Download citation
Download citation
link to html
A detailed description of the procedures utilized in the non-routine X-ray single-crystal structural determination and refinement of a pseudo-merohedrally twinned crystal of an Fe/Ni organometallic complex is presented. It illustrates to the practitioners of crystallography how to properly handle such cases and describes the logic and concrete steps necessary to account for the twinning, pseudo-symmetry and atomic positional disorder.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768112002728/ps5014sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112002728/ps5014Isup2.hkl
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768112002728/ps5014sup3.pdf
Output from XPREP

CCDC reference: 879420

Refinement top

All H-atoms were placed in idealized locations and refined as riding with appropriate thermal displacement coefficients Uiso(H) = 1.2 or 1.5 times Ueq(bearing atom).

Computing details top

Data collection: APEX2 Ver. 2.1-4 (Bruker-AXS, 2007); cell refinement: SAINT Ver. 7.24A (Bruker-AXS, 2007); data reduction: SAINT Ver. 7.24A; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
Figure 1. Molecular structure of (I). The thermal ellipsoids are shown at 50% probability level.
(I) top
Crystal data top
C44H42Br5Fe3N6NiO4F(000) = 2644
Mr = 1344.65Dx = 1.895 Mg m3
Monoclinic, CcCu Kα radiation, λ = 1.54178 Å
Hall symbol: C -2ycCell parameters from 999 reflections
a = 15.2181 (3) Åθ = 3.1–72.1°
b = 22.0080 (3) ŵ = 13.07 mm1
c = 16.0005 (3) ÅT = 100 K
β = 118.393 (2)°Block, red
V = 4714.25 (14) Å30.19 × 0.11 × 0.09 mm
Z = 4
Data collection top
Bruker SMART APEX2 area detector
diffractometer
8033 independent reflections
Radiation source: fine-focus sealed tube7903 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
0.50° ω and 0.5 ° ϕ scansθmax = 72.1°, θmin = 3.1°
Absorption correction: analytical
SADABS (Bruker-AXS, 2007)
h = 1718
Tmin = 0.186, Tmax = 0.376k = 2725
35920 measured reflectionsl = 1918
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.078 w = 1/[σ2(Fo2) + (0.0581P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
8033 reflectionsΔρmax = 0.70 e Å3
599 parametersΔρmin = 0.66 e Å3
4 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.008 (4)
Crystal data top
C44H42Br5Fe3N6NiO4V = 4714.25 (14) Å3
Mr = 1344.65Z = 4
Monoclinic, CcCu Kα radiation
a = 15.2181 (3) ŵ = 13.07 mm1
b = 22.0080 (3) ÅT = 100 K
c = 16.0005 (3) Å0.19 × 0.11 × 0.09 mm
β = 118.393 (2)°
Data collection top
Bruker SMART APEX2 area detector
diffractometer
8033 independent reflections
Absorption correction: analytical
SADABS (Bruker-AXS, 2007)
7903 reflections with I > 2σ(I)
Tmin = 0.186, Tmax = 0.376Rint = 0.031
35920 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.078Δρmax = 0.70 e Å3
S = 1.05Δρmin = 0.66 e Å3
8033 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
599 parametersAbsolute structure parameter: 0.008 (4)
4 restraints
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)
Br10.29003 (5)0.62030 (3)0.66511 (4)0.02583 (15)
Ni10.20175 (8)0.62397 (5)0.49182 (7)0.01679 (19)
Fe10.07292 (7)0.58052 (5)0.59258 (7)0.0220 (2)
Fe20.58354 (7)0.67777 (5)0.59805 (8)0.0238 (2)
O10.0385 (4)0.3437 (2)0.4396 (5)0.0395 (13)
O20.1836 (4)0.3649 (2)0.4416 (5)0.0402 (14)
O30.2928 (4)0.9093 (2)0.4472 (4)0.0357 (12)
O40.1420 (4)0.8748 (2)0.4217 (5)0.0406 (15)
N10.2374 (4)0.5853 (2)0.3956 (4)0.0207 (11)
N20.1603 (4)0.4908 (2)0.4768 (4)0.0209 (11)
N30.1236 (4)0.5445 (2)0.4860 (4)0.0185 (10)
N40.0732 (4)0.6635 (2)0.3887 (4)0.0186 (10)
N50.2240 (4)0.7578 (2)0.4837 (4)0.0205 (11)
N60.2764 (4)0.7055 (2)0.4968 (4)0.0179 (10)
C10.2373 (5)0.6184 (3)0.3235 (5)0.0261 (15)
H10.22090.66030.31870.031*
C20.2597 (6)0.5933 (3)0.2586 (5)0.0303 (16)
H20.26030.61800.21020.036*
C30.2817 (6)0.5323 (3)0.2623 (6)0.0349 (17)
H30.29860.51450.21780.042*
C40.2784 (5)0.4988 (3)0.3316 (5)0.0273 (15)
H40.29100.45640.33480.033*
C50.2566 (4)0.5260 (3)0.3987 (4)0.0179 (13)
C60.2589 (5)0.4895 (3)0.4797 (5)0.0177 (12)
H6A0.27740.44700.47520.021*
H6B0.31020.50650.54090.021*
C70.0952 (5)0.4448 (3)0.4631 (5)0.0224 (14)
C80.1034 (5)0.3791 (3)0.4476 (5)0.0231 (14)
C90.1974 (7)0.3010 (3)0.4233 (6)0.043 (2)
H9A0.15010.27470.43280.051*
H9B0.26630.28760.46760.051*
C100.1785 (7)0.2960 (4)0.3214 (5)0.050 (2)
H10A0.11040.30970.27810.075*
H10B0.18650.25370.30730.075*
H10C0.22640.32160.31300.075*
C110.0135 (5)0.4709 (3)0.4681 (5)0.0202 (13)
H110.04440.45070.46210.024*
C120.0353 (5)0.5327 (3)0.4837 (5)0.0212 (13)
C130.0264 (5)0.5798 (3)0.4929 (5)0.0233 (13)
C140.1331 (5)0.5782 (4)0.4482 (5)0.0275 (15)
H140.17490.54730.40700.033*
C150.1652 (6)0.6317 (4)0.4767 (7)0.039 (2)
H150.23240.64290.45730.047*
