Redetermination of the iron-zinc phase FeZn₁₃

In iron tridecazinc, the FeZn₁₃ unit cell contains two Zn₁₂ icosahedra which are Fe-centred and two Zn₂ dumb-bells coordinated by eight icosahedra. Zn₁₂ icosahedra form chains along the c axis by vertex-sharing, and are further interlinked through octahedra-sharing and vertex-to-vertex bonds.

S1. Comment

In our general study of icosahedron-based intermetallic phases, we have reinvestigated the Fe—Zn binary system. Several phases, cubic γ-Fe₃Zn₁₀ (Brandon et al., 1974) and monoclinic ζ-FeZn₁₃ (Brown, 1962), were known but their structures poorly determined while hexagonal δ-FeZn₁₀ was not yet structurally characterized. For FeZn₁₃, intensities have been determined visually from Weissenberg photographs and the structure refined in the monoclinic space group C2/m with reflections from the [010] and [001] projections. Agreement factors R(F) were 0.121 ([010] projection) and 0.098 ([001] projection). Such refinements based on a restricted number of intensities led to an incomplete description of the structure. Since the limited quality of data did not allow any atomic differentiation, positions 2(a) and 2(c) were ambiguously assigned to iron and/or zinc atoms. Difficulty in obtaining good quality single crystals (having sharp reflections) was underlined by Brown (1962) who prepared FeZn₁₃ by an electrochemical process. With a flux method, we have obtained needles which display satisfactory diffraction spots. Structural refinement has allowed location of iron atoms at only the 2(c) position, the centre of zinc icosahedron. In the structure, icosahedra are packed in chains along the c axis by sharing opposite vertices. Furthermore, their linking is achieved by octahedra sharing in planes parallel to (402) and by vertex to vertex bonding in planes parallel to (001). Each icosahedron is then surrounded by 12 alike units. Zn3 atoms form dumbbells which complement the metallic bonding.

S2. Experimental

Single crystals of FeZn₁₃ were obtained by using a flux method. A mixture Fe/Zn containing 98 at.% Zn was melted at 1000 K in a silica tube, homogenized for 10 d and then air quenched. The resulting ingot (2.9 g) was inserted with dried ZnCl₂ (5 g) in a silica tube, flame sealed, heated to 973 K for a week and then was cooled at the rate of 3 K h^- to room temperature for crystal growth. The nearly spherical ingot obtained displayed on its surface, at the interface with ZnCl₂, some small flat needles. Chemical analysis, FeZn_13.08 (6), indicated the ζ phase, which has a very narrow range in the phase diagram (Bastin et al., 1974, 1977).

S3. Refinement

Refinement with a Zn atom at 2(a) position and a Fe atom at the 2(c) position gives R(F) = 0.0417 while the opposite [Fe at 2(a) and Zn at 2(c)] leads to R(F)=0.534. Refinement of Fe/Zn statistical site occupation would give 86 (2)% Zn on 2(a) site and 91 (5)% Fe on 2(c) site with R(F) = 0.0415. Within the 3σ limits, we consider 2(a) and 2(c) sites fully occupied by Zn and Fe, respectively

Computing details

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: local program; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 1993).

Figures

Fig. 1. Representation of atomic packing in the FeZn13 unit cell.

'Iron-Zinc (1:13) alloy'

Crystal data

FeZn13	F(000) = 832
Mr = 905.66	Dx = 7.327 Mg m^−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71069 Å
a = 13.394 (3) Å	Cell parameters from 25 reflections
b = 7.5980 (9) Å	θ = 9.4–20.6°
c = 5.066 (2) Å	µ = 38.82 mm^−1
β = 127.23 (2)°	T = 293 K
V = 410.49 (19) Å^3	Triangular platelet, metallic grey
Z = 2	0.10 × 0.05 × 0.02 mm

Data collection

Nonius CAD-4 diffractometer	439 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.059
Graphite monochromator	θmax = 29.9°, θmin = 3.3°
ω–2θ scans	h = −18→18
Absorption correction: numerical (The absorption effects have been corrected using the numerical procedure provided by SHELX76; Sheldrick, 1976)	k = 0→10
Tmin = 0.118, Tmax = 0.462	l = −7→7
1091 measured reflections	3 standard reflections every 100 reflections
604 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.042	Calculated w = 1/[σ^2(Fo^2) + (0.0521P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.109	(Δ/σ)max < 0.001
S = 1.03	Δρmax = 2.15 e Å^−3
604 reflections	Δρmin = −1.50 e Å^−3
40 parameters	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0019 (5)

