The crystal structure of Zr₂NiD_4.5

The crystal structure of Zr₂NiD_4.5 has been determined by a combination of synchrotron radiation powder X-ray diffraction, electron diffraction and powder neutron diffraction data. Deuterium ordering results in a triclinic supercell given by a_super = 6.81560 (7), b_super = 8.85137 (9), c_super = 8.88007 (10) Å, α_super = 79.8337 (8), β_super = 90.0987 (9), γ_super = 90.3634 (9)°, which relates to the non-super unit cell as a_super = −a, b_super = −b − c, c_super = −b + c. The centrosymmetric and fully ordered deuterium sublattice was determined by simulated annealing and Rietveld refinement. Deuterium was found to occupy three types of tetrahedral sites: two that are coordinated by four Zr atoms and one that is coordinated by three Zr atoms and one Ni atom. All D—D distances are longer than 2 Å. The feasibility of the crystal structure was supported by density functional theory calculations.

Computing details

Figures

(B34_P-1_HRPD_ONLY_phase_1)

Crystal data

D9Ni2Zr4	β = 90.0987 (9)°
Mr = 500.41	γ = 90.3634 (9)°
Triclinic, P1	V = 527.29 (1) Å^3
Hall symbol: -P 1	Z = 4
a = 6.81560 (7) Å	? radiation
b = 8.85137 (9) Å	T = 298 K
c = 8.88007 (10) Å	?; ?, ?; ? × ?; ? mm
α = 79.8337 (8)°

Data collection

Scan method: time of flight

2θfixed = 168.33

Refinement

Least-squares matrix: full	? data points
Rp = 0.040	Profile function: TOF Profile function number 2 with 15 terms Profile coefficients for W.I.F. David function; a convolution of the Ikeda-Carpenter and Pseudo-Voight functions W.I.F. David, J. Appl. Cryst., 19,63-64,(1986) W.I.F. David - unpublished (1986). #1 (alp-0) = 0.0000 #5 (sig-0) = 0.00 #8 (gam-0) = 0.00 #2 (alp-1) = 1.8080 #6 (sig-1) = 516.69 #9 (gam-1) = 69.79 #3 (beta ) = 30.58 #7 (sig-2) = 0.00 #10(gam-2) = 0.00 #4(switch) = 77.14 #11(ptec ) = 0.00 #12(stec ) = 0.00 #13(difc ) = 0.00 #14(difa ) = 0.00 #15(zero ) = 0.00 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.045	109 parameters
Rexp = 0.035	71 restraints
R(F^2) = 0.04587	(Δ/σ)max = 0.03
χ^2 = 4.000	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 0.536090 2: 9.643680E-02 3: 7.823360E-02 4: 6.959260E-02 5: 5.735480E-02 6: 6.019780E-02 7: 3.477360E-02 8: 2.645520E-02 9: 1.302490E-0210: 2.223830E-0211: 1.431470E-0212: 3.864190E-03

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Zr1	0.5672 (15)	0.9167 (11)	0.1705 (10)	0.0034 (3)*
Zr2	0.9093 (17)	0.5778 (11)	0.8328 (12)	0.0034 (3)*
Zr3	0.0941 (17)	0.8348 (11)	0.0841 (12)	0.0034 (3)*
Zr4	0.4129 (17)	0.6616 (12)	0.9199 (12)	0.0034 (3)*
Zr5	0.5994 (16)	0.8336 (11)	0.5808 (12)	0.0034 (3)*
Zr6	0.0840 (17)	0.3393 (12)	0.5841 (12)	0.0034 (3)*
Zr7	0.5877 (16)	0.4270 (11)	0.6662 (12)	0.0034 (3)*
Zr8	0.0797 (15)	0.9208 (11)	0.6805 (11)	0.0034 (3)*