C160.0794 (6)0.6652 (3)0.5390 (6)0.0344 (18)
H160.07970.70250.56860.041*
C170.0062 (6)0.6345 (3)0.5501 (6)0.0281 (15)
H170.07330.64730.58810.034*
C180.0213 (6)0.5606 (4)0.7314 (5)0.0311 (16)
H180.08760.57530.76790.037*
C190.0077 (6)0.5074 (3)0.6772 (5)0.0339 (16)
H190.03610.47970.66990.041*
C200.1128 (7)0.5014 (4)0.6349 (5)0.0377 (18)
H200.15200.46900.59530.045*
C210.1484 (5)0.5529 (4)0.6630 (5)0.0311 (16)
H210.21650.56140.64450.037*
C220.0685 (7)0.5887 (4)0.7213 (6)0.0380 (18)
H220.07200.62580.75010.046*
C230.0101 (5)0.6323 (3)0.3113 (5)0.0238 (14)
H230.02390.59060.30710.029*
C240.0740 (5)0.6576 (3)0.2373 (5)0.0280 (15)
H240.11520.63460.18210.034*
C250.0966 (5)0.7178 (3)0.2460 (5)0.0267 (14)
H250.15530.73640.19790.032*
C260.0307 (5)0.7508 (3)0.3276 (5)0.0246 (14)
H260.04400.79210.33480.030*
C270.0531 (4)0.7224 (3)0.3965 (5)0.0194 (13)
C280.1286 (5)0.7547 (3)0.4849 (5)0.0223 (13)
H28A0.10480.79620.48720.027*
H28B0.13710.73240.54210.027*
C290.2752 (5)0.8057 (3)0.4748 (5)0.0206 (12)
C300.2389 (6)0.8699 (3)0.4486 (6)0.0281 (16)
C310.0928 (8)0.9307 (4)0.3692 (7)0.050 (2)
H31A0.02060.92350.32720.060*
H31B0.12320.94440.32990.060*
C320.1084 (10)0.9774 (4)0.4443 (7)0.070 (3)
H32A0.10170.95800.49610.106*
H32B0.05821.00960.41620.106*
H32C0.17530.99510.46930.106*
C330.3627 (5)0.7837 (3)0.4824 (5)0.0241 (13)
H330.41410.80640.47920.029*
C340.3610 (4)0.7204 (3)0.4961 (5)0.0204 (13)
C350.4356 (5)0.6761 (3)0.5031 (5)0.0243 (14)
C360.4924 (5)0.6820 (4)0.4538 (5)0.0306 (16)
H360.48850.71410.41240.037*
C370.5568 (6)0.6298 (3)0.4792 (6)0.0305 (16)
H370.60420.62150.45800.037*
C380.5377 (6)0.5926 (3)0.5413 (7)0.0380 (19)
H380.56950.55500.56760.046*
C390.4625 (6)0.6211 (3)0.5579 (6)0.0309 (16)
H390.43590.60660.59710.037*
C400.6302 (6)0.6998 (5)0.7369 (6)0.044 (2)
H400.59970.68750.77390.053*
C410.6084 (6)0.7525 (4)0.6815 (6)0.041 (2)
H410.55960.78200.67420.050*
C420.6707 (6)0.7548 (4)0.6383 (6)0.0374 (18)
H420.67130.78600.59760.045*
C430.7316 (6)0.7029 (4)0.6660 (6)0.0378 (18)
H430.78040.69300.64710.045*
C440.7076 (6)0.6672 (4)0.7275 (5)0.0386 (19)
H440.73690.62960.75640.046*
Br20.43364 (6)0.36557 (4)0.47749 (6)0.0455 (2)
Br30.49508 (8)0.47066 (4)0.68743 (8)0.0435 (3)0.852 (2)
Br40.44443 (8)0.30422 (4)0.70425 (8)0.0384 (2)0.852 (2)
Br50.68356 (7)0.35652 (4)0.69552 (7)0.0371 (2)0.852 (2)
Br3A0.4315 (11)0.3893 (5)0.7007 (12)0.102 (4)0.148 (2)
Br4A0.6172 (13)0.2750 (6)0.6963 (15)0.125 (6)0.148 (2)
Br5A0.6694 (7)0.4413 (6)0.6917 (9)0.102 (4)0.148 (2)
Fe30.51627 (9)0.37325 (6)0.64296 (8)0.0333 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0288 (4)0.0276 (3)0.0197 (3)0.0068 (3)0.0105 (3)0.0017 (3)
Ni10.0160 (5)0.0167 (4)0.0183 (5)0.0022 (4)0.0087 (5)0.0014 (5)
Fe10.0189 (5)0.0286 (5)0.0214 (6)0.0027 (4)0.0120 (5)0.0019 (4)
Fe20.0190 (5)0.0317 (5)0.0237 (6)0.0048 (4)0.0125 (5)0.0013 (5)
O10.037 (3)0.029 (3)0.060 (4)0.010 (2)0.029 (3)0.006 (2)
O20.044 (3)0.021 (2)0.070 (4)0.006 (2)0.039 (3)0.008 (2)
O30.035 (3)0.018 (2)0.053 (3)0.003 (2)0.020 (3)0.004 (2)
O40.034 (3)0.026 (2)0.063 (4)0.012 (2)0.024 (3)0.024 (3)
N10.019 (3)0.029 (3)0.021 (3)0.004 (2)0.015 (2)0.002 (2)
N20.020 (3)0.024 (3)0.022 (3)0.002 (2)0.012 (2)0.001 (2)
N30.024 (3)0.011 (2)0.025 (3)0.0046 (19)0.015 (2)0.002 (2)
N40.020 (3)0.018 (2)0.019 (3)0.003 (2)0.011 (2)0.001 (2)
N50.018 (3)0.021 (3)0.018 (3)0.001 (2)0.005 (2)0.001 (2)
N60.018 (2)0.018 (2)0.018 (3)0.002 (2)0.009 (2)0.003 (2)
C10.030 (4)0.020 (3)0.035 (4)0.004 (3)0.020 (3)0.005 (3)
C20.046 (4)0.026 (3)0.026 (4)0.008 (3)0.024 (4)0.003 (3)
C30.035 (4)0.033 (4)0.046 (5)0.008 (3)0.026 (4)0.007 (3)
C40.032 (4)0.026 (3)0.032 (4)0.002 (3)0.022 (3)0.009 (3)
C50.014 (3)0.018 (3)0.020 (3)0.002 (2)0.006 (2)0.001 (2)
C60.017 (3)0.021 (3)0.020 (3)0.001 (2)0.012 (3)0.003 (2)
C70.023 (3)0.028 (3)0.015 (3)0.004 (2)0.008 (3)0.002 (3)
C80.025 (3)0.022 (3)0.025 (4)0.001 (3)0.014 (3)0.003 (2)
C90.055 (5)0.016 (3)0.078 (6)0.002 (3)0.049 (5)0.005 (4)
C100.057 (5)0.040 (5)0.060 (6)0.010 (4)0.034 (5)0.014 (4)
C110.019 (3)0.027 (3)0.022 (3)0.005 (2)0.016 (3)0.000 (3)
C120.020 (3)0.023 (3)0.018 (3)0.005 (2)0.007 (3)0.001 (3)
C130.030 (3)0.033 (3)0.016 (3)0.000 (3)0.018 (3)0.004 (3)
C140.011 (3)0.046 (4)0.022 (3)0.001 (3)0.005 (3)0.008 (3)
C150.028 (4)0.058 (5)0.042 (5)0.026 (4)0.024 (4)0.023 (4)
C160.046 (5)0.030 (4)0.033 (4)0.006 (3)0.023 (4)0.001 (3)
C170.035 (4)0.028 (3)0.035 (4)0.000 (3)0.028 (3)0.004 (3)
C180.025 (4)0.047 (4)0.020 (3)0.013 (3)0.010 (3)0.010 (3)
C190.039 (4)0.038 (4)0.025 (4)0.014 (3)0.016 (3)0.015 (3)
C200.045 (5)0.044 (4)0.027 (4)0.010 (4)0.019 (4)0.012 (3)
C210.023 (4)0.050 (4)0.026 (4)0.005 (3)0.016 (3)0.009 (3)
C220.044 (5)0.048 (4)0.027 (4)0.010 (4)0.021 (4)0.001 (3)
C230.020 (3)0.027 (3)0.024 (3)0.001 (2)0.010 (3)0.004 (3)