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
Zn1	0.0000	0.0000	0.0000	0.0134 (5)
Fe2	0.0000	0.0000	0.5000	0.0045 (5)
Zn3	0.11406 (12)	0.5000	0.2942 (3)	0.0109 (4)
Zn4	0.22002 (13)	0.0000	0.0693 (4)	0.0148 (4)
Zn5	0.07635 (9)	0.29477 (17)	0.8340 (3)	0.0172 (3)
Zn6	0.17545 (9)	0.17895 (15)	0.5486 (3)	0.0114 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0125 (9)	0.0216 (12)	0.0057 (9)	0.000	0.0052 (8)	0.000
Fe2	0.0058 (10)	0.0051 (11)	0.0014 (9)	0.000	0.0015 (8)	0.000
Zn3	0.0105 (7)	0.0086 (8)	0.0065 (6)	0.000	0.0013 (6)	0.000
Zn4	0.0122 (7)	0.0182 (9)	0.0063 (7)	0.000	0.0015 (6)	0.000
Zn5	0.0149 (5)	0.0156 (6)	0.0171 (6)	−0.0013 (4)	0.0076 (4)	−0.0092 (4)
Zn6	0.0114 (5)	0.0098 (5)	0.0129 (5)	−0.0010 (4)	0.0074 (4)	0.0015 (4)

Geometric parameters (Å, º)