Ni1	0.7494 (16)	0.1451 (13)	0.6011 (15)	0.0050 (3)*
Ni2	0.7496 (16)	0.3764 (12)	0.3794 (13)	0.0050 (3)*
Ni3	0.7487 (17)	0.8522 (13)	0.8978 (14)	0.0050 (3)*
Ni4	0.7511 (17)	0.6289 (12)	0.1266 (12)	0.0050 (3)*
D1	0.951 (2)	0.1401 (14)	0.6931 (16)	0.0126 (3)*
D2	0.8782 (19)	0.5062 (15)	0.6242 (14)	0.0126 (3)*
D3	0.458 (2)	0.1443 (14)	0.1996 (16)	0.0126 (3)*
D4	0.541 (2)	0.3621 (14)	0.3035 (16)	0.0126 (3)*
D5	0.2406 (18)	0.1256 (12)	0.6359 (13)	0.0126 (3)*
D6	0.8857 (15)	0.7631 (9)	0.6421 (11)	0.0126 (3)*
D7	0.967 (2)	0.6390 (14)	0.1944 (16)	0.0126 (3)*
D8	0.1624 (18)	0.0086 (13)	0.4585 (14)	0.0126 (3)*
D9	0.2470 (19)	0.8803 (13)	0.8755 (13)	0.0126 (3)*
D10	0.3669 (14)	0.7320 (9)	0.1269 (10)	0.0126 (3)*
D11	0.0500 (17)	0.0567 (13)	0.1027 (14)	0.0126 (3)*
D12	0.1297 (19)	0.6192 (14)	0.9976 (15)	0.0126 (3)*
D13	0.621 (2)	0.6244 (14)	0.4968 (15)	0.0126 (3)*
D14	0.3307 (19)	1.0025 (12)	0.0494 (14)	0.0126 (3)*
D15	0.379 (2)	0.4993 (15)	0.1229 (14)	0.0126 (3)*
D16	0.8389 (19)	0.2982 (16)	0.2391 (17)	0.0126 (3)*
D17	0.658 (2)	0.7018 (16)	0.2639 (16)	0.0126 (3)*
D18	0.5296 (17)	0.0571 (13)	0.6159 (14)	0.0126 (3)*

Geometric parameters (Å, º)

Zr1—Zr1^i	3.259 (19)	Ni2—Zr7^iv	2.877 (15)
Zr1—Zr3	3.416 (16)	Ni2—Zr8^iv	3.015 (13)
Zr1—Zr4^ii	3.591 (12)	Ni2—Ni1	2.578 (19)
Zr1—Zr5	3.594 (15)	Ni2—Ni4	2.875 (4)
Zr1—Zr5^iii	3.580 (12)	Ni2—D4	1.584 (15)
Zr1—Zr7^iv	3.298 (12)	Ni2—D16	1.647 (14)
Zr1—Zr8^iii	3.198 (6)	Ni3—Zr1^x	2.869 (15)
Zr1—Ni1^iv	2.945 (15)	Ni3—Zr1^iii	2.967 (15)
Zr1—Ni3^ii	2.869 (15)	Ni3—Zr2	2.821 (14)
Zr1—Ni3^iii	2.967 (15)	Ni3—Zr3^xxi	2.864 (18)
Zr1—Ni4	2.933 (14)	Ni3—Zr3^iii	2.995 (14)
Zr1—D3^v	2.209 (14)	Ni3—Zr4	2.821 (16)
Zr1—D5^iv	2.141 (14)	Ni3—Zr5	3.023 (15)
Zr1—D9^iii	2.171 (14)	Ni3—Zr8^viii	2.961 (15)
Zr1—D10	2.209 (12)	Ni3—Ni4^x	2.572 (19)
Zr1—D14	2.014 (14)	Ni3—D3^iv	1.652 (15)
Zr1—D14^i	2.077 (14)	Ni3—D11^iv	1.587 (13)
Zr1—D17	2.036 (15)	Ni3—D14^iii	1.546 (12)
Zr1—D18^iv	2.061 (14)	Ni4—Zr1	2.933 (14)
Zr2—Zr2^vi	3.29 (2)	Ni4—Zr2^ii	2.933 (14)
Zr2—Zr3^iv	3.596 (14)	Ni4—Zr2^ix	2.941 (15)
Zr2—Zr4	3.583 (15)	Ni4—Zr3^viii	2.938 (15)
Zr2—Zr4^vii	3.529 (15)	Ni4—Zr4^ii	2.928 (16)
Zr2—Zr5	3.585 (16)	Ni4—Zr4^iv	2.893 (14)
Zr2—Zr6^viii	3.527 (13)	Ni4—Zr6^iv	2.861 (14)
Zr2—Zr7	3.071 (6)	Ni4—Zr7^iv	2.940 (16)
Zr2—Zr8^viii	3.302 (12)	Ni4—Ni2	2.875 (4)
Zr2—Ni2^ix	2.975 (16)	Ni4—Ni3^ii	2.572 (19)
Zr2—Ni3	2.821 (14)	Ni4—D7	1.597 (15)
Zr2—Ni4^x	2.933 (14)	Ni4—D17	1.610 (14)
Zr2—Ni4^ix	2.941 (15)	D1—Zr3^iv	2.053 (15)
Zr2—D2	2.071 (14)	D1—Zr6^viii	2.062 (14)
Zr2—D6	2.146 (13)	D1—Zr8^xix	2.156 (14)
Zr2—D7^ix	2.153 (14)	D1—Ni1	1.593 (14)
Zr2—D12^viii	2.169 (15)	D1—D5^viii	2.050 (18)
Zr2—D12^vii	2.109 (16)	D1—D8^xx	2.179 (18)
Zr2—D15^iv	2.090 (16)	D1—D11^xx	2.282 (19)
Zr2—D16^ix	2.071 (15)	D2—Zr2	2.071 (14)
Zr3—Zr1	3.416 (16)	D2—Zr6^viii	2.119 (14)
