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As representative porphyrin model compounds, the structures of `picket-fence' porphyrins have been studied intensively. The title solvated complex salt {systematic name: (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium(I) [5,10,15,20-tetrakis(2-tert-butanamidophenyl)porphyrinato]iron(II) n-hexane monosolvate}, [K(C18H36N2O6)][Fe(C64H64N8O4)Cl]·C6H14 or [K(222)][Fe(TpivPP)Cl]·C6H14 [222 is cryptand-222 or 4,7,13,16,21,24-hexaoxa-1,10-di­aza­bi­cyclo[8.8.8]hexacosane, and TpivPP is meso-α,α,α,α-tetrakis(o-piv­al­am­ido­phenyl)por­phy­rin­ate(2−)], [K(222)][Fe(TpivPP)Cl]·C6H14, is a five-coordinate high-spin iron(II) picket-fence porphyrin complex. It crystallizes with a potassium cation chelated inside a cryptand-222 molecule; the average K—O and K—N distances are 2.81 (2) and 3.05 (2) Å, respectively. One of the protecting tert-butyl pickets is disordered. The porphyrin plane presents a moderately ruffled distortion, as suggested by the atomic displacements. The axial chloride ligand is located inside the molecular cavity on the hindered porphyrin side and the Fe—Cl bond is tilted slightly off the normal to the porphyrin plane by 4.1°. The out-of-plane displacement of the metal centre relative to the 24-atom mean plane (Δ24) is 0.62 Å, indicating a noticeable doming of the porphyrin core.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229615015478/fn3203sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229615015478/fn3203Isup2.hkl
Contains datablock I

CCDC reference: 1407804

Experimental top

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Results and discussion top

Computing details top

Data collection: CrysAlis PRO (Agilent, 2011); cell refinement: CrysAlis PRO (Agilent, 2011); data reduction: CrysAlis PRO (Agilent, 2011); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015) and publCIF (Westrip, 2010).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium(I) [5,10,15,20-tetrakis(2-tert-butanamidophenyl)porphyrinato]iron(II) n-hexane monosolvate top
Crystal data top
[K(C18H36N2O6)]·[Fe(C64H64N8O4)Cl]·C6H14Z = 2
Mr = 1602.29F(000) = 1708
Triclinic, P1Dx = 1.219 Mg m3
a = 13.0174 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 14.3273 (8) ÅCell parameters from 5751 reflections
c = 24.1557 (13) Åθ = 3.1–28.5°
α = 80.946 (4)°µ = 0.31 mm1
β = 79.029 (4)°T = 120 K
γ = 87.039 (3)°Block, black
V = 4366.6 (4) Å30.20 × 0.15 × 0.15 mm
Data collection top
Agilent Xcalibur Gemini
diffractometer with Eos detector
18570 independent reflections
Radiation source: Enhance (Mo) X-ray source11295 reflections with I > 2σ(I)
Detector resolution: 16.2141 pixels mm-1Rint = 0.040
ω scansθmax = 28.5°, θmin = 3.1°
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2011)
h = 1716
Tmin = 0.968, Tmax = 1.000k = 1818
35844 measured reflectionsl = 3132
Refinement top
Refinement on F2108 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.069H-atom parameters constrained
wR(F2) = 0.168 w = 1/[σ2(Fo2) + (0.0515P)2 + 5.1988P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
18570 reflectionsΔρmax = 0.96 e Å3
1029 parametersΔρmin = 0.39 e Å3
Crystal data top
[K(C18H36N2O6)]·[Fe(C64H64N8O4)Cl]·C6H14γ = 87.039 (3)°
Mr = 1602.29V = 4366.6 (4) Å3
Triclinic, P1Z = 2
a = 13.0174 (4) ÅMo Kα radiation
b = 14.3273 (8) ŵ = 0.31 mm1
c = 24.1557 (13) ÅT = 120 K
α = 80.946 (4)°0.20 × 0.15 × 0.15 mm
β = 79.029 (4)°
Data collection top
Agilent Xcalibur Gemini
diffractometer with Eos detector
18570 independent reflections
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2011)
11295 reflections with I > 2σ(I)
Tmin = 0.968, Tmax = 1.000Rint = 0.040
35844 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.069108 restraints
wR(F2) = 0.168H-atom parameters constrained
S = 1.02Δρmax = 0.96 e Å3
18570 reflectionsΔρmin = 0.39 e Å3
1029 parameters
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)
Fe10.64044 (4)0.35943 (3)0.25958 (2)0.02729 (13)
K10.28282 (6)0.68487 (5)0.23927 (3)0.03283 (19)
Cl10.80572 (8)0.29080 (8)0.24814 (5)0.0566 (3)
C1010.6562 (2)0.4890 (3)0.14163 (14)0.0291 (8)
C1020.5868 (2)0.3532 (2)0.13925 (14)0.0282 (7)
C1030.5058 (3)0.2240 (2)0.21404 (14)0.0285 (7)
C1040.4831 (3)0.1946 (2)0.30797 (14)0.0294 (8)
C1050.5382 (3)0.2701 (2)0.38372 (14)0.0293 (8)
C1060.6246 (2)0.3978 (2)0.38445 (14)0.0274 (7)