Zn1—Fe2^i	2.5330 (10)	Zn3—Zn6^xiv	2.7775 (16)
Zn1—Fe2	2.5330 (10)	Zn3—Zn6^ix	2.7775 (16)
Zn1—Zn6	2.6819 (14)	Zn4—Zn3^ix	2.582 (2)
Zn1—Zn6^ii	2.6819 (14)	Zn4—Fe2^i	2.5919 (17)
Zn1—Zn6^iii	2.6819 (14)	Zn4—Zn6^v	2.6939 (19)
Zn1—Zn6^iv	2.6819 (14)	Zn4—Zn6^i	2.6939 (19)
Zn1—Zn4	2.7488 (17)	Zn4—Zn5^v	2.7137 (15)
Zn1—Zn4^ii	2.7488 (17)	Zn4—Zn5^i	2.7137 (15)
Zn1—Zn5^i	2.7946 (14)	Zn4—Zn6^ix	2.8945 (14)
Zn1—Zn5^v	2.7946 (14)	Zn4—Zn6^xv	2.8945 (14)
Zn1—Zn5^vi	2.7946 (14)	Zn4—Zn5^ix	2.9143 (18)
Zn1—Zn5^vii	2.7946 (14)	Zn4—Zn5^xv	2.9143 (18)
Fe2—Zn1	2.5330 (10)	Zn4—Zn6	3.139 (2)
Fe2—Zn1^viii	2.5330 (10)	Zn5—Zn3^viii	2.5878 (17)
Fe2—Zn4^ii	2.5919 (17)	Zn5—Zn6	2.6358 (17)
Fe2—Zn4^viii	2.5919 (17)	Zn5—Zn5^vii	2.694 (3)
Fe2—Zn6	2.5945 (11)	Zn5—Zn3^xiii	2.7119 (16)
Fe2—Zn6^vi	2.5945 (11)	Zn5—Zn4^viii	2.7137 (15)
Fe2—Zn6^iv	2.5945 (11)	Zn5—Zn1^viii	2.7946 (14)
Fe2—Zn6^vii	2.5945 (11)	Zn5—Zn6^vii	2.8277 (17)
Fe2—Zn5^vi	2.6136 (12)	Zn5—Zn6^xvi	2.8797 (18)
Fe2—Zn5	2.6136 (12)	Zn5—Zn4^ix	2.9143 (18)
Fe2—Zn5^vii	2.6136 (12)	Zn5—Zn5^xi	3.119 (3)
Fe2—Zn5^iv	2.6136 (12)	Zn5—Zn6^viii	3.135 (2)
Zn3—Zn4^ix	2.582 (2)	Zn6—Zn6^ix	2.567 (2)
Zn3—Zn5^i	2.5878 (17)	Zn6—Zn4^viii	2.6939 (19)
Zn3—Zn5^x	2.5878 (17)	Zn6—Zn6^iv	2.719 (2)
Zn3—Zn6^xi	2.6468 (13)	Zn6—Zn3^ix	2.7775 (16)
Zn3—Zn6	2.6468 (13)	Zn6—Zn5^vii	2.8277 (17)
Zn3—Zn3^xii	2.683 (3)	Zn6—Zn5^xvi	2.8797 (18)
Zn3—Zn5^vii	2.7119 (16)	Zn6—Zn4^ix	2.8945 (14)
Zn3—Zn5^xiii	2.7119 (16)	Zn6—Zn5^i	3.135 (2)
Fe2^i—Zn1—Fe2	180.0	Fe2^i—Zn4—Zn5^i	58.97 (4)
Fe2^i—Zn1—Zn6	120.41 (3)	Zn6^v—Zn4—Zn5^i	107.95 (6)
Fe2—Zn1—Zn6	59.59 (3)	Zn6^i—Zn4—Zn5^i	58.34 (4)
Fe2^i—Zn1—Zn6^ii	59.59 (3)	Zn5^v—Zn4—Zn5^i	111.24 (7)
Fe2—Zn1—Zn6^ii	120.41 (3)	Zn3^ix—Zn4—Zn1	101.86 (7)
Zn6—Zn1—Zn6^ii	180.0	Fe2^i—Zn4—Zn1	56.53 (4)
Fe2^i—Zn1—Zn6^iii	59.59 (3)	Zn6^v—Zn4—Zn1	106.83 (5)
Fe2—Zn1—Zn6^iii	120.41 (3)	Zn6^i—Zn4—Zn1	106.83 (5)
Zn6—Zn1—Zn6^iii	119.07 (5)	Zn5^v—Zn4—Zn1	61.54 (4)
Zn6^ii—Zn1—Zn6^iii	60.93 (5)	Zn5^i—Zn4—Zn1	61.54 (4)
Fe2^i—Zn1—Zn6^iv	120.41 (3)	Zn3^ix—Zn4—Zn6^ix	57.46 (3)
