.031*
H24C0.09180.70690.68130.031*
O990.37355 (6)0.54030 (12)0.50654 (13)0.0277 (3)
H99A0.3761 (9)0.4822 (9)0.4736 (17)0.033*
H99B0.4041 (6)0.5783 (13)0.4924 (18)0.033*
O100.18233 (7)0.61067 (12)0.30785 (11)0.0182 (3)
N100.14137 (9)0.50361 (18)0.22049 (17)0.0166 (5)*0.667 (5)
C100.18218 (10)0.55841 (19)0.23655 (18)0.0142 (5)*0.667 (5)
C110.13814 (9)0.44220 (17)0.13759 (17)0.0273 (4)*0.667 (5)
H11A0.14040.47840.08110.041*0.667 (5)
H11B0.10510.40950.13860.041*0.667 (5)
H11C0.16690.39890.13920.041*0.667 (5)
C120.09920 (13)0.5018 (3)0.2945 (2)0.0501 (8)*0.667 (5)
H12A0.10230.44610.33070.075*0.667 (5)
H12B0.06500.50400.26510.075*0.667 (5)
H12C0.10330.55420.33530.075*0.667 (5)
C130.22585 (11)0.5530 (2)0.1635 (2)0.0369 (6)*0.667 (5)
H13A0.25060.60230.17360.055*0.667 (5)
H13B0.21080.55850.10170.055*0.667 (5)
H13C0.24380.49490.16890.055*0.667 (5)
N10A0.17024 (19)0.5109 (4)0.1910 (3)0.0168 (10)*0.333 (5)
C10A0.15679 (18)0.5426 (4)0.2750 (3)0.0125 (9)*0.333 (5)
C12A0.13814 (9)0.44220 (17)0.13759 (17)0.0273 (4)*0.333 (5)
H12D0.11090.41770.17770.041*0.333 (5)
H12E0.16070.39300.11660.041*0.333 (5)
H12F0.12220.47170.08410.041*0.333 (5)
C13A0.09920 (13)0.5018 (3)0.2945 (2)0.0501 (8)*0.333 (5)
H13D0.09060.50910.35990.075*0.333 (5)
H13E0.09860.43750.27850.075*0.333 (5)
H13F0.07370.53430.25690.075*0.333 (5)
C11A0.22585 (11)0.5530 (2)0.1635 (2)0.0369 (6)*0.333 (5)
H11D0.23760.59380.21250.055*0.333 (5)
H11E0.22260.58680.10560.055*0.333 (5)
H11F0.25110.50410.15560.055*0.333 (5)
O600.08617 (7)0.11926 (18)0.34371 (15)0.0368 (6)
N600.15366 (11)0.1048 (2)0.2498 (2)0.0166 (6)*0.554 (5)
C610.13126 (12)0.0773 (2)0.3294 (2)0.0147 (6)*0.554 (5)
C620.12683 (10)0.1798 (2)0.19222 (19)0.0273 (5)*0.554 (5)
H62A0.09950.15290.15410.041*0.554 (5)
H62B0.15250.20910.15240.041*0.554 (5)
H62C0.11160.22470.23380.041*0.554 (5)
C630.20506 (10)0.0625 (2)0.21932 (19)0.0329 (5)*0.554 (5)
H63A0.21680.01930.26620.049*0.554 (5)
H63B0.23120.11000.21170.049*0.554 (5)
H63C0.20010.03100.16050.049*0.554 (5)
C640.15882 (9)0.00915 (18)0.38757 (17)0.0283 (4)*0.554 (5)
H64A0.18650.03900.42250.042*0.554 (5)
