Detailed example of the identification and crystallographic analysis of a pseudo-merohedrally twinned crystal

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.

S1. Refinement

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

Computing details

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

Figure 1. Molecular structure of (I). The thermal ellipsoids are shown at 50% probability level.

(I)

Crystal data

C44H42Br5Fe3N6NiO4	F(000) = 2644
Mr = 1344.65	Dx = 1.895 Mg m^−3
Monoclinic, Cc	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: C -2yc	Cell parameters from 999 reflections
a = 15.2181 (3) Å	θ = 3.1–72.1°
b = 22.0080 (3) Å	µ = 13.07 mm^−1
c = 16.0005 (3) Å	T = 100 K
β = 118.393 (2)°	Block, red
V = 4714.25 (14) Å^3	0.19 × 0.11 × 0.09 mm
Z = 4

Data collection

Bruker SMART APEX2 area detector diffractometer	8033 independent reflections
Radiation source: fine-focus sealed tube	7903 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.031
0.50° ω and 0.5 ° ϕ scans	θmax = 72.1°, θmin = 3.1°
Absorption correction: analytical SADABS (Bruker-AXS, 2007)	h = −17→18
Tmin = 0.186, Tmax = 0.376	k = −27→25
35920 measured reflections	l = −19→18

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.032	H-atom parameters constrained
wR(F^2) = 0.078	w = 1/[σ^2(Fo^2) + (0.0581P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
8033 reflections	Δρmax = 0.70 e Å^−3
599 parameters	Δρmin = −0.66 e Å^−3
4 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.008 (4)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Br1	0.29003 (5)	0.62030 (3)	0.66511 (4)	0.02583 (15)
Ni1	0.20175 (8)	0.62397 (5)	0.49182 (7)	0.01679 (19)
Fe1	−0.07292 (7)	0.58052 (5)	0.59258 (7)	0.0220 (2)
Fe2	0.58354 (7)	0.67777 (5)	0.59805 (8)	0.0238 (2)
O1	0.0385 (4)	0.3437 (2)	0.4396 (5)	0.0395 (13)
O2	0.1836 (4)	0.3649 (2)	0.4416 (5)	0.0402 (14)
O3	0.2928 (4)	0.9093 (2)	0.4472 (4)	0.0357 (12)
O4	0.1420 (4)	0.8748 (2)	0.4217 (5)	0.0406 (15)
N1	0.2374 (4)	0.5853 (2)	0.3956 (4)	0.0207 (11)
N2	0.1603 (4)	0.4908 (2)	0.4768 (4)	0.0209 (11)
N3	0.1236 (4)	0.5445 (2)	0.4860 (4)	0.0185 (10)
N4	0.0732 (4)	0.6635 (2)	0.3887 (4)	0.0186 (10)
N5	0.2240 (4)	0.7578 (2)	0.4837 (4)	0.0205 (11)
N6	0.2764 (4)	0.7055 (2)	0.4968 (4)	0.0179 (10)
C1	0.2373 (5)	0.6184 (3)	0.3235 (5)	0.0261 (15)
H1	0.2209	0.6603	0.3187	0.031*
C2	0.2597 (6)	0.5933 (3)	0.2586 (5)	0.0303 (16)
H2	0.2603	0.6180	0.2102	0.036*
C3	0.2817 (6)	0.5323 (3)	0.2623 (6)	0.0349 (17)
H3	0.2986	0.5145	0.2178	0.042*
C4	0.2784 (5)	0.4988 (3)	0.3316 (5)	0.0273 (15)
H4	0.2910	0.4564	0.3348	0.033*
C5	0.2566 (4)	0.5260 (3)	0.3987 (4)	0.0179 (13)
C6	0.2589 (5)	0.4895 (3)	0.4797 (5)	0.0177 (12)
H6A	0.2774	0.4470	0.4752	0.021*
H6B	0.3102	0.5065	0.5409	0.021*
C7	0.0952 (5)	0.4448 (3)	0.4631 (5)	0.0224 (14)
C8	0.1034 (5)	0.3791 (3)	0.4476 (5)	0.0231 (14)
C9	0.1974 (7)	0.3010 (3)	0.4233 (6)	0.043 (2)
H9A	0.1501	0.2747	0.4328	0.051*
H9B	0.2663	0.2876	0.4676	0.051*
C10	0.1785 (7)	0.2960 (4)	0.3214 (5)	0.050 (2)
H10A	0.1104	0.3097	0.2781	0.075*
H10B	0.1865	0.2537	0.3073	0.075*
H10C	0.2264	0.3216	0.3130	0.075*
C11	0.0135 (5)	0.4709 (3)	0.4681 (5)	0.0202 (13)
H11	−0.0444	0.4507	0.4621	0.024*
C12	0.0353 (5)	0.5327 (3)	0.4837 (5)	0.0212 (13)
C13	−0.0264 (5)	0.5798 (3)	0.4929 (5)	0.0233 (13)
C14	−0.1331 (5)	0.5782 (4)	0.4482 (5)	0.0275 (15)
H14	−0.1749	0.5473	0.4070	0.033*
C15	−0.1652 (6)	0.6317 (4)	0.4767 (7)	0.039 (2)
H15	−0.2324	0.6429	0.4573	0.047*
C16	−0.0794 (6)	0.6652 (3)	0.5390 (6)	0.0344 (18)
H16	−0.0797	0.7025	0.5686	0.041*
C17	0.0062 (6)	0.6345 (3)	0.5501 (6)	0.0281 (15)
H17	0.0733	0.6473	0.5881	0.034*
C18	0.0213 (6)	0.5606 (4)	0.7314 (5)	0.0311 (16)
H18	0.0876	0.5753	0.7679	0.037*
C19	−0.0077 (6)	0.5074 (3)	0.6772 (5)	0.0339 (16)
H19	0.0361	0.4797	0.6699	0.041*
C20	−0.1128 (7)	0.5014 (4)	0.6349 (5)	0.0377 (18)
H20	−0.1520	0.4690	0.5953	0.045*
C21	−0.1484 (5)	0.5529 (4)	0.6630 (5)	0.0311 (16)
H21	−0.2165	0.5614	0.6445	0.037*
C22	−0.0685 (7)	0.5887 (4)	0.7213 (6)	0.0380 (18)
H22	−0.0720	0.6258	0.7501	0.046*
C23	0.0101 (5)	0.6323 (3)	0.3113 (5)	0.0238 (14)
H23	0.0239	0.5906	0.3071	0.029*
C24	−0.0740 (5)	0.6576 (3)	0.2373 (5)	0.0280 (15)
