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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889801000462/zm0081sup1.cif
Contains datablocks hs100, hs50, ls100

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889801000462/zm0081hs100sup2.hkl
fmtzb1_10K 100% HS after LIESST from 100% LS in P2(1)/n'

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889801000462/zm0081hs50sup3.hkl
fmtzb1_10Ks in P2(1)/n

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0021889801000462/zm0081ls100sup4.hkl
fmtzb1 LS(100%)_10K after 630nm from 50%LS in 10K in P2(1)/n

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0021889801000462/zm0081sup5.pdf
Bond angles and bond lengths

CCDC references: 214222; 214223; 214224

Computing details top

For all compounds, program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993).

(hs100) top
Crystal data top
C12H24B2F8FeN24Z = 4
Mr = 734.02F(000) = 1488
Monoclinic, P21/nDx = 1.615 Mg m3
a = 17.566 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.0964 (8) ŵ = 0.60 mm1
c = 18.696 (2) ÅT = 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 tubeRint = 0.089
Graphite monochromatorθmax = 28.1°, θmin = 3.3°
44836 measured reflectionsh = 2222
6430 independent reflectionsk = 125
4581 reflections with I > 2σ(I)l = 2323
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)] = 0.056H-atom parameters not defined?
wR(F2) = 0.147Calculated w = 1/[σ2(Fo2) + (0.0612P)2 + 7.9846P]
where P = (Fo2 + 2Fc2)/3
S = 1.08Δρmax = 0.50 e Å3
6430 reflectionsΔρmin = 0.71 e Å3
524 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction 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
xyzUiso*/Ueq
Fe10.00000.00000.00000.00915 (10)
N4110.07511 (11)0.1168 (2)0.04332 (10)0.0108 (4)
N3110.14760 (12)0.1809 (2)0.00324 (11)0.0146 (5)
N2110.18791 (12)0.2146 (2)0.03851 (11)0.0146 (5)
N1110.14156 (11)0.1703 (2)0.11274 (10)0.0124 (5)
C1110.07363 (13)0.1131 (3)0.11432 (13)0.0131 (5)
H1110.0328 (16)0.072 (3)0.1557 (15)0.014 (7)*
C2110.16806 (14)0.1940 (3)0.17646 (13)0.0167 (6)
H21A0.2266 (15)0.162 (3)0.1609 (14)0.011 (7)*
H21B0.168 (2)0.287 (4)0.1849 (19)0.038 (10)*
H21C0.1293 (15)0.152 (3)0.2188 (15)0.012 (7)*
N4210.07674 (11)0.1697 (2)0.00322 (10)0.0118 (5)
N3210.12894 (11)0.1764 (2)0.03459 (11)0.0144 (5)
N2210.16866 (12)0.2879 (2)0.01903 (11)0.0137 (5)
N1210.14314 (11)0.3554 (2)0.02974 (10)0.0123 (5)
C1210.08752 (14)0.2823 (3)0.04243 (12)0.0125 (5)
H1210.0625 (18)0.302 (3)0.0725 (17)0.025 (8)*
C2210.17141 (14)0.4907 (3)0.05481 (13)0.0151 (6)
H22A0.165 (3)0.506 (4)0.099 (3)0.066 (14)*
H22B0.226 (2)0.488 (3)0.0641 (19)0.039 (10)*
H22C0.146 (3)0.562 (5)0.013 (3)0.089 (16)*
N4310.08428 (11)0.0517 (2)0.12185 (10)0.0114 (4)
N3310.14633 (11)0.0291 (2)0.17039 (10)0.0128 (5)
N2310.19060 (11)0.0305 (2)0.23589 (11)0.0133 (5)
N1310.15645 (11)0.1521 (2)0.23056 (11)0.0124 (5)
C1310.09212 (13)0.1648 (3)0.16109 (13)0.0129 (5)
H1310.0621 (15)0.241 (3)0.1450 (14)0.011 (7)*
C2310.18854 (14)0.2469 (3)0.29569 (13)0.0158 (6)
H23A0.1564 (18)0.331 (3)0.2777 (16)0.025 (8)*
H23B0.1781 (15)0.209 (3)0.3419 (14)0.010 (6)*
H23C0.2436 (14)0.261 (3)0.3075 (13)0.003 (6)*
Fe20.50000.00000.00000.01023 (11)
N4120.43442 (12)0.1294 (2)0.10039 (11)0.0134 (5)
N3120.39066 (12)0.2401 (2)0.09778 (11)0.0140 (5)
N2120.36321 (12)0.3010 (2)0.16496 (11)0.0149 (5)
N1120.38856 (11)0.2285 (2)0.21208 (10)0.0119 (5)
C1120.43167 (14)0.1252 (3)0.17205 (13)0.0145 (5)
H1120.4609 (18)0.064 (3)0.1892 (17)0.027 (8)*
C2120.37708 (14)0.2780 (3)0.28943 (13)0.0150 (6)
H21A0.4273 (19)0.340 (3)0.2794 (18)0.034 (9)*
H21B0.3752 (14)0.204 (3)0.3196 (13)0.001 (6)*
H21C0.3207 (18)0.319 (3)0.3175 (17)0.028 (8)*
N4220.57820 (12)0.1668 (2)0.06243 (10)0.0132 (5)
N3220.62467 (12)0.1694 (2)0.14193 (11)0.0139 (5)
N2220.67300 (12)0.2721 (2)0.16090 (11)0.0146 (5)
N1220.65769 (11)0.3381 (2)0.09301 (11)0.0119 (5)
C1220.60018 (14)0.2729 (3)0.03421 (12)0.0131 (5)
H1220.5828 (17)0.297 (3)0.0143 (16)0.022 (8)*
C2220.70358 (14)0.4592 (3)0.09313 (14)0.0156 (6)
H22A0.6722 (18)0.512 (3)0.0539 (17)0.023 (8)*
H22B0.7529 (17)0.442 (3)0.0878 (16)0.022 (8)*
H23C0.7189 (17)0.504 (3)0.1439 (16)0.019 (7)*
N4320.41181 (11)0.0467 (2)0.05130 (11)0.0128 (5)
N3320.35662 (11)0.0457 (2)0.05689 (11)0.0138 (5)
N2320.31929 (11)0.0018 (2)0.09785 (11)0.0129 (4)
N1320.34933 (11)0.1257 (2)0.11961 (11)0.0119 (5)
C1320.40535 (14)0.1527 (3)0.09082 (13)0.0136 (5)
H1330.4358 (14)0.227 (3)0.0964 (13)0.000 (6)*
C2320.32108 (14)0.2057 (3)0.16883 (13)0.0137 (6)
H23A0.2638 (16)0.224 (3)0.1413 (15)0.017 (7)*
H23B0.3276 (16)0.162 (3)0.2128 (15)0.015 (7)*