C1070.6926 (2)0.5330 (2)0.31100 (14)0.0286 (7)
C1080.6975 (2)0.5708 (2)0.21870 (14)0.0288 (7)
C2010.6507 (3)0.4861 (3)0.08268 (15)0.0335 (8)
H2010.67230.53370.05100.040*
C2020.6084 (3)0.4018 (3)0.08165 (14)0.0358 (9)
H2020.59550.37910.04880.043*
C2030.4414 (3)0.1416 (2)0.23219 (15)0.0361 (8)
H2030.41400.10670.20810.043*
C2040.4272 (3)0.1233 (2)0.28961 (16)0.0373 (9)
H2040.38810.07320.31350.045*
C2050.5446 (3)0.2737 (2)0.44261 (14)0.0325 (8)
H2050.51650.22960.47490.039*
C2060.5980 (3)0.3516 (3)0.44272 (14)0.0343 (8)
H2060.61510.37240.47520.041*
C2070.7385 (3)0.6254 (3)0.29375 (15)0.0358 (8)
H2070.76250.66260.31780.043*
C2080.7408 (3)0.6489 (3)0.23741 (15)0.0342 (8)
H2080.76600.70590.21430.041*
C3010.6916 (2)0.5667 (2)0.16164 (14)0.0286 (7)
C3020.5335 (2)0.2678 (2)0.15757 (14)0.0281 (7)
C3030.4878 (3)0.1996 (2)0.36495 (14)0.0303 (8)
C3040.6753 (2)0.4839 (2)0.36704 (14)0.0284 (7)
N10.61826 (19)0.40727 (19)0.17502 (11)0.0260 (6)
N20.5309 (2)0.25479 (19)0.26100 (11)0.0276 (6)
N30.5883 (2)0.34554 (19)0.34930 (11)0.0262 (6)
N40.6685 (2)0.5010 (2)0.26420 (11)0.0279 (6)
C10.7263 (3)0.6520 (3)0.11989 (14)0.0306 (8)
C20.6623 (3)0.7331 (3)0.11709 (15)0.0357 (8)
H2A0.59450.73160.14020.043*
C30.6952 (3)0.8153 (3)0.08153 (16)0.0407 (9)
H3A0.65110.87030.08080.049*
C40.7934 (3)0.8169 (3)0.04686 (16)0.0397 (9)
H4A0.81570.87290.02160.048*
C50.8591 (3)0.7381 (3)0.04870 (16)0.0391 (9)
H5A0.92610.74000.02470.047*
C60.8271 (3)0.6555 (3)0.08581 (15)0.0325 (8)
C70.4976 (3)0.2210 (2)0.11308 (14)0.0308 (8)
C80.3974 (3)0.2405 (3)0.10123 (17)0.0443 (10)
H8A0.35390.28600.11970.053*
C90.3601 (3)0.1945 (3)0.06281 (18)0.0528 (12)
H9A0.29250.21000.05410.063*
C100.4217 (3)0.1263 (3)0.03754 (16)0.0463 (10)
H10A0.39490.09250.01270.056*
C110.5218 (3)0.1062 (3)0.04766 (15)0.0380 (9)
H11A0.56420.06010.02910.046*
C120.5606 (3)0.1537 (2)0.08537 (14)0.0322 (8)
C130.4314 (3)0.1246 (2)0.40880 (15)0.0343 (8)
C140.3327 (3)0.1429 (3)0.44018 (16)0.0443 (10)
H14A0.30280.20480.43500.053*
C150.2770 (4)0.0723 (3)0.47892 (17)0.0541 (11)
H15A0.21010.08600.50010.065*
C160.3203 (4)0.0173 (4)0.48610 (18)0.0589 (12)
H16A0.28220.06580.51210.071*
C170.4186 (4)0.0383 (3)0.45623 (18)0.0560 (12)
H17A0.44740.10060.46200.067*
C180.4748 (3)0.0324 (3)0.41768 (16)0.0394 (9)
C190.7144 (3)0.5309 (2)0.41040 (14)0.0286 (7)
C200.6603 (3)0.6066 (3)0.43215 (17)0.0432 (10)
H20A0.59420.62520.42220.052*
C210.6998 (3)0.6562 (3)0.46815 (17)0.0448 (10)
H21A0.66200.70870.48210.054*
C220.7948 (3)0.6280 (3)0.48328 (14)0.0348 (8)
H22A0.82250.66170.50780.042*
C230.8501 (3)0.5518 (2)0.46327 (14)0.0314 (8)
H23A0.91500.53250.47440.038*
C240.8106 (2)0.5026 (2)0.42648 (13)0.0267 (7)
C250.9982 (3)0.5651 (3)0.07878 (15)0.0375 (9)
C261.0433 (3)0.4682 (3)0.09938 (16)0.0419 (9)
C270.9748 (3)0.3871 (3)0.09591 (19)0.0523 (11)
H27A1.01270.32690.10340.079*
H27B0.95740.39430.05770.079*
H27C0.91030.38800.12440.079*
C281.0554 (3)0.4682 (3)0.16146 (18)0.0576 (12)
H28A1.09960.52070.16320.086*
H28B0.98640.47580.18510.086*
H28C1.08810.40830.17560.086*
C291.1517 (3)0.4565 (4)0.0627 (2)0.0647 (13)
H29A1.19590.50870.06490.097*
H29B1.18390.39630.07680.097*
H29C1.14460.45710.02300.097*
C300.7451 (3)0.0897 (2)0.07057 (17)0.0391 (9)
C310.8481 (3)0.0944 (3)0.09241 (19)0.0449 (10)
C320.8864 (7)0.0069 (5)0.1151 (4)0.057 (2)0.622 (6)
H32A0.83150.03750.14490.085*0.622 (6)
H32B0.90210.04420.08370.085*0.622 (6)
H32C0.94960.00250.13090.085*0.622 (6)
C330.8388 (5)0.1484 (5)0.1472 (3)0.0484 (18)0.622 (6)
H33A0.78610.11790.17840.073*0.622 (6)
H33B0.90660.14530.15950.073*0.622 (6)
H33C0.81810.21460.13700.073*0.622 (6)
C340.9287 (6)0.1438 (6)0.0470 (3)0.065 (2)0.622 (6)
H34A0.99360.14620.06170.097*0.622 (6)
H34B0.94190.10960.01420.097*0.622 (6)
H34C0.90390.20830.03530.097*0.622 (6)
C32A0.8356 (11)0.0308 (12)0.1431 (7)0.075 (4)0.378 (6)
H32D0.82050.03180.13550.112*0.378 (6)
H32E0.90010.02710.15870.112*0.378 (6)
H32F0.77740.05240.17060.112*0.378 (6)
C33A0.8715 (9)0.1948 (8)0.0905 (6)0.057 (3)0.378 (6)
H33D0.87730.22760.05130.086*0.378 (6)
H33E0.81510.22430.11540.086*0.378 (6)
H33F0.93780.19900.10350.086*0.378 (6)
C34A0.9346 (8)0.0597 (10)0.0406 (6)0.060 (3)0.378 (6)
H34D0.93930.10760.00650.090*0.378 (6)
H34E1.00310.05110.05220.090*0.378 (6)
H34F0.91330.00030.03210.090*0.378 (6)
C350.6293 (3)0.0639 (3)0.37802 (18)0.0469 (10)
C360.7363 (4)0.0523 (3)0.3390 (2)0.0567 (12)