C240.032 (4)0.028 (3)0.017 (3)0.004 (3)0.006 (3)0.005 (3)
C250.019 (3)0.035 (4)0.021 (3)0.004 (3)0.005 (3)0.008 (3)
C260.020 (3)0.022 (3)0.035 (4)0.005 (3)0.016 (3)0.006 (3)
C270.017 (3)0.024 (3)0.023 (3)0.003 (2)0.014 (3)0.001 (2)
C280.021 (3)0.014 (3)0.033 (4)0.001 (2)0.014 (3)0.008 (3)
C290.017 (3)0.022 (3)0.019 (3)0.006 (2)0.005 (3)0.002 (3)
C300.030 (4)0.030 (4)0.026 (4)0.001 (3)0.016 (3)0.000 (3)
C310.048 (5)0.041 (4)0.066 (6)0.017 (4)0.031 (5)0.015 (4)
C320.080 (8)0.059 (6)0.068 (7)0.008 (6)0.031 (6)0.015 (5)
C330.025 (3)0.023 (3)0.026 (3)0.002 (3)0.013 (3)0.004 (3)
C340.013 (3)0.024 (3)0.023 (3)0.001 (2)0.008 (2)0.004 (2)
C350.013 (3)0.032 (3)0.027 (3)0.001 (2)0.009 (3)0.004 (3)
C360.025 (4)0.040 (4)0.021 (4)0.002 (3)0.005 (3)0.004 (3)
C370.031 (4)0.042 (4)0.025 (4)0.006 (3)0.019 (3)0.010 (3)
C380.026 (4)0.027 (3)0.057 (6)0.004 (3)0.017 (4)0.011 (3)
C390.024 (3)0.032 (3)0.048 (5)0.007 (3)0.026 (4)0.004 (3)
C400.029 (4)0.071 (6)0.030 (4)0.007 (4)0.013 (3)0.000 (4)
C410.029 (4)0.053 (5)0.032 (4)0.011 (3)0.007 (3)0.017 (4)
C420.027 (4)0.035 (4)0.042 (4)0.006 (3)0.009 (3)0.008 (3)
C430.017 (4)0.056 (5)0.030 (4)0.003 (3)0.003 (3)0.002 (4)
C440.024 (4)0.063 (5)0.021 (4)0.015 (4)0.005 (3)0.007 (3)
Br20.0361 (5)0.0623 (6)0.0334 (4)0.0137 (4)0.0126 (4)0.0062 (4)
Br30.0405 (5)0.0342 (5)0.0392 (5)0.0055 (4)0.0054 (4)0.0105 (4)
Br40.0439 (5)0.0414 (5)0.0418 (5)0.0085 (4)0.0300 (5)0.0053 (4)
Br50.0197 (4)0.0515 (5)0.0361 (5)0.0053 (4)0.0099 (4)0.0034 (5)
Br3A0.100 (8)0.130 (8)0.122 (10)0.023 (7)0.091 (9)0.026 (8)
Br4A0.164 (15)0.101 (9)0.162 (14)0.003 (8)0.119 (13)0.032 (9)
Br5A0.055 (5)0.147 (9)0.069 (7)0.013 (6)0.002 (5)0.042 (7)
Fe30.0318 (7)0.0357 (5)0.0283 (6)0.0002 (5)0.0110 (5)0.0022 (5)
Geometric parameters (Å, º) top
Br1—Ni12.4407 (10)C13—C171.450 (10)
Ni1—N12.047 (5)C14—C151.431 (11)
Ni1—N42.058 (5)C14—H140.9500
Ni1—N32.092 (5)C15—C161.415 (13)
Ni1—N62.105 (5)C15—H150.9500
Fe1—C172.026 (7)C16—C171.401 (10)
Fe1—C132.030 (6)C16—H160.9500
Fe1—C192.032 (7)C17—H170.9500
Fe1—C162.033 (8)C18—C191.398 (11)
Fe1—C222.037 (8)C18—C221.438 (11)
Fe1—C182.038 (7)C18—H180.9500
Fe1—C142.042 (7)C19—C201.416 (12)
Fe1—C212.047 (7)C19—H190.9500
Fe1—C152.050 (8)C20—C211.420 (12)
Fe1—C202.062 (7)C20—H200.9500
Fe2—C352.031 (7)C21—C221.376 (12)
Fe2—C412.038 (8)C21—H210.9500
Fe2—C372.040 (7)C22—H220.9500
Fe2—C402.042 (9)C23—C241.381 (10)
Fe2—C442.047 (7)C23—H230.9500
Fe2—C362.053 (7)C24—C251.394 (10)
Fe2—C382.055 (8)C24—H240.9500
Fe2—C432.057 (8)C25—C261.411 (10)
Fe2—C392.058 (7)C25—H250.9500
Fe2—C422.058 (8)C26—C271.376 (9)
O1—C81.217 (9)C26—H260.9500
O2—C81.307 (9)C27—C281.510 (9)
O2—C91.473 (8)C28—H28A0.9900
O3—C301.201 (9)C28—H28B0.9900
O4—C301.330 (9)C29—C331.366 (10)
O4—C311.475 (9)C29—C301.503 (9)
N1—C51.331 (8)C31—C321.513 (4)
N1—C11.363 (9)C31—H31A0.9900
N2—N31.346 (7)C31—H31B0.9900
N2—C71.360 (9)C32—H32A0.9800
N2—C61.480 (8)C32—H32B0.9800
N3—C121.351 (8)C32—H32C0.9800
N4—C231.341 (9)C33—C341.413 (9)
N4—C271.353 (8)C33—H330.9500
N5—C291.356 (8)C34—C351.459 (9)
N5—N61.358 (7)C35—C361.427 (10)
N5—C281.464 (8)C35—C391.435 (10)
N6—C341.335 (8)C36—C371.438 (10)
C1—C21.356 (10)C36—H360.9500
C1—H10.9500C37—C381.420 (12)
C2—C31.378 (10)C37—H370.9500
C2—H20.9500C38—C391.436 (10)
C3—C41.353 (11)C38—H380.9500
C3—H30.9500C39—H390.9500
C4—C51.400 (9)C40—C411.401 (13)
C4—H40.9500C40—C441.445 (12)
C5—C61.510 (9)C40—H400.9500
C6—H6A0.9900C41—C421.416 (13)
C6—H6B0.9900C41—H410.9500
C7—C111.405 (10)C42—C431.402 (12)
C7—C81.482 (9)C42—H420.9500
C9—C101.519 (4)C43—C441.436 (12)
C9—H9A0.9900C43—H430.9500
C9—H9B0.9900C44—H440.9500
C10—H10A0.9800Br2—Fe32.3352 (13)
C10—H10B0.9800Br3—Fe32.3290 (16)
C10—H10C0.9800Br4—Fe32.3419 (16)
C11—C121.395 (9)Br5—Fe32.2995 (16)
C11—H110.9500Br3A—Fe31.943 (10)
C12—C131.451 (9)Br4A—Fe32.553 (15)
C13—C141.430 (9)Br5A—Fe32.560 (11)
N1—Ni1—N493.66 (19)Fe1—C14—H14126.4
N1—Ni1—N388.1 (2)C16—C15—C14108.2 (6)
N4—Ni1—N390.8 (2)C16—C15—Fe169.1 (5)
N1—Ni1—N693.0 (2)C14—C15—Fe169.2 (4)
N4—Ni1—N687.7 (2)C16—C15—H15125.9
N3—Ni1—N6178.2 (2)C14—C15—H15125.9
N1—Ni1—Br1129.90 (17)Fe1—C15—H15127.3
N4—Ni1—Br1136.43 (16)C17—C16—C15109.3 (6)
N3—Ni1—Br190.97 (16)C17—C16—Fe169.5 (4)
N6—Ni1—Br189.41 (15)C15—C16—Fe170.3 (4)
C17—Fe1—C1341.9 (3)C17—C16—H16125.4
C17—Fe1—C19120.5 (3)C15—C16—H16125.4
C13—Fe1—C19105.9 (3)Fe1—C16—H16126.3
C17—Fe1—C1640.4 (3)C16—C17—C13107.6 (7)
C13—Fe1—C1668.9 (3)C16—C17—Fe170.1 (4)
C19—Fe1—C16156.4 (3)C13—C17—Fe169.2 (4)
C17—Fe1—C22123.3 (4)C16—C17—H17126.2
C13—Fe1—C22159.9 (3)C13—C17—H17126.2
C19—Fe1—C2268.0 (3)Fe1—C17—H17126.0
C16—Fe1—C22108.5 (3)C19—C18—C22106.8 (7)
C17—Fe1—C18105.6 (3)C19—C18—Fe169.7 (4)
C13—Fe1—C18121.8 (3)C22—C18—Fe169.3 (4)
C19—Fe1—C1840.2 (3)C19—C18—H18126.6
