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In the spin-crossover compound [Fe(ptz)6](BF4)2 (where ptz=1-n-propyltetrazole) six different phases are observed. When a single crystal is slowly cooled from high temperatures to those below 125 K, the reflections broaden into diffuse maxima and split into two maxima along the c* direction [Kusz, Gütlich & Spiering (2004). Top. Curr. Chem. 234, 129-153]. As both maxima are broad along the c* direction, the short-range order exists only along the c direction and in the ab plane the structure remains long-range ordered. In this disordered phase additional satellite reflections appear. Upon heating above 135 K, the diffuse maxima return to their previous shape and this process is completely reversible. Rapidly cooled samples, on the other hand, do not show such splitting and the symmetry remains R\bar 3, despite a jump in lattice parameters. We use a special technique to analyse the disorder model of the slowly cooled samples, which consists of layered domains shifted in the hexagonal ab plane. The low-spin disordered phase was solved in a novel approach to accommodate the very unusual twinning and refined in the non-standard space group C\bar 1. In contrast to the ordered low-spin phase, the Fe ion is in a non-centrosymmetric coordination polyhedron and two of the six propyl groups change their conformation.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768111053298/pc5004sup1.cif
Contains datablocks PTZ_LS-dis_P-1, PTZ_LS-dis_C-1, PTZ_LS-ord_C-1, PTZ_LS-ord_R-3

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768111053298/pc5004LS-dis_p-1sup2.fcf
Contains datablock LS-dis_p-1

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768111053298/pc5004LS-dis_c-1sup3.fcf
Contains datablock LS-dis_c-1

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768111053298/pc5004LS-ord_c-1sup4.fcf
Contains datablock LS-ord_c-1

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768111053298/pc5004LS-ord_r-3sup5.fcf
Contains datablock LS-ord_r-3

CCDC references: 866764; 866765; 866766; 866767

Computing details top

For all compounds, data collection: CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29; cell refinement: CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29; data reduction: CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29. Program(s) used to solve structure: SuperFlip (Palatinus, 2007) for PTZ_LS-dis_P-1, PTZ_LS-dis_C-1, PTZ_LS-ord_C-1; SHELXS97 (Sheldrick, 2008) for PTZ_LS-ord_R-3. For all compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 2008).

(PTZ_LS-dis_P-1) top
Crystal data top
C24H48FeN24·2(BF4)V = 4148.2 (5) Å3
Mr = 902.33Z = 4
Triclinic, P1F(000) = 1872
Hall symbol: -P 1Dx = 1.445 Mg m3
a = 16.1235 (12) ÅMo Kα radiation, λ = 0.71073 Å
b = 16.0450 (11) ŵ = 0.45 mm1
c = 16.3134 (12) ÅT = 84 K
α = 83.583 (6)°Plate, violet
β = 96.870 (6)°0.61 × 0.53 × 0.14 mm
γ = 95.663 (6)°
Data collection top
Oxford Diffraction Diffractometer with Sapphire3 detector12420 independent reflections
Radiation source: fine-focus sealed tube8851 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
Detector resolution: 16.0328 pixels mm-1θmax = 25.1°, θmin = 3.4°
ω – scanh = 1919
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1919
Tmin = 0.770, Tmax = 0.939l = 1919
24788 measured reflections
Refinement top
Refinement on F2Primary atom site location: iterative
Least-squares matrix: full with fixed elements per cycleSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.070Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.218H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.1074P)2 + 8.908P]
where P = (Fo2 + 2Fc2)/3
12420 reflections(Δ/σ)max = 1.256
771 parametersΔρmax = 0.72 e Å3
0 restraintsΔρmin = 0.90 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.25312 (4)0.50534 (4)0.24988 (4)0.0180 (2)
N1110.3762 (2)0.4895 (2)0.2712 (3)0.0200 (5)
N1120.4318 (3)0.5177 (3)0.2165 (3)0.0240 (6)
N1130.5056 (3)0.4938 (3)0.2465 (3)0.0294 (6)
N1140.4982 (2)0.4529 (3)0.3229 (3)0.0251 (6)
C1110.4199 (3)0.4498 (3)0.3372 (3)0.0208 (6)
H1110.39750.42380.38600.025*
C1120.5714 (3)0.4172 (3)0.3746 (4)0.0304 (7)
H11A0.55400.39250.42890.036*
H11B0.61580.46320.38500.036*
C1130.6073 (3)0.3499 (3)0.3336 (4)0.0318 (8)
H11C0.65530.32830.37080.038*
H11D0.62870.37580.28140.038*
C1140.5430 (4)0.2761 (4)0.3143 (5)0.0460 (10)
H11E0.57100.23170.29470.069*
H11F0.49950.29540.27110.069*
H11G0.51730.25370.36460.069*
N1210.2642 (3)0.5276 (3)0.1297 (3)0.0231 (6)
N1220.2400 (3)0.4706 (3)0.0727 (3)0.0294 (6)
N1230.2584 (3)0.5007 (3)0.0003 (3)0.0296 (6)
N1240.2934 (3)0.5807 (3)0.0084 (3)0.0236 (6)
C1210.2982 (3)0.5948 (3)0.0861 (3)0.0187 (6)
H1210.32220.64520.10820.022*
C1220.3216 (3)0.6361 (3)0.0618 (3)0.0287 (7)
H12C0.32720.69500.04790.034*
H12D0.27860.63180.11020.034*
C1230.4067 (3)0.6145 (3)0.0859 (4)0.0319 (8)
H12A0.39950.55780.10550.038*
H12B0.42360.65530.13230.038*
C1240.4768 (4)0.6162 (4)0.0134 (4)0.0385 (8)
H12E0.53000.60730.03310.058*
H12F0.46350.57150.03030.058*
H12G0.48170.67100.00890.058*
N1310.2785 (3)0.6275 (3)0.2611 (3)0.0197 (5)
N1320.2272 (3)0.6883 (3)0.2279 (3)0.0267 (6)
N1330.2597 (3)0.7635 (3)0.2443 (3)0.0245 (6)
N1340.3340 (3)0.7509 (2)0.2900 (3)0.0201 (5)
C1310.3470 (3)0.6706 (3)0.2983 (3)0.0204 (6)
H1310.39580.64670.32560.025*
C1320.3930 (3)0.8242 (3)0.3165 (4)0.0266 (7)
H13A0.44730.80380.34130.032*
H13B0.40340.86430.26740.032*
C1330.3581 (3)0.8670 (3)0.3766 (4)0.0316 (8)
H13C0.30660.89180.34970.038*
H13D0.39890.91360.39420.038*
C1340.3368 (4)0.8091 (4)0.4531 (4)0.0446 (9)
H13E0.31620.84180.49250.067*
H13F0.38720.78300.47940.067*
H13G0.29340.76510.43670.067*
N1410.1293 (2)0.5224 (3)0.2273 (3)0.0219 (5)
N1420.0725 (3)0.4960 (3)0.2824 (3)0.0271 (6)
N1430.0023 (3)0.5162 (3)0.2490 (3)0.0304 (6)
N1440.0073 (2)0.5531 (3)0.1711 (3)0.0247 (6)
C1410.0878 (3)0.5578 (3)0.1590 (3)0.0223 (7)
H1410.11140.58200.11030.027*
C1420.0636 (3)0.5833 (3)0.1136 (4)0.0304 (7)
H14C0.11540.54750.12470.036*
H14D0.05320.57830.05580.036*
C1430.0759 (4)0.6757 (3)0.1231 (4)0.0373 (8)
H14E0.02240.71060.11770.045*
H14F0.09230.67970.17900.045*
C1440.1442 (4)0.7097 (4)0.0566 (4)0.0440 (9)
H14G0.15940.76360.07080.066*
H14H0.19390.66920.05450.066*
H14I0.12270.71800.00230.066*
N1510.2444 (3)0.4828 (3)0.3699 (3)0.0234 (6)
N1520.2758 (3)0.5363 (3)0.4294 (3)0.0272 (6)
N1530.2624 (3)0.5029 (3)0.5020 (3)0.0273 (9)
N1540.2219 (3)0.4254 (2)0.4934 (3)0.0234 (9)
C1510.2104 (3)0.4148 (3)0.4145 (3)0.0196 (6)
H1510.18230.36630.39190.024*
C1520.2008 (3)0.3673 (3)0.5649 (3)0.0262 (7)
H15A0.25020.36550.60730.031*
H15B0.18700.31000.54740.031*
C1530.1279 (3)0.3929 (3)0.6029 (4)0.0291 (7)
H15C0.14400.44770.62530.035*
H15D0.11510.35090.64990.035*
C1540.0482 (4)0.4004 (4)0.5408 (4)0.0432 (9)
H15E0.00180.41250.57000.065*
H15F0.03380.34740.51580.065*
H15G0.05860.44620.49720.065*
N1610.2286 (2)0.3825 (3)0.2401 (2)0.0180 (5)
N1620.2815 (3)0.3240 (3)0.2743 (3)0.0298 (6)
N1630.2489 (3)0.2479 (3)0.2607 (3)0.0284 (6)
N1640.1740 (3)0.2579 (2)0.2154 (3)0.0218 (5)
C1610.1607 (3)0.3387 (3)0.2039 (3)0.0208 (6)
H1610.11200.36170.17530.025*
C1620.1134 (3)0.1835 (3)0.1955 (4)0.0286 (7)
H16A0.09600.15350.24790.034*
H16B0.06270.20400.16210.034*
C1630.1494 (3)0.1238 (3)0.1494 (3)0.0262 (7)
H16C0.17600.15620.10270.031*
H16D0.10300.08570.12530.031*
C1640.2159 (4)0.0687 (4)0.2022 (4)0.0361 (8)
H16E0.22920.02500.16950.054*
H16F0.19300.04210.25270.054*
H16G0.26700.10450.21730.054*
Fe20.75223 (4)0.00501 (4)0.25002 (4)0.0207 (2)
N2110.8752 (3)0.0108 (3)0.2731 (3)0.0200 (5)
N2120.9313 (3)0.0170 (3)0.2186 (3)0.0240 (6)
N2131.0048 (3)0.0059 (3)0.2481 (3)0.0294 (6)
N2140.9978 (3)0.0490 (3)0.3218 (3)0.0251 (6)
C2110.9179 (3)0.0543 (3)0.3351 (4)0.0208 (6)
H2110.89490.08460.38170.025*
C2121.0699 (3)0.0843 (4)0.3746 (4)0.0304 (7)
H21C1.05130.11020.42810.036*
H21D1.11360.03820.38670.036*
C2131.1074 (4)0.1501 (4)0.3334 (4)0.0318 (8)
H21A1.15530.17160.37090.038*
H21B1.12920.12330.28170.038*
C2141.0432 (4)0.2246 (4)0.3125 (5)0.0460 (10)
H21E1.06930.26350.28330.069*
H21F0.99470.20350.27710.069*
H21G1.02480.25420.36400.069*
N2210.7636 (3)0.0278 (3)0.1295 (3)0.0231 (6)
N2220.7393 (3)0.0316 (3)0.0726 (3)0.0294 (6)
N2230.7565 (3)0.0013 (3)0.0004 (3)0.0296 (6)
N2240.7934 (3)0.0804 (3)0.0082 (3)0.0236 (6)
C2210.7964 (3)0.0956 (3)0.0858 (3)0.0187 (6)
H2210.81850.14670.10740.022*
C2220.8224 (4)0.1345 (4)0.0640 (4)0.0287 (7)
H22A0.82810.19400.05160.034*
H22B0.77960.12920.11240.034*
C2230.9051 (4)0.1124 (4)0.0862 (4)0.0319 (8)
H22C0.92150.15190.13390.038*
H22D0.89730.05510.10460.038*
C2240.9778 (4)0.1151 (4)0.0154 (4)0.0385 (8)
H22E1.02890.10030.03520.058*
H22F0.96330.07480.03150.058*
H22G0.98720.17190.00250.058*
N2310.7786 (3)0.1274 (3)0.2619 (3)0.0197 (5)
N2320.7256 (3)0.1895 (3)0.2266 (3)0.0267 (6)
N2330.7609 (3)0.2626 (3)0.2434 (3)0.0245 (6)
N2340.8353 (3)0.2502 (3)0.2884 (3)0.0201 (5)
C2310.8459 (3)0.1686 (3)0.2994 (3)0.0204 (6)
H2310.89320.14370.32890.025*
C2320.8928 (4)0.3237 (3)0.3175 (4)0.0266 (7)
H23A0.94700.30330.34260.032*
H23B0.90390.36440.26890.032*
C2330.8572 (4)0.3677 (4)0.3791 (4)0.0316 (8)
H23C0.80540.39210.35240.038*
H23D0.89780.41470.39610.038*
C2340.8368 (4)0.3104 (4)0.4563 (4)0.0446 (9)
H23E0.81750.34370.49610.067*
H23F0.88710.28380.48170.067*
H23G0.79250.26680.44080.067*
N2410.6289 (3)0.0198 (3)0.2265 (3)0.0219 (5)
N2420.5729 (3)0.0041 (3)0.2819 (3)0.0271 (6)
N2430.5003 (3)0.0166 (3)0.2481 (3)0.0304 (6)
N2440.5064 (3)0.0520 (3)0.1711 (3)0.0247 (6)
C2410.5854 (3)0.0562 (3)0.1590 (4)0.0223 (7)
H2410.60830.08110.11010.027*
C2420.4351 (3)0.0849 (4)0.1146 (4)0.0304 (7)
H24A0.38290.05000.12630.036*
H24B0.44430.07950.05650.036*
C2430.4238 (4)0.1760 (4)0.1229 (5)0.0373 (8)
H24C0.47750.21060.11730.045*
H24D0.40710.18090.17860.045*
C2440.3562 (4)0.2086 (4)0.0558 (5)0.0440 (9)
H24E0.35220.26860.05930.066*
H24F0.30200.17730.06430.066*
H24G0.37120.20060.00090.066*
N2510.7423 (3)0.0187 (3)0.3713 (3)0.0234 (6)
N2520.7757 (3)0.0366 (3)0.4294 (3)0.0272 (6)
N2530.7211 (3)0.0749 (3)0.4929 (3)0.0273 (9)
N2540.7616 (3)0.0019 (3)0.5029 (3)0.0234 (9)
C2510.7083 (3)0.0870 (3)0.4136 (4)0.0196 (6)
H2510.68010.13540.39080.024*
C2520.6991 (4)0.1331 (4)0.5655 (4)0.0262 (7)
H25C0.74840.13480.60790.031*
H25D0.68550.19050.54820.031*
C2530.6257 (4)0.1081 (4)0.6038 (4)0.0291 (7)
H25A0.64190.05390.62760.035*
H25B0.61220.15110.64980.035*
C2540.5470 (4)0.0989 (5)0.5411 (5)0.0432 (9)