C370.8108 (5)0.1242 (5)0.3653 (3)0.120 (3)
H37A0.78130.18740.37160.181*
H37B0.87860.12390.33940.181*
H37C0.82040.10760.40180.181*
C380.7806 (4)0.0437 (4)0.3293 (4)0.126 (3)
H38A0.78550.06240.36600.189*
H38B0.85050.04320.30550.189*
H38C0.73490.08900.31000.189*
C390.7283 (6)0.0817 (5)0.2827 (3)0.122 (3)
H39A0.69900.14510.28940.184*
H39B0.68250.03680.26330.184*
H39C0.79810.08250.25880.184*
C400.9507 (3)0.3771 (3)0.41663 (18)0.0465 (10)
C410.9906 (3)0.2993 (3)0.3807 (2)0.0521 (11)
C421.0211 (4)0.3433 (4)0.3170 (2)0.0670 (14)
H42A0.95930.37390.30370.101*
H42B1.07520.39030.31280.101*
H42C1.04810.29350.29420.101*
C430.9039 (3)0.2263 (3)0.3881 (2)0.0584 (12)
H43A0.84240.25730.37470.088*
H43B0.92970.17550.36580.088*
H43C0.88450.19960.42850.088*
C441.0865 (4)0.2519 (4)0.4014 (2)0.0725 (15)
H44A1.11320.20170.37880.109*
H44B1.14070.29880.39700.109*
H44C1.06730.22450.44170.109*
N50.8916 (2)0.5739 (2)0.09159 (13)0.0388 (7)
H5B0.85850.52090.10550.047*
N60.6626 (2)0.1374 (2)0.09742 (13)0.0411 (8)
H6A0.67440.16190.12680.049*
N70.5758 (3)0.0189 (2)0.38596 (14)0.0437 (8)
H7A0.60870.07080.36900.052*
N80.8657 (2)0.4267 (2)0.40297 (13)0.0367 (7)
H8B0.84090.40880.37500.044*
O11.0522 (2)0.6318 (2)0.05414 (13)0.0577 (8)
O20.7388 (2)0.04667 (19)0.03173 (12)0.0507 (7)
O30.5950 (3)0.1415 (2)0.39870 (15)0.0699 (9)
O40.9920 (3)0.3932 (2)0.45530 (16)0.0832 (12)
C450.1639 (4)0.8446 (3)0.12612 (19)0.0612 (13)
H45A0.14920.86610.08730.073*
H45B0.16770.90140.14420.073*
C460.0746 (3)0.7846 (3)0.1605 (2)0.0590 (12)
H46A0.00720.81890.15840.071*
H46B0.07350.72500.14480.071*
C470.0028 (3)0.7124 (3)0.2537 (2)0.0555 (12)
H47A0.00130.64920.24230.067*
H47B0.06400.74600.24890.067*
C480.0146 (3)0.7021 (3)0.3141 (2)0.0574 (12)
H48A0.02400.76490.32440.069*
H48B0.04910.67410.33910.069*
C490.1180 (4)0.6335 (4)0.38016 (19)0.0714 (15)
H49A0.05150.61730.40680.086*
H49B0.14240.69380.38780.086*
C500.1996 (4)0.5556 (4)0.3885 (2)0.0767 (16)
H50A0.20280.54060.42960.092*
H50B0.17800.49790.37630.092*
C510.2749 (3)0.7276 (3)0.08001 (17)0.0509 (11)
H51A0.29710.76240.04110.061*
H51B0.20520.70130.08190.061*
C520.3514 (3)0.6475 (3)0.09031 (17)0.0489 (10)
H52A0.36000.60870.05920.059*
H52B0.42050.67290.09080.059*
C530.3752 (3)0.5061 (3)0.15096 (19)0.0494 (11)
H53A0.44940.52180.14810.059*
H53B0.37110.46810.12060.059*
C540.3360 (3)0.4499 (3)0.2080 (2)0.0518 (11)
H54A0.25990.44040.21260.062*
H54B0.37160.38710.21100.062*
C550.3386 (3)0.4413 (3)0.3060 (2)0.0582 (12)
H55A0.38160.38240.30460.070*
H55B0.26410.42400.31730.070*
C560.3681 (4)0.4954 (3)0.34890 (19)0.0583 (12)
H56A0.36110.45370.38620.070*
H56B0.44250.51280.33680.070*
C570.3515 (4)0.8626 (3)0.10370 (18)0.0573 (12)
H57A0.33200.91290.07420.069*
H57B0.41530.82980.08610.069*
C580.3763 (4)0.9074 (3)0.15156 (19)0.0591 (12)
H58A0.42820.95750.13620.071*
H58B0.31200.93680.17140.071*
C590.4528 (5)0.8827 (4)0.2317 (3)0.0925 (19)
H59A0.51090.92500.21260.111*
H59B0.39520.92190.25010.111*
C600.4868 (5)0.8163 (5)0.2731 (3)0.103 (2)
H60A0.51900.84910.29850.123*
H60B0.54080.77430.25460.123*
C610.4424 (4)0.6982 (4)0.3481 (2)0.0714 (15)
H61A0.47680.73410.37110.086*
H61B0.49510.65480.32980.086*
C620.3547 (4)0.6433 (4)0.38540 (19)0.0700 (15)
H62A0.38150.60430.41740.084*
H62B0.30130.68810.40180.084*
N90.2658 (2)0.7940 (2)0.12142 (14)0.0449 (8)
N100.3042 (3)0.5815 (3)0.35629 (15)0.0537 (9)
O50.08794 (19)0.76418 (19)0.21812 (12)0.0480 (7)
O60.1024 (2)0.6431 (2)0.32193 (12)0.0532 (8)
O70.31385 (18)0.59096 (18)0.14331 (11)0.0415 (6)
O80.3557 (2)0.49855 (19)0.25133 (12)0.0462 (7)
O90.4169 (2)0.8381 (2)0.19019 (12)0.0530 (7)
O100.4013 (3)0.7606 (3)0.30651 (14)0.0714 (10)
C1S0.0962 (8)0.1062 (7)0.4316 (4)0.177 (4)
H1SA0.14300.13640.45680.265*
H1SB0.05310.05730.44970.265*
H1SC0.05080.15380.42450.265*
C2S0.1654 (6)0.0585 (7)0.3716 (3)0.141 (3)
H2SA0.21210.01140.37900.170*
H2SB0.20980.10790.35370.170*
C3S0.1005 (7)0.0130 (6)0.3327 (4)0.136 (3)
H3SA0.05040.02950.35360.163*
H3SB0.05890.06270.32380.163*
C4S0.1469 (5)0.0418 (7)0.2789 (3)0.131 (3)
H4S10.20610.00280.26200.157*
H4S20.17820.09720.28870.157*
C5S0.0892 (6)0.0796 (7)0.2313 (5)0.147 (3)
H5S10.06950.02450.21570.177*
H5S20.02320.10960.24860.177*
C6S0.1344 (6)0.1414 (8)0.1869 (3)0.159 (4)
H6SA0.08610.15820.16030.238*
H6SB0.15190.19840.20060.238*
H6SC0.19850.11270.16750.238*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0272 (3)0.0308 (3)0.0277 (3)0.0028 (2)0.0119 (2)0.0090 (2)