C16—Fe1—C18121.6 (3)C22—C18—H18126.6
C22—Fe1—C1841.3 (3)Fe1—C18—H18126.0
C17—Fe1—C1469.7 (3)C18—C19—C20109.1 (7)
C13—Fe1—C1441.1 (3)C18—C19—Fe170.1 (4)
C19—Fe1—C14123.2 (3)C20—C19—Fe170.9 (4)
C16—Fe1—C1468.9 (3)C18—C19—H19125.5
C22—Fe1—C14158.2 (3)C20—C19—H19125.5
C18—Fe1—C14158.8 (3)Fe1—C19—H19125.1
C17—Fe1—C21159.7 (3)C19—C20—C21106.8 (7)
C13—Fe1—C21158.0 (3)C19—C20—Fe168.6 (4)
C19—Fe1—C2167.8 (3)C21—C20—Fe169.2 (4)
C16—Fe1—C21125.2 (3)C19—C20—H20126.6
C22—Fe1—C2139.4 (3)C21—C20—H20126.6
C18—Fe1—C2168.0 (3)Fe1—C20—H20127.1
C14—Fe1—C21123.3 (3)C22—C21—C20109.0 (7)
C17—Fe1—C1568.6 (3)C22—C21—Fe169.9 (4)
C13—Fe1—C1568.8 (3)C20—C21—Fe170.4 (4)
C19—Fe1—C15160.9 (4)C22—C21—H21125.5
C16—Fe1—C1540.5 (4)C20—C21—H21125.5
C22—Fe1—C15123.0 (3)Fe1—C21—H21125.8
C18—Fe1—C15158.2 (3)C21—C22—C18108.5 (7)
C14—Fe1—C1541.0 (3)C21—C22—Fe170.7 (4)
C21—Fe1—C15109.8 (3)C18—C22—Fe169.4 (4)
C17—Fe1—C20157.0 (3)C21—C22—H22125.8
C13—Fe1—C20121.2 (3)C18—C22—H22125.8
C19—Fe1—C2040.5 (4)Fe1—C22—H22125.7
C16—Fe1—C20161.7 (4)N4—C23—C24123.3 (6)
C22—Fe1—C2067.4 (3)N4—C23—H23118.3
C18—Fe1—C2068.0 (3)C24—C23—H23118.3
C14—Fe1—C20107.8 (3)C23—C24—C25118.1 (6)
C21—Fe1—C2040.4 (3)C23—C24—H24121.0
C15—Fe1—C20125.4 (4)C25—C24—H24121.0
C35—Fe2—C41107.4 (3)C24—C25—C26118.8 (6)
C35—Fe2—C3768.6 (3)C24—C25—H25120.6
C41—Fe2—C37157.2 (3)C26—C25—H25120.6
C35—Fe2—C40120.4 (3)C27—C26—C25119.2 (6)
C41—Fe2—C4040.2 (4)C27—C26—H26120.4
C37—Fe2—C40161.5 (4)C25—C26—H26120.4
C35—Fe2—C44156.3 (3)N4—C27—C26121.7 (6)
C41—Fe2—C4468.5 (3)N4—C27—C28115.6 (6)
C37—Fe2—C44124.3 (3)C26—C27—C28122.6 (6)
C40—Fe2—C4441.4 (3)N5—C28—C27109.1 (5)
C35—Fe2—C3640.9 (3)N5—C28—H28A109.9
C41—Fe2—C36121.0 (3)C27—C28—H28A109.9
C37—Fe2—C3641.1 (3)N5—C28—H28B109.9
C40—Fe2—C36155.7 (3)C27—C28—H28B109.9
C44—Fe2—C36161.4 (3)H28A—C28—H28B108.3
C35—Fe2—C3868.3 (3)N5—C29—C33107.5 (5)
C41—Fe2—C38160.8 (4)N5—C29—C30127.3 (6)
C37—Fe2—C3840.6 (3)C33—C29—C30124.8 (6)
C40—Fe2—C38124.5 (4)O3—C30—O4126.6 (7)
C44—Fe2—C38107.4 (3)O3—C30—C29121.4 (6)
C36—Fe2—C3868.8 (4)O4—C30—C29111.8 (6)
C35—Fe2—C43161.0 (3)O4—C31—C32105.6 (8)
C41—Fe2—C4367.8 (3)O4—C31—H31A110.6
C37—Fe2—C43108.3 (3)C32—C31—H31A110.6
C40—Fe2—C4368.6 (3)O4—C31—H31B110.6
C44—Fe2—C4340.9 (3)C32—C31—H31B110.6
C36—Fe2—C43124.5 (3)H31A—C31—H31B108.7
C38—Fe2—C43122.3 (3)C29—C33—C34105.9 (6)
C35—Fe2—C3941.1 (3)C29—C33—H33127.0
C41—Fe2—C39123.6 (3)C34—C33—H33127.0
C37—Fe2—C3969.1 (3)N6—C34—C33109.3 (5)
C40—Fe2—C39106.3 (4)N6—C34—C35123.7 (6)
C44—Fe2—C39120.4 (4)C33—C34—C35126.9 (6)
C36—Fe2—C3969.5 (3)C36—C35—C39110.0 (6)
C38—Fe2—C3940.9 (3)C36—C35—C34123.4 (6)
C43—Fe2—C39157.0 (3)C39—C35—C34126.6 (6)
C35—Fe2—C42124.7 (3)C36—C35—Fe270.4 (4)
C41—Fe2—C4240.5 (4)C39—C35—Fe270.4 (4)
C37—Fe2—C42122.1 (3)C34—C35—Fe2126.2 (5)
C40—Fe2—C4268.0 (4)C35—C36—C37106.3 (7)
C44—Fe2—C4268.2 (3)C35—C36—Fe268.7 (4)
C36—Fe2—C42107.7 (3)C37—C36—Fe268.9 (4)
C38—Fe2—C42157.3 (3)C35—C36—H36126.8
C43—Fe2—C4239.8 (3)C37—C36—H36126.8
C39—Fe2—C42160.9 (3)Fe2—C36—H36127.0
C8—O2—C9118.0 (6)C38—C37—C36108.7 (6)
C30—O4—C31115.9 (6)C38—C37—Fe270.3 (4)
C5—N1—C1117.9 (5)C36—C37—Fe269.9 (4)
C5—N1—Ni1120.7 (4)C38—C37—H37125.6
C1—N1—Ni1121.3 (4)C36—C37—H37125.6
N3—N2—C7111.2 (5)Fe2—C37—H37125.7
N3—N2—C6118.8 (5)C37—C38—C39108.8 (7)
C7—N2—C6130.0 (6)C37—C38—Fe269.1 (4)
N2—N3—C12106.7 (5)C39—C38—Fe269.7 (4)
N2—N3—Ni1118.8 (4)C37—C38—H38125.6
C12—N3—Ni1134.3 (4)C39—C38—H38125.6
C23—N4—C27118.9 (6)Fe2—C38—H38127.2
C23—N4—Ni1120.9 (4)C35—C39—C38106.1 (7)
C27—N4—Ni1120.1 (4)C35—C39—Fe268.5 (4)
C29—N5—N6110.5 (5)C38—C39—Fe269.5 (4)
C29—N5—C28131.4 (5)C35—C39—H39127.0
N6—N5—C28118.1 (5)C38—C39—H39127.0
C34—N6—N5106.8 (5)Fe2—C39—H39126.7
C34—N6—Ni1135.6 (4)C41—C40—C44107.8 (8)
N5—N6—Ni1116.8 (4)C41—C40—Fe269.7 (5)
C2—C1—N1122.1 (6)C44—C40—Fe269.5 (5)
C2—C1—H1119.0C41—C40—H40126.1
N1—C1—H1119.0C44—C40—H40126.1
C1—C2—C3120.5 (7)Fe2—C40—H40126.2
C1—C2—H2119.7C40—C41—C42108.9 (7)
C3—C2—H2119.7C40—C41—Fe270.1 (5)
C4—C3—C2117.6 (7)C42—C41—Fe270.5 (4)
C4—C3—H3121.2C40—C41—H41125.5
C2—C3—H3121.2C42—C41—H41125.5
C3—C4—C5120.7 (6)Fe2—C41—H41125.4
C3—C4—H4119.7C43—C42—C41108.2 (8)
C5—C4—H4119.7C43—C42—Fe270.1 (4)
N1—C5—C4121.1 (6)C41—C42—Fe269.0 (5)
N1—C5—C6118.0 (6)C43—C42—H42125.9
C4—C5—C6120.8 (5)C41—C42—H42125.9
N2—C6—C5110.7 (5)Fe2—C42—H42126.6
N2—C6—H6A109.5C42—C43—C44108.5 (8)
C5—C6—H6A109.5C42—C43—Fe270.1 (4)
N2—C6—H6B109.5C44—C43—Fe269.1 (4)
C5—C6—H6B109.5C42—C43—H43125.8
H6A—C6—H6B108.1C44—C43—H43125.8
N2—C7—C11106.5 (6)Fe2—C43—H43126.6
N2—C7—C8129.7 (6)C43—C44—C40106.6 (7)
C11—C7—C8123.8 (6)C43—C44—Fe269.9 (4)
O1—C8—O2125.4 (6)C40—C44—Fe269.1 (5)
O1—C8—C7120.9 (6)C43—C44—H44126.7
O2—C8—C7113.7 (6)C40—C44—H44126.7
O2—C9—C10108.0 (6)Fe2—C44—H44125.8
O2—C9—H9A110.1Br3A—Fe3—Br5136.5 (5)