Zr3—Zr2^iv	3.596 (14)	D2—Zr6^iv	2.112 (15)
Zr3—Zr3^xi	3.31 (2)	D2—Zr7	2.108 (15)
Zr3—Zr4^ii	3.169 (14)	D2—D6	2.307 (15)
Zr3—Zr6^xii	3.304 (14)	D2—D7^ix	2.15 (2)
Zr3—Zr8^ii	3.531 (15)	D2—D13	2.25 (2)
Zr3—Zr8^xiii	3.477 (13)	D3—Zr1^xviii	2.209 (14)
Zr3—Ni1^iv	3.024 (16)	D3—Zr4^iv	2.046 (14)
Zr3—Ni3^xiv	2.864 (18)	D3—Zr5^iv	2.034 (15)
Zr3—Ni3^iii	2.995 (14)	D3—Ni3^iv	1.652 (15)
Zr3—Ni4^xv	2.938 (15)	D3—D4	2.345 (18)
Zr3—D1^iv	2.053 (15)	D3—D9^iv	2.141 (18)
Zr3—D7^xv	2.024 (14)	D3—D14^xviii	2.165 (18)
Zr3—D9^ii	2.102 (14)	D3—D18^xx	2.200 (19)
Zr3—D10	2.081 (14)	D4—Zr4^iv	2.056 (15)
Zr3—D11^v	2.024 (14)	D4—Zr5^iv	2.081 (14)
Zr3—D11^xvi	2.020 (15)	D4—Zr7^iv	2.128 (15)
Zr3—D12^ii	2.195 (13)	D4—Ni2	1.584 (15)
Zr3—D14	2.170 (14)	D4—D3	2.345 (18)
Zr4—Zr1^x	3.591 (12)	D4—D13^iv	2.11 (2)
Zr4—Zr2	3.583 (15)	D4—D15	2.15 (2)
Zr4—Zr2^vii	3.529 (15)	D4—D16	2.212 (18)
Zr4—Zr3^x	3.169 (14)	D5—Zr1^iv	2.141 (14)
Zr4—Zr4^vii	3.20 (2)	D5—Zr5^iv	2.186 (14)
Zr4—Zr5	3.372 (14)	D5—Zr6	2.155 (14)
Zr4—Zr7	3.535 (13)	D5—Zr8^xviii	2.090 (14)
Zr4—Ni2^iv	2.950 (13)	D5—D1^xv	2.050 (18)
Zr4—Ni3	2.821 (16)	D5—D8	2.099 (16)
Zr4—Ni4^x	2.928 (16)	D5—D17^iv	2.016 (18)
Zr4—Ni4^iv	2.893 (14)	D5—D18	2.082 (15)
Zr4—D3^iv	2.046 (14)	D6—Zr2	2.146 (13)
Zr4—D4^iv	2.056 (15)	D6—Zr5	2.094 (15)
Zr4—D9	2.222 (14)	D6—Zr6^iv	2.354 (13)
Zr4—D10^x	2.068 (13)	D6—Zr8^viii	1.989 (11)
Zr4—D12	2.061 (15)	D6—D2	2.307 (15)
Zr4—D15^x	2.110 (15)	D6—D8^iv	2.088 (14)
Zr4—D15^iv	2.099 (14)	D6—D16^ix	2.176 (17)
Zr4—D16^iv	2.210 (15)	D7—Zr2^ix	2.153 (14)
Zr5—Zr1	3.594 (15)	D7—Zr3^viii	2.024 (14)
Zr5—Zr1^iii	3.580 (12)	D7—Zr6^iv	2.040 (15)
Zr5—Zr2	3.585 (16)	D7—Ni4	1.597 (15)
Zr5—Zr4	3.372 (14)	D7—D2^ix	2.15 (2)
Zr5—Zr5^iii	3.34 (2)	D7—D12^xxii	2.11 (2)
Zr5—Zr6^iv	3.160 (14)	D7—D17	2.294 (19)
Zr5—Zr7	3.545 (14)	D8—Zr5^iv	2.123 (14)
Zr5—Zr8^viii	3.506 (14)	D8—Zr8^xviii	2.066 (14)
Zr5—Ni1^v	2.969 (13)	D8—Zr8^xii	2.091 (14)
Zr5—Ni1^iv	2.860 (17)	D8—Ni1^xx	1.660 (13)
Zr5—Ni2^iv	2.992 (15)	D8—D1^xx	2.179 (18)
Zr5—Ni3	3.023 (15)	D8—D5	2.099 (16)
Zr5—D3^iv	2.034 (15)	D8—D6^iv	2.088 (14)
Zr5—D4^iv	2.081 (14)	D8—D8^xxiii	2.33 (2)
Zr5—D5^iv	2.186 (14)	D8—D18^xx	2.310 (16)
Zr5—D6	2.094 (15)	D9—Zr1^iii	2.171 (14)
Zr5—D8^iv	2.123 (14)	D9—Zr3^x	2.102 (14)
Zr5—D13	2.121 (13)	D9—Zr4	2.222 (14)
Zr5—D18^v	2.114 (14)	D9—Zr8	2.050 (14)
Zr5—D18^iv	2.042 (15)	D9—D3^iv	2.141 (18)
Zr6—Zr2^xv	3.527 (13)	D9—D11^xii	2.121 (16)
Zr6—Zr3^xii	3.304 (14)	D9—D14^x	2.111 (18)
Zr6—Zr5^iv	3.160 (14)	D9—D16^iv	2.104 (19)
Zr6—Zr6^xii	3.19 (2)	D10—Zr1	2.209 (12)
Zr6—Zr7^xv	3.580 (15)	D10—Zr3	2.081 (14)
Zr6—Zr7^iv	3.544 (16)	D10—Zr4^ii	2.068 (13)
Zr6—Ni1^xv	2.836 (15)	D10—Zr7^iv	2.131 (13)
Zr6—Ni2^xv	2.896 (15)	D10—D12^ii	2.304 (13)
Zr6—Ni2^iv	2.824 (14)	D10—D14	2.386 (13)
Zr6—Ni4^iv	2.861 (14)	D10—D15	2.068 (16)