K10.0270 (4)0.0340 (4)0.0343 (4)0.0009 (3)0.0012 (3)0.0013 (3)
Cl10.0353 (5)0.0733 (8)0.0636 (7)0.0176 (5)0.0195 (5)0.0116 (6)
C1010.0211 (16)0.042 (2)0.0260 (18)0.0031 (15)0.0056 (14)0.0101 (16)
C1020.0242 (17)0.036 (2)0.0264 (18)0.0081 (15)0.0070 (14)0.0119 (15)
C1030.0327 (18)0.0279 (18)0.0300 (19)0.0060 (15)0.0135 (15)0.0129 (15)
C1040.0374 (19)0.0242 (17)0.0310 (19)0.0035 (15)0.0154 (15)0.0079 (15)
C1050.0327 (18)0.0294 (19)0.0293 (19)0.0051 (15)0.0125 (15)0.0085 (15)
C1060.0271 (17)0.0315 (19)0.0279 (18)0.0025 (14)0.0126 (14)0.0094 (15)
C1070.0252 (17)0.0331 (19)0.0321 (19)0.0012 (14)0.0137 (14)0.0083 (15)
C1080.0229 (16)0.0330 (19)0.0333 (19)0.0008 (14)0.0117 (14)0.0064 (16)
C2010.0283 (18)0.046 (2)0.0266 (19)0.0020 (16)0.0029 (15)0.0089 (17)
C2020.037 (2)0.050 (2)0.0229 (18)0.0001 (17)0.0045 (15)0.0154 (17)
C2030.050 (2)0.0274 (19)0.038 (2)0.0032 (17)0.0176 (17)0.0119 (16)
C2040.054 (2)0.0266 (19)0.039 (2)0.0047 (17)0.0236 (18)0.0059 (16)
C2050.043 (2)0.0293 (19)0.0267 (18)0.0013 (16)0.0111 (16)0.0040 (15)
C2060.043 (2)0.039 (2)0.0265 (19)0.0014 (17)0.0151 (16)0.0113 (16)
C2070.036 (2)0.038 (2)0.040 (2)0.0060 (16)0.0186 (17)0.0096 (17)
C2080.0323 (19)0.034 (2)0.039 (2)0.0067 (16)0.0136 (16)0.0021 (16)
C3010.0226 (17)0.036 (2)0.0288 (18)0.0010 (14)0.0079 (14)0.0052 (15)
C3020.0292 (18)0.0318 (19)0.0279 (18)0.0062 (15)0.0111 (14)0.0137 (15)
C3030.0369 (19)0.0247 (18)0.0331 (19)0.0049 (15)0.0164 (16)0.0061 (15)
C3040.0267 (17)0.0324 (19)0.0301 (19)0.0025 (15)0.0114 (14)0.0106 (15)
N10.0239 (14)0.0338 (16)0.0233 (14)0.0007 (12)0.0074 (11)0.0102 (12)
N20.0350 (15)0.0244 (15)0.0280 (15)0.0036 (12)0.0137 (12)0.0098 (12)
N30.0299 (15)0.0260 (15)0.0272 (15)0.0013 (12)0.0128 (12)0.0087 (12)
N40.0260 (14)0.0346 (16)0.0269 (15)0.0000 (12)0.0122 (12)0.0081 (13)
C10.0284 (18)0.038 (2)0.0275 (18)0.0047 (15)0.0100 (15)0.0055 (16)
C20.0311 (19)0.046 (2)0.030 (2)0.0047 (17)0.0075 (15)0.0074 (17)
C30.047 (2)0.041 (2)0.037 (2)0.0058 (18)0.0173 (18)0.0059 (18)
C40.050 (2)0.038 (2)0.034 (2)0.0068 (18)0.0158 (18)0.0007 (17)
C50.037 (2)0.043 (2)0.037 (2)0.0102 (18)0.0060 (17)0.0049 (18)
C60.0314 (19)0.035 (2)0.034 (2)0.0041 (16)0.0096 (15)0.0077 (16)
C70.0371 (19)0.0325 (19)0.0262 (18)0.0002 (16)0.0095 (15)0.0105 (15)
C80.051 (2)0.048 (2)0.044 (2)0.0131 (19)0.0246 (19)0.025 (2)
C90.061 (3)0.056 (3)0.058 (3)0.013 (2)0.041 (2)0.026 (2)
C100.074 (3)0.040 (2)0.035 (2)0.003 (2)0.025 (2)0.0155 (18)
C110.056 (2)0.033 (2)0.0274 (19)0.0012 (18)0.0046 (17)0.0130 (16)
C120.041 (2)0.0292 (19)0.0264 (18)0.0041 (16)0.0023 (15)0.0073 (15)
C130.048 (2)0.031 (2)0.0293 (19)0.0059 (17)0.0198 (17)0.0055 (16)
C140.052 (2)0.051 (3)0.033 (2)0.005 (2)0.0142 (19)0.0094 (19)
C150.057 (3)0.068 (3)0.038 (2)0.020 (2)0.005 (2)0.007 (2)
C160.072 (3)0.064 (3)0.040 (3)0.029 (3)0.013 (2)0.005 (2)
C170.086 (3)0.038 (2)0.050 (3)0.015 (2)0.036 (3)0.009 (2)
C180.052 (2)0.034 (2)0.036 (2)0.0040 (18)0.0181 (18)0.0023 (17)
C190.0308 (18)0.0323 (19)0.0258 (18)0.0049 (15)0.0108 (14)0.0061 (15)
C200.045 (2)0.047 (2)0.047 (2)0.0120 (19)0.0256 (19)0.022 (2)
C210.054 (2)0.046 (2)0.044 (2)0.0064 (19)0.0200 (19)0.023 (2)
C220.046 (2)0.037 (2)0.0269 (19)0.0100 (17)0.0153 (16)0.0068 (16)
C230.0335 (19)0.035 (2)0.0286 (19)0.0086 (16)0.0134 (15)0.0012 (16)
C240.0282 (17)0.0298 (18)0.0230 (17)0.0047 (14)0.0054 (14)0.0044 (14)
C250.0292 (19)0.055 (3)0.032 (2)0.0042 (18)0.0069 (16)0.0141 (18)
C260.031 (2)0.057 (3)0.038 (2)0.0058 (18)0.0037 (16)0.0102 (19)
C270.051 (3)0.047 (3)0.061 (3)0.006 (2)0.012 (2)0.012 (2)
C280.059 (3)0.068 (3)0.047 (3)0.012 (2)0.018 (2)0.006 (2)
C290.040 (2)0.076 (3)0.073 (3)0.013 (2)0.002 (2)0.015 (3)
C300.045 (2)0.0228 (19)0.043 (2)0.0004 (17)0.0049 (18)0.0042 (17)
C310.039 (2)0.031 (2)0.060 (3)0.0007 (17)0.0013 (19)0.009 (2)
C320.068 (5)0.039 (4)0.072 (5)0.012 (3)0.035 (4)0.013 (4)
C330.040 (3)0.048 (4)0.061 (4)0.003 (3)0.006 (3)0.021 (3)
C340.059 (4)0.068 (5)0.061 (5)0.009 (4)0.004 (4)0.005 (4)
C32A0.058 (7)0.082 (8)0.081 (8)0.013 (6)0.029 (6)0.009 (7)
C33A0.054 (6)0.051 (6)0.072 (7)0.003 (5)0.009 (6)0.030 (6)
C34A0.039 (5)0.065 (7)0.080 (7)0.012 (5)0.011 (5)0.043 (6)
C350.064 (3)0.026 (2)0.059 (3)0.0018 (19)0.035 (2)0.0065 (19)
C360.072 (3)0.038 (2)0.071 (3)0.013 (2)0.032 (2)0.022 (2)
C370.094 (4)0.132 (6)0.111 (5)0.070 (4)0.004 (4)0.004 (4)