C10—C9—H9A110.1Br3A—Fe3—Br357.9 (4)
O2—C9—H9B110.1Br5—Fe3—Br3109.01 (6)
C10—C9—H9B110.1Br3A—Fe3—Br2115.5 (5)
H9A—C9—H9B108.4Br5—Fe3—Br2107.98 (6)
C12—C11—C7105.5 (6)Br3—Fe3—Br2109.57 (6)
C12—C11—H11127.2Br3A—Fe3—Br451.0 (3)
C7—C11—H11127.2Br5—Fe3—Br4113.52 (7)
N3—C12—C11109.9 (6)Br3—Fe3—Br4108.00 (7)
N3—C12—C13122.9 (6)Br2—Fe3—Br4108.71 (6)
C11—C12—C13127.1 (6)Br3A—Fe3—Br4A115.1 (5)
C14—C13—C17107.6 (6)Br5—Fe3—Br4A49.9 (3)
C14—C13—C12124.5 (7)Br3—Fe3—Br4A145.7 (4)
C17—C13—C12127.8 (6)Br2—Fe3—Br4A103.4 (4)
C14—C13—Fe169.9 (4)Br4—Fe3—Br4A68.7 (3)
C17—C13—Fe168.9 (4)Br3A—Fe3—Br5A117.6 (6)
C12—C13—Fe1124.7 (5)Br5—Fe3—Br5A45.0 (3)
C13—C14—C15107.4 (7)Br3—Fe3—Br5A66.9 (3)
C13—C14—Fe169.0 (4)Br2—Fe3—Br5A108.0 (3)
C15—C14—Fe169.8 (5)Br4—Fe3—Br5A142.2 (3)
C13—C14—H14126.3Br4A—Fe3—Br5A94.5 (4)
C15—C14—H14126.3
N4—Ni1—N1—C5127.2 (5)Fe1—C18—C22—C2160.2 (6)
N3—Ni1—N1—C536.5 (5)C19—C18—C22—Fe159.9 (5)
N6—Ni1—N1—C5144.9 (5)C17—Fe1—C22—C21165.6 (4)
Br1—Ni1—N1—C553.2 (5)C13—Fe1—C22—C21157.4 (8)
N4—Ni1—N1—C149.3 (6)C19—Fe1—C22—C2181.4 (5)
N3—Ni1—N1—C1140.0 (5)C16—Fe1—C22—C21123.4 (5)
N6—Ni1—N1—C138.6 (5)C18—Fe1—C22—C21119.3 (7)
Br1—Ni1—N1—C1130.3 (5)C14—Fe1—C22—C2144.2 (11)
C7—N2—N3—C123.5 (8)C15—Fe1—C22—C2181.0 (6)
C6—N2—N3—C12178.3 (6)C20—Fe1—C22—C2137.5 (5)
C7—N2—N3—Ni1172.9 (4)C17—Fe1—C22—C1875.1 (6)
C6—N2—N3—Ni15.3 (8)C13—Fe1—C22—C1838.1 (11)
N1—Ni1—N3—N236.3 (5)C19—Fe1—C22—C1837.9 (5)
N4—Ni1—N3—N2130.0 (5)C16—Fe1—C22—C18117.2 (5)
Br1—Ni1—N3—N293.5 (5)C14—Fe1—C22—C18163.5 (8)
N1—Ni1—N3—C12138.8 (7)C21—Fe1—C22—C18119.3 (7)
N4—Ni1—N3—C1245.1 (7)C15—Fe1—C22—C18159.6 (5)
Br1—Ni1—N3—C1291.3 (7)C20—Fe1—C22—C1881.8 (5)
N1—Ni1—N4—C2344.4 (5)C27—N4—C23—C241.5 (10)
N3—Ni1—N4—C2343.8 (5)Ni1—N4—C23—C24176.0 (5)
N6—Ni1—N4—C23137.2 (5)N4—C23—C24—C253.2 (11)
Br1—Ni1—N4—C23136.1 (4)C23—C24—C25—C262.7 (11)
N1—Ni1—N4—C27133.1 (5)C24—C25—C26—C270.8 (10)
N3—Ni1—N4—C27138.7 (5)C23—N4—C27—C260.6 (9)
N6—Ni1—N4—C2740.2 (5)Ni1—N4—C27—C26178.1 (5)
Br1—Ni1—N4—C2746.5 (6)C23—N4—C27—C28179.0 (6)
C29—N5—N6—C340.0 (7)Ni1—N4—C27—C281.5 (7)
C28—N5—N6—C34177.9 (6)C25—C26—C27—N40.9 (10)
C29—N5—N6—Ni1171.1 (4)C25—C26—C27—C28178.7 (6)
C28—N5—N6—Ni111.0 (7)C29—N5—C28—C27112.3 (7)
N1—Ni1—N6—C3438.9 (7)N6—N5—C28—C2770.4 (7)
N4—Ni1—N6—C34132.4 (7)N4—C27—C28—N564.4 (7)
Br1—Ni1—N6—C3491.0 (7)C26—C27—C28—N5115.2 (6)
N1—Ni1—N6—N5128.9 (4)N6—N5—C29—C330.1 (8)
N4—Ni1—N6—N535.3 (5)C28—N5—C29—C33177.4 (7)
Br1—Ni1—N6—N5101.2 (4)N6—N5—C29—C30172.4 (6)
C5—N1—C1—C22.7 (10)C28—N5—C29—C3010.1 (12)
Ni1—N1—C1—C2179.3 (6)C31—O4—C30—O311.9 (12)
N1—C1—C2—C31.4 (11)C31—O4—C30—C29163.2 (7)
C1—C2—C3—C41.0 (11)N5—C29—C30—O3176.4 (7)
C2—C3—C4—C52.1 (11)C33—C29—C30—O312.3 (12)
C1—N1—C5—C41.6 (9)N5—C29—C30—O48.2 (10)
Ni1—N1—C5—C4178.2 (5)C33—C29—C30—O4163.1 (7)
C1—N1—C5—C6178.7 (6)C30—O4—C31—C3286.7 (9)
Ni1—N1—C5—C64.6 (7)N5—C29—C33—C340.1 (8)
C3—C4—C5—N10.8 (10)C30—C29—C33—C34172.6 (6)
C3—C4—C5—C6176.3 (7)N5—N6—C34—C330.1 (8)
N3—N2—C6—C562.0 (8)Ni1—N6—C34—C33168.7 (5)
C7—N2—C6—C5115.9 (7)N5—N6—C34—C35176.7 (6)
N1—C5—C6—N262.2 (7)Ni1—N6—C34—C358.0 (11)
C4—C5—C6—N2120.7 (6)C29—C33—C34—N60.1 (8)
N3—N2—C7—C112.6 (8)C29—C33—C34—C35176.5 (6)
C6—N2—C7—C11179.4 (6)N6—C34—C35—C36144.1 (7)
N3—N2—C7—C8178.5 (6)C33—C34—C35—C3632.0 (11)
C6—N2—C7—C80.5 (12)N6—C34—C35—C3935.3 (11)
C9—O2—C8—O10.2 (12)C33—C34—C35—C39148.5 (8)
C9—O2—C8—C7178.2 (6)N6—C34—C35—Fe2126.8 (6)
N2—C7—C8—O1177.5 (7)C33—C34—C35—Fe257.0 (10)
C11—C7—C8—O11.2 (11)C41—Fe2—C35—C36117.6 (5)
N2—C7—C8—O23.9 (11)C37—Fe2—C35—C3638.5 (4)
C11—C7—C8—O2177.4 (7)C40—Fe2—C35—C36159.5 (5)
C8—O2—C9—C10106.9 (8)C44—Fe2—C35—C36166.3 (8)
N2—C7—C11—C120.8 (8)C38—Fe2—C35—C3682.3 (5)
C8—C7—C11—C12179.7 (6)C43—Fe2—C35—C3645.6 (11)
N2—N3—C12—C112.9 (8)C39—Fe2—C35—C36120.8 (6)
Ni1—N3—C12—C11172.6 (5)C42—Fe2—C35—C3676.5 (5)
N2—N3—C12—C13179.2 (6)C41—Fe2—C35—C39121.5 (5)
Ni1—N3—C12—C135.3 (11)C37—Fe2—C35—C3982.3 (4)
C7—C11—C12—N31.3 (8)C40—Fe2—C35—C3979.7 (5)
C7—C11—C12—C13179.1 (6)C44—Fe2—C35—C3945.5 (9)
N3—C12—C13—C14148.3 (7)C36—Fe2—C35—C39120.8 (6)
C11—C12—C13—C1429.3 (11)C38—Fe2—C35—C3938.5 (5)
N3—C12—C13—C1734.5 (10)C43—Fe2—C35—C39166.4 (9)
C11—C12—C13—C17148.0 (7)C42—Fe2—C35—C39162.7 (5)
N3—C12—C13—Fe1123.5 (7)C41—Fe2—C35—C340.0 (7)
C11—C12—C13—Fe159.0 (9)C37—Fe2—C35—C34156.1 (7)
C17—Fe1—C13—C14119.1 (6)C40—Fe2—C35—C3441.9 (8)
C19—Fe1—C13—C14122.6 (5)C44—Fe2—C35—C3476.1 (10)
C16—Fe1—C13—C1481.6 (5)C36—Fe2—C35—C34117.6 (8)
C22—Fe1—C13—C14168.0 (9)C38—Fe2—C35—C34160.1 (7)
C18—Fe1—C13—C14163.4 (5)C43—Fe2—C35—C3472.0 (12)
C21—Fe1—C13—C1452.5 (9)C39—Fe2—C35—C34121.6 (8)
C15—Fe1—C13—C1438.0 (5)C42—Fe2—C35—C3441.1 (7)
C20—Fe1—C13—C1481.4 (5)C39—C35—C36—C370.5 (8)
C19—Fe1—C13—C17118.2 (5)C34—C35—C36—C37180.0 (6)
C16—Fe1—C13—C1737.5 (4)Fe2—C35—C36—C3758.9 (5)