H25E0.50110.08380.56940.065*
H25F0.53060.15240.51740.065*
H25G0.55930.05470.49660.065*
N2610.7283 (3)0.1172 (3)0.2384 (3)0.0180 (5)
N2620.7809 (3)0.1776 (3)0.2749 (3)0.0298 (6)
N2630.7481 (3)0.2518 (3)0.2615 (3)0.0284 (6)
N2640.6730 (3)0.2420 (3)0.2148 (3)0.0218 (5)
C2610.6596 (3)0.1614 (3)0.2030 (3)0.0208 (6)
H2610.61060.13840.17490.025*
C2620.6127 (3)0.3168 (3)0.1944 (4)0.0286 (7)
H26A0.59430.34650.24660.034*
H26B0.56250.29660.15990.034*
C2630.6499 (3)0.3774 (3)0.1493 (4)0.0262 (7)
H26C0.67760.34550.10310.031*
H26D0.60390.41570.12470.031*
C2640.7132 (4)0.4303 (4)0.2026 (4)0.0361 (8)
H26E0.73180.47060.16920.054*
H26F0.68700.46090.24960.054*
H26G0.76150.39350.22330.054*
B1000.0776 (4)0.1732 (4)0.4294 (4)0.0203 (6)
F1010.12768 (19)0.1695 (2)0.5044 (2)0.0397 (10)
F1020.0075 (2)0.1807 (3)0.4487 (3)0.0751 (15)
F1030.0835 (4)0.1084 (2)0.3905 (3)0.0801 (17)
F1040.1004 (2)0.24742 (19)0.3812 (2)0.0352 (10)
B2000.4322 (4)0.3203 (4)0.5669 (4)0.0203 (6)
F2010.3748 (2)0.3334 (3)0.4957 (3)0.0562 (14)
F2020.4015 (2)0.2522 (2)0.6186 (2)0.0393 (11)
F2030.5044 (2)0.3163 (4)0.5495 (3)0.090 (2)
F2040.4335 (5)0.3897 (3)0.6122 (3)0.143 (3)
B3000.0854 (4)0.3406 (4)0.0857 (4)0.0203 (6)
F3010.0027 (2)0.3665 (3)0.0762 (2)0.0463 (12)
F3020.1223 (2)0.39330 (19)0.1186 (2)0.0382 (10)
F3030.0837 (2)0.2587 (2)0.1272 (2)0.0372 (11)
F3040.1216 (2)0.3284 (2)0.0011 (2)0.0390 (11)
B4000.4249 (4)0.8324 (4)0.0760 (4)0.0203 (6)
F4010.5044 (2)0.8663 (3)0.0775 (3)0.0569 (14)
F4020.4134 (2)0.7592 (2)0.1293 (2)0.0353 (10)
F4030.3795 (3)0.8916 (3)0.1160 (3)0.0534 (13)
F4040.3790 (2)0.8316 (3)0.0010 (2)0.0392 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0167 (4)0.0180 (4)0.0180 (5)0.0052 (4)0.0012 (4)0.0059 (4)
N1110.0211 (10)0.0206 (10)0.0178 (10)0.0108 (9)0.0052 (9)0.0074 (9)
N1120.0171 (10)0.0251 (11)0.0295 (12)0.0041 (9)0.0049 (10)0.0031 (10)
N1130.0218 (11)0.0314 (12)0.0329 (13)0.0044 (10)0.0039 (10)0.0009 (11)
N1140.0163 (10)0.0278 (11)0.0269 (12)0.0105 (9)0.0034 (9)0.0017 (10)
C1110.0175 (12)0.0234 (12)0.0214 (13)0.0019 (11)0.0017 (11)0.0089 (11)
C1120.0158 (12)0.0375 (14)0.0324 (15)0.0109 (12)0.0084 (12)0.0031 (13)
C1130.0238 (13)0.0285 (14)0.0435 (17)0.0001 (12)0.0016 (13)0.0101 (13)
C1140.0464 (18)0.0329 (15)0.057 (2)0.0064 (15)0.0017 (17)0.0127 (15)
N1210.0216 (10)0.0195 (10)0.0271 (12)0.0052 (9)0.0002 (10)0.0065 (9)
N1220.0371 (12)0.0236 (11)0.0255 (12)0.0080 (10)0.0029 (11)0.0036 (10)
N1230.0399 (13)0.0219 (10)0.0255 (12)0.0120 (10)0.0043 (11)0.0074 (10)
N1240.0252 (11)0.0185 (10)0.0262 (12)0.0077 (9)0.0023 (10)0.0073 (9)
C1210.0133 (11)0.0200 (11)0.0213 (13)0.0096 (10)0.0033 (10)0.0109 (10)
C1220.0365 (14)0.0265 (13)0.0210 (14)0.0110 (12)0.0038 (12)0.0038 (11)
C1230.0379 (15)0.0257 (13)0.0323 (15)0.0099 (13)0.0079 (13)0.0106 (12)
C1240.0256 (14)0.0454 (17)0.0429 (18)0.0047 (13)0.0009 (14)0.0097 (15)
N1310.0233 (10)0.0274 (11)0.0093 (9)0.0035 (9)0.0040 (9)0.0020 (9)
N1320.0268 (11)0.0227 (10)0.0281 (12)0.0075 (9)0.0027 (10)0.0067 (10)
N1330.0210 (10)0.0219 (10)0.0287 (12)0.0049 (9)0.0013 (10)0.0042 (10)
N1340.0232 (10)0.0157 (9)0.0186 (10)0.0095 (9)0.0016 (9)0.0027 (8)
C1310.0167 (11)0.0255 (12)0.0194 (13)0.0064 (10)0.0068 (10)0.0056 (11)
C1320.0251 (13)0.0127 (11)0.0384 (15)0.0103 (11)0.0059 (12)0.0072 (11)
C1330.0258 (14)0.0221 (12)0.0489 (18)0.0005 (12)0.0014 (14)0.0200 (13)
C1340.0398 (16)0.0469 (17)0.0489 (19)0.0126 (15)0.0057 (15)0.0260 (15)
N1410.0199 (10)0.0246 (10)0.0205 (11)0.0099 (9)0.0049 (9)0.0067 (9)
N1420.0179 (10)0.0318 (11)0.0290 (12)0.0051 (10)0.0044 (10)0.0042 (10)
N1430.0215 (11)0.0352 (12)0.0324 (13)0.0031 (10)0.0039 (10)0.0025 (11)
N1440.0163 (10)0.0269 (11)0.0265 (12)0.0090 (9)0.0032 (9)0.0013 (10)
C1410.0197 (12)0.0211 (12)0.0243 (14)0.0040 (11)0.0006 (11)0.0024 (11)
C1420.0203 (12)0.0352 (14)0.0312 (15)0.0125 (12)0.0045 (12)0.0046 (12)
C1430.0294 (14)0.0293 (14)0.0497 (18)0.0089 (13)0.0036 (14)0.0068 (14)
C1440.0317 (15)0.0402 (16)0.054 (2)0.0071 (14)0.0049 (15)0.0010 (16)
N1510.0175 (10)0.0213 (10)0.0307 (12)0.0058 (9)0.0005 (9)0.0102 (9)
N1520.0287 (11)0.0218 (10)0.0281 (12)0.0093 (9)0.0006 (10)0.0043 (10)
N1530.0306 (16)0.0250 (15)0.0232 (17)0.0093 (14)0.0013 (15)0.0012 (14)
N1540.0205 (16)0.0192 (15)0.0291 (19)0.0104 (14)0.0018 (15)0.0081 (15)
C1510.0148 (11)0.0163 (11)0.0266 (13)0.0053 (10)0.0002 (11)0.0053 (11)
C1520.0322 (14)0.0220 (12)0.0221 (13)0.0060 (11)0.0027 (12)0.0003 (11)
C1530.0300 (14)0.0233 (13)0.0364 (16)0.0021 (12)0.0110 (13)0.0093 (12)
C1540.0247 (14)0.0448 (17)0.059 (2)0.0026 (14)0.0040 (15)0.0021 (17)
N1610.0200 (10)0.0269 (10)0.0076 (9)0.0024 (9)0.0007 (8)0.0049 (9)
N1620.0280 (11)0.0255 (11)0.0298 (12)0.0075 (10)0.0112 (10)0.0001 (10)
N1630.0254 (11)0.0227 (10)0.0323 (13)0.0099 (9)0.0059 (10)0.0025 (10)
N1640.0218 (10)0.0169 (9)0.0232 (11)0.0116 (9)0.0010 (9)0.0021 (9)
C1610.0166 (11)0.0233 (12)0.0235 (13)0.0067 (10)0.0073 (11)0.0087 (11)
C1620.0191 (12)0.0230 (12)0.0390 (16)0.0154 (11)0.0023 (12)0.0033 (12)
C1630.0224 (12)0.0248 (12)0.0317 (15)0.0079 (11)0.0021 (12)0.0135 (12)
C1640.0292 (14)0.0350 (14)0.0438 (17)0.0084 (13)0.0007 (14)0.0156 (14)
Fe20.0168 (5)0.0231 (5)0.0189 (5)0.0109 (4)0.0014 (4)0.0020 (4)
N2110.0211 (10)0.0206 (10)0.0178 (10)0.0108 (9)0.0052 (9)0.0074 (9)
N2120.0171 (10)0.0251 (11)0.0295 (12)0.0041 (9)0.0049 (10)0.0031 (10)
N2130.0218 (11)0.0314 (12)0.0329 (13)0.0044 (10)0.0039 (10)0.0009 (11)
N2140.0163 (10)0.0278 (11)0.0269 (12)0.0105 (9)0.0034 (9)0.0017 (10)
C2110.0175 (12)0.0234 (12)0.0214 (13)0.0019 (11)0.0017 (11)0.0089 (11)
C2120.0158 (12)0.0375 (14)0.0324 (15)0.0109 (12)0.0084 (12)0.0031 (13)
C2130.0238 (13)0.0285 (14)0.0435 (17)0.0001 (12)0.0016 (13)0.0101 (13)
C2140.0464 (18)0.0329 (15)0.057 (2)0.0064 (15)0.0017 (17)0.0127 (15)
N2210.0216 (10)0.0195 (10)0.0271 (12)0.0052 (9)0.0002 (10)0.0065 (9)
N2220.0371 (12)0.0236 (11)0.0255 (12)0.0080 (10)0.0029 (11)0.0036 (10)
N2230.0399 (13)0.0219 (10)0.0255 (12)0.0120 (10)0.0043 (11)0.0074 (10)
N2240.0252 (11)0.0185 (10)0.0262 (12)0.0077 (9)0.0023 (10)0.0073 (9)
C2210.0133 (11)0.0200 (11)0.0213 (13)0.0096 (10)0.0033 (10)0.0109 (10)
C2220.0365 (14)0.0265 (13)0.0210 (14)0.0110 (12)0.0038 (12)0.0038 (11)
C2230.0379 (15)0.0257 (13)0.0323 (15)0.0099 (13)0.0079 (13)0.0106 (12)
C2240.0256 (14)0.0454 (17)0.0429 (18)0.0047 (13)0.0009 (14)0.0097 (15)
N2310.0233 (10)0.0274 (11)0.0093 (9)0.0035 (9)0.0040 (9)0.0020 (9)
N2320.0268 (11)0.0227 (10)0.0281 (12)0.0075 (9)0.0027 (10)0.0067 (10)
N2330.0210 (10)0.0219 (10)0.0287 (12)0.0049 (9)0.0013 (10)0.0042 (10)
N2340.0232 (10)0.0157 (9)0.0186 (10)0.0095 (9)0.0016 (9)0.0027 (8)
C2310.0167 (11)0.0255 (12)0.0194 (13)0.0064 (10)0.0068 (10)0.0056 (11)
C2320.0251 (13)0.0127 (11)0.0384 (15)0.0103 (11)0.0059 (12)0.0072 (11)
C2330.0258 (14)0.0221 (12)0.0489 (18)0.0005 (12)0.0014 (14)0.0200 (13)
C2340.0398 (16)0.0469 (17)0.0489 (19)0.0126 (15)0.0057 (15)0.0260 (15)
N2410.0199 (10)0.0246 (10)0.0205 (11)0.0099 (9)0.0049 (9)0.0067 (9)
N2420.0179 (10)0.0318 (11)0.0290 (12)0.0051 (10)0.0044 (10)0.0042 (10)
N2430.0215 (11)0.0352 (12)0.0324 (13)0.0031 (10)0.0039 (10)0.0025 (11)
N2440.0163 (10)0.0269 (11)0.0265 (12)0.0090 (9)0.0032 (9)0.0013 (10)
C2410.0197 (12)0.0211 (12)0.0243 (14)0.0040 (11)0.0006 (11)0.0024 (11)
C2420.0203 (12)0.0352 (14)0.0312 (15)0.0125 (12)0.0045 (12)0.0046 (12)
C2430.0294 (14)0.0293 (14)0.0497 (18)0.0089 (13)0.0036 (14)0.0068 (14)
C2440.0317 (15)0.0402 (16)0.054 (2)0.0071 (14)0.0049 (15)0.0010 (16)
N2510.0175 (10)0.0213 (10)0.0307 (12)0.0058 (9)0.0005 (9)0.0102 (9)
N2520.0287 (11)0.0218 (10)0.0281 (12)0.0093 (9)0.0006 (10)0.0043 (10)
N2530.0306 (16)0.0250 (15)0.0232 (17)0.0093 (14)0.0013 (15)0.0012 (14)
N2540.0205 (16)0.0192 (15)0.0291 (19)0.0104 (14)0.0018 (15)0.0081 (15)
C2510.0148 (11)0.0163 (11)0.0266 (13)0.0053 (10)0.0002 (11)0.0053 (11)
C2520.0322 (14)0.0220 (12)0.0221 (13)0.0060 (11)0.0027 (12)0.0003 (11)
C2530.0300 (14)0.0233 (13)0.0364 (16)0.0021 (12)0.0110 (13)0.0093 (12)
C2540.0247 (14)0.0448 (17)0.059 (2)0.0026 (14)0.0040 (15)0.0021 (17)
N2610.0200 (10)0.0269 (10)0.0076 (9)0.0024 (9)0.0007 (8)0.0049 (9)
N2620.0280 (11)0.0255 (11)0.0298 (12)0.0075 (10)0.0112 (10)0.0001 (10)
N2630.0254 (11)0.0227 (10)0.0323 (13)0.0099 (9)0.0059 (10)0.0025 (10)
N2640.0218 (10)0.0169 (9)0.0232 (11)0.0116 (9)0.0010 (9)0.0021 (9)
C2610.0166 (11)0.0233 (12)0.0235 (13)0.0067 (10)0.0073 (11)0.0087 (11)
C2620.0191 (12)0.0230 (12)0.0390 (16)0.0154 (11)0.0023 (12)0.0033 (12)
C2630.0224 (12)0.0248 (12)0.0317 (15)0.0079 (11)0.0021 (12)0.0135 (12)
C2640.0292 (14)0.0350 (14)0.0438 (17)0.0084 (13)0.0007 (14)0.0156 (14)
B1000.0204 (13)0.0253 (13)0.0158 (12)0.0016 (12)0.0020 (12)0.0115 (12)
F1010.0162 (14)0.074 (2)0.0245 (17)0.0117 (16)0.0015 (14)0.0008 (18)
F1020.038 (2)0.099 (3)0.071 (3)0.013 (2)0.007 (2)0.041 (3)
F1030.167 (5)0.0258 (18)0.048 (3)0.018 (2)0.003 (3)0.0118 (19)
F1040.0457 (19)0.0268 (15)0.0310 (18)0.0160 (15)0.0014 (16)0.0137 (14)
B2000.0204 (13)0.0253 (13)0.0158 (12)0.0016 (12)0.0020 (12)0.0115 (12)
F2010.032 (2)0.068 (3)0.052 (3)0.007 (2)0.0196 (19)0.027 (2)
F2020.039 (2)0.039 (2)0.037 (2)0.0148 (17)0.0077 (18)0.0006 (18)
F2030.0268 (19)0.166 (5)0.075 (3)0.041 (3)0.034 (2)0.064 (3)
F2040.326 (8)0.041 (2)0.057 (3)0.081 (3)0.061 (4)0.022 (2)
B3000.0204 (13)0.0253 (13)0.0158 (12)0.0016 (12)0.0020 (12)0.0115 (12)
F3010.0168 (16)0.068 (2)0.051 (2)0.0063 (17)0.0016 (16)0.006 (2)
F3020.053 (2)0.0216 (15)0.046 (2)0.0070 (16)0.0033 (18)0.0250 (16)
F3030.056 (2)0.0163 (15)0.041 (2)0.0033 (16)0.0031 (19)0.0118 (15)
F3040.044 (2)0.0360 (18)0.029 (2)0.0180 (17)0.0124 (17)0.0040 (16)
B4000.0204 (13)0.0253 (13)0.0158 (12)0.0016 (12)0.0020 (12)0.0115 (12)
F4010.035 (2)0.083 (3)0.040 (2)0.024 (2)0.0020 (19)0.018 (2)
F4020.040 (2)0.041 (2)0.0213 (19)0.0166 (17)0.0066 (17)0.0028 (17)
F4030.054 (2)0.049 (2)0.050 (3)0.008 (2)0.001 (2)0.009 (2)
F4040.037 (2)0.050 (2)0.023 (2)0.0189 (19)0.0069 (18)0.0014 (18)
Geometric parameters (Å, º) top
Fe1—N1511.971 (5)N212—N2131.296 (7)
Fe1—N1211.979 (5)N213—N2141.328 (7)
Fe1—N1311.987 (4)N214—C2111.324 (7)
Fe1—N1611.991 (4)N214—C2121.483 (7)
Fe1—N1112.009 (4)C211—H2110.9500
Fe1—N1412.026 (4)C212—C2131.521 (10)
N111—N1121.351 (6)C212—H21C0.9900
N111—C1111.348 (7)C212—H21D0.9900
N112—N1131.308 (6)C213—C2141.543 (9)
N113—N1141.355 (7)C213—H21A0.9900
N114—C1111.306 (7)C213—H21B0.9900
N114—C1121.491 (7)C214—H21E0.9800
C111—H1110.9500C214—H21F0.9800
C112—C1131.525 (9)C214—H21G0.9800
