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The low-spin iron(II) ion in the title compound, [Fe(C12H12N2)3](ClO4)2·C12H12N2, possesses an octa­hedral geometry formed by three bidentate 5,5′-dimeth­yl-2,2′-bipyrid­yl ligands. An uncoordinated ligand and two perchlorate anions are also present in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805019574/rz6093sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805019574/rz6093Isup2.hkl
Contains datablock I

CCDC reference: 277770

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.006 Å
  • Disorder in main residue
  • R factor = 0.078
  • wR factor = 0.238
  • Data-to-parameter ratio = 16.9

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O23
Author Response: the A alert (and also some B alerts) come from the treatment of the disordered perchlorate anion

Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O22
Author Response: the A alert (and also some B alerts) come from the treatment of the disordered perchlorate anion
PLAT241_ALERT_2_B Check High      Ueq as Compared to Neighbors for        O34
Author Response: the A alert (and also some B alerts) come from the treatment of the disordered perchlorate anion
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for        Cl3

Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.108 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT215_ALERT_3_C Disordered O32 has ADP max/min Ratio ....... 3.30 PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.26 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O21
Author Response: the A alert (and also some B alerts) come from the treatment of the disordered perchlorate anion
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cl2
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        O33
PLAT301_ALERT_3_C Main Residue  Disorder .........................       7.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O22
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O24
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O32
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O34
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C17
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C27
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C37
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C57
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C67
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C77
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C87
