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Iron(II) complexes exhibiting thermal spin-crossover may be converted from the 1A1 low-spin (LS) state to the 5T2 high-spin (HS) state by irradiation with green light (light-induced excited spin-state trapping, LIESST) and from the LS to the HS state by irradiation with red light (reverse LIESST). The lifetime of the metastable LIESST states may be sufficiently long to enable an X-ray diffraction study. The lattice parameters of a single crystal of [Fe(mtz)6](BF4)2 (mtz = methyltetrazole) (space group P21/n) were measured between 300 and 10 K. While one Fe lattice site (A) of the crystal changes from the HS to the LS state near 78 K, the other site (B) remains in the LS state. Using the green light (514 nm) of an argon ion laser the crystal was quantitatively converted to the HS state at 10 K. Irradiation of the crystal at 10 K by red light of a laser diode (820 nm) with site A in the LS and site B in the HS state converts site B almost completely to the LS state. The lattice parameters of both metastable states were measured up to 50 K, where they start to decay on a minute timescale. At 10 K, a full data set for evaluation of the crystal structure was recorded. The volume change of the crystal per complex molecule accompanying the spin transition is 31.5 Å3 at site A and close to zero [-0.21 (14) Å3] at site B.
Supporting information
CCDC references: 214222; 214223; 214224
For all compounds, program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993).
Crystal data top
C12H24B2F8FeN24 | Z = 4 |
Mr = 734.02 | F(000) = 1488 |
Monoclinic, P21/n | Dx = 1.615 Mg m−3 |
a = 17.566 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.0964 (8) Å | µ = 0.60 mm−1 |
c = 18.696 (2) Å | T = 10 K |
β = 114.458 (11)° | 0.7 × 0.5 × 0.2 mm |
V = 3018.3 (5) Å3 | |
Data collection top
Radiation source: fine-focus sealed tube | Rint = 0.089 |
Graphite monochromator | θmax = 28.1°, θmin = 3.3° |
44836 measured reflections | h = −22→22 |
6430 independent reflections | k = −12→5 |
4581 reflections with I > 2σ(I) | l = −23→23 |
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)] = 0.056 | H-atom parameters not defined? |
wR(F2) = 0.147 | Calculated w = 1/[σ2(Fo2) + (0.0612P)2 + 7.9846P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | Δρmax = 0.50 e Å−3 |
6430 reflections | Δρmin = −0.71 e Å−3 |
524 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0017 (3) |
Primary atom site location: structure-invariant direct methods | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Refinement on F2 for ALL reflections except for 0 with very negative F2
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F2, conventional R-factors R
are based on F, with F set to zero for negative F2. The observed criterion
of F2 > 2sigma(F2) is used only for calculating _R_factor_obs 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 | |
Fe1 | 0.0000 | 0.0000 | 0.0000 | 0.00915 (10) | |
N411 | 0.07511 (11) | 0.1168 (2) | −0.04332 (10) | 0.0108 (4) | |
N311 | 0.14760 (12) | 0.1809 (2) | 0.00324 (11) | 0.0146 (5) | |
N211 | 0.18791 (12) | 0.2146 (2) | −0.03851 (11) | 0.0146 (5) | |
N111 | 0.14156 (11) | 0.1703 (2) | −0.11274 (10) | 0.0124 (5) | |
C111 | 0.07363 (13) | 0.1131 (3) | −0.11432 (13) | 0.0131 (5) | |
H111 | 0.0328 (16) | 0.072 (3) | −0.1557 (15) | 0.014 (7)* | |
C211 | 0.16806 (14) | 0.1940 (3) | −0.17646 (13) | 0.0167 (6) | |
H21A | 0.2266 (15) | 0.162 (3) | −0.1609 (14) | 0.011 (7)* | |
H21B | 0.168 (2) | 0.287 (4) | −0.1849 (19) | 0.038 (10)* | |
H21C | 0.1293 (15) | 0.152 (3) | −0.2188 (15) | 0.012 (7)* | |
N421 | −0.07674 (11) | 0.1697 (2) | −0.00322 (10) | 0.0118 (5) | |
N321 | −0.12894 (11) | 0.1764 (2) | 0.03459 (11) | 0.0144 (5) | |
N221 | −0.16866 (12) | 0.2879 (2) | 0.01903 (11) | 0.0137 (5) | |
N121 | −0.14314 (11) | 0.3554 (2) | −0.02974 (10) | 0.0123 (5) | |
C121 | −0.08752 (14) | 0.2823 (3) | −0.04243 (12) | 0.0125 (5) | |
H121 | −0.0625 (18) | 0.302 (3) | −0.0725 (17) | 0.025 (8)* | |
C221 | −0.17141 (14) | 0.4907 (3) | −0.05481 (13) | 0.0151 (6) | |
H22A | −0.165 (3) | 0.506 (4) | −0.099 (3) | 0.066 (14)* | |
H22B | −0.226 (2) | 0.488 (3) | −0.0641 (19) | 0.039 (10)* | |
H22C | −0.146 (3) | 0.562 (5) | −0.013 (3) | 0.089 (16)* | |
N431 | 0.08428 (11) | 0.0517 (2) | 0.12185 (10) | 0.0114 (4) | |
N331 | 0.14633 (11) | −0.0291 (2) | 0.17039 (10) | 0.0128 (5) | |
N231 | 0.19060 (11) | 0.0305 (2) | 0.23589 (11) | 0.0133 (5) | |
N131 | 0.15645 (11) | 0.1521 (2) | 0.23056 (11) | 0.0124 (5) | |
C131 | 0.09212 (13) | 0.1648 (3) | 0.16109 (13) | 0.0129 (5) | |
H131 | 0.0621 (15) | 0.241 (3) | 0.1450 (14) | 0.011 (7)* | |
C231 | 0.18854 (14) | 0.2469 (3) | 0.29569 (13) | 0.0158 (6) | |
H23A | 0.1564 (18) | 0.331 (3) | 0.2777 (16) | 0.025 (8)* | |
H23B | 0.1781 (15) | 0.209 (3) | 0.3419 (14) | 0.010 (6)* | |
H23C | 0.2436 (14) | 0.261 (3) | 0.3075 (13) | 0.003 (6)* | |
Fe2 | 0.5000 | 0.0000 | 0.0000 | 0.01023 (11) | |
N412 | 0.43442 (12) | 0.1294 (2) | −0.10039 (11) | 0.0134 (5) | |
N312 | 0.39066 (12) | 0.2401 (2) | −0.09778 (11) | 0.0140 (5) | |
N212 | 0.36321 (12) | 0.3010 (2) | −0.16496 (11) | 0.0149 (5) | |
N112 | 0.38856 (11) | 0.2285 (2) | −0.21208 (10) | 0.0119 (5) | |
C112 | 0.43167 (14) | 0.1252 (3) | −0.17205 (13) | 0.0145 (5) | |
H112 | 0.4609 (18) | 0.064 (3) | −0.1892 (17) | 0.027 (8)* | |
C212 | 0.37708 (14) | 0.2780 (3) | −0.28943 (13) | 0.0150 (6) | |
H21A | 0.4273 (19) | 0.340 (3) | −0.2794 (18) | 0.034 (9)* | |
H21B | 0.3752 (14) | 0.204 (3) | −0.3196 (13) | 0.001 (6)* | |
H21C | 0.3207 (18) | 0.319 (3) | −0.3175 (17) | 0.028 (8)* | |
N422 | 0.57820 (12) | 0.1668 (2) | 0.06243 (10) | 0.0132 (5) | |
N322 | 0.62467 (12) | 0.1694 (2) | 0.14193 (11) | 0.0139 (5) | |
N222 | 0.67300 (12) | 0.2721 (2) | 0.16090 (11) | 0.0146 (5) | |
N122 | 0.65769 (11) | 0.3381 (2) | 0.09301 (11) | 0.0119 (5) | |
C122 | 0.60018 (14) | 0.2729 (3) | 0.03421 (12) | 0.0131 (5) | |
H122 | 0.5828 (17) | 0.297 (3) | −0.0143 (16) | 0.022 (8)* | |
C222 | 0.70358 (14) | 0.4592 (3) | 0.09313 (14) | 0.0156 (6) | |
H22A | 0.6722 (18) | 0.512 (3) | 0.0539 (17) | 0.023 (8)* | |
H22B | 0.7529 (17) | 0.442 (3) | 0.0878 (16) | 0.022 (8)* | |
H23C | 0.7189 (17) | 0.504 (3) | 0.1439 (16) | 0.019 (7)* | |