Zr6—D1^xv	2.062 (14)	D10—D17	2.318 (17)
Zr6—D2^xv	2.119 (14)	D11—Zr3^xviii	2.024 (14)
Zr6—D2^iv	2.112 (15)	D11—Zr3^xvi	2.020 (15)
Zr6—D5	2.155 (14)	D11—Zr8^xii	2.161 (15)
Zr6—D6^iv	2.354 (13)	D11—Ni3^iv	1.587 (13)
Zr6—D7^iv	2.040 (15)	D11—D1^xx	2.282 (19)
Zr6—D13^iv	2.140 (15)	D11—D9^xii	2.121 (16)
Zr6—D17^iv	2.207 (15)	D11—D11^xxiv	2.33 (2)
Zr7—Zr1^iv	3.298 (12)	D11—D14^xviii	2.051 (16)
Zr7—Zr2	3.071 (6)	D12—Zr2^xv	2.169 (15)
Zr7—Zr4	3.535 (13)	D12—Zr2^vii	2.109 (16)
Zr7—Zr5	3.545 (14)	D12—Zr3^x	2.195 (13)
Zr7—Zr6^viii	3.580 (15)	D12—Zr4	2.061 (15)
Zr7—Zr6^iv	3.544 (16)	D12—D7^xxv	2.11 (2)
Zr7—Zr7^iv	3.24 (2)	D12—D10^x	2.304 (13)
Zr7—Ni1	2.885 (14)	D12—D15^x	2.20 (2)
Zr7—Ni2	2.885 (14)	D12—D16^iv	2.11 (2)
Zr7—Ni2^iv	2.877 (15)	D13—Zr5	2.121 (13)
Zr7—Ni4^iv	2.940 (16)	D13—Zr6^iv	2.140 (15)
Zr7—D2	2.108 (15)	D13—Zr7	2.106 (16)
Zr7—D4^iv	2.128 (15)	D13—Zr7^iv	2.130 (14)
Zr7—D10^iv	2.131 (13)	D13—D2	2.25 (2)
Zr7—D13	2.106 (16)	D13—D4^iv	2.11 (2)
Zr7—D13^iv	2.130 (14)	D13—D17	2.076 (19)
Zr7—D15^iv	2.101 (14)	D14—Zr1	2.014 (14)
Zr7—D17^iv	2.055 (15)	D14—Zr1^i	2.077 (14)
Zr8—Zr1^iii	3.198 (6)	D14—Zr3	2.170 (14)
Zr8—Zr2^xv	3.302 (12)	D14—Ni3^iii	1.546 (12)
Zr8—Zr3^x	3.531 (15)	D14—D3^v	2.165 (18)
Zr8—Zr3^xiii	3.477 (13)	D14—D9^ii	2.111 (18)
Zr8—Zr5^xv	3.506 (14)	D14—D10	2.386 (13)
Zr8—Zr8^xiii	3.442 (19)	D14—D11^v	2.051 (16)
Zr8—Ni1^xvii	3.011 (15)	D15—Zr2^iv	2.090 (16)
Zr8—Ni1^iv	2.913 (15)	D15—Zr4^ii	2.110 (15)
Zr8—Ni2^iv	3.015 (13)	D15—Zr4^iv	2.099 (14)
Zr8—Ni3^xv	2.961 (15)	D15—Zr7^iv	2.101 (14)
Zr8—D1^xvii	2.156 (14)	D15—D4	2.15 (2)
Zr8—D5^v	2.090 (14)	D15—D10	2.068 (16)
Zr8—D6^xv	1.989 (11)	D15—D12^ii	2.20 (2)
Zr8—D8^v	2.066 (14)	D16—Zr2^ix	2.071 (15)
Zr8—D8^xii	2.091 (14)	D16—Zr4^iv	2.210 (15)
Zr8—D9	2.050 (14)	D16—Zr8^iv	2.024 (15)
Zr8—D11^xii	2.161 (15)	D16—Ni2	1.647 (14)
Zr8—D16^iv	2.024 (15)	D16—D4	2.212 (18)
Ni1—Zr1^iv	2.945 (15)	D16—D6^ix	2.176 (17)
Ni1—Zr3^iv	3.024 (16)	D16—D9^iv	2.104 (19)
Ni1—Zr5^xviii	2.969 (13)	D16—D12^iv	2.11 (2)
Ni1—Zr5^iv	2.860 (17)	D17—Zr1	2.036 (15)
Ni1—Zr6^viii	2.836 (15)	D17—Zr6^iv	2.207 (15)
Ni1—Zr7	2.885 (14)	D17—Zr7^iv	2.055 (15)
Ni1—Zr8^xix	3.011 (15)	D17—Ni4	1.610 (14)
Ni1—Zr8^iv	2.913 (15)	D17—D5^iv	2.016 (18)
Ni1—Ni2	2.578 (19)	D17—D7	2.294 (19)
Ni1—D1	1.593 (14)	D17—D10	2.318 (17)
Ni1—D8^xx	1.660 (13)	D17—D13	2.076 (19)
Ni1—D18	1.679 (14)	D18—Zr1^iv	2.061 (14)
Ni2—Zr2^ix	2.975 (16)	D18—Zr5^xviii	2.114 (14)
Ni2—Zr4^iv	2.950 (13)	D18—Zr5^iv	2.042 (15)
Ni2—Zr5^iv	2.992 (15)	D18—Ni1	1.679 (14)
Ni2—Zr6^viii	2.896 (15)	D18—D3^xx	2.200 (19)
Ni2—Zr6^iv	2.824 (14)	D18—D5	2.082 (15)
Ni2—Zr7	2.885 (14)	D18—D8^xx	2.310 (16)
Zr8^iii—Zr1—D3^v	73.8 (4)	Ni2^iv—Zr6—D1^xv	145.5 (6)
Zr8^iii—Zr1—D5^iv	40.3 (4)	Ni2^iv—Zr6—D2^xv	65.3 (5)
Zr8^iii—Zr1—D9^iii	39.4 (4)	Ni2^iv—Zr6—D2^iv	66.5 (5)