PLAT413_ALERT_2_C Short Inter XH3 .. XHn     H27A   ..  H33A    ..       2.14 Ang.
PLAT413_ALERT_2_C Short Inter XH3 .. XHn     H47A   ..  H73A    ..       2.10 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2
              C12 H12 N2
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          4
              Cl O4

1 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 24 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 14 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 9 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 2002); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1990); software used to prepare material for publication: SHELXTL.

Tris(5,5'-dimethyl-2,2'-bipyridyl-κ2N,N')iron(II) bis(perchlorate) 5,5'-dimethyl-2,2'-bipyridyl solvate top
Crystal data top
[Fe(C12H12N2)3](ClO4)2·C12H12N2Z = 2
Mr = 991.69F(000) = 1032
Triclinic, P1Dx = 1.431 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.670 (2) ÅCell parameters from 32869 reflections
b = 13.466 (3) Åθ = 2.7–27.5°
c = 14.792 (3) ŵ = 0.51 mm1
α = 94.77 (3)°T = 173 K
β = 90.82 (3)°Plate, red
γ = 96.26 (3)°0.35 × 0.10 × 0.02 mm
V = 2302.0 (8) Å3
Data collection top
Nonius KappaCCD
diffractometer
10528 independent reflections
Radiation source: fine-focus sealed tube6461 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.108
ω scansθmax = 27.5°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1515
Tmin = 0.842, Tmax = 0.990k = 1717
32869 measured reflectionsl = 1919
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)] = 0.078Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.238H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.130P)2 + 0.9561P]
where P = (Fo2 + 2Fc2)/3
10528 reflections(Δ/σ)max = 0.001
622 parametersΔρmax = 0.98 e Å3
18 restraintsΔρmin = 0.94 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*/UeqOcc. (<1)
Fe10.72986 (4)0.14446 (4)0.25751 (4)0.02072 (18)
N110.8357 (3)0.2596 (2)0.3139 (2)0.0217 (7)
C120.8028 (3)0.3512 (3)0.3022 (3)0.0232 (9)
C130.8652 (3)0.4398 (3)0.3397 (3)0.0276 (9)
H13A0.84020.50310.33050.033*
C140.9643 (4)0.4335 (3)0.3909 (3)0.0299 (10)
H14A1.00800.49310.41650.036*
C151.0001 (3)0.3418 (3)0.4049 (3)0.0298 (10)
C160.9331 (3)0.2566 (3)0.3644 (3)0.0276 (9)
H16A0.95730.19280.37290.033*
C171.1072 (4)0.3324 (4)0.4609 (4)0.0435 (13)
H17A1.14250.39930.48360.065*
H17B1.16210.29870.42310.065*
H17C1.08640.29300.51220.065*
N210.6542 (3)0.2550 (2)0.2098 (2)0.0203 (7)