N432 | 0.41181 (11) | 0.0467 (2) | 0.05130 (11) | 0.0128 (5) | |
N332 | 0.35662 (11) | −0.0457 (2) | 0.05689 (11) | 0.0138 (5) | |
N232 | 0.31929 (11) | 0.0018 (2) | 0.09785 (11) | 0.0129 (4) | |
N132 | 0.34933 (11) | 0.1257 (2) | 0.11961 (11) | 0.0119 (5) | |
C132 | 0.40535 (14) | 0.1527 (3) | 0.09082 (13) | 0.0136 (5) | |
H133 | 0.4358 (14) | 0.227 (3) | 0.0964 (13) | 0.000 (6)* | |
C232 | 0.32108 (14) | 0.2057 (3) | 0.16883 (13) | 0.0137 (6) | |
H23A | 0.2638 (16) | 0.224 (3) | 0.1413 (15) | 0.017 (7)* | |
H23B | 0.3276 (16) | 0.162 (3) | 0.2128 (15) | 0.015 (7)* | |
H23C | 0.3485 (17) | 0.292 (3) | 0.1817 (16) | 0.021 (8)* | |
B1 | 0.4483 (2) | 0.5044 (3) | 0.14742 (14) | 0.0134 (6) | |
F11 | 0.37005 (8) | 0.4627 (2) | 0.09452 (8) | 0.0173 (4) | |
F21 | 0.45754 (8) | 0.63926 (15) | 0.13814 (7) | 0.0156 (3) | |
F31 | 0.45628 (8) | 0.4821 (2) | 0.22440 (7) | 0.0172 (3) | |
F41 | 0.51038 (8) | 0.4321 (2) | 0.13604 (8) | 0.0211 (4) | |
B2 | −0.0075 (2) | 0.5194 (3) | 0.16441 (14) | 0.0123 (6) | |
F12 | 0.00780 (8) | 0.45079 (15) | 0.10607 (8) | 0.0162 (3) | |
F22 | 0.02277 (8) | 0.64785 (15) | 0.16913 (7) | 0.0156 (3) | |
F32 | 0.03449 (8) | 0.45465 (15) | 0.23636 (7) | 0.0156 (3) | |
F42 | −0.09292 (8) | 0.52131 (15) | 0.14500 (8) | 0.0169 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0089 (2) | 0.0124 (2) | 0.0068 (2) | 0.0003 (2) | 0.00385 (14) | 0.0002 (2) |
N411 | 0.0104 (8) | 0.0128 (10) | 0.0084 (7) | −0.0003 (8) | 0.0030 (6) | −0.0007 (7) |
N311 | 0.0138 (8) | 0.0167 (11) | 0.0144 (8) | −0.0033 (8) | 0.0071 (7) | −0.0025 (8) |
N211 | 0.0147 (8) | 0.0183 (11) | 0.0106 (8) | −0.0025 (8) | 0.0050 (6) | −0.0013 (8) |
N111 | 0.0130 (8) | 0.0146 (11) | 0.0098 (8) | 0.0003 (8) | 0.0050 (6) | 0.0000 (7) |
C111 | 0.0100 (9) | 0.0182 (13) | 0.0102 (9) | 0.0004 (9) | 0.0033 (7) | 0.0006 (9) |
C211 | 0.0178 (10) | 0.0234 (15) | 0.0134 (9) | −0.0028 (10) | 0.0110 (8) | 0.0020 (9) |
N421 | 0.0123 (8) | 0.0168 (11) | 0.0073 (7) | −0.0014 (8) | 0.0051 (6) | −0.0008 (7) |
N321 | 0.0127 (8) | 0.0193 (11) | 0.0135 (8) | 0.0017 (8) | 0.0078 (6) | −0.0011 (8) |
N221 | 0.0155 (8) | 0.0156 (11) | 0.0120 (8) | −0.0016 (8) | 0.0078 (6) | −0.0010 (7) |
N121 | 0.0143 (8) | 0.0137 (11) | 0.0096 (8) | 0.0002 (8) | 0.0056 (6) | 0.0008 (7) |
C121 | 0.0135 (9) | 0.0166 (13) | 0.0077 (9) | −0.0006 (9) | 0.0046 (7) | −0.0015 (8) |
C221 | 0.0163 (10) | 0.0141 (13) | 0.0135 (9) | 0.0023 (10) | 0.0047 (8) | 0.0001 (9) |
N431 | 0.0121 (8) | 0.0136 (10) | 0.0097 (8) | 0.0006 (8) | 0.0056 (6) | 0.0005 (7) |
N331 | 0.0117 (8) | 0.0181 (11) | 0.0080 (7) | 0.0005 (8) | 0.0034 (6) | 0.0016 (7) |
N231 | 0.0128 (8) | 0.0174 (11) | 0.0102 (8) | 0.0015 (8) | 0.0052 (6) | −0.0010 (7) |
N131 | 0.0122 (8) | 0.0139 (11) | 0.0108 (8) | −0.0015 (8) | 0.0044 (6) | −0.0010 (7) |
C131 | 0.0120 (9) | 0.0163 (13) | 0.0113 (9) | 0.0000 (9) | 0.0057 (7) | 0.0004 (9) |
C231 | 0.0144 (10) | 0.0178 (13) | 0.0132 (10) | 0.0002 (10) | 0.0037 (8) | −0.0056 (9) |
Fe2 | 0.0098 (2) | 0.0136 (2) | 0.0081 (2) | −0.0003 (2) | 0.00460 (14) | −0.0004 (2) |
N412 | 0.0152 (8) | 0.0149 (11) | 0.0121 (8) | 0.0010 (8) | 0.0077 (6) | −0.0003 (7) |
N312 | 0.0130 (8) | 0.0167 (11) | 0.0124 (8) | 0.0003 (8) | 0.0052 (6) | 0.0002 (8) |
N212 | 0.0147 (8) | 0.0197 (12) | 0.0107 (8) | −0.0001 (8) | 0.0057 (6) | −0.0016 (8) |
N112 | 0.0106 (8) | 0.0172 (11) | 0.0079 (7) | −0.0025 (8) | 0.0037 (6) | −0.0004 (7) |
C112 | 0.0143 (9) | 0.0160 (13) | 0.0143 (9) | −0.0005 (9) | 0.0071 (8) | −0.0009 (9) |
C212 | 0.0195 (10) | 0.0191 (13) | 0.0085 (9) | 0.0023 (10) | 0.0079 (7) | 0.0037 (9) |
N422 | 0.0165 (8) | 0.0173 (11) | 0.0076 (7) | −0.0010 (8) | 0.0067 (6) | −0.0019 (7) |
N322 | 0.0129 (8) | 0.0175 (11) | 0.0102 (8) | −0.0006 (8) | 0.0037 (7) | −0.0008 (8) |
N222 | 0.0158 (8) | 0.0173 (11) | 0.0114 (8) | −0.0002 (8) | 0.0064 (7) | 0.0017 (8) |
N122 | 0.0118 (8) | 0.0135 (11) | 0.0101 (8) | 0.0016 (8) | 0.0040 (6) | 0.0019 (7) |
C122 | 0.0138 (9) | 0.0178 (13) | 0.0076 (9) | −0.0006 (9) | 0.0044 (7) | −0.0018 (9) |
C222 | 0.0154 (10) | 0.0170 (13) | 0.0155 (10) | −0.0009 (9) | 0.0075 (8) | 0.0010 (9) |
N432 | 0.0133 (8) | 0.0149 (11) | 0.0118 (8) | −0.0011 (8) | 0.0069 (6) | 0.0005 (7) |
N332 | 0.0151 (8) | 0.0144 (11) | 0.0147 (8) | 0.0000 (8) | 0.0090 (7) | 0.0008 (8) |
N232 | 0.0131 (8) | 0.0146 (11) | 0.0130 (8) | 0.0000 (8) | 0.0075 (6) | 0.0002 (8) |
N132 | 0.0123 (8) | 0.0140 (11) | 0.0099 (8) | −0.0009 (8) | 0.0050 (6) | −0.0008 (7) |
C132 | 0.0133 (9) | 0.0161 (13) | 0.0138 (9) | −0.0026 (9) | 0.0081 (7) | −0.0017 (9) |
C232 | 0.0154 (9) | 0.0173 (13) | 0.0099 (9) | −0.0016 (9) | 0.0067 (7) | −0.0026 (9) |
B1 | 0.0157 (10) | 0.0152 (14) | 0.0107 (10) | 0.0015 (11) | 0.0068 (8) | 0.0016 (10) |
F11 | 0.0152 (6) | 0.0207 (8) | 0.0133 (6) | −0.0029 (6) | 0.0031 (5) | −0.0004 (5) |
F21 | 0.0156 (6) | 0.0175 (8) | 0.0126 (6) | −0.0010 (6) | 0.0047 (5) | 0.0012 (5) |
F31 | 0.0188 (6) | 0.0223 (8) | 0.0102 (5) | 0.0001 (6) | 0.0058 (5) | 0.0039 (5) |
F41 | 0.0180 (6) | 0.0209 (8) | 0.0290 (7) | 0.0010 (6) | 0.0142 (5) | −0.0054 (6) |
B2 | 0.0135 (10) | 0.0137 (14) | 0.0085 (10) | 0.0017 (10) | 0.0034 (8) | 0.0027 (9) |
F12 | 0.0186 (6) | 0.0175 (8) | 0.0137 (6) | 0.0005 (6) | 0.0078 (5) | −0.0037 (5) |
F22 | 0.0170 (6) | 0.0165 (8) | 0.0149 (6) | −0.0023 (6) | 0.0081 (5) | −0.0002 (5) |
F32 | 0.0158 (6) | 0.0191 (8) | 0.0120 (6) | 0.0016 (6) | 0.0058 (5) | 0.0052 (5) |
F42 | 0.0125 (5) | 0.0220 (8) | 0.0161 (6) | 0.0005 (6) | 0.0059 (5) | −0.0004 (6) |
Geometric parameters (Å, º) top
Fe1—N411i | 2.162 (2) | Fe2—N412ii | 2.183 (2) |
Fe1—N411 | 2.162 (2) | Fe2—N412 | 2.183 (2) |
Fe1—N421i | 2.166 (2) | N412—C112 | 1.321 (3) |
Fe1—N421 | 2.166 (2) | N412—N312 | 1.369 (3) |
Fe1—N431 | 2.205 (2) | N312—N212 | 1.299 (3) |
Fe1—N431i | 2.205 (2) | N212—N112 | 1.355 (3) |
N411—C111 | 1.317 (3) | N112—C112 | 1.324 (3) |
N411—N311 | 1.371 (3) | N112—C212 | 1.463 (3) |
N311—N211 | 1.298 (3) | C112—H112 | 0.94 (3) |
N211—N111 | 1.361 (3) | C212—H21A | 1.03 (3) |
N111—C111 | 1.315 (3) | C212—H21B | 0.93 (2) |
N111—C211 | 1.467 (3) | C212—H21C | 1.00 (3) |
C111—H111 | 0.91 (2) | N422—C122 | 1.320 (3) |
C211—H21A | 1.00 (3) | N422—N322 | 1.368 (2) |
C211—H21B | 0.95 (4) | N322—N222 | 1.293 (3) |
C211—H21C | 0.91 (2) | N222—N122 | 1.358 (3) |