H23C0.3485 (17)0.292 (3)0.1817 (16)0.021 (8)*
B10.4483 (2)0.5044 (3)0.14742 (14)0.0134 (6)
F110.37005 (8)0.4627 (2)0.09452 (8)0.0173 (4)
F210.45754 (8)0.63926 (15)0.13814 (7)0.0156 (3)
F310.45628 (8)0.4821 (2)0.22440 (7)0.0172 (3)
F410.51038 (8)0.4321 (2)0.13604 (8)0.0211 (4)
B20.0075 (2)0.5194 (3)0.16441 (14)0.0123 (6)
F120.00780 (8)0.45079 (15)0.10607 (8)0.0162 (3)
F220.02277 (8)0.64785 (15)0.16913 (7)0.0156 (3)
F320.03449 (8)0.45465 (15)0.23636 (7)0.0156 (3)
F420.09292 (8)0.52131 (15)0.14500 (8)0.0169 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0089 (2)0.0124 (2)0.0068 (2)0.0003 (2)0.00385 (14)0.0002 (2)
N4110.0104 (8)0.0128 (10)0.0084 (7)0.0003 (8)0.0030 (6)0.0007 (7)
N3110.0138 (8)0.0167 (11)0.0144 (8)0.0033 (8)0.0071 (7)0.0025 (8)
N2110.0147 (8)0.0183 (11)0.0106 (8)0.0025 (8)0.0050 (6)0.0013 (8)
N1110.0130 (8)0.0146 (11)0.0098 (8)0.0003 (8)0.0050 (6)0.0000 (7)
C1110.0100 (9)0.0182 (13)0.0102 (9)0.0004 (9)0.0033 (7)0.0006 (9)
C2110.0178 (10)0.0234 (15)0.0134 (9)0.0028 (10)0.0110 (8)0.0020 (9)
N4210.0123 (8)0.0168 (11)0.0073 (7)0.0014 (8)0.0051 (6)0.0008 (7)
N3210.0127 (8)0.0193 (11)0.0135 (8)0.0017 (8)0.0078 (6)0.0011 (8)
N2210.0155 (8)0.0156 (11)0.0120 (8)0.0016 (8)0.0078 (6)0.0010 (7)
N1210.0143 (8)0.0137 (11)0.0096 (8)0.0002 (8)0.0056 (6)0.0008 (7)
C1210.0135 (9)0.0166 (13)0.0077 (9)0.0006 (9)0.0046 (7)0.0015 (8)
C2210.0163 (10)0.0141 (13)0.0135 (9)0.0023 (10)0.0047 (8)0.0001 (9)
N4310.0121 (8)0.0136 (10)0.0097 (8)0.0006 (8)0.0056 (6)0.0005 (7)
N3310.0117 (8)0.0181 (11)0.0080 (7)0.0005 (8)0.0034 (6)0.0016 (7)
N2310.0128 (8)0.0174 (11)0.0102 (8)0.0015 (8)0.0052 (6)0.0010 (7)
N1310.0122 (8)0.0139 (11)0.0108 (8)0.0015 (8)0.0044 (6)0.0010 (7)
C1310.0120 (9)0.0163 (13)0.0113 (9)0.0000 (9)0.0057 (7)0.0004 (9)
C2310.0144 (10)0.0178 (13)0.0132 (10)0.0002 (10)0.0037 (8)0.0056 (9)
Fe20.0098 (2)0.0136 (2)0.0081 (2)0.0003 (2)0.00460 (14)0.0004 (2)
N4120.0152 (8)0.0149 (11)0.0121 (8)0.0010 (8)0.0077 (6)0.0003 (7)
N3120.0130 (8)0.0167 (11)0.0124 (8)0.0003 (8)0.0052 (6)0.0002 (8)
N2120.0147 (8)0.0197 (12)0.0107 (8)0.0001 (8)0.0057 (6)0.0016 (8)
N1120.0106 (8)0.0172 (11)0.0079 (7)0.0025 (8)0.0037 (6)0.0004 (7)
C1120.0143 (9)0.0160 (13)0.0143 (9)0.0005 (9)0.0071 (8)0.0009 (9)
C2120.0195 (10)0.0191 (13)0.0085 (9)0.0023 (10)0.0079 (7)0.0037 (9)
N4220.0165 (8)0.0173 (11)0.0076 (7)0.0010 (8)0.0067 (6)0.0019 (7)
N3220.0129 (8)0.0175 (11)0.0102 (8)0.0006 (8)0.0037 (7)0.0008 (8)
N2220.0158 (8)0.0173 (11)0.0114 (8)0.0002 (8)0.0064 (7)0.0017 (8)
N1220.0118 (8)0.0135 (11)0.0101 (8)0.0016 (8)0.0040 (6)0.0019 (7)
C1220.0138 (9)0.0178 (13)0.0076 (9)0.0006 (9)0.0044 (7)0.0018 (9)
C2220.0154 (10)0.0170 (13)0.0155 (10)0.0009 (9)0.0075 (8)0.0010 (9)
N4320.0133 (8)0.0149 (11)0.0118 (8)0.0011 (8)0.0069 (6)0.0005 (7)
N3320.0151 (8)0.0144 (11)0.0147 (8)0.0000 (8)0.0090 (7)0.0008 (8)
N2320.0131 (8)0.0146 (11)0.0130 (8)0.0000 (8)0.0075 (6)0.0002 (8)
N1320.0123 (8)0.0140 (11)0.0099 (8)0.0009 (8)0.0050 (6)0.0008 (7)
C1320.0133 (9)0.0161 (13)0.0138 (9)0.0026 (9)0.0081 (7)0.0017 (9)
C2320.0154 (9)0.0173 (13)0.0099 (9)0.0016 (9)0.0067 (7)0.0026 (9)
B10.0157 (10)0.0152 (14)0.0107 (10)0.0015 (11)0.0068 (8)0.0016 (10)
F110.0152 (6)0.0207 (8)0.0133 (6)0.0029 (6)0.0031 (5)0.0004 (5)
F210.0156 (6)0.0175 (8)0.0126 (6)0.0010 (6)0.0047 (5)0.0012 (5)
F310.0188 (6)0.0223 (8)0.0102 (5)0.0001 (6)0.0058 (5)0.0039 (5)
F410.0180 (6)0.0209 (8)0.0290 (7)0.0010 (6)0.0142 (5)0.0054 (6)
B20.0135 (10)0.0137 (14)0.0085 (10)0.0017 (10)0.0034 (8)0.0027 (9)
F120.0186 (6)0.0175 (8)0.0137 (6)0.0005 (6)0.0078 (5)0.0037 (5)
F220.0170 (6)0.0165 (8)0.0149 (6)0.0023 (6)0.0081 (5)0.0002 (5)
F320.0158 (6)0.0191 (8)0.0120 (6)0.0016 (6)0.0058 (5)0.0052 (5)
F420.0125 (5)0.0220 (8)0.0161 (6)0.0005 (6)0.0059 (5)0.0004 (6)
Geometric parameters (Å, º) top
Fe1—N411i2.162 (2)Fe2—N412ii2.183 (2)
Fe1—N4112.162 (2)Fe2—N4122.183 (2)
Fe1—N421i2.166 (2)N412—C1121.321 (3)
Fe1—N4212.166 (2)N412—N3121.369 (3)
Fe1—N4312.205 (2)N312—N2121.299 (3)
Fe1—N431i2.205 (2)N212—N1121.355 (3)
N411—C1111.317 (3)N112—C1121.324 (3)
N411—N3111.371 (3)N112—C2121.463 (3)
N311—N2111.298 (3)C112—H1120.94 (3)
N211—N1111.361 (3)C212—H21A1.03 (3)
N111—C1111.315 (3)C212—H21B0.93 (2)
N111—C2111.467 (3)C212—H21C1.00 (3)
C111—H1110.91 (2)N422—C1221.320 (3)
C211—H21A1.00 (3)N422—N3221.368 (2)
C211—H21B0.95 (4)N322—N2221.293 (3)
C211—H21C0.91 (2)N222—N1221.358 (3)
N421—C1211.323 (3)N122—C1221.320 (3)
N421—N3211.372 (3)N122—C2221.464 (3)
N321—N2211.293 (3)C122—H1220.86 (3)
N221—N1211.355 (3)C222—H22A0.89 (3)
N121—C1211.322 (3)C222—H22B0.93 (3)
N121—C2211.463 (3)C222—H23C0.99 (3)