Fe2—Zn1—Zn6^iv	59.59 (3)	Fe2^i—Zn4—Zn6^ix	120.56 (4)
Zn6—Zn1—Zn6^iv	60.93 (5)	Zn6^v—Zn4—Zn6^ix	144.21 (6)
Zn6^ii—Zn1—Zn6^iv	119.07 (5)	Zn6^i—Zn4—Zn6^ix	87.73 (4)
Zn6^iii—Zn1—Zn6^iv	180.0	Zn5^v—Zn4—Zn6^ix	156.47 (7)
Fe2^i—Zn1—Zn4	58.60 (4)	Zn5^i—Zn4—Zn6^ix	61.69 (4)
Fe2—Zn1—Zn4	121.40 (4)	Zn1—Zn4—Zn6^ix	97.63 (4)
Zn6—Zn1—Zn4	70.62 (4)	Zn3^ix—Zn4—Zn6^xv	57.46 (4)
Zn6^ii—Zn1—Zn4	109.38 (4)	Fe2^i—Zn4—Zn6^xv	120.56 (4)
Zn6^iii—Zn1—Zn4	109.38 (4)	Zn6^v—Zn4—Zn6^xv	87.73 (4)
Zn6^iv—Zn1—Zn4	70.62 (4)	Zn6^i—Zn4—Zn6^xv	144.21 (6)
Fe2^i—Zn1—Zn4^ii	121.40 (4)	Zn5^v—Zn4—Zn6^xv	61.69 (4)
Fe2—Zn1—Zn4^ii	58.60 (4)	Zn5^i—Zn4—Zn6^xv	156.47 (7)
Zn6—Zn1—Zn4^ii	109.38 (4)	Zn1—Zn4—Zn6^xv	97.63 (4)
Zn6^ii—Zn1—Zn4^ii	70.62 (4)	Zn6^ix—Zn4—Zn6^xv	114.86 (7)
Zn6^iii—Zn1—Zn4^ii	70.62 (4)	Zn3^ix—Zn4—Zn5^ix	77.25 (5)
Zn6^iv—Zn1—Zn4^ii	109.38 (4)	Fe2^i—Zn4—Zn5^ix	120.36 (5)
Zn4—Zn1—Zn4^ii	180.0	Zn6^v—Zn4—Zn5^ix	93.74 (6)
Fe2^i—Zn1—Zn5^i	58.51 (2)	Zn6^i—Zn4—Zn5^ix	61.64 (4)
Fe2—Zn1—Zn5^i	121.49 (2)	Zn5^v—Zn4—Zn5^ix	149.12 (6)
Zn6—Zn1—Zn5^i	69.81 (4)	Zn5^i—Zn4—Zn5^ix	88.57 (4)
Zn6^ii—Zn1—Zn5^i	110.19 (4)	Zn1—Zn4—Zn5^ix	147.50 (3)
Zn6^iii—Zn1—Zn5^i	62.13 (3)	Zn6^ix—Zn4—Zn5^ix	53.97 (4)
Zn6^iv—Zn1—Zn5^i	117.87 (3)	Zn6^xv—Zn4—Zn5^ix	108.28 (5)
Zn4—Zn1—Zn5^i	58.61 (3)	Zn3^ix—Zn4—Zn5^xv	77.25 (5)
Zn4^ii—Zn1—Zn5^i	121.39 (3)	Fe2^i—Zn4—Zn5^xv	120.36 (5)
Fe2^i—Zn1—Zn5^v	58.51 (2)	Zn6^v—Zn4—Zn5^xv	61.64 (4)
Fe2—Zn1—Zn5^v	121.49 (2)	Zn6^i—Zn4—Zn5^xv	93.74 (6)
Zn6—Zn1—Zn5^v	117.87 (3)	Zn5^v—Zn4—Zn5^xv	88.57 (4)
Zn6^ii—Zn1—Zn5^v	62.13 (3)	Zn5^i—Zn4—Zn5^xv	149.12 (6)
Zn6^iii—Zn1—Zn5^v	110.19 (4)	Zn1—Zn4—Zn5^xv	147.50 (3)
Zn6^iv—Zn1—Zn5^v	69.81 (4)	Zn6^ix—Zn4—Zn5^xv	108.28 (5)
Zn4—Zn1—Zn5^v	58.61 (3)	Zn6^xv—Zn4—Zn5^xv	53.97 (4)
Zn4^ii—Zn1—Zn5^v	121.39 (3)	Zn5^ix—Zn4—Zn5^xv	64.70 (6)
Zn5^i—Zn1—Zn5^v	106.53 (5)	Zn3^ix—Zn4—Zn6	57.09 (5)
Fe2^i—Zn1—Zn5^vi	121.49 (2)	Fe2^i—Zn4—Zn6	103.91 (6)
Fe2—Zn1—Zn5^vi	58.51 (2)	Zn6^v—Zn4—Zn6	160.52 (7)
Zn6—Zn1—Zn5^vi	110.19 (4)	Zn6^i—Zn4—Zn6	120.37 (5)
Zn6^ii—Zn1—Zn5^vi	69.81 (4)	Zn5^v—Zn4—Zn6	106.32 (6)