N421—C121 | 1.323 (3) | N122—C122 | 1.320 (3) |
N421—N321 | 1.372 (3) | N122—C222 | 1.464 (3) |
N321—N221 | 1.293 (3) | C122—H122 | 0.86 (3) |
N221—N121 | 1.355 (3) | C222—H22A | 0.89 (3) |
N121—C121 | 1.322 (3) | C222—H22B | 0.93 (3) |
N121—C221 | 1.463 (3) | C222—H23C | 0.99 (3) |
C121—H121 | 0.87 (3) | N432—C132 | 1.332 (3) |
C221—H22A | 0.89 (5) | N432—N332 | 1.380 (3) |
C221—H22B | 0.89 (4) | N332—N232 | 1.289 (3) |
C221—H22C | 1.02 (5) | N232—N132 | 1.354 (3) |
N431—C131 | 1.334 (3) | N132—C132 | 1.331 (3) |
N431—N331 | 1.363 (3) | N132—C232 | 1.457 (3) |
N331—N231 | 1.296 (3) | C132—H133 | 0.90 (2) |
N231—N131 | 1.351 (3) | C232—H23A | 0.94 (3) |
N131—C131 | 1.329 (3) | C232—H23B | 0.90 (3) |
N131—C231 | 1.466 (3) | C232—H23C | 0.98 (3) |
C131—H131 | 0.91 (3) | B1—F11 | 1.385 (3) |
C231—H23A | 1.00 (3) | B1—F21 | 1.391 (3) |
C231—H23B | 1.03 (3) | B1—F41 | 1.400 (3) |
C231—H23C | 0.91 (2) | B1—F31 | 1.405 (3) |
Fe2—N422 | 2.181 (2) | B2—F22 | 1.390 (3) |
Fe2—N422ii | 2.181 (2) | B2—F42 | 1.391 (3) |
Fe2—N432 | 2.185 (2) | B2—F32 | 1.400 (3) |
Fe2—N432ii | 2.185 (2) | B2—F12 | 1.409 (3) |
| | | |
N411i—Fe1—N411 | 180.0 | N422—Fe2—N412ii | 90.61 (7) |
N411i—Fe1—N421i | 91.56 (8) | N422ii—Fe2—N412ii | 89.39 (7) |
N411—Fe1—N421i | 88.44 (8) | N432—Fe2—N412ii | 88.24 (7) |
N411i—Fe1—N421 | 88.44 (8) | N432ii—Fe2—N412ii | 91.76 (7) |
N411—Fe1—N421 | 91.56 (8) | N422—Fe2—N412 | 89.39 (7) |
N421i—Fe1—N421 | 180.0 | N422ii—Fe2—N412 | 90.61 (7) |
N411i—Fe1—N431 | 89.70 (7) | N432—Fe2—N412 | 91.76 (7) |
N411—Fe1—N431 | 90.30 (7) | N432ii—Fe2—N412 | 88.24 (7) |
N421i—Fe1—N431 | 90.83 (7) | N412ii—Fe2—N412 | 180.0 |
N421—Fe1—N431 | 89.17 (7) | C112—N412—N312 | 106.1 (2) |
N411i—Fe1—N431i | 90.30 (7) | C112—N412—Fe2 | 129.6 (2) |
N411—Fe1—N431i | 89.70 (7) | N312—N412—Fe2 | 124.21 (14) |
N421i—Fe1—N431i | 89.17 (7) | N212—N312—N412 | 109.9 (2) |
N421—Fe1—N431i | 90.83 (7) | N312—N212—N112 | 106.4 (2) |
N431—Fe1—N431i | 180.0 | C112—N112—N212 | 108.9 (2) |
C111—N411—N311 | 106.2 (2) | C112—N112—C212 | 129.8 (2) |
C111—N411—Fe1 | 127.0 (2) | N212—N112—C212 | 120.7 (2) |
N311—N411—Fe1 | 124.74 (14) | N112—C112—N412 | 108.7 (2) |
N211—N311—N411 | 109.7 (2) | N112—C112—H112 | 126.3 (19) |
N311—N211—N111 | 106.4 (2) | N412—C112—H112 | 124.7 (18) |
C111—N111—N211 | 108.7 (2) | N112—C212—H21A | 105.6 (17) |
C111—N111—C211 | 130.0 (2) | N112—C212—H21B | 106.2 (15) |
N211—N111—C211 | 121.2 (2) | H21A—C212—H21B | 114 (2) |
N411—C111—N111 | 109.0 (2) | N112—C212—H21C | 111.1 (19) |
N411—C111—H111 | 123.3 (19) | H21A—C212—H21C | 116 (3) |
N111—C111—H111 | 127.5 (19) | H21B—C212—H21C | 104 (2) |
N111—C211—H21A | 110.3 (15) | C122—N422—N322 | 106.1 (2) |
N111—C211—H21B | 108 (2) | C122—N422—Fe2 | 129.49 (14) |
H21A—C211—H21B | 108 (3) | N322—N422—Fe2 | 123.8 (2) |
N111—C211—H21C | 104.8 (18) | N222—N322—N422 | 110.0 (2) |
H21A—C211—H21C | 114 (2) | N322—N222—N122 | 106.5 (2) |
H21B—C211—H21C | 112 (3) | C122—N122—N222 | 108.7 (2) |
C121—N421—N321 | 105.7 (2) | C122—N122—C222 | 130.4 (2) |
C121—N421—Fe1 | 129.8 (2) | N222—N122—C222 | 120.8 (2) |
N321—N421—Fe1 | 124.5 (2) | N122—C122—N422 | 108.7 (2) |
N221—N321—N421 | 109.9 (2) | N122—C122—H122 | 124 (2) |
N321—N221—N121 | 106.9 (2) | N422—C122—H122 | 128 (2) |
C121—N121—N221 | 108.4 (2) | N122—C222—H22A | 110.1 (19) |
C121—N121—C221 | 129.9 (2) | N122—C222—H22B | 112.1 (19) |
N221—N121—C221 | 121.5 (2) | H22A—C222—H22B | 108 (3) |
N421—C121—N121 | 109.1 (2) | N122—C222—H23C | 108.5 (18) |
N421—C121—H121 | 124 (2) | H22A—C222—H23C | 110 (3) |
N121—C121—H121 | 127 (2) | H22B—C222—H23C | 107 (2) |
N121—C221—H22A | 107 (3) | C132—N432—N332 | 106.1 (2) |
N121—C221—H22B | 103 (2) | C132—N432—Fe2 | 131.0 (2) |
H22A—C221—H22B | 111 (3) | N332—N432—Fe2 | 122.4 (2) |
N121—C221—H22C | 116 (3) | N232—N332—N432 | 109.9 (2) |
H22A—C221—H22C | 114 (4) | N332—N232—N132 | 106.9 (2) |
H22B—C221—H22C | 105 (4) | C132—N132—N232 | 109.2 (2) |
C131—N431—N331 | 105.9 (2) | C132—N132—C232 | 130.1 (2) |
C131—N431—Fe1 | 130.04 (15) | N232—N132—C232 | 120.6 (2) |
N331—N431—Fe1 | 123.8 (2) | N132—C132—N432 | 107.9 (2) |
N231—N331—N431 | 110.7 (2) | N132—C132—H133 | 128.6 (16) |
N331—N231—N131 | 106.1 (2) | N432—C132—H133 | 123.5 (16) |
C131—N131—N231 | 109.4 (2) | N132—C232—H23A | 109.2 (18) |
C131—N131—C231 | 128.9 (2) | N132—C232—H23B | 111.1 (19) |
N231—N131—C231 | 121.7 (2) | H23A—C232—H23B | 107 (3) |
N431—C131—N131 | 107.9 (2) | N132—C232—H23C | 112.8 (18) |
N431—C131—H131 | 128.8 (16) | H23A—C232—H23C | 106 (2) |
N131—C131—H131 | 123.2 (16) | H23B—C232—H23C | 111 (2) |
N131—C231—H23A | 107.9 (16) | F11—B1—F21 | 109.9 (2) |
N131—C231—H23B | 108.1 (15) | F11—B1—F41 | 109.8 (2) |
H23A—C231—H23B | 109 (2) | F21—B1—F41 | 110.7 (2) |
N131—C231—H23C | 108.0 (16) | F11—B1—F31 | 109.4 (2) |
H23A—C231—H23C | 110 (2) | F21—B1—F31 | 108.5 (2) |
H23B—C231—H23C | 113 (2) | F41—B1—F31 | 108.6 (2) |
N422—Fe2—N422ii | 180.0 | F22—B2—F42 | 110.3 (2) |
N422—Fe2—N432 | 90.14 (8) | F22—B2—F32 | 109.9 (2) |
N422ii—Fe2—N432 | 89.86 (8) | F42—B2—F32 | 109.8 (2) |
N422—Fe2—N432ii | 89.86 (8) | F22—B2—F12 | 108.5 (2) |
N422ii—Fe2—N432ii | 90.14 (8) | F42—B2—F12 | 109.6 (2) |
N432—Fe2—N432ii | 180.0 | F32—B2—F12 | 108.7 (2) |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z. |
Crystal data top
C12H24B2F8FeN24 | V = 2955.9 (5) Å3 |
Mr = 734.02 | Z = 4 |
a = 17.4887 (15) Å | F(000) = 1488 |
b = 10.0914 (8) Å | Dx = 1.649 Mg m−3 |
c = 18.517 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
α = 90° | µ = 0.61 mm−1 |
β = 115.243 (10)° | T = 10 K |
γ = 90° | 0.7 × 0.5 × 0.2 mm |
Data collection top
Radiation source: fine-focus sealed tube | Rint = 0.083 |
Graphite monochromator | θmax = 28.2°, θmin = 3.3° |
44334 measured reflections | h = −22→22 |
6461 independent reflections | k = −12→6 |
4693 reflections with I > 2σ(I) | l = −23→23 |
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)] = 0.053 | H-atom parameters not defined? |
wR(F2) = 0.155 | Calculated w = 1/[σ2(Fo2) + (0.0728P)2 + 2.1968P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | Δρmax = 0.65 e Å−3 |
6411 reflections | Δρmin = −0.68 e Å−3 |
524 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0052 (6) |