C112—H11A0.9900N221—C2211.331 (7)
C112—H11B0.9900N221—N2221.399 (7)
C113—C1141.530 (8)N222—N2231.297 (7)
C113—H11C0.9900N223—N2241.362 (6)
C113—H11D0.9900N224—C2211.310 (8)
C114—H11E0.9800N224—C2221.477 (8)
C114—H11F0.9800C221—H2210.9500
C114—H11G0.9800C222—C2231.508 (9)
N121—C1211.332 (6)C222—H22A0.9900
N121—N1221.374 (6)C222—H22B0.9900
N122—N1231.290 (7)C223—C2241.545 (9)
N123—N1241.367 (6)C223—H22C0.9900
N124—C1211.304 (7)C223—H22D0.9900
N124—C1221.459 (7)C224—H22E0.9800
C121—H1210.9500C224—H22F0.9800
C122—C1231.553 (9)C224—H22G0.9800
C122—H12C0.9900N231—C2311.333 (7)
C122—H12D0.9900N231—N2321.405 (7)
C123—C1241.536 (8)N232—N2331.296 (6)
C123—H12A0.9900N233—N2341.350 (6)
C123—H12B0.9900N234—C2311.326 (7)
C124—H12E0.9800N234—C2321.511 (7)
C124—H12F0.9800C231—H2310.9500
C124—H12G0.9800C232—C2331.489 (10)
N131—C1311.359 (6)C232—H23A0.9900
N131—N1321.365 (6)C232—H23B0.9900
N132—N1331.310 (6)C233—C2341.523 (10)
N133—N1341.354 (6)C233—H23C0.9900
N134—C1311.316 (7)C233—H23D0.9900
N134—C1321.506 (6)C234—H23E0.9800
C131—H1310.9500C234—H23F0.9800
C132—C1331.452 (9)C234—H23G0.9800
C132—H13A0.9900N241—C2411.341 (7)
C132—H13B0.9900N241—N2421.353 (7)
C133—C1341.523 (9)N242—N2431.290 (7)
C133—H13C0.9900N243—N2441.330 (7)
C133—H13D0.9900N244—C2411.306 (7)
C134—H13E0.9800N244—C2421.486 (7)
C134—H13F0.9800C241—H2410.9500
C134—H13G0.9800C242—C2431.513 (9)
N141—C1411.329 (7)C242—H24A0.9900
N141—N1421.363 (6)C242—H24B0.9900
N142—N1431.318 (6)C243—C2441.536 (9)
N143—N1441.360 (7)C243—H24C0.9900
N144—C1411.328 (7)C243—H24D0.9900
N144—C1421.474 (7)C244—H24E0.9800
C141—H1410.9500C244—H24F0.9800
C142—C1431.543 (8)C244—H24G0.9800
C142—H14C0.9900N251—C2511.334 (7)
C142—H14D0.9900N251—N2521.395 (7)
C143—C1441.545 (9)N252—N2541.300 (7)
C143—H14E0.9900N253—C2511.319 (8)
C143—H14F0.9900N253—N2541.353 (6)
C144—H14G0.9800N253—C2521.479 (7)
C144—H14H0.9800C251—H2510.9500
C144—H14I0.9800C252—C2531.510 (9)
N151—C1511.349 (6)C252—H25C0.9900
N151—N1521.384 (6)C252—H25D0.9900
N152—N1531.279 (6)C253—C2541.540 (9)
N153—N1541.360 (6)C253—H25A0.9900
N154—C1511.306 (7)C253—H25B0.9900
N154—C1521.461 (7)C254—H25E0.9800
C151—H1510.9500C254—H25F0.9800
C152—C1531.503 (8)C254—H25G0.9800
C152—H15A0.9900N261—C2611.359 (7)
C152—H15B0.9900N261—N2621.387 (7)
C153—C1541.544 (8)N262—N2631.284 (7)
C153—H15C0.9900N263—N2641.364 (7)
C153—H15D0.9900N264—C2611.322 (7)
C154—H15E0.9800N264—C2621.510 (7)
C154—H15F0.9800C261—H2610.9500
C154—H15G0.9800C262—C2631.492 (9)
N161—C1611.353 (6)C262—H26A0.9900
N161—N1621.359 (6)C262—H26B0.9900
N162—N1631.312 (6)C263—C2641.520 (9)
N163—N1641.352 (6)C263—H26C0.9900
N164—C1611.323 (7)C263—H26D0.9900
N164—C1621.505 (6)C264—H26E0.9800
C161—H1610.9500C264—H26F0.9800
C162—C1631.482 (8)C264—H26G0.9800
C162—H16A0.9900B100—F1031.295 (8)
C162—H16B0.9900B100—F1011.382 (7)
C163—C1641.572 (8)B100—F1041.395 (7)
C163—H16C0.9900B100—F1021.463 (8)
C163—H16D0.9900B200—F2031.240 (8)
C164—H16E0.9800B200—F2041.401 (8)
C164—H16F0.9800B200—F2021.392 (7)
C164—H16G0.9800B200—F2011.407 (8)
Fe2—N2211.987 (5)B300—F3021.278 (8)
Fe2—N2611.986 (5)B300—F3031.411 (7)
Fe2—N2311.994 (5)B300—F3041.460 (7)
Fe2—N2511.996 (5)B300—F3011.461 (7)
Fe2—N2112.009 (5)B400—F4011.340 (8)
Fe2—N2412.011 (5)B400—F4041.353 (8)
N211—C2111.324 (7)B400—F4021.392 (8)
N211—N2121.354 (7)B400—F4031.501 (9)
N151—Fe1—N121178.94 (13)N231—Fe2—N24191.29 (13)
N151—Fe1—N13190.52 (12)N251—Fe2—N24191.00 (14)
N121—Fe1—N13189.49 (12)N211—Fe2—N241179.46 (14)
N151—Fe1—N16188.85 (12)C211—N211—N212105.2 (5)
N121—Fe1—N16191.13 (12)C211—N211—Fe2131.1 (4)
N131—Fe1—N161179.23 (12)N212—N211—Fe2123.4 (3)
N151—Fe1—N11189.56 (12)N213—N212—N211109.9 (5)
N121—Fe1—N11189.38 (13)N212—N213—N214107.7 (5)
N131—Fe1—N11189.81 (12)C211—N214—N213107.8 (5)
N161—Fe1—N11189.74 (12)C211—N214—C212129.3 (5)
N151—Fe1—N14191.00 (12)N213—N214—C212122.9 (5)
N121—Fe1—N14190.06 (13)N211—C211—N214109.3 (5)
N131—Fe1—N14189.79 (12)N211—C211—H211125.3
N161—Fe1—N14190.68 (12)N214—C211—H211125.3
N111—Fe1—N141179.32 (13)N214—C212—C213112.1 (5)
N112—N111—C111106.4 (4)N214—C212—H21C109.2
N112—N111—Fe1123.7 (3)C213—C212—H21C109.2
C111—N111—Fe1129.9 (4)N214—C212—H21D109.2
N113—N112—N111109.1 (4)C213—C212—H21D109.2
N112—N113—N114107.4 (4)H21C—C212—H21D107.9
C111—N114—N113108.5 (4)C212—C213—C214112.5 (5)
C111—N114—C112130.2 (5)C212—C213—H21A109.1
N113—N114—C112121.3 (4)C214—C213—H21A109.1
N114—C111—N111108.6 (5)C212—C213—H21B109.1
N114—C111—H111125.7C214—C213—H21B109.1
N111—C111—H111125.7H21A—C213—H21B107.8
N114—C112—C113112.6 (5)C213—C214—H21E109.5
N114—C112—H11A109.1C213—C214—H21F109.5
C113—C112—H11A109.1H21E—C214—H21F109.5
N114—C112—H11B109.1C213—C214—H21G109.5
C113—C112—H11B109.1H21E—C214—H21G109.5
H11A—C112—H11B107.8H21F—C214—H21G109.5
C112—C113—C114113.0 (5)C221—N221—N222105.6 (5)
C112—C113—H11C109.0C221—N221—Fe2130.8 (4)
C114—C113—H11C109.0N222—N221—Fe2123.5 (3)
C112—C113—H11D109.0N223—N222—N221108.8 (4)
C114—C113—H11D109.0N222—N223—N224107.2 (5)
H11C—C113—H11D107.8C221—N224—N223109.2 (5)
C113—C114—H11E109.5C221—N224—C222130.0 (5)
C113—C114—H11F109.5N223—N224—C222120.8 (5)
H11E—C114—H11F109.5N224—C221—N221109.1 (5)
C113—C114—H11G109.5N224—C221—H221125.4
H11E—C114—H11G109.5N221—C221—H221125.4
H11F—C114—H11G109.5N224—C222—C223112.9 (5)
C121—N121—N122104.5 (4)N224—C222—H22A109.0
C121—N121—Fe1130.7 (4)C223—C222—H22A109.0
N122—N121—Fe1124.7 (3)N224—C222—H22B109.0
N123—N122—N121111.4 (4)C223—C222—H22B109.0
N122—N123—N124105.3 (4)H22A—C222—H22B107.8
C121—N124—N123109.4 (4)C222—C223—C224114.9 (6)
C121—N124—C122128.9 (4)C222—C223—H22C108.5
N123—N124—C122121.7 (5)C224—C223—H22C108.5
N124—C121—N121109.4 (4)C222—C223—H22D108.5
N124—C121—H121125.3C224—C223—H22D108.5
N121—C121—H121125.3H22C—C223—H22D107.5
N124—C122—C123112.7 (5)C223—C224—H22E109.5
N124—C122—H12C109.1C223—C224—H22F109.5
C123—C122—H12C109.1H22E—C224—H22F109.5
N124—C122—H12D109.1C223—C224—H22G109.5
C123—C122—H12D109.1H22E—C224—H22G109.5
H12C—C122—H12D107.8H22F—C224—H22G109.5
C124—C123—C122112.8 (5)C231—N231—N232105.8 (4)
C124—C123—H12A109.0C231—N231—Fe2130.6 (4)
C122—C123—H12A109.0N232—N231—Fe2123.6 (3)
C124—C123—H12B109.0N233—N232—N231108.9 (4)
C122—C123—H12B109.0N232—N233—N234107.3 (4)
H12A—C123—H12B107.8C231—N234—N233109.7 (4)
C123—C124—H12E109.5C231—N234—C232129.6 (5)
C123—C124—H12F109.5N233—N234—C232120.6 (4)
H12E—C124—H12F109.5N234—C231—N231108.2 (5)
C123—C124—H12G109.5N234—C231—H231125.9
H12E—C124—H12G109.5N231—C231—H231125.9
H12F—C124—H12G109.5C233—C232—N234112.8 (5)
C131—N131—N132104.5 (4)C233—C232—H23A109.0
C131—N131—Fe1130.9 (4)N234—C232—H23A109.0
N132—N131—Fe1124.6 (3)C233—C232—H23B109.0
N133—N132—N131111.7 (4)N234—C232—H23B109.0
N132—N133—N134105.1 (4)H23A—C232—H23B107.8
C131—N134—N133110.3 (4)C232—C233—C234113.4 (5)
C131—N134—C132128.5 (4)C232—C233—H23C108.9
N133—N134—C132120.9 (4)C234—C233—H23C108.9
N134—C131—N131108.3 (4)C232—C233—H23D108.9
N134—C131—H131125.8C234—C233—H23D108.9
N131—C131—H131125.8H23C—C233—H23D107.7
C133—C132—N134110.8 (4)C233—C234—H23E109.5
C133—C132—H13A109.5C233—C234—H23F109.5
N134—C132—H13A109.5H23E—C234—H23F109.5
C133—C132—H13B109.5C233—C234—H23G109.5
N134—C132—H13B109.5H23E—C234—H23G109.5
H13A—C132—H13B108.1H23F—C234—H23G109.5
C132—C133—C134113.2 (5)C241—N241—N242105.8 (5)
C132—C133—H13C108.9C241—N241—Fe2130.2 (4)
C134—C133—H13C108.9N242—N241—Fe2123.9 (4)
C132—C133—H13D108.9N243—N242—N241108.1 (5)
C134—C133—H13D108.9N242—N243—N244109.7 (5)
H13C—C133—H13D107.8C241—N244—N243107.1 (5)
C133—C134—H13E109.5C241—N244—C242128.6 (5)
C133—C134—H13F109.5N243—N244—C242124.2 (5)
H13E—C134—H13F109.5N244—C241—N241109.2 (5)
C133—C134—H13G109.5N244—C241—H241125.4
H13E—C134—H13G109.5N241—C241—H241125.4
H13F—C134—H13G109.5N244—C242—C243113.2 (5)
C141—N141—N142107.5 (4)N244—C242—H24A108.9
C141—N141—Fe1128.6 (4)C243—C242—H24A108.9
N142—N141—Fe1123.9 (3)N244—C242—H24B108.9
N143—N142—N141109.0 (4)C243—C242—H24B108.9
N142—N143—N144106.5 (4)H24A—C242—H24B107.7
C141—N144—N143109.2 (4)C242—C243—C244110.2 (6)
C141—N144—C142128.4 (5)C242—C243—H24C109.6
N143—N144—C142122.4 (4)C244—C243—H24C109.6
N141—C141—N144107.8 (5)C242—C243—H24D109.6
N141—C141—H141126.1C244—C243—H24D109.6
N144—C141—H141126.1H24C—C243—H24D108.1
N144—C142—C143111.4 (5)C243—C244—H24E109.5
N144—C142—H14C109.4C243—C244—H24F109.5
C143—C142—H14C109.4H24E—C244—H24F109.5
N144—C142—H14D109.4C243—C244—H24G109.5
C143—C142—H14D109.4H24E—C244—H24G109.5
H14C—C142—H14D108.0H24F—C244—H24G109.5
C142—C143—C144111.1 (5)C251—N251—N252106.8 (5)
C142—C143—H14E109.4C251—N251—Fe2129.8 (4)
C144—C143—H14E109.4N252—N251—Fe2123.3 (3)
C142—C143—H14F109.4N254—N252—N251108.5 (4)
C144—C143—H14F109.4C251—N253—N254110.5 (5)
H14E—C143—H14F108.0C251—N253—C252128.7 (5)
C143—C144—H14G109.5N254—N253—C252120.8 (5)
C143—C144—H14H109.5N252—N254—N253106.9 (5)
H14G—C144—H14H109.5N253—C251—N251107.3 (5)
C143—C144—H14I109.5N253—C251—H251126.4
H14G—C144—H14I109.5N251—C251—H251126.4
H14H—C144—H14I109.5N253—C252—C253113.0 (5)
C151—N151—N152103.5 (4)N253—C252—H25C109.0
C151—N151—Fe1130.7 (4)C253—C252—H25C109.0
N152—N151—Fe1125.7 (3)N253—C252—H25D109.0
N153—N152—N151111.0 (4)C253—C252—H25D109.0
N152—N153—N154107.1 (4)H25C—C252—H25D107.8
C151—N154—N153108.3 (4)C252—C253—C254112.9 (6)
C151—N154—C152129.6 (4)C252—C253—H25A109.0
N153—N154—C152122.0 (4)C254—C253—H25A109.0
N154—C151—N151110.0 (4)C252—C253—H25B109.0
N154—C151—H151125.0C254—C253—H25B109.0
N151—C151—H151125.0H25A—C253—H25B107.8
N154—C152—C153112.0 (5)C253—C254—H25E109.5
N154—C152—H15A109.2C253—C254—H25F109.5
C153—C152—H15A109.2H25E—C254—H25F109.5
N154—C152—H15B109.2C253—C254—H25G109.5
C153—C152—H15B109.2H25E—C254—H25G109.5
H15A—C152—H15B107.9H25F—C254—H25G109.5
C152—C153—C154113.2 (5)C261—N261—N262105.1 (4)
C152—C153—H15C108.9C261—N261—Fe2131.1 (4)
C154—C153—H15C108.9N262—N261—Fe2123.6 (3)
C152—C153—H15D108.9N263—N262—N261110.7 (4)
C154—C153—H15D108.9N262—N263—N264106.7 (5)
H15C—C153—H15D107.7C261—N264—N263109.7 (4)
C153—C154—H15E109.5C261—N264—C262128.1 (5)
C153—C154—H15F109.5N263—N264—C262121.4 (4)
H15E—C154—H15F109.5N264—C261—N261107.7 (5)
C153—C154—H15G109.5N264—C261—H261126.1
H15E—C154—H15G109.5N261—C261—H261126.1
H15F—C154—H15G109.5C263—C262—N264113.0 (5)
C161—N161—N162105.6 (4)C263—C262—H26A109.0
C161—N161—Fe1131.0 (4)N264—C262—H26A109.0
N162—N161—Fe1123.4 (3)C263—C262—H26B109.0
N163—N162—N161110.8 (4)N264—C262—H26B109.0
N162—N163—N164105.8 (4)H26A—C262—H26B107.8
C161—N164—N163109.9 (4)C262—C263—C264114.7 (6)