H64B0.17390.03760.34790.042*0.554 (5)
H64C0.13410.01870.43040.042*0.554 (5)
N60A0.16084 (15)0.0639 (3)0.2918 (3)0.0204 (8)*0.446 (5)
C61A0.12333 (15)0.1259 (3)0.2764 (3)0.0148 (8)*0.446 (5)
C64A0.12683 (10)0.1798 (2)0.19222 (19)0.0273 (5)*0.446 (5)
H64D0.15800.21760.19460.041*0.446 (5)
H64E0.09610.21830.18690.041*0.446 (5)
H64F0.12880.13950.13870.041*0.446 (5)
C62A0.20506 (10)0.0625 (2)0.21932 (19)0.0329 (5)*0.446 (5)
H62D0.19300.03140.16360.049*0.446 (5)
H62E0.23510.03050.24470.049*0.446 (5)
H62F0.21490.12460.20390.049*0.446 (5)
C63A0.15882 (9)0.00915 (18)0.38757 (17)0.0283 (4)*0.446 (5)
H63D0.17740.04320.43520.042*0.446 (5)
H63E0.17520.05010.37950.042*0.446 (5)
H63F0.12260.00090.40640.042*0.446 (5)
O500.08175 (7)0.11465 (15)0.55938 (13)0.0273 (4)
N500.11019 (16)0.0176 (3)0.6672 (3)0.0360 (10)*0.582 (6)
C510.10565 (14)0.1047 (3)0.6374 (3)0.0213 (8)*0.582 (6)
C520.13149 (13)0.1855 (3)0.6957 (2)0.0399 (7)*0.582 (6)
H52A0.13670.23800.65560.060*0.582 (6)
H52B0.16500.16570.72030.060*0.582 (6)
H52C0.10850.20210.74680.060*0.582 (6)
C530.08662 (15)0.0553 (3)0.6133 (3)0.0540 (8)*0.582 (6)
H53A0.06740.02950.56130.081*0.582 (6)
H53B0.06280.08980.65250.081*0.582 (6)
H53C0.11390.09550.59000.081*0.582 (6)
C540.14007 (18)0.0096 (3)0.7637 (3)0.0687 (11)*0.582 (6)
H54A0.16300.06190.77160.103*0.582 (6)
H54B0.16080.04600.76450.103*0.582 (6)
H54C0.11480.00800.81410.103*0.582 (6)
N50A0.12534 (19)0.0832 (4)0.6930 (4)0.0288 (12)*0.418 (6)
C51A0.09864 (19)0.0542 (4)0.6194 (4)0.0220 (11)*0.418 (6)
C54A0.13149 (13)0.1855 (3)0.6957 (2)0.0399 (7)*0.418 (6)
H54D0.15050.20570.64090.060*0.418 (6)
H54E0.15080.20270.75120.060*0.418 (6)
H54F0.09710.21390.69680.060*0.418 (6)
C52A0.08662 (15)0.0553 (3)0.6133 (3)0.0540 (8)*0.418 (6)
H52D0.05920.06630.56790.081*0.418 (6)
H52E0.07540.07730.67380.081*0.418 (6)
H52F0.11820.08740.59460.081*0.418 (6)
C53A0.14007 (18)0.0096 (3)0.7637 (3)0.0687 (11)*0.418 (6)
H53D0.10850.01410.79270.103*0.418 (6)
H53E0.16270.03580.81110.103*0.418 (6)
H53F0.15840.03960.73230.103*0.418 (6)
O700.02283 (6)0.19947 (13)0.54452 (11)0.0287 (4)
N700.07197 (7)0.15684 (15)0.66686 (13)0.0226 (5)0.937 (5)