H24	−0.1152	0.6346	0.1821	0.034*
C25	−0.0966 (5)	0.7178 (3)	0.2460 (5)	0.0267 (14)
H25	−0.1553	0.7364	0.1979	0.032*
C26	−0.0307 (5)	0.7508 (3)	0.3276 (5)	0.0246 (14)
H26	−0.0440	0.7921	0.3348	0.030*
C27	0.0531 (4)	0.7224 (3)	0.3965 (5)	0.0194 (13)
C28	0.1286 (5)	0.7547 (3)	0.4849 (5)	0.0223 (13)
H28A	0.1048	0.7962	0.4872	0.027*
H28B	0.1371	0.7324	0.5421	0.027*
C29	0.2752 (5)	0.8057 (3)	0.4748 (5)	0.0206 (12)
C30	0.2389 (6)	0.8699 (3)	0.4486 (6)	0.0281 (16)
C31	0.0928 (8)	0.9307 (4)	0.3692 (7)	0.050 (2)
H31A	0.0206	0.9235	0.3272	0.060*
H31B	0.1232	0.9444	0.3299	0.060*
C32	0.1084 (10)	0.9774 (4)	0.4443 (7)	0.070 (3)
H32A	0.1017	0.9580	0.4961	0.106*
H32B	0.0582	1.0096	0.4162	0.106*
H32C	0.1753	0.9951	0.4693	0.106*
C33	0.3627 (5)	0.7837 (3)	0.4824 (5)	0.0241 (13)
H33	0.4141	0.8064	0.4792	0.029*
C34	0.3610 (4)	0.7204 (3)	0.4961 (5)	0.0204 (13)
C35	0.4356 (5)	0.6761 (3)	0.5031 (5)	0.0243 (14)
C36	0.4924 (5)	0.6820 (4)	0.4538 (5)	0.0306 (16)
H36	0.4885	0.7141	0.4124	0.037*
C37	0.5568 (6)	0.6298 (3)	0.4792 (6)	0.0305 (16)
H37	0.6042	0.6215	0.4580	0.037*
C38	0.5377 (6)	0.5926 (3)	0.5413 (7)	0.0380 (19)
H38	0.5695	0.5550	0.5676	0.046*
C39	0.4625 (6)	0.6211 (3)	0.5579 (6)	0.0309 (16)
H39	0.4359	0.6066	0.5971	0.037*
C40	0.6302 (6)	0.6998 (5)	0.7369 (6)	0.044 (2)
H40	0.5997	0.6875	0.7739	0.053*
C41	0.6084 (6)	0.7525 (4)	0.6815 (6)	0.041 (2)
H41	0.5596	0.7820	0.6742	0.050*
C42	0.6707 (6)	0.7548 (4)	0.6383 (6)	0.0374 (18)
H42	0.6713	0.7860	0.5976	0.045*
C43	0.7316 (6)	0.7029 (4)	0.6660 (6)	0.0378 (18)
H43	0.7804	0.6930	0.6471	0.045*
C44	0.7076 (6)	0.6672 (4)	0.7275 (5)	0.0386 (19)
H44	0.7369	0.6296	0.7564	0.046*
Br2	0.43364 (6)	0.36557 (4)	0.47749 (6)	0.0455 (2)
Br3	0.49508 (8)	0.47066 (4)	0.68743 (8)	0.0435 (3)	0.852 (2)
Br4	0.44443 (8)	0.30422 (4)	0.70425 (8)	0.0384 (2)	0.852 (2)
Br5	0.68356 (7)	0.35652 (4)	0.69552 (7)	0.0371 (2)	0.852 (2)
Br3A	0.4315 (11)	0.3893 (5)	0.7007 (12)	0.102 (4)	0.148 (2)
Br4A	0.6172 (13)	0.2750 (6)	0.6963 (15)	0.125 (6)	0.148 (2)
Br5A	0.6694 (7)	0.4413 (6)	0.6917 (9)	0.102 (4)	0.148 (2)
Fe3	0.51627 (9)	0.37325 (6)	0.64296 (8)	0.0333 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Br1	0.0288 (4)	0.0276 (3)	0.0197 (3)	−0.0068 (3)	0.0105 (3)	−0.0017 (3)
Ni1	0.0160 (5)	0.0167 (4)	0.0183 (5)	−0.0022 (4)	0.0087 (5)	−0.0014 (5)
Fe1	0.0189 (5)	0.0286 (5)	0.0214 (6)	0.0027 (4)	0.0120 (5)	0.0019 (4)
Fe2	0.0190 (5)	0.0317 (5)	0.0237 (6)	0.0048 (4)	0.0125 (5)	0.0013 (5)
O1	0.037 (3)	0.029 (3)	0.060 (4)	−0.010 (2)	0.029 (3)	−0.006 (2)
O2	0.044 (3)	0.021 (2)	0.070 (4)	−0.006 (2)	0.039 (3)	−0.008 (2)
O3	0.035 (3)	0.018 (2)	0.053 (3)	−0.003 (2)	0.020 (3)	0.004 (2)
O4	0.034 (3)	0.026 (2)	0.063 (4)	0.012 (2)	0.024 (3)	0.024 (3)
N1	0.019 (3)	0.029 (3)	0.021 (3)	−0.004 (2)	0.015 (2)	−0.002 (2)
N2	0.020 (3)	0.024 (3)	0.022 (3)	−0.002 (2)	0.012 (2)	0.001 (2)
N3	0.024 (3)	0.011 (2)	0.025 (3)	−0.0046 (19)	0.015 (2)	−0.002 (2)
N4	0.020 (3)	0.018 (2)	0.019 (3)	−0.003 (2)	0.011 (2)	−0.001 (2)
N5	0.018 (3)	0.021 (3)	0.018 (3)	0.001 (2)	0.005 (2)	−0.001 (2)
N6	0.018 (2)	0.018 (2)	0.018 (3)	−0.002 (2)	0.009 (2)	−0.003 (2)
C1	0.030 (4)	0.020 (3)	0.035 (4)	−0.004 (3)	0.020 (3)	−0.005 (3)
C2	0.046 (4)	0.026 (3)	0.026 (4)	−0.008 (3)	0.024 (4)	−0.003 (3)
C3	0.035 (4)	0.033 (4)	0.046 (5)	−0.008 (3)	0.026 (4)	−0.007 (3)
C4	0.032 (4)	0.026 (3)	0.032 (4)	−0.002 (3)	0.022 (3)	−0.009 (3)
C5	0.014 (3)	0.018 (3)	0.020 (3)	−0.002 (2)	0.006 (2)	−0.001 (2)
C6	0.017 (3)	0.021 (3)	0.020 (3)	−0.001 (2)	0.012 (3)	−0.003 (2)
C7	0.023 (3)	0.028 (3)	0.015 (3)	−0.004 (2)	0.008 (3)	0.002 (3)
C8	0.025 (3)	0.022 (3)	0.025 (4)	−0.001 (3)	0.014 (3)	−0.003 (2)
C9	0.055 (5)	0.016 (3)	0.078 (6)	−0.002 (3)	0.049 (5)	−0.005 (4)
C10	0.057 (5)	0.040 (5)	0.060 (6)	−0.010 (4)	0.034 (5)	−0.014 (4)
C11	0.019 (3)	0.027 (3)	0.022 (3)	−0.005 (2)	0.016 (3)	0.000 (3)
C12	0.020 (3)	0.023 (3)	0.018 (3)	−0.005 (2)	0.007 (3)	0.001 (3)
C13	0.030 (3)	0.033 (3)	0.016 (3)	0.000 (3)	0.018 (3)	0.004 (3)
C14	0.011 (3)	0.046 (4)	0.022 (3)	0.001 (3)	0.005 (3)	0.008 (3)
C15	0.028 (4)	0.058 (5)	0.042 (5)	0.026 (4)	0.024 (4)	0.023 (4)
C16	0.046 (5)	0.030 (4)	0.033 (4)	0.006 (3)	0.023 (4)	−0.001 (3)
C17	0.035 (4)	0.028 (3)	0.035 (4)	0.000 (3)	0.028 (3)	0.004 (3)