C161—N164—C162128.1 (4)C262—C263—H26C108.6
N163—N164—C162121.4 (4)C264—C263—H26C108.6
N164—C161—N161107.9 (4)C262—C263—H26D108.6
N164—C161—H161126.0C264—C263—H26D108.6
N161—C161—H161126.0H26C—C263—H26D107.6
C163—C162—N164112.8 (4)C263—C264—H26E109.5
C163—C162—H16A109.0C263—C264—H26F109.5
N164—C162—H16A109.0H26E—C264—H26F109.5
C163—C162—H16B109.0C263—C264—H26G109.5
N164—C162—H16B109.0H26E—C264—H26G109.5
H16A—C162—H16B107.8H26F—C264—H26G109.5
C162—C163—C164115.2 (5)F103—B100—F101111.2 (5)
C162—C163—H16C108.5F103—B100—F104110.5 (5)
C164—C163—H16C108.5F101—B100—F104109.3 (4)
C162—C163—H16D108.5F103—B100—F102113.3 (5)
C164—C163—H16D108.5F101—B100—F102106.2 (5)
H16C—C163—H16D107.5F104—B100—F102106.0 (5)
C163—C164—H16E109.5F203—B200—F204107.7 (7)
C163—C164—H16F109.5F203—B200—F202115.0 (6)
H16E—C164—H16F109.5F204—B200—F202104.6 (5)
C163—C164—H16G109.5F203—B200—F201112.2 (6)
H16E—C164—H16G109.5F204—B200—F201107.2 (6)
H16F—C164—H16G109.5F202—B200—F201109.5 (5)
N221—Fe2—N26190.45 (13)F302—B300—F303116.8 (5)
N221—Fe2—N23189.48 (13)F302—B300—F304112.9 (5)
N261—Fe2—N231178.91 (13)F303—B300—F304104.8 (4)
N221—Fe2—N251179.21 (14)F302—B300—F301114.1 (5)
N261—Fe2—N25189.27 (13)F303—B300—F301103.7 (5)
N231—Fe2—N25190.79 (13)F304—B300—F301103.1 (5)
N221—Fe2—N21190.11 (14)F401—B400—F404117.2 (6)
N261—Fe2—N21189.69 (13)F401—B400—F402114.8 (6)
N231—Fe2—N21189.23 (13)F404—B400—F402114.7 (5)
N251—Fe2—N21189.15 (13)F401—B400—F403105.7 (5)
N221—Fe2—N24189.74 (14)F404—B400—F403100.8 (5)
N261—Fe2—N24189.79 (13)F402—B400—F403100.5 (5)
N151—Fe1—N111—N112161.5 (4)N221—Fe2—N211—C211154.6 (5)
N121—Fe1—N111—N11218.5 (4)N261—Fe2—N211—C21164.2 (5)
N131—Fe1—N111—N11270.9 (4)N231—Fe2—N211—C211115.9 (5)
N161—Fe1—N111—N112109.7 (4)N251—Fe2—N211—C21125.1 (5)
N141—Fe1—N111—N11217 (12)N241—Fe2—N211—C21181 (17)
N151—Fe1—N111—C11120.2 (4)N221—Fe2—N211—N21217.9 (4)
N121—Fe1—N111—C111159.8 (4)N261—Fe2—N211—N212108.4 (4)
N131—Fe1—N111—C111110.7 (4)N231—Fe2—N211—N21271.5 (4)
N161—Fe1—N111—C11168.7 (4)N251—Fe2—N211—N212162.3 (4)
N141—Fe1—N111—C111164 (55)N241—Fe2—N211—N21291 (17)
C111—N111—N112—N1132.1 (6)C211—N211—N212—N2132.4 (6)
Fe1—N111—N112—N113176.6 (3)Fe2—N211—N212—N213176.6 (4)
N111—N112—N113—N1142.6 (6)N211—N212—N213—N2140.2 (6)
N112—N113—N114—C1112.3 (6)N212—N213—N214—C2112.2 (6)
N112—N113—N114—C112180.0 (5)N212—N213—N214—C212179.2 (5)
N113—N114—C111—N1111.0 (6)N212—N211—C211—N2143.7 (6)
C112—N114—C111—N111178.5 (5)Fe2—N211—C211—N214177.3 (4)
N112—N111—C111—N1140.6 (6)N213—N214—C211—N2113.8 (6)
Fe1—N111—C111—N114178.0 (4)C212—N214—C211—N211177.7 (5)
C111—N114—C112—C113115.8 (6)C211—N214—C212—C213115.5 (7)
N113—N114—C112—C11361.4 (6)N213—N214—C212—C21362.9 (7)
N114—C112—C113—C11458.3 (7)N214—C212—C213—C21458.9 (7)
N151—Fe1—N121—C12175 (7)N261—Fe2—N221—C221164.8 (5)
N131—Fe1—N121—C12115.8 (5)N231—Fe2—N221—C22114.1 (5)
N161—Fe1—N121—C121163.7 (5)N251—Fe2—N221—C22196 (10)
N111—Fe1—N121—C12174.0 (5)N211—Fe2—N221—C22175.1 (5)
N141—Fe1—N121—C121105.6 (5)N241—Fe2—N221—C221105.4 (5)
N151—Fe1—N121—N122102 (7)N261—Fe2—N221—N22212.1 (4)
N131—Fe1—N121—N122167.9 (4)N231—Fe2—N221—N222169.0 (4)
N161—Fe1—N121—N12212.6 (4)N251—Fe2—N221—N22281 (10)
N111—Fe1—N121—N122102.3 (4)N211—Fe2—N221—N222101.8 (4)
N141—Fe1—N121—N12278.1 (4)N241—Fe2—N221—N22277.7 (4)
C121—N121—N122—N1230.4 (6)C221—N221—N222—N2230.8 (6)
Fe1—N121—N122—N123176.7 (4)Fe2—N221—N222—N223178.4 (4)
N121—N122—N123—N1241.8 (6)N221—N222—N223—N2241.4 (6)
N122—N123—N124—C1212.7 (6)N222—N223—N224—C2211.5 (7)
N122—N123—N124—C122179.0 (5)N222—N223—N224—C222178.7 (5)
N123—N124—C121—N1212.5 (6)N223—N224—C221—N2211.0 (6)
C122—N124—C121—N121179.4 (5)C222—N224—C221—N221179.3 (5)
N122—N121—C121—N1241.3 (6)N222—N221—C221—N2240.1 (6)
Fe1—N121—C121—N124178.2 (4)Fe2—N221—C221—N224177.2 (4)
C121—N124—C122—C123100.8 (6)C221—N224—C222—C223101.4 (7)
N123—N124—C122—C12377.2 (6)N223—N224—C222—C22378.8 (7)
N124—C122—C123—C12456.6 (6)N224—C222—C223—C22456.8 (7)
N151—Fe1—N131—C13169.0 (5)N221—Fe2—N231—C231110.6 (5)
N121—Fe1—N131—C131109.9 (5)N261—Fe2—N231—C23124 (8)
N161—Fe1—N131—C13133 (10)N251—Fe2—N231—C23168.7 (5)
N111—Fe1—N131—C13120.5 (5)N211—Fe2—N231—C23120.5 (5)
N141—Fe1—N131—C131160.0 (5)N241—Fe2—N231—C231159.7 (5)
N151—Fe1—N131—N132113.4 (4)N221—Fe2—N231—N23267.0 (4)
N121—Fe1—N131—N13267.6 (4)N261—Fe2—N231—N232153 (7)
N161—Fe1—N131—N132149 (10)N251—Fe2—N231—N232113.8 (4)
N111—Fe1—N131—N132157.0 (4)N211—Fe2—N231—N232157.1 (4)
N141—Fe1—N131—N13222.5 (4)N241—Fe2—N231—N23222.7 (4)
C131—N131—N132—N1331.4 (6)C231—N231—N232—N2330.2 (6)
Fe1—N131—N132—N133179.5 (4)Fe2—N231—N232—N233178.3 (4)
N131—N132—N133—N1340.3 (6)N231—N232—N233—N2340.2 (6)
N132—N133—N134—C1312.1 (6)N232—N233—N234—C2310.1 (7)
N132—N133—N134—C132176.0 (5)N232—N233—N234—C232179.4 (5)
N133—N134—C131—N1313.0 (6)N233—N234—C231—N2310.0 (7)
C132—N134—C131—N131176.4 (5)C232—N234—C231—N231179.5 (5)
N132—N131—C131—N1342.7 (6)N232—N231—C231—N2340.2 (6)
Fe1—N131—C131—N134179.5 (4)Fe2—N231—C231—N234178.1 (4)
C131—N134—C132—C133119.1 (6)C231—N234—C232—C233114.4 (7)
N133—N134—C132—C13368.1 (6)N233—N234—C232—C23366.2 (7)
N134—C132—C133—C13456.9 (6)N234—C232—C233—C23458.1 (7)
N151—Fe1—N141—C141164.4 (4)N221—Fe2—N241—C24117.4 (5)
N121—Fe1—N141—C14115.6 (4)N261—Fe2—N241—C241107.9 (5)
N131—Fe1—N141—C14173.9 (4)N231—Fe2—N241—C24172.1 (5)
N161—Fe1—N141—C141106.7 (4)N251—Fe2—N241—C241162.9 (5)
N111—Fe1—N141—C14120 (13)N211—Fe2—N241—C24191 (17)
N151—Fe1—N141—N14217.2 (4)N221—Fe2—N241—N242165.8 (4)
N121—Fe1—N141—N142162.8 (4)N261—Fe2—N241—N24275.3 (4)
N131—Fe1—N141—N142107.8 (4)N231—Fe2—N241—N242104.7 (4)
N161—Fe1—N141—N14271.6 (4)N251—Fe2—N241—N24213.9 (4)
N111—Fe1—N141—N142161 (55)N211—Fe2—N241—N24292 (17)
C141—N141—N142—N1431.1 (6)C241—N241—N242—N2430.7 (6)
Fe1—N141—N142—N143179.7 (3)Fe2—N241—N242—N243178.1 (4)
N141—N142—N143—N1442.0 (6)N241—N242—N243—N2441.2 (7)
N142—N143—N144—C1412.3 (6)N242—N243—N244—C2412.7 (7)
N142—N143—N144—C142179.1 (5)N242—N243—N244—C242178.8 (5)
N142—N141—C141—N1440.4 (6)N243—N244—C241—N2413.1 (6)
Fe1—N141—C141—N144178.2 (3)C242—N244—C241—N241178.9 (5)
N143—N144—C141—N1411.6 (6)N242—N241—C241—N2442.3 (6)
C142—N144—C141—N141179.8 (5)Fe2—N241—C241—N244179.6 (4)
C141—N144—C142—C14388.5 (7)C241—N244—C242—C24386.5 (8)
N143—N144—C142—C14389.9 (6)N243—N244—C242—C24388.7 (7)
N144—C142—C143—C144174.1 (5)N244—C242—C243—C244173.2 (5)
N121—Fe1—N151—C151106 (7)N221—Fe2—N251—C25185 (10)
N131—Fe1—N151—C151163.7 (5)N261—Fe2—N251—C25116.6 (5)
N161—Fe1—N151—C15116.7 (5)N231—Fe2—N251—C251164.5 (5)
N111—Fe1—N151—C151106.5 (5)N211—Fe2—N251—C251106.3 (5)
N141—Fe1—N151—C15173.9 (5)N241—Fe2—N251—C25173.2 (5)
N121—Fe1—N151—N15272 (7)N221—Fe2—N251—N25291 (10)
N131—Fe1—N151—N15218.1 (4)N261—Fe2—N251—N252160.2 (4)
N161—Fe1—N151—N152161.4 (4)N231—Fe2—N251—N25218.7 (4)
N111—Fe1—N151—N15271.7 (4)N211—Fe2—N251—N25270.5 (4)
N141—Fe1—N151—N152107.9 (4)N241—Fe2—N251—N252110.0 (4)
C151—N151—N152—N1530.6 (6)C251—N251—N252—N2540.2 (6)
Fe1—N151—N152—N153178.0 (4)Fe2—N251—N252—N254177.6 (4)
N151—N152—N153—N1540.4 (6)N251—N252—N254—N2531.0 (6)
N152—N153—N154—C1511.2 (6)C251—N253—N254—N2521.6 (6)
N152—N153—N154—C152176.6 (5)C252—N253—N254—N252177.0 (5)
N153—N154—C151—N1511.6 (6)N254—N253—C251—N2511.5 (7)
C152—N154—C151—N151175.9 (5)C252—N253—C251—N251177.0 (6)
N152—N151—C151—N1541.3 (6)N252—N251—C251—N2530.8 (6)
Fe1—N151—C151—N154177.1 (4)Fe2—N251—C251—N253176.4 (4)
C151—N154—C152—C153107.8 (6)C251—N253—C252—C253106.6 (7)
N153—N154—C152—C15374.9 (6)N254—N253—C252—C25375.0 (7)
N154—C152—C153—C15457.0 (6)N253—C252—C253—C25455.5 (7)
N151—Fe1—N161—C161110.8 (5)N221—Fe2—N261—C26172.2 (5)
N121—Fe1—N161—C16170.3 (5)N231—Fe2—N261—C261158 (7)
N131—Fe1—N161—C161147 (10)N251—Fe2—N261—C261108.6 (5)
N111—Fe1—N161—C161159.6 (5)N211—Fe2—N261—C261162.3 (5)
N141—Fe1—N161—C16119.8 (5)N241—Fe2—N261—C26117.6 (5)
N151—Fe1—N161—N16266.8 (4)N221—Fe2—N261—N262114.4 (4)
N121—Fe1—N161—N162112.2 (4)N231—Fe2—N261—N26228 (7)
N131—Fe1—N161—N16231 (10)N251—Fe2—N261—N26264.9 (4)
N111—Fe1—N161—N16222.8 (4)N211—Fe2—N261—N26224.3 (4)
N141—Fe1—N161—N162157.7 (4)N241—Fe2—N261—N262155.9 (4)
C161—N161—N162—N1630.1 (6)C261—N261—N262—N2631.4 (6)
Fe1—N161—N162—N163178.0 (4)Fe2—N261—N262—N263176.3 (4)
N161—N162—N163—N1641.2 (6)N261—N262—N263—N2640.5 (7)
N162—N163—N164—C1611.8 (6)N262—N263—N264—C2612.3 (7)
N162—N163—N164—C162173.1 (5)N262—N263—N264—C262173.6 (5)
N163—N164—C161—N1611.8 (6)N263—N264—C261—N2613.2 (7)
C162—N164—C161—N161172.3 (5)C262—N264—C261—N261173.7 (5)
N162—N161—C161—N1641.0 (6)N262—N261—C261—N2642.7 (6)
Fe1—N161—C161—N164178.9 (4)Fe2—N261—C261—N264177.1 (4)
C161—N164—C162—C163131.7 (6)C261—N264—C262—C263132.2 (6)
N163—N164—C162—C16358.8 (7)N263—N264—C262—C26358.3 (7)
N164—C162—C163—C16473.4 (6)N264—C262—C263—C26473.6 (6)
(PTZ_LS-dis_C-1) top
Crystal data top
C24H48FeN24·2(BF4)V = 4148.2 (5) Å3
Mr = 902.33Z = 4
Triclinic, C1F(000) = 1872
Hall symbol: -C 1Dx = 1.445 Mg m3
a = 16.1235 (12) ÅMo Kα radiation, λ = 0.71073 Å
b = 16.0450 (11) ŵ = 0.45 mm1
c = 16.3134 (12) ÅT = 84 K
α = 83.583 (6)°Plate, violet
β = 96.870 (6)°0.61 × 0.53 × 0.14 mm
γ = 95.663 (6)°
Data collection top
Oxford Diffraction Diffractometer with Sapphire3 detector12420 independent reflections
Radiation source: fine-focus sealed tube8851 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
Detector resolution: 16.0328 pixels mm-1θmax = 25.1°, θmin = 3.4°
ω – scanh = 1919
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1919
Tmin = 0.771, Tmax = 0.939l = 1919
24788 measured reflections
Refinement top
Refinement on F2Primary atom site location: iterative
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.074Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.224H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.1029P)2 + 11.1251P]
where P = (Fo2 + 2Fc2)/3
12420 reflections(Δ/σ)max < 0.001
534 parametersΔρmax = 0.59 e Å3
0 restraintsΔρmin = 0.79 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.49726 (3)0.24473 (3)0.25004 (3)0.0192 (2)
N6040.2520 (3)0.2983 (3)0.1776 (3)0.0255 (12)
N4010.5066 (3)0.2680 (3)0.1292 (3)0.0228 (11)
N5030.4897 (3)0.0132 (3)0.2562 (3)0.0245 (11)
N1030.4916 (3)0.2491 (3)0.5004 (3)0.0293 (12)
N6010.3742 (3)0.2608 (3)0.2280 (3)0.0206 (11)
N5020.5235 (3)0.0610 (3)0.2724 (3)0.0259 (12)
N6030.2447 (3)0.2555 (3)0.2527 (3)0.0295 (12)
N3040.7428 (3)0.1974 (3)0.3291 (3)0.0252 (12)
N4020.4742 (3)0.2134 (3)0.0708 (3)0.0270 (12)
N5040.4149 (3)0.0003 (3)0.2105 (3)0.0198 (11)