Primary atom site location: structure-invariant direct methods | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Refinement on F2 for ALL reflections except for 50 with very negative F2
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F2, conventional R-factors R
are based on F, with F set to zero for negative F2. The observed criterion
of F2 > 2sigma(F2) is used only for calculating _R_factor_obs 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 | |
Fe1 | 0.0000 | 0.0000 | 0.0000 | 0.00804 (15) | |
N411 | 0.06899 (14) | 0.1076 (3) | −0.03971 (14) | 0.0111 (5) | |
N311 | 0.13426 (14) | 0.1893 (3) | 0.00721 (14) | 0.0122 (5) | |
N211 | 0.17488 (15) | 0.2304 (3) | −0.03295 (14) | 0.0131 (5) | |
N111 | 0.13613 (14) | 0.1747 (2) | −0.10635 (14) | 0.0109 (5) | |
C111 | 0.0720 (2) | 0.1019 (3) | −0.1094 (2) | 0.0122 (6) | |
H111 | 0.037 (2) | 0.057 (3) | −0.1531 (19) | 0.007 (7)* | |
C211 | 0.1644 (2) | 0.2017 (3) | −0.1688 (2) | 0.0149 (6) | |
H21A | 0.225 (2) | 0.178 (4) | −0.151 (2) | 0.022 (9)* | |
H21B | 0.154 (3) | 0.291 (4) | −0.183 (2) | 0.031 (11)* | |
H21C | 0.130 (2) | 0.154 (4) | −0.212 (2) | 0.021 (9)* | |
N421 | −0.07010 (14) | 0.1574 (2) | −0.00370 (13) | 0.0100 (5) | |
N321 | −0.12165 (14) | 0.1654 (3) | 0.03524 (14) | 0.0124 (5) | |
N221 | −0.16190 (15) | 0.2765 (2) | 0.01861 (14) | 0.0124 (5) | |
N121 | −0.13728 (14) | 0.3433 (3) | −0.03111 (14) | 0.0116 (5) | |
C121 | −0.0811 (2) | 0.2695 (3) | −0.0438 (2) | 0.0110 (6) | |
H121 | −0.056 (2) | 0.291 (4) | −0.074 (2) | 0.018 (9)* | |
C221 | −0.1663 (2) | 0.4778 (3) | −0.0573 (2) | 0.0141 (6) | |
H22A | −0.166 (3) | 0.485 (4) | −0.113 (3) | 0.045 (13)* | |
H22B | −0.223 (3) | 0.490 (4) | −0.064 (3) | 0.046 (13)* | |
H22C | −0.128 (3) | 0.546 (5) | −0.022 (3) | 0.060 (15)* | |
N431 | 0.07916 (14) | 0.0455 (3) | 0.11240 (14) | 0.0110 (5) | |
N331 | 0.14090 (14) | −0.0374 (3) | 0.16249 (14) | 0.0126 (5) | |
N231 | 0.18565 (15) | 0.0219 (2) | 0.22915 (14) | 0.0127 (5) | |
N131 | 0.15326 (14) | 0.1460 (2) | 0.22287 (14) | 0.0114 (5) | |
C131 | 0.0885 (2) | 0.1581 (3) | 0.1521 (2) | 0.0115 (6) | |
H131 | 0.060 (2) | 0.228 (3) | 0.1371 (19) | 0.005 (8)* | |
C231 | 0.1872 (2) | 0.2403 (3) | 0.2890 (2) | 0.0136 (6) | |
H23A | 0.158 (3) | 0.314 (5) | 0.272 (3) | 0.033 (11)* | |
H23B | 0.179 (2) | 0.204 (4) | 0.333 (2) | 0.021 (9)* | |
H23C | 0.243 (2) | 0.253 (3) | 0.3047 (18) | 0.004 (7)* | |
Fe2 | 0.5000 | 0.0000 | 0.0000 | 0.0095 (2) | |
N412 | 0.43279 (15) | 0.1305 (3) | −0.10150 (14) | 0.0128 (5) | |
N312 | 0.38908 (15) | 0.2415 (3) | −0.09772 (14) | 0.0125 (5) | |
N212 | 0.36133 (15) | 0.3044 (3) | −0.16529 (14) | 0.0142 (5) | |
N112 | 0.38630 (14) | 0.2346 (2) | −0.21350 (14) | 0.0113 (5) | |
C112 | 0.4300 (2) | 0.1296 (3) | −0.1737 (2) | 0.0133 (6) | |
H112 | 0.454 (2) | 0.070 (4) | −0.189 (2) | 0.016 (9)* | |
C212 | 0.3746 (2) | 0.2871 (3) | −0.2911 (2) | 0.0152 (6) | |
H21A | 0.425 (2) | 0.346 (4) | −0.280 (2) | 0.020 (9)* | |
H21B | 0.373 (2) | 0.213 (3) | −0.325 (2) | 0.012 (8)* | |
H21C | 0.324 (2) | 0.335 (4) | −0.313 (2) | 0.017 (9)* | |
N422 | 0.57845 (15) | 0.1679 (3) | 0.06467 (14) | 0.0116 (5) | |
N322 | 0.62313 (15) | 0.1730 (3) | 0.14587 (14) | 0.0135 (5) | |
N222 | 0.6725 (2) | 0.2750 (3) | 0.16521 (14) | 0.0142 (5) | |
N122 | 0.65962 (14) | 0.3378 (3) | 0.09610 (14) | 0.0121 (5) | |
C122 | 0.6026 (2) | 0.2701 (3) | 0.0360 (2) | 0.0134 (6) | |
H122 | 0.5833 (19) | 0.293 (3) | −0.0150 (19) | 0.004 (7)* | |
C222 | 0.7074 (2) | 0.4569 (3) | 0.0956 (2) | 0.0141 (6) | |
H22A | 0.675 (2) | 0.522 (4) | 0.067 (2) | 0.018 (9)* | |
H22B | 0.749 (2) | 0.433 (4) | 0.082 (2) | 0.024 (10)* | |
H23C | 0.727 (2) | 0.496 (4) | 0.153 (2) | 0.023 (10)* | |
N432 | 0.41083 (15) | 0.0466 (3) | 0.05108 (14) | 0.0127 (5) | |
N332 | 0.35224 (15) | −0.0427 (3) | 0.05271 (14) | 0.0135 (5) | |
N232 | 0.3140 (2) | 0.0055 (3) | 0.09330 (15) | 0.0136 (5) | |
N132 | 0.34754 (14) | 0.1272 (3) | 0.11870 (14) | 0.0112 (5) | |
C132 | 0.4064 (2) | 0.1504 (3) | 0.0924 (2) | 0.0125 (6) | |
H133 | 0.441 (2) | 0.221 (3) | 0.1036 (18) | 0.005 (7)* | |
C232 | 0.3207 (2) | 0.2069 (3) | 0.1692 (2) | 0.0138 (6) | |
H23A | 0.264 (3) | 0.238 (4) | 0.141 (2) | 0.032 (11)* | |
H23B | 0.325 (2) | 0.157 (4) | 0.213 (2) | 0.025 (10)* | |
H23C | 0.359 (2) | 0.284 (4) | 0.187 (2) | 0.018 (9)* | |
B1 | 0.4455 (2) | 0.5047 (4) | 0.1457 (2) | 0.0138 (7) | |
F11 | 0.36522 (11) | 0.4637 (2) | 0.09302 (10) | 0.0177 (4) | |
F21 | 0.45429 (10) | 0.6402 (2) | 0.13771 (10) | 0.0159 (4) | |
F31 | 0.45674 (11) | 0.4788 (2) | 0.22399 (10) | 0.0200 (4) | |
F41 | 0.50668 (11) | 0.4344 (2) | 0.13178 (12) | 0.0251 (4) | |
B2 | −0.0068 (2) | 0.5162 (3) | 0.1658 (2) | 0.0125 (7) | |
F12 | 0.01043 (10) | 0.4490 (2) | 0.10831 (10) | 0.0150 (4) | |
F22 | 0.01686 (10) | 0.6481 (2) | 0.16811 (10) | 0.0142 (4) | |
F32 | 0.03949 (10) | 0.4578 (2) | 0.24059 (10) | 0.0150 (4) | |
F42 | −0.09282 (10) | 0.5078 (2) | 0.14710 (10) | 0.0148 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0068 (3) | 0.0107 (3) | 0.0072 (3) | 0.0002 (2) | 0.0035 (2) | 0.0001 (2) |
N411 | 0.0090 (11) | 0.0128 (13) | 0.0106 (12) | −0.0005 (9) | 0.0034 (9) | −0.0015 (10) |
N311 | 0.0091 (11) | 0.0163 (14) | 0.0126 (12) | −0.0039 (10) | 0.0059 (9) | −0.0009 (10) |
N211 | 0.0117 (11) | 0.0181 (14) | 0.0104 (12) | −0.0022 (10) | 0.0056 (9) | 0.0003 (10) |
N111 | 0.0118 (11) | 0.0118 (13) | 0.0107 (11) | −0.0007 (9) | 0.0063 (9) | −0.0002 (10) |
C111 | 0.0099 (13) | 0.016 (2) | 0.0104 (14) | 0.0010 (11) | 0.0044 (11) | 0.0004 (12) |
C211 | 0.018 (2) | 0.017 (2) | 0.0128 (15) | −0.0021 (13) | 0.0101 (12) | 0.0012 (13) |
N421 | 0.0098 (11) | 0.0137 (13) | 0.0081 (11) | −0.0021 (9) | 0.0054 (9) | −0.0009 (9) |
N321 | 0.0103 (11) | 0.0164 (14) | 0.0129 (12) | 0.0017 (10) | 0.0073 (10) | −0.0011 (10) |
N221 | 0.0124 (11) | 0.0136 (14) | 0.0127 (12) | −0.0001 (10) | 0.0067 (9) | 0.0004 (10) |
N121 | 0.0104 (11) | 0.0160 (14) | 0.0087 (11) | 0.0011 (10) | 0.0044 (9) | 0.0006 (10) |
C121 | 0.0114 (13) | 0.013 (2) | 0.0087 (13) | −0.0013 (11) | 0.0044 (11) | −0.0020 (11) |
C221 | 0.0144 (14) | 0.014 (2) | 0.0134 (14) | 0.0026 (12) | 0.0059 (12) | 0.0026 (12) |
N431 | 0.0096 (11) | 0.0124 (13) | 0.0134 (12) | 0.0013 (9) | 0.0072 (9) | 0.0021 (10) |
N331 | 0.0084 (11) | 0.0205 (14) | 0.0068 (11) | 0.0013 (10) | 0.0011 (9) | 0.0009 (10) |