C220.6979 (3)0.3483 (3)0.2449 (3)0.0228 (9)
C230.6447 (3)0.4326 (3)0.2285 (3)0.0285 (10)
H23A0.67580.49690.25450.034*
C240.5455 (4)0.4220 (3)0.1738 (3)0.0296 (10)
H24A0.50760.47900.16280.035*
C250.5020 (3)0.3268 (3)0.1350 (3)0.0274 (9)
C260.5584 (3)0.2462 (3)0.1561 (3)0.0251 (9)
H26A0.52810.18110.13140.030*
C270.3958 (4)0.3109 (4)0.0727 (3)0.0340 (11)
H27A0.37900.23940.05310.051*
H27B0.41000.34880.01950.051*
H27C0.32990.33420.10530.051*
N310.6223 (3)0.0359 (2)0.1921 (2)0.0220 (7)
C320.6533 (3)0.0091 (3)0.1066 (3)0.0235 (9)
C330.5886 (4)0.0673 (3)0.0517 (3)0.0309 (10)
H33A0.61140.08520.00830.037*
C340.4905 (4)0.1162 (3)0.0867 (3)0.0324 (10)
H34A0.44520.16760.05010.039*
C350.4581 (3)0.0911 (3)0.1743 (3)0.0292 (10)
C360.5264 (3)0.0125 (3)0.2239 (3)0.0271 (9)
H36A0.50350.00770.28350.033*
C370.3556 (4)0.1474 (4)0.2158 (4)0.0396 (12)
H37A0.31860.19900.17080.059*
H37B0.30020.10060.23490.059*
H37C0.38150.17920.26860.059*
N410.8186 (3)0.1266 (2)0.1448 (2)0.0224 (7)
C420.7622 (3)0.0618 (3)0.0783 (3)0.0231 (9)
C430.8088 (4)0.0459 (3)0.0066 (3)0.0297 (10)
H43A0.76670.00340.05290.036*
C440.9175 (4)0.0925 (3)0.0234 (3)0.0323 (10)
H44A0.95060.08150.08120.039*
C450.9777 (3)0.1556 (3)0.0449 (3)0.0271 (9)
C460.9247 (3)0.1711 (3)0.1274 (3)0.0230 (9)
H46A0.96470.21500.17390.028*
C471.0981 (4)0.2070 (4)0.0303 (3)0.0340 (11)
H47A1.12640.24690.08620.051*
H47B1.09510.25100.01900.051*
H47C1.15020.15630.01440.051*
N510.6401 (3)0.1492 (2)0.3694 (2)0.0223 (7)
C520.6762 (3)0.0941 (3)0.4354 (3)0.0247 (9)
C530.6256 (4)0.0938 (3)0.5196 (3)0.0306 (10)
H53A0.65330.05550.56470.037*
C540.5345 (4)0.1497 (4)0.5377 (3)0.0352 (11)
H54A0.49890.14900.59510.042*
C550.4946 (3)0.2070 (3)0.4720 (3)0.0271 (9)
C560.5510 (3)0.2039 (3)0.3887 (3)0.0243 (9)
H56A0.52520.24250.34300.029*
C570.3981 (4)0.2699 (4)0.4867 (3)0.0391 (12)
H57A0.36900.26390.54800.059*
H57B0.33590.24700.44210.059*
H57C0.42590.34010.47960.059*
N610.8039 (3)0.0436 (2)0.3202 (2)0.0219 (7)
C620.7698 (3)0.0341 (3)0.4067 (3)0.0229 (9)
C630.8187 (4)0.0284 (3)0.4623 (3)0.0328 (10)
H63A0.79470.03270.52300.039*
C640.9035 (4)0.0850 (4)0.4278 (4)0.0377 (11)
H64A0.93930.12700.46550.045*
C650.9357 (4)0.0800 (3)0.3381 (3)0.0311 (10)
C660.8842 (3)0.0134 (3)0.2873 (3)0.0267 (9)
H66A0.90700.00810.22640.032*
C671.02254 (19)0.14333 (17)0.29802 (17)0.0500 (14)
H67A1.04850.18500.34380.075*
H67B1.08860.10010.27780.075*
H67C0.98750.18650.24610.075*
N711.09456 (19)0.39381 (17)0.23883 (17)0.0402 (10)
C721.07515 (19)0.48679 (17)0.19626 (17)0.0308 (10)