C18	0.025 (4)	0.047 (4)	0.020 (3)	0.013 (3)	0.010 (3)	0.010 (3)
C19	0.039 (4)	0.038 (4)	0.025 (4)	0.014 (3)	0.016 (3)	0.015 (3)
C20	0.045 (5)	0.044 (4)	0.027 (4)	−0.010 (4)	0.019 (4)	0.012 (3)
C21	0.023 (4)	0.050 (4)	0.026 (4)	0.005 (3)	0.016 (3)	0.009 (3)
C22	0.044 (5)	0.048 (4)	0.027 (4)	0.010 (4)	0.021 (4)	−0.001 (3)
C23	0.020 (3)	0.027 (3)	0.024 (3)	−0.001 (2)	0.010 (3)	−0.004 (3)
C24	0.032 (4)	0.028 (3)	0.017 (3)	−0.004 (3)	0.006 (3)	−0.005 (3)
C25	0.019 (3)	0.035 (4)	0.021 (3)	0.004 (3)	0.005 (3)	0.008 (3)
C26	0.020 (3)	0.022 (3)	0.035 (4)	−0.005 (3)	0.016 (3)	−0.006 (3)
C27	0.017 (3)	0.024 (3)	0.023 (3)	−0.003 (2)	0.014 (3)	−0.001 (2)
C28	0.021 (3)	0.014 (3)	0.033 (4)	−0.001 (2)	0.014 (3)	−0.008 (3)
C29	0.017 (3)	0.022 (3)	0.019 (3)	−0.006 (2)	0.005 (3)	−0.002 (3)
C30	0.030 (4)	0.030 (4)	0.026 (4)	−0.001 (3)	0.016 (3)	0.000 (3)
C31	0.048 (5)	0.041 (4)	0.066 (6)	0.017 (4)	0.031 (5)	0.015 (4)
C32	0.080 (8)	0.059 (6)	0.068 (7)	−0.008 (6)	0.031 (6)	0.015 (5)
C33	0.025 (3)	0.023 (3)	0.026 (3)	−0.002 (3)	0.013 (3)	0.004 (3)
C34	0.013 (3)	0.024 (3)	0.023 (3)	−0.001 (2)	0.008 (2)	−0.004 (2)
C35	0.013 (3)	0.032 (3)	0.027 (3)	−0.001 (2)	0.009 (3)	−0.004 (3)
C36	0.025 (4)	0.040 (4)	0.021 (4)	0.002 (3)	0.005 (3)	−0.004 (3)
C37	0.031 (4)	0.042 (4)	0.025 (4)	−0.006 (3)	0.019 (3)	−0.010 (3)
C38	0.026 (4)	0.027 (3)	0.057 (6)	0.004 (3)	0.017 (4)	−0.011 (3)
C39	0.024 (3)	0.032 (3)	0.048 (5)	0.007 (3)	0.026 (4)	0.004 (3)
C40	0.029 (4)	0.071 (6)	0.030 (4)	0.007 (4)	0.013 (3)	0.000 (4)
C41	0.029 (4)	0.053 (5)	0.032 (4)	0.011 (3)	0.007 (3)	−0.017 (4)
C42	0.027 (4)	0.035 (4)	0.042 (4)	−0.006 (3)	0.009 (3)	−0.008 (3)
C43	0.017 (4)	0.056 (5)	0.030 (4)	−0.003 (3)	0.003 (3)	−0.002 (4)
C44	0.024 (4)	0.063 (5)	0.021 (4)	0.015 (4)	0.005 (3)	0.007 (3)
Br2	0.0361 (5)	0.0623 (6)	0.0334 (4)	0.0137 (4)	0.0126 (4)	−0.0062 (4)
Br3	0.0405 (5)	0.0342 (5)	0.0392 (5)	0.0055 (4)	0.0054 (4)	−0.0105 (4)
Br4	0.0439 (5)	0.0414 (5)	0.0418 (5)	−0.0085 (4)	0.0300 (5)	−0.0053 (4)
Br5	0.0197 (4)	0.0515 (5)	0.0361 (5)	0.0053 (4)	0.0099 (4)	0.0034 (5)
Br3A	0.100 (8)	0.130 (8)	0.122 (10)	0.023 (7)	0.091 (9)	0.026 (8)
Br4A	0.164 (15)	0.101 (9)	0.162 (14)	0.003 (8)	0.119 (13)	−0.032 (9)
Br5A	0.055 (5)	0.147 (9)	0.069 (7)	−0.013 (6)	0.002 (5)	0.042 (7)
Fe3	0.0318 (7)	0.0357 (5)	0.0283 (6)	0.0002 (5)	0.0110 (5)	−0.0022 (5)

Geometric parameters (Å, º)

Br1—Ni1	2.4407 (10)	C13—C17	1.450 (10)
Ni1—N1	2.047 (5)	C14—C15	1.431 (11)
Ni1—N4	2.058 (5)	C14—H14	0.9500
Ni1—N3	2.092 (5)	C15—C16	1.415 (13)
Ni1—N6	2.105 (5)	C15—H15	0.9500
Fe1—C17	2.026 (7)	C16—C17	1.401 (10)
Fe1—C13	2.030 (6)	C16—H16	0.9500
Fe1—C19	2.032 (7)	C17—H17	0.9500
Fe1—C16	2.033 (8)	C18—C19	1.398 (11)
Fe1—C22	2.037 (8)	C18—C22	1.438 (11)
Fe1—C18	2.038 (7)	C18—H18	0.9500
Fe1—C14	2.042 (7)	C19—C20	1.416 (12)
Fe1—C21	2.047 (7)	C19—H19	0.9500
Fe1—C15	2.050 (8)	C20—C21	1.420 (12)
Fe1—C20	2.062 (7)	C20—H20	0.9500
Fe2—C35	2.031 (7)	C21—C22	1.376 (12)
Fe2—C41	2.038 (8)	C21—H21	0.9500
Fe2—C37	2.040 (7)	C22—H22	0.9500
Fe2—C40	2.042 (9)	C23—C24	1.381 (10)
Fe2—C44	2.047 (7)	C23—H23	0.9500
Fe2—C36	2.053 (7)	C24—C25	1.394 (10)
Fe2—C38	2.055 (8)	C24—H24	0.9500
Fe2—C43	2.057 (8)	C25—C26	1.411 (10)
Fe2—C39	2.058 (7)	C25—H25	0.9500
Fe2—C42	2.058 (8)	C26—C27	1.376 (9)
O1—C8	1.217 (9)	C26—H26	0.9500
O2—C8	1.307 (9)	C27—C28	1.510 (9)
O2—C9	1.473 (8)	C28—H28A	0.9900
O3—C30	1.201 (9)	C28—H28B	0.9900
O4—C30	1.330 (9)	C29—C33	1.366 (10)
O4—C31	1.475 (9)	C29—C30	1.503 (9)
N1—C5	1.331 (8)	C31—C32	1.513 (4)
N1—C1	1.363 (9)	C31—H31A	0.9900
N2—N3	1.346 (7)	C31—H31B	0.9900
N2—C7	1.360 (9)	C32—H32A	0.9800
N2—C6	1.480 (8)	C32—H32B	0.9800
N3—C12	1.351 (8)	C32—H32C	0.9800
N4—C23	1.341 (9)	C33—C34	1.413 (9)
N4—C27	1.353 (8)	C33—H33	0.9500
N5—C29	1.356 (8)	C34—C35	1.459 (9)
N5—N6	1.358 (7)	C35—C36	1.427 (10)
N5—C28	1.464 (8)	C35—C39	1.435 (10)
N6—C34	1.335 (8)	C36—C37	1.438 (10)
C1—C2	1.356 (10)	C36—H36	0.9500
C1—H1	0.9500	C37—C38	1.420 (12)
C2—C3	1.378 (10)	C37—H37	0.9500
C2—H2	0.9500	C38—C39	1.436 (10)
C3—C4	1.353 (11)	C38—H38	0.9500
C3—H3	0.9500	C39—H39	0.9500
C4—C5	1.400 (9)	C40—C41	1.401 (13)
C4—H4	0.9500	C40—C44	1.445 (12)
C5—C6	1.510 (9)	C40—H40	0.9500