Zr8^iii—Zr1—D10	158.8 (4)	Ni2^iv—Zr6—D5	123.0 (6)
Zr8^iii—Zr1—D14	131.8 (4)	Ni2^iv—Zr6—D6^iv	123.1 (6)
Zr8^iii—Zr1—D14^i	91.9 (5)	Ni2^iv—Zr6—D7^iv	73.8 (5)
Zr8^iii—Zr1—D17	93.2 (5)	Ni2^iv—Zr6—D13^iv	65.3 (5)
Zr8^iii—Zr1—D18^iv	74.3 (4)	Ni2^iv—Zr6—D17^iv	70.7 (5)
D3^v—Zr1—D5^iv	98.6 (6)	D1^xv—Zr6—D2^xv	101.2 (7)
D3^v—Zr1—D9^iii	58.5 (5)	D1^xv—Zr6—D2^iv	146.2 (7)
D3^v—Zr1—D10	122.0 (6)	D1^xv—Zr6—D5	58.1 (6)
D3^v—Zr1—D14	61.5 (6)	D1^xv—Zr6—D6^iv	90.8 (6)
D3^v—Zr1—D14^i	93.1 (6)	D1^xv—Zr6—D7^iv	72.0 (6)
D3^v—Zr1—D17	149.8 (7)	D1^xv—Zr6—D13^iv	129.2 (7)
D3^v—Zr1—D18^iv	61.9 (6)	D1^xv—Zr6—D17^iv	91.4 (6)
D5^iv—Zr1—D9^iii	79.6 (5)	D2^xv—Zr6—D2^iv	82.2 (7)
D5^iv—Zr1—D10	119.1 (6)	D2^xv—Zr6—D5	155.4 (8)
D5^iv—Zr1—D14	156.3 (7)	D2^xv—Zr6—D6^iv	126.1 (7)
D5^iv—Zr1—D14^i	122.2 (7)	D2^xv—Zr6—D7^iv	62.3 (6)
D5^iv—Zr1—D17	57.7 (6)	D2^xv—Zr6—D13^iv	127.9 (7)
D5^iv—Zr1—D18^iv	59.4 (5)	D2^xv—Zr6—D17^iv	118.2 (7)
D9^iii—Zr1—D10	159.2 (6)	D2^iv—Zr6—D5	122.4 (7)
D9^iii—Zr1—D14	98.2 (6)	D2^iv—Zr6—D6^iv	61.9 (5)
D9^iii—Zr1—D14^i	59.6 (5)	D2^iv—Zr6—D7^iv	135.1 (7)
D9^iii—Zr1—D17	125.4 (6)	D2^iv—Zr6—D13^iv	63.8 (6)
D9^iii—Zr1—D18^iv	97.8 (5)	D2^iv—Zr6—D17^iv	116.9 (8)
D10—Zr1—D14	68.6 (5)	D5—Zr6—D6^iv	71.4 (5)
D10—Zr1—D14^i	100.5 (6)	D5—Zr6—D7^iv	96.2 (7)
D10—Zr1—D17	66.1 (5)	D5—Zr6—D13^iv	71.1 (6)
D10—Zr1—D18^iv	99.8 (6)	D5—Zr6—D17^iv	55.0 (6)
D14—Zr1—D14^i	74.4 (7)	D6^iv—Zr6—D7^iv	162.5 (7)
D14—Zr1—D17	134.7 (7)	D6^iv—Zr6—D13^iv	71.7 (5)
D14—Zr1—D18^iv	98.1 (7)	D6^iv—Zr6—D17^iv	113.7 (6)
D14^i—Zr1—D17	114.9 (6)	D7^iv—Zr6—D13^iv	116.9 (7)
D14^i—Zr1—D18^iv	153.7 (7)	D7^iv—Zr6—D17^iv	65.3 (6)
D17—Zr1—D18^iv	88.5 (6)	D13^iv—Zr6—D17^iv	57.0 (6)
Zr7—Zr2—Ni3	106.4 (3)	Zr2—Zr7—D2	42.2 (4)
Zr7—Zr2—D2	43.2 (4)	Zr2—Zr7—D4^iv	76.8 (5)
Zr7—Zr2—D6	84.3 (3)	Zr2—Zr7—D10^iv	75.9 (3)
Zr7—Zr2—D7^ix	75.9 (5)	Zr2—Zr7—D13	83.9 (5)
Zr7—Zr2—D12^viii	162.7 (5)	Zr2—Zr7—D13^iv	164.3 (5)
Zr7—Zr2—D12^vii	83.2 (5)	Zr2—Zr7—D15^iv	42.8 (4)
Zr7—Zr2—D15^iv	43.0 (4)	Zr2—Zr7—D17^iv	134.2 (5)
Zr7—Zr2—D16^ix	133.6 (5)	D2—Zr7—D4^iv	98.2 (6)
Ni3—Zr2—D2	123.7 (7)	D2—Zr7—D10^iv	99.3 (7)
Ni3—Zr2—D6	64.2 (5)	D2—Zr7—D13	64.5 (6)
Ni3—Zr2—D7^ix	174.7 (7)	D2—Zr7—D13^iv	127.4 (7)
Ni3—Zr2—D12^viii	83.1 (5)	D2—Zr7—D15^iv	85.0 (5)
Ni3—Zr2—D12^vii	116.0 (6)	D2—Zr7—D17^iv	164.7 (8)
Ni3—Zr2—D15^iv	81.8 (6)	D4^iv—Zr7—D10^iv	114.4 (6)
Ni3—Zr2—D16^ix	87.7 (5)	D4^iv—Zr7—D13	59.9 (6)
D2—Zr2—D6	66.3 (6)	D4^iv—Zr7—D13^iv	96.0 (7)
D2—Zr2—D7^ix	61.3 (6)	D4^iv—Zr7—D15^iv	60.9 (6)
D2—Zr2—D12^viii	141.8 (7)	D4^iv—Zr7—D17^iv	94.2 (7)
D2—Zr2—D12^vii	106.4 (7)	D10^iv—Zr7—D13	159.9 (7)
D2—Zr2—D15^iv	86.2 (5)	D10^iv—Zr7—D13^iv	119.8 (6)
D2—Zr2—D16^ix	92.0 (6)	D10^iv—Zr7—D15^iv	58.5 (5)
D6—Zr2—D7^ix	121.0 (7)	D10^iv—Zr7—D17^iv	67.2 (6)
D6—Zr2—D12^viii	113.0 (5)	D13—Zr7—D13^iv	80.4 (6)
D6—Zr2—D12^vii	167.0 (7)	D13—Zr7—D15^iv	106.1 (7)