C380.048 (3)0.068 (4)0.258 (8)0.013 (3)0.023 (4)0.071 (5)
C390.144 (6)0.156 (6)0.067 (4)0.065 (5)0.001 (4)0.021 (4)
C400.049 (2)0.043 (2)0.058 (3)0.0034 (19)0.031 (2)0.017 (2)
C410.045 (2)0.053 (3)0.070 (3)0.011 (2)0.030 (2)0.024 (2)
C420.050 (3)0.092 (4)0.066 (3)0.006 (3)0.016 (2)0.031 (3)
C430.068 (3)0.041 (3)0.077 (3)0.009 (2)0.035 (3)0.021 (2)
C440.063 (3)0.071 (3)0.103 (4)0.024 (3)0.046 (3)0.041 (3)
N50.0274 (16)0.0333 (17)0.054 (2)0.0053 (13)0.0023 (14)0.0048 (15)
N60.0376 (18)0.045 (2)0.0444 (19)0.0020 (15)0.0025 (15)0.0246 (16)
N70.060 (2)0.0217 (16)0.053 (2)0.0009 (15)0.0223 (17)0.0004 (15)
N80.0325 (16)0.0444 (19)0.0420 (18)0.0038 (14)0.0201 (14)0.0191 (15)
O10.0289 (14)0.071 (2)0.065 (2)0.0111 (14)0.0056 (13)0.0125 (17)
O20.0679 (19)0.0400 (16)0.0431 (17)0.0179 (14)0.0047 (14)0.0154 (14)
O30.089 (2)0.0280 (17)0.100 (3)0.0016 (16)0.039 (2)0.0085 (17)
O40.097 (3)0.073 (2)0.114 (3)0.038 (2)0.084 (2)0.053 (2)
C450.070 (3)0.059 (3)0.051 (3)0.010 (2)0.023 (2)0.011 (2)
C460.044 (2)0.068 (3)0.065 (3)0.008 (2)0.021 (2)0.001 (3)
C470.027 (2)0.058 (3)0.075 (3)0.0018 (19)0.000 (2)0.005 (2)
C480.032 (2)0.063 (3)0.066 (3)0.011 (2)0.010 (2)0.000 (2)
C490.059 (3)0.084 (4)0.048 (3)0.019 (3)0.021 (2)0.017 (3)
C500.070 (3)0.082 (4)0.054 (3)0.020 (3)0.015 (2)0.025 (3)
C510.058 (3)0.057 (3)0.036 (2)0.013 (2)0.008 (2)0.001 (2)
C520.046 (2)0.066 (3)0.034 (2)0.005 (2)0.0015 (18)0.012 (2)
C530.038 (2)0.052 (3)0.063 (3)0.0147 (19)0.012 (2)0.023 (2)
C540.047 (2)0.039 (2)0.073 (3)0.0126 (19)0.019 (2)0.013 (2)
C550.051 (3)0.046 (3)0.071 (3)0.012 (2)0.016 (2)0.013 (2)
C560.061 (3)0.060 (3)0.050 (3)0.022 (2)0.017 (2)0.005 (2)
C570.071 (3)0.051 (3)0.041 (2)0.017 (2)0.001 (2)0.012 (2)
C580.074 (3)0.041 (3)0.056 (3)0.020 (2)0.002 (2)0.000 (2)
C590.112 (5)0.086 (4)0.092 (4)0.055 (4)0.040 (4)0.007 (4)
C600.099 (5)0.124 (6)0.102 (5)0.039 (4)0.049 (4)0.019 (4)
C610.066 (3)0.100 (4)0.059 (3)0.011 (3)0.031 (3)0.026 (3)
C620.092 (4)0.084 (4)0.036 (3)0.034 (3)0.025 (3)0.013 (3)
N90.0470 (19)0.046 (2)0.0391 (19)0.0065 (16)0.0074 (15)0.0028 (16)
N100.053 (2)0.058 (2)0.042 (2)0.0174 (18)0.0030 (17)0.0044 (18)
O50.0357 (15)0.0511 (17)0.0535 (18)0.0013 (13)0.0090 (13)0.0033 (14)
O60.0364 (15)0.0532 (18)0.0569 (19)0.0108 (13)0.0110 (13)0.0043 (15)
O70.0358 (14)0.0447 (16)0.0424 (16)0.0043 (12)0.0037 (12)0.0076 (13)
O80.0440 (15)0.0417 (16)0.0513 (17)0.0082 (13)0.0103 (13)0.0031 (14)
O90.0614 (18)0.0518 (18)0.0478 (17)0.0221 (15)0.0110 (14)0.0058 (15)
O100.070 (2)0.094 (3)0.056 (2)0.028 (2)0.0265 (17)0.0028 (19)
C1S0.201 (10)0.210 (11)0.130 (8)0.065 (8)0.028 (7)0.042 (8)
C2S0.100 (6)0.227 (10)0.113 (6)0.031 (6)0.048 (5)0.031 (7)
C3S0.150 (7)0.105 (6)0.176 (9)0.017 (6)0.059 (7)0.054 (6)
C4S0.048 (4)0.230 (10)0.101 (5)0.007 (5)0.004 (4)0.005 (6)
C5S0.098 (6)0.143 (8)0.204 (11)0.004 (5)0.056 (7)0.002 (7)
C6S0.086 (5)0.271 (13)0.102 (6)0.008 (7)0.011 (4)0.011 (7)
Geometric parameters (Å, º) top
Fe1—N42.103 (3)C34—H34B0.9800
Fe1—N22.114 (3)C34—H34C0.9800
Fe1—N12.119 (3)C32A—H32D0.9800
Fe1—N32.125 (3)C32A—H32E0.9800
Fe1—Cl12.3050 (10)C32A—H32F0.9800
K1—O82.776 (3)C33A—H33D0.9800
K1—O62.801 (3)C33A—H33E0.9800
K1—O102.806 (3)C33A—H33F0.9800
K1—O72.813 (3)C34A—H34D0.9800
K1—O52.828 (3)C34A—H34E0.9800
K1—O92.839 (3)C34A—H34F0.9800
K1—N103.033 (3)C35—O31.214 (5)
K1—N93.066 (3)C35—N71.366 (5)
C101—N11.370 (4)C35—C361.526 (6)
C101—C3011.412 (5)C36—C381.486 (6)
C101—C2011.446 (4)C36—C391.510 (7)
C102—N11.376 (4)C36—C371.527 (7)
C102—C3021.405 (5)C37—H37A0.9800
C102—C2021.438 (5)C37—H37B0.9800
C103—N21.379 (4)C37—H37C0.9800
C103—C3021.397 (5)C38—H38A0.9800
C103—C2031.446 (5)C38—H38B0.9800
C104—N21.377 (4)C38—H38C0.9800
C104—C3031.403 (4)C39—H39A0.9800
C104—C2041.453 (4)C39—H39B0.9800
C105—N31.367 (4)C39—H39C0.9800
C105—C3031.408 (4)C40—O41.219 (4)
C105—C2051.450 (4)C40—N81.349 (4)
C106—N31.377 (4)C40—C411.529 (5)
C106—C3041.395 (5)C41—C441.521 (6)
C106—C2061.444 (5)C41—C431.546 (6)
C107—N41.379 (4)C41—C421.554 (6)
C107—C3041.407 (5)C42—H42A0.9800
C107—C2071.448 (5)C42—H42B0.9800
C108—N41.373 (4)C42—H42C0.9800
C108—C3011.405 (4)C43—H43A0.9800
C108—C2081.447 (5)C43—H43B0.9800
C201—C2021.359 (5)C43—H43C0.9800
C201—H2010.9500C44—H44A0.9800
C202—H2020.9500C44—H44B0.9800
C203—C2041.349 (5)C44—H44C0.9800
C203—H2030.9500N5—H5B0.8800
C204—H2040.9500N6—H6A0.8800
C205—C2061.345 (5)N7—H7A0.8800
C205—H2050.9500N8—H8B0.8800