C731.14403 (19)0.56191 (17)0.20998 (17)0.0360 (11)
H73A1.12650.62690.17960.043*
C741.2390 (4)0.5410 (4)0.2687 (4)0.0407 (12)
H74A1.28760.59150.27830.049*
C751.2625 (4)0.4463 (4)0.3130 (4)0.0405 (12)
C761.1873 (5)0.3770 (4)0.2967 (4)0.0498 (14)
H76A1.20170.31250.32850.060*
C771.3644 (5)0.4196 (5)0.3798 (5)0.0677 (19)
H77A1.36620.34950.40390.102*
H77B1.43630.42920.34850.102*
H77C1.35610.46310.42980.102*
N810.9518 (3)0.5978 (3)0.0893 (3)0.0365 (9)
C820.9701 (4)0.5062 (3)0.1337 (3)0.0312 (10)
C830.8965 (4)0.4336 (4)0.1231 (3)0.0375 (11)
H83A0.91180.36890.15450.045*
C840.8010 (4)0.4566 (4)0.0665 (3)0.0360 (11)
H84A0.74880.40810.06010.043*
C850.7802 (4)0.5505 (4)0.0184 (3)0.0327 (10)
C860.8593 (4)0.6179 (4)0.0339 (3)0.0399 (12)
H86A0.84650.68280.00280.048*
C870.6780 (4)0.5809 (4)0.0460 (4)0.0416 (12)
H87A0.68080.64990.07200.062*
H87B0.68060.53580.09480.062*
H87C0.60630.57660.01290.062*
Cl10.68163 (10)0.26625 (8)0.24199 (9)0.0368 (3)
O110.5830 (4)0.3282 (3)0.2013 (4)0.0729 (14)
O120.7531 (3)0.2278 (3)0.1723 (3)0.0574 (10)
O130.6447 (3)0.1838 (3)0.2977 (3)0.0472 (9)
O140.7471 (3)0.3244 (3)0.2961 (3)0.0503 (10)
Cl20.2480 (5)0.1252 (4)0.2634 (4)0.0473 (18)0.50
O210.2833 (8)0.2308 (4)0.2782 (6)0.076 (3)0.50
O220.2914 (9)0.0874 (8)0.1786 (6)0.084 (4)0.50
O230.1245 (5)0.1080 (8)0.2611 (8)0.137 (5)0.50
O240.2930 (10)0.0749 (7)0.3356 (6)0.043 (3)0.50
Cl30.2337 (4)0.1160 (3)0.2539 (3)0.0280 (12)0.50
O310.2066 (7)0.2161 (4)0.2772 (6)0.079 (4)0.50
O320.3256 (5)0.1182 (7)0.1906 (6)0.059 (3)0.50
O330.1338 (5)0.0562 (4)0.2137 (4)0.0450 (19)0.50
O340.2688 (8)0.0736 (7)0.3343 (5)0.072 (6)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0169 (3)0.0200 (3)0.0260 (3)0.0083 (2)0.0033 (2)0.0021 (2)
N110.0154 (15)0.0229 (18)0.0275 (19)0.0069 (13)0.0048 (13)0.0006 (14)
C120.0189 (18)0.023 (2)0.028 (2)0.0068 (16)0.0067 (16)0.0029 (17)
C130.027 (2)0.026 (2)0.031 (2)0.0083 (18)0.0035 (17)0.0002 (19)
C140.025 (2)0.031 (2)0.033 (2)0.0039 (18)0.0032 (18)0.0022 (19)
C150.020 (2)0.036 (3)0.034 (3)0.0063 (18)0.0020 (17)0.001 (2)
C160.024 (2)0.029 (2)0.031 (2)0.0101 (18)0.0009 (17)0.0032 (19)
C170.026 (2)0.047 (3)0.057 (3)0.003 (2)0.012 (2)0.004 (3)
N210.0167 (15)0.0228 (18)0.0223 (18)0.0083 (13)0.0047 (13)0.0016 (14)
C220.0210 (19)0.023 (2)0.025 (2)0.0078 (16)0.0044 (16)0.0024 (17)
C230.023 (2)0.020 (2)0.042 (3)0.0068 (17)0.0005 (18)0.0029 (19)
C240.027 (2)0.021 (2)0.042 (3)0.0114 (17)0.0010 (19)0.0025 (19)
C250.0194 (19)0.024 (2)0.040 (3)0.0064 (17)0.0030 (17)0.0028 (19)