C6—H6A	0.9900	C41—C42	1.416 (13)
C6—H6B	0.9900	C41—H41	0.9500
C7—C11	1.405 (10)	C42—C43	1.402 (12)
C7—C8	1.482 (9)	C42—H42	0.9500
C9—C10	1.519 (4)	C43—C44	1.436 (12)
C9—H9A	0.9900	C43—H43	0.9500
C9—H9B	0.9900	C44—H44	0.9500
C10—H10A	0.9800	Br2—Fe3	2.3352 (13)
C10—H10B	0.9800	Br3—Fe3	2.3290 (16)
C10—H10C	0.9800	Br4—Fe3	2.3419 (16)
C11—C12	1.395 (9)	Br5—Fe3	2.2995 (16)
C11—H11	0.9500	Br3A—Fe3	1.943 (10)
C12—C13	1.451 (9)	Br4A—Fe3	2.553 (15)
C13—C14	1.430 (9)	Br5A—Fe3	2.560 (11)
N1—Ni1—N4	93.66 (19)	Fe1—C14—H14	126.4
N1—Ni1—N3	88.1 (2)	C16—C15—C14	108.2 (6)
N4—Ni1—N3	90.8 (2)	C16—C15—Fe1	69.1 (5)
N1—Ni1—N6	93.0 (2)	C14—C15—Fe1	69.2 (4)
N4—Ni1—N6	87.7 (2)	C16—C15—H15	125.9
N3—Ni1—N6	178.2 (2)	C14—C15—H15	125.9
N1—Ni1—Br1	129.90 (17)	Fe1—C15—H15	127.3
N4—Ni1—Br1	136.43 (16)	C17—C16—C15	109.3 (6)
N3—Ni1—Br1	90.97 (16)	C17—C16—Fe1	69.5 (4)
N6—Ni1—Br1	89.41 (15)	C15—C16—Fe1	70.3 (4)
C17—Fe1—C13	41.9 (3)	C17—C16—H16	125.4
C17—Fe1—C19	120.5 (3)	C15—C16—H16	125.4
C13—Fe1—C19	105.9 (3)	Fe1—C16—H16	126.3
C17—Fe1—C16	40.4 (3)	C16—C17—C13	107.6 (7)
C13—Fe1—C16	68.9 (3)	C16—C17—Fe1	70.1 (4)
C19—Fe1—C16	156.4 (3)	C13—C17—Fe1	69.2 (4)
C17—Fe1—C22	123.3 (4)	C16—C17—H17	126.2
C13—Fe1—C22	159.9 (3)	C13—C17—H17	126.2
C19—Fe1—C22	68.0 (3)	Fe1—C17—H17	126.0
C16—Fe1—C22	108.5 (3)	C19—C18—C22	106.8 (7)
C17—Fe1—C18	105.6 (3)	C19—C18—Fe1	69.7 (4)
C13—Fe1—C18	121.8 (3)	C22—C18—Fe1	69.3 (4)
C19—Fe1—C18	40.2 (3)	C19—C18—H18	126.6
C16—Fe1—C18	121.6 (3)	C22—C18—H18	126.6
C22—Fe1—C18	41.3 (3)	Fe1—C18—H18	126.0
C17—Fe1—C14	69.7 (3)	C18—C19—C20	109.1 (7)
C13—Fe1—C14	41.1 (3)	C18—C19—Fe1	70.1 (4)
C19—Fe1—C14	123.2 (3)	C20—C19—Fe1	70.9 (4)
C16—Fe1—C14	68.9 (3)	C18—C19—H19	125.5
C22—Fe1—C14	158.2 (3)	C20—C19—H19	125.5
C18—Fe1—C14	158.8 (3)	Fe1—C19—H19	125.1
C17—Fe1—C21	159.7 (3)	C19—C20—C21	106.8 (7)
C13—Fe1—C21	158.0 (3)	C19—C20—Fe1	68.6 (4)
C19—Fe1—C21	67.8 (3)	C21—C20—Fe1	69.2 (4)
C16—Fe1—C21	125.2 (3)	C19—C20—H20	126.6
C22—Fe1—C21	39.4 (3)	C21—C20—H20	126.6
C18—Fe1—C21	68.0 (3)	Fe1—C20—H20	127.1
C14—Fe1—C21	123.3 (3)	C22—C21—C20	109.0 (7)
C17—Fe1—C15	68.6 (3)	C22—C21—Fe1	69.9 (4)
C13—Fe1—C15	68.8 (3)	C20—C21—Fe1	70.4 (4)
C19—Fe1—C15	160.9 (4)	C22—C21—H21	125.5
C16—Fe1—C15	40.5 (4)	C20—C21—H21	125.5
C22—Fe1—C15	123.0 (3)	Fe1—C21—H21	125.8
C18—Fe1—C15	158.2 (3)	C21—C22—C18	108.5 (7)
C14—Fe1—C15	41.0 (3)	C21—C22—Fe1	70.7 (4)
C21—Fe1—C15	109.8 (3)	C18—C22—Fe1	69.4 (4)
C17—Fe1—C20	157.0 (3)	C21—C22—H22	125.8
C13—Fe1—C20	121.2 (3)	C18—C22—H22	125.8
C19—Fe1—C20	40.5 (4)	Fe1—C22—H22	125.7
C16—Fe1—C20	161.7 (4)	N4—C23—C24	123.3 (6)
C22—Fe1—C20	67.4 (3)	N4—C23—H23	118.3
C18—Fe1—C20	68.0 (3)	C24—C23—H23	118.3
C14—Fe1—C20	107.8 (3)	C23—C24—C25	118.1 (6)
C21—Fe1—C20	40.4 (3)	C23—C24—H24	121.0
C15—Fe1—C20	125.4 (4)	C25—C24—H24	121.0
C35—Fe2—C41	107.4 (3)	C24—C25—C26	118.8 (6)
C35—Fe2—C37	68.6 (3)	C24—C25—H25	120.6
C41—Fe2—C37	157.2 (3)	C26—C25—H25	120.6
C35—Fe2—C40	120.4 (3)	C27—C26—C25	119.2 (6)
C41—Fe2—C40	40.2 (4)	C27—C26—H26	120.4
C37—Fe2—C40	161.5 (4)	C25—C26—H26	120.4
C35—Fe2—C44	156.3 (3)	N4—C27—C26	121.7 (6)
C41—Fe2—C44	68.5 (3)	N4—C27—C28	115.6 (6)
C37—Fe2—C44	124.3 (3)	C26—C27—C28	122.6 (6)
C40—Fe2—C44	41.4 (3)	N5—C28—C27	109.1 (5)
C35—Fe2—C36	40.9 (3)	N5—C28—H28A	109.9
C41—Fe2—C36	121.0 (3)	C27—C28—H28A	109.9
C37—Fe2—C36	41.1 (3)	N5—C28—H28B	109.9
C40—Fe2—C36	155.7 (3)	C27—C28—H28B	109.9
C44—Fe2—C36	161.4 (3)	H28A—C28—H28B	108.3
C35—Fe2—C38	68.3 (3)	N5—C29—C33	107.5 (5)
C41—Fe2—C38	160.8 (4)	N5—C29—C30	127.3 (6)
C37—Fe2—C38	40.6 (3)	C33—C29—C30	124.8 (6)
C40—Fe2—C38	124.5 (4)	O3—C30—O4	126.6 (7)
C44—Fe2—C38	107.4 (3)	O3—C30—C29	121.4 (6)
C36—Fe2—C38	68.8 (4)	O4—C30—C29	111.8 (6)
C35—Fe2—C43	161.0 (3)	O4—C31—C32	105.6 (8)
C41—Fe2—C43	67.8 (3)	O4—C31—H31A	110.6
C37—Fe2—C43	108.3 (3)	C32—C31—H31A	110.6
C40—Fe2—C43	68.6 (3)	O4—C31—H31B	110.6
C44—Fe2—C43	40.9 (3)	C32—C31—H31B	110.6
C36—Fe2—C43	124.5 (3)	H31A—C31—H31B	108.7
C38—Fe2—C43	122.3 (3)	C29—C33—C34	105.9 (6)
C35—Fe2—C39	41.1 (3)	C29—C33—H33	127.0
C41—Fe2—C39	123.6 (3)	C34—C33—H33	127.0
C37—Fe2—C39	69.1 (3)	N6—C34—C33	109.3 (5)
C40—Fe2—C39	106.3 (4)	N6—C34—C35	123.7 (6)
C44—Fe2—C39	120.4 (4)	C33—C34—C35	126.9 (6)
C36—Fe2—C39	69.5 (3)	C36—C35—C39	110.0 (6)