C700.06098 (8)0.21686 (17)0.59945 (15)0.0219 (5)0.937 (5)
C710.03964 (10)0.07341 (19)0.6778 (2)0.0339 (11)0.937 (5)
H71A0.02380.05780.61850.051*0.937 (5)
H71B0.06170.02340.69860.051*0.937 (5)
H71C0.01230.08450.72340.051*0.937 (5)
C720.11259 (10)0.1742 (2)0.73816 (18)0.0386 (11)0.937 (5)
H72A0.12410.23720.73410.058*0.937 (5)
H72B0.09810.16280.79960.058*0.937 (5)
H72C0.14220.13400.72760.058*0.937 (5)
C730.09324 (8)0.30308 (16)0.58858 (17)0.0258 (8)0.937 (5)
H73A0.08080.34890.63210.039*0.937 (5)
H73B0.12980.28960.60130.039*0.937 (5)
H73C0.08980.32590.52540.039*0.937 (5)
N70A0.0839 (8)0.2074 (16)0.6484 (14)0.007 (4)*0.063 (5)
C70A0.0444 (9)0.1529 (18)0.6214 (17)0.009 (4)*0.063 (5)
C73A0.03964 (10)0.07341 (19)0.6778 (2)0.033 (13)*0.063 (5)
H73D0.02250.08910.73590.049*0.063 (5)
H73E0.01900.02790.64520.049*0.063 (5)
H73F0.07420.04900.69070.049*0.063 (5)
C71A0.11259 (10)0.1742 (2)0.73816 (18)0.028 (10)*0.063 (5)
H71D0.13720.12630.72210.042*0.063 (5)
H71E0.13130.22500.76600.042*0.063 (5)
H71F0.08710.15080.78220.042*0.063 (5)
C72A0.09324 (8)0.30308 (16)0.58858 (17)0.023 (9)*0.063 (5)
H72D0.06680.34760.60600.035*0.063 (5)
H72E0.12780.32730.60240.035*0.063 (5)
H72F0.09060.29030.52240.035*0.063 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe30.00779 (6)0.00993 (7)0.00838 (8)0.00066 (5)0.00005 (9)0.00045 (12)
Fe40.00786 (7)0.00766 (8)0.00817 (9)0.00007 (6)0.00031 (6)0.00004 (6)
Yb10.00773 (2)0.00794 (2)0.00950 (2)0.00058 (1)0.00043 (3)0.00033 (3)
Yb20.00752 (2)0.01259 (2)0.00987 (2)0.00048 (2)0.00077 (3)0.00003 (3)
C10.0111 (4)0.0125 (5)0.0169 (7)0.0010 (4)0.0011 (7)0.0024 (9)
C1A0.0118 (4)0.0121 (5)0.0117 (7)0.0003 (4)0.0017 (5)0.0003 (6)
C20.0131 (7)0.0154 (9)0.0132 (7)0.0002 (6)0.0000 (5)0.0025 (6)
C2A0.0153 (6)0.0119 (7)0.0126 (6)0.0012 (5)0.0001 (5)0.0001 (6)
C30.0145 (5)0.0141 (6)0.0138 (5)0.0012 (4)0.0003 (8)0.0006 (9)
C3A0.0116 (5)0.0124 (6)0.0150 (7)0.0002 (5)0.0003 (4)0.0004 (5)
C40.0135 (7)0.0176 (10)0.0135 (7)0.0007 (7)0.0005 (5)0.0009 (7)
C4A0.0134 (6)0.0124 (7)0.0121 (6)0.0026 (5)0.0015 (5)0.0006 (6)