C206—H2060.9500C45—N91.473 (5)
C207—C2081.344 (5)C45—C461.514 (6)
C207—H2070.9500C45—H45A0.9900
C208—H2080.9500C45—H45B0.9900
C301—C11.487 (5)C46—O51.418 (5)
C302—C71.508 (4)C46—H46A0.9900
C303—C131.497 (5)C46—H46B0.9900
C304—C191.507 (4)C47—O51.427 (5)
C1—C21.394 (5)C47—C481.480 (6)
C1—C61.409 (5)C47—H47A0.9900
C2—C31.380 (5)C47—H47B0.9900
C2—H2A0.9500C48—O61.409 (5)
C3—C41.387 (5)C48—H48A0.9900
C3—H3A0.9500C48—H48B0.9900
C4—C51.382 (5)C49—O61.444 (5)
C4—H4A0.9500C49—C501.518 (6)
C5—C61.397 (5)C49—H49A0.9900
C5—H5A0.9500C49—H49B0.9900
C6—N51.408 (4)C50—N101.468 (6)
C7—C81.392 (5)C50—H50A0.9900
C7—C121.401 (5)C50—H50B0.9900
C8—C91.389 (5)C51—N91.471 (5)
C8—H8A0.9500C51—C521.502 (6)
C9—C101.376 (5)C51—H51A0.9900
C9—H9A0.9500C51—H51B0.9900
C10—C111.378 (5)C52—O71.418 (5)
C10—H10A0.9500C52—H52A0.9900
C11—C121.399 (5)C52—H52B0.9900
C11—H11A0.9500C53—O71.427 (4)
C12—N61.412 (4)C53—C541.494 (6)
C13—C141.398 (5)C53—H53A0.9900
C13—C181.410 (5)C53—H53B0.9900
C14—C151.393 (6)C54—O81.412 (5)
C14—H14A0.9500C54—H54A0.9900
C15—C161.374 (6)C54—H54B0.9900
C15—H15A0.9500C55—O81.426 (5)
C16—C171.387 (6)C55—C561.501 (6)
C16—H16A0.9500C55—H55A0.9900
C17—C181.397 (5)C55—H55B0.9900
C17—H17A0.9500C56—N101.467 (5)
C18—N71.410 (5)C56—H56A0.9900
C19—C201.382 (5)C56—H56B0.9900
C19—C241.402 (4)C57—N91.480 (5)
C20—C211.389 (5)C57—C581.501 (6)
C20—H20A0.9500C57—H57A0.9900
C21—C221.378 (5)C57—H57B0.9900
C21—H21A0.9500C58—O91.407 (5)
C22—C231.378 (5)C58—H58A0.9900
C22—H22A0.9500C58—H58B0.9900
C23—C241.400 (4)C59—C601.388 (8)
C23—H23A0.9500C59—O91.431 (5)
C24—N81.407 (4)C59—H59A0.9900
C25—O11.221 (4)C59—H59B0.9900
C25—N51.367 (4)C60—O101.440 (7)
C25—C261.527 (5)C60—H60A0.9900
C26—C271.522 (5)C60—H60B0.9900
C26—C291.533 (5)C61—O101.403 (6)
C26—C281.537 (5)C61—C621.487 (7)
C27—H27A0.9800C61—H61A0.9900
C27—H27B0.9800C61—H61B0.9900
C27—H27C0.9800C62—N101.464 (6)
C28—H28A0.9800C62—H62A0.9900
C28—H28B0.9800C62—H62B0.9900
C28—H28C0.9800C1S—C2S1.623 (11)
C29—H29A0.9800C1S—H1SA0.9800
C29—H29B0.9800C1S—H1SB0.9800
C29—H29C0.9800C1S—H1SC0.9800
C30—O21.218 (4)C2S—C3S1.440 (10)
C30—N61.357 (4)C2S—H2SA0.9900
C30—C311.539 (6)C2S—H2SB0.9900
C31—C32A1.393 (14)C3S—C4S1.448 (10)
C31—C33A1.478 (11)C3S—H3SA0.9900
C31—C341.483 (8)C3S—H3SB0.9900
C31—C321.560 (8)C4S—C5S1.508 (10)
C31—C331.619 (7)C4S—H4S10.9900
C31—C34A1.638 (11)C4S—H4S20.9900
C32—H32A0.9800C5S—C6S1.338 (10)
C32—H32B0.9800C5S—H5S10.9900
C32—H32C0.9800C5S—H5S20.9900
C33—H33A0.9800C6S—H6SA0.9800
C33—H33B0.9800C6S—H6SB0.9800
C33—H33C0.9800C6S—H6SC0.9800
C34—H34A0.9800
N4—Fe1—N2148.21 (10)H33D—C33A—H33E109.5
N4—Fe1—N186.77 (10)C31—C33A—H33F109.5
N2—Fe1—N185.85 (10)H33D—C33A—H33F109.5
N4—Fe1—N385.64 (10)H33E—C33A—H33F109.5
N2—Fe1—N386.12 (10)C31—C34A—H34D109.5
N1—Fe1—N3151.21 (10)C31—C34A—H34E109.5
N4—Fe1—Cl1103.25 (8)H34D—C34A—H34E109.5
N2—Fe1—Cl1108.53 (8)C31—C34A—H34F109.5
N1—Fe1—Cl1103.92 (8)H34D—C34A—H34F109.5
N3—Fe1—Cl1104.85 (8)H34E—C34A—H34F109.5
O8—K1—O692.88 (8)O3—C35—N7123.8 (4)
O8—K1—O10100.14 (10)O3—C35—C36121.6 (4)
O6—K1—O1098.48 (10)N7—C35—C36114.6 (4)
O8—K1—O761.78 (8)C38—C36—C39109.9 (5)
O6—K1—O7117.49 (9)C38—C36—C35115.7 (4)
O10—K1—O7139.25 (9)C39—C36—C35108.2 (4)
O8—K1—O5130.96 (8)C38—C36—C37109.8 (5)
O6—K1—O560.77 (8)C39—C36—C37105.9 (5)
O10—K1—O5122.74 (10)C35—C36—C37106.9 (4)
O7—K1—O592.85 (8)C36—C37—H37A109.5
O8—K1—O9122.22 (9)C36—C37—H37B109.5
O6—K1—O9140.15 (9)H37A—C37—H37B109.5
O10—K1—O960.12 (9)C36—C37—H37C109.5
O7—K1—O997.09 (8)H37A—C37—H37C109.5
O5—K1—O9100.75 (9)H37B—C37—H37C109.5
O8—K1—N1060.08 (9)C36—C38—H38A109.5
O6—K1—N1060.70 (9)C36—C38—H38B109.5
O10—K1—N1059.41 (10)H38A—C38—H38B109.5
O7—K1—N10121.52 (9)C36—C38—H38C109.5
O5—K1—N10120.78 (9)H38A—C38—H38C109.5
O9—K1—N10118.36 (10)H38B—C38—H38C109.5
O8—K1—N9120.85 (9)C36—C39—H39A109.5
O6—K1—N9120.32 (9)C36—C39—H39B109.5
O10—K1—N9118.82 (10)H39A—C39—H39B109.5
O7—K1—N959.61 (8)C36—C39—H39C109.5
O5—K1—N960.00 (8)H39A—C39—H39C109.5
O9—K1—N959.88 (8)H39B—C39—H39C109.5
N10—K1—N9178.22 (10)O4—C40—N8122.0 (4)
N1—C101—C301125.4 (3)O4—C40—C41122.5 (4)
N1—C101—C201110.1 (3)N8—C40—C41115.5 (3)
C301—C101—C201124.5 (3)C44—C41—C40108.4 (3)
N1—C102—C302124.5 (3)C44—C41—C43109.9 (4)
N1—C102—C202109.4 (3)C40—C41—C43109.2 (4)
C302—C102—C202125.8 (3)C44—C41—C42109.5 (4)
N2—C103—C302125.7 (3)C40—C41—C42109.7 (4)
N2—C103—C203109.7 (3)C43—C41—C42110.1 (3)
C302—C103—C203124.6 (3)C41—C42—H42A109.5