C260.0203 (19)0.024 (2)0.031 (2)0.0078 (17)0.0027 (17)0.0001 (18)
C270.024 (2)0.033 (3)0.047 (3)0.0124 (19)0.0065 (19)0.002 (2)
N310.0221 (16)0.0174 (17)0.0274 (19)0.0077 (14)0.0036 (14)0.0021 (14)
C320.0190 (18)0.021 (2)0.031 (2)0.0067 (16)0.0021 (16)0.0021 (17)
C330.031 (2)0.029 (2)0.031 (2)0.0072 (19)0.0013 (18)0.0083 (19)
C340.030 (2)0.027 (2)0.037 (3)0.0020 (19)0.0026 (19)0.009 (2)
C350.024 (2)0.024 (2)0.039 (3)0.0060 (17)0.0016 (18)0.0023 (19)
C360.025 (2)0.027 (2)0.030 (2)0.0068 (18)0.0032 (17)0.0009 (19)
C370.029 (2)0.038 (3)0.049 (3)0.006 (2)0.006 (2)0.004 (2)
N410.0213 (16)0.0166 (17)0.0298 (19)0.0063 (13)0.0022 (14)0.0005 (14)
C420.0239 (19)0.019 (2)0.028 (2)0.0074 (16)0.0048 (16)0.0012 (17)
C430.028 (2)0.032 (2)0.029 (2)0.0075 (19)0.0030 (18)0.0039 (19)
C440.035 (2)0.034 (3)0.029 (2)0.012 (2)0.0115 (19)0.002 (2)
C450.023 (2)0.027 (2)0.032 (2)0.0075 (17)0.0062 (17)0.0009 (19)
C460.0181 (18)0.025 (2)0.027 (2)0.0076 (16)0.0045 (16)0.0005 (17)
C470.024 (2)0.040 (3)0.039 (3)0.0082 (19)0.0118 (19)0.003 (2)
N510.0186 (16)0.0197 (17)0.0286 (19)0.0073 (13)0.0038 (13)0.0045 (14)
C520.025 (2)0.020 (2)0.029 (2)0.0053 (17)0.0031 (17)0.0013 (17)
C530.034 (2)0.032 (2)0.028 (2)0.013 (2)0.0054 (18)0.0027 (19)
C540.033 (2)0.041 (3)0.033 (3)0.014 (2)0.0136 (19)0.002 (2)
C550.022 (2)0.027 (2)0.032 (2)0.0058 (17)0.0045 (17)0.0040 (19)
C560.0211 (19)0.024 (2)0.028 (2)0.0103 (17)0.0039 (16)0.0023 (18)
C570.031 (2)0.049 (3)0.040 (3)0.022 (2)0.009 (2)0.002 (2)
N610.0191 (16)0.0189 (17)0.0275 (19)0.0053 (13)0.0021 (13)0.0044 (14)
C620.025 (2)0.019 (2)0.025 (2)0.0064 (16)0.0037 (16)0.0023 (17)
C630.035 (2)0.033 (3)0.033 (3)0.013 (2)0.0042 (19)0.004 (2)
C640.034 (2)0.034 (3)0.049 (3)0.016 (2)0.002 (2)0.008 (2)
C650.031 (2)0.025 (2)0.041 (3)0.0150 (19)0.0054 (19)0.002 (2)
C660.025 (2)0.019 (2)0.037 (3)0.0091 (17)0.0070 (18)0.0012 (18)
C670.048 (3)0.047 (3)0.062 (4)0.033 (3)0.012 (3)0.007 (3)
N710.038 (2)0.028 (2)0.055 (3)0.0060 (18)0.0007 (19)0.0028 (19)
C720.028 (2)0.028 (2)0.038 (3)0.0061 (18)0.0113 (19)0.004 (2)
C730.033 (2)0.032 (3)0.044 (3)0.010 (2)0.002 (2)0.003 (2)
C740.031 (2)0.043 (3)0.050 (3)0.011 (2)0.005 (2)0.003 (2)
C750.034 (2)0.032 (3)0.055 (3)0.004 (2)0.005 (2)0.002 (2)
C760.050 (3)0.028 (3)0.070 (4)0.003 (2)0.003 (3)0.002 (3)
C770.054 (4)0.053 (4)0.093 (5)0.004 (3)0.022 (3)0.003 (3)
N810.036 (2)0.031 (2)0.044 (2)0.0158 (17)0.0007 (18)0.0042 (18)
C820.029 (2)0.030 (2)0.036 (3)0.0076 (19)0.0139 (19)0.004 (2)
C830.035 (2)0.030 (3)0.048 (3)0.013 (2)0.009 (2)0.000 (2)