N5010.4715 (3)0.1227 (3)0.2385 (3)0.0191 (10)
N3030.7510 (3)0.2339 (3)0.2517 (3)0.0304 (12)
N1040.4571 (3)0.1699 (3)0.4920 (3)0.0228 (11)
N4040.5281 (3)0.3244 (3)0.0064 (3)0.0219 (11)
N1010.4862 (3)0.2219 (3)0.3704 (3)0.0219 (11)
C4020.5499 (4)0.3830 (4)0.0654 (4)0.0267 (14)
H40A0.56390.44010.04750.032*
H40B0.50060.38520.10770.032*
N2040.5767 (3)0.4918 (3)0.2854 (3)0.0221 (11)
C1010.4527 (4)0.1549 (3)0.4136 (3)0.0189 (12)
H1010.42930.10420.39180.023*
N3010.6210 (3)0.2286 (3)0.2730 (3)0.0213 (11)
N2010.5215 (3)0.3671 (3)0.2607 (3)0.0177 (10)
C6010.3309 (4)0.3019 (4)0.1635 (4)0.0222 (14)
H6010.35340.32920.11530.027*
C5010.4036 (4)0.0802 (4)0.2009 (4)0.0203 (13)
H5010.35570.10460.17220.024*
N2030.5015 (3)0.5018 (3)0.2386 (3)0.0289 (12)
C3020.8140 (4)0.1661 (4)0.3856 (4)0.0297 (15)
H30A0.80440.17130.44360.036*
H30B0.86580.20150.37390.036*
N6020.3183 (3)0.2326 (3)0.2826 (3)0.0246 (11)
N4030.4882 (3)0.2477 (3)0.0024 (3)0.0285 (12)
C2020.6369 (4)0.5668 (4)0.3045 (4)0.0275 (14)
H20A0.68780.54690.33810.033*
H20B0.65400.59650.25190.033*
N3020.6773 (3)0.2539 (3)0.2179 (3)0.0273 (12)
N1020.5104 (3)0.2804 (3)0.4272 (3)0.0293 (12)
C4010.5404 (4)0.3358 (3)0.0859 (4)0.0195 (13)
H4010.56870.38420.10870.023*
C6020.1794 (4)0.3335 (4)0.1255 (4)0.0306 (15)
H60A0.13550.28730.11430.037*
H60B0.19740.35890.07160.037*
C3010.6636 (4)0.1931 (4)0.3414 (4)0.0228 (14)
H3010.64040.16890.39040.027*
C2010.5895 (4)0.4112 (4)0.2968 (4)0.0207 (13)
H2010.63810.38800.32540.025*
C4030.6228 (3)0.3577 (3)0.1036 (3)0.0291 (12)
H40C0.63600.40020.15010.035*
H40D0.60650.30320.12680.035*
C5020.3569 (4)0.0740 (3)0.1831 (4)0.0262 (15)
H50A0.34670.11440.23210.031*
H50B0.30240.05390.15860.031*
N2020.4690 (3)0.4268 (3)0.2257 (3)0.0288 (13)
C4040.7023 (3)0.3491 (3)0.0409 (4)0.0428 (14)
H40E0.74770.33290.06910.064*
H40F0.69010.30600.00450.064*
H40G0.71930.40320.01850.064*
C6030.1427 (3)0.3998 (3)0.1667 (3)0.0308 (11)
H60C0.12110.37340.21870.037*
H60D0.09470.42140.12940.037*
C2030.6005 (3)0.6269 (3)0.3504 (3)0.0259 (13)
H20C0.64670.66510.37460.031*
H20D0.57340.59470.39690.031*
C1020.4278 (4)0.1146 (4)0.5632 (4)0.0281 (15)
H10A0.47050.11890.61180.034*
H10B0.42190.05550.54960.034*
C1030.3437 (3)0.1369 (3)0.5861 (3)0.0319 (13)
H10C0.35130.19400.60470.038*
H10D0.32700.09700.63330.038*
C3030.8262 (3)0.0740 (3)0.3769 (3)0.0361 (12)
H30C0.84270.06950.32110.043*
H30D0.77260.03920.38240.043*
C5030.3920 (3)0.1172 (3)0.1218 (3)0.0310 (14)
H50C0.35110.16380.10430.037*
H50D0.44350.14220.14850.037*
C5040.4132 (3)0.0595 (3)0.0451 (3)0.0433 (13)
H50E0.43560.09200.00660.065*
H50F0.45520.01430.06150.065*
H50G0.36240.03510.01770.065*
C2040.5356 (3)0.6807 (3)0.2977 (3)0.0346 (11)
H20E0.51540.71870.33240.052*
H20F0.48830.64380.27510.052*
H20G0.56190.71380.25200.052*
C6040.2071 (3)0.4740 (3)0.1868 (3)0.0446 (13)
H60E0.18030.51510.21280.067*
H60F0.22800.50100.13550.067*
H60G0.25390.45330.22500.067*
C1040.2727 (3)0.1343 (3)0.5145 (3)0.0386 (13)
H10E0.22110.14920.53330.058*
H10F0.26360.07750.49660.058*
H10G0.28800.17460.46790.058*
C3040.8942 (3)0.0405 (3)0.4437 (3)0.0430 (13)
H30E0.90080.01830.43690.064*
H30F0.87750.04420.49890.064*
H30G0.94750.07440.43760.064*
B1000.8309 (4)0.4122 (4)0.4190 (4)0.0247 (12)
F1010.74644 (19)0.3831 (2)0.4231 (2)0.0503 (10)
F1020.8351 (2)0.4911 (2)0.3718 (2)0.0360 (9)
F1030.8714 (2)0.4199 (2)0.4989 (2)0.0389 (10)
F1040.8722 (2)0.35695 (19)0.3829 (2)0.0431 (9)
B2000.1774 (4)0.0735 (4)0.0681 (4)0.0244 (11)
F2010.1233 (2)0.0821 (3)0.0044 (2)0.0470 (11)
F2020.2562 (2)0.0677 (3)0.0504 (2)0.0790 (14)
F2030.1504 (2)0.0025 (2)0.1184 (2)0.0377 (9)
F2040.1740 (4)0.1413 (2)0.1098 (3)0.113 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0173 (5)0.0206 (5)0.0175 (5)0.0077 (4)0.0015 (4)0.0037 (4)
N6040.018 (2)0.028 (2)0.026 (3)0.0116 (19)0.0021 (19)0.002 (2)
N4010.016 (2)0.020 (2)0.032 (3)0.0033 (18)0.001 (2)0.010 (2)
N5030.021 (2)0.023 (2)0.028 (2)0.0036 (18)0.0016 (18)0.0029 (18)
N1030.038 (3)0.025 (2)0.024 (2)0.0119 (19)0.005 (2)0.0090 (19)
N6010.020 (2)0.022 (2)0.019 (2)0.0110 (19)0.0049 (19)0.0072 (18)
N5020.026 (2)0.022 (2)0.027 (2)0.0074 (19)0.0037 (19)0.0071 (19)
N6030.023 (2)0.033 (2)0.030 (3)0.0058 (19)0.003 (2)0.001 (2)
N3040.018 (2)0.026 (2)0.027 (2)0.0101 (19)0.0018 (19)0.002 (2)
N4020.029 (2)0.023 (2)0.026 (2)0.0104 (19)0.0002 (19)0.004 (2)
N5040.023 (2)0.017 (2)0.017 (2)0.0091 (18)0.0028 (18)0.0040 (17)
N5010.021 (2)0.028 (2)0.009 (2)0.0052 (19)0.0032 (18)0.0023 (18)
N3030.023 (2)0.037 (3)0.029 (3)0.003 (2)0.002 (2)0.003 (2)
N1040.026 (2)0.018 (2)0.024 (2)0.0066 (18)0.0033 (19)0.0058 (19)
N4040.021 (2)0.019 (2)0.022 (2)0.0098 (17)0.0009 (17)0.0017 (18)
N1010.021 (2)0.019 (2)0.025 (2)0.0033 (18)0.001 (2)0.007 (2)
C4020.033 (3)0.022 (2)0.023 (3)0.005 (2)0.002 (2)0.000 (2)
N2040.023 (2)0.017 (2)0.023 (2)0.0112 (18)0.0006 (19)0.0021 (18)
C1010.014 (2)0.022 (2)0.020 (3)0.009 (2)0.002 (2)0.011 (2)
N3010.019 (2)0.024 (2)0.021 (2)0.0080 (19)0.0042 (19)0.0063 (19)
N2010.019 (2)0.026 (2)0.0078 (19)0.0030 (18)0.0002 (17)0.0049 (18)
C6010.019 (3)0.026 (3)0.021 (3)0.002 (2)0.003 (2)0.008 (2)
C5010.018 (3)0.025 (3)0.018 (3)0.004 (2)0.004 (2)0.006 (2)
N2030.027 (2)0.024 (2)0.031 (2)0.0118 (19)0.0060 (19)0.0025 (18)
C3020.021 (3)0.034 (3)0.030 (3)0.013 (2)0.004 (2)0.004 (2)
N6020.018 (2)0.028 (2)0.027 (2)0.0049 (18)0.004 (2)0.0036 (19)
N4030.031 (2)0.026 (2)0.027 (2)0.0102 (18)0.0027 (19)0.0066 (19)
C2020.018 (3)0.024 (3)0.038 (3)0.014 (2)0.000 (2)0.007 (2)
N3020.020 (2)0.033 (2)0.026 (2)0.0057 (19)0.004 (2)0.003 (2)
N1020.037 (3)0.026 (2)0.024 (2)0.009 (2)0.004 (2)0.004 (2)
C4010.014 (2)0.017 (2)0.026 (3)0.004 (2)0.000 (2)0.005 (2)
C6020.017 (2)0.037 (3)0.031 (3)0.012 (2)0.009 (2)0.001 (2)
C3010.021 (3)0.023 (3)0.021 (3)0.004 (2)0.002 (2)0.002 (2)
C2010.017 (3)0.024 (3)0.022 (3)0.005 (2)0.006 (2)0.008 (2)
C4030.031 (3)0.022 (2)0.036 (3)0.002 (2)0.010 (2)0.008 (2)
C5020.025 (3)0.012 (2)0.039 (3)0.010 (2)0.005 (2)0.008 (2)
N2020.028 (2)0.026 (2)0.027 (2)0.0063 (19)0.011 (2)0.0003 (19)
C4040.026 (3)0.044 (3)0.057 (4)0.002 (2)0.003 (3)0.001 (3)
C6030.024 (2)0.029 (2)0.041 (3)0.000 (2)0.002 (2)0.010 (2)
C2030.022 (2)0.025 (2)0.031 (3)0.008 (2)0.003 (2)0.012 (2)
C1020.036 (3)0.026 (3)0.020 (3)0.010 (2)0.003 (2)0.004 (2)
C1030.037 (3)0.027 (2)0.032 (3)0.009 (2)0.008 (2)0.010 (2)
C3030.027 (2)0.030 (2)0.048 (3)0.008 (2)0.003 (2)0.006 (2)
C5030.025 (2)0.023 (2)0.048 (3)0.000 (2)0.000 (2)0.022 (2)
C5040.038 (3)0.047 (3)0.048 (3)0.011 (2)0.008 (2)0.026 (2)
C2040.028 (2)0.034 (2)0.042 (3)0.0065 (19)0.001 (2)0.016 (2)
C6040.046 (3)0.033 (2)0.054 (3)0.006 (2)0.001 (2)0.013 (2)
C1040.025 (2)0.046 (3)0.043 (3)0.006 (2)0.001 (2)0.009 (2)
C3040.031 (2)0.040 (3)0.052 (3)0.006 (2)0.005 (2)0.001 (2)
B1000.020 (3)0.029 (3)0.022 (3)0.003 (3)0.006 (2)0.005 (3)
F1010.0257 (15)0.076 (2)0.0415 (18)0.0155 (15)0.0014 (13)0.0065 (16)
F1020.0483 (19)0.0261 (15)0.0323 (17)0.0064 (14)0.0034 (15)0.0060 (14)
F1030.040 (2)0.045 (2)0.0244 (17)0.0184 (16)0.0085 (15)0.0040 (15)
F1040.0491 (17)0.0332 (16)0.0481 (19)0.0014 (14)0.0050 (14)0.0107 (15)
B2000.025 (3)0.031 (3)0.014 (3)0.002 (3)0.008 (2)0.008 (2)
F2010.0222 (17)0.074 (3)0.036 (2)0.0078 (17)0.0068 (15)0.0121 (18)
F2020.0305 (17)0.125 (3)0.073 (3)0.020 (2)0.0170 (17)0.051 (3)
F2030.0430 (18)0.0328 (16)0.0334 (18)0.0170 (14)0.0024 (14)0.0058 (14)
F2040.256 (7)0.0313 (19)0.048 (2)0.028 (3)0.029 (4)0.0146 (17)
Geometric parameters (Å, º) top
Fe1—N1011.983 (5)C602—C6031.522 (8)
Fe1—N4011.986 (6)C602—H60A0.9900
Fe1—N2011.987 (5)C602—H60B0.9900
Fe1—N5011.987 (5)C301—H3010.9500
Fe1—N6012.010 (5)C201—H2010.9500
Fe1—N3012.022 (5)C403—C4041.548 (6)
N604—C6011.314 (8)C403—H40C0.9900
N604—N6031.347 (7)C403—H40D0.9900
N604—C6021.482 (8)C502—C5031.474 (10)
N401—C4011.335 (7)C502—H50A0.9900
N401—N4021.387 (7)C502—H50B0.9900
N503—N5021.302 (6)C404—H40E0.9800
N503—N5041.361 (7)C404—H40F0.9800
N103—N1021.301 (7)C404—H40G0.9800
N103—N1041.351 (6)C603—C6041.538 (5)
N601—C6011.337 (8)C603—H60C0.9900
N601—N6021.354 (7)C603—H60D0.9900
N502—N5011.385 (7)C203—C2041.541 (7)
N603—N6021.300 (8)C203—H20C0.9900
N304—C3011.311 (8)C203—H20D0.9900
N304—N3031.346 (7)C102—C1031.533 (8)
N304—C3021.476 (8)C102—H10A0.9900
N402—N4031.293 (7)C102—H10B0.9900
N504—C5011.311 (8)C103—C1041.536 (6)
N504—C5021.507 (6)C103—H10C0.9900
N501—C5011.351 (7)C103—H10D0.9900
N303—N3021.303 (8)C303—C3041.542 (6)
N104—C1011.319 (8)C303—H30C0.9900
N104—C1021.476 (7)C303—H30D0.9900
N404—C4011.320 (8)C503—C5041.523 (7)
N404—N4031.346 (6)C503—H50C0.9900
N404—C4021.471 (7)C503—H50D0.9900
N101—C1011.324 (7)C504—H50E0.9800
N101—N1021.387 (7)C504—H50F0.9800
C402—C4031.504 (8)C504—H50G0.9800
C402—H40A0.9900C204—H20E0.9800
C402—H40B0.9900C204—H20F0.9800
N204—C2011.319 (8)C204—H20G0.9800
N204—N2031.368 (7)C604—H60E0.9800
N204—C2021.505 (6)C604—H60F0.9800
C101—H1010.9500C604—H60G0.9800
N301—C3011.340 (8)C104—H10E0.9800
N301—N3021.356 (7)C104—H10F0.9800
N201—C2011.354 (7)C104—H10G0.9800
N201—N2021.372 (7)C304—H30E0.9800
C601—H6010.9500C304—H30F0.9800
C501—H5010.9500C304—H30G0.9800
N203—N2021.294 (6)B100—F1041.380 (7)
C302—C3031.534 (8)B100—F1031.398 (8)
C302—H30A0.9900B100—F1011.402 (7)
C302—H30B0.9900B100—F1021.406 (7)
C202—C2031.487 (9)B200—F2021.351 (7)
C202—H20A0.9900B200—F2041.354 (7)
C202—H20B0.9900B200—F2011.385 (8)
C401—H4010.9500B200—F2031.393 (8)
N101—Fe1—N401179.14 (11)N204—C201—N201108.4 (5)
N101—Fe1—N20190.90 (19)N204—C201—H201125.8
N401—Fe1—N20188.98 (19)N201—C201—H201125.8
N101—Fe1—N50189.4 (2)C402—C403—C404112.9 (5)
N401—Fe1—N50190.8 (2)C402—C403—H40C109.0
N201—Fe1—N501179.21 (11)C404—C403—H40C109.0
N101—Fe1—N60189.8 (2)C402—C403—H40D109.0
N401—Fe1—N60189.4 (2)C404—C403—H40D109.0
N201—Fe1—N60189.62 (19)H40C—C403—H40D107.8
N501—Fe1—N60189.64 (19)C503—C502—N504111.8 (5)
N101—Fe1—N30189.9 (2)C503—C502—H50A109.3
N401—Fe1—N30191.0 (2)N504—C502—H50A109.3
N201—Fe1—N30190.31 (19)C503—C502—H50B109.3
N501—Fe1—N30190.4 (2)N504—C502—H50B109.3
N601—Fe1—N301179.65 (11)H50A—C502—H50B107.9
C601—N604—N603108.1 (5)N203—N202—N201111.3 (4)
C601—N604—C602129.8 (5)C403—C404—H40E109.5
N603—N604—C602122.1 (5)C403—C404—H40F109.5
C401—N401—N402105.4 (5)H40E—C404—H40F109.5
C401—N401—Fe1130.3 (4)C403—C404—H40G109.5
N402—N401—Fe1124.2 (4)H40E—C404—H40G109.5
N502—N503—N504105.8 (4)H40F—C404—H40G109.5
N102—N103—N104106.2 (5)C602—C603—C604112.6 (4)
C601—N601—N602105.9 (5)C602—C603—H60C109.1
C601—N601—Fe1130.5 (4)C604—C603—H60C109.1