C121—H1210.87 (3)N432—C1321.332 (3)
C221—H22A0.89 (5)N432—N3321.380 (3)
C221—H22B0.89 (4)N332—N2321.289 (3)
C221—H22C1.02 (5)N232—N1321.354 (3)
N431—C1311.334 (3)N132—C1321.331 (3)
N431—N3311.363 (3)N132—C2321.457 (3)
N331—N2311.296 (3)C132—H1330.90 (2)
N231—N1311.351 (3)C232—H23A0.94 (3)
N131—C1311.329 (3)C232—H23B0.90 (3)
N131—C2311.466 (3)C232—H23C0.98 (3)
C131—H1310.91 (3)B1—F111.385 (3)
C231—H23A1.00 (3)B1—F211.391 (3)
C231—H23B1.03 (3)B1—F411.400 (3)
C231—H23C0.91 (2)B1—F311.405 (3)
Fe2—N4222.181 (2)B2—F221.390 (3)
Fe2—N422ii2.181 (2)B2—F421.391 (3)
Fe2—N4322.185 (2)B2—F321.400 (3)
Fe2—N432ii2.185 (2)B2—F121.409 (3)
N411i—Fe1—N411180.0N422—Fe2—N412ii90.61 (7)
N411i—Fe1—N421i91.56 (8)N422ii—Fe2—N412ii89.39 (7)
N411—Fe1—N421i88.44 (8)N432—Fe2—N412ii88.24 (7)
N411i—Fe1—N42188.44 (8)N432ii—Fe2—N412ii91.76 (7)
N411—Fe1—N42191.56 (8)N422—Fe2—N41289.39 (7)
N421i—Fe1—N421180.0N422ii—Fe2—N41290.61 (7)
N411i—Fe1—N43189.70 (7)N432—Fe2—N41291.76 (7)
N411—Fe1—N43190.30 (7)N432ii—Fe2—N41288.24 (7)
N421i—Fe1—N43190.83 (7)N412ii—Fe2—N412180.0
N421—Fe1—N43189.17 (7)C112—N412—N312106.1 (2)
N411i—Fe1—N431i90.30 (7)C112—N412—Fe2129.6 (2)
N411—Fe1—N431i89.70 (7)N312—N412—Fe2124.21 (14)
N421i—Fe1—N431i89.17 (7)N212—N312—N412109.9 (2)
N421—Fe1—N431i90.83 (7)N312—N212—N112106.4 (2)
N431—Fe1—N431i180.0C112—N112—N212108.9 (2)
C111—N411—N311106.2 (2)C112—N112—C212129.8 (2)
C111—N411—Fe1127.0 (2)N212—N112—C212120.7 (2)
N311—N411—Fe1124.74 (14)N112—C112—N412108.7 (2)
N211—N311—N411109.7 (2)N112—C112—H112126.3 (19)
N311—N211—N111106.4 (2)N412—C112—H112124.7 (18)
C111—N111—N211108.7 (2)N112—C212—H21A105.6 (17)
C111—N111—C211130.0 (2)N112—C212—H21B106.2 (15)
N211—N111—C211121.2 (2)H21A—C212—H21B114 (2)
N411—C111—N111109.0 (2)N112—C212—H21C111.1 (19)
N411—C111—H111123.3 (19)H21A—C212—H21C116 (3)
N111—C111—H111127.5 (19)H21B—C212—H21C104 (2)
N111—C211—H21A110.3 (15)C122—N422—N322106.1 (2)
N111—C211—H21B108 (2)C122—N422—Fe2129.49 (14)
H21A—C211—H21B108 (3)N322—N422—Fe2123.8 (2)
N111—C211—H21C104.8 (18)N222—N322—N422110.0 (2)
H21A—C211—H21C114 (2)N322—N222—N122106.5 (2)
H21B—C211—H21C112 (3)C122—N122—N222108.7 (2)
C121—N421—N321105.7 (2)C122—N122—C222130.4 (2)
C121—N421—Fe1129.8 (2)N222—N122—C222120.8 (2)
N321—N421—Fe1124.5 (2)N122—C122—N422108.7 (2)
N221—N321—N421109.9 (2)N122—C122—H122124 (2)
N321—N221—N121106.9 (2)N422—C122—H122128 (2)
C121—N121—N221108.4 (2)N122—C222—H22A110.1 (19)
C121—N121—C221129.9 (2)N122—C222—H22B112.1 (19)
N221—N121—C221121.5 (2)H22A—C222—H22B108 (3)
N421—C121—N121109.1 (2)N122—C222—H23C108.5 (18)
N421—C121—H121124 (2)H22A—C222—H23C110 (3)
N121—C121—H121127 (2)H22B—C222—H23C107 (2)
N121—C221—H22A107 (3)C132—N432—N332106.1 (2)
N121—C221—H22B103 (2)C132—N432—Fe2131.0 (2)
H22A—C221—H22B111 (3)N332—N432—Fe2122.4 (2)
N121—C221—H22C116 (3)N232—N332—N432109.9 (2)
H22A—C221—H22C114 (4)N332—N232—N132106.9 (2)
H22B—C221—H22C105 (4)C132—N132—N232109.2 (2)
C131—N431—N331105.9 (2)C132—N132—C232130.1 (2)
C131—N431—Fe1130.04 (15)N232—N132—C232120.6 (2)
N331—N431—Fe1123.8 (2)N132—C132—N432107.9 (2)
N231—N331—N431110.7 (2)N132—C132—H133128.6 (16)
N331—N231—N131106.1 (2)N432—C132—H133123.5 (16)
C131—N131—N231109.4 (2)N132—C232—H23A109.2 (18)
C131—N131—C231128.9 (2)N132—C232—H23B111.1 (19)
N231—N131—C231121.7 (2)H23A—C232—H23B107 (3)
N431—C131—N131107.9 (2)N132—C232—H23C112.8 (18)
N431—C131—H131128.8 (16)H23A—C232—H23C106 (2)
N131—C131—H131123.2 (16)H23B—C232—H23C111 (2)
N131—C231—H23A107.9 (16)F11—B1—F21109.9 (2)
N131—C231—H23B108.1 (15)F11—B1—F41109.8 (2)
H23A—C231—H23B109 (2)F21—B1—F41110.7 (2)
N131—C231—H23C108.0 (16)F11—B1—F31109.4 (2)
H23A—C231—H23C110 (2)F21—B1—F31108.5 (2)
H23B—C231—H23C113 (2)F41—B1—F31108.6 (2)
N422—Fe2—N422ii180.0F22—B2—F42110.3 (2)
N422—Fe2—N43290.14 (8)F22—B2—F32109.9 (2)
N422ii—Fe2—N43289.86 (8)F42—B2—F32109.8 (2)
N422—Fe2—N432ii89.86 (8)F22—B2—F12108.5 (2)
N422ii—Fe2—N432ii90.14 (8)F42—B2—F12109.6 (2)
N432—Fe2—N432ii180.0F32—B2—F12108.7 (2)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z.
(hs50) top
Crystal data top
C12H24B2F8FeN24V = 2955.9 (5) Å3
Mr = 734.02Z = 4
a = 17.4887 (15) ÅF(000) = 1488
b = 10.0914 (8) ÅDx = 1.649 Mg m3
c = 18.517 (2) ÅMo Kα radiation, λ = 0.71073 Å
α = 90°µ = 0.61 mm1
β = 115.243 (10)°T = 10 K
γ = 90°0.7 × 0.5 × 0.2 mm
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.083
Graphite monochromatorθmax = 28.2°, θmin = 3.3°
44334 measured reflectionsh = 2222
6461 independent reflectionsk = 126
4693 reflections with I > 2σ(I)l = 2323
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)] = 0.053H-atom parameters not defined?