C22—Fe1—C13—C1748.9 (11)C39—C35—C36—Fe259.5 (5)
C18—Fe1—C13—C1777.5 (5)C34—C35—C36—Fe2121.0 (6)
C14—Fe1—C13—C17119.1 (6)C41—Fe2—C36—C3580.7 (5)
C21—Fe1—C13—C17171.6 (7)C37—Fe2—C36—C35118.2 (6)
C15—Fe1—C13—C1781.1 (5)C40—Fe2—C36—C3547.3 (10)
C20—Fe1—C13—C17159.5 (5)C44—Fe2—C36—C35162.7 (10)
C17—Fe1—C13—C12122.1 (8)C38—Fe2—C36—C3580.9 (5)
C19—Fe1—C13—C123.9 (7)C43—Fe2—C36—C35163.6 (4)
C16—Fe1—C13—C12159.6 (7)C39—Fe2—C36—C3537.0 (4)
C22—Fe1—C13—C1273.3 (11)C42—Fe2—C36—C35122.9 (4)
C18—Fe1—C13—C1244.6 (7)C35—Fe2—C36—C37118.2 (6)
C14—Fe1—C13—C12118.7 (8)C41—Fe2—C36—C37161.1 (4)
C21—Fe1—C13—C1266.2 (10)C40—Fe2—C36—C37165.5 (8)
C15—Fe1—C13—C12156.8 (7)C44—Fe2—C36—C3744.4 (13)
C20—Fe1—C13—C1237.3 (7)C38—Fe2—C36—C3737.3 (4)
C17—C13—C14—C150.8 (8)C43—Fe2—C36—C3778.1 (5)
C12—C13—C14—C15178.5 (6)C39—Fe2—C36—C3781.2 (4)
Fe1—C13—C14—C1559.5 (5)C42—Fe2—C36—C37118.8 (5)
C17—C13—C14—Fe158.8 (5)C35—C36—C37—C381.0 (8)
C12—C13—C14—Fe1119.0 (6)Fe2—C36—C37—C3859.8 (6)
C17—Fe1—C14—C1338.5 (4)C35—C36—C37—Fe258.8 (5)
C19—Fe1—C14—C1375.4 (5)C35—Fe2—C37—C3881.3 (5)
C16—Fe1—C14—C1381.7 (5)C41—Fe2—C37—C38165.2 (7)
C22—Fe1—C14—C13168.9 (8)C40—Fe2—C37—C3841.5 (12)
C18—Fe1—C14—C1342.4 (11)C44—Fe2—C37—C3876.1 (5)
C21—Fe1—C14—C13159.2 (4)C36—Fe2—C37—C38119.6 (6)
C15—Fe1—C14—C13118.8 (6)C43—Fe2—C37—C38118.6 (5)
C20—Fe1—C14—C13117.3 (5)C39—Fe2—C37—C3837.1 (4)
C17—Fe1—C14—C1580.3 (5)C42—Fe2—C37—C38160.3 (4)
C13—Fe1—C14—C15118.8 (6)C35—Fe2—C37—C3638.3 (4)
C19—Fe1—C14—C15165.8 (5)C41—Fe2—C37—C3645.7 (10)
C16—Fe1—C14—C1537.0 (5)C40—Fe2—C37—C36161.0 (10)
C22—Fe1—C14—C1550.1 (11)C44—Fe2—C37—C36164.3 (5)
C18—Fe1—C14—C15161.1 (8)C38—Fe2—C37—C36119.6 (6)
C21—Fe1—C14—C1582.0 (5)C43—Fe2—C37—C36121.8 (5)
C20—Fe1—C14—C15123.9 (5)C39—Fe2—C37—C3682.5 (5)
C13—C14—C15—C160.7 (9)C42—Fe2—C37—C3680.1 (5)
Fe1—C14—C15—C1658.3 (6)C36—C37—C38—C391.1 (9)
C13—C14—C15—Fe159.0 (5)Fe2—C37—C38—C3958.5 (6)
C17—Fe1—C15—C1636.8 (4)C36—C37—C38—Fe259.6 (5)
C13—Fe1—C15—C1682.0 (5)C35—Fe2—C38—C3781.9 (5)
C19—Fe1—C15—C16159.2 (9)C41—Fe2—C38—C37162.5 (9)
C22—Fe1—C15—C1679.7 (6)C40—Fe2—C38—C37165.2 (5)
C18—Fe1—C15—C1641.5 (10)C44—Fe2—C38—C37122.8 (5)
C14—Fe1—C15—C16120.2 (6)C36—Fe2—C38—C3737.8 (4)
C21—Fe1—C15—C16121.5 (5)C43—Fe2—C38—C3780.4 (5)
C20—Fe1—C15—C16164.0 (5)C39—Fe2—C38—C37120.7 (7)
C17—Fe1—C15—C1483.3 (5)C42—Fe2—C38—C3747.6 (11)
C13—Fe1—C15—C1438.2 (4)C35—Fe2—C38—C3938.7 (5)
C19—Fe1—C15—C1439.1 (12)C41—Fe2—C38—C3941.9 (12)
C16—Fe1—C15—C14120.2 (6)C37—Fe2—C38—C39120.7 (7)
C22—Fe1—C15—C14160.1 (5)C40—Fe2—C38—C3974.1 (6)
C18—Fe1—C15—C14161.7 (8)C44—Fe2—C38—C39116.5 (5)
C21—Fe1—C15—C14118.4 (5)C36—Fe2—C38—C3982.8 (5)
C20—Fe1—C15—C1475.8 (5)C43—Fe2—C38—C39158.9 (5)
C14—C15—C16—C170.5 (9)C42—Fe2—C38—C39168.3 (8)
Fe1—C15—C16—C1758.8 (5)C36—C35—C39—C380.1 (9)
C14—C15—C16—Fe158.3 (5)C34—C35—C39—C38179.3 (7)
C13—Fe1—C16—C1738.9 (5)Fe2—C35—C39—C3859.6 (5)
C19—Fe1—C16—C1742.7 (10)C36—C35—C39—Fe259.4 (5)
C22—Fe1—C16—C17120.0 (5)C34—C35—C39—Fe2121.1 (7)
C18—Fe1—C16—C1776.4 (5)C37—C38—C39—C350.8 (9)
C14—Fe1—C16—C1783.1 (5)Fe2—C38—C39—C3558.9 (5)
C21—Fe1—C16—C17160.4 (5)C37—C38—C39—Fe258.1 (6)
C15—Fe1—C16—C17120.5 (7)C41—Fe2—C39—C3577.5 (5)
C20—Fe1—C16—C17166.1 (9)C37—Fe2—C39—C3581.0 (5)
C17—Fe1—C16—C15120.5 (7)C40—Fe2—C39—C35117.9 (5)
C13—Fe1—C16—C1581.6 (5)C44—Fe2—C39—C35160.6 (4)
C19—Fe1—C16—C15163.2 (7)C36—Fe2—C39—C3536.9 (4)
C22—Fe1—C16—C15119.6 (5)C38—Fe2—C39—C35117.8 (7)
C18—Fe1—C16—C15163.2 (4)C43—Fe2—C39—C35168.7 (8)
C14—Fe1—C16—C1537.4 (4)C42—Fe2—C39—C3548.4 (12)
C21—Fe1—C16—C1579.2 (5)C35—Fe2—C39—C38117.8 (7)
C20—Fe1—C16—C1545.7 (12)C41—Fe2—C39—C38164.7 (5)
C15—C16—C17—C130.0 (8)C37—Fe2—C39—C3836.8 (5)
Fe1—C16—C17—C1359.3 (5)C40—Fe2—C39—C38124.3 (5)
C15—C16—C17—Fe159.3 (6)C44—Fe2—C39—C3881.6 (6)
C14—C13—C17—C160.5 (8)C36—Fe2—C39—C3880.9 (6)
C12—C13—C17—C16178.1 (6)C43—Fe2—C39—C3851.0 (11)
Fe1—C13—C17—C1659.9 (5)C42—Fe2—C39—C38166.1 (10)
C14—C13—C17—Fe159.4 (5)C35—Fe2—C40—C4180.9 (6)
C12—C13—C17—Fe1118.3 (7)C37—Fe2—C40—C41164.3 (9)
C13—Fe1—C17—C16118.7 (7)C44—Fe2—C40—C41119.1 (7)
C19—Fe1—C17—C16161.7 (5)C36—Fe2—C40—C4147.0 (11)
C22—Fe1—C17—C1679.3 (6)C38—Fe2—C40—C41164.2 (5)
C18—Fe1—C17—C16120.8 (5)C43—Fe2—C40—C4180.5 (5)
C14—Fe1—C17—C1681.0 (5)C39—Fe2—C40—C41123.2 (5)
C21—Fe1—C17—C1652.3 (11)C42—Fe2—C40—C4137.5 (5)
C15—Fe1—C17—C1637.0 (5)C35—Fe2—C40—C44160.0 (5)
C20—Fe1—C17—C16168.9 (8)C41—Fe2—C40—C44119.1 (7)
C19—Fe1—C17—C1379.6 (5)C37—Fe2—C40—C4445.2 (13)
C16—Fe1—C17—C13118.7 (7)C36—Fe2—C40—C44166.1 (8)
C22—Fe1—C17—C13162.0 (4)C38—Fe2—C40—C4476.7 (6)
C18—Fe1—C17—C13120.5 (4)C43—Fe2—C40—C4438.6 (5)
C14—Fe1—C17—C1337.8 (4)C39—Fe2—C40—C44117.7 (5)
C21—Fe1—C17—C13171.0 (8)C42—Fe2—C40—C4481.6 (6)
C15—Fe1—C17—C1381.7 (5)C44—C40—C41—C420.8 (9)