C38—Fe2—C39	40.9 (3)	C36—C35—C34	123.4 (6)
C43—Fe2—C39	157.0 (3)	C39—C35—C34	126.6 (6)
C35—Fe2—C42	124.7 (3)	C36—C35—Fe2	70.4 (4)
C41—Fe2—C42	40.5 (4)	C39—C35—Fe2	70.4 (4)
C37—Fe2—C42	122.1 (3)	C34—C35—Fe2	126.2 (5)
C40—Fe2—C42	68.0 (4)	C35—C36—C37	106.3 (7)
C44—Fe2—C42	68.2 (3)	C35—C36—Fe2	68.7 (4)
C36—Fe2—C42	107.7 (3)	C37—C36—Fe2	68.9 (4)
C38—Fe2—C42	157.3 (3)	C35—C36—H36	126.8
C43—Fe2—C42	39.8 (3)	C37—C36—H36	126.8
C39—Fe2—C42	160.9 (3)	Fe2—C36—H36	127.0
C8—O2—C9	118.0 (6)	C38—C37—C36	108.7 (6)
C30—O4—C31	115.9 (6)	C38—C37—Fe2	70.3 (4)
C5—N1—C1	117.9 (5)	C36—C37—Fe2	69.9 (4)
C5—N1—Ni1	120.7 (4)	C38—C37—H37	125.6
C1—N1—Ni1	121.3 (4)	C36—C37—H37	125.6
N3—N2—C7	111.2 (5)	Fe2—C37—H37	125.7
N3—N2—C6	118.8 (5)	C37—C38—C39	108.8 (7)
C7—N2—C6	130.0 (6)	C37—C38—Fe2	69.1 (4)
N2—N3—C12	106.7 (5)	C39—C38—Fe2	69.7 (4)
N2—N3—Ni1	118.8 (4)	C37—C38—H38	125.6
C12—N3—Ni1	134.3 (4)	C39—C38—H38	125.6
C23—N4—C27	118.9 (6)	Fe2—C38—H38	127.2
C23—N4—Ni1	120.9 (4)	C35—C39—C38	106.1 (7)
C27—N4—Ni1	120.1 (4)	C35—C39—Fe2	68.5 (4)
C29—N5—N6	110.5 (5)	C38—C39—Fe2	69.5 (4)
C29—N5—C28	131.4 (5)	C35—C39—H39	127.0
N6—N5—C28	118.1 (5)	C38—C39—H39	127.0
C34—N6—N5	106.8 (5)	Fe2—C39—H39	126.7
C34—N6—Ni1	135.6 (4)	C41—C40—C44	107.8 (8)
N5—N6—Ni1	116.8 (4)	C41—C40—Fe2	69.7 (5)
C2—C1—N1	122.1 (6)	C44—C40—Fe2	69.5 (5)
C2—C1—H1	119.0	C41—C40—H40	126.1
N1—C1—H1	119.0	C44—C40—H40	126.1
C1—C2—C3	120.5 (7)	Fe2—C40—H40	126.2
C1—C2—H2	119.7	C40—C41—C42	108.9 (7)
C3—C2—H2	119.7	C40—C41—Fe2	70.1 (5)
C4—C3—C2	117.6 (7)	C42—C41—Fe2	70.5 (4)
C4—C3—H3	121.2	C40—C41—H41	125.5
C2—C3—H3	121.2	C42—C41—H41	125.5
C3—C4—C5	120.7 (6)	Fe2—C41—H41	125.4
C3—C4—H4	119.7	C43—C42—C41	108.2 (8)
C5—C4—H4	119.7	C43—C42—Fe2	70.1 (4)
N1—C5—C4	121.1 (6)	C41—C42—Fe2	69.0 (5)
N1—C5—C6	118.0 (6)	C43—C42—H42	125.9
C4—C5—C6	120.8 (5)	C41—C42—H42	125.9
N2—C6—C5	110.7 (5)	Fe2—C42—H42	126.6
N2—C6—H6A	109.5	C42—C43—C44	108.5 (8)
C5—C6—H6A	109.5	C42—C43—Fe2	70.1 (4)
N2—C6—H6B	109.5	C44—C43—Fe2	69.1 (4)
C5—C6—H6B	109.5	C42—C43—H43	125.8
H6A—C6—H6B	108.1	C44—C43—H43	125.8
N2—C7—C11	106.5 (6)	Fe2—C43—H43	126.6
N2—C7—C8	129.7 (6)	C43—C44—C40	106.6 (7)
C11—C7—C8	123.8 (6)	C43—C44—Fe2	69.9 (4)
O1—C8—O2	125.4 (6)	C40—C44—Fe2	69.1 (5)
O1—C8—C7	120.9 (6)	C43—C44—H44	126.7
O2—C8—C7	113.7 (6)	C40—C44—H44	126.7
O2—C9—C10	108.0 (6)	Fe2—C44—H44	125.8
O2—C9—H9A	110.1	Br3A—Fe3—Br5	136.5 (5)
C10—C9—H9A	110.1	Br3A—Fe3—Br3	57.9 (4)
O2—C9—H9B	110.1	Br5—Fe3—Br3	109.01 (6)
C10—C9—H9B	110.1	Br3A—Fe3—Br2	115.5 (5)
H9A—C9—H9B	108.4	Br5—Fe3—Br2	107.98 (6)
C12—C11—C7	105.5 (6)	Br3—Fe3—Br2	109.57 (6)
C12—C11—H11	127.2	Br3A—Fe3—Br4	51.0 (3)
C7—C11—H11	127.2	Br5—Fe3—Br4	113.52 (7)
N3—C12—C11	109.9 (6)	Br3—Fe3—Br4	108.00 (7)
N3—C12—C13	122.9 (6)	Br2—Fe3—Br4	108.71 (6)
C11—C12—C13	127.1 (6)	Br3A—Fe3—Br4A	115.1 (5)
C14—C13—C17	107.6 (6)	Br5—Fe3—Br4A	49.9 (3)
C14—C13—C12	124.5 (7)	Br3—Fe3—Br4A	145.7 (4)
C17—C13—C12	127.8 (6)	Br2—Fe3—Br4A	103.4 (4)
C14—C13—Fe1	69.9 (4)	Br4—Fe3—Br4A	68.7 (3)
C17—C13—Fe1	68.9 (4)	Br3A—Fe3—Br5A	117.6 (6)
C12—C13—Fe1	124.7 (5)	Br5—Fe3—Br5A	45.0 (3)
C13—C14—C15	107.4 (7)	Br3—Fe3—Br5A	66.9 (3)
C13—C14—Fe1	69.0 (4)	Br2—Fe3—Br5A	108.0 (3)
C15—C14—Fe1	69.8 (5)	Br4—Fe3—Br5A	142.2 (3)
C13—C14—H14	126.3	Br4A—Fe3—Br5A	94.5 (4)
C15—C14—H14	126.3
N4—Ni1—N1—C5	−127.2 (5)	Fe1—C18—C22—C21	60.2 (6)
N3—Ni1—N1—C5	−36.5 (5)	C19—C18—C22—Fe1	−59.9 (5)
N6—Ni1—N1—C5	144.9 (5)	C17—Fe1—C22—C21	165.6 (4)
Br1—Ni1—N1—C5	53.2 (5)	C13—Fe1—C22—C21	−157.4 (8)
N4—Ni1—N1—C1	49.3 (6)	C19—Fe1—C22—C21	−81.4 (5)
N3—Ni1—N1—C1	140.0 (5)	C16—Fe1—C22—C21	123.4 (5)
N6—Ni1—N1—C1	−38.6 (5)	C18—Fe1—C22—C21	−119.3 (7)
Br1—Ni1—N1—C1	−130.3 (5)	C14—Fe1—C22—C21	44.2 (11)
C7—N2—N3—C12	3.5 (8)	C15—Fe1—C22—C21	81.0 (6)
C6—N2—N3—C12	−178.3 (6)	C20—Fe1—C22—C21	−37.5 (5)
C7—N2—N3—Ni1	−172.9 (4)	C17—Fe1—C22—C18	−75.1 (6)
C6—N2—N3—Ni1	5.3 (8)	C13—Fe1—C22—C18	−38.1 (11)
N1—Ni1—N3—N2	36.3 (5)	C19—Fe1—C22—C18	37.9 (5)
N4—Ni1—N3—N2	130.0 (5)	C16—Fe1—C22—C18	−117.2 (5)
Br1—Ni1—N3—N2	−93.5 (5)	C14—Fe1—C22—C18	163.5 (8)
N1—Ni1—N3—C12	−138.8 (7)	C21—Fe1—C22—C18	119.3 (7)
N4—Ni1—N3—C12	−45.1 (7)	C15—Fe1—C22—C18	−159.6 (5)
Br1—Ni1—N3—C12	91.3 (7)	C20—Fe1—C22—C18	81.8 (5)
N1—Ni1—N4—C23	44.4 (5)	C27—N4—C23—C24	1.5 (10)