C60.0112 (4)0.0129 (5)0.0115 (5)0.0008 (4)0.0009 (6)0.0003 (9)
C6A0.0116 (5)0.0122 (6)0.0135 (8)0.0017 (4)0.0016 (5)0.0013 (5)
C50.0128 (5)0.0150 (6)0.0200 (10)0.0001 (5)0.0007 (6)0.0002 (6)
C5A0.0141 (6)0.0117 (7)0.0183 (7)0.0008 (5)0.0005 (5)0.0008 (6)
C210.0125 (6)0.0181 (8)0.0145 (7)0.0013 (5)0.0017 (5)0.0013 (6)
C220.0223 (9)0.0348 (13)0.0294 (11)0.0038 (8)0.0116 (8)0.0074 (9)
C230.0305 (10)0.0168 (9)0.0299 (10)0.0010 (8)0.0045 (8)0.0027 (8)
N10.0107 (4)0.0192 (6)0.0355 (8)0.0007 (4)0.0010 (8)0.0051 (11)
N1A0.0183 (5)0.0119 (5)0.0198 (6)0.0010 (4)0.0019 (7)0.0004 (8)
N20.0237 (8)0.0271 (10)0.0114 (6)0.0030 (7)0.0007 (6)0.0016 (6)
N2A0.0262 (8)0.0223 (9)0.0133 (6)0.0048 (6)0.0007 (6)0.0007 (6)
N30.0280 (6)0.0146 (6)0.0239 (7)0.0027 (5)0.0011 (9)0.0012 (9)
N3A0.0128 (5)0.0183 (7)0.0307 (9)0.0010 (5)0.0009 (5)0.0038 (6)
N40.0227 (8)0.0316 (11)0.0138 (7)0.0005 (8)0.0018 (6)0.0005 (7)
N4A0.0219 (7)0.0256 (9)0.0126 (6)0.0045 (6)0.0014 (5)0.0005 (6)
N60.0110 (4)0.0183 (6)0.0167 (5)0.0007 (4)0.0003 (7)0.0027 (9)
N6A0.0122 (4)0.0186 (6)0.0171 (8)0.0034 (4)0.0027 (5)0.0020 (6)
N50.0230 (7)0.0161 (7)0.0346 (11)0.0011 (5)0.0013 (6)0.0018 (7)
N5A0.0263 (8)0.0126 (7)0.0361 (10)0.0013 (6)0.0010 (7)0.0005 (7)
N200.0174 (6)0.0191 (8)0.0183 (7)0.0012 (6)0.0048 (5)0.0029 (6)
O10.0224 (6)0.0165 (7)0.0089 (5)0.0069 (5)0.0011 (4)0.0006 (4)
O20.0211 (6)0.0125 (6)0.0106 (5)0.0042 (5)0.0010 (4)0.0011 (4)
O30.0098 (4)0.0152 (5)0.0505 (12)0.0016 (4)0.0057 (6)0.0054 (8)
O40.0091 (4)0.0151 (6)0.0302 (7)0.0017 (4)0.0013 (4)0.0062 (5)
O50.0213 (6)0.0173 (6)0.0111 (5)0.0025 (5)0.0025 (4)0.0014 (5)
O60.0262 (6)0.0146 (6)0.0102 (5)0.0025 (5)0.0025 (5)0.0010 (4)
O980.0140 (4)0.0105 (5)0.0249 (6)0.0001 (4)0.0021 (4)0.0013 (5)
O200.0143 (6)0.0164 (7)0.0139 (6)0.0002 (5)0.0024 (4)0.0039 (5)
C240.0175 (7)0.0183 (9)0.0262 (9)0.0005 (6)0.0024 (6)0.0057 (7)
O990.0172 (6)0.0217 (7)0.0444 (10)0.0020 (5)0.0007 (6)0.0083 (7)
O100.0250 (7)0.0145 (7)0.0151 (6)0.0028 (6)0.0057 (5)0.0048 (5)
O600.0109 (6)0.0520 (14)0.0476 (11)0.0041 (8)0.0066 (6)0.0378 (10)
O500.0237 (8)0.0299 (10)0.0282 (8)0.0004 (7)0.0067 (6)0.0140 (7)