wR(F2) = 0.155Calculated w = 1/[σ2(Fo2) + (0.0728P)2 + 2.1968P]
where P = (Fo2 + 2Fc2)/3
S = 1.08Δρmax = 0.65 e Å3
6411 reflectionsΔρmin = 0.68 e Å3
524 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction 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
xyzUiso*/Ueq
Fe10.00000.00000.00000.00804 (15)
N4110.06899 (14)0.1076 (3)0.03971 (14)0.0111 (5)
N3110.13426 (14)0.1893 (3)0.00721 (14)0.0122 (5)
N2110.17488 (15)0.2304 (3)0.03295 (14)0.0131 (5)
N1110.13613 (14)0.1747 (2)0.10635 (14)0.0109 (5)
C1110.0720 (2)0.1019 (3)0.1094 (2)0.0122 (6)
H1110.037 (2)0.057 (3)0.1531 (19)0.007 (7)*
C2110.1644 (2)0.2017 (3)0.1688 (2)0.0149 (6)
H21A0.225 (2)0.178 (4)0.151 (2)0.022 (9)*
H21B0.154 (3)0.291 (4)0.183 (2)0.031 (11)*
H21C0.130 (2)0.154 (4)0.212 (2)0.021 (9)*
N4210.07010 (14)0.1574 (2)0.00370 (13)0.0100 (5)
N3210.12165 (14)0.1654 (3)0.03524 (14)0.0124 (5)
N2210.16190 (15)0.2765 (2)0.01861 (14)0.0124 (5)
N1210.13728 (14)0.3433 (3)0.03111 (14)0.0116 (5)
C1210.0811 (2)0.2695 (3)0.0438 (2)0.0110 (6)
H1210.056 (2)0.291 (4)0.074 (2)0.018 (9)*
C2210.1663 (2)0.4778 (3)0.0573 (2)0.0141 (6)
H22A0.166 (3)0.485 (4)0.113 (3)0.045 (13)*
H22B0.223 (3)0.490 (4)0.064 (3)0.046 (13)*
H22C0.128 (3)0.546 (5)0.022 (3)0.060 (15)*
N4310.07916 (14)0.0455 (3)0.11240 (14)0.0110 (5)
N3310.14090 (14)0.0374 (3)0.16249 (14)0.0126 (5)
N2310.18565 (15)0.0219 (2)0.22915 (14)0.0127 (5)
N1310.15326 (14)0.1460 (2)0.22287 (14)0.0114 (5)
C1310.0885 (2)0.1581 (3)0.1521 (2)0.0115 (6)
H1310.060 (2)0.228 (3)0.1371 (19)0.005 (8)*
C2310.1872 (2)0.2403 (3)0.2890 (2)0.0136 (6)
H23A0.158 (3)0.314 (5)0.272 (3)0.033 (11)*
H23B0.179 (2)0.204 (4)0.333 (2)0.021 (9)*
H23C0.243 (2)0.253 (3)0.3047 (18)0.004 (7)*
Fe20.50000.00000.00000.0095 (2)
N4120.43279 (15)0.1305 (3)0.10150 (14)0.0128 (5)
N3120.38908 (15)0.2415 (3)0.09772 (14)0.0125 (5)
N2120.36133 (15)0.3044 (3)0.16529 (14)0.0142 (5)
N1120.38630 (14)0.2346 (2)0.21350 (14)0.0113 (5)
C1120.4300 (2)0.1296 (3)0.1737 (2)0.0133 (6)
H1120.454 (2)0.070 (4)0.189 (2)0.016 (9)*
C2120.3746 (2)0.2871 (3)0.2911 (2)0.0152 (6)
H21A0.425 (2)0.346 (4)0.280 (2)0.020 (9)*
H21B0.373 (2)0.213 (3)0.325 (2)0.012 (8)*
H21C0.324 (2)0.335 (4)0.313 (2)0.017 (9)*
N4220.57845 (15)0.1679 (3)0.06467 (14)0.0116 (5)
N3220.62313 (15)0.1730 (3)0.14587 (14)0.0135 (5)
N2220.6725 (2)0.2750 (3)0.16521 (14)0.0142 (5)
N1220.65962 (14)0.3378 (3)0.09610 (14)0.0121 (5)
C1220.6026 (2)0.2701 (3)0.0360 (2)0.0134 (6)
H1220.5833 (19)0.293 (3)0.0150 (19)0.004 (7)*
C2220.7074 (2)0.4569 (3)0.0956 (2)0.0141 (6)
H22A0.675 (2)0.522 (4)0.067 (2)0.018 (9)*
H22B0.749 (2)0.433 (4)0.082 (2)0.024 (10)*
H23C0.727 (2)0.496 (4)0.153 (2)0.023 (10)*
N4320.41083 (15)0.0466 (3)0.05108 (14)0.0127 (5)
N3320.35224 (15)0.0427 (3)0.05271 (14)0.0135 (5)
N2320.3140 (2)0.0055 (3)0.09330 (15)0.0136 (5)
N1320.34754 (14)0.1272 (3)0.11870 (14)0.0112 (5)
C1320.4064 (2)0.1504 (3)0.0924 (2)0.0125 (6)
H1330.441 (2)0.221 (3)0.1036 (18)0.005 (7)*
C2320.3207 (2)0.2069 (3)0.1692 (2)0.0138 (6)
H23A0.264 (3)0.238 (4)0.141 (2)0.032 (11)*
H23B0.325 (2)0.157 (4)0.213 (2)0.025 (10)*
H23C0.359 (2)0.284 (4)0.187 (2)0.018 (9)*
B10.4455 (2)0.5047 (4)0.1457 (2)0.0138 (7)
F110.36522 (11)0.4637 (2)0.09302 (10)0.0177 (4)
F210.45429 (10)0.6402 (2)0.13771 (10)0.0159 (4)
F310.45674 (11)0.4788 (2)0.22399 (10)0.0200 (4)
F410.50668 (11)0.4344 (2)0.13178 (12)0.0251 (4)
B20.0068 (2)0.5162 (3)0.1658 (2)0.0125 (7)
F120.01043 (10)0.4490 (2)0.10831 (10)0.0150 (4)
F220.01686 (10)0.6481 (2)0.16811 (10)0.0142 (4)
F320.03949 (10)0.4578 (2)0.24059 (10)0.0150 (4)
F420.09282 (10)0.5078 (2)0.14710 (10)0.0148 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0068 (3)0.0107 (3)0.0072 (3)0.0002 (2)0.0035 (2)0.0001 (2)
N4110.0090 (11)0.0128 (13)0.0106 (12)0.0005 (9)0.0034 (9)0.0015 (10)
N3110.0091 (11)0.0163 (14)0.0126 (12)0.0039 (10)0.0059 (9)0.0009 (10)
N2110.0117 (11)0.0181 (14)0.0104 (12)0.0022 (10)0.0056 (9)0.0003 (10)
N1110.0118 (11)0.0118 (13)0.0107 (11)0.0007 (9)0.0063 (9)0.0002 (10)
C1110.0099 (13)0.016 (2)0.0104 (14)0.0010 (11)0.0044 (11)0.0004 (12)
C2110.018 (2)0.017 (2)0.0128 (15)0.0021 (13)0.0101 (12)0.0012 (13)
N4210.0098 (11)0.0137 (13)0.0081 (11)0.0021 (9)0.0054 (9)0.0009 (9)
N3210.0103 (11)0.0164 (14)0.0129 (12)0.0017 (10)0.0073 (10)0.0011 (10)
N2210.0124 (11)0.0136 (14)0.0127 (12)0.0001 (10)0.0067 (9)0.0004 (10)
N1210.0104 (11)0.0160 (14)0.0087 (11)0.0011 (10)0.0044 (9)0.0006 (10)
C1210.0114 (13)0.013 (2)0.0087 (13)0.0013 (11)0.0044 (11)0.0020 (11)
C2210.0144 (14)0.014 (2)0.0134 (14)0.0026 (12)0.0059 (12)0.0026 (12)
N4310.0096 (11)0.0124 (13)0.0134 (12)0.0013 (9)0.0072 (9)0.0021 (10)
N3310.0084 (11)0.0205 (14)0.0068 (11)0.0013 (10)0.0011 (9)0.0009 (10)
N2310.0111 (11)0.0139 (14)0.0135 (12)0.0004 (9)0.0054 (10)0.0014 (10)