N3—Ni1—N4—C23	−43.8 (5)	Ni1—N4—C23—C24	−176.0 (5)
N6—Ni1—N4—C23	137.2 (5)	N4—C23—C24—C25	−3.2 (11)
Br1—Ni1—N4—C23	−136.1 (4)	C23—C24—C25—C26	2.7 (11)
N1—Ni1—N4—C27	−133.1 (5)	C24—C25—C26—C27	−0.8 (10)
N3—Ni1—N4—C27	138.7 (5)	C23—N4—C27—C26	0.6 (9)
N6—Ni1—N4—C27	−40.2 (5)	Ni1—N4—C27—C26	178.1 (5)
Br1—Ni1—N4—C27	46.5 (6)	C23—N4—C27—C28	−179.0 (6)
C29—N5—N6—C34	0.0 (7)	Ni1—N4—C27—C28	−1.5 (7)
C28—N5—N6—C34	−177.9 (6)	C25—C26—C27—N4	−0.9 (10)
C29—N5—N6—Ni1	−171.1 (4)	C25—C26—C27—C28	178.7 (6)
C28—N5—N6—Ni1	11.0 (7)	C29—N5—C28—C27	112.3 (7)
N1—Ni1—N6—C34	−38.9 (7)	N6—N5—C28—C27	−70.4 (7)
N4—Ni1—N6—C34	−132.4 (7)	N4—C27—C28—N5	64.4 (7)
Br1—Ni1—N6—C34	91.0 (7)	C26—C27—C28—N5	−115.2 (6)
N1—Ni1—N6—N5	128.9 (4)	N6—N5—C29—C33	−0.1 (8)
N4—Ni1—N6—N5	35.3 (5)	C28—N5—C29—C33	177.4 (7)
Br1—Ni1—N6—N5	−101.2 (4)	N6—N5—C29—C30	172.4 (6)
C5—N1—C1—C2	−2.7 (10)	C28—N5—C29—C30	−10.1 (12)
Ni1—N1—C1—C2	−179.3 (6)	C31—O4—C30—O3	11.9 (12)
N1—C1—C2—C3	1.4 (11)	C31—O4—C30—C29	−163.2 (7)
C1—C2—C3—C4	1.0 (11)	N5—C29—C30—O3	176.4 (7)
C2—C3—C4—C5	−2.1 (11)	C33—C29—C30—O3	−12.3 (12)
C1—N1—C5—C4	1.6 (9)	N5—C29—C30—O4	−8.2 (10)
Ni1—N1—C5—C4	178.2 (5)	C33—C29—C30—O4	163.1 (7)
C1—N1—C5—C6	178.7 (6)	C30—O4—C31—C32	−86.7 (9)
Ni1—N1—C5—C6	−4.6 (7)	N5—C29—C33—C34	0.1 (8)
C3—C4—C5—N1	0.8 (10)	C30—C29—C33—C34	−172.6 (6)
C3—C4—C5—C6	−176.3 (7)	N5—N6—C34—C33	0.1 (8)
N3—N2—C6—C5	−62.0 (8)	Ni1—N6—C34—C33	168.7 (5)
C7—N2—C6—C5	115.9 (7)	N5—N6—C34—C35	−176.7 (6)
N1—C5—C6—N2	62.2 (7)	Ni1—N6—C34—C35	−8.0 (11)
C4—C5—C6—N2	−120.7 (6)	C29—C33—C34—N6	−0.1 (8)
N3—N2—C7—C11	−2.6 (8)	C29—C33—C34—C35	176.5 (6)
C6—N2—C7—C11	179.4 (6)	N6—C34—C35—C36	144.1 (7)
N3—N2—C7—C8	178.5 (6)	C33—C34—C35—C36	−32.0 (11)
C6—N2—C7—C8	0.5 (12)	N6—C34—C35—C39	−35.3 (11)
C9—O2—C8—O1	0.2 (12)	C33—C34—C35—C39	148.5 (8)
C9—O2—C8—C7	−178.2 (6)	N6—C34—C35—Fe2	−126.8 (6)
N2—C7—C8—O1	177.5 (7)	C33—C34—C35—Fe2	57.0 (10)
C11—C7—C8—O1	−1.2 (11)	C41—Fe2—C35—C36	117.6 (5)
N2—C7—C8—O2	−3.9 (11)	C37—Fe2—C35—C36	−38.5 (4)
C11—C7—C8—O2	177.4 (7)	C40—Fe2—C35—C36	159.5 (5)
C8—O2—C9—C10	106.9 (8)	C44—Fe2—C35—C36	−166.3 (8)
N2—C7—C11—C12	0.8 (8)	C38—Fe2—C35—C36	−82.3 (5)
C8—C7—C11—C12	179.7 (6)	C43—Fe2—C35—C36	45.6 (11)
N2—N3—C12—C11	−2.9 (8)	C39—Fe2—C35—C36	−120.8 (6)
Ni1—N3—C12—C11	172.6 (5)	C42—Fe2—C35—C36	76.5 (5)
N2—N3—C12—C13	179.2 (6)	C41—Fe2—C35—C39	−121.5 (5)
Ni1—N3—C12—C13	−5.3 (11)	C37—Fe2—C35—C39	82.3 (4)
C7—C11—C12—N3	1.3 (8)	C40—Fe2—C35—C39	−79.7 (5)
C7—C11—C12—C13	179.1 (6)	C44—Fe2—C35—C39	−45.5 (9)
N3—C12—C13—C14	148.3 (7)	C36—Fe2—C35—C39	120.8 (6)
C11—C12—C13—C14	−29.3 (11)	C38—Fe2—C35—C39	38.5 (5)
N3—C12—C13—C17	−34.5 (10)	C43—Fe2—C35—C39	166.4 (9)
C11—C12—C13—C17	148.0 (7)	C42—Fe2—C35—C39	−162.7 (5)
N3—C12—C13—Fe1	−123.5 (7)	C41—Fe2—C35—C34	0.0 (7)
C11—C12—C13—Fe1	59.0 (9)	C37—Fe2—C35—C34	−156.1 (7)
C17—Fe1—C13—C14	−119.1 (6)	C40—Fe2—C35—C34	41.9 (8)
C19—Fe1—C13—C14	122.6 (5)	C44—Fe2—C35—C34	76.1 (10)
C16—Fe1—C13—C14	−81.6 (5)	C36—Fe2—C35—C34	−117.6 (8)
C22—Fe1—C13—C14	−168.0 (9)	C38—Fe2—C35—C34	160.1 (7)
C18—Fe1—C13—C14	163.4 (5)	C43—Fe2—C35—C34	−72.0 (12)
C21—Fe1—C13—C14	52.5 (9)	C39—Fe2—C35—C34	121.6 (8)
C15—Fe1—C13—C14	−38.0 (5)	C42—Fe2—C35—C34	−41.1 (7)
C20—Fe1—C13—C14	81.4 (5)	C39—C35—C36—C37	−0.5 (8)
C19—Fe1—C13—C17	−118.2 (5)	C34—C35—C36—C37	180.0 (6)
C16—Fe1—C13—C17	37.5 (4)	Fe2—C35—C36—C37	58.9 (5)
C22—Fe1—C13—C17	−48.9 (11)	C39—C35—C36—Fe2	−59.5 (5)
C18—Fe1—C13—C17	−77.5 (5)	C34—C35—C36—Fe2	121.0 (6)
C14—Fe1—C13—C17	119.1 (6)	C41—Fe2—C36—C35	−80.7 (5)
C21—Fe1—C13—C17	171.6 (7)	C37—Fe2—C36—C35	118.2 (6)
C15—Fe1—C13—C17	81.1 (5)	C40—Fe2—C36—C35	−47.3 (10)
C20—Fe1—C13—C17	−159.5 (5)	C44—Fe2—C36—C35	162.7 (10)
C17—Fe1—C13—C12	122.1 (8)	C38—Fe2—C36—C35	80.9 (5)
C19—Fe1—C13—C12	3.9 (7)	C43—Fe2—C36—C35	−163.6 (4)
C16—Fe1—C13—C12	159.6 (7)	C39—Fe2—C36—C35	37.0 (4)
C22—Fe1—C13—C12	73.3 (11)	C42—Fe2—C36—C35	−122.9 (4)
C18—Fe1—C13—C12	44.6 (7)	C35—Fe2—C36—C37	−118.2 (6)
C14—Fe1—C13—C12	−118.7 (8)	C41—Fe2—C36—C37	161.1 (4)
C21—Fe1—C13—C12	−66.2 (10)	C40—Fe2—C36—C37	−165.5 (8)
C15—Fe1—C13—C12	−156.8 (7)	C44—Fe2—C36—C37	44.4 (13)
C20—Fe1—C13—C12	−37.3 (7)	C38—Fe2—C36—C37	−37.3 (4)
C17—C13—C14—C15	0.8 (8)	C43—Fe2—C36—C37	78.1 (5)