D6—Zr2—D15^iv	104.7 (7)	D13—Zr7—D17^iv	130.2 (8)
D6—Zr2—D16^ix	62.1 (5)	D13^iv—Zr7—D15^iv	144.4 (7)
D7^ix—Zr2—D12^viii	93.5 (7)	D13^iv—Zr7—D17^iv	59.5 (6)
D7^ix—Zr2—D12^vii	59.2 (6)	D15^iv—Zr7—D17^iv	93.4 (6)
D7^ix—Zr2—D15^iv	97.2 (7)	Zr1^iii—Zr8—D1^xvii	79.2 (4)
D7^ix—Zr2—D16^ix	94.1 (7)	Zr1^iii—Zr8—D5^v	41.5 (4)
D12^viii—Zr2—D12^vii	79.6 (6)	Zr1^iii—Zr8—D6^xv	161.0 (4)
D12^viii—Zr2—D15^iv	127.5 (7)	Zr1^iii—Zr8—D8^v	94.0 (5)
D12^viii—Zr2—D16^ix	59.7 (6)	Zr1^iii—Zr8—D8^xii	136.6 (4)
D12^vii—Zr2—D15^iv	63.2 (6)	Zr1^iii—Zr8—D9	42.2 (4)
D12^vii—Zr2—D16^ix	130.3 (8)	Zr1^iii—Zr8—D11^xii	79.7 (4)
D15^iv—Zr2—D16^ix	166.0 (8)	Zr1^iii—Zr8—D16^iv	96.7 (5)
Zr4^ii—Zr3—D1^iv	133.7 (7)	D1^xvii—Zr8—D5^v	57.7 (5)
Zr4^ii—Zr3—D7^xv	94.1 (6)	D1^xvii—Zr8—D6^xv	113.7 (7)
Zr4^ii—Zr3—D9^ii	44.4 (4)	D1^xvii—Zr8—D8^v	88.4 (6)
Zr4^ii—Zr3—D10	40.0 (4)	D1^xvii—Zr8—D8^xii	61.7 (6)
Zr4^ii—Zr3—D11^v	134.4 (6)	D1^xvii—Zr8—D9	102.2 (6)
Zr4^ii—Zr3—D11^xvi	99.0 (5)	D1^xvii—Zr8—D11^xii	63.8 (6)
Zr4^ii—Zr3—D12^ii	40.3 (4)	D1^xvii—Zr8—D16^iv	155.8 (7)
Zr4^ii—Zr3—D14	78.4 (5)	D5^v—Zr8—D6^xv	157.2 (6)
D1^iv—Zr3—D7^xv	72.5 (6)	D5^v—Zr8—D8^v	60.7 (5)
D1^iv—Zr3—D9^ii	152.6 (8)	D5^v—Zr8—D8^xii	98.0 (6)
D1^iv—Zr3—D10	94.5 (7)	D5^v—Zr8—D9	83.6 (5)
D1^iv—Zr3—D11^v	68.1 (6)	D5^v—Zr8—D11^xii	99.7 (5)
D1^iv—Zr3—D11^xvi	126.9 (7)	D5^v—Zr8—D16^iv	131.8 (6)
D1^iv—Zr3—D12^ii	127.1 (7)	D6^xv—Zr8—D8^v	100.0 (6)
D1^iv—Zr3—D14	93.5 (6)	D6^xv—Zr8—D8^xii	61.5 (5)
D7^xv—Zr3—D9^ii	130.6 (7)	D6^xv—Zr8—D9	119.2 (6)
D7^xv—Zr3—D10	88.9 (6)	D6^xv—Zr8—D11^xii	93.4 (6)
D7^xv—Zr3—D11^v	130.9 (6)	D6^xv—Zr8—D16^iv	65.7 (6)
D7^xv—Zr3—D11^xvi	115.7 (7)	D8^v—Zr8—D8^xii	68.2 (7)
D7^xv—Zr3—D12^ii	59.7 (6)	D8^v—Zr8—D9	129.4 (7)
D7^xv—Zr3—D14	152.5 (8)	D8^v—Zr8—D11^xii	152.1 (7)
D9^ii—Zr3—D10	74.1 (6)	D8^v—Zr8—D16^iv	115.8 (6)
D9^ii—Zr3—D11^v	96.4 (6)	D8^xii—Zr8—D9	158.0 (7)
D9^ii—Zr3—D11^xvi	61.9 (5)	D8^xii—Zr8—D11^xii	97.8 (6)
D9^ii—Zr3—D12^ii	71.1 (6)	D8^xii—Zr8—D16^iv	126.7 (6)
D9^ii—Zr3—D14	59.2 (6)	D9—Zr8—D11^xii	60.4 (5)
D10—Zr3—D11^v	121.5 (7)	D9—Zr8—D16^iv	62.2 (6)
D10—Zr3—D11^xvi	135.8 (7)	D11^xii—Zr8—D16^iv	92.0 (6)
D10—Zr3—D12^ii	65.2 (5)	Zr6^viii—Ni1—D1	45.6 (6)
D10—Zr3—D14	68.3 (5)	Zr6^viii—Ni1—D8^xx	102.2 (6)
D11^v—Zr3—D11^xvi	70.4 (7)	Zr6^viii—Ni1—D18	170.0 (7)
D11^v—Zr3—D12^ii	164.4 (9)	D1—Ni1—D8^xx	84.1 (8)
D11^v—Zr3—D14	58.4 (5)	D1—Ni1—D18	139.1 (11)
D11^xvi—Zr3—D12^ii	95.0 (7)	D8^xx—Ni1—D18	87.5 (7)
D11^xvi—Zr3—D14	91.7 (7)	Zr6^iv—Ni2—D4	122.8 (8)
D12^ii—Zr3—D14	118.6 (6)	Zr6^iv—Ni2—D16	116.2 (7)
Zr3^x—Zr4—Zr4^vii	121.5 (6)	D4—Ni2—D16	86.4 (8)
Zr3^x—Zr4—Ni3	104.9 (4)	Zr2—Ni3—Zr4	78.9 (4)
Zr3^x—Zr4—D3^iv	95.8 (5)	Zr2—Ni3—D3^iv	99.6 (6)
Zr3^x—Zr4—D4^iv	133.7 (6)	Zr2—Ni3—D11^iv	96.6 (7)
Zr3^x—Zr4—D9	41.4 (4)	Zr2—Ni3—D14^iii	174.0 (9)
Zr3^x—Zr4—D10^x	40.3 (4)	Zr4—Ni3—D3^iv	45.8 (6)