N1310.0105 (11)0.0130 (14)0.0115 (12)0.0007 (9)0.0055 (9)0.0021 (10)
C1310.0088 (13)0.014 (2)0.0113 (14)0.0006 (12)0.0043 (11)0.0002 (12)
C2310.0136 (15)0.015 (2)0.0108 (14)0.0008 (12)0.0035 (12)0.0038 (12)
Fe20.0085 (3)0.0124 (3)0.0088 (3)0.0001 (2)0.0047 (2)0.0002 (2)
N4120.0123 (11)0.0152 (14)0.0117 (12)0.0004 (10)0.0058 (10)0.0002 (10)
N3120.0107 (11)0.0151 (14)0.0118 (12)0.0014 (9)0.0047 (10)0.0008 (10)
N2120.0150 (12)0.0171 (14)0.0111 (12)0.0009 (10)0.0062 (10)0.0018 (10)
N1120.0100 (11)0.0146 (14)0.0110 (12)0.0001 (9)0.0061 (9)0.0003 (10)
C1120.0108 (13)0.015 (2)0.0151 (15)0.0001 (11)0.0063 (12)0.0006 (12)
C2120.018 (2)0.017 (2)0.0121 (14)0.0006 (13)0.0081 (12)0.0034 (13)
N4220.0144 (12)0.0135 (14)0.0083 (11)0.0004 (10)0.0062 (9)0.0004 (9)
N3220.0123 (11)0.0165 (14)0.0110 (12)0.0011 (10)0.0041 (10)0.0013 (10)
N2220.0144 (12)0.0167 (14)0.0130 (12)0.0010 (10)0.0072 (10)0.0003 (10)
N1220.0110 (11)0.0148 (14)0.0111 (12)0.0010 (10)0.0052 (9)0.0004 (10)
C1220.0127 (13)0.017 (2)0.0117 (14)0.0005 (11)0.0059 (11)0.0017 (12)
C2220.0140 (14)0.014 (2)0.017 (2)0.0006 (12)0.0087 (12)0.0002 (13)
N4320.0121 (11)0.0155 (14)0.0112 (12)0.0006 (10)0.0056 (9)0.0019 (10)
N3320.0133 (12)0.0161 (14)0.0140 (12)0.0015 (10)0.0086 (10)0.0016 (10)
N2320.0139 (12)0.0145 (14)0.0147 (12)0.0012 (10)0.0083 (10)0.0020 (10)
N1320.0099 (11)0.0128 (13)0.0118 (12)0.0009 (9)0.0056 (9)0.0013 (10)
C1320.0114 (13)0.014 (2)0.0127 (14)0.0009 (12)0.0054 (11)0.0003 (12)
C2320.0130 (14)0.018 (2)0.0119 (14)0.0020 (12)0.0073 (12)0.0018 (13)
B10.0135 (15)0.017 (2)0.013 (2)0.0030 (13)0.0072 (12)0.0038 (13)
F110.0149 (8)0.0213 (10)0.0138 (9)0.0039 (7)0.0031 (7)0.0010 (7)
F210.0158 (8)0.0166 (10)0.0143 (9)0.0006 (7)0.0054 (7)0.0010 (7)
F310.0231 (9)0.0246 (11)0.0099 (8)0.0054 (8)0.0047 (7)0.0023 (7)
F410.0214 (9)0.0202 (11)0.0423 (12)0.0000 (8)0.0219 (9)0.0071 (9)
B20.0098 (14)0.015 (2)0.013 (2)0.0012 (12)0.0051 (12)0.0007 (13)
F120.0157 (8)0.0165 (9)0.0142 (8)0.0015 (7)0.0078 (7)0.0012 (7)
F220.0158 (8)0.0133 (10)0.0155 (9)0.0016 (7)0.0084 (7)0.0012 (7)
F320.0141 (8)0.0189 (10)0.0125 (8)0.0019 (7)0.0062 (7)0.0038 (7)
F420.0100 (8)0.0185 (10)0.0160 (9)0.0002 (7)0.0058 (7)0.0009 (7)
Geometric parameters (Å, º) top
Fe1—N4111.983 (2)Fe2—N4322.192 (2)
Fe1—N411i1.983 (2)Fe2—N432ii2.192 (2)
Fe1—N421i1.989 (2)N412—C1121.318 (4)
Fe1—N4211.989 (2)N412—N3121.374 (3)
Fe1—N4312.000 (2)N312—N2121.299 (3)
Fe1—N431i2.000 (2)N212—N1121.347 (3)
N411—C1111.315 (4)N112—C1121.330 (4)
N411—N3111.375 (3)N112—C2121.462 (4)
N311—N2111.297 (3)C112—H1120.84 (4)
N211—N1111.356 (3)C212—H21A1.01 (4)
N111—C1111.322 (4)C212—H21B0.97 (3)
N111—C2111.464 (4)C212—H21C0.94 (4)
C111—H1110.90 (3)N422—C1221.311 (4)
C211—H21A0.99 (4)N422—N3221.368 (3)
C211—H21B0.94 (4)N322—N2221.292 (4)
C211—H21C0.91 (4)N222—N1221.358 (3)
N421—C1211.321 (4)N122—C1221.324 (4)
N421—N3211.376 (3)N122—C2221.466 (4)
N321—N2211.289 (4)C122—H1220.89 (3)
N221—N1211.351 (3)C222—H22A0.88 (4)
N121—C1211.331 (4)C222—H22B0.89 (4)
N121—C2211.458 (4)C222—H23C1.04 (4)
C121—H1210.88 (4)N432—C1321.319 (4)
C221—H22A1.04 (5)N432—N3321.374 (3)
C221—H22B0.95 (5)N332—N2321.295 (3)
C221—H22C0.99 (5)N232—N1321.356 (3)
N431—C1311.325 (4)N132—C1321.334 (4)
N431—N3311.368 (3)N132—C2321.454 (4)
N331—N2311.292 (3)C132—H1330.90 (3)
N231—N1311.358 (3)C232—H23A0.96 (4)
N131—C1311.322 (4)C232—H23B0.93 (4)
N131—C2311.462 (4)C232—H23C0.98 (4)
C131—H1310.84 (3)B1—F111.387 (4)
C231—H23A0.88 (5)B1—F211.390 (4)
C231—H23B0.96 (4)B1—F411.397 (4)
C231—H23C0.91 (3)B1—F311.402 (4)
Fe2—N412ii2.183 (2)B2—F221.389 (4)
Fe2—N4122.183 (2)B2—F421.395 (3)
Fe2—N4222.187 (2)B2—F121.400 (4)
Fe2—N422ii2.187 (2)B2—F321.401 (4)
N411—Fe1—N411i180.0N412ii—Fe2—N43288.78 (9)
N411—Fe1—N421i89.22 (10)N412—Fe2—N43291.22 (9)
N411i—Fe1—N421i90.78 (10)N422—Fe2—N43289.62 (9)
N411—Fe1—N42190.78 (10)N422ii—Fe2—N43290.38 (9)
N411i—Fe1—N42189.22 (10)N412ii—Fe2—N432ii91.22 (9)
N421i—Fe1—N421180.0N412—Fe2—N432ii88.78 (9)
N411—Fe1—N43189.97 (9)N422—Fe2—N432ii90.38 (9)
N411i—Fe1—N43190.03 (9)N422ii—Fe2—N432ii89.62 (9)
N421i—Fe1—N43190.27 (10)N432—Fe2—N432ii180.0
N421—Fe1—N43189.73 (10)C112—N412—N312106.1 (2)
N411—Fe1—N431i90.03 (9)C112—N412—Fe2130.0 (2)
N411i—Fe1—N431i89.97 (9)N312—N412—Fe2123.7 (2)
N421i—Fe1—N431i89.73 (10)N212—N312—N412109.7 (2)
N421—Fe1—N431i90.27 (10)N312—N212—N112106.8 (2)
N431—Fe1—N431i180.0C112—N112—N212108.8 (2)
C111—N411—N311106.1 (2)C112—N112—C212129.8 (3)
C111—N411—Fe1128.7 (2)N212—N112—C212120.8 (2)
N311—N411—Fe1124.5 (2)N412—C112—N112108.7 (3)
N211—N311—N411109.9 (2)N412—C112—H112122 (2)
N311—N211—N111106.3 (2)N112—C112—H112129 (2)
C111—N111—N211109.0 (2)N112—C212—H21A106 (2)
C111—N111—C211129.5 (3)N112—C212—H21B108.3 (19)
N211—N111—C211121.4 (2)H21A—C212—H21B112 (3)
N411—C111—N111108.8 (3)N112—C212—H21C109 (2)