O700.0171 (6)0.0501 (11)0.0188 (6)0.0098 (6)0.0092 (5)0.0085 (7)
N700.0183 (7)0.0313 (12)0.0182 (8)0.0078 (7)0.0069 (6)0.0061 (7)
C700.0144 (7)0.0335 (12)0.0180 (9)0.0080 (7)0.0044 (6)0.0106 (8)
C710.0327 (16)0.0329 (16)0.0360 (16)0.0045 (10)0.0035 (10)0.0019 (11)
C720.0297 (13)0.062 (3)0.0243 (12)0.0119 (12)0.0166 (10)0.0098 (12)
C730.0199 (10)0.0293 (14)0.0283 (13)0.0006 (8)0.0001 (8)0.0063 (9)
Geometric parameters (Å, º) top
Fe3—C11.9187 (13)O99—H99A0.965 (15)
Fe3—C61.9296 (12)O99—H99B0.969 (16)
Fe3—C21.941 (2)O10—C101.265 (3)
Fe3—C31.9430 (15)O10—C10A1.268 (5)
Fe3—C41.944 (2)N10—C101.321 (4)
Fe3—C51.9494 (17)N10—C111.478 (3)
Fe4—C1A1.9265 (15)N10—C121.497 (4)
Fe4—C3A1.9326 (16)C10—C131.516 (4)
Fe4—C5A1.9329 (18)C11—H11A0.9600
Fe4—C4A1.9370 (18)C11—H11B0.9600
Fe4—C2A1.9418 (17)C11—H11C0.9600
Fe4—C6A1.9440 (14)C12—H12A0.9600
Yb1—O202.2154 (14)C12—H12B0.9600
Yb1—O102.2293 (15)C12—H12C0.9600
Yb1—O12.2836 (13)C13—H13A0.9600
Yb1—O32.2866 (11)C13—H13B0.9600
Yb1—O22.3143 (14)C13—H13C0.9600
Yb1—N1A2.3535 (13)N10A—C10A1.322 (7)
Yb1—N62.3578 (11)O60—C611.307 (4)
Yb2—O502.1779 (18)O60—C61A1.343 (4)
Yb2—O702.1947 (14)N60—C611.326 (4)
Yb2—O602.2106 (18)N60—C631.499 (4)
Yb2—O62.2567 (13)N60—C621.519 (4)
Yb2—O42.3504 (13)C61—C641.463 (4)
Yb2—O52.3549 (14)C62—H62A0.9600
Yb2—N6A2.4026 (13)C62—H62B0.9600
C1—N11.1568 (18)C62—H62C0.9600
C1A—N1A1.154 (2)C63—H63A0.9600
C2—N21.155 (3)C63—H63B0.9600
C2A—N2A1.157 (2)C63—H63C0.9600
C3—N31.154 (2)C64—H64A0.9600
C3A—N3A1.156 (2)C64—H64B0.9600
C4—N41.151 (3)C64—H64C0.9600
C4A—N4A1.158 (2)N60A—C61A1.324 (6)
C6—N61.1616 (17)O50—C511.270 (4)
C6A—N6A1.1538 (18)O50—C51A1.294 (6)
C5—N51.156 (2)N50—C511.337 (6)
C5A—N5A1.153 (2)N50—C531.434 (5)
C21—O201.263 (2)N50—C541.569 (6)
C21—N201.319 (3)C51—C521.576 (5)
C21—C241.492 (3)C52—H52A0.9600
C22—N201.469 (3)C52—H52B0.9600
C22—H22A0.9600C52—H52C0.9600
C22—H22B0.9600C53—H53A0.9600
C22—H22C0.9600C53—H53B0.9600
C23—N201.460 (3)C53—H53C0.9600
C23—H23A0.9600C54—H54A0.9600
C23—H23B0.9600C54—H54B0.9600
C23—H23C0.9600C54—H54C0.9600
O1—H1A0.966 (3)N50A—C51A1.313 (7)
O1—H1B0.969 (13)O70—C701.265 (2)