N231 | 0.0111 (11) | 0.0139 (14) | 0.0135 (12) | −0.0004 (9) | 0.0054 (10) | −0.0014 (10) |
N131 | 0.0105 (11) | 0.0130 (14) | 0.0115 (12) | 0.0007 (9) | 0.0055 (9) | −0.0021 (10) |
C131 | 0.0088 (13) | 0.014 (2) | 0.0113 (14) | 0.0006 (12) | 0.0043 (11) | −0.0002 (12) |
C231 | 0.0136 (15) | 0.015 (2) | 0.0108 (14) | −0.0008 (12) | 0.0035 (12) | −0.0038 (12) |
Fe2 | 0.0085 (3) | 0.0124 (3) | 0.0088 (3) | −0.0001 (2) | 0.0047 (2) | −0.0002 (2) |
N412 | 0.0123 (11) | 0.0152 (14) | 0.0117 (12) | 0.0004 (10) | 0.0058 (10) | −0.0002 (10) |
N312 | 0.0107 (11) | 0.0151 (14) | 0.0118 (12) | 0.0014 (9) | 0.0047 (10) | 0.0008 (10) |
N212 | 0.0150 (12) | 0.0171 (14) | 0.0111 (12) | 0.0009 (10) | 0.0062 (10) | −0.0018 (10) |
N112 | 0.0100 (11) | 0.0146 (14) | 0.0110 (12) | −0.0001 (9) | 0.0061 (9) | −0.0003 (10) |
C112 | 0.0108 (13) | 0.015 (2) | 0.0151 (15) | −0.0001 (11) | 0.0063 (12) | 0.0006 (12) |
C212 | 0.018 (2) | 0.017 (2) | 0.0121 (14) | 0.0006 (13) | 0.0081 (12) | 0.0034 (13) |
N422 | 0.0144 (12) | 0.0135 (14) | 0.0083 (11) | 0.0004 (10) | 0.0062 (9) | −0.0004 (9) |
N322 | 0.0123 (11) | 0.0165 (14) | 0.0110 (12) | −0.0011 (10) | 0.0041 (10) | 0.0013 (10) |
N222 | 0.0144 (12) | 0.0167 (14) | 0.0130 (12) | −0.0010 (10) | 0.0072 (10) | 0.0003 (10) |
N122 | 0.0110 (11) | 0.0148 (14) | 0.0111 (12) | 0.0010 (10) | 0.0052 (9) | 0.0004 (10) |
C122 | 0.0127 (13) | 0.017 (2) | 0.0117 (14) | −0.0005 (11) | 0.0059 (11) | −0.0017 (12) |
C222 | 0.0140 (14) | 0.014 (2) | 0.017 (2) | −0.0006 (12) | 0.0087 (12) | −0.0002 (13) |
N432 | 0.0121 (11) | 0.0155 (14) | 0.0112 (12) | −0.0006 (10) | 0.0056 (9) | −0.0019 (10) |
N332 | 0.0133 (12) | 0.0161 (14) | 0.0140 (12) | −0.0015 (10) | 0.0086 (10) | −0.0016 (10) |
N232 | 0.0139 (12) | 0.0145 (14) | 0.0147 (12) | −0.0012 (10) | 0.0083 (10) | −0.0020 (10) |
N132 | 0.0099 (11) | 0.0128 (13) | 0.0118 (12) | −0.0009 (9) | 0.0056 (9) | −0.0013 (10) |
C132 | 0.0114 (13) | 0.014 (2) | 0.0127 (14) | −0.0009 (12) | 0.0054 (11) | 0.0003 (12) |
C232 | 0.0130 (14) | 0.018 (2) | 0.0119 (14) | 0.0020 (12) | 0.0073 (12) | −0.0018 (13) |
B1 | 0.0135 (15) | 0.017 (2) | 0.013 (2) | 0.0030 (13) | 0.0072 (12) | 0.0038 (13) |
F11 | 0.0149 (8) | 0.0213 (10) | 0.0138 (9) | −0.0039 (7) | 0.0031 (7) | 0.0010 (7) |
F21 | 0.0158 (8) | 0.0166 (10) | 0.0143 (9) | −0.0006 (7) | 0.0054 (7) | 0.0010 (7) |
F31 | 0.0231 (9) | 0.0246 (11) | 0.0099 (8) | −0.0054 (8) | 0.0047 (7) | 0.0023 (7) |
F41 | 0.0214 (9) | 0.0202 (11) | 0.0423 (12) | 0.0000 (8) | 0.0219 (9) | −0.0071 (9) |
B2 | 0.0098 (14) | 0.015 (2) | 0.013 (2) | 0.0012 (12) | 0.0051 (12) | 0.0007 (13) |
F12 | 0.0157 (8) | 0.0165 (9) | 0.0142 (8) | 0.0015 (7) | 0.0078 (7) | −0.0012 (7) |
F22 | 0.0158 (8) | 0.0133 (10) | 0.0155 (9) | −0.0016 (7) | 0.0084 (7) | −0.0012 (7) |
F32 | 0.0141 (8) | 0.0189 (10) | 0.0125 (8) | 0.0019 (7) | 0.0062 (7) | 0.0038 (7) |
F42 | 0.0100 (8) | 0.0185 (10) | 0.0160 (9) | 0.0002 (7) | 0.0058 (7) | −0.0009 (7) |
Geometric parameters (Å, º) top
Fe1—N411 | 1.983 (2) | Fe2—N432 | 2.192 (2) |
Fe1—N411i | 1.983 (2) | Fe2—N432ii | 2.192 (2) |
Fe1—N421i | 1.989 (2) | N412—C112 | 1.318 (4) |
Fe1—N421 | 1.989 (2) | N412—N312 | 1.374 (3) |
Fe1—N431 | 2.000 (2) | N312—N212 | 1.299 (3) |
Fe1—N431i | 2.000 (2) | N212—N112 | 1.347 (3) |
N411—C111 | 1.315 (4) | N112—C112 | 1.330 (4) |
N411—N311 | 1.375 (3) | N112—C212 | 1.462 (4) |
N311—N211 | 1.297 (3) | C112—H112 | 0.84 (4) |
N211—N111 | 1.356 (3) | C212—H21A | 1.01 (4) |
N111—C111 | 1.322 (4) | C212—H21B | 0.97 (3) |
N111—C211 | 1.464 (4) | C212—H21C | 0.94 (4) |
C111—H111 | 0.90 (3) | N422—C122 | 1.311 (4) |
C211—H21A | 0.99 (4) | N422—N322 | 1.368 (3) |
C211—H21B | 0.94 (4) | N322—N222 | 1.292 (4) |
C211—H21C | 0.91 (4) | N222—N122 | 1.358 (3) |
N421—C121 | 1.321 (4) | N122—C122 | 1.324 (4) |
N421—N321 | 1.376 (3) | N122—C222 | 1.466 (4) |
N321—N221 | 1.289 (4) | C122—H122 | 0.89 (3) |
N221—N121 | 1.351 (3) | C222—H22A | 0.88 (4) |
N121—C121 | 1.331 (4) | C222—H22B | 0.89 (4) |
N121—C221 | 1.458 (4) | C222—H23C | 1.04 (4) |
C121—H121 | 0.88 (4) | N432—C132 | 1.319 (4) |
C221—H22A | 1.04 (5) | N432—N332 | 1.374 (3) |
C221—H22B | 0.95 (5) | N332—N232 | 1.295 (3) |
C221—H22C | 0.99 (5) | N232—N132 | 1.356 (3) |
N431—C131 | 1.325 (4) | N132—C132 | 1.334 (4) |
N431—N331 | 1.368 (3) | N132—C232 | 1.454 (4) |
N331—N231 | 1.292 (3) | C132—H133 | 0.90 (3) |
N231—N131 | 1.358 (3) | C232—H23A | 0.96 (4) |
N131—C131 | 1.322 (4) | C232—H23B | 0.93 (4) |
N131—C231 | 1.462 (4) | C232—H23C | 0.98 (4) |
C131—H131 | 0.84 (3) | B1—F11 | 1.387 (4) |
C231—H23A | 0.88 (5) | B1—F21 | 1.390 (4) |
C231—H23B | 0.96 (4) | B1—F41 | 1.397 (4) |
C231—H23C | 0.91 (3) | B1—F31 | 1.402 (4) |
Fe2—N412ii | 2.183 (2) | B2—F22 | 1.389 (4) |
Fe2—N412 | 2.183 (2) | B2—F42 | 1.395 (3) |
Fe2—N422 | 2.187 (2) | B2—F12 | 1.400 (4) |
Fe2—N422ii | 2.187 (2) | B2—F32 | 1.401 (4) |
| | | |
N411—Fe1—N411i | 180.0 | N412ii—Fe2—N432 | 88.78 (9) |
N411—Fe1—N421i | 89.22 (10) | N412—Fe2—N432 | 91.22 (9) |
N411i—Fe1—N421i | 90.78 (10) | N422—Fe2—N432 | 89.62 (9) |
N411—Fe1—N421 | 90.78 (10) | N422ii—Fe2—N432 | 90.38 (9) |
N411i—Fe1—N421 | 89.22 (10) | N412ii—Fe2—N432ii | 91.22 (9) |
N421i—Fe1—N421 | 180.0 | N412—Fe2—N432ii | 88.78 (9) |
N411—Fe1—N431 | 89.97 (9) | N422—Fe2—N432ii | 90.38 (9) |
N411i—Fe1—N431 | 90.03 (9) | N422ii—Fe2—N432ii | 89.62 (9) |
N421i—Fe1—N431 | 90.27 (10) | N432—Fe2—N432ii | 180.0 |
N421—Fe1—N431 | 89.73 (10) | C112—N412—N312 | 106.1 (2) |
N411—Fe1—N431i | 90.03 (9) | C112—N412—Fe2 | 130.0 (2) |
N411i—Fe1—N431i | 89.97 (9) | N312—N412—Fe2 | 123.7 (2) |
N421i—Fe1—N431i | 89.73 (10) | N212—N312—N412 | 109.7 (2) |
N421—Fe1—N431i | 90.27 (10) | N312—N212—N112 | 106.8 (2) |
N431—Fe1—N431i | 180.0 | C112—N112—N212 | 108.8 (2) |
C111—N411—N311 | 106.1 (2) | C112—N112—C212 | 129.8 (3) |
C111—N411—Fe1 | 128.7 (2) | N212—N112—C212 | 120.8 (2) |
N311—N411—Fe1 | 124.5 (2) | N412—C112—N112 | 108.7 (3) |
N211—N311—N411 | 109.9 (2) | N412—C112—H112 | 122 (2) |
N311—N211—N111 | 106.3 (2) | N112—C112—H112 | 129 (2) |
C111—N111—N211 | 109.0 (2) | N112—C212—H21A | 106 (2) |
C111—N111—C211 | 129.5 (3) | N112—C212—H21B | 108.3 (19) |
N211—N111—C211 | 121.4 (2) | H21A—C212—H21B | 112 (3) |
N411—C111—N111 | 108.8 (3) | N112—C212—H21C | 109 (2) |