N602—N601—Fe1123.5 (4)C602—C603—H60D109.1
N503—N502—N501110.7 (4)C604—C603—H60D109.1
N602—N603—N604107.6 (5)H60C—C603—H60D107.8
C301—N304—N303108.6 (5)C202—C203—C204114.9 (4)
C301—N304—C302128.5 (5)C202—C203—H20C108.5
N303—N304—C302122.8 (5)C204—C203—H20C108.5
N403—N402—N401109.4 (4)C202—C203—H20D108.5
C501—N504—N503110.0 (4)C204—C203—H20D108.5
C501—N504—C502129.6 (5)H20C—C203—H20D107.5
N503—N504—C502120.3 (5)N104—C102—C103112.7 (5)
C501—N501—N502104.7 (5)N104—C102—H10A109.1
C501—N501—Fe1131.0 (4)C103—C102—H10A109.1
N502—N501—Fe1124.3 (3)N104—C102—H10B109.1
N302—N303—N304107.9 (5)C103—C102—H10B109.1
C101—N104—N103109.6 (5)H10A—C102—H10B107.8
C101—N104—C102128.9 (5)C102—C103—C104113.8 (4)
N103—N104—C102121.5 (5)C102—C103—H10C108.8
C401—N404—N403109.1 (5)C104—C103—H10C108.8
C401—N404—C402128.8 (5)C102—C103—H10D108.8
N403—N404—C402122.1 (5)C104—C103—H10D108.8
C101—N101—N102105.3 (5)H10C—C103—H10D107.7
C101—N101—Fe1130.7 (4)C302—C303—C304111.0 (4)
N102—N101—Fe1123.9 (4)C302—C303—H30C109.4
N404—C402—C403112.4 (5)C304—C303—H30C109.4
N404—C402—H40A109.1C302—C303—H30D109.4
C403—C402—H40A109.1C304—C303—H30D109.4
N404—C402—H40B109.1H30C—C303—H30D108.0
C403—C402—H40B109.1C502—C503—C504113.5 (4)
H40A—C402—H40B107.8C502—C503—H50C108.9
C201—N204—N203109.4 (4)C504—C503—H50C108.9
C201—N204—C202128.9 (5)C502—C503—H50D108.9
N203—N204—C202120.9 (5)C504—C503—H50D108.9
N104—C101—N101108.9 (5)H50C—C503—H50D107.7
N104—C101—H101125.5C503—C504—H50E109.5
N101—C101—H101125.5C503—C504—H50F109.5
C301—N301—N302106.8 (5)H50E—C504—H50F109.5
C301—N301—Fe1129.2 (4)C503—C504—H50G109.5
N302—N301—Fe1124.0 (4)H50E—C504—H50G109.5
C201—N201—N202104.9 (4)H50F—C504—H50G109.5
C201—N201—Fe1131.2 (4)C203—C204—H20E109.5
N202—N201—Fe1123.7 (3)C203—C204—H20F109.5
N604—C601—N601108.9 (5)H20E—C204—H20F109.5
N604—C601—H601125.5C203—C204—H20G109.5
N601—C601—H601125.5H20E—C204—H20G109.5
N504—C501—N501108.7 (5)H20F—C204—H20G109.5
N504—C501—H501125.6C603—C604—H60E109.5
N501—C501—H501125.6C603—C604—H60F109.5
N202—N203—N204105.9 (5)H60E—C604—H60F109.5
N304—C302—C303112.6 (4)C603—C604—H60G109.5
N304—C302—H30A109.1H60E—C604—H60G109.5
C303—C302—H30A109.1H60F—C604—H60G109.5
N304—C302—H30B109.1C103—C104—H10E109.5
C303—C302—H30B109.1C103—C104—H10F109.5
H30A—C302—H30B107.8H10E—C104—H10F109.5
N603—N602—N601109.4 (5)C103—C104—H10G109.5
N402—N403—N404107.5 (5)H10E—C104—H10G109.5
C203—C202—N204112.9 (5)H10F—C104—H10G109.5
C203—C202—H20A109.0C303—C304—H30E109.5
N204—C202—H20A109.0C303—C304—H30F109.5
C203—C202—H20B109.0H30E—C304—H30F109.5
N204—C202—H20B109.0C303—C304—H30G109.5
H20A—C202—H20B107.8H30E—C304—H30G109.5
N303—N302—N301108.5 (5)H30F—C304—H30G109.5
N103—N102—N101109.9 (4)F104—B100—F103107.8 (5)
N404—C401—N401108.7 (4)F104—B100—F101111.1 (5)
N404—C401—H401125.7F103—B100—F101110.2 (5)
N401—C401—H401125.7F104—B100—F102109.3 (5)
N604—C602—C603112.3 (5)F103—B100—F102109.7 (5)
N604—C602—H60A109.2F101—B100—F102108.9 (5)
C603—C602—H60A109.2F202—B200—F204110.9 (6)
N604—C602—H60B109.2F202—B200—F201110.2 (5)
C603—C602—H60B109.2F204—B200—F201108.1 (6)
H60A—C602—H60B107.9F202—B200—F203110.4 (5)
N304—C301—N301108.2 (5)F204—B200—F203107.4 (5)
N304—C301—H301125.9F201—B200—F203109.8 (5)
N301—C301—H301125.9
N101—Fe1—N401—C40198 (8)N201—Fe1—N301—N30273.2 (5)
N201—Fe1—N401—C40116.7 (5)N501—Fe1—N301—N302106.5 (5)
N501—Fe1—N401—C401164.0 (5)N601—Fe1—N301—N302151 (45)
N601—Fe1—N401—C401106.3 (5)N101—Fe1—N201—C20170.7 (5)
N301—Fe1—N401—C40173.6 (5)N401—Fe1—N201—C201110.1 (5)
N101—Fe1—N401—N40279 (8)N501—Fe1—N201—C201180 (100)
N201—Fe1—N401—N402161.0 (5)N601—Fe1—N201—C201160.5 (6)
N501—Fe1—N401—N40218.3 (5)N301—Fe1—N201—C20119.2 (6)
N601—Fe1—N401—N40271.4 (5)N101—Fe1—N201—N202113.1 (5)
N301—Fe1—N401—N402108.7 (5)N401—Fe1—N201—N20266.0 (5)
N101—Fe1—N601—C601158.1 (6)N501—Fe1—N201—N2024 (9)
N401—Fe1—N601—C60121.7 (6)N601—Fe1—N201—N20223.4 (4)
N201—Fe1—N601—C60167.2 (5)N301—Fe1—N201—N202157.0 (4)
N501—Fe1—N601—C601112.5 (5)N603—N604—C601—N6011.0 (7)
N301—Fe1—N601—C601145 (19)C602—N604—C601—N601179.8 (5)
N101—Fe1—N601—N60218.4 (4)N602—N601—C601—N6040.6 (6)
N401—Fe1—N601—N602161.8 (4)Fe1—N601—C601—N604177.5 (4)
N201—Fe1—N601—N602109.3 (5)N503—N504—C501—N5011.2 (7)
N501—Fe1—N601—N60271.0 (5)C502—N504—C501—N501177.6 (5)
N301—Fe1—N601—N60231 (19)N502—N501—C501—N5040.8 (7)
N504—N503—N502—N5010.6 (6)Fe1—N501—C501—N504179.3 (4)
C601—N604—N603—N6021.0 (7)C201—N204—N203—N2022.6 (7)
C602—N604—N603—N602179.7 (5)C202—N204—N203—N202173.2 (5)
C401—N401—N402—N4030.2 (7)C301—N304—C302—C30387.6 (8)
Fe1—N401—N402—N403178.0 (4)N303—N304—C302—C30389.7 (6)
N502—N503—N504—C5011.1 (7)N604—N603—N602—N6010.6 (6)
N502—N503—N504—C502177.9 (5)C601—N601—N602—N6030.1 (6)
N503—N502—N501—C5010.1 (7)Fe1—N601—N602—N603177.2 (4)
N503—N502—N501—Fe1178.7 (4)N401—N402—N403—N4040.9 (7)
N101—Fe1—N501—C501110.6 (5)C401—N404—N403—N4021.7 (7)
N401—Fe1—N501—C50168.5 (5)C402—N404—N403—N402176.7 (5)
N201—Fe1—N501—C5011 (9)C201—N204—C202—C203131.9 (7)
N601—Fe1—N501—C50120.9 (6)N203—N204—C202—C20359.6 (7)
N301—Fe1—N501—C501159.5 (6)N304—N303—N302—N3011.3 (6)
N101—Fe1—N501—N50267.6 (5)C301—N301—N302—N3030.3 (6)
N401—Fe1—N501—N502113.3 (5)Fe1—N301—N302—N303179.8 (4)
N201—Fe1—N501—N502177 (100)N104—N103—N102—N1011.4 (7)
N601—Fe1—N501—N502157.3 (4)C101—N101—N102—N1030.3 (7)
N301—Fe1—N501—N50222.3 (4)Fe1—N101—N102—N103176.7 (4)
C301—N304—N303—N3021.8 (7)N403—N404—C401—N4011.8 (7)
C302—N304—N303—N302179.5 (5)C402—N404—C401—N401176.4 (5)
N102—N103—N104—C1012.1 (7)N402—N401—C401—N4041.2 (7)
N102—N103—N104—C102180.0 (5)Fe1—N401—C401—N404176.8 (4)
N401—Fe1—N101—C10182 (8)C601—N604—C602—C603116.5 (7)
N201—Fe1—N101—C101164.0 (6)N603—N604—C602—C60362.7 (6)
N501—Fe1—N101—C10115.3 (6)N303—N304—C301—N3011.6 (7)
N601—Fe1—N101—C10174.4 (5)C302—N304—C301—N301179.2 (6)
N301—Fe1—N101—C101105.7 (5)N302—N301—C301—N3040.8 (7)
N401—Fe1—N101—N10294 (8)Fe1—N301—C301—N304179.1 (4)
N201—Fe1—N101—N10212.2 (5)N203—N204—C201—N2012.5 (7)
N501—Fe1—N101—N102168.5 (5)C202—N204—C201—N201172.1 (5)
N601—Fe1—N101—N102101.8 (5)N202—N201—C201—N2041.4 (7)
N301—Fe1—N101—N10278.1 (5)Fe1—N201—C201—N204178.1 (4)
C401—N404—C402—C403107.5 (7)N404—C402—C403—C40456.6 (5)
N403—N404—C402—C40374.5 (7)C501—N504—C502—C503116.2 (7)
N103—N104—C101—N1011.9 (7)N503—N504—C502—C50367.7 (7)
C102—N104—C101—N101179.7 (5)N204—N203—N202—N2011.7 (7)
N102—N101—C101—N1041.0 (7)C201—N201—N202—N2030.2 (7)
Fe1—N101—C101—N104177.7 (4)Fe1—N201—N202—N203176.8 (4)
N101—Fe1—N301—C30115.8 (6)N604—C602—C603—C60458.5 (6)
N401—Fe1—N301—C301164.4 (6)N204—C202—C203—C20474.1 (6)
N201—Fe1—N301—C301106.7 (5)C101—N104—C102—C103100.8 (7)
N501—Fe1—N301—C30173.6 (5)N103—N104—C102—C10376.7 (6)
N601—Fe1—N301—C30129 (19)N104—C102—C103—C10457.4 (6)
N101—Fe1—N301—N302164.1 (5)N304—C302—C303—C304173.4 (4)
N401—Fe1—N301—N30215.8 (5)N504—C502—C503—C50456.8 (6)
(PTZ_LS-ord_C-1) top
Crystal data top
C24H48FeN24·2(BF4)V = 4246.89 (9) Å3
Mr = 902.33Z = 4
Triclinic, C1F(000) = 1872
Hall symbol: -C 1Dx = 1.411 Mg m3
a = 16.3473 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 16.3475 (2) ŵ = 0.44 mm1
c = 16.3475 (2) ÅT = 84 K
α = 81.815 (1)°Plate, violet
β = 98.175 (1)°0.61 × 0.53 × 0.14 mm
γ = 98.180 (1)°
Data collection top
Oxford Diffraction Diffractometer with Sapphire3 detector6402 independent reflections
Radiation source: fine-focus sealed tube3391 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.009
Detector resolution: 16.0328 pixels mm-1θmax = 25.1°, θmin = 3.4°
ω – scanh = 1919
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1919
Tmin = 0.774, Tmax = 0.941l = 1919
13053 measured reflections
Refinement top
Refinement on F2Primary atom site location: iterative
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.118H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0608P)2 + 1.9945P]
where P = (Fo2 + 2Fc2)/3
6402 reflections(Δ/σ)max = 0.018
538 parametersΔρmax = 0.39 e Å3
0 restraintsΔρmin = 0.35 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.499971 (19)0.249981 (19)0.249878 (19)0.00824 (12)
N6040.25743 (10)0.28838 (10)0.16747 (10)0.0122 (4)
N4010.51118 (10)0.27550 (10)0.12918 (10)0.0102 (4)
N5030.49279 (11)0.00208 (11)0.25460 (11)0.0167 (4)
N1030.50471 (11)0.24270 (11)0.50205 (11)0.0172 (4)
N6010.37889 (10)0.26130 (10)0.22447 (10)0.0107 (4)
N5020.52735 (11)0.07181 (11)0.27059 (11)0.0161 (4)
N6030.24792 (11)0.24494 (11)0.24300 (11)0.0170 (4)
N3040.74252 (10)0.21155 (10)0.33265 (10)0.0113 (4)
N4020.47920 (11)0.22279 (11)0.07161 (10)0.0150 (4)
N5040.41749 (11)0.00721 (10)0.21123 (10)0.0123 (4)
N5010.47409 (10)0.12905 (10)0.23862 (10)0.0130 (4)
N3030.75167 (11)0.25456 (11)0.25734 (11)0.0155 (4)
N1040.46150 (10)0.16739 (10)0.49244 (10)0.0124 (4)
N4040.53832 (10)0.33263 (10)0.00756 (10)0.0115 (4)
N1010.48867 (10)0.22423 (10)0.37112 (10)0.0114 (4)
C4020.56130 (14)0.39187 (13)0.06530 (13)0.0163 (5)
H40A0.59070.44420.04600.020*
H40B0.51000.40530.10180.020*
N2040.58249 (10)0.49221 (10)0.28806 (10)0.0116 (4)
C1010.45204 (12)0.15684 (12)0.41268 (12)0.0106 (5)
H1010.42380.10900.38930.013*
N3010.62082 (10)0.23894 (10)0.27572 (10)0.0110 (4)
N2010.52555 (10)0.37080 (10)0.26121 (10)0.0090 (4)
C6010.33734 (12)0.29774 (12)0.15666 (13)0.0122 (5)
H6010.36070.32570.10870.015*
C5010.40700 (13)0.08721 (12)0.20170 (12)0.0110 (5)
H5010.35930.11050.17310.013*
N2030.50721 (11)0.50171 (10)0.24510 (11)0.0158 (4)
C3020.81493 (13)0.18857 (14)0.39127 (13)0.0170 (5)
H30A0.79550.15920.44360.020*
H30B0.85130.23990.40480.020*
N6020.32143 (11)0.22928 (11)0.27738 (11)0.0162 (4)
N4030.49534 (11)0.25699 (11)0.00184 (11)0.0160 (4)
C2020.64194 (13)0.56483 (12)0.31146 (13)0.0146 (5)
H20A0.65590.60130.26030.018*
H20B0.69400.54520.34130.018*
N3020.67871 (11)0.27074 (11)0.22289 (11)0.0144 (4)
N1020.52059 (11)0.27734 (11)0.42885 (11)0.0162 (4)
C4010.54775 (12)0.34292 (13)0.08671 (12)0.0115 (5)
H4010.57610.39080.10990.014*
C6020.18479 (13)0.31131 (13)0.10807 (13)0.0155 (5)
H60A0.14840.26000.09430.019*
H60B0.20430.34100.05590.019*
C3010.66313 (13)0.20217 (12)0.34287 (12)0.0111 (5)
H3010.63990.17360.39070.013*
C2010.59316 (13)0.41310 (13)0.29738 (12)0.0114 (5)
H2010.64130.39000.32530.014*
C4030.61659 (14)0.35657 (15)0.11472 (14)0.0203 (5)
H40C0.63020.39820.16260.024*
H40D0.58530.30650.13730.024*
C5020.35874 (14)0.06549 (13)0.18857 (14)0.0183 (6)
H50A0.30630.04620.15920.022*
H50B0.34540.10180.24000.022*
N2020.47304 (11)0.42888 (11)0.22909 (11)0.0150 (4)
C4040.69719 (15)0.33303 (15)0.06440 (16)0.0259 (6)