O2—H2A0.970 (18)O70—C70A1.39 (2)
O2—H2B0.970 (18)N70—C701.323 (3)
O3—H3A0.968 (19)N70—C721.463 (3)
O3—H3B0.970 (14)N70—C711.467 (4)
O4—H4A0.968 (8)C70—C731.499 (3)
O4—H4B0.967 (9)C71—H71A0.9600
O5—H5A0.971 (13)C71—H71B0.9600
O5—H5B0.971 (7)C71—H71C0.9600
O6—H6A0.972 (3)C72—H72A0.9600
O6—H6B0.971 (15)C72—H72B0.9600
O98—H98A0.969 (13)C72—H72C0.9600
O98—H98B0.966 (7)C73—H73A0.9600
C24—H24A0.9600C73—H73B0.9600
C24—H24B0.9600C73—H73C0.9600
C24—H24C0.9600N70A—C70A1.33 (3)
C1—Fe3—C6178.80 (9)Yb2—O6—H6B124.2 (12)
C1—Fe3—C288.09 (9)H6A—O6—H6B108.2 (16)
C6—Fe3—C293.00 (9)H98A—O98—H98B109.3 (14)
C1—Fe3—C391.23 (6)C21—O20—Yb1149.72 (13)
C6—Fe3—C389.33 (6)C21—C24—H24A109.5
C2—Fe3—C386.68 (11)C21—C24—H24B109.5
C1—Fe3—C489.17 (10)H24A—C24—H24B109.5
C6—Fe3—C489.78 (9)C21—C24—H24C109.5
C2—Fe3—C4174.85 (7)H24A—C24—H24C109.5
C3—Fe3—C489.02 (11)H24B—C24—H24C109.5
C1—Fe3—C587.88 (6)H99A—O99—H99B110.0 (16)
C6—Fe3—C591.61 (6)C10—O10—Yb1158.73 (17)
C2—Fe3—C590.29 (10)C10A—O10—Yb1138.9 (3)
C3—Fe3—C5176.87 (9)C10—N10—C11122.9 (2)
C4—Fe3—C593.97 (10)C10—N10—C12116.3 (3)
C1A—Fe4—C3A89.48 (6)C11—N10—C12120.7 (2)
C1A—Fe4—C5A177.57 (7)O10—C10—N10120.1 (2)
C3A—Fe4—C5A88.20 (7)O10—C10—C13125.2 (2)
C1A—Fe4—C4A90.10 (8)N10—C10—C13114.7 (2)
C3A—Fe4—C4A90.22 (7)N10—C11—H11A109.5
C5A—Fe4—C4A89.19 (8)N10—C11—H11B109.5
C1A—Fe4—C2A90.82 (8)H11A—C11—H11B109.5
C3A—Fe4—C2A89.94 (7)N10—C11—H11C109.5
C5A—Fe4—C2A89.89 (8)H11A—C11—H11C109.5
C4A—Fe4—C2A179.07 (8)H11B—C11—H11C109.5
C1A—Fe4—C6A89.31 (6)N10—C12—H12A109.5
C3A—Fe4—C6A178.79 (7)N10—C12—H12B109.5
C5A—Fe4—C6A93.01 (7)H12A—C12—H12B109.5
C4A—Fe4—C6A89.75 (7)N10—C12—H12C109.5
C2A—Fe4—C6A90.11 (7)H12A—C12—H12C109.5
O20—Yb1—O10130.54 (5)H12B—C12—H12C109.5
O20—Yb1—O1151.74 (6)C10—C13—H13A109.5
O10—Yb1—O174.18 (6)C10—C13—H13B109.5
O20—Yb1—O398.45 (7)H13A—C13—H13B109.5
O10—Yb1—O3110.43 (7)C10—C13—H13C109.5
O1—Yb1—O381.28 (6)H13A—C13—H13C109.5
O20—Yb1—O279.16 (6)H13B—C13—H13C109.5
O10—Yb1—O2143.42 (6)O10—C10A—N10A118.1 (4)
O1—Yb1—O272.95 (5)C61—O60—C61A46.7 (2)
O3—Yb1—O279.92 (5)C61—O60—Yb2139.21 (19)
O20—Yb1—N1A77.26 (7)C61A—O60—Yb2140.4 (2)