Zr3^x—Zr4—D12	43.5 (4)	Zr4—Ni3—D11^iv	173.4 (9)
Zr3^x—Zr4—D15^x	81.0 (6)	Zr4—Ni3—D14^iii	102.2 (7)
Zr3^x—Zr4—D15^iv	162.1 (7)	D3^iv—Ni3—D11^iv	140.5 (11)
Zr3^x—Zr4—D16^iv	73.9 (5)	D3^iv—Ni3—D14^iii	85.2 (9)
Zr4^vii—Zr4—Ni3	101.8 (6)	D11^iv—Ni3—D14^iii	81.8 (7)
Zr4^vii—Zr4—D3^iv	132.4 (7)	D7—Ni4—D17	91.4 (8)
Zr4^vii—Zr4—D4^iv	97.8 (6)	Zr3^iv—D1—Zr6^viii	106.8 (7)
Zr4^vii—Zr4—D9	162.8 (7)	Zr3^iv—D1—Zr8^xix	111.3 (7)
Zr4^vii—Zr4—D10^x	92.8 (6)	Zr3^iv—D1—Ni1	111.5 (9)
Zr4^vii—Zr4—D12	96.2 (7)	Zr6^viii—D1—Zr8^xix	119.9 (7)
Zr4^vii—Zr4—D15^x	40.5 (4)	Zr6^viii—D1—Ni1	101.0 (8)
Zr4^vii—Zr4—D15^iv	40.7 (4)	Zr8^xix—D1—Ni1	105.9 (8)
Zr4^vii—Zr4—D16^iv	127.4 (7)	Zr2—D2—Zr6^viii	114.6 (8)
Ni3—Zr4—D3^iv	35.3 (5)	Zr2—D2—Zr6^iv	121.2 (7)
Ni3—Zr4—D4^iv	88.3 (6)	Zr2—D2—Zr7	94.6 (6)
Ni3—Zr4—D9	84.9 (5)	Zr6^viii—D2—Zr6^iv	97.8 (7)
Ni3—Zr4—D10^x	85.2 (5)	Zr6^viii—D2—Zr7	115.8 (7)
Ni3—Zr4—D12	148.3 (6)	Zr6^iv—D2—Zr7	114.2 (8)
Ni3—Zr4—D15^x	117.0 (6)	Zr1^xviii—D3—Zr4^iv	119.6 (7)
Ni3—Zr4—D15^iv	81.6 (5)	Zr1^xviii—D3—Zr5^iv	115.0 (7)
Ni3—Zr4—D16^iv	123.8 (6)	Zr1^xviii—D3—Ni3^iv	99.4 (7)
D3^iv—Zr4—D4^iv	69.7 (6)	Zr4^iv—D3—Zr5^iv	111.5 (7)
D3^iv—Zr4—D9	60.0 (6)	Zr4^iv—D3—Ni3^iv	98.9 (8)
D3^iv—Zr4—D10^x	99.8 (6)	Zr5^iv—D3—Ni3^iv	109.8 (9)
D3^iv—Zr4—D12	131.1 (7)	Zr4^iv—D4—Zr5^iv	109.2 (7)
D3^iv—Zr4—D15^x	150.6 (8)	Zr4^iv—D4—Zr7^iv	115.3 (8)
D3^iv—Zr4—D15^iv	98.7 (7)	Zr4^iv—D4—Ni2	107.6 (9)
D3^iv—Zr4—D16^iv	88.4 (6)	Zr5^iv—D4—Zr7^iv	114.7 (7)
D4^iv—Zr4—D9	98.2 (6)	Zr5^iv—D4—Ni2	108.7 (9)
D4^iv—Zr4—D10^x	168.5 (7)	Zr7^iv—D4—Ni2	100.6 (7)
D4^iv—Zr4—D12	115.1 (7)	Zr1^iv—D5—Zr5^iv	112.3 (6)
D4^iv—Zr4—D15^x	132.2 (7)	Zr1^iv—D5—Zr6	120.0 (6)
D4^iv—Zr4—D15^iv	62.1 (6)	Zr1^iv—D5—Zr8^xviii	98.2 (6)
D4^iv—Zr4—D16^iv	62.3 (6)	Zr5^iv—D5—Zr6	93.4 (6)
D9—Zr4—D10^x	71.8 (5)	Zr5^iv—D5—Zr8^xviii	115.4 (6)
D9—Zr4—D12	71.3 (6)	Zr6—D5—Zr8^xviii	118.7 (7)
D9—Zr4—D15^x	122.5 (7)	Zr2—D6—Zr5	115.4 (6)
D9—Zr4—D15^iv	156.3 (8)	Zr2—D6—Zr6^iv	108.1 (5)
D9—Zr4—D16^iv	56.7 (6)	Zr2—D6—Zr8^viii	105.9 (5)
D10^x—Zr4—D12	67.8 (5)	Zr5—D6—Zr6^iv	90.3 (5)
D10^x—Zr4—D15^x	59.3 (5)	Zr5—D6—Zr8^viii	118.3 (6)
D10^x—Zr4—D15^iv	125.9 (7)	Zr6^iv—D6—Zr8^viii	118.3 (7)
D10^x—Zr4—D16^iv	114.1 (6)	Zr2^ix—D7—Zr3^viii	118.8 (7)
D12—Zr4—D15^x	63.7 (7)	Zr2^ix—D7—Zr6^iv	114.5 (7)
D12—Zr4—D15^iv	127.5 (8)	Zr2^ix—D7—Ni4	102.3 (8)
D12—Zr4—D16^iv	59.1 (6)	Zr3^viii—D7—Zr6^iv	108.8 (7)
D15^x—Zr4—D15^iv	81.2 (7)	Zr3^viii—D7—Ni4	107.9 (9)
D15^x—Zr4—D16^iv	118.1 (8)	Zr6^iv—D7—Ni4	103.0 (9)
D15^iv—Zr4—D16^iv	116.8 (7)	Zr5^iv—D8—Zr8^xviii	119.3 (7)
Zr6^iv—Zr5—D3^iv	135.7 (7)	Zr5^iv—D8—Zr8^xii	112.6 (7)
Zr6^iv—Zr5—D4^iv	96.5 (6)	Zr5^iv—D8—Ni1^xx	102.7 (7)
Zr6^iv—Zr5—D5^iv	42.9 (4)	Zr8^xviii—D8—Zr8^xii	111.8 (7)
Zr6^iv—Zr5—D6	48.2 (4)	Zr8^xviii—D8—Ni1^xx	102.3 (8)
Zr6^iv—Zr5—D8^iv	76.1 (5)	Zr8^xii—D8—Ni1^xx	106.2 (8)