N411—C111—H111 | 128 (2) | H21A—C212—H21C | 112 (3) |
N111—C111—H111 | 124 (2) | H21B—C212—H21C | 111 (3) |
N111—C211—H21A | 112 (2) | C122—N422—N322 | 106.5 (2) |
N111—C211—H21B | 108 (3) | C122—N422—Fe2 | 128.5 (2) |
H21A—C211—H21B | 112 (3) | N322—N422—Fe2 | 124.2 (2) |
N111—C211—H21C | 105 (2) | N222—N322—N422 | 109.6 (2) |
H21A—C211—H21C | 112 (3) | N322—N222—N122 | 106.7 (2) |
H21B—C211—H21C | 107 (3) | C122—N122—N222 | 108.3 (2) |
C121—N421—N321 | 105.8 (2) | C122—N122—C222 | 130.1 (3) |
C121—N421—Fe1 | 130.0 (2) | N222—N122—C222 | 121.5 (2) |
N321—N421—Fe1 | 124.1 (2) | N422—C122—N122 | 108.8 (3) |
N221—N321—N421 | 109.8 (2) | N422—C122—H122 | 127 (2) |
N321—N221—N121 | 107.3 (2) | N122—C122—H122 | 125 (2) |
C121—N121—N221 | 108.3 (2) | N122—C222—H22A | 113 (2) |
C121—N121—C221 | 129.9 (2) | N122—C222—H22B | 108 (3) |
N221—N121—C221 | 121.6 (2) | H22A—C222—H22B | 116 (3) |
N421—C121—N121 | 108.8 (2) | N122—C222—H23C | 104 (2) |
N421—C121—H121 | 125 (2) | H22A—C222—H23C | 100 (3) |
N121—C121—H121 | 126 (2) | H22B—C222—H23C | 115 (3) |
N121—C221—H22A | 105 (2) | C132—N432—N332 | 106.2 (2) |
N121—C221—H22B | 111 (3) | C132—N432—Fe2 | 130.5 (2) |
H22A—C221—H22B | 108 (4) | N332—N432—Fe2 | 122.9 (2) |
N121—C221—H22C | 113 (3) | N232—N332—N432 | 109.9 (2) |
H22A—C221—H22C | 109 (4) | N332—N232—N132 | 106.7 (2) |
H22B—C221—H22C | 112 (4) | C132—N132—N232 | 108.6 (2) |
C131—N431—N331 | 105.8 (2) | C132—N132—C232 | 130.4 (3) |
C131—N431—Fe1 | 129.9 (2) | N232—N132—C232 | 120.9 (2) |
N331—N431—Fe1 | 124.1 (2) | N432—C132—N132 | 108.5 (3) |
N231—N331—N431 | 110.2 (2) | N432—C132—H133 | 124 (2) |
N331—N231—N131 | 106.5 (2) | N132—C132—H133 | 128 (2) |
C131—N131—N231 | 108.6 (2) | N132—C232—H23A | 113 (2) |
C131—N131—C231 | 129.8 (3) | N132—C232—H23B | 110 (2) |
N231—N131—C231 | 121.5 (2) | H23A—C232—H23B | 108 (3) |
N131—C131—N431 | 108.8 (3) | N132—C232—H23C | 107 (2) |
N131—C131—H131 | 123 (2) | H23A—C232—H23C | 109 (3) |
N431—C131—H131 | 128 (2) | H23B—C232—H23C | 110 (3) |
N131—C231—H23A | 106 (3) | F11—B1—F21 | 110.1 (3) |
N131—C231—H23B | 108 (2) | F11—B1—F41 | 110.1 (3) |
H23A—C231—H23B | 111 (3) | F21—B1—F41 | 110.6 (2) |
N131—C231—H23C | 111.0 (19) | F11—B1—F31 | 109.0 (2) |
H23A—C231—H23C | 113 (3) | F21—B1—F31 | 108.7 (3) |
H23B—C231—H23C | 108 (3) | F41—B1—F31 | 108.3 (3) |
N412ii—Fe2—N412 | 180.0 | F22—B2—F42 | 110.0 (2) |
N412ii—Fe2—N422 | 90.81 (9) | F22—B2—F12 | 109.2 (2) |
N412—Fe2—N422 | 89.19 (9) | F42—B2—F12 | 109.9 (2) |
N412ii—Fe2—N422ii | 89.19 (9) | F22—B2—F32 | 109.5 (2) |
N412—Fe2—N422ii | 90.81 (9) | F42—B2—F32 | 109.1 (2) |
N422—Fe2—N422ii | 180.0 | F12—B2—F32 | 109.1 (2) |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z. |
Crystal data top
C12H24B2F8FeN24 | V = 2957.3 (7) Å3 |
Mr = 734.02 | Z = 4 |
a = 17.207 (2) Å | F(000) = 1488 |
b = 10.2140 (14) Å | Dx = 1.649 Mg m−3 |
c = 18.406 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
α = 90° | µ = 0.61 mm−1 |
β = 113.912 (15)° | T = 10 K |
γ = 90° | 0.7 × 0.5 × 0.2 mm |
Data collection top
Radiation source: fine-focus sealed tube | Rint = 0.072 |
Graphite monochromator | θmax = 28.0°, θmin = 3.3° |
34261 measured reflections | h = −21→21 |
6057 independent reflections | k = −12→5 |
4245 reflections with I > 2σ(I) | l = −23→23 |
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)] = 0.055 | H-atom parameters not defined? |
wR(F2) = 0.156 | Calculated w = 1/[σ2(Fo2) + (0.0737P)2 + 3.966P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | Δρmax = 0.56 e Å−3 |
6057 reflections | Δρmin = −0.81 e Å−3 |
524 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0024 (6) |
Primary atom site location: structure-invariant direct methods | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Refinement on F2 for ALL reflections except for 0 with very negative F2
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F2, conventional R-factors R
are based on F, with F set to zero for negative F2. The observed criterion
of F2 > 2sigma(F2) is used only for calculating _R_factor_obs 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 | |
Fe1 | 0.0000 | 0.0000 | 0.0000 | 0.0100 (2) | |
N411 | 0.0695 (2) | 0.1120 (3) | −0.0420 (2) | 0.0128 (7) | |
N311 | 0.1357 (2) | 0.1905 (4) | 0.0038 (2) | 0.0184 (7) | |
N211 | 0.1755 (2) | 0.2321 (3) | −0.0380 (2) | 0.0183 (7) | |
N111 | 0.1353 (2) | 0.1799 (3) | −0.1115 (2) | 0.0147 (7) | |
C111 | 0.0706 (2) | 0.1086 (4) | −0.1132 (2) | 0.0138 (8) | |
H111 | 0.031 (3) | 0.066 (5) | −0.155 (3) | 0.024 (12)* | |
C211 | 0.1617 (3) | 0.2091 (5) | −0.1761 (2) | 0.0179 (9) | |
H21A | 0.219 (3) | 0.179 (5) | −0.162 (3) | 0.043 (15)* | |
H21B | 0.157 (3) | 0.301 (5) | −0.181 (2) | 0.011 (10)* | |
H21C | 0.125 (2) | 0.172 (4) | −0.217 (2) | 0.007 (9)* | |
N421 | −0.0731 (2) | 0.1570 (3) | −0.0008 (2) | 0.0148 (7) | |
N321 | −0.1242 (2) | 0.1614 (3) | 0.0404 (2) | 0.0166 (7) | |
N221 | −0.1655 (2) | 0.2704 (4) | 0.0257 (2) | 0.0174 (7) | |
N121 | −0.1415 (2) | 0.3383 (3) | −0.0255 (2) | 0.0148 (7) | |
C121 | −0.0853 (2) | 0.2677 (4) | −0.0404 (2) | 0.0148 (8) | |
H121 | −0.064 (3) | 0.286 (4) | −0.070 (3) | 0.021 (12)* | |
C221 | −0.1718 (3) | 0.4717 (5) | −0.0500 (2) | 0.0201 (9) | |
H22A | −0.156 (5) | 0.495 (7) | −0.088 (4) | 0.08 (2)* | |
H22B | −0.230 (3) | 0.477 (5) | −0.069 (3) | 0.027 (12)* | |
H22C | −0.141 (5) | 0.534 (8) | −0.007 (5) | 0.11 (3)* | |
N431 | 0.0806 (2) | 0.0453 (3) | 0.1135 (2) | 0.0141 (7) | |
N331 | 0.1418 (2) | −0.0360 (3) | 0.1633 (2) | 0.0148 (7) | |
N231 | 0.1864 (2) | 0.0223 (3) | 0.2286 (2) | 0.0176 (7) | |
N131 | 0.1546 (2) | 0.1449 (3) | 0.2228 (2) | 0.0141 (7) | |
C131 | 0.0897 (2) | 0.1578 (4) | 0.1526 (2) | 0.0148 (8) | |
H131 | 0.064 (2) | 0.236 (4) | 0.137 (2) | 0.007 (10)* | |
C231 | 0.1886 (2) | 0.2396 (4) | 0.2881 (2) | 0.0170 (8) | |
H23A | 0.159 (3) | 0.324 (5) | 0.272 (2) | 0.021 (11)* | |
H23B | 0.174 (3) | 0.211 (5) | 0.330 (3) | 0.026 (12)* | |
H23C | 0.246 (3) | 0.246 (4) | 0.305 (2) | 0.008 (9)* | |
Fe2 | 0.5000 | 0.0000 | 0.0000 | 0.0109 (2) | |
N412 | 0.4413 (2) | 0.1229 (3) | −0.0910 (2) | 0.0147 (7) | |
N312 | 0.3938 (2) | 0.2284 (3) | −0.0868 (2) | 0.0157 (7) | |
N212 | 0.3652 (2) | 0.2925 (4) | −0.1533 (2) | 0.0183 (8) | |
N112 | 0.3935 (2) | 0.2262 (3) | −0.2019 (2) | 0.0139 (7) | |