H40E0.72690.38120.03860.039*
H40F0.73210.31580.10120.039*
H40G0.68460.28700.02090.039*
C6030.13522 (13)0.36603 (14)0.14338 (14)0.0185 (5)
H60C0.11300.33460.19360.022*
H60D0.08720.37940.10190.022*
C2030.60657 (14)0.61431 (13)0.36621 (14)0.0198 (6)
H20C0.55660.63680.33460.024*
H20D0.64820.66220.37980.024*
C1020.43845 (13)0.10838 (13)0.56506 (13)0.0165 (5)
H10A0.48970.09460.60140.020*
H10B0.40870.05620.54560.020*
C1030.38384 (14)0.14327 (14)0.61487 (13)0.0189 (5)
H10C0.41520.19330.63740.023*
H10D0.37040.10150.66270.023*
C3030.81430 (16)0.05306 (14)0.33317 (15)0.0265 (6)
H30C0.78840.02340.38130.040*
H30D0.85090.01790.31580.040*
H30E0.77080.06600.28720.040*
C5030.39345 (14)0.11545 (13)0.13338 (14)0.0184 (5)
H50C0.35160.16320.11990.022*
H50D0.44360.13800.16440.022*
C5040.41632 (16)0.06440 (16)0.05272 (14)0.0259 (6)
H50E0.36770.03930.02320.039*
H50F0.43420.10070.01760.039*
H50G0.46180.02030.06540.039*
C2040.58269 (16)0.56419 (16)0.44690 (15)0.0266 (6)
H20E0.53730.52000.43420.040*
H20F0.56430.60100.48120.040*
H20G0.63100.53930.47730.040*
C6040.18564 (16)0.44732 (15)0.16672 (15)0.0257 (6)
H60E0.23020.43490.21170.039*
H60F0.14900.48160.18540.039*
H60G0.21000.47770.11800.039*
C1040.30286 (15)0.16684 (15)0.56459 (16)0.0262 (6)
H10E0.31530.21390.52210.039*
H10F0.26740.18260.60180.039*
H10G0.27390.11920.53760.039*
C3040.86499 (13)0.13334 (14)0.35678 (14)0.0194 (5)
H30F0.91240.11960.39890.023*
H30G0.88810.16450.30690.023*
B1000.81750 (15)0.43254 (15)0.43192 (16)0.0134 (6)
F1010.76319 (8)0.37093 (8)0.39618 (9)0.0317 (4)
F1020.85355 (9)0.48691 (8)0.37057 (8)0.0310 (4)
F1030.87951 (8)0.39611 (9)0.48681 (8)0.0309 (4)
F1040.77452 (9)0.47529 (9)0.47526 (9)0.0335 (4)
B2000.18214 (15)0.06807 (17)0.06730 (16)0.0162 (6)
F2010.12068 (8)0.10344 (9)0.01317 (8)0.0312 (4)
F2020.22545 (9)0.02441 (9)0.02451 (9)0.0348 (4)
F2030.14613 (9)0.01320 (8)0.12937 (8)0.0314 (4)
F2040.23697 (8)0.12964 (8)0.10321 (9)0.0301 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.00921 (16)0.00714 (16)0.00746 (16)0.00030 (11)0.00058 (11)0.00091 (11)
N6040.0146 (9)0.0097 (8)0.0116 (9)0.0018 (7)0.0006 (8)0.0015 (7)
N4010.0109 (8)0.0105 (8)0.0094 (8)0.0026 (7)0.0005 (7)0.0014 (7)
N5030.0188 (10)0.0131 (9)0.0173 (9)0.0025 (8)0.0000 (8)0.0004 (8)
N1030.0193 (9)0.0180 (10)0.0131 (9)0.0018 (8)0.0023 (8)0.0015 (8)
N6010.0115 (8)0.0107 (8)0.0096 (8)0.0015 (7)0.0028 (7)0.0013 (7)
N5020.0166 (9)0.0109 (9)0.0183 (10)0.0011 (8)0.0022 (8)0.0011 (8)
N6030.0146 (9)0.0186 (10)0.0166 (10)0.0018 (8)0.0027 (8)0.0025 (8)
N3040.0095 (9)0.0125 (9)0.0119 (9)0.0012 (7)0.0018 (7)0.0013 (8)
N4020.0178 (9)0.0151 (9)0.0109 (9)0.0010 (8)0.0006 (8)0.0025 (8)
N5040.0148 (9)0.0104 (9)0.0121 (9)0.0010 (8)0.0041 (8)0.0003 (7)
N5010.0116 (9)0.0135 (9)0.0128 (9)0.0011 (8)0.0013 (7)0.0011 (8)
N3030.0132 (9)0.0180 (9)0.0150 (9)0.0020 (8)0.0043 (8)0.0012 (8)
N1040.0143 (9)0.0112 (9)0.0108 (9)0.0017 (8)0.0014 (7)0.0017 (7)
N4040.0127 (9)0.0124 (9)0.0090 (9)0.0018 (7)0.0018 (7)0.0011 (7)
N1010.0100 (8)0.0108 (9)0.0134 (9)0.0013 (7)0.0006 (7)0.0016 (7)
C4020.0229 (12)0.0157 (11)0.0091 (10)0.0019 (10)0.0042 (9)0.0041 (9)
N2040.0126 (9)0.0100 (9)0.0107 (9)0.0012 (7)0.0002 (7)0.0003 (7)
C1010.0126 (10)0.0088 (10)0.0107 (10)0.0033 (9)0.0010 (9)0.0003 (9)
N3010.0135 (9)0.0063 (8)0.0124 (9)0.0008 (7)0.0012 (7)0.0002 (7)
N2010.0122 (8)0.0096 (8)0.0054 (8)0.0034 (7)0.0027 (7)0.0020 (7)
C6010.0113 (10)0.0108 (10)0.0137 (10)0.0004 (9)0.0003 (9)0.0016 (9)
C5010.0117 (10)0.0098 (10)0.0118 (10)0.0027 (9)0.0017 (9)0.0001 (9)
N2030.0166 (9)0.0105 (9)0.0201 (10)0.0032 (8)0.0001 (8)0.0017 (8)
C3020.0140 (11)0.0218 (12)0.0141 (11)0.0042 (10)0.0046 (9)0.0030 (10)
N6020.0144 (9)0.0181 (10)0.0141 (9)0.0004 (8)0.0050 (8)0.0051 (8)
N4030.0221 (10)0.0136 (9)0.0119 (9)0.0005 (8)0.0023 (8)0.0024 (8)
C2020.0157 (11)0.0081 (10)0.0204 (12)0.0018 (9)0.0054 (10)0.0028 (10)
N3020.0126 (9)0.0153 (9)0.0150 (9)0.0019 (8)0.0026 (8)0.0003 (8)
N1020.0185 (10)0.0162 (9)0.0124 (9)0.0022 (8)0.0019 (8)0.0014 (8)
C4010.0120 (10)0.0115 (10)0.0121 (11)0.0025 (9)0.0042 (9)0.0012 (9)
C6020.0112 (10)0.0173 (11)0.0171 (11)0.0030 (9)0.0025 (9)0.0017 (10)
C3010.0157 (11)0.0100 (10)0.0072 (10)0.0011 (9)0.0009 (8)0.0004 (9)
C2010.0126 (10)0.0137 (10)0.0081 (10)0.0006 (9)0.0040 (9)0.0005 (9)
C4030.0279 (13)0.0223 (12)0.0123 (11)0.0030 (11)0.0092 (10)0.0014 (10)
C5020.0188 (11)0.0126 (11)0.0206 (12)0.0061 (10)0.0016 (10)0.0010 (10)
N2020.0165 (9)0.0116 (9)0.0164 (9)0.0049 (8)0.0003 (8)0.0011 (8)
C4040.0219 (12)0.0276 (13)0.0319 (14)0.0083 (11)0.0117 (11)0.0021 (11)
C6030.0143 (11)0.0258 (12)0.0174 (11)0.0104 (10)0.0017 (10)0.0022 (10)
C2030.0199 (12)0.0131 (11)0.0271 (13)0.0003 (10)0.0034 (11)0.0062 (11)
C1020.0209 (11)0.0155 (11)0.0118 (11)0.0054 (10)0.0028 (9)0.0064 (10)
C1030.0279 (13)0.0160 (11)0.0136 (11)0.0035 (10)0.0087 (10)0.0025 (10)
C3030.0378 (15)0.0192 (12)0.0258 (13)0.0105 (11)0.0024 (12)0.0088 (11)
C5030.0196 (11)0.0131 (11)0.0251 (13)0.0032 (10)0.0046 (10)0.0084 (11)
C5040.0278 (13)0.0326 (14)0.0209 (12)0.0016 (11)0.0104 (11)0.0109 (11)
C2040.0278 (13)0.0318 (14)0.0229 (13)0.0035 (11)0.0065 (11)0.0098 (11)
C6040.0304 (13)0.0233 (13)0.0264 (13)0.0114 (11)0.0031 (11)0.0055 (11)
C1040.0261 (13)0.0233 (13)0.0332 (14)0.0084 (11)0.0130 (12)0.0019 (11)
C3040.0148 (11)0.0242 (12)0.0201 (12)0.0061 (10)0.0014 (10)0.0026 (10)
B1000.0173 (12)0.0081 (11)0.0140 (12)0.0019 (11)0.0015 (11)0.0016 (11)
F1010.0254 (7)0.0203 (7)0.0469 (9)0.0018 (6)0.0074 (7)0.0125 (7)
F1020.0458 (9)0.0239 (7)0.0204 (7)0.0080 (7)0.0121 (7)0.0026 (6)
F1030.0239 (7)0.0443 (9)0.0225 (7)0.0134 (7)0.0006 (6)0.0093 (7)
F1040.0362 (8)0.0354 (9)0.0349 (8)0.0120 (8)0.0115 (7)0.0101 (7)
B2000.0140 (12)0.0202 (13)0.0126 (12)0.0008 (11)0.0002 (11)0.0001 (11)
F2010.0206 (7)0.0466 (9)0.0238 (7)0.0125 (7)0.0023 (6)0.0076 (7)
F2020.0374 (9)0.0365 (9)0.0358 (9)0.0108 (8)0.0114 (8)0.0097 (8)
F2030.0487 (9)0.0221 (7)0.0206 (7)0.0074 (7)0.0132 (7)0.0039 (6)
F2040.0229 (7)0.0208 (7)0.0455 (9)0.0002 (6)0.0051 (7)0.0118 (7)
Geometric parameters (Å, º) top
Fe1—N4011.9868 (16)C602—C6031.509 (3)
Fe1—N2011.9892 (16)C602—H60A0.9900
Fe1—N3011.9891 (17)C602—H60B0.9900
Fe1—N5011.9912 (17)C301—H3010.9500
Fe1—N6011.9933 (17)C201—H2010.9500
Fe1—N1011.9960 (17)C403—C4041.519 (3)
N604—C6011.328 (3)C403—H40C0.9900
N604—N6031.351 (2)C403—H40D0.9900
N604—C6021.479 (2)C502—C5031.513 (3)
N401—C4011.329 (3)C502—H50A0.9900
N401—N4021.365 (2)C502—H50B0.9900
N503—N5021.304 (2)C404—H40E0.9800
N503—N5041.347 (2)C404—H40F0.9800
N103—N1021.294 (2)C404—H40G0.9800
N103—N1041.347 (2)C603—C6041.528 (3)
N601—C6011.326 (3)C603—H60C0.9900
N601—N6021.366 (2)C603—H60D0.9900
N502—N5011.368 (2)C203—C2041.520 (3)
N603—N6021.296 (2)C203—H20C0.9900
N304—C3011.317 (3)C203—H20D0.9900
N304—N3031.345 (2)C102—C1031.506 (3)
N304—C3021.470 (2)C102—H10A0.9900
N402—N4031.297 (2)C102—H10B0.9900
N504—C5011.327 (3)C103—C1041.524 (3)
N504—C5021.474 (3)C103—H10C0.9900
N501—C5011.323 (3)C103—H10D0.9900
N303—N3021.291 (2)C303—C3041.517 (3)
N104—C1011.324 (3)C303—H30C0.9800
N104—C1021.476 (2)C303—H30D0.9800
N404—C4011.313 (3)C303—H30E0.9800
N404—N4031.350 (2)C503—C5041.521 (3)
N404—C4021.481 (2)C503—H50C0.9900
N101—C1011.322 (2)C503—H50D0.9900
N101—N1021.372 (2)C504—H50E0.9800
C402—C4031.514 (3)C504—H50F0.9800
C402—H40A0.9900C504—H50G0.9800
C402—H40B0.9900C204—H20E0.9800
N204—C2011.314 (3)C204—H20F0.9800
N204—N2031.345 (2)C204—H20G0.9800
N204—C2021.482 (2)C604—H60E0.9800
C101—H1010.9500C604—H60F0.9800
N301—C3011.326 (2)C604—H60G0.9800
N301—N3021.370 (2)C104—H10E0.9800
N201—C2011.328 (3)C104—H10F0.9800
N201—N2021.370 (2)C104—H10G0.9800
C601—H6010.9500C304—H30F0.9900
C501—H5010.9500C304—H30G0.9900
N203—N2021.287 (2)B100—F1041.381 (3)
C302—C3041.513 (3)B100—F1011.382 (3)
C302—H30A0.9900B100—F1021.381 (3)
C302—H30B0.9900B100—F1031.396 (3)
C202—C2031.509 (3)B200—F2011.376 (3)
C202—H20A0.9900B200—F2021.388 (3)
C202—H20B0.9900B200—F2041.387 (3)
C401—H4010.9500B200—F2031.393 (3)
N401—Fe1—N20189.60 (7)N204—C201—N201108.64 (18)
N401—Fe1—N30190.59 (7)N204—C201—H201125.7
N201—Fe1—N30189.42 (7)N201—C201—H201125.7
N401—Fe1—N50190.47 (7)C402—C403—C404113.82 (19)
N201—Fe1—N501179.85 (8)C402—C403—H40C108.8
N301—Fe1—N50190.71 (7)C404—C403—H40C108.8
N401—Fe1—N60189.63 (7)C402—C403—H40D108.8
N201—Fe1—N60190.42 (7)C404—C403—H40D108.8
N301—Fe1—N601179.73 (8)H40C—C403—H40D107.7
N501—Fe1—N60189.45 (7)N504—C502—C503112.32 (18)
N401—Fe1—N101179.94 (10)N504—C502—H50A109.1
N201—Fe1—N10190.45 (7)C503—C502—H50A109.1
N301—Fe1—N10189.42 (7)N504—C502—H50B109.1
N501—Fe1—N10189.48 (7)C503—C502—H50B109.1
N601—Fe1—N10190.36 (7)H50A—C502—H50B107.9
C601—N604—N603108.96 (16)N203—N202—N201110.02 (16)
C601—N604—C602129.38 (17)C403—C404—H40E109.5
N603—N604—C602121.39 (16)C403—C404—H40F109.5
C401—N401—N402105.59 (16)H40E—C404—H40F109.5
C401—N401—Fe1130.35 (14)C403—C404—H40G109.5
N402—N401—Fe1124.05 (13)H40E—C404—H40G109.5
N502—N503—N504106.93 (16)H40F—C404—H40G109.5
N102—N103—N104106.92 (16)C602—C603—C604113.61 (19)
C601—N601—N602106.42 (16)C602—C603—H60C108.8
C601—N601—Fe1129.59 (14)C604—C603—H60C108.8
N602—N601—Fe1123.98 (13)C602—C603—H60D108.8
N503—N502—N501109.51 (16)C604—C603—H60D108.8
N602—N603—N604106.74 (16)H60C—C603—H60D107.7
C301—N304—N303108.50 (16)C202—C203—C204113.83 (19)
C301—N304—C302129.95 (17)C202—C203—H20C108.8
N303—N304—C302121.34 (16)C204—C203—H20C108.8
N403—N402—N401109.91 (16)C202—C203—H20D108.8
C501—N504—N503108.68 (17)C204—C203—H20D108.8
C501—N504—C502129.91 (18)H20C—C203—H20D107.7
N503—N504—C502121.16 (17)N104—C102—C103112.19 (17)
C501—N501—N502106.23 (16)N104—C102—H10A109.2
C501—N501—Fe1130.20 (14)C103—C102—H10A109.2
N502—N501—Fe1123.57 (13)N104—C102—H10B109.2
N302—N303—N304107.26 (16)C103—C102—H10B109.2
C101—N104—N103108.97 (16)H10A—C102—H10B107.9
C101—N104—C102129.66 (18)C102—C103—C104113.50 (19)
N103—N104—C102121.14 (17)C102—C103—H10C108.9
C401—N404—N403108.76 (16)C104—C103—H10C108.9
C401—N404—C402129.77 (18)C102—C103—H10D108.9
N403—N404—C402121.27 (16)C104—C103—H10D108.9
C101—N101—N102106.20 (16)H10C—C103—H10D107.7
C101—N101—Fe1129.85 (14)C304—C303—H30C109.5
N102—N101—Fe1123.95 (13)C304—C303—H30D109.5
N404—C402—C403111.79 (17)H30C—C303—H30D109.5
N404—C402—H40A109.3C304—C303—H30E109.5
C403—C402—H40A109.3H30C—C303—H30E109.5
N404—C402—H40B109.3H30D—C303—H30E109.5
C403—C402—H40B109.3C502—C503—C504112.93 (19)
H40A—C402—H40B107.9C502—C503—H50C109.0
C201—N204—N203109.03 (16)C504—C503—H50C109.0