O10—Yb1—N1A73.72 (7)C61—N60—C63119.5 (3)
O1—Yb1—N1A128.57 (6)C61—N60—C62119.0 (3)
O3—Yb1—N1A73.73 (4)C63—N60—C62121.5 (2)
O2—Yb1—N1A141.27 (6)O60—C61—N60111.3 (3)
O20—Yb1—N679.59 (7)O60—C61—C64129.8 (3)
O10—Yb1—N680.23 (7)N60—C61—C64118.8 (3)
O1—Yb1—N694.07 (6)N60—C62—H62A109.5
O3—Yb1—N6166.39 (5)N60—C62—H62B109.5
O2—Yb1—N686.50 (5)H62A—C62—H62B109.5
N1A—Yb1—N6118.45 (4)N60—C62—H62C109.5
O50—Yb2—O7083.77 (7)H62A—C62—H62C109.5
O50—Yb2—O6088.65 (7)H62B—C62—H62C109.5
O70—Yb2—O60139.27 (7)N60—C63—H63A109.5
O50—Yb2—O6172.33 (7)N60—C63—H63B109.5
O70—Yb2—O695.85 (6)H63A—C63—H63B109.5
O60—Yb2—O696.51 (8)N60—C63—H63C109.5
O50—Yb2—O4102.55 (7)H63A—C63—H63C109.5
O70—Yb2—O471.83 (5)H63B—C63—H63C109.5
O60—Yb2—O470.94 (6)C61—C64—H64A109.5
O6—Yb2—O484.54 (5)C61—C64—H64B109.5
O50—Yb2—O594.23 (7)H64A—C64—H64B109.5
O70—Yb2—O573.89 (6)C61—C64—H64C109.5
O60—Yb2—O5146.74 (6)H64A—C64—H64C109.5
O6—Yb2—O578.35 (5)H64B—C64—H64C109.5
O4—Yb2—O5139.63 (5)N60A—C61A—O60109.4 (4)
O50—Yb2—N6A83.73 (6)C51—O50—Yb2149.9 (2)
O70—Yb2—N6A144.41 (6)C51A—O50—Yb2173.4 (3)
O60—Yb2—N6A73.43 (6)C51—N50—C53119.4 (4)
O6—Yb2—N6A92.29 (5)C51—N50—C54112.8 (4)
O4—Yb2—N6A143.59 (5)C53—N50—C54127.7 (4)
O5—Yb2—N6A73.97 (5)O50—C51—N50115.1 (4)
N1—C1—Fe3178.82 (14)O50—C51—C52124.8 (3)
N1A—C1A—Fe4179.00 (15)N50—C51—C52120.0 (3)
N2—C2—Fe3176.1 (2)C51—C52—H52A109.5
N2A—C2A—Fe4179.26 (18)C51—C52—H52B109.5
N3—C3—Fe3177.0 (3)H52A—C52—H52B109.5
N3A—C3A—Fe4178.37 (16)C51—C52—H52C109.5
N4—C4—Fe3177.2 (2)H52A—C52—H52C109.5
N4A—C4A—Fe4178.46 (17)H52B—C52—H52C109.5
N6—C6—Fe3178.53 (13)N50—C53—H53A109.5
N6A—C6A—Fe4178.85 (15)N50—C53—H53B109.5
N5—C5—Fe3177.35 (18)H53A—C53—H53B109.5
N5A—C5A—Fe4178.37 (16)N50—C53—H53C109.5
O20—C21—N20120.88 (18)H53A—C53—H53C109.5
O20—C21—C24120.01 (18)H53B—C53—H53C109.5
N20—C21—C24119.11 (16)N50—C54—H54A109.5
N20—C22—H22A109.5N50—C54—H54B109.5
N20—C22—H22B109.5H54A—C54—H54B109.5
H22A—C22—H22B109.5N50—C54—H54C109.5
N20—C22—H22C109.5H54A—C54—H54C109.5
H22A—C22—H22C109.5H54B—C54—H54C109.5
H22B—C22—H22C109.5O50—C51A—N50A118.5 (5)
N20—C23—H23A109.5C70—O70—C70A46.9 (10)
N20—C23—H23B109.5C70—O70—Yb2166.50 (17)