N411—C111—H111128 (2)H21A—C212—H21C112 (3)
N111—C111—H111124 (2)H21B—C212—H21C111 (3)
N111—C211—H21A112 (2)C122—N422—N322106.5 (2)
N111—C211—H21B108 (3)C122—N422—Fe2128.5 (2)
H21A—C211—H21B112 (3)N322—N422—Fe2124.2 (2)
N111—C211—H21C105 (2)N222—N322—N422109.6 (2)
H21A—C211—H21C112 (3)N322—N222—N122106.7 (2)
H21B—C211—H21C107 (3)C122—N122—N222108.3 (2)
C121—N421—N321105.8 (2)C122—N122—C222130.1 (3)
C121—N421—Fe1130.0 (2)N222—N122—C222121.5 (2)
N321—N421—Fe1124.1 (2)N422—C122—N122108.8 (3)
N221—N321—N421109.8 (2)N422—C122—H122127 (2)
N321—N221—N121107.3 (2)N122—C122—H122125 (2)
C121—N121—N221108.3 (2)N122—C222—H22A113 (2)
C121—N121—C221129.9 (2)N122—C222—H22B108 (3)
N221—N121—C221121.6 (2)H22A—C222—H22B116 (3)
N421—C121—N121108.8 (2)N122—C222—H23C104 (2)
N421—C121—H121125 (2)H22A—C222—H23C100 (3)
N121—C121—H121126 (2)H22B—C222—H23C115 (3)
N121—C221—H22A105 (2)C132—N432—N332106.2 (2)
N121—C221—H22B111 (3)C132—N432—Fe2130.5 (2)
H22A—C221—H22B108 (4)N332—N432—Fe2122.9 (2)
N121—C221—H22C113 (3)N232—N332—N432109.9 (2)
H22A—C221—H22C109 (4)N332—N232—N132106.7 (2)
H22B—C221—H22C112 (4)C132—N132—N232108.6 (2)
C131—N431—N331105.8 (2)C132—N132—C232130.4 (3)
C131—N431—Fe1129.9 (2)N232—N132—C232120.9 (2)
N331—N431—Fe1124.1 (2)N432—C132—N132108.5 (3)
N231—N331—N431110.2 (2)N432—C132—H133124 (2)
N331—N231—N131106.5 (2)N132—C132—H133128 (2)
C131—N131—N231108.6 (2)N132—C232—H23A113 (2)
C131—N131—C231129.8 (3)N132—C232—H23B110 (2)
N231—N131—C231121.5 (2)H23A—C232—H23B108 (3)
N131—C131—N431108.8 (3)N132—C232—H23C107 (2)
N131—C131—H131123 (2)H23A—C232—H23C109 (3)
N431—C131—H131128 (2)H23B—C232—H23C110 (3)
N131—C231—H23A106 (3)F11—B1—F21110.1 (3)
N131—C231—H23B108 (2)F11—B1—F41110.1 (3)
H23A—C231—H23B111 (3)F21—B1—F41110.6 (2)
N131—C231—H23C111.0 (19)F11—B1—F31109.0 (2)
H23A—C231—H23C113 (3)F21—B1—F31108.7 (3)
H23B—C231—H23C108 (3)F41—B1—F31108.3 (3)
N412ii—Fe2—N412180.0F22—B2—F42110.0 (2)
N412ii—Fe2—N42290.81 (9)F22—B2—F12109.2 (2)
N412—Fe2—N42289.19 (9)F42—B2—F12109.9 (2)
N412ii—Fe2—N422ii89.19 (9)F22—B2—F32109.5 (2)
N412—Fe2—N422ii90.81 (9)F42—B2—F32109.1 (2)
N422—Fe2—N422ii180.0F12—B2—F32109.1 (2)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z.
(ls100) top
Crystal data top
C12H24B2F8FeN24V = 2957.3 (7) Å3
Mr = 734.02Z = 4
a = 17.207 (2) ÅF(000) = 1488
b = 10.2140 (14) ÅDx = 1.649 Mg m3
c = 18.406 (3) ÅMo Kα radiation, λ = 0.71073 Å
α = 90°µ = 0.61 mm1
β = 113.912 (15)°T = 10 K
γ = 90°0.7 × 0.5 × 0.2 mm
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.072
Graphite monochromatorθmax = 28.0°, θmin = 3.3°
34261 measured reflectionsh = 2121
6057 independent reflectionsk = 125
4245 reflections with I > 2σ(I)l = 2323
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)] = 0.055H-atom parameters not defined?
wR(F2) = 0.156Calculated w = 1/[σ2(Fo2) + (0.0737P)2 + 3.966P]
where P = (Fo2 + 2Fc2)/3
S = 1.10Δρmax = 0.56 e Å3
6057 reflectionsΔρmin = 0.81 e Å3
524 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction 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
xyzUiso*/Ueq
Fe10.00000.00000.00000.0100 (2)
N4110.0695 (2)0.1120 (3)0.0420 (2)0.0128 (7)
N3110.1357 (2)0.1905 (4)0.0038 (2)0.0184 (7)
N2110.1755 (2)0.2321 (3)0.0380 (2)0.0183 (7)
N1110.1353 (2)0.1799 (3)0.1115 (2)0.0147 (7)
C1110.0706 (2)0.1086 (4)0.1132 (2)0.0138 (8)
H1110.031 (3)0.066 (5)0.155 (3)0.024 (12)*
C2110.1617 (3)0.2091 (5)0.1761 (2)0.0179 (9)
H21A0.219 (3)0.179 (5)0.162 (3)0.043 (15)*
H21B0.157 (3)0.301 (5)0.181 (2)0.011 (10)*
H21C0.125 (2)0.172 (4)0.217 (2)0.007 (9)*
N4210.0731 (2)0.1570 (3)0.0008 (2)0.0148 (7)
N3210.1242 (2)0.1614 (3)0.0404 (2)0.0166 (7)
N2210.1655 (2)0.2704 (4)0.0257 (2)0.0174 (7)
N1210.1415 (2)0.3383 (3)0.0255 (2)0.0148 (7)
C1210.0853 (2)0.2677 (4)0.0404 (2)0.0148 (8)
H1210.064 (3)0.286 (4)0.070 (3)0.021 (12)*
C2210.1718 (3)0.4717 (5)0.0500 (2)0.0201 (9)
H22A0.156 (5)0.495 (7)0.088 (4)0.08 (2)*
H22B0.230 (3)0.477 (5)0.069 (3)0.027 (12)*
H22C0.141 (5)0.534 (8)0.007 (5)0.11 (3)*
N4310.0806 (2)0.0453 (3)0.1135 (2)0.0141 (7)
N3310.1418 (2)0.0360 (3)0.1633 (2)0.0148 (7)
N2310.1864 (2)0.0223 (3)0.2286 (2)0.0176 (7)
N1310.1546 (2)0.1449 (3)0.2228 (2)0.0141 (7)
C1310.0897 (2)0.1578 (4)0.1526 (2)0.0148 (8)
H1310.064 (2)0.236 (4)0.137 (2)0.007 (10)*
C2310.1886 (2)0.2396 (4)0.2881 (2)0.0170 (8)
H23A0.159 (3)0.324 (5)0.272 (2)0.021 (11)*
H23B0.174 (3)0.211 (5)0.330 (3)0.026 (12)*
H23C0.246 (3)0.246 (4)0.305 (2)0.008 (9)*
Fe20.50000.00000.00000.0109 (2)
N4120.4413 (2)0.1229 (3)0.0910 (2)0.0147 (7)
N3120.3938 (2)0.2284 (3)0.0868 (2)0.0157 (7)
N2120.3652 (2)0.2925 (4)0.1533 (2)0.0183 (8)
N1120.3935 (2)0.2262 (3)0.2019 (2)0.0139 (7)
C1120.4398 (2)0.1252 (4)0.1631 (2)0.0151 (8)
H1120.470 (2)0.072 (4)0.179 (2)0.005 (9)*
C2120.3811 (3)0.2801 (5)0.2798 (2)0.0188 (9)
H21A0.431 (3)0.340 (5)0.269 (3)0.026 (12)*