Zn6^iii—Zn1—Zn5^vi	117.87 (3)	Zn5^i—Zn4—Zn6	64.29 (5)
Zn6^iv—Zn1—Zn5^vi	62.13 (3)	Zn1—Zn4—Zn6	53.69 (4)
Zn4—Zn1—Zn5^vi	121.39 (3)	Zn6^ix—Zn4—Zn6	50.14 (4)
Zn4^ii—Zn1—Zn5^vi	58.61 (3)	Zn6^xv—Zn4—Zn6	95.11 (5)
Zn5^i—Zn1—Zn5^vi	180.0	Zn5^ix—Zn4—Zn6	103.58 (4)
Zn5^v—Zn1—Zn5^vi	73.47 (5)	Zn5^xv—Zn4—Zn6	134.29 (6)
Fe2^i—Zn1—Zn5^vii	121.49 (2)	Zn3^viii—Zn5—Fe2	152.40 (6)
Fe2—Zn1—Zn5^vii	58.51 (2)	Zn3^viii—Zn5—Zn6	143.77 (6)
Zn6—Zn1—Zn5^vii	62.13 (3)	Fe2—Zn5—Zn6	59.24 (4)
Zn6^ii—Zn1—Zn5^vii	117.87 (3)	Zn3^viii—Zn5—Zn5^vii	135.85 (5)
Zn6^iii—Zn1—Zn5^vii	69.81 (4)	Fe2—Zn5—Zn5^vii	58.97 (3)
Zn6^iv—Zn1—Zn5^vii	110.19 (4)	Zn6—Zn5—Zn5^vii	64.07 (6)
Zn4—Zn1—Zn5^vii	121.39 (3)	Zn3^viii—Zn5—Zn3^xiii	60.78 (6)
Zn4^ii—Zn1—Zn5^vii	58.61 (3)	Fe2—Zn5—Zn3^xiii	113.25 (5)
Zn5^i—Zn1—Zn5^vii	73.47 (5)	Zn6—Zn5—Zn3^xiii	140.66 (6)
Zn5^v—Zn1—Zn5^vii	180.0	Zn5^vii—Zn5—Zn3^xiii	79.05 (5)
Zn5^vi—Zn1—Zn5^vii	106.53 (5)	Zn3^viii—Zn5—Zn4^viii	113.67 (6)
Zn1^viii—Fe2—Zn1	180.0	Fe2—Zn5—Zn4^viii	58.19 (4)
Zn1^viii—Fe2—Zn4^ii	115.14 (5)	Zn6—Zn5—Zn4^viii	60.45 (5)
Zn1—Fe2—Zn4^ii	64.86 (5)	Zn5^vii—Zn5—Zn4^viii	110.45 (5)
Zn1^viii—Fe2—Zn4^viii	64.86 (5)	Zn3^xiii—Zn5—Zn4^viii	153.37 (7)
Zn1—Fe2—Zn4^viii	115.14 (5)	Zn3^viii—Zn5—Zn1^viii	96.85 (5)
Zn4^ii—Fe2—Zn4^viii	180.0	Fe2—Zn5—Zn1^viii	55.73 (3)
Zn1^viii—Fe2—Zn6	116.94 (3)	Zn6—Zn5—Zn1^viii	107.15 (5)
Zn1—Fe2—Zn6	63.06 (3)	Zn5^vii—Zn5—Zn1^viii	103.89 (4)
Zn4^ii—Fe2—Zn6	117.41 (4)	Zn3^xiii—Zn5—Zn1^viii	94.04 (4)
Zn4^viii—Fe2—Zn6	62.59 (4)	Zn4^viii—Zn5—Zn1^viii	59.85 (4)
Zn1^viii—Fe2—Zn6^vi	63.06 (3)	Zn3^viii—Zn5—Zn6^vii	107.87 (6)
Zn1—Fe2—Zn6^vi	116.94 (3)	Fe2—Zn5—Zn6^vii	56.79 (3)
Zn4^ii—Fe2—Zn6^vi	62.59 (4)	Zn6—Zn5—Zn6^vii	107.92 (5)
Zn4^viii—Fe2—Zn6^vi	117.41 (4)	Zn5^vii—Zn5—Zn6^vii	56.96 (5)
Zn6—Fe2—Zn6^vi	180.0	Zn3^xiii—Zn5—Zn6^vii	57.04 (4)
Zn1^viii—Fe2—Zn6^iv	116.94 (3)	Zn4^viii—Zn5—Zn6^vii	106.20 (6)
Zn1—Fe2—Zn6^iv	63.06 (3)	Zn1^viii—Zn5—Zn6^vii	56.98 (4)
Zn4^ii—Fe2—Zn6^iv	117.41 (4)	Zn3^viii—Zn5—Zn6^xvi	60.78 (5)
Zn4^viii—Fe2—Zn6^iv	62.59 (4)	Fe2—Zn5—Zn6^xvi	120.33 (5)
Zn6—Fe2—Zn6^iv	63.21 (5)	Zn6—Zn5—Zn6^xvi	89.16 (5)
Zn6^vi—Fe2—Zn6^iv	116.79 (5)	Zn5^vii—Zn5—Zn6^xvi	149.82 (7)
Zn1^viii—Fe2—Zn6^vii	63.06 (3)	Zn3^xiii—Zn5—Zn6^xvi	121.37 (6)
Zn1—Fe2—Zn6^vii	116.94 (3)	Zn4^viii—Zn5—Zn6^xvi	62.24 (4)
Zn4^ii—Fe2—Zn6^vii	62.59 (4)	Zn1^viii—Zn5—Zn6^xvi	96.94 (5)
Zn4^viii—Fe2—Zn6^vii	117.41 (4)	Zn6^vii—Zn5—Zn6^xvi	151.70 (6)
Zn6—Fe2—Zn6^vii	116.79 (5)	Zn3^viii—Zn5—Zn4^ix	82.72 (5)
Zn6^vi—Fe2—Zn6^vii	63.21 (5)	Fe2—Zn5—Zn4^ix	121.82 (5)
Zn6^iv—Fe2—Zn6^vii	180.0	Zn6—Zn5—Zn4^ix	62.63 (4)
Zn1^viii—Fe2—Zn5^vi	114.24 (3)	Zn5^vii—Zn5—Zn4^ix	97.66 (6)
Zn1—Fe2—Zn5^vi	65.76 (3)	Zn3^xiii—Zn5—Zn4^ix	112.43 (5)
Zn4^ii—Fe2—Zn5^vi	62.84 (3)	Zn4^viii—Zn5—Zn4^ix	91.43 (4)
Zn4^viii—Fe2—Zn5^vi	117.16 (3)	Zn1^viii—Zn5—Zn4^ix	148.63 (5)
Zn6—Fe2—Zn5^vi	119.19 (4)	Zn6^vii—Zn5—Zn4^ix	152.69 (6)
Zn6^vi—Fe2—Zn5^vi	60.81 (4)	Zn6^xvi—Zn5—Zn4^ix	55.41 (4)
Zn6^iv—Fe2—Zn5^vi	65.77 (4)	Zn3^viii—Zn5—Zn5^xi	52.94 (4)
Zn6^vii—Fe2—Zn5^vi	114.23 (4)	Fe2—Zn5—Zn5^xi	148.97 (3)
Zn1^viii—Fe2—Zn5	65.76 (3)	Zn6—Zn5—Zn5^xi	109.50 (4)
Zn1—Fe2—Zn5	114.24 (3)	Zn5^vii—Zn5—Zn5^xi	90.0
Zn4^ii—Fe2—Zn5	117.16 (3)	Zn3^xiii—Zn5—Zn5^xi	54.90 (3)
Zn4^viii—Fe2—Zn5	62.84 (3)	Zn4^viii—Zn5—Zn5^xi	145.62 (4)
Zn6—Fe2—Zn5	60.81 (4)	Zn1^viii—Zn5—Zn5^xi	143.26 (2)
Zn6^vi—Fe2—Zn5	119.19 (4)	Zn6^vii—Zn5—Zn5^xi	108.13 (4)
Zn6^iv—Fe2—Zn5	114.23 (4)	Zn6^xvi—Zn5—Zn5^xi	86.02 (3)
Zn6^vii—Fe2—Zn5	65.77 (4)	Zn4^ix—Zn5—Zn5^xi	57.65 (3)
Zn5^vi—Fe2—Zn5	180.0	Zn3^viii—Zn5—Zn6^viii	54.08 (4)
Zn1^viii—Fe2—Zn5^vii	114.24 (3)	Fe2—Zn5—Zn6^viii	103.50 (5)
Zn1—Fe2—Zn5^vii	65.76 (3)	Zn6—Zn5—Zn6^viii	122.53 (6)
Zn4^ii—Fe2—Zn5^vii	62.84 (3)	Zn5^vii—Zn5—Zn6^viii	156.88 (5)
Zn4^viii—Fe2—Zn5^vii	117.16 (3)	Zn3^xiii—Zn5—Zn6^viii	96.75 (5)
Zn6—Fe2—Zn5^vii	65.77 (4)	Zn4^viii—Zn5—Zn6^viii	64.46 (5)
Zn6^vi—Fe2—Zn5^vii	114.23 (4)	Zn1^viii—Zn5—Zn6^viii	53.41 (3)
Zn6^iv—Fe2—Zn5^vii	119.19 (4)	Zn6^vii—Zn5—Zn6^viii	101.55 (5)
Zn6^vii—Fe2—Zn5^vii	60.81 (4)	Zn6^xvi—Zn5—Zn6^viii	50.30 (4)
Zn5^vi—Fe2—Zn5^vii	117.95 (6)	Zn4^ix—Zn5—Zn6^viii	104.87 (5)
Zn5—Fe2—Zn5^vii	62.05 (6)	Zn5^xi—Zn5—Zn6^viii	106.30 (3)
Zn1^viii—Fe2—Zn5^iv	65.76 (3)	Zn6^ix—Zn6—Fe2	165.36 (8)
Zn1—Fe2—Zn5^iv	114.24 (3)	Zn6^ix—Zn6—Zn5	132.33 (8)
Zn4^ii—Fe2—Zn5^iv	117.16 (3)	Fe2—Zn6—Zn5	59.95 (4)
Zn4^viii—Fe2—Zn5^iv	62.84 (3)	Zn6^ix—Zn6—Zn3	64.36 (6)
Zn6—Fe2—Zn5^iv	114.23 (4)	Fe2—Zn6—Zn3	116.11 (5)
Zn6^vi—Fe2—Zn5^iv	65.77 (4)	Zn5—Zn6—Zn3	81.28 (6)
Zn6^iv—Fe2—Zn5^iv	60.81 (4)	Zn6^ix—Zn6—Zn1	108.06 (7)
Zn6^vii—Fe2—Zn5^iv	119.19 (4)	Fe2—Zn6—Zn1	57.35 (3)
Zn5^vi—Fe2—Zn5^iv	62.05 (6)	Zn5—Zn6—Zn1	108.75 (5)
Zn5—Fe2—Zn5^iv	117.95 (6)	Zn3—Zn6—Zn1	98.24 (5)
Zn5^vii—Fe2—Zn5^iv	180.0	Zn6^ix—Zn6—Zn4^viii	131.53 (7)
Zn4^ix—Zn3—Zn5^i	132.58 (5)	Fe2—Zn6—Zn4^viii	58.66 (4)
Zn4^ix—Zn3—Zn5^x	132.58 (5)	Zn5—Zn6—Zn4^viii	61.20 (5)
Zn5^i—Zn3—Zn5^x	74.11 (8)	Zn3—Zn6—Zn4^viii	139.60 (6)
Zn4^ix—Zn3—Zn6^xi	67.21 (4)	Zn1—Zn6—Zn4^viii	107.16 (5)
Zn5^i—Zn3—Zn6^xi	145.89 (7)	Zn6^ix—Zn6—Zn6^iv	114.88 (5)
Zn5^x—Zn3—Zn6^xi	73.57 (5)	Fe2—Zn6—Zn6^iv	58.39 (3)
Zn4^ix—Zn3—Zn6	67.21 (4)	Zn5—Zn6—Zn6^iv	109.50 (4)
Zn5^i—Zn3—Zn6	73.57 (5)	Zn3—Zn6—Zn6^iv	157.16 (4)
Zn5^x—Zn3—Zn6	145.89 (7)	Zn1—Zn6—Zn6^iv	59.54 (3)
Zn6^xi—Zn3—Zn6	134.32 (7)	Zn4^viii—Zn6—Zn6^iv	59.69 (3)
Zn4^ix—Zn3—Zn3^xii	158.21 (10)	Zn6^ix—Zn6—Zn3^ix	59.22 (4)
Zn5^i—Zn3—Zn3^xii	61.90 (5)	Fe2—Zn6—Zn3^ix	118.33 (5)
Zn5^x—Zn3—Zn3^xii	61.90 (5)	Zn5—Zn6—Zn3^ix	140.06 (6)
Zn6^xi—Zn3—Zn3^xii	110.51 (4)	Zn3—Zn6—Zn3^ix	123.58 (4)
Zn6—Zn3—Zn3^xii	110.51 (4)	Zn1—Zn6—Zn3^ix	98.62 (5)
Zn4^ix—Zn3—Zn5^vii	105.85 (6)	Zn4^viii—Zn6—Zn3^ix	83.51 (5)
Zn5^i—Zn3—Zn5^vii	78.18 (6)	Zn6^iv—Zn6—Zn3^ix	60.69 (3)
Zn5^x—Zn3—Zn5^vii	119.22 (6)	Zn6^ix—Zn6—Zn5^vii	118.78 (7)
Zn6^xi—Zn3—Zn5^vii	128.06 (6)	Fe2—Zn6—Zn5^vii	57.44 (3)
Zn6—Zn3—Zn5^vii	63.68 (4)	Zn5—Zn6—Zn5^vii	58.97 (5)
Zn3^xii—Zn3—Zn5^vii	57.32 (5)	Zn3—Zn6—Zn5^vii	59.28 (4)
Zn4^ix—Zn3—Zn5^xiii	105.85 (6)	Zn1—Zn6—Zn5^vii	60.89 (4)
Zn5^i—Zn3—Zn5^xiii	119.22 (6)	Zn4^viii—Zn6—Zn5^vii	107.10 (5)
Zn5^x—Zn3—Zn5^xiii	78.18 (6)	Zn6^iv—Zn6—Zn5^vii	108.13 (4)
Zn6^xi—Zn3—Zn5^xiii	63.68 (4)	Zn3^ix—Zn6—Zn5^vii	158.70 (6)
Zn6—Zn3—Zn5^xiii	128.06 (6)	Zn6^ix—Zn6—Zn5^xvi	70.02 (6)
Zn3^xii—Zn3—Zn5^xiii	57.32 (5)	Fe2—Zn6—Zn5^xvi	121.57 (5)
Zn5^vii—Zn3—Zn5^xiii	70.20 (6)	Zn5—Zn6—Zn5^xvi	90.84 (5)
Zn4^ix—Zn3—Zn6^xiv	71.61 (5)	Zn3—Zn6—Zn5^xvi	106.22 (5)
Zn5^i—Zn3—Zn6^xiv	99.46 (6)	Zn1—Zn6—Zn5^xvi	150.77 (5)
Zn5^x—Zn3—Zn6^xiv	64.81 (5)	Zn4^viii—Zn6—Zn5^xvi	62.95 (5)
Zn6^xi—Zn3—Zn6^xiv	56.42 (4)	Zn6^iv—Zn6—Zn5^xvi	93.98 (3)
Zn6—Zn3—Zn6^xiv	110.44 (5)	Zn3^ix—Zn6—Zn5^xvi	54.41 (4)
Zn3^xii—Zn3—Zn6^xiv	126.49 (7)	Zn5^vii—Zn6—Zn5^xvi	146.86 (6)
Zn5^vii—Zn3—Zn6^xiv	174.03 (5)	Zn6^ix—Zn6—Zn4^ix	69.89 (6)
Zn5^xiii—Zn3—Zn6^xiv	115.57 (4)	Fe2—Zn6—Zn4^ix	123.30 (5)
Zn4^ix—Zn3—Zn6^ix	71.61 (5)	Zn5—Zn6—Zn4^ix	63.40 (5)
Zn5^i—Zn3—Zn6^ix	64.81 (5)	Zn3—Zn6—Zn4^ix	55.32 (5)
Zn5^x—Zn3—Zn6^ix	99.46 (6)	Zn1—Zn6—Zn4^ix	152.42 (5)
Zn6^xi—Zn3—Zn6^ix	110.44 (5)	Zn4^viii—Zn6—Zn4^ix	92.27 (4)
Zn6—Zn3—Zn6^ix	56.42 (4)	Zn6^iv—Zn6—Zn4^ix	147.43 (3)
Zn3^xii—Zn3—Zn6^ix	126.49 (7)	Zn3^ix—Zn6—Zn4^ix	102.97 (5)
Zn5^vii—Zn3—Zn6^ix	115.57 (4)	Zn5^vii—Zn6—Zn4^ix	95.16 (6)
Zn5^xiii—Zn3—Zn6^ix	174.03 (5)	Zn5^xvi—Zn6—Zn4^ix	56.06 (4)
Zn6^xiv—Zn3—Zn6^ix	58.62 (5)	Zn6^ix—Zn6—Zn5^i	59.68 (5)
Zn3^ix—Zn4—Fe2^i	158.40 (8)	Fe2—Zn6—Zn5^i	108.13 (5)
Zn3^ix—Zn4—Zn6^v	137.42 (6)	Zn5—Zn6—Zn5^i	122.53 (6)
Fe2^i—Zn4—Zn6^v	58.75 (4)	Zn3—Zn6—Zn5^i	52.35 (4)
Zn3^ix—Zn4—Zn6^i	137.42 (6)	Zn1—Zn6—Zn5^i	56.79 (4)
Fe2^i—Zn4—Zn6^i	58.75 (4)	Zn4^viii—Zn6—Zn5^i	163.86 (5)
Zn6^v—Zn4—Zn6^i	60.63 (7)	Zn6^iv—Zn6—Zn5^i	106.30 (3)
Zn3^ix—Zn4—Zn5^v	113.23 (5)	Zn3^ix—Zn6—Zn5^i	96.64 (5)
Fe2^i—Zn4—Zn5^v	58.97 (4)	Zn5^vii—Zn6—Zn5^i	67.98 (5)
Zn6^v—Zn4—Zn5^v	58.34 (4)	Zn5^xvi—Zn6—Zn5^i	129.70 (4)
Zn6^i—Zn4—Zn5^v	107.95 (6)	Zn4^ix—Zn6—Zn5^i	103.37 (5)
Zn3^ix—Zn4—Zn5^i	113.23 (5)

Symmetry codes: (i) x, y, z−1; (ii) −x, −y, −z; (iii) −x, y, −z; (iv) x, −y, z; (v) x, −y, z−1; (vi) −x, −y, −z+1; (vii) −x, y, −z+1; (viii) x, y, z+1; (ix) −x+1/2, −y+1/2, −z+1; (x) x, −y+1, z−1; (xi) x, −y+1, z; (xii) −x, −y+1, −z; (xiii) −x, −y+1, −z+1; (xiv) −x+1/2, y+1/2, −z+1; (xv) −x+1/2, y−1/2, −z+1; (xvi) −x+1/2, −y+1/2, −z+2.