H23A—C23—H23B109.5C70A—O70—Yb2142.5 (10)
N20—C23—H23C109.5C70—N70—C72122.3 (2)
H23A—C23—H23C109.5C70—N70—C71120.14 (19)
H23B—C23—H23C109.5C72—N70—C71117.3 (2)
C1A—N1A—Yb1173.94 (18)O70—C70—N70118.4 (2)
C6—N6—Yb1166.07 (12)O70—C70—C73121.1 (2)
C6A—N6A—Yb2169.72 (14)N70—C70—C73120.57 (19)
C21—N20—C23120.64 (16)N70—C71—H71A109.5
C21—N20—C22123.01 (19)N70—C71—H71B109.5
C23—N20—C22116.34 (18)H71A—C71—H71B109.5
Yb1—O1—H1A131.1 (12)N70—C71—H71C109.5
Yb1—O1—H1B117.2 (12)H71A—C71—H71C109.5
H1A—O1—H1B109.6 (17)H71B—C71—H71C109.5
Yb1—O2—H2A110.4 (15)N70—C72—H72A109.5
Yb1—O2—H2B113.0 (14)N70—C72—H72B109.5
H2A—O2—H2B108.8 (16)H72A—C72—H72B109.5
Yb1—O3—H3A116.1 (14)N70—C72—H72C109.5
Yb1—O3—H3B123.3 (13)H72A—C72—H72C109.5
H3A—O3—H3B108.7 (16)H72B—C72—H72C109.5
Yb2—O4—H4A117.0 (14)C70—C73—H73A109.5
Yb2—O4—H4B118.7 (14)C70—C73—H73B109.5
H4A—O4—H4B109.6 (16)H73A—C73—H73B109.5
Yb2—O5—H5A120.9 (13)C70—C73—H73C109.5
Yb2—O5—H5B119.9 (14)H73A—C73—H73C109.5
H5A—O5—H5B108.5 (16)H73B—C73—H73C109.5
Yb2—O6—H6A127.5 (12)N70A—C70A—O70103.3 (19)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···O980.97 (2)1.71 (2)2.6604 (19)167 (2)
O1—H1A···N2Ai0.97 (1)1.78 (1)2.728 (2)168 (2)
O2—H2B···O980.97 (2)1.76 (2)2.7154 (19)170 (2)
O2—H2A···N4Aii0.97 (1)1.81 (1)2.721 (2)155 (2)
O3—H3A···O990.97 (2)1.91 (2)2.714 (2)139 (2)
O3—H3B···N1iii0.97 (2)1.86 (1)2.7821 (18)158 (2)
O4—H4A···N5iv0.97 (1)1.96 (1)2.914 (2)169 (2)
O4—H4B···N3Av0.97 (1)1.91 (1)2.8567 (19)167 (2)
O5—H5B···N2vi0.97 (1)1.82 (1)2.775 (2)169 (2)
O5—H5A···N30.97 (1)1.96 (1)2.889 (2)159 (2)
O6—H6B···N30.97 (2)1.96 (1)2.855 (2)153 (2)
O6—H6A···N4vii0.97 (1)1.74 (1)2.708 (2)180 (2)
O98—H98B···N5Aviii0.97 (1)1.74 (1)2.695 (2)169 (2)
O98—H98A···N1iii0.97 (1)1.84 (1)2.7718 (19)162 (2)
O99—H99A···N3A0.97 (2)2.01 (2)2.961 (2)170 (2)
O99—H99B···N5iii0.97 (2)2.23 (1)3.094 (2)148 (2)
Symmetry codes: (i) x+1/2, y+1/2, z1/2; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1/2, y+3/2, z; (iv) x, y1, z; (v) x1/2, y+1/2, z; (vi) x, y+1, z+1/2; (vii) x, y+1, z1/2; (viii) x, y+1, z.
 

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