H21B0.380 (3)0.202 (5)0.316 (3)0.035 (13)*
H21C0.321 (3)0.314 (5)0.304 (3)0.038 (14)*
N4220.5759 (2)0.1485 (4)0.0612 (2)0.0161 (7)
N3220.6226 (2)0.1472 (4)0.1417 (2)0.0168 (7)
N2220.6709 (2)0.2490 (4)0.1622 (2)0.0179 (7)
N1220.6552 (2)0.3186 (3)0.0952 (2)0.0141 (7)
C1220.5978 (2)0.2566 (4)0.0348 (2)0.0144 (8)
H1220.575 (2)0.290 (4)0.019 (2)0.006 (9)*
C2220.6990 (3)0.4428 (4)0.0976 (2)0.0172 (8)
H22A0.672 (3)0.485 (4)0.052 (2)0.011 (10)*
H22B0.751 (3)0.439 (5)0.098 (3)0.035 (14)*
H23C0.705 (3)0.495 (4)0.145 (3)0.018 (11)*
N4320.4170 (2)0.0432 (3)0.0490 (2)0.0150 (7)
N3320.3593 (2)0.0463 (3)0.0538 (2)0.0160 (7)
N2320.3196 (2)0.0039 (3)0.0932 (2)0.0161 (7)
N1320.3503 (2)0.1254 (3)0.1152 (2)0.0133 (7)
C1320.4097 (2)0.1483 (4)0.0879 (2)0.0159 (8)
H1330.438 (2)0.221 (4)0.096 (2)0.003 (9)*
C2320.3218 (2)0.2054 (4)0.1650 (2)0.0154 (8)
H23A0.264 (3)0.235 (5)0.136 (3)0.023 (11)*
H23B0.323 (3)0.159 (5)0.204 (3)0.030 (13)*
H23C0.361 (2)0.283 (4)0.188 (2)0.007 (9)*
B10.4488 (3)0.4994 (5)0.1436 (2)0.0145 (9)
F110.37172 (13)0.4500 (2)0.08997 (11)0.0193 (5)
F210.45344 (13)0.6329 (2)0.13204 (11)0.0187 (5)
F310.45556 (13)0.4779 (2)0.22126 (11)0.0186 (5)
F410.51535 (13)0.4329 (2)0.13410 (13)0.0217 (5)
B20.0041 (3)0.5138 (5)0.1662 (2)0.0144 (9)
F120.01330 (13)0.4452 (2)0.10821 (12)0.0182 (5)
F220.02077 (13)0.6436 (2)0.16672 (11)0.0181 (5)
F320.04182 (13)0.4574 (2)0.24033 (11)0.0175 (5)
F420.09067 (13)0.5080 (2)0.14841 (12)0.0181 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0098 (3)0.0131 (5)0.0077 (3)0.0002 (3)0.0042 (2)0.0004 (3)
N4110.0125 (14)0.014 (2)0.0105 (13)0.0016 (13)0.0032 (11)0.0032 (12)
N3110.019 (2)0.022 (2)0.0143 (14)0.0039 (15)0.0065 (12)0.0006 (13)
N2110.022 (2)0.017 (2)0.0127 (14)0.0050 (15)0.0035 (12)0.0001 (13)
N1110.0167 (15)0.015 (2)0.0114 (13)0.0013 (14)0.0050 (11)0.0006 (13)
C1110.012 (2)0.015 (2)0.014 (2)0.001 (2)0.0049 (14)0.001 (2)
C2110.022 (2)0.021 (3)0.015 (2)0.004 (2)0.012 (2)0.000 (2)
N4210.0153 (14)0.020 (2)0.0103 (13)0.0049 (14)0.0068 (11)0.0018 (13)
N3210.0166 (15)0.020 (2)0.0150 (14)0.0001 (15)0.0085 (12)0.0016 (13)
N2210.019 (2)0.022 (2)0.0114 (14)0.0040 (15)0.0061 (12)0.0022 (13)
N1210.0182 (15)0.015 (2)0.0102 (13)0.0038 (14)0.0043 (11)0.0007 (12)
C1210.019 (2)0.017 (2)0.009 (2)0.004 (2)0.0059 (14)0.0017 (15)
C2210.022 (2)0.019 (3)0.017 (2)0.002 (2)0.005 (2)0.001 (2)
N4310.0129 (14)0.014 (2)0.0198 (15)0.0008 (13)0.0106 (12)0.0021 (13)
N3310.0122 (14)0.018 (2)0.0136 (14)0.0015 (13)0.0046 (11)0.0034 (13)
N2310.0155 (15)0.019 (2)0.021 (2)0.0013 (14)0.0104 (12)0.0027 (14)
N1310.0121 (14)0.013 (2)0.0186 (14)0.0013 (13)0.0078 (12)0.0018 (13)
C1310.016 (2)0.012 (2)0.017 (2)0.001 (2)0.0072 (14)0.001 (2)
C2310.016 (2)0.015 (2)0.019 (2)0.000 (2)0.0061 (15)0.002 (2)
Fe20.0111 (3)0.0144 (5)0.0084 (3)0.0012 (3)0.0053 (3)0.0005 (3)
N4120.0157 (15)0.017 (2)0.0145 (14)0.0026 (14)0.0093 (12)0.0029 (13)
N3120.0155 (15)0.015 (2)0.0178 (15)0.0008 (14)0.0080 (12)0.0012 (13)
N2120.016 (2)0.025 (2)0.0163 (15)0.0006 (14)0.0088 (12)0.0019 (14)
N1120.0154 (15)0.014 (2)0.0150 (14)0.0005 (14)0.0089 (12)0.0015 (13)
C1120.016 (2)0.013 (2)0.019 (2)0.001 (2)0.0096 (15)0.001 (2)
C2120.021 (2)0.025 (3)0.013 (2)0.003 (2)0.0086 (15)0.003 (2)
N4220.0161 (15)0.026 (2)0.0086 (13)0.0059 (14)0.0072 (11)0.0022 (13)
N3220.0154 (15)0.025 (2)0.0093 (13)0.0004 (15)0.0044 (11)0.0014 (13)
N2220.020 (2)0.022 (2)0.0135 (14)0.003 (2)0.0087 (12)0.0025 (14)
N1220.0149 (14)0.018 (2)0.0106 (13)0.0033 (14)0.0062 (11)0.0001 (12)
C1220.016 (2)0.020 (2)0.009 (2)0.000 (2)0.0074 (13)0.0012 (15)
C2220.020 (2)0.015 (2)0.016 (2)0.001 (2)0.007 (2)0.002 (2)
N4320.0141 (14)0.019 (2)0.0113 (13)0.0003 (14)0.0044 (11)0.0015 (13)
N3320.0169 (15)0.016 (2)0.0168 (15)0.0046 (14)0.0090 (12)0.0013 (13)
N2320.0182 (15)0.015 (2)0.0158 (14)0.0010 (14)0.0076 (12)0.0002 (13)
N1320.0148 (14)0.013 (2)0.0122 (13)0.0020 (13)0.0051 (11)0.0017 (12)
C1320.016 (2)0.019 (2)0.014 (2)0.005 (2)0.0072 (14)0.003 (2)
C2320.017 (2)0.019 (2)0.012 (2)0.003 (2)0.0078 (14)0.001 (2)
B10.017 (2)0.014 (3)0.013 (2)0.002 (2)0.0056 (15)0.000 (2)
F110.0197 (11)0.0216 (14)0.0141 (10)0.0035 (10)0.0043 (8)0.0004 (9)
F210.0188 (11)0.0221 (14)0.0143 (10)0.0010 (10)0.0058 (8)0.0021 (9)
F310.0206 (11)0.0254 (15)0.0102 (9)0.0002 (10)0.0068 (8)0.0018 (9)
F410.0202 (11)0.0212 (15)0.0291 (12)0.0032 (10)0.0157 (10)0.0026 (10)
B20.017 (2)0.013 (3)0.014 (2)0.002 (2)0.0068 (15)0.002 (2)
F120.0216 (11)0.0195 (14)0.0148 (10)0.0002 (10)0.0085 (8)0.0019 (9)
F220.0197 (11)0.0194 (14)0.0163 (10)0.0014 (10)0.0087 (8)0.0011 (9)
F320.0180 (10)0.0215 (14)0.0132 (10)0.0043 (10)0.0066 (8)0.0050 (9)
F420.0150 (10)0.0237 (15)0.0158 (10)0.0006 (10)0.0065 (8)0.0009 (9)
Geometric parameters (Å, º) top
Fe1—N4112.021 (3)Fe2—N432ii2.023 (3)