C12—C13—C14—C15	178.5 (6)	C39—Fe2—C36—C37	−81.2 (4)
Fe1—C13—C14—C15	59.5 (5)	C42—Fe2—C36—C37	118.8 (5)
C17—C13—C14—Fe1	−58.8 (5)	C35—C36—C37—C38	1.0 (8)
C12—C13—C14—Fe1	119.0 (6)	Fe2—C36—C37—C38	59.8 (6)
C17—Fe1—C14—C13	38.5 (4)	C35—C36—C37—Fe2	−58.8 (5)
C19—Fe1—C14—C13	−75.4 (5)	C35—Fe2—C37—C38	−81.3 (5)
C16—Fe1—C14—C13	81.7 (5)	C41—Fe2—C37—C38	−165.2 (7)
C22—Fe1—C14—C13	168.9 (8)	C40—Fe2—C37—C38	41.5 (12)
C18—Fe1—C14—C13	−42.4 (11)	C44—Fe2—C37—C38	76.1 (5)
C21—Fe1—C14—C13	−159.2 (4)	C36—Fe2—C37—C38	−119.6 (6)
C15—Fe1—C14—C13	118.8 (6)	C43—Fe2—C37—C38	118.6 (5)
C20—Fe1—C14—C13	−117.3 (5)	C39—Fe2—C37—C38	−37.1 (4)
C17—Fe1—C14—C15	−80.3 (5)	C42—Fe2—C37—C38	160.3 (4)
C13—Fe1—C14—C15	−118.8 (6)	C35—Fe2—C37—C36	38.3 (4)
C19—Fe1—C14—C15	165.8 (5)	C41—Fe2—C37—C36	−45.7 (10)
C16—Fe1—C14—C15	−37.0 (5)	C40—Fe2—C37—C36	161.0 (10)
C22—Fe1—C14—C15	50.1 (11)	C44—Fe2—C37—C36	−164.3 (5)
C18—Fe1—C14—C15	−161.1 (8)	C38—Fe2—C37—C36	119.6 (6)
C21—Fe1—C14—C15	82.0 (5)	C43—Fe2—C37—C36	−121.8 (5)
C20—Fe1—C14—C15	123.9 (5)	C39—Fe2—C37—C36	82.5 (5)
C13—C14—C15—C16	−0.7 (9)	C42—Fe2—C37—C36	−80.1 (5)
Fe1—C14—C15—C16	58.3 (6)	C36—C37—C38—C39	−1.1 (9)
C13—C14—C15—Fe1	−59.0 (5)	Fe2—C37—C38—C39	58.5 (6)
C17—Fe1—C15—C16	−36.8 (4)	C36—C37—C38—Fe2	−59.6 (5)
C13—Fe1—C15—C16	−82.0 (5)	C35—Fe2—C38—C37	81.9 (5)
C19—Fe1—C15—C16	−159.2 (9)	C41—Fe2—C38—C37	162.5 (9)
C22—Fe1—C15—C16	79.7 (6)	C40—Fe2—C38—C37	−165.2 (5)
C18—Fe1—C15—C16	41.5 (10)	C44—Fe2—C38—C37	−122.8 (5)
C14—Fe1—C15—C16	−120.2 (6)	C36—Fe2—C38—C37	37.8 (4)
C21—Fe1—C15—C16	121.5 (5)	C43—Fe2—C38—C37	−80.4 (5)
C20—Fe1—C15—C16	164.0 (5)	C39—Fe2—C38—C37	120.7 (7)
C17—Fe1—C15—C14	83.3 (5)	C42—Fe2—C38—C37	−47.6 (11)
C13—Fe1—C15—C14	38.2 (4)	C35—Fe2—C38—C39	−38.7 (5)
C19—Fe1—C15—C14	−39.1 (12)	C41—Fe2—C38—C39	41.9 (12)
C16—Fe1—C15—C14	120.2 (6)	C37—Fe2—C38—C39	−120.7 (7)
C22—Fe1—C15—C14	−160.1 (5)	C40—Fe2—C38—C39	74.1 (6)
C18—Fe1—C15—C14	161.7 (8)	C44—Fe2—C38—C39	116.5 (5)
C21—Fe1—C15—C14	−118.4 (5)	C36—Fe2—C38—C39	−82.8 (5)
C20—Fe1—C15—C14	−75.8 (5)	C43—Fe2—C38—C39	158.9 (5)
C14—C15—C16—C17	0.5 (9)	C42—Fe2—C38—C39	−168.3 (8)
Fe1—C15—C16—C17	58.8 (5)	C36—C35—C39—C38	−0.1 (9)
C14—C15—C16—Fe1	−58.3 (5)	C34—C35—C39—C38	179.3 (7)
C13—Fe1—C16—C17	−38.9 (5)	Fe2—C35—C39—C38	−59.6 (5)
C19—Fe1—C16—C17	42.7 (10)	C36—C35—C39—Fe2	59.4 (5)
C22—Fe1—C16—C17	120.0 (5)	C34—C35—C39—Fe2	−121.1 (7)
C18—Fe1—C16—C17	76.4 (5)	C37—C38—C39—C35	0.8 (9)
C14—Fe1—C16—C17	−83.1 (5)	Fe2—C38—C39—C35	58.9 (5)
C21—Fe1—C16—C17	160.4 (5)	C37—C38—C39—Fe2	−58.1 (6)
C15—Fe1—C16—C17	−120.5 (7)	C41—Fe2—C39—C35	77.5 (5)
C20—Fe1—C16—C17	−166.1 (9)	C37—Fe2—C39—C35	−81.0 (5)
C17—Fe1—C16—C15	120.5 (7)	C40—Fe2—C39—C35	117.9 (5)
C13—Fe1—C16—C15	81.6 (5)	C44—Fe2—C39—C35	160.6 (4)
C19—Fe1—C16—C15	163.2 (7)	C36—Fe2—C39—C35	−36.9 (4)
C22—Fe1—C16—C15	−119.6 (5)	C38—Fe2—C39—C35	−117.8 (7)
C18—Fe1—C16—C15	−163.2 (4)	C43—Fe2—C39—C35	−168.7 (8)
C14—Fe1—C16—C15	37.4 (4)	C42—Fe2—C39—C35	48.4 (12)
C21—Fe1—C16—C15	−79.2 (5)	C35—Fe2—C39—C38	117.8 (7)
C20—Fe1—C16—C15	−45.7 (12)	C41—Fe2—C39—C38	−164.7 (5)
C15—C16—C17—C13	0.0 (8)	C37—Fe2—C39—C38	36.8 (5)
Fe1—C16—C17—C13	59.3 (5)	C40—Fe2—C39—C38	−124.3 (5)
C15—C16—C17—Fe1	−59.3 (6)	C44—Fe2—C39—C38	−81.6 (6)
C14—C13—C17—C16	−0.5 (8)	C36—Fe2—C39—C38	80.9 (6)
C12—C13—C17—C16	−178.1 (6)	C43—Fe2—C39—C38	−51.0 (11)
Fe1—C13—C17—C16	−59.9 (5)	C42—Fe2—C39—C38	166.1 (10)
C14—C13—C17—Fe1	59.4 (5)	C35—Fe2—C40—C41	−80.9 (6)
C12—C13—C17—Fe1	−118.3 (7)	C37—Fe2—C40—C41	164.3 (9)
C13—Fe1—C17—C16	118.7 (7)	C44—Fe2—C40—C41	119.1 (7)
C19—Fe1—C17—C16	−161.7 (5)	C36—Fe2—C40—C41	−47.0 (11)
C22—Fe1—C17—C16	−79.3 (6)	C38—Fe2—C40—C41	−164.2 (5)
C18—Fe1—C17—C16	−120.8 (5)	C43—Fe2—C40—C41	80.5 (5)
C14—Fe1—C17—C16	81.0 (5)	C39—Fe2—C40—C41	−123.2 (5)
C21—Fe1—C17—C16	−52.3 (11)	C42—Fe2—C40—C41	37.5 (5)
C15—Fe1—C17—C16	37.0 (5)	C35—Fe2—C40—C44	160.0 (5)
C20—Fe1—C17—C16	168.9 (8)	C41—Fe2—C40—C44	−119.1 (7)
C19—Fe1—C17—C13	79.6 (5)	C37—Fe2—C40—C44	45.2 (13)
C16—Fe1—C17—C13	−118.7 (7)	C36—Fe2—C40—C44	−166.1 (8)
C22—Fe1—C17—C13	162.0 (4)	C38—Fe2—C40—C44	76.7 (6)
C18—Fe1—C17—C13	120.5 (4)	C43—Fe2—C40—C44	−38.6 (5)
C14—Fe1—C17—C13	−37.8 (4)	C39—Fe2—C40—C44	117.7 (5)