C840.029 (2)0.032 (3)0.050 (3)0.016 (2)0.003 (2)0.007 (2)
C850.028 (2)0.034 (3)0.037 (3)0.008 (2)0.0090 (19)0.006 (2)
C860.045 (3)0.030 (3)0.045 (3)0.012 (2)0.000 (2)0.004 (2)
C870.035 (2)0.039 (3)0.053 (3)0.009 (2)0.001 (2)0.010 (2)
Cl10.0362 (6)0.0280 (6)0.0476 (7)0.0125 (5)0.0107 (5)0.0009 (5)
O110.057 (2)0.045 (2)0.113 (4)0.003 (2)0.017 (3)0.001 (2)
O120.064 (2)0.055 (2)0.057 (3)0.018 (2)0.028 (2)0.007 (2)
O130.054 (2)0.037 (2)0.054 (2)0.0242 (17)0.0200 (17)0.0034 (17)
O140.061 (2)0.043 (2)0.053 (2)0.0271 (18)0.0073 (18)0.0068 (18)
Cl20.042 (3)0.047 (3)0.051 (3)0.016 (2)0.010 (2)0.013 (2)
O210.134 (10)0.038 (5)0.060 (6)0.029 (6)0.010 (7)0.012 (4)
O220.123 (8)0.080 (7)0.047 (6)0.040 (6)0.010 (6)0.035 (5)
O230.073 (7)0.147 (9)0.196 (10)0.012 (7)0.000 (7)0.054 (8)
O240.047 (5)0.045 (8)0.041 (8)0.026 (4)0.012 (4)0.010 (6)
Cl30.0253 (17)0.0249 (19)0.036 (2)0.0088 (14)0.0041 (15)0.0068 (16)
O310.105 (7)0.052 (5)0.081 (6)0.047 (5)0.029 (6)0.031 (4)
O320.019 (3)0.109 (9)0.057 (6)0.006 (5)0.016 (4)0.044 (6)
O330.048 (4)0.043 (4)0.039 (4)0.010 (4)0.012 (3)0.006 (3)
O340.102 (11)0.074 (11)0.039 (9)0.001 (7)0.020 (7)0.018 (8)
Geometric parameters (Å, º) top
Fe1—N511.972 (4)C52—C621.474 (6)
Fe1—N611.973 (3)C53—C541.385 (6)
Fe1—N211.983 (3)C53—H53A0.9500
Fe1—N411.987 (4)C54—C551.395 (6)
Fe1—N111.991 (3)C54—H54A0.9500
Fe1—N311.995 (3)C55—C561.404 (6)
N11—C121.355 (5)C55—C571.489 (6)
N11—C161.358 (5)C56—H56A0.9500
C12—C131.397 (6)C57—H57A0.9800
C12—C221.474 (5)C57—H57B0.9800
C13—C141.387 (6)C57—H57C0.9800
C13—H13A0.9500N61—C661.347 (5)
C14—C151.377 (6)N61—C621.358 (5)
C14—H14A0.9500C62—C631.385 (6)
C15—C161.401 (6)C63—C641.390 (6)
C15—C171.512 (6)C63—H63A0.9500
C16—H16A0.9500C64—C651.389 (7)
C17—H17A0.9800C64—H64A0.9500
C17—H17B0.9800C65—C661.394 (6)
C17—H17C0.9800C65—C671.493 (5)
N21—C261.351 (5)C66—H66A0.9500
N21—C221.361 (5)C67—H67A0.9800
C22—C231.388 (6)C67—H67B0.9800
C23—C241.391 (6)C67—H67C0.9800
C23—H23A0.9500N71—C721.349 (3)
C24—C251.399 (6)N71—C761.358 (6)
C24—H24A0.9500C72—C731.384 (3)
C25—C261.384 (6)C72—C821.512 (5)
C25—C271.519 (6)C73—C741.387 (5)
C26—H26A0.9500C73—H73A0.9500
C27—H27A0.9800C74—C751.383 (7)
C27—H27B0.9800C74—H74A0.9500
C27—H27C0.9800C75—C761.382 (7)
N31—C361.344 (5)C75—C771.527 (7)
N31—C321.352 (5)C76—H76A0.9500
C32—C331.401 (6)C77—H77A0.9800
C32—C421.470 (6)C77—H77B0.9800
C33—C341.386 (6)C77—H77C0.9800
C33—H33A0.9500N81—C861.335 (6)
C34—C351.380 (6)N81—C821.343 (6)
C34—H34A0.9500C82—C831.387 (6)