C20—Fe1—C17—C1350.2 (10)Fe2—C40—C41—C4260.0 (5)
C17—Fe1—C18—C19119.1 (5)C44—C40—C41—Fe259.3 (6)
C13—Fe1—C18—C1976.5 (6)C35—Fe2—C41—C40116.9 (5)
C16—Fe1—C18—C19159.9 (5)C37—Fe2—C41—C40167.2 (7)
C22—Fe1—C18—C19117.9 (7)C44—Fe2—C41—C4038.4 (5)
C14—Fe1—C18—C1945.1 (11)C36—Fe2—C41—C40159.5 (5)
C21—Fe1—C18—C1981.3 (5)C38—Fe2—C41—C4043.0 (12)
C15—Fe1—C18—C19169.7 (8)C43—Fe2—C41—C4082.7 (5)
C20—Fe1—C18—C1937.5 (5)C39—Fe2—C41—C4074.6 (6)
C17—Fe1—C18—C22123.0 (5)C42—Fe2—C41—C40119.6 (7)
C13—Fe1—C18—C22165.6 (5)C35—Fe2—C41—C42123.5 (5)
C19—Fe1—C18—C22117.9 (7)C37—Fe2—C41—C4247.6 (10)
C16—Fe1—C18—C2282.1 (6)C40—Fe2—C41—C42119.6 (7)
C14—Fe1—C18—C22163.0 (8)C44—Fe2—C41—C4281.2 (5)
C21—Fe1—C18—C2236.6 (5)C36—Fe2—C41—C4280.9 (5)
C15—Fe1—C18—C2251.7 (11)C38—Fe2—C41—C42162.6 (9)
C20—Fe1—C18—C2280.4 (5)C43—Fe2—C41—C4237.0 (5)
C22—C18—C19—C200.8 (8)C39—Fe2—C41—C42165.8 (5)
Fe1—C18—C19—C2060.5 (5)C40—C41—C42—C430.5 (9)
C22—C18—C19—Fe159.7 (5)Fe2—C41—C42—C4359.3 (5)
C17—Fe1—C19—C1877.7 (5)C40—C41—C42—Fe259.8 (6)
C13—Fe1—C19—C18120.8 (5)C35—Fe2—C42—C43164.9 (5)
C16—Fe1—C19—C1847.0 (10)C41—Fe2—C42—C43119.7 (7)
C22—Fe1—C19—C1839.0 (5)C37—Fe2—C42—C4380.1 (6)
C14—Fe1—C19—C18162.2 (4)C40—Fe2—C42—C4382.5 (6)
C21—Fe1—C19—C1881.6 (5)C44—Fe2—C42—C4337.7 (5)
C15—Fe1—C19—C18168.2 (9)C36—Fe2—C42—C43123.0 (5)
C20—Fe1—C19—C18119.5 (7)C38—Fe2—C42—C4345.5 (12)
C17—Fe1—C19—C20162.8 (5)C39—Fe2—C42—C43158.4 (10)
C13—Fe1—C19—C20119.7 (5)C35—Fe2—C42—C4175.4 (5)
C16—Fe1—C19—C20166.5 (7)C37—Fe2—C42—C41160.2 (5)
C22—Fe1—C19—C2080.5 (5)C40—Fe2—C42—C4137.2 (5)
C18—Fe1—C19—C20119.5 (7)C44—Fe2—C42—C4182.0 (5)
C14—Fe1—C19—C2078.3 (5)C36—Fe2—C42—C41117.3 (5)
C21—Fe1—C19—C2037.9 (5)C38—Fe2—C42—C41165.2 (9)
C15—Fe1—C19—C2048.7 (12)C43—Fe2—C42—C41119.7 (7)
C18—C19—C20—C211.1 (8)C39—Fe2—C42—C4138.7 (12)
Fe1—C19—C20—C2158.9 (5)C41—C42—C43—C440.0 (9)
C18—C19—C20—Fe160.0 (5)Fe2—C42—C43—C4458.6 (6)
C17—Fe1—C20—C1940.7 (10)C41—C42—C43—Fe258.7 (5)
C13—Fe1—C20—C1977.5 (5)C35—Fe2—C43—C4241.2 (12)
C16—Fe1—C20—C19162.7 (9)C41—Fe2—C43—C4237.5 (5)
C22—Fe1—C20—C1982.1 (5)C37—Fe2—C43—C42118.5 (5)
C18—Fe1—C20—C1937.3 (4)C40—Fe2—C43—C4280.9 (6)
C14—Fe1—C20—C19120.6 (5)C44—Fe2—C43—C42119.9 (8)
C21—Fe1—C20—C19118.7 (6)C36—Fe2—C43—C4275.8 (6)
C15—Fe1—C20—C19162.5 (5)C38—Fe2—C43—C42161.0 (5)
C17—Fe1—C20—C21159.4 (8)C39—Fe2—C43—C42162.0 (8)
C13—Fe1—C20—C21163.8 (4)C35—Fe2—C43—C44161.1 (8)
C19—Fe1—C20—C21118.7 (6)C41—Fe2—C43—C4482.4 (6)
C16—Fe1—C20—C2144.1 (12)C37—Fe2—C43—C44121.6 (5)
C22—Fe1—C20—C2136.6 (5)C40—Fe2—C43—C4439.0 (5)
C18—Fe1—C20—C2181.4 (5)C36—Fe2—C43—C44164.3 (5)
C14—Fe1—C20—C21120.7 (5)C38—Fe2—C43—C4479.1 (6)
C15—Fe1—C20—C2178.8 (5)C39—Fe2—C43—C4442.1 (11)
C19—C20—C21—C220.9 (8)C42—Fe2—C43—C44119.9 (8)
Fe1—C20—C21—C2259.5 (5)C42—C43—C44—C400.5 (9)
C19—C20—C21—Fe158.6 (5)Fe2—C43—C44—C4059.7 (6)
C17—Fe1—C21—C2236.8 (11)C42—C43—C44—Fe259.2 (5)
C13—Fe1—C21—C22159.4 (7)C41—C40—C44—C430.8 (9)
C19—Fe1—C21—C2281.9 (5)Fe2—C40—C44—C4360.2 (6)
C16—Fe1—C21—C2275.6 (6)C41—C40—C44—Fe259.4 (6)
C18—Fe1—C21—C2238.4 (5)C35—Fe2—C44—C43164.8 (7)
C14—Fe1—C21—C22162.0 (5)C41—Fe2—C44—C4380.4 (6)
C15—Fe1—C21—C22118.3 (5)C37—Fe2—C44—C4378.1 (6)
C20—Fe1—C21—C22119.8 (7)C40—Fe2—C44—C43117.7 (7)
C17—Fe1—C21—C20156.6 (9)C36—Fe2—C44—C4344.3 (13)
C13—Fe1—C21—C2039.6 (10)C38—Fe2—C44—C43119.6 (5)
C19—Fe1—C21—C2037.9 (5)C39—Fe2—C44—C43162.3 (5)
C16—Fe1—C21—C20164.5 (5)C42—Fe2—C44—C4336.7 (5)
C22—Fe1—C21—C20119.8 (7)C35—Fe2—C44—C4047.1 (10)
C18—Fe1—C21—C2081.5 (5)C41—Fe2—C44—C4037.3 (6)
C14—Fe1—C21—C2078.2 (5)C37—Fe2—C44—C40164.2 (5)
C15—Fe1—C21—C20121.8 (5)C36—Fe2—C44—C40161.9 (10)
C20—C21—C22—C180.4 (9)C38—Fe2—C44—C40122.7 (6)
Fe1—C21—C22—C1859.3 (5)C43—Fe2—C44—C40117.7 (7)
C20—C21—C22—Fe159.7 (5)C39—Fe2—C44—C4080.0 (6)
C19—C18—C22—C210.2 (9)C42—Fe2—C44—C4081.0 (6)

Experimental details

Crystal data
Chemical formulaC44H42Br5Fe3N6NiO4
Mr1344.65
Crystal system, space groupMonoclinic, Cc
Temperature (K)100
a, b, c (Å)15.2181 (3), 22.0080 (3), 16.0005 (3)
β (°) 118.393 (2)
V3)4714.25 (14)
Z4
Radiation typeCu Kα
µ (mm1)13.07
Crystal size (mm)0.19 × 0.11 × 0.09
Data collection
DiffractometerBruker SMART APEX2 area detector
diffractometer
Absorption correctionAnalytical
SADABS (Bruker-AXS, 2007)
Tmin, Tmax0.186, 0.376
No. of measured, independent and
observed [I > 2σ(I)] reflections
35920, 8033, 7903
Rint0.031
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.078, 1.05
No. of reflections8033
No. of parameters599
No. of restraints4
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.70, 0.66
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter0.008 (4)

Computer programs: APEX2 Ver. 2.1-4 (Bruker-AXS, 2007), SAINT Ver. 7.24A (Bruker-AXS, 2007), SAINT Ver. 7.24A, SHELXTL (Sheldrick, 2008), SHELXTL.