Fe1—N411i2.021 (3)Fe2—N4322.023 (3)
Fe1—N421i2.034 (3)N412—C1121.319 (4)
Fe1—N4212.034 (3)N412—N3121.373 (4)
Fe1—N4312.038 (3)N312—N2121.296 (4)
Fe1—N431i2.038 (3)N212—N1121.359 (4)
N411—C1111.319 (4)N112—C1121.322 (5)
N411—N3111.367 (4)N112—C2121.468 (5)
N311—N2111.292 (4)C112—H1120.87 (4)
N211—N1111.354 (4)C212—H21A1.00 (5)
N111—C1111.319 (5)C212—H21B1.03 (5)
N111—C2111.466 (4)C212—H21C1.00 (5)
C111—H1110.91 (5)N422—C1221.321 (5)
C211—H21A0.97 (5)N422—N3221.369 (4)
C211—H21B0.95 (4)N322—N2221.288 (5)
C211—H21C0.86 (4)N222—N1221.353 (4)
N421—C1211.315 (5)N122—C1221.313 (5)
N421—N3211.376 (4)N122—C2221.468 (5)
N321—N2211.289 (5)C122—H1220.96 (4)
N221—N1211.361 (4)C222—H22A0.89 (4)
N121—C1211.321 (5)C222—H22B0.89 (5)
N121—C2211.463 (5)C222—H23C1.00 (4)
C121—H1210.79 (4)N432—C1321.325 (5)
C221—H22A0.89 (7)N432—N3321.378 (4)
C221—H22B0.91 (5)N332—N2321.289 (4)
C221—H22C0.98 (8)N232—N1321.345 (5)
N431—C1311.331 (5)N132—C1321.329 (5)
N431—N3311.363 (4)N132—C2321.454 (5)
N331—N2311.281 (4)C132—H1330.87 (4)
N231—N1311.353 (5)C232—H23A0.97 (4)
N131—C1311.328 (5)C232—H23B0.86 (5)
N131—C2311.468 (5)C232—H23C1.01 (4)
C131—H1310.90 (4)B1—F111.387 (5)
C231—H23A0.99 (5)B1—F211.388 (5)
C231—H23B0.95 (4)B1—F311.404 (4)
C231—H23C0.91 (4)B1—F411.402 (5)
Fe2—N412ii2.007 (3)B2—F221.392 (5)
Fe2—N4122.007 (3)B2—F421.391 (5)
Fe2—N422ii2.021 (3)B2—F321.395 (4)
Fe2—N4222.021 (3)B2—F121.406 (5)
N411—Fe1—N411i180.0N412ii—Fe2—N432ii91.59 (12)
N411—Fe1—N421i89.39 (12)N412—Fe2—N432ii88.41 (12)
N411i—Fe1—N421i90.61 (12)N422ii—Fe2—N432ii90.07 (12)
N411—Fe1—N42190.61 (12)N422—Fe2—N432ii89.93 (12)
N411i—Fe1—N42189.39 (12)N412ii—Fe2—N43288.41 (12)
N421i—Fe1—N421180.0N412—Fe2—N43291.59 (12)
N411—Fe1—N43190.02 (11)N422ii—Fe2—N43289.93 (12)
N411i—Fe1—N43189.98 (11)N422—Fe2—N43290.07 (12)
N421i—Fe1—N43190.53 (12)N432ii—Fe2—N432180.0
N421—Fe1—N43189.47 (12)C112—N412—N312105.9 (3)
N411—Fe1—N431i89.98 (11)C112—N412—Fe2130.4 (3)
N411i—Fe1—N431i90.02 (11)N312—N412—Fe2123.7 (2)
N421i—Fe1—N431i89.47 (12)N212—N312—N412110.5 (3)
N421—Fe1—N431i90.53 (12)N312—N212—N112105.6 (3)
N431—Fe1—N431i180.0C112—N112—N212109.4 (3)
C111—N411—N311106.5 (3)C112—N112—C212129.5 (3)
C111—N411—Fe1127.9 (3)N212—N112—C212120.4 (3)
N311—N411—Fe1124.8 (2)N412—C112—N112108.6 (3)
N211—N311—N411109.7 (3)N412—C112—H112123 (2)
N311—N211—N111106.5 (3)N112—C112—H112128 (2)
C111—N111—N211109.1 (3)N112—C212—H21A105 (2)
C111—N111—C211129.0 (3)N112—C212—H21B107 (3)
N211—N111—C211121.9 (3)H21A—C212—H21B113 (4)
N111—C111—N411108.3 (3)N112—C212—H21C107 (3)
N111—C111—H111129 (3)H21A—C212—H21C121 (4)
N411—C111—H111123 (3)H21B—C212—H21C103 (4)
N111—C211—H21A110 (3)C122—N422—N322106.1 (3)
N111—C211—H21B104 (2)C122—N422—Fe2129.6 (2)
H21A—C211—H21B113 (4)N322—N422—Fe2124.0 (3)
N111—C211—H21C105 (3)N222—N322—N422109.6 (3)
H21A—C211—H21C114 (4)N322—N222—N122106.9 (3)
H21B—C211—H21C110 (4)C122—N122—N222108.8 (3)
C121—N421—N321106.4 (3)C122—N122—C222130.1 (3)
C121—N421—Fe1129.9 (2)N222—N122—C222121.2 (3)
N321—N421—Fe1123.6 (2)N122—C122—N422108.7 (3)
N221—N321—N421109.5 (3)N122—C122—H122124 (2)
N321—N221—N121106.8 (3)N422—C122—H122128 (2)
C121—N121—N221108.6 (3)N122—C222—H22A109 (3)
C121—N121—C221130.0 (3)N122—C222—H22B117 (4)
N221—N121—C221121.2 (3)H22A—C222—H22B100 (4)
N421—C121—N121108.7 (3)N122—C222—H23C111 (2)
N421—C121—H121125 (3)H22A—C222—H23C113 (4)
N121—C121—H121127 (3)H22B—C222—H23C106 (4)
N121—C221—H22A108 (4)C132—N432—N332105.9 (3)
N121—C221—H22B112 (3)C132—N432—Fe2131.1 (3)
H22A—C221—H22B109 (5)N332—N432—Fe2122.7 (2)
N121—C221—H22C110 (5)N232—N332—N432109.4 (3)
H22A—C221—H22C103 (6)N332—N232—N132107.6 (3)
H22B—C221—H22C115 (5)C132—N132—N232108.5 (3)
C131—N431—N331105.8 (3)C132—N132—C232130.2 (4)
C131—N431—Fe1129.2 (3)N232—N132—C232121.1 (3)
N331—N431—Fe1124.8 (2)N432—C132—N132108.5 (4)
N231—N331—N431110.8 (3)N432—C132—H133128 (2)
N331—N231—N131106.6 (3)N132—C132—H133123 (2)
C131—N131—N231108.9 (3)N132—C232—H23A111 (3)
C131—N131—C231129.0 (3)N132—C232—H23B109 (3)
N231—N131—C231122.1 (3)H23A—C232—H23B108 (4)
N131—C131—N431108.0 (4)N132—C232—H23C111 (2)
N131—C131—H131121 (2)H23A—C232—H23C111 (4)
N431—C131—H131131 (2)H23B—C232—H23C107 (4)
N131—C231—H23A110 (2)F11—B1—F21110.3 (3)
N131—C231—H23B108 (3)F11—B1—F31109.2 (3)
H23A—C231—H23B104 (4)F21—B1—F31108.8 (3)
N131—C231—H23C110 (2)F11—B1—F41109.2 (3)
H23A—C231—H23C114 (4)F21—B1—F41110.9 (3)
H23B—C231—H23C111 (3)F31—B1—F41108.4 (3)
N412ii—Fe2—N412180.0F22—B2—F42109.8 (3)
N412ii—Fe2—N422ii89.34 (13)F22—B2—F32109.6 (3)
N412—Fe2—N422ii90.66 (13)F42—B2—F32109.9 (3)
N412ii—Fe2—N42290.66 (13)F22—B2—F12108.7 (3)
N412—Fe2—N42289.34 (13)F42—B2—F12109.7 (3)
N422ii—Fe2—N422180.0F32—B2—F12109.0 (3)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z.
 

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