C35—C361.402 (6)C83—C841.377 (7)
C35—C371.511 (6)C83—H83A0.9500
C36—H36A0.9500C84—C851.393 (7)
C37—H37A0.9800C84—H84A0.9500
C37—H37B0.9800C85—C861.392 (6)
C37—H37C0.9800C85—C871.515 (6)
N41—C461.353 (5)C86—H86A0.9500
N41—C421.369 (5)C87—H87A0.9800
C42—C431.385 (6)C87—H87B0.9800
C43—C441.388 (6)C87—H87C0.9800
C43—H43A0.9500Cl1—O121.431 (4)
C44—C451.393 (6)Cl1—O141.433 (4)
C44—H44A0.9500Cl1—O131.435 (3)
C45—C461.387 (6)Cl1—O111.439 (4)
C45—C471.523 (6)Cl2—O221.4339
C46—H46A0.9500Cl2—O231.4340
C47—H47A0.9800Cl2—O211.4340
C47—H47B0.9800Cl2—O241.4340
C47—H47C0.9800Cl3—O321.4339
N51—C561.360 (5)Cl3—O311.4340
N51—C521.363 (5)Cl3—O331.4340
C52—C531.385 (6)Cl3—O341.4340
N51—Fe1—N6181.75 (14)C56—N51—C52117.5 (4)
N51—Fe1—N2192.40 (14)C56—N51—Fe1127.3 (3)
N61—Fe1—N21172.76 (14)C52—N51—Fe1115.1 (3)
N51—Fe1—N41174.93 (13)N51—C52—C53122.0 (4)
N61—Fe1—N4194.54 (14)N51—C52—C62113.3 (4)
N21—Fe1—N4191.55 (14)C53—C52—C62124.7 (4)
N51—Fe1—N1188.26 (14)C52—C53—C54119.7 (4)
N61—Fe1—N1194.09 (13)C52—C53—H53A120.2
N21—Fe1—N1181.42 (13)C54—C53—H53A120.2
N41—Fe1—N1195.48 (14)C53—C54—C55120.2 (4)
N51—Fe1—N3194.61 (14)C53—C54—H54A119.9
N61—Fe1—N3190.17 (13)C55—C54—H54A119.9
N21—Fe1—N3194.56 (13)C54—C55—C56116.7 (4)
N41—Fe1—N3181.90 (14)C54—C55—C57123.4 (4)
N11—Fe1—N31175.17 (14)C56—C55—C57119.9 (4)
C12—N11—C16117.2 (4)N51—C56—C55124.0 (4)
C12—N11—Fe1114.9 (3)N51—C56—H56A118.0
C16—N11—Fe1127.8 (3)C55—C56—H56A118.0
N11—C12—C13122.4 (4)C55—C57—H57A109.5
N11—C12—C22113.9 (3)C55—C57—H57B109.5
C13—C12—C22123.7 (4)H57A—C57—H57B109.5
C14—C13—C12118.7 (4)C55—C57—H57C109.5
C14—C13—H13A120.7H57A—C57—H57C109.5
C12—C13—H13A120.7H57B—C57—H57C109.5
C15—C14—C13120.7 (4)C66—N61—C62118.1 (4)
C15—C14—H14A119.7C66—N61—Fe1127.4 (3)
C13—C14—H14A119.7C62—N61—Fe1114.5 (3)
C14—C15—C16117.1 (4)N61—C62—C63122.0 (4)
C14—C15—C17121.9 (4)N61—C62—C52114.7 (3)
C16—C15—C17121.0 (4)C63—C62—C52123.3 (4)
N11—C16—C15124.0 (4)C62—C63—C64119.1 (4)
N11—C16—H16A118.0C62—C63—H63A120.5
C15—C16—H16A118.0C64—C63—H63A120.5
C15—C17—H17A109.5C65—C64—C63119.8 (4)
C15—C17—H17B109.5C65—C64—H64A120.1
H17A—C17—H17B109.5C63—C64—H64A120.1
C15—C17—H17C109.5C64—C65—C66117.5 (4)
H17A—C17—H17C109.5C64—C65—C67121.1 (4)
H17B—C17—H17C109.5C66—C65—C67121.4 (4)
C26—N21—C22118.1 (3)N61—C66—C65123.4 (4)
C26—N21—Fe1127.0 (3)N61—C66—H66A118.3
C22—N21—Fe1114.4 (2)C65—C66—H66A118.3
N21—C22—C23121.6 (4)C65—C67—H67A109.5
N21—C22—C12114.7 (3)C65—C67—H67B109.5
C23—C22—C12123.7 (4)H67A—C67—H67B109.5
C22—C23—C24119.5 (4)C65—C67—H67C109.5