Selected geometric parameters (Å, º) top
Br1—Ni12.4407 (10)Fe2—C412.038 (8)
Ni1—N12.047 (5)Fe2—C372.040 (7)
Ni1—N42.058 (5)Fe2—C402.042 (9)
Ni1—N32.092 (5)Fe2—C442.047 (7)
Ni1—N62.105 (5)Fe2—C362.053 (7)
Fe1—C172.026 (7)Fe2—C382.055 (8)
Fe1—C132.030 (6)Fe2—C432.057 (8)
Fe1—C192.032 (7)Fe2—C392.058 (7)
Fe1—C162.033 (8)Fe2—C422.058 (8)
Fe1—C222.037 (8)Br2—Fe32.3352 (13)
Fe1—C182.038 (7)Br3—Fe32.3290 (16)
Fe1—C142.042 (7)Br4—Fe32.3419 (16)
Fe1—C212.047 (7)Br5—Fe32.2995 (16)
Fe1—C152.050 (8)Br3A—Fe31.943 (10)
Fe1—C202.062 (7)Br4A—Fe32.553 (15)
Fe2—C352.031 (7)Br5A—Fe32.560 (11)
N1—Ni1—N493.66 (19)C35—Fe2—C44156.3 (3)
N1—Ni1—N388.1 (2)C41—Fe2—C4468.5 (3)
N4—Ni1—N390.8 (2)C37—Fe2—C44124.3 (3)
N1—Ni1—N693.0 (2)C40—Fe2—C4441.4 (3)
N4—Ni1—N687.7 (2)C35—Fe2—C3640.9 (3)
N3—Ni1—N6178.2 (2)C41—Fe2—C36121.0 (3)
N1—Ni1—Br1129.90 (17)C37—Fe2—C3641.1 (3)
N4—Ni1—Br1136.43 (16)C40—Fe2—C36155.7 (3)
N3—Ni1—Br190.97 (16)C44—Fe2—C36161.4 (3)
N6—Ni1—Br189.41 (15)C35—Fe2—C3868.3 (3)
C17—Fe1—C1341.9 (3)C41—Fe2—C38160.8 (4)
C17—Fe1—C19120.5 (3)C37—Fe2—C3840.6 (3)
C13—Fe1—C19105.9 (3)C40—Fe2—C38124.5 (4)
C17—Fe1—C1640.4 (3)C44—Fe2—C38107.4 (3)
C13—Fe1—C1668.9 (3)C36—Fe2—C3868.8 (4)
C19—Fe1—C16156.4 (3)C35—Fe2—C43161.0 (3)
C17—Fe1—C22123.3 (4)C41—Fe2—C4367.8 (3)
C13—Fe1—C22159.9 (3)C37—Fe2—C43108.3 (3)
C19—Fe1—C2268.0 (3)C40—Fe2—C4368.6 (3)
C16—Fe1—C22108.5 (3)C44—Fe2—C4340.9 (3)
C17—Fe1—C18105.6 (3)C36—Fe2—C43124.5 (3)
C13—Fe1—C18121.8 (3)C38—Fe2—C43122.3 (3)
C19—Fe1—C1840.2 (3)C35—Fe2—C3941.1 (3)
C16—Fe1—C18121.6 (3)C41—Fe2—C39123.6 (3)
C22—Fe1—C1841.3 (3)C37—Fe2—C3969.1 (3)
C17—Fe1—C1469.7 (3)C40—Fe2—C39106.3 (4)
C13—Fe1—C1441.1 (3)C44—Fe2—C39120.4 (4)
C19—Fe1—C14123.2 (3)C36—Fe2—C3969.5 (3)
C16—Fe1—C1468.9 (3)C38—Fe2—C3940.9 (3)
C22—Fe1—C14158.2 (3)C43—Fe2—C39157.0 (3)
C18—Fe1—C14158.8 (3)C35—Fe2—C42124.7 (3)
C17—Fe1—C21159.7 (3)C41—Fe2—C4240.5 (4)
C13—Fe1—C21158.0 (3)C37—Fe2—C42122.1 (3)
C19—Fe1—C2167.8 (3)C40—Fe2—C4268.0 (4)
C16—Fe1—C21125.2 (3)C44—Fe2—C4268.2 (3)
C22—Fe1—C2139.4 (3)C36—Fe2—C42107.7 (3)
C18—Fe1—C2168.0 (3)C38—Fe2—C42157.3 (3)
C14—Fe1—C21123.3 (3)C43—Fe2—C4239.8 (3)
C17—Fe1—C1568.6 (3)C39—Fe2—C42160.9 (3)
C13—Fe1—C1568.8 (3)Br3A—Fe3—Br5136.5 (5)
C19—Fe1—C15160.9 (4)Br3A—Fe3—Br357.9 (4)
C16—Fe1—C1540.5 (4)Br5—Fe3—Br3109.01 (6)
C22—Fe1—C15123.0 (3)Br3A—Fe3—Br2115.5 (5)
C18—Fe1—C15158.2 (3)Br5—Fe3—Br2107.98 (6)
C14—Fe1—C1541.0 (3)Br3—Fe3—Br2109.57 (6)
C21—Fe1—C15109.8 (3)Br3A—Fe3—Br451.0 (3)
C17—Fe1—C20157.0 (3)Br5—Fe3—Br4113.52 (7)
C13—Fe1—C20121.2 (3)Br3—Fe3—Br4108.00 (7)
C19—Fe1—C2040.5 (4)Br2—Fe3—Br4108.71 (6)
C16—Fe1—C20161.7 (4)Br3A—Fe3—Br4A115.1 (5)
C22—Fe1—C2067.4 (3)Br5—Fe3—Br4A49.9 (3)
C18—Fe1—C2068.0 (3)Br3—Fe3—Br4A145.7 (4)
C14—Fe1—C20107.8 (3)Br2—Fe3—Br4A103.4 (4)
C21—Fe1—C2040.4 (3)Br4—Fe3—Br4A68.7 (3)
C15—Fe1—C20125.4 (4)Br3A—Fe3—Br5A117.6 (6)
C35—Fe2—C41107.4 (3)Br5—Fe3—Br5A45.0 (3)
C35—Fe2—C3768.6 (3)Br3—Fe3—Br5A66.9 (3)
C41—Fe2—C37157.2 (3)Br2—Fe3—Br5A108.0 (3)
C35—Fe2—C40120.4 (3)Br4—Fe3—Br5A142.2 (3)
C41—Fe2—C4040.2 (4)Br4A—Fe3—Br5A94.5 (4)
C37—Fe2—C40161.5 (4)
 

Follow Acta Cryst. B
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds