Aminoguanidinium(1+) pentafluorozirconate: multiple redetermination and comparisons

The structure of CN₄H₇ZrF₅ reported by Bukvetskii et al. [Koord. Khim. (1992). 18, 576–579] has been independently redetermined on the basis of measurements on three different crystals. Assuming all four resulting structures are drawn from a normal distribution, normal probability analysis of the atomic coordinates taken in pairs reveals joint standard uncertainties that are underestimated by factors as large as 16.5 for the x(Zr) coordinate. Unit-cell parameters in the four crystals similarly have joint uncertainties, under the same assumption, that are underestimated by factors as large as 83.0 for the b axis. The variations in axial lengths from crystal to crystal and the declines in standard reflection intensities by 13–15% in at least two of the crystals measured are consistent with the inference that the distribution is not normal. Rather, the differences observed may be assumed to be caused by small but highly significant radiation-induced structural changes. The large underestimations hence reflect physical differences among the four irradiated crystals. The determinations show that the CN₄H₇⁺¹ cation is exactly planar except for the two H atoms bonded to the terminal N atom; the plane of this NH₂ group is normal to that of the cation. The average length of the three independent C—N bonds is 1.318 (11) Å; the N—N bond length is 1.397 (3) Å. Distorted ZrF₇ pentagonal bipyramids share edges, forming chains linked by N—H...F bonds to the CN₄H₇⁺¹ ions.

Computing details

Data collection: Siemens (1993) XSCANS for (1); CAD-4 EXPRESS (Enraf-Nonius, 1989) for (2), (3). Cell refinement: Siemens (1993) XSCANS for (1); CAD-4 EXPRESS (Enraf-Nonius, 1989) for (2), (3). Data reduction: Siemens (1993) XSCANS for (1); XCAD4 (Harms, 1996) for (2), (3). For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: ORTEP-III (Burnett and Johnson, 1996) for (2), (3).

Figures

(1) 'aminoguanidinium pentafluorozirconate'

Crystal data

CH7N4^+·F5Zr^−	F(000) = 504
Mr = 261.33	Dx = 2.340 Mg m^−3 Dm = 2.305 (5) Mg m^−3 Dm measured by pycnometric
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71065 Å
Hall symbol: -P 2ac 2n	Cell parameters from 30 reflections
a = 6.6524 (5) Å	θ = 29.5–30.0°
b = 6.9466 (4) Å	µ = 1.52 mm^−1
c = 16.0497 (9) Å	T = 295 K
V = 741.68 (8) Å^3	Blocky, colorless
Z = 4	0.36 × 0.28 × 0.22 mm

Data collection

Siemens P4 diffractometer	1600 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.030
Graphite monochromator	θmax = 35.0°, θmin = 3.3°
2θ/ω scans	h = −1→10
Absorption correction: ψ scan XEMP (Siemens, 1993)	k = −1→11
Tmin = 0.621, Tmax = 0.716	l = −1→25
2318 measured reflections	3 standard reflections every 97 reflections
1731 independent reflections	intensity decay: 12.8%

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)] = 0.028	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.076	w = 1/[σ^2(Fo^2) + (0.0185P)^2 + 0.4487P] where P = (Fo^2 + 2Fc^2)/3
S = 1.22	(Δ/σ)max = 0.001
1731 reflections	Δρmax = 1.06 e Å^−3
79 parameters	Δρmin = −0.54 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0101 (16)

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
Zr	0.56044 (3)	0.2500	0.208400 (12)	0.02012 (9)
F1	0.8699 (2)	0.2500	0.18310 (9)	0.0329 (4)
F2	0.7472 (2)	0.2500	0.32044 (9)	0.0305 (3)
F3	0.5615 (2)	0.2500	0.08622 (10)	0.0398 (5)
F4	0.5539 (2)	0.5323 (2)	0.21690 (9)	0.0409 (3)
C	0.6078 (5)	0.2500	0.55445 (16)	0.0320 (5)
N1	0.8044 (5)	0.2500	0.5580 (2)	0.0607 (11)
H1A	0.884 (8)	0.2500	0.509 (4)	0.070 (8)*
H1B	0.854 (9)	0.2500	0.604 (3)	0.070 (8)*
N2	0.5113 (5)	0.2500	0.48224 (15)	0.0419 (6)
H2A	0.579 (7)	0.2500	0.439 (4)	0.070 (8)*
H2B	0.384 (8)	0.2500	0.485 (3)	0.070 (8)*
N3	0.5019 (5)	0.2500	0.62461 (15)	0.0445 (7)
H3	0.565 (8)	0.2500	0.668 (4)	0.067*
N4	0.2918 (5)	0.2500	0.62100 (19)	0.0455 (7)
H4	0.244 (5)	0.160 (5)	0.6494 (19)	0.068*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zr	0.01083 (11)	0.03497 (14)	0.01457 (11)	0.000	−0.00021 (6)	0.000
F1	0.0135 (5)	0.0692 (12)	0.0160 (5)	0.000	0.0005 (5)	0.000
F2	0.0120 (5)	0.0623 (11)	0.0171 (5)	0.000	0.0009 (4)	0.000
F3	0.0236 (8)	0.0796 (15)	0.0161 (6)	0.000	−0.0016 (5)	0.000
F4	0.0481 (9)	0.0362 (7)	0.0385 (7)	0.0006 (6)	−0.0005 (5)	0.0003 (5)
C	0.0332 (12)	0.0440 (14)	0.0188 (9)	0.000	0.0024 (9)	0.000
N1	0.0305 (13)	0.121 (4)	0.0304 (12)	0.000	0.0032 (11)	0.000
N2	0.0414 (14)	0.0655 (19)	0.0188 (9)	0.000	−0.0011 (10)	0.000
N3	0.0343 (12)	0.081 (2)	0.0182 (9)	0.000	0.0036 (9)	0.000
N4	0.0319 (13)	0.068 (2)	0.0370 (13)	0.000	0.0090 (11)	0.000

Geometric parameters (Å, º)

Zr—F3	1.9610 (16)	C—N3	1.328 (4)
Zr—F4	1.9665 (16)	N1—H1A	0.95 (6)
Zr—F1	2.0984 (15)	N1—H1B	0.80 (6)
Zr—F2^i	2.1348 (14)	N2—H2A	0.83 (5)
Zr—F1^i	2.1539 (15)	N2—H2B	0.85 (6)
Zr—F2	2.1856 (14)	N3—N4	1.399 (4)
C—N1	1.309 (4)	N3—H3	0.81 (6)
C—N2	1.325 (4)	N4—H4	0.84 (3)
F3—Zr—F4	93.98 (4)	Zr—F1—Zr^iii	114.89 (6)
F4—Zr—F4^ii	171.65 (8)	Zr^iii—F2—Zr	112.11 (6)
F3—Zr—F1	78.64 (6)	N1—C—N2	121.5 (3)
F4—Zr—F1	92.00 (4)	N1—C—N3	119.6 (3)
F3—Zr—F2^i	77.68 (6)	N2—C—N3	119.0 (3)
F4—Zr—F2^i	89.63 (4)	C—N1—H1A	122 (3)
F1—Zr—F2^i	156.32 (6)	C—N1—H1B	117 (4)
F3—Zr—F1^i	144.15 (6)	H1A—N1—H1B	122 (5)
F4—Zr—F1^i	86.04 (4)	C—N2—H2A	118 (4)
F1—Zr—F1^i	137.21 (4)	C—N2—H2B	116 (4)
F2^i—Zr—F1^i	66.47 (6)	H2A—N2—H2B	126 (5)
F3—Zr—F2	145.16 (6)	C—N3—N4	119.7 (3)
F4—Zr—F2	87.44 (4)	C—N3—H3	117 (4)
F1—Zr—F2	66.52 (5)	N4—N3—H3	124 (4)
F2^i—Zr—F2	137.16 (4)	N3—N4—H4	111 (3)
F1^i—Zr—F2	70.68 (6)

Symmetry codes: (i) x−1/2, y, −z+1/2; (ii) x, −y+1/2, z; (iii) x+1/2, y, −z+1/2.

(2) aminoguanidinium pentafluorozirconate

Crystal data

CH7N4^+·F5Zr^−	F(000) = 504
Mr = 261.33	Dx = 2.370 Mg m^−3 Dm = 2.305 (5) Mg m^−3 Dm measured by pycnometric
Orthorhombic, Pnma	Cu Kα radiation, λ = 1.5418 Å
Hall symbol: -P 2ac 2n	Cell parameters from 24 reflections
a = 6.6404 (6) Å	θ = 32.7–44.2°
b = 6.8981 (5) Å	µ = 12.88 mm^−1
c = 15.9872 (9) Å	T = 200 K
V = 732.31 (9) Å^3	Blocky, colorless
Z = 4	0.13 × 0.11 × 0.06 mm

Data collection

Nonius MACH3 diffractometer	751 reflections with I > 2σ(I)
Radiation source: rotating-anode	Rint = 0.036
Graphite monochromator	θmax = 69.9°, θmin = 5.5°
ω–2θ scans	h = −8→8
Absorption correction: analytical ABSPSI, (Alcock and Marks, 1994)	k = −1→8
Tmin = 0.22, Tmax = 0.48	l = −19→19
3283 measured reflections	5 standard reflections every 60 min
757 independent reflections	intensity decay: 15.

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)] = 0.019	All H-atom parameters refined
wR(F^2) = 0.046	w = 1/[σ^2(Fo^2) + (0.019P)^2 + 0.2678P] where P = (Fo^2 + 2Fc^2)/3
S = 1.34	(Δ/σ)max = 0.036
757 reflections	Δρmax = 0.52 e Å^−3
84 parameters	Δρmin = −0.58 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00379 (19)

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
Zr	0.06210 (3)	0.2500	0.208242 (13)	0.01609 (13)
F1	0.3712 (3)	0.2500	0.18291 (9)	0.0253 (4)
F2	0.2482 (2)	0.2500	0.32066 (9)	0.0246 (4)
F3	0.0636 (2)	0.2500	0.08555 (11)	0.0289 (4)
F4	0.05497 (18)	−0.0341 (2)	0.21687 (8)	0.0316 (4)
N1	0.0015 (5)	0.2500	0.62498 (16)	0.0334 (6)
N2	0.2900 (4)	0.2500	0.87881 (18)	0.0338 (7)
N3	0.3046 (4)	0.2500	0.55830 (19)	0.0422 (8)
N4	0.0115 (5)	0.2500	0.48236 (16)	0.0310 (6)
C	0.1078 (5)	0.2500	0.55448 (18)	0.0251 (6)
H1	0.064 (7)	0.2500	0.669 (4)	0.064 (17)*
H2	0.242 (5)	0.335 (5)	0.8516 (18)	0.067 (11)*
H3	0.368 (8)	0.2500	0.602 (3)	0.051 (13)*
H4	0.380 (7)	0.2500	0.514 (3)	0.048 (12)*
H5	0.080 (5)	0.2500	0.432 (3)	0.029 (10)*
H6	−0.111 (6)	0.2500	0.487 (2)	0.020 (9)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zr	0.00818 (17)	0.02989 (18)	0.01020 (17)	0.000	−0.00006 (6)	0.000
F1	0.0110 (8)	0.0543 (11)	0.0106 (8)	0.000	0.0000 (6)	0.000
F2	0.0101 (7)	0.0527 (10)	0.0110 (7)	0.000	0.0012 (6)	0.000
F3	0.0176 (9)	0.0570 (12)	0.0122 (8)	0.000	−0.0009 (6)	0.000
F4	0.0387 (9)	0.0299 (7)	0.0262 (7)	0.0000 (6)	−0.0001 (4)	0.0004 (5)
N1	0.0226 (13)	0.0645 (18)	0.0132 (12)	0.000	0.0011 (12)	0.000
N2	0.0233 (15)	0.0523 (17)	0.0259 (13)	0.000	−0.0065 (12)	0.000
N3	0.0233 (14)	0.085 (2)	0.0180 (13)	0.000	0.0020 (12)	0.000
N4	0.0260 (14)	0.0525 (16)	0.0146 (13)	0.000	0.0011 (12)	0.000
C	0.0266 (14)	0.0323 (15)	0.0163 (13)	0.000	−0.0011 (12)	0.000

Geometric parameters (Å, º)

Zr—F3	1.9615 (18)	N1—C	1.330 (4)
Zr—F4	1.9649 (15)	N1—N2^v	1.406 (4)
Zr—F4^i	1.9649 (15)	N1—H1	0.81 (6)
Zr—F1	2.0921 (17)	N2—N1^vi	1.406 (4)
Zr—F2^ii	2.1350 (16)	N2—H2	0.80 (3)
Zr—F1^iii	2.1530 (16)	N3—C	1.308 (4)
Zr—F2	2.1812 (15)	N3—H3	0.81 (5)
Zr—Zr^iv	3.5786 (3)	N3—H4	0.86 (5)
Zr—Zr^ii	3.5786 (3)	N4—C	1.318 (4)
F1—Zr^iv	2.1530 (16)	N4—H5	0.92 (4)
F2—Zr^iv	2.1350 (16)	N4—H6	0.81 (4)
F3—Zr—F4	94.03 (4)	F1^iii—Zr—Zr^iv	104.16 (4)
F3—Zr—F4^i	94.03 (4)	F2—Zr—Zr^iv	33.58 (4)
F4—Zr—F4^i	171.49 (7)	F3—Zr—Zr^ii	112.20 (4)
F3—Zr—F1	78.54 (6)	F4—Zr—Zr^ii	87.22 (4)
F4—Zr—F1	92.13 (4)	F4^i—Zr—Zr^ii	87.22 (4)
F4^i—Zr—F1	92.13 (4)	F1—Zr—Zr^ii	169.25 (4)
F3—Zr—F2^ii	77.79 (6)	F2^ii—Zr—Zr^ii	34.41 (4)
F4—Zr—F2^ii	89.52 (4)	F1^iii—Zr—Zr^ii	32.02 (4)
F4^i—Zr—F2^ii	89.52 (4)	F2—Zr—Zr^ii	102.60 (4)
F1—Zr—F2^ii	156.34 (6)	Zr^iv—Zr—Zr^ii	136.185 (13)
F3—Zr—F1^iii	144.22 (6)	Zr—F1—Zr^iv	114.91 (7)
F4—Zr—F1^iii	85.93 (4)	Zr^iv—F2—Zr	112.01 (6)
F4^i—Zr—F1^iii	85.93 (4)	C—N1—N2^v	119.6 (3)
F1—Zr—F1^iii	137.23 (5)	C—N1—H1	117 (4)
F2^ii—Zr—F1^iii	66.43 (6)	N2^v—N1—H1	123 (4)
F3—Zr—F2	145.19 (6)	N1^vi—N2—H2	112 (3)
F4—Zr—F2	87.47 (4)	C—N3—H3	124 (3)
F4^i—Zr—F2	87.47 (4)	C—N3—H4	123 (3)
F1—Zr—F2	66.65 (6)	H3—N3—H4	113 (4)
F2^ii—Zr—F2	137.01 (5)	C—N4—H5	121 (2)
F1^iii—Zr—F2	70.58 (6)	C—N4—H6	114 (2)
F3—Zr—Zr^iv	111.61 (4)	H5—N4—H6	125 (3)
F4—Zr—Zr^iv	89.78 (4)	N3—C—N4	121.7 (3)
F4^i—Zr—Zr^iv	89.78 (4)	N3—C—N1	119.4 (3)
F1—Zr—Zr^iv	33.07 (4)	N4—C—N1	118.9 (3)
F2^ii—Zr—Zr^iv	170.59 (4)

Symmetry codes: (i) x, −y+1/2, z; (ii) x−1/2, −y+1/2, −z+1/2; (iii) x−1/2, y, −z+1/2; (iv) x+1/2, −y+1/2, −z+1/2; (v) x−1/2, −y+1/2, −z+3/2; (vi) x+1/2, −y+1/2, −z+3/2.

(3) 'aminoguanidinium pentafluorozirconate'

Crystal data

CH7N4^+·F5Zr^−	F(000) = 504
Mr = 261.33	Dx = 2.348 Mg m^−3 Dm = 2.305 (5) Mg m^−3 Dm measured by pycnometric
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71065 Å
Hall symbol: -P 2ac 2n	Cell parameters from 25 reflections
a = 6.6485 (4) Å	θ = 20.1–23.9°
b = 6.9340 (4) Å	µ = 1.53 mm^−1
c = 16.0344 (4) Å	T = 283 K
V = 739.20 (6) Å^3	Blocky, colorless
Z = 4	0.27 × 0.11 × 0.09 mm

Data collection

Nonius MACH3 diffractometer	Rint = 0.010
Radiation source: fine-focus sealed tube	θmax = 30.0°, θmin = 2.5°
Graphite monochromator	h = −1→9
ω–2θ scans	k = −1→9
3001 measured reflections	l = −22→22
1159 independent reflections	5 standard reflections every 60 min
1076 reflections with I > 2σ(I)	intensity decay: 1.8%

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.041	w = 1/[σ^2(Fo^2) + (0.0087P)^2 + 0.149P] where P = (Fo^2 + 2Fc^2)/3
S = 1.20	(Δ/σ)max = 0.011
1159 reflections	Δρmax = 0.40 e Å^−3
79 parameters	Δρmin = −0.29 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0073 (5)
Secondary atom site location: difference Fourier map

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
Zr	0.06087 (2)	0.2500	0.208348 (8)	0.02069 (7)
F1	0.37020 (15)	0.2500	0.18304 (6)	0.0328 (3)
F2	0.24709 (15)	0.2500	0.32051 (5)	0.0313 (2)
F3	0.06197 (14)	0.2500	0.08617 (6)	0.0381 (3)
F4	0.05457 (13)	0.53240 (15)	0.21687 (5)	0.0400 (2)
C	0.1072 (3)	0.2500	0.55408 (10)	0.0317 (3)
N1	0.0017 (3)	0.2500	0.62458 (10)	0.0433 (5)
H1	0.065 (5)	0.2500	0.670 (2)	0.065*
N2	0.2918 (3)	0.2500	0.87913 (11)	0.0451 (4)
H2	0.243 (3)	0.341 (3)	0.8524 (11)	0.068*
N3	0.3045 (3)	0.2500	0.55818 (12)	0.0560 (6)
H3	0.370 (5)	0.2500	0.6024 (18)	0.053 (4)*
H4	0.386 (4)	0.2500	0.5156 (18)	0.053 (4)*
N4	0.0121 (3)	0.2500	0.48250 (10)	0.0405 (4)
H5	0.082 (4)	0.2500	0.4339 (19)	0.053 (4)*
H6	−0.103 (4)	0.2500	0.4856 (18)	0.053 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zr	0.01134 (9)	0.03592 (10)	0.01482 (9)	0.000	−0.00024 (4)	0.000
F1	0.0131 (4)	0.0690 (8)	0.0163 (4)	0.000	0.0007 (3)	0.000
F2	0.0130 (4)	0.0643 (7)	0.0166 (4)	0.000	0.0013 (3)	0.000
F3	0.0233 (5)	0.0737 (9)	0.0173 (4)	0.000	−0.0012 (3)	0.000
F4	0.0462 (6)	0.0379 (5)	0.0360 (4)	0.0005 (4)	−0.0010 (3)	−0.0001 (3)
C	0.0338 (8)	0.0412 (9)	0.0201 (7)	0.000	0.0020 (7)	0.000
N1	0.0319 (8)	0.0799 (14)	0.0181 (6)	0.000	0.0020 (7)	0.000
N2	0.0334 (9)	0.0660 (12)	0.0359 (8)	0.000	−0.0085 (7)	0.000
N3	0.0301 (8)	0.1093 (19)	0.0287 (8)	0.000	0.0024 (7)	0.000
N4	0.0380 (8)	0.0641 (12)	0.0195 (6)	0.000	−0.0002 (7)	0.000

Geometric parameters (Å, º)

Zr—F3	1.9590 (10)	C—N3	1.313 (3)
Zr—F4	1.9634 (10)	C—N1	1.330 (2)
Zr—F1	2.0962 (10)	N1—N2^iii	1.397 (3)
Zr—F2^i	2.1369 (10)	N1—H1	0.84 (3)
Zr—F1^i	2.1541 (9)	N2—H2	0.831 (19)
Zr—F2	2.1834 (9)	N3—H3	0.83 (3)
Zr—Zr^i	3.5826 (2)	N3—H4	0.87 (3)
F1—Zr^ii	2.1540 (9)	N4—H5	0.91 (3)
F2—Zr^ii	2.1368 (10)	N4—H6	0.76 (3)
C—N4	1.310 (2)
F3—Zr—F4	94.00 (2)	F3—Zr—Zr^i	112.10 (3)
F4—Zr—F4^iv	171.65 (5)	F4—Zr—Zr^i	87.38 (3)
F3—Zr—F1	78.62 (4)	F1—Zr—Zr^i	169.27 (3)
F4—Zr—F1	91.97 (3)	F2^i—Zr—Zr^i	34.40 (2)
F3—Zr—F2^i	77.71 (4)	F1^i—Zr—Zr^i	32.06 (3)
F4—Zr—F2^i	89.67 (3)	F2—Zr—Zr^i	102.66 (3)
F1—Zr—F2^i	156.33 (4)	Zr^ii—Zr—Zr^i	136.221 (8)
F3—Zr—F1^i	144.16 (4)	Zr—F1—Zr^ii	114.89 (4)
F4—Zr—F1^i	86.05 (2)	Zr^ii—F2—Zr	112.04 (4)
F1—Zr—F1^i	137.21 (3)	N4—C—N3	121.72 (18)
F2^i—Zr—F1^i	66.46 (4)	N4—C—N1	119.32 (19)
F3—Zr—F2	145.24 (4)	N3—C—N1	118.96 (18)
F4—Zr—F2	87.41 (2)	C—N1—N2^iii	119.39 (17)
F1—Zr—F2	66.62 (4)	C—N1—H1	118 (2)
F2^i—Zr—F2	137.05 (3)	N2^iii—N1—H1	122 (2)
F1^i—Zr—F2	70.60 (4)	N1^v—N2—H2	111.6 (16)
F3—Zr—Zr^ii	111.68 (3)	C—N3—H3	124 (2)
F4—Zr—Zr^ii	89.65 (3)	C—N3—H4	125.6 (19)
F1—Zr—Zr^ii	33.05 (2)	H3—N3—H4	110 (3)
F2^i—Zr—Zr^ii	170.62 (2)	C—N4—H5	120.2 (18)
F1^i—Zr—Zr^ii	104.16 (3)	C—N4—H6	115 (2)
F2—Zr—Zr^ii	33.57 (2)	H5—N4—H6	125 (3)

Symmetry codes: (i) x−1/2, y, −z+1/2; (ii) x+1/2, y, −z+1/2; (iii) x−1/2, y, −z+3/2; (iv) x, −y+1/2, z; (v) x+1/2, y, −z+3/2.