N2—C104—C303125.9 (3)C41—C42—H42B109.5
N2—C104—C204109.5 (3)H42A—C42—H42B109.5
C303—C104—C204124.6 (3)C41—C42—H42C109.5
N3—C105—C303125.3 (3)H42A—C42—H42C109.5
N3—C105—C205109.7 (3)H42B—C42—H42C109.5
C303—C105—C205125.1 (3)C41—C43—H43A109.5
N3—C106—C304125.6 (3)C41—C43—H43B109.5
N3—C106—C206109.2 (3)H43A—C43—H43B109.5
C304—C106—C206125.2 (3)C41—C43—H43C109.5
N4—C107—C304125.5 (3)H43A—C43—H43C109.5
N4—C107—C207109.6 (3)H43B—C43—H43C109.5
C304—C107—C207125.0 (3)C41—C44—H44A109.5
N4—C108—C301125.9 (3)C41—C44—H44B109.5
N4—C108—C208110.0 (3)H44A—C44—H44B109.5
C301—C108—C208124.1 (3)C41—C44—H44C109.5
C202—C201—C101106.3 (3)H44A—C44—H44C109.5
C202—C201—H201126.9H44B—C44—H44C109.5
C101—C201—H201126.9C25—N5—C6129.4 (3)
C201—C202—C102107.7 (3)C25—N5—H5B115.3
C201—C202—H202126.2C6—N5—H5B115.3
C102—C202—H202126.2C30—N6—C12129.8 (3)
C204—C203—C103107.4 (3)C30—N6—H6A115.1
C204—C203—H203126.3C12—N6—H6A115.1
C103—C203—H203126.3C35—N7—C18128.7 (3)
C203—C204—C104107.1 (3)C35—N7—H7A115.6
C203—C204—H204126.5C18—N7—H7A115.6
C104—C204—H204126.5C40—N8—C24130.1 (3)
C206—C205—C105106.8 (3)C40—N8—H8B114.9
C206—C205—H205126.6C24—N8—H8B114.9
C105—C205—H205126.6N9—C45—C46113.0 (4)
C205—C206—C106107.6 (3)N9—C45—H45A109.0
C205—C206—H206126.2C46—C45—H45A109.0
C106—C206—H206126.2N9—C45—H45B109.0
C208—C207—C107107.3 (3)C46—C45—H45B109.0
C208—C207—H207126.3H45A—C45—H45B107.8
C107—C207—H207126.3O5—C46—C45109.3 (3)
C207—C208—C108107.0 (3)O5—C46—H46A109.8
C207—C208—H208126.5C45—C46—H46A109.8
C108—C208—H208126.5O5—C46—H46B109.8
C108—C301—C101125.3 (3)C45—C46—H46B109.8
C108—C301—C1116.1 (3)H46A—C46—H46B108.3
C101—C301—C1118.6 (3)O5—C47—C48110.0 (3)
C103—C302—C102125.9 (3)O5—C47—H47A109.7
C103—C302—C7116.3 (3)C48—C47—H47A109.7
C102—C302—C7117.7 (3)O5—C47—H47B109.7
C104—C303—C105125.4 (3)C48—C47—H47B109.7
C104—C303—C13116.3 (3)H47A—C47—H47B108.2
C105—C303—C13118.3 (3)O6—C48—C47109.2 (3)
C106—C304—C107125.0 (3)O6—C48—H48A109.8
C106—C304—C19119.4 (3)C47—C48—H48A109.8
C107—C304—C19115.6 (3)O6—C48—H48B109.8
C101—N1—C102106.5 (3)C47—C48—H48B109.8
C101—N1—Fe1125.8 (2)H48A—C48—H48B108.3
C102—N1—Fe1126.0 (2)O6—C49—C50107.9 (4)
C104—N2—C103106.4 (3)O6—C49—H49A110.1
C104—N2—Fe1126.9 (2)C50—C49—H49A110.1
C103—N2—Fe1126.1 (2)O6—C49—H49B110.1
C105—N3—C106106.7 (3)C50—C49—H49B110.1
C105—N3—Fe1126.6 (2)H49A—C49—H49B108.4
C106—N3—Fe1124.4 (2)N10—C50—C49112.7 (4)
C108—N4—C107106.1 (3)N10—C50—H50A109.0
C108—N4—Fe1126.1 (2)C49—C50—H50A109.0
C107—N4—Fe1125.1 (2)N10—C50—H50B109.0
C2—C1—C6118.6 (3)C49—C50—H50B109.0
C2—C1—C301120.2 (3)H50A—C50—H50B107.8
C6—C1—C301121.0 (3)N9—C51—C52113.0 (3)
C3—C2—C1121.6 (3)N9—C51—H51A109.0
C3—C2—H2A119.2C52—C51—H51A109.0
C1—C2—H2A119.2N9—C51—H51B109.0
C2—C3—C4119.3 (4)C52—C51—H51B109.0
C2—C3—H3A120.4H51A—C51—H51B107.8
C4—C3—H3A120.4O7—C52—C51109.3 (3)
C5—C4—C3120.8 (4)O7—C52—H52A109.8
C5—C4—H4A119.6C51—C52—H52A109.8
C3—C4—H4A119.6O7—C52—H52B109.8
C4—C5—C6120.1 (3)C51—C52—H52B109.8
C4—C5—H5A120.0H52A—C52—H52B108.3
C6—C5—H5A120.0O7—C53—C54110.0 (3)
C5—C6—N5123.1 (3)O7—C53—H53A109.7
C5—C6—C1119.7 (3)C54—C53—H53A109.7
N5—C6—C1117.2 (3)O7—C53—H53B109.7
C8—C7—C12118.7 (3)C54—C53—H53B109.7
C8—C7—C302119.8 (3)H53A—C53—H53B108.2
C12—C7—C302121.4 (3)O8—C54—C53109.6 (3)
C9—C8—C7121.1 (4)O8—C54—H54A109.8
C9—C8—H8A119.5C53—C54—H54A109.8
C7—C8—H8A119.5O8—C54—H54B109.8
C10—C9—C8119.4 (4)C53—C54—H54B109.8
C10—C9—H9A120.3H54A—C54—H54B108.2
C8—C9—H9A120.3O8—C55—C56109.2 (4)
C9—C10—C11121.0 (3)O8—C55—H55A109.8
C9—C10—H10A119.5C56—C55—H55A109.8
C11—C10—H10A119.5O8—C55—H55B109.8
C10—C11—C12119.8 (3)C56—C55—H55B109.8
C10—C11—H11A120.1H55A—C55—H55B108.3
C12—C11—H11A120.1N10—C56—C55113.7 (3)
C11—C12—C7120.0 (3)N10—C56—H56A108.8
C11—C12—N6122.9 (3)C55—C56—H56A108.8
C7—C12—N6117.1 (3)N10—C56—H56B108.8
C14—C13—C18118.3 (4)C55—C56—H56B108.8
C14—C13—C303121.0 (3)H56A—C56—H56B107.7
C18—C13—C303120.7 (3)N9—C57—C58114.0 (3)
C15—C14—C13121.5 (4)N9—C57—H57A108.7
C15—C14—H14A119.3C58—C57—H57A108.7
C13—C14—H14A119.3N9—C57—H57B108.7
C16—C15—C14119.1 (4)C58—C57—H57B108.7
C16—C15—H15A120.5H57A—C57—H57B107.6
C14—C15—H15A120.5O9—C58—C57109.3 (4)
C15—C16—C17121.3 (4)O9—C58—H58A109.8
C15—C16—H16A119.3C57—C58—H58A109.8
C17—C16—H16A119.3O9—C58—H58B109.8
C16—C17—C18119.7 (4)C57—C58—H58B109.8
C16—C17—H17A120.2H58A—C58—H58B108.3
C18—C17—H17A120.2C60—C59—O9111.2 (5)
C17—C18—C13120.1 (4)C60—C59—H59A109.4