Zr6^iv—Zr5—D13	42.4 (4)	Zr1^iii—D9—Zr3^x	118.4 (6)
Zr6^iv—Zr5—D18^v	140.3 (6)	Zr1^iii—D9—Zr4	113.7 (7)
Zr6^iv—Zr5—D18^iv	95.5 (5)	Zr1^iii—D9—Zr8	98.5 (6)
D3^iv—Zr5—D4^iv	69.5 (6)	Zr3^x—D9—Zr4	94.2 (6)
D3^iv—Zr5—D5^iv	155.9 (7)	Zr3^x—D9—Zr8	116.5 (7)
D3^iv—Zr5—D6	90.5 (7)	Zr4—D9—Zr8	116.9 (6)
D3^iv—Zr5—D8^iv	97.7 (7)	Zr1—D10—Zr3	105.5 (5)
D3^iv—Zr5—D13	126.1 (7)	Zr1—D10—Zr4^ii	114.2 (6)
D3^iv—Zr5—D18^v	64.0 (6)	Zr1—D10—Zr7^iv	98.9 (5)
D3^iv—Zr5—D18^iv	128.6 (7)	Zr3—D10—Zr4^ii	99.6 (5)
D4^iv—Zr5—D5^iv	131.0 (7)	Zr3—D10—Zr7^iv	119.4 (6)
D4^iv—Zr5—D6	96.5 (6)	Zr4^ii—D10—Zr7^iv	119.1 (6)
D4^iv—Zr5—D8^iv	153.4 (8)	Zr3^xviii—D11—Zr3^xvi	109.6 (7)
D4^iv—Zr5—D13	60.4 (6)	Zr3^xviii—D11—Zr8^xii	112.3 (7)
D4^iv—Zr5—D18^v	122.7 (6)	Zr3^xviii—D11—Ni3^iv	111.5 (8)
D4^iv—Zr5—D18^iv	116.9 (7)	Zr3^xvi—D11—Zr8^xii	115.2 (7)
D5^iv—Zr5—D6	76.0 (6)	Zr3^xvi—D11—Ni3^iv	104.5 (9)
D5^iv—Zr5—D8^iv	58.3 (5)	Zr8^xii—D11—Ni3^iv	103.3 (7)
D5^iv—Zr5—D13	70.8 (6)	Zr2^xv—D12—Zr2^vii	100.4 (6)
D5^iv—Zr5—D18^v	103.4 (6)	Zr2^xv—D12—Zr3^x	114.6 (7)
D5^iv—Zr5—D18^iv	58.9 (5)	Zr2^xv—D12—Zr4	117.5 (7)
D6—Zr5—D8^iv	59.4 (5)	Zr2^vii—D12—Zr3^x	113.4 (7)
D6—Zr5—D13	77.5 (5)	Zr2^vii—D12—Zr4	115.6 (8)
D6—Zr5—D18^v	114.9 (7)	Zr3^x—D12—Zr4	96.2 (6)
D6—Zr5—D18^iv	134.4 (7)	Zr5—D13—Zr6^iv	95.7 (6)
D8^iv—Zr5—D13	118.4 (7)	Zr5—D13—Zr7	114.0 (7)
D8^iv—Zr5—D18^v	66.1 (5)	Zr5—D13—Zr7^iv	119.6 (7)
D8^iv—Zr5—D18^iv	89.4 (7)	Zr6^iv—D13—Zr7	113.1 (8)
D13—Zr5—D18^v	165.3 (9)	Zr6^iv—D13—Zr7^iv	115.7 (7)
D13—Zr5—D18^iv	92.5 (7)	Zr7—D13—Zr7^iv	99.6 (6)
D18^v—Zr5—D18^iv	73.2 (6)	Zr1—D14—Zr1^i	105.6 (7)
Zr5^iv—Zr6—Zr6^xii	119.9 (6)	Zr1—D14—Zr3	109.4 (7)
Zr5^iv—Zr6—Ni1^xv	103.6 (4)	Zr1—D14—Ni3^iii	112.2 (8)
Zr5^iv—Zr6—Ni2^iv	107.2 (5)	Zr1^i—D14—Zr3	119.6 (7)
Zr5^iv—Zr6—D1^xv	94.2 (6)	Zr1^i—D14—Ni3^iii	103.7 (9)
Zr5^iv—Zr6—D2^xv	160.9 (7)	Zr3—D14—Ni3^iii	106.2 (8)
Zr5^iv—Zr6—D2^iv	78.7 (6)	Zr2^iv—D15—Zr4^ii	114.3 (8)
Zr5^iv—Zr6—D5	43.7 (4)	Zr2^iv—D15—Zr4^iv	117.6 (7)
Zr5^iv—Zr6—D6^iv	41.5 (4)	Zr2^iv—D15—Zr7^iv	94.2 (6)
Zr5^iv—Zr6—D7^iv	134.5 (6)	Zr4^ii—D15—Zr4^iv	98.8 (7)
Zr5^iv—Zr6—D13^iv	41.9 (4)	Zr4^ii—D15—Zr7^iv	118.6 (7)
Zr5^iv—Zr6—D17^iv	72.3 (5)	Zr4^iv—D15—Zr7^iv	114.6 (8)
Zr6^xii—Zr6—Ni1^xv	102.5 (6)	Zr2^ix—D16—Zr4^iv	115.3 (8)
Zr6^xii—Zr6—Ni2^iv	57.2 (4)	Zr2^ix—D16—Zr8^iv	107.5 (7)
Zr6^xii—Zr6—D1^xv	132.8 (8)	Zr2^ix—D16—Ni2	105.7 (8)
Zr6^xii—Zr6—D2^xv	41.0 (4)	Zr4^iv—D16—Zr8^iv	118.6 (7)
Zr6^xii—Zr6—D2^iv	41.2 (4)	Zr4^iv—D16—Ni2	98.7 (7)
Zr6^xii—Zr6—D5	163.5 (7)	Zr8^iv—D16—Ni2	110.0 (9)
Zr6^xii—Zr6—D6^iv	94.6 (5)	Zr1—D17—Zr6^iv	122.5 (7)
Zr6^xii—Zr6—D7^iv	99.2 (6)	Zr1—D17—Zr7^iv	107.5 (7)
Zr6^xii—Zr6—D13^iv	96.7 (7)	Zr1—D17—Ni4	106.6 (9)
Zr6^xii—Zr6—D17^iv	127.9 (7)	Zr6^iv—D17—Zr7^iv	116.0 (8)
Ni1^xv—Zr6—Ni2^iv	148.7 (5)	Zr6^iv—D17—Ni4	95.8 (8)
Ni1^xv—Zr6—D1^xv	33.5 (4)	Zr7^iv—D17—