C21—Fe1—C17—C13	−171.0 (8)	C42—Fe2—C40—C44	−81.6 (6)
C15—Fe1—C17—C13	−81.7 (5)	C44—C40—C41—C42	−0.8 (9)
C20—Fe1—C17—C13	50.2 (10)	Fe2—C40—C41—C42	−60.0 (5)
C17—Fe1—C18—C19	−119.1 (5)	C44—C40—C41—Fe2	59.3 (6)
C13—Fe1—C18—C19	−76.5 (6)	C35—Fe2—C41—C40	116.9 (5)
C16—Fe1—C18—C19	−159.9 (5)	C37—Fe2—C41—C40	−167.2 (7)
C22—Fe1—C18—C19	117.9 (7)	C44—Fe2—C41—C40	−38.4 (5)
C14—Fe1—C18—C19	−45.1 (11)	C36—Fe2—C41—C40	159.5 (5)
C21—Fe1—C18—C19	81.3 (5)	C38—Fe2—C41—C40	43.0 (12)
C15—Fe1—C18—C19	169.7 (8)	C43—Fe2—C41—C40	−82.7 (5)
C20—Fe1—C18—C19	37.5 (5)	C39—Fe2—C41—C40	74.6 (6)
C17—Fe1—C18—C22	123.0 (5)	C42—Fe2—C41—C40	−119.6 (7)
C13—Fe1—C18—C22	165.6 (5)	C35—Fe2—C41—C42	−123.5 (5)
C19—Fe1—C18—C22	−117.9 (7)	C37—Fe2—C41—C42	−47.6 (10)
C16—Fe1—C18—C22	82.1 (6)	C40—Fe2—C41—C42	119.6 (7)
C14—Fe1—C18—C22	−163.0 (8)	C44—Fe2—C41—C42	81.2 (5)
C21—Fe1—C18—C22	−36.6 (5)	C36—Fe2—C41—C42	−80.9 (5)
C15—Fe1—C18—C22	51.7 (11)	C38—Fe2—C41—C42	162.6 (9)
C20—Fe1—C18—C22	−80.4 (5)	C43—Fe2—C41—C42	37.0 (5)
C22—C18—C19—C20	−0.8 (8)	C39—Fe2—C41—C42	−165.8 (5)
Fe1—C18—C19—C20	−60.5 (5)	C40—C41—C42—C43	0.5 (9)
C22—C18—C19—Fe1	59.7 (5)	Fe2—C41—C42—C43	−59.3 (5)
C17—Fe1—C19—C18	77.7 (5)	C40—C41—C42—Fe2	59.8 (6)
C13—Fe1—C19—C18	120.8 (5)	C35—Fe2—C42—C43	−164.9 (5)
C16—Fe1—C19—C18	47.0 (10)	C41—Fe2—C42—C43	119.7 (7)
C22—Fe1—C19—C18	−39.0 (5)	C37—Fe2—C42—C43	−80.1 (6)
C14—Fe1—C19—C18	162.2 (4)	C40—Fe2—C42—C43	82.5 (6)
C21—Fe1—C19—C18	−81.6 (5)	C44—Fe2—C42—C43	37.7 (5)
C15—Fe1—C19—C18	−168.2 (9)	C36—Fe2—C42—C43	−123.0 (5)
C20—Fe1—C19—C18	−119.5 (7)	C38—Fe2—C42—C43	−45.5 (12)
C17—Fe1—C19—C20	−162.8 (5)	C39—Fe2—C42—C43	158.4 (10)
C13—Fe1—C19—C20	−119.7 (5)	C35—Fe2—C42—C41	75.4 (5)
C16—Fe1—C19—C20	166.5 (7)	C37—Fe2—C42—C41	160.2 (5)
C22—Fe1—C19—C20	80.5 (5)	C40—Fe2—C42—C41	−37.2 (5)
C18—Fe1—C19—C20	119.5 (7)	C44—Fe2—C42—C41	−82.0 (5)
C14—Fe1—C19—C20	−78.3 (5)	C36—Fe2—C42—C41	117.3 (5)
C21—Fe1—C19—C20	37.9 (5)	C38—Fe2—C42—C41	−165.2 (9)
C15—Fe1—C19—C20	−48.7 (12)	C43—Fe2—C42—C41	−119.7 (7)
C18—C19—C20—C21	1.1 (8)	C39—Fe2—C42—C41	38.7 (12)
Fe1—C19—C20—C21	−58.9 (5)	C41—C42—C43—C44	0.0 (9)
C18—C19—C20—Fe1	60.0 (5)	Fe2—C42—C43—C44	−58.6 (6)
C17—Fe1—C20—C19	40.7 (10)	C41—C42—C43—Fe2	58.7 (5)
C13—Fe1—C20—C19	77.5 (5)	C35—Fe2—C43—C42	41.2 (12)
C16—Fe1—C20—C19	−162.7 (9)	C41—Fe2—C43—C42	−37.5 (5)
C22—Fe1—C20—C19	−82.1 (5)	C37—Fe2—C43—C42	118.5 (5)
C18—Fe1—C20—C19	−37.3 (4)	C40—Fe2—C43—C42	−80.9 (6)
C14—Fe1—C20—C19	120.6 (5)	C44—Fe2—C43—C42	−119.9 (8)
C21—Fe1—C20—C19	−118.7 (6)	C36—Fe2—C43—C42	75.8 (6)
C15—Fe1—C20—C19	162.5 (5)	C38—Fe2—C43—C42	161.0 (5)
C17—Fe1—C20—C21	159.4 (8)	C39—Fe2—C43—C42	−162.0 (8)
C13—Fe1—C20—C21	−163.8 (4)	C35—Fe2—C43—C44	161.1 (8)
C19—Fe1—C20—C21	118.7 (6)	C41—Fe2—C43—C44	82.4 (6)
C16—Fe1—C20—C21	−44.1 (12)	C37—Fe2—C43—C44	−121.6 (5)
C22—Fe1—C20—C21	36.6 (5)	C40—Fe2—C43—C44	39.0 (5)
C18—Fe1—C20—C21	81.4 (5)	C36—Fe2—C43—C44	−164.3 (5)
C14—Fe1—C20—C21	−120.7 (5)	C38—Fe2—C43—C44	−79.1 (6)
C15—Fe1—C20—C21	−78.8 (5)	C39—Fe2—C43—C44	−42.1 (11)
C19—C20—C21—C22	−0.9 (8)	C42—Fe2—C43—C44	119.9 (8)
Fe1—C20—C21—C22	−59.5 (5)	C42—C43—C44—C40	−0.5 (9)
C19—C20—C21—Fe1	58.6 (5)	Fe2—C43—C44—C40	−59.7 (6)
C17—Fe1—C21—C22	−36.8 (11)	C42—C43—C44—Fe2	59.2 (5)
C13—Fe1—C21—C22	159.4 (7)	C41—C40—C44—C43	0.8 (9)
C19—Fe1—C21—C22	81.9 (5)	Fe2—C40—C44—C43	60.2 (6)
C16—Fe1—C21—C22	−75.6 (6)	C41—C40—C44—Fe2	−59.4 (6)
C18—Fe1—C21—C22	38.4 (5)	C35—Fe2—C44—C43	−164.8 (7)
C14—Fe1—C21—C22	−162.0 (5)	C41—Fe2—C44—C43	−80.4 (6)
C15—Fe1—C21—C22	−118.3 (5)	C37—Fe2—C44—C43	78.1 (6)
C20—Fe1—C21—C22	119.8 (7)	C40—Fe2—C44—C43	−117.7 (7)
C17—Fe1—C21—C20	−156.6 (9)	C36—Fe2—C44—C43	44.3 (13)
C13—Fe1—C21—C20	39.6 (10)	C38—Fe2—C44—C43	119.6 (5)
C19—Fe1—C21—C20	−37.9 (5)	C39—Fe2—C44—C43	162.3 (5)
C16—Fe1—C21—C20	164.5 (5)	C42—Fe2—C44—C43	−36.7 (5)
C22—Fe1—C21—C20	−119.8 (7)	C35—Fe2—C44—C40	−47.1 (10)
C18—Fe1—C21—C20	−81.5 (5)	C41—Fe2—C44—C40	37.3 (6)
C14—Fe1—C21—C20	78.2 (5)	C37—Fe2—C44—C40	−164.2 (5)
C15—Fe1—C21—C20	121.8 (5)	C36—Fe2—C44—C40	161.9 (10)
C20—C21—C22—C18	0.4 (9)	C38—Fe2—C44—C40	−122.7 (6)
Fe1—C21—C22—C18	−59.3 (5)	C43—Fe2—C44—C40	117.7 (7)
C20—C21—C22—Fe1	59.7 (5)	C39—Fe2—C44—C40	−80.0 (6)
C19—C18—C22—C21	0.2 (9)	C42—Fe2—C44—C40	81.0 (6)