C17—C18—N7124.2 (4)O9—C59—H59A109.4
C13—C18—N7115.7 (3)C60—C59—H59B109.4
C20—C19—C24118.6 (3)O9—C59—H59B109.4
C20—C19—C304121.0 (3)H59A—C59—H59B108.0
C24—C19—C304120.3 (3)C59—C60—O10111.1 (5)
C19—C20—C21121.8 (3)C59—C60—H60A109.4
C19—C20—H20A119.1O10—C60—H60A109.4
C21—C20—H20A119.1C59—C60—H60B109.4
C22—C21—C20119.0 (4)O10—C60—H60B109.4
C22—C21—H21A120.5H60A—C60—H60B108.0
C20—C21—H21A120.5O10—C61—C62108.2 (4)
C21—C22—C23120.9 (3)O10—C61—H61A110.1
C21—C22—H22A119.6C62—C61—H61A110.1
C23—C22—H22A119.6O10—C61—H61B110.1
C22—C23—C24120.0 (3)C62—C61—H61B110.1
C22—C23—H23A120.0H61A—C61—H61B108.4
C24—C23—H23A120.0N10—C62—C61114.3 (4)
C23—C24—C19119.8 (3)N10—C62—H62A108.7
C23—C24—N8122.3 (3)C61—C62—H62A108.7
C19—C24—N8117.9 (3)N10—C62—H62B108.7
O1—C25—N5121.4 (4)C61—C62—H62B108.7
O1—C25—C26123.4 (3)H62A—C62—H62B107.6
N5—C25—C26115.1 (3)C51—N9—C45110.7 (3)
C27—C26—C25113.1 (3)C51—N9—C57109.8 (3)
C27—C26—C29109.4 (3)C45—N9—C57109.9 (3)
C25—C26—C29108.2 (3)C51—N9—K1109.6 (2)
C27—C26—C28110.2 (4)C45—N9—K1108.1 (2)
C25—C26—C28106.9 (3)C57—N9—K1108.7 (2)
C29—C26—C28109.0 (3)C62—N10—C56110.4 (3)
C26—C27—H27A109.5C62—N10—C50110.9 (4)
C26—C27—H27B109.5C56—N10—C50109.4 (4)
H27A—C27—H27B109.5C62—N10—K1108.9 (3)
C26—C27—H27C109.5C56—N10—K1108.4 (2)
H27A—C27—H27C109.5C50—N10—K1108.8 (3)
H27B—C27—H27C109.5C46—O5—C47112.2 (3)
C26—C28—H28A109.5C46—O5—K1117.5 (2)
C26—C28—H28B109.5C47—O5—K1111.3 (2)
H28A—C28—H28B109.5C48—O6—C49110.7 (3)
C26—C28—H28C109.5C48—O6—K1115.0 (2)
H28A—C28—H28C109.5C49—O6—K1114.8 (2)
H28B—C28—H28C109.5C52—O7—C53111.4 (3)
C26—C29—H29A109.5C52—O7—K1115.5 (2)
C26—C29—H29B109.5C53—O7—K1112.2 (2)
H29A—C29—H29B109.5C54—O8—C55112.4 (3)
C26—C29—H29C109.5C54—O8—K1112.8 (2)
H29A—C29—H29C109.5C55—O8—K1120.1 (2)
H29B—C29—H29C109.5C58—O9—C59109.2 (4)
O2—C30—N6122.7 (4)C58—O9—K1115.2 (2)
O2—C30—C31122.2 (3)C59—O9—K1113.1 (3)
N6—C30—C31115.1 (3)C61—O10—C60106.9 (4)
C32A—C31—C33A121.8 (9)C61—O10—K1118.1 (3)
C32A—C31—C30104.5 (6)C60—O10—K1112.9 (3)
C33A—C31—C30108.5 (6)C2S—C1S—H1SA109.5
C34—C31—C30110.6 (4)C2S—C1S—H1SB109.5
C34—C31—C32111.5 (5)H1SA—C1S—H1SB109.5
C30—C31—C32110.4 (4)C2S—C1S—H1SC109.5
C34—C31—C33106.7 (5)H1SA—C1S—H1SC109.5
C30—C31—C33114.8 (3)H1SB—C1S—H1SC109.5
C32—C31—C33102.6 (5)C3S—C2S—C1S111.9 (8)
C32A—C31—C34A113.9 (9)C3S—C2S—H2SA109.2
C33A—C31—C34A104.3 (7)C1S—C2S—H2SA109.2
C30—C31—C34A102.0 (5)C3S—C2S—H2SB109.2
C31—C32—H32A109.5C1S—C2S—H2SB109.2
C31—C32—H32B109.5H2SA—C2S—H2SB107.9
H32A—C32—H32B109.5C2S—C3S—C4S120.5 (8)
C31—C32—H32C109.5C2S—C3S—H3SA107.2
H32A—C32—H32C109.5C4S—C3S—H3SA107.2
H32B—C32—H32C109.5C2S—C3S—H3SB107.2
C31—C33—H33A109.5C4S—C3S—H3SB107.2
C31—C33—H33B109.5H3SA—C3S—H3SB106.8
H33A—C33—H33B109.5C3S—C4S—C5S125.0 (7)
C31—C33—H33C109.5C3S—C4S—H4S1106.1
H33A—C33—H33C109.5C5S—C4S—H4S1106.1
H33B—C33—H33C109.5C3S—C4S—H4S2106.1
C31—C34—H34A109.5C5S—C4S—H4S2106.1
C31—C34—H34B109.5H4S1—C4S—H4S2106.3
H34A—C34—H34B109.5C6S—C5S—C4S120.5 (8)
C31—C34—H34C109.5C6S—C5S—H5S1107.2
H34A—C34—H34C109.5C4S—C5S—H5S1107.2
H34B—C34—H34C109.5C6S—C5S—H5S2107.2
C31—C32A—H32D109.5C4S—C5S—H5S2107.2
C31—C32A—H32E109.5H5S1—C5S—H5S2106.8
H32D—C32A—H32E109.5C5S—C6S—H6SA109.5
C31—C32A—H32F109.5C5S—C6S—H6SB109.5
H32D—C32A—H32F109.5H6SA—C6S—H6SB109.5
H32E—C32A—H32F109.5C5S—C6S—H6SC109.5
C31—C33A—H33D109.5H6SA—C6S—H6SC109.5
C31—C33A—H33E109.5H6SB—C6S—H6SC109.5

Experimental details

Crystal data
Chemical formula[K(C18H36N2O6)]·[Fe(C64H64N8O4)Cl]·C6H14
Mr1602.29
Crystal system, space groupTriclinic, P1
Temperature (K)120
a, b, c (Å)13.0174 (4), 14.3273 (8), 24.1557 (13)
α, β, γ (°)80.946 (4), 79.029 (4), 87.039 (3)
V3)4366.6 (4)
Z2
Radiation typeMo Kα
µ (mm1)0.31
Crystal size (mm)0.20 × 0.15 × 0.15
Data collection
DiffractometerAgilent Xcalibur Gemini
diffractometer with Eos detector
Absorption correctionMulti-scan
(CrysAlis PRO; Agilent, 2011)
Tmin, Tmax0.968, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
35844, 18570, 11295
Rint0.040
(sin θ/λ)max1)0.672
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.069, 0.168, 1.02
No. of reflections18570
No. of parameters1029
No. of restraints108
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.96, 0.39

Computer programs: CrysAlis PRO (Agilent, 2011), SHELXS97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), SHELXL2014 (Sheldrick, 2015) and publCIF (Westrip, 2010).

 

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