C201—N204—C202129.30 (18)C502—C503—H50D109.0
N203—N204—C202121.46 (16)C504—C503—H50D109.0
N101—C101—N104108.33 (18)H50C—C503—H50D107.8
N101—C101—H101125.8C503—C504—H50E109.5
N104—C101—H101125.8C503—C504—H50F109.5
C301—N301—N302105.45 (16)H50E—C504—H50F109.5
C301—N301—Fe1130.44 (14)C503—C504—H50G109.5
N302—N301—Fe1124.12 (12)H50E—C504—H50G109.5
C201—N201—N202105.46 (16)H50F—C504—H50G109.5
C201—N201—Fe1130.24 (14)C203—C204—H20E109.5
N202—N201—Fe1124.29 (13)C203—C204—H20F109.5
N601—C601—N604108.09 (18)H20E—C204—H20F109.5
N601—C601—H601126.0C203—C204—H20G109.5
N604—C601—H601126.0H20E—C204—H20G109.5
N501—C501—N504108.64 (18)H20F—C204—H20G109.5
N501—C501—H501125.7C603—C604—H60E109.5
N504—C501—H501125.7C603—C604—H60F109.5
N202—N203—N204106.85 (16)H60E—C604—H60F109.5
N304—C302—C304112.56 (17)C603—C604—H60G109.5
N304—C302—H30A109.1H60E—C604—H60G109.5
C304—C302—H30A109.1H60F—C604—H60G109.5
N304—C302—H30B109.1C103—C104—H10E109.5
C304—C302—H30B109.1C103—C104—H10F109.5
H30A—C302—H30B107.8H10E—C104—H10F109.5
N603—N602—N601109.79 (16)C103—C104—H10G109.5
N402—N403—N404106.76 (16)H10E—C104—H10G109.5
N204—C202—C203111.78 (17)H10F—C104—H10G109.5
N204—C202—H20A109.3C302—C304—C303113.20 (19)
C203—C202—H20A109.3C302—C304—H30F108.9
N204—C202—H20B109.3C303—C304—H30F108.9
C203—C202—H20B109.3C302—C304—H30G108.9
H20A—C202—H20B107.9C303—C304—H30G108.9
N303—N302—N301109.73 (16)H30F—C304—H30G107.8
N103—N102—N101109.57 (16)F104—B100—F101109.45 (19)
N404—C401—N401108.98 (18)F104—B100—F102109.70 (18)
N404—C401—H401125.5F101—B100—F102109.70 (19)
N401—C401—H401125.5F104—B100—F103109.28 (19)
N604—C602—C603111.67 (17)F101—B100—F103109.25 (18)
N604—C602—H60A109.3F102—B100—F103109.45 (19)
C603—C602—H60A109.3F201—B200—F202109.7 (2)
N604—C602—H60B109.3F201—B200—F204109.9 (2)
C603—C602—H60B109.3F202—B200—F204109.25 (19)
H60A—C602—H60B107.9F201—B200—F203109.42 (19)
N304—C301—N301109.05 (18)F202—B200—F203109.0 (2)
N304—C301—H301125.5F204—B200—F203109.52 (19)
N301—C301—H301125.5
N201—Fe1—N401—C40118.40 (18)N501—Fe1—N301—N302109.42 (15)
N301—Fe1—N401—C40171.02 (18)N601—Fe1—N301—N302124 (20)
N501—Fe1—N401—C401161.73 (18)N101—Fe1—N301—N302161.11 (16)
N601—Fe1—N401—C401108.82 (18)N401—Fe1—N201—C201108.40 (18)
N101—Fe1—N401—C401173 (100)N301—Fe1—N201—C20117.81 (18)
N201—Fe1—N401—N402160.78 (16)N501—Fe1—N201—C201133 (49)
N301—Fe1—N401—N402109.80 (15)N601—Fe1—N201—C201161.97 (18)
N501—Fe1—N401—N40219.09 (16)N101—Fe1—N201—C20171.61 (18)
N601—Fe1—N401—N40270.36 (16)N401—Fe1—N201—N20270.09 (15)
N101—Fe1—N401—N4028 (91)N301—Fe1—N201—N202160.68 (16)
N401—Fe1—N601—C60118.03 (18)N501—Fe1—N201—N20248 (47)
N201—Fe1—N601—C60171.57 (18)N601—Fe1—N201—N20219.54 (16)
N301—Fe1—N601—C601125 (20)N101—Fe1—N201—N202109.90 (15)
N501—Fe1—N601—C601108.50 (18)N602—N601—C601—N6040.1 (2)
N101—Fe1—N601—C601162.02 (18)Fe1—N601—C601—N604178.89 (14)
N401—Fe1—N601—N602160.76 (16)N603—N604—C601—N6010.4 (2)
N201—Fe1—N601—N602109.64 (16)C602—N604—C601—N601174.39 (19)
N301—Fe1—N601—N60256 (20)N502—N501—C501—N5040.8 (2)
N501—Fe1—N601—N60270.29 (16)Fe1—N501—C501—N504179.12 (14)
N101—Fe1—N601—N60219.19 (16)N503—N504—C501—N5010.4 (2)
N504—N503—N502—N5010.8 (2)C502—N504—C501—N501173.90 (19)
C601—N604—N603—N6020.7 (2)C201—N204—N203—N2020.2 (2)
C602—N604—N603—N602175.26 (17)C202—N204—N203—N202175.34 (17)
C401—N401—N402—N4030.3 (2)C301—N304—C302—C304125.0 (2)
Fe1—N401—N402—N403179.02 (13)N303—N304—C302—C30460.8 (3)
N502—N503—N504—C5010.3 (2)N604—N603—N602—N6010.7 (2)
N502—N503—N504—C502175.15 (18)C601—N601—N602—N6030.5 (2)
N503—N502—N501—C5011.0 (2)Fe1—N601—N602—N603178.53 (13)
N503—N502—N501—Fe1178.92 (13)N401—N402—N403—N4040.1 (2)
N401—Fe1—N501—C50170.63 (19)C401—N404—N403—N4020.2 (2)
N201—Fe1—N501—C50147 (47)C402—N404—N403—N402175.08 (17)
N301—Fe1—N501—C501161.22 (19)C201—N204—C202—C203125.5 (2)
N601—Fe1—N501—C50118.99 (19)N203—N204—C202—C20360.4 (3)
N101—Fe1—N501—C501109.36 (19)N304—N303—N302—N3010.5 (2)
N401—Fe1—N501—N502109.42 (16)C301—N301—N302—N3030.8 (2)
N201—Fe1—N501—N502132 (49)Fe1—N301—N302—N303179.15 (13)
N301—Fe1—N501—N50218.82 (16)N104—N103—N102—N1010.8 (2)
N601—Fe1—N501—N502160.96 (16)C101—N101—N102—N1030.8 (2)
N101—Fe1—N501—N50270.59 (16)Fe1—N101—N102—N103178.72 (13)
C301—N304—N303—N3020.0 (2)N403—N404—C401—N4010.4 (2)
C302—N304—N303—N302175.32 (17)C402—N404—C401—N401174.34 (18)
N102—N103—N104—C1010.4 (2)N402—N401—C401—N4040.5 (2)
N102—N103—N104—C102175.49 (17)Fe1—N401—C401—N404178.84 (13)
N401—Fe1—N101—C1017 (91)C601—N604—C602—C603125.8 (2)
N201—Fe1—N101—C101161.56 (18)N603—N604—C602—C60360.9 (2)
N301—Fe1—N101—C101109.03 (18)N303—N304—C301—N3010.5 (2)
N501—Fe1—N101—C10118.32 (18)C302—N304—C301—N301174.30 (19)
N601—Fe1—N101—C10171.13 (18)N302—N301—C301—N3040.7 (2)
N401—Fe1—N101—N102172 (100)Fe1—N301—C301—N304179.15 (14)
N201—Fe1—N101—N10218.99 (16)N203—N204—C201—N2010.2 (2)
N301—Fe1—N101—N10270.42 (16)C202—N204—C201—N201174.85 (18)
N501—Fe1—N101—N102161.14 (16)N202—N201—C201—N2040.1 (2)
N601—Fe1—N101—N102109.41 (16)Fe1—N201—C201—N204178.84 (14)
C401—N404—C402—C403125.0 (2)N404—C402—C403—C40458.5 (2)
N403—N404—C402—C40360.8 (3)C501—N504—C502—C503125.1 (2)
N102—N101—C101—N1040.6 (2)N503—N504—C502—C50361.2 (3)
Fe1—N101—C101—N104178.97 (13)N204—N203—N202—N2010.1 (2)
N103—N104—C101—N1010.1 (2)C201—N201—N202—N2030.0 (2)
C102—N104—C101—N101174.41 (18)Fe1—N201—N202—N203178.82 (13)
N401—Fe1—N301—C301161.18 (18)N604—C602—C603—C60459.0 (2)
N201—Fe1—N301—C301109.22 (18)N204—C202—C203—C20458.9 (2)
N501—Fe1—N301—C30170.71 (18)C101—N104—C102—C103125.4 (2)
N601—Fe1—N301—C30156 (20)N103—N104—C102—C10360.6 (3)
N101—Fe1—N301—C30118.77 (18)N104—C102—C103—C10458.7 (2)
N401—Fe1—N301—N30218.94 (16)N504—C502—C503—C50458.5 (2)
N201—Fe1—N301—N30270.65 (15)N304—C302—C304—C30358.2 (2)
(PTZ_LS-ord_R-3) top
Crystal data top
C24H48FeN24·2(BF4)F(000) = 1404
Mr = 902.33Dx = 1.412 Mg m3
Hexagonal, R3Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -R 3µ = 0.44 mm1
a = 10.7023 (2) ÅT = 84 K
c = 32.0931 (15) ÅPlate, violet
V = 3183.44 (17) Å30.61 × 0.53 × 0.14 mm
Z = 3
Data collection top
Oxford Diffraction Diffractometer with Sapphire3 detector1105 independent reflections
Radiation source: fine-focus sealed tube1099 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.011
Detector resolution: 16.0328 pixels mm-1θmax = 25.0°, θmin = 3.4°
ω – scanh = 1212
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1212
Tmin = 0.774, Tmax = 0.941l = 2826
6536 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.067H atoms treated by a mixture of independent and constrained refinement
S = 0.97 w = 1/[σ2(Fo2) + (0.0368P)2 + 7.1948P]
where P = (Fo2 + 2Fc2)/3
1105 reflections(Δ/σ)max < 0.001
91 parametersΔρmax = 0.25 e Å3
0 restraintsΔρmin = 0.25 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.00001.00000.00000.00906 (16)
N10.04844 (11)0.87760 (12)0.03551 (4)0.0115 (3)
N20.16484 (12)0.93107 (12)0.06167 (4)0.0161 (3)
N30.16950 (12)0.82575 (12)0.08001 (4)0.0173 (3)
N40.05541 (12)0.70258 (12)0.06607 (4)0.0126 (3)
C10.01721 (14)0.73544 (14)0.03917 (5)0.0119 (3)
H10.10230.66830.02490.014*
C20.03365 (16)0.56000 (15)0.07827 (5)0.0167 (4)
H2A0.11720.55160.06880.020*
H2B0.05370.48360.06430.020*
C30.01692 (17)0.53692 (16)0.12481 (5)0.0202 (4)
H3A0.00280.44030.13130.024*
H3B0.10710.60950.13860.024*
C40.10880 (18)0.54811 (18)0.14268 (6)0.0272 (4)
H4A0.09080.64670.13900.041*
H4B0.11880.52450.17240.041*
H4C0.19780.48040.12810.041*
B10.66670.33330.01567 (11)0.0154 (7)
F10.66670.33330.05870 (6)0.0344 (5)
F20.76145 (10)0.29031 (11)0.00127 (3)0.0317 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.00754 (17)0.00754 (17)0.0121 (4)0.00377 (9)0.0000.000
N10.0094 (5)0.0125 (5)0.0127 (8)0.0054 (4)0.0006 (4)0.0006 (4)
N20.0132 (6)0.0151 (6)0.0195 (9)0.0066 (5)0.0033 (5)0.0006 (5)
N30.0151 (6)0.0150 (6)0.0209 (10)0.0070 (5)0.0040 (5)0.0004 (5)
N40.0126 (6)0.0119 (6)0.0143 (9)0.0069 (5)0.0004 (5)0.0005 (5)
C10.0119 (6)0.0125 (6)0.0118 (10)0.0064 (5)0.0005 (5)0.0006 (5)
C20.0218 (7)0.0133 (7)0.0196 (12)0.0121 (6)0.0001 (6)0.0019 (6)
C30.0268 (8)0.0175 (7)0.0180 (12)0.0124 (6)0.0026 (6)0.0026 (6)
C40.0332 (9)0.0269 (8)0.0198 (12)0.0138 (7)0.0074 (7)0.0022 (7)
B10.0140 (8)0.0140 (8)0.018 (2)0.0070 (4)0.0000.000
F10.0429 (7)0.0429 (7)0.0175 (15)0.0215 (3)0.0000.000
F20.0315 (5)0.0379 (6)0.0386 (8)0.0270 (5)0.0133 (4)0.0100 (4)
Geometric parameters (Å, º) top
Fe1—N1i1.9907 (12)C2—C31.510 (3)
Fe1—N1ii1.9907 (12)C2—H2A0.9900
Fe1—N1iii1.9907 (12)C2—H2B0.9900
Fe1—N1iv1.9907 (12)C3—C41.521 (2)
Fe1—N11.9907 (12)C3—H3A0.9900
Fe1—N1v1.9907 (12)C3—H3B0.9900
N1—C11.3241 (18)C4—H4A0.9800
N1—N21.3679 (17)C4—H4B0.9800
N2—N31.2944 (17)C4—H4C0.9800
N3—N41.3487 (16)B1—F11.381 (4)
N4—C11.3215 (19)B1—F21.3863 (14)
N4—C21.4768 (17)B1—F2vi1.3863 (14)
C1—H10.9500B1—F2vii1.3863 (14)
N1i—Fe1—N1ii90.48 (5)N1—C1—H1125.7
N1i—Fe1—N1iii180.00 (6)N4—C2—C3112.08 (12)
N1ii—Fe1—N1iii89.52 (5)N4—C2—H2A109.2
N1i—Fe1—N1iv90.48 (5)C3—C2—H2A109.2
N1ii—Fe1—N1iv90.48 (5)N4—C2—H2B109.2
N1iii—Fe1—N1iv89.52 (5)C3—C2—H2B109.2
N1i—Fe1—N189.52 (5)H2A—C2—H2B107.9
N1ii—Fe1—N189.52 (5)C4—C3—C2113.40 (13)
N1iii—Fe1—N190.48 (5)C4—C3—H3A108.9
N1iv—Fe1—N1180.00 (6)C2—C3—H3A108.9
N1i—Fe1—N1v89.52 (5)C4—C3—H3B108.9
N1ii—Fe1—N1v180.00 (6)C2—C3—H3B108.9
N1iii—Fe1—N1v90.48 (5)H3A—C3—H3B107.7
N1iv—Fe1—N1v89.52 (5)C3—C4—H4A109.5
N1—Fe1—N1v90.48 (5)C3—C4—H4B109.5
C1—N1—N2105.98 (11)H4A—C4—H4B109.5
C1—N1—Fe1130.07 (10)C3—C4—H4C109.5
N2—N1—Fe1123.94 (9)H4A—C4—H4C109.5
N3—N2—N1109.77 (11)H4B—C4—H4C109.5
N2—N3—N4106.86 (11)F1—B1—F2109.47 (14)
C1—N4—N3108.78 (11)F1—B1—F2vi109.47 (14)
C1—N4—C2129.67 (12)F2—B1—F2vi109.47 (14)
N3—N4—C2121.33 (12)F1—B1—F2vii109.47 (14)
N4—C1—N1108.60 (12)F2—B1—F2vii109.47 (14)
N4—C1—H1125.7F2vi—B1—F2vii109.47 (14)
N1i—Fe1—N1—C118.27 (12)Fe1—N1—N2—N3178.88 (9)
N1ii—Fe1—N1—C1108.75 (15)N1—N2—N3—N40.32 (16)
N1iii—Fe1—N1—C1161.73 (12)N2—N3—N4—C10.11 (16)
N1iv—Fe1—N1—C194 (3)N2—N3—N4—C2175.29 (12)
N1v—Fe1—N1—C171.25 (15)N3—N4—C1—N10.15 (16)
N1i—Fe1—N1—N2160.84 (12)C2—N4—C1—N1174.50 (13)
N1ii—Fe1—N1—N270.36 (9)N2—N1—C1—N40.34 (15)
N1iii—Fe1—N1—N219.16 (12)Fe1—N1—C1—N4178.90 (10)
N1iv—Fe1—N1—N287 (2)C1—N4—C2—C3125.31 (16)
N1v—Fe1—N1—N2109.64 (9)N3—N4—C2—C360.62 (17)
C1—N1—N2—N30.41 (16)N4—C2—C3—C458.69 (17)
Symmetry codes: (i) y1, x+y, z; (ii) xy+1, x+1, z; (iii) y+1, xy+2, z; (iv) x, y+2, z; (v) x+y1, x+1, z; (vi) x+y+1, x+1, z; (vii) y+1, xy, z.
 

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