C112 | 0.4398 (2) | 0.1252 (4) | −0.1631 (2) | 0.0151 (8) | |
H112 | 0.470 (2) | 0.072 (4) | −0.179 (2) | 0.005 (9)* | |
C212 | 0.3811 (3) | 0.2801 (5) | −0.2798 (2) | 0.0188 (9) | |
H21A | 0.431 (3) | 0.340 (5) | −0.269 (3) | 0.026 (12)* | |
H21B | 0.380 (3) | 0.202 (5) | −0.316 (3) | 0.035 (13)* | |
H21C | 0.321 (3) | 0.314 (5) | −0.304 (3) | 0.038 (14)* | |
N422 | 0.5759 (2) | 0.1485 (4) | 0.0612 (2) | 0.0161 (7) | |
N322 | 0.6226 (2) | 0.1472 (4) | 0.1417 (2) | 0.0168 (7) | |
N222 | 0.6709 (2) | 0.2490 (4) | 0.1622 (2) | 0.0179 (7) | |
N122 | 0.6552 (2) | 0.3186 (3) | 0.0952 (2) | 0.0141 (7) | |
C122 | 0.5978 (2) | 0.2566 (4) | 0.0348 (2) | 0.0144 (8) | |
H122 | 0.575 (2) | 0.290 (4) | −0.019 (2) | 0.006 (9)* | |
C222 | 0.6990 (3) | 0.4428 (4) | 0.0976 (2) | 0.0172 (8) | |
H22A | 0.672 (3) | 0.485 (4) | 0.052 (2) | 0.011 (10)* | |
H22B | 0.751 (3) | 0.439 (5) | 0.098 (3) | 0.035 (14)* | |
H23C | 0.705 (3) | 0.495 (4) | 0.145 (3) | 0.018 (11)* | |
N432 | 0.4170 (2) | 0.0432 (3) | 0.0490 (2) | 0.0150 (7) | |
N332 | 0.3593 (2) | −0.0463 (3) | 0.0538 (2) | 0.0160 (7) | |
N232 | 0.3196 (2) | 0.0039 (3) | 0.0932 (2) | 0.0161 (7) | |
N132 | 0.3503 (2) | 0.1254 (3) | 0.1152 (2) | 0.0133 (7) | |
C132 | 0.4097 (2) | 0.1483 (4) | 0.0879 (2) | 0.0159 (8) | |
H133 | 0.438 (2) | 0.221 (4) | 0.096 (2) | 0.003 (9)* | |
C232 | 0.3218 (2) | 0.2054 (4) | 0.1650 (2) | 0.0154 (8) | |
H23A | 0.264 (3) | 0.235 (5) | 0.136 (3) | 0.023 (11)* | |
H23B | 0.323 (3) | 0.159 (5) | 0.204 (3) | 0.030 (13)* | |
H23C | 0.361 (2) | 0.283 (4) | 0.188 (2) | 0.007 (9)* | |
B1 | 0.4488 (3) | 0.4994 (5) | 0.1436 (2) | 0.0145 (9) | |
F11 | 0.37172 (13) | 0.4500 (2) | 0.08997 (11) | 0.0193 (5) | |
F21 | 0.45344 (13) | 0.6329 (2) | 0.13204 (11) | 0.0187 (5) | |
F31 | 0.45556 (13) | 0.4779 (2) | 0.22126 (11) | 0.0186 (5) | |
F41 | 0.51535 (13) | 0.4329 (2) | 0.13410 (13) | 0.0217 (5) | |
B2 | −0.0041 (3) | 0.5138 (5) | 0.1662 (2) | 0.0144 (9) | |
F12 | 0.01330 (13) | 0.4452 (2) | 0.10821 (12) | 0.0182 (5) | |
F22 | 0.02077 (13) | 0.6436 (2) | 0.16672 (11) | 0.0181 (5) | |
F32 | 0.04182 (13) | 0.4574 (2) | 0.24033 (11) | 0.0175 (5) | |
F42 | −0.09067 (13) | 0.5080 (2) | 0.14841 (12) | 0.0181 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0098 (3) | 0.0131 (5) | 0.0077 (3) | 0.0002 (3) | 0.0042 (2) | 0.0004 (3) |
N411 | 0.0125 (14) | 0.014 (2) | 0.0105 (13) | 0.0016 (13) | 0.0032 (11) | −0.0032 (12) |
N311 | 0.019 (2) | 0.022 (2) | 0.0143 (14) | −0.0039 (15) | 0.0065 (12) | −0.0006 (13) |
N211 | 0.022 (2) | 0.017 (2) | 0.0127 (14) | −0.0050 (15) | 0.0035 (12) | −0.0001 (13) |
N111 | 0.0167 (15) | 0.015 (2) | 0.0114 (13) | −0.0013 (14) | 0.0050 (11) | −0.0006 (13) |
C111 | 0.012 (2) | 0.015 (2) | 0.014 (2) | 0.001 (2) | 0.0049 (14) | 0.001 (2) |
C211 | 0.022 (2) | 0.021 (3) | 0.015 (2) | −0.004 (2) | 0.012 (2) | 0.000 (2) |
N421 | 0.0153 (14) | 0.020 (2) | 0.0103 (13) | −0.0049 (14) | 0.0068 (11) | −0.0018 (13) |
N321 | 0.0166 (15) | 0.020 (2) | 0.0150 (14) | 0.0001 (15) | 0.0085 (12) | −0.0016 (13) |
N221 | 0.019 (2) | 0.022 (2) | 0.0114 (14) | −0.0040 (15) | 0.0061 (12) | −0.0022 (13) |
N121 | 0.0182 (15) | 0.015 (2) | 0.0102 (13) | −0.0038 (14) | 0.0043 (11) | −0.0007 (12) |
C121 | 0.019 (2) | 0.017 (2) | 0.009 (2) | −0.004 (2) | 0.0059 (14) | −0.0017 (15) |
C221 | 0.022 (2) | 0.019 (3) | 0.017 (2) | 0.002 (2) | 0.005 (2) | −0.001 (2) |
N431 | 0.0129 (14) | 0.014 (2) | 0.0198 (15) | −0.0008 (13) | 0.0106 (12) | 0.0021 (13) |
N331 | 0.0122 (14) | 0.018 (2) | 0.0136 (14) | 0.0015 (13) | 0.0046 (11) | 0.0034 (13) |
N231 | 0.0155 (15) | 0.019 (2) | 0.021 (2) | 0.0013 (14) | 0.0104 (12) | 0.0027 (14) |
N131 | 0.0121 (14) | 0.013 (2) | 0.0186 (14) | 0.0013 (13) | 0.0078 (12) | 0.0018 (13) |
C131 | 0.016 (2) | 0.012 (2) | 0.017 (2) | −0.001 (2) | 0.0072 (14) | 0.001 (2) |
C231 | 0.016 (2) | 0.015 (2) | 0.019 (2) | 0.000 (2) | 0.0061 (15) | −0.002 (2) |
Fe2 | 0.0111 (3) | 0.0144 (5) | 0.0084 (3) | −0.0012 (3) | 0.0053 (3) | −0.0005 (3) |
N412 | 0.0157 (15) | 0.017 (2) | 0.0145 (14) | −0.0026 (14) | 0.0093 (12) | −0.0029 (13) |
N312 | 0.0155 (15) | 0.015 (2) | 0.0178 (15) | 0.0008 (14) | 0.0080 (12) | −0.0012 (13) |
N212 | 0.016 (2) | 0.025 (2) | 0.0163 (15) | 0.0006 (14) | 0.0088 (12) | −0.0019 (14) |
N112 | 0.0154 (15) | 0.014 (2) | 0.0150 (14) | 0.0005 (14) | 0.0089 (12) | −0.0015 (13) |
C112 | 0.016 (2) | 0.013 (2) | 0.019 (2) | 0.001 (2) | 0.0096 (15) | −0.001 (2) |
C212 | 0.021 (2) | 0.025 (3) | 0.013 (2) | 0.003 (2) | 0.0086 (15) | 0.003 (2) |
N422 | 0.0161 (15) | 0.026 (2) | 0.0086 (13) | 0.0059 (14) | 0.0072 (11) | 0.0022 (13) |
N322 | 0.0154 (15) | 0.025 (2) | 0.0093 (13) | −0.0004 (15) | 0.0044 (11) | −0.0014 (13) |
N222 | 0.020 (2) | 0.022 (2) | 0.0135 (14) | 0.003 (2) | 0.0087 (12) | 0.0025 (14) |
N122 | 0.0149 (14) | 0.018 (2) | 0.0106 (13) | 0.0033 (14) | 0.0062 (11) | 0.0001 (12) |
C122 | 0.016 (2) | 0.020 (2) | 0.009 (2) | 0.000 (2) | 0.0074 (13) | 0.0012 (15) |
C222 | 0.020 (2) | 0.015 (2) | 0.016 (2) | 0.001 (2) | 0.007 (2) | 0.002 (2) |
N432 | 0.0141 (14) | 0.019 (2) | 0.0113 (13) | −0.0003 (14) | 0.0044 (11) | 0.0015 (13) |
N332 | 0.0169 (15) | 0.016 (2) | 0.0168 (15) | −0.0046 (14) | 0.0090 (12) | −0.0013 (13) |
N232 | 0.0182 (15) | 0.015 (2) | 0.0158 (14) | −0.0010 (14) | 0.0076 (12) | −0.0002 (13) |
N132 | 0.0148 (14) | 0.013 (2) | 0.0122 (13) | −0.0020 (13) | 0.0051 (11) | −0.0017 (12) |
C132 | 0.016 (2) | 0.019 (2) | 0.014 (2) | −0.005 (2) | 0.0072 (14) | −0.003 (2) |
C232 | 0.017 (2) | 0.019 (2) | 0.012 (2) | 0.003 (2) | 0.0078 (14) | −0.001 (2) |
B1 | 0.017 (2) | 0.014 (3) | 0.013 (2) | 0.002 (2) | 0.0056 (15) | 0.000 (2) |
F11 | 0.0197 (11) | 0.0216 (14) | 0.0141 (10) | −0.0035 (10) | 0.0043 (8) | −0.0004 (9) |
F21 | 0.0188 (11) | 0.0221 (14) | 0.0143 (10) | −0.0010 (10) | 0.0058 (8) | 0.0021 (9) |
F31 | 0.0206 (11) | 0.0254 (15) | 0.0102 (9) | −0.0002 (10) | 0.0068 (8) | 0.0018 (9) |
F41 | 0.0202 (11) | 0.0212 (15) | 0.0291 (12) | 0.0032 (10) | 0.0157 (10) | −0.0026 (10) |
B2 | 0.017 (2) | 0.013 (3) | 0.014 (2) | 0.002 (2) | 0.0068 (15) | 0.002 (2) |
F12 | 0.0216 (11) | 0.0195 (14) | 0.0148 (10) | 0.0002 (10) | 0.0085 (8) | −0.0019 (9) |
F22 | 0.0197 (11) | 0.0194 (14) | 0.0163 (10) | −0.0014 (10) | 0.0087 (8) | 0.0011 (9) |