C22—C23—H23A120.3H67A—C67—H67C109.5
C24—C23—H23A120.3H67B—C67—H67C109.5
C23—C24—C25119.4 (4)C72—N71—C76115.9 (2)
C23—C24—H24A120.3N71—C72—C73123.0 (2)
C25—C24—H24A120.3N71—C72—C82115.89 (19)
C26—C25—C24117.7 (4)C73—C72—C82121.07 (19)
C26—C25—C27120.4 (4)C72—C73—C74119.1 (2)
C24—C25—C27121.9 (4)C72—C73—H73A120.4
N21—C26—C25123.7 (4)C74—C73—H73A120.4
N21—C26—H26A118.2C75—C74—C73119.6 (4)
C25—C26—H26A118.2C75—C74—H74A120.2
C25—C27—H27A109.5C73—C74—H74A120.2
C25—C27—H27B109.5C76—C75—C74117.0 (4)
H27A—C27—H27B109.5C76—C75—C77121.0 (5)
C25—C27—H27C109.5C74—C75—C77121.9 (5)
H27A—C27—H27C109.5N71—C76—C75125.2 (5)
H27B—C27—H27C109.5N71—C76—H76A117.4
C36—N31—C32118.3 (3)C75—C76—H76A117.4
C36—N31—Fe1127.5 (3)C75—C77—H77A109.5
C32—N31—Fe1114.2 (3)C75—C77—H77B109.5
N31—C32—C33121.6 (4)H77A—C77—H77B109.5
N31—C32—C42115.1 (3)C75—C77—H77C109.5
C33—C32—C42123.2 (4)H77A—C77—H77C109.5
C34—C33—C32118.6 (4)H77B—C77—H77C109.5
C34—C33—H33A120.7C86—N81—C82117.9 (4)
C32—C33—H33A120.7N81—C82—C83121.9 (4)
C35—C34—C33120.7 (4)N81—C82—C72116.3 (4)
C35—C34—H34A119.6C83—C82—C72121.8 (4)
C33—C34—H34A119.6C84—C83—C82119.0 (5)
C34—C35—C36117.0 (4)C84—C83—H83A120.5
C34—C35—C37121.7 (4)C82—C83—H83A120.5
C36—C35—C37121.4 (4)C83—C84—C85120.6 (4)
N31—C36—C35123.7 (4)C83—C84—H84A119.7
N31—C36—H36A118.2C85—C84—H84A119.7
C35—C36—H36A118.2C86—C85—C84115.8 (4)
C35—C37—H37A109.5C86—C85—C87120.6 (4)
C35—C37—H37B109.5C84—C85—C87123.6 (4)
H37A—C37—H37B109.5N81—C86—C85124.8 (4)
C35—C37—H37C109.5N81—C86—H86A117.6
H37A—C37—H37C109.5C85—C86—H86A117.6
H37B—C37—H37C109.5C85—C87—H87A109.5
C46—N41—C42118.3 (4)C85—C87—H87B109.5
C46—N41—Fe1127.7 (3)H87A—C87—H87B109.5
C42—N41—Fe1114.0 (3)C85—C87—H87C109.5
N41—C42—C43121.4 (4)H87A—C87—H87C109.5
N41—C42—C32114.4 (4)H87B—C87—H87C109.5
C43—C42—C32124.2 (4)O12—Cl1—O14108.9 (2)
C42—C43—C44119.5 (4)O12—Cl1—O13109.0 (2)
C42—C43—H43A120.3O14—Cl1—O13109.7 (2)
C44—C43—H43A120.3O12—Cl1—O11109.5 (3)
C43—C44—C45119.7 (4)O14—Cl1—O11109.8 (2)
C43—C44—H44A120.2O13—Cl1—O11109.9 (2)
C45—C44—H44A120.2O22—Cl2—O23109.5
C46—C45—C44118.0 (4)O22—Cl2—O21109.4
C46—C45—C47120.3 (4)O23—Cl2—O21109.4
C44—C45—C47121.7 (4)O22—Cl2—O24109.5
N41—C46—C45123.0 (4)O23—Cl2—O24109.5
N41—C46—H46A118.5O21—Cl2—O24109.4
C45—C46—H46A118.5O32—Cl3—O31109.4
C45—C47—H47A109.5O32—Cl3—O33109.5
C45—C47—H47B109.5O31—Cl3—O33109.4
H47A—C47—H47B109.5O32—Cl3—O34109.5
C45—C47—H47C109.5O31—Cl3—O34109.4
H47A—C47—H47C109.5O33—Cl3—O34109.5
H47B—C47—H47C109.5
 

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