F32 | 0.0180 (10) | 0.0215 (14) | 0.0132 (10) | 0.0043 (10) | 0.0066 (8) | 0.0050 (9) |
F42 | 0.0150 (10) | 0.0237 (15) | 0.0158 (10) | 0.0006 (10) | 0.0065 (8) | −0.0009 (9) |
Geometric parameters (Å, º) top
Fe1—N411 | 2.021 (3) | Fe2—N432ii | 2.023 (3) |
Fe1—N411i | 2.021 (3) | Fe2—N432 | 2.023 (3) |
Fe1—N421i | 2.034 (3) | N412—C112 | 1.319 (4) |
Fe1—N421 | 2.034 (3) | N412—N312 | 1.373 (4) |
Fe1—N431 | 2.038 (3) | N312—N212 | 1.296 (4) |
Fe1—N431i | 2.038 (3) | N212—N112 | 1.359 (4) |
N411—C111 | 1.319 (4) | N112—C112 | 1.322 (5) |
N411—N311 | 1.367 (4) | N112—C212 | 1.468 (5) |
N311—N211 | 1.292 (4) | C112—H112 | 0.87 (4) |
N211—N111 | 1.354 (4) | C212—H21A | 1.00 (5) |
N111—C111 | 1.319 (5) | C212—H21B | 1.03 (5) |
N111—C211 | 1.466 (4) | C212—H21C | 1.00 (5) |
C111—H111 | 0.91 (5) | N422—C122 | 1.321 (5) |
C211—H21A | 0.97 (5) | N422—N322 | 1.369 (4) |
C211—H21B | 0.95 (4) | N322—N222 | 1.288 (5) |
C211—H21C | 0.86 (4) | N222—N122 | 1.353 (4) |
N421—C121 | 1.315 (5) | N122—C122 | 1.313 (5) |
N421—N321 | 1.376 (4) | N122—C222 | 1.468 (5) |
N321—N221 | 1.289 (5) | C122—H122 | 0.96 (4) |
N221—N121 | 1.361 (4) | C222—H22A | 0.89 (4) |
N121—C121 | 1.321 (5) | C222—H22B | 0.89 (5) |
N121—C221 | 1.463 (5) | C222—H23C | 1.00 (4) |
C121—H121 | 0.79 (4) | N432—C132 | 1.325 (5) |
C221—H22A | 0.89 (7) | N432—N332 | 1.378 (4) |
C221—H22B | 0.91 (5) | N332—N232 | 1.289 (4) |
C221—H22C | 0.98 (8) | N232—N132 | 1.345 (5) |
N431—C131 | 1.331 (5) | N132—C132 | 1.329 (5) |
N431—N331 | 1.363 (4) | N132—C232 | 1.454 (5) |
N331—N231 | 1.281 (4) | C132—H133 | 0.87 (4) |
N231—N131 | 1.353 (5) | C232—H23A | 0.97 (4) |
N131—C131 | 1.328 (5) | C232—H23B | 0.86 (5) |
N131—C231 | 1.468 (5) | C232—H23C | 1.01 (4) |
C131—H131 | 0.90 (4) | B1—F11 | 1.387 (5) |
C231—H23A | 0.99 (5) | B1—F21 | 1.388 (5) |
C231—H23B | 0.95 (4) | B1—F31 | 1.404 (4) |
C231—H23C | 0.91 (4) | B1—F41 | 1.402 (5) |
Fe2—N412ii | 2.007 (3) | B2—F22 | 1.392 (5) |
Fe2—N412 | 2.007 (3) | B2—F42 | 1.391 (5) |
Fe2—N422ii | 2.021 (3) | B2—F32 | 1.395 (4) |
Fe2—N422 | 2.021 (3) | B2—F12 | 1.406 (5) |
| | | |
N411—Fe1—N411i | 180.0 | N412ii—Fe2—N432ii | 91.59 (12) |
N411—Fe1—N421i | 89.39 (12) | N412—Fe2—N432ii | 88.41 (12) |
N411i—Fe1—N421i | 90.61 (12) | N422ii—Fe2—N432ii | 90.07 (12) |
N411—Fe1—N421 | 90.61 (12) | N422—Fe2—N432ii | 89.93 (12) |
N411i—Fe1—N421 | 89.39 (12) | N412ii—Fe2—N432 | 88.41 (12) |
N421i—Fe1—N421 | 180.0 | N412—Fe2—N432 | 91.59 (12) |
N411—Fe1—N431 | 90.02 (11) | N422ii—Fe2—N432 | 89.93 (12) |
N411i—Fe1—N431 | 89.98 (11) | N422—Fe2—N432 | 90.07 (12) |
N421i—Fe1—N431 | 90.53 (12) | N432ii—Fe2—N432 | 180.0 |
N421—Fe1—N431 | 89.47 (12) | C112—N412—N312 | 105.9 (3) |
N411—Fe1—N431i | 89.98 (11) | C112—N412—Fe2 | 130.4 (3) |
N411i—Fe1—N431i | 90.02 (11) | N312—N412—Fe2 | 123.7 (2) |
N421i—Fe1—N431i | 89.47 (12) | N212—N312—N412 | 110.5 (3) |
N421—Fe1—N431i | 90.53 (12) | N312—N212—N112 | 105.6 (3) |
N431—Fe1—N431i | 180.0 | C112—N112—N212 | 109.4 (3) |
C111—N411—N311 | 106.5 (3) | C112—N112—C212 | 129.5 (3) |
C111—N411—Fe1 | 127.9 (3) | N212—N112—C212 | 120.4 (3) |
N311—N411—Fe1 | 124.8 (2) | N412—C112—N112 | 108.6 (3) |
N211—N311—N411 | 109.7 (3) | N412—C112—H112 | 123 (2) |
N311—N211—N111 | 106.5 (3) | N112—C112—H112 | 128 (2) |
C111—N111—N211 | 109.1 (3) | N112—C212—H21A | 105 (2) |
C111—N111—C211 | 129.0 (3) | N112—C212—H21B | 107 (3) |
N211—N111—C211 | 121.9 (3) | H21A—C212—H21B | 113 (4) |
N111—C111—N411 | 108.3 (3) | N112—C212—H21C | 107 (3) |
N111—C111—H111 | 129 (3) | H21A—C212—H21C | 121 (4) |
N411—C111—H111 | 123 (3) | H21B—C212—H21C | 103 (4) |
N111—C211—H21A | 110 (3) | C122—N422—N322 | 106.1 (3) |
N111—C211—H21B | 104 (2) | C122—N422—Fe2 | 129.6 (2) |
H21A—C211—H21B | 113 (4) | N322—N422—Fe2 | 124.0 (3) |
N111—C211—H21C | 105 (3) | N222—N322—N422 | 109.6 (3) |
H21A—C211—H21C | 114 (4) | N322—N222—N122 | 106.9 (3) |
H21B—C211—H21C | 110 (4) | C122—N122—N222 | 108.8 (3) |
C121—N421—N321 | 106.4 (3) | C122—N122—C222 | 130.1 (3) |
C121—N421—Fe1 | 129.9 (2) | N222—N122—C222 | 121.2 (3) |
N321—N421—Fe1 | 123.6 (2) | N122—C122—N422 | 108.7 (3) |
N221—N321—N421 | 109.5 (3) | N122—C122—H122 | 124 (2) |
N321—N221—N121 | 106.8 (3) | N422—C122—H122 | 128 (2) |
C121—N121—N221 | 108.6 (3) | N122—C222—H22A | 109 (3) |
C121—N121—C221 | 130.0 (3) | N122—C222—H22B | 117 (4) |
N221—N121—C221 | 121.2 (3) | H22A—C222—H22B | 100 (4) |
N421—C121—N121 | 108.7 (3) | N122—C222—H23C | 111 (2) |
N421—C121—H121 | 125 (3) | H22A—C222—H23C | 113 (4) |
N121—C121—H121 | 127 (3) | H22B—C222—H23C | 106 (4) |
N121—C221—H22A | 108 (4) | C132—N432—N332 | 105.9 (3) |
N121—C221—H22B | 112 (3) | C132—N432—Fe2 | 131.1 (3) |
H22A—C221—H22B | 109 (5) | N332—N432—Fe2 | 122.7 (2) |
N121—C221—H22C | 110 (5) | N232—N332—N432 | 109.4 (3) |
H22A—C221—H22C | 103 (6) | N332—N232—N132 | 107.6 (3) |
H22B—C221—H22C | 115 (5) | C132—N132—N232 | 108.5 (3) |
C131—N431—N331 | 105.8 (3) | C132—N132—C232 | 130.2 (4) |
C131—N431—Fe1 | 129.2 (3) | N232—N132—C232 | 121.1 (3) |
N331—N431—Fe1 | 124.8 (2) | N432—C132—N132 | 108.5 (4) |
N231—N331—N431 | 110.8 (3) | N432—C132—H133 | 128 (2) |
N331—N231—N131 | 106.6 (3) | N132—C132—H133 | 123 (2) |
C131—N131—N231 | 108.9 (3) | N132—C232—H23A | 111 (3) |
C131—N131—C231 | 129.0 (3) | N132—C232—H23B | 109 (3) |
N231—N131—C231 | 122.1 (3) | H23A—C232—H23B | 108 (4) |
N131—C131—N431 | 108.0 (4) | N132—C232—H23C | 111 (2) |
N131—C131—H131 | 121 (2) | H23A—C232—H23C | 111 (4) |
N431—C131—H131 | 131 (2) | H23B—C232—H23C | 107 (4) |
N131—C231—H23A | 110 (2) | F11—B1—F21 | 110.3 (3) |
N131—C231—H23B | 108 (3) | F11—B1—F31 | 109.2 (3) |
H23A—C231—H23B | 104 (4) | F21—B1—F31 | 108.8 (3) |
N131—C231—H23C | 110 (2) | F11—B1—F41 | 109.2 (3) |
H23A—C231—H23C | 114 (4) | F21—B1—F41 | 110.9 (3) |
H23B—C231—H23C | 111 (3) | F31—B1—F41 | 108.4 (3) |
N412ii—Fe2—N412 | 180.0 | F22—B2—F42 | 109.8 (3) |
N412ii—Fe2—N422ii | 89.34 (13) | F22—B2—F32 | 109.6 (3) |
N412—Fe2—N422ii | 90.66 (13) | F42—B2—F32 | 109.9 (3) |
N412ii—Fe2—N422 | 90.66 (13) | F22—B2—F12 | 108.7 (3) |
N412—Fe2—N422 | 89.34 (13) | F42—B2—F12 | 109.7 (3) |
N422ii—Fe2—N422 | 180.0 | F32—B2—F12 | 109.0 (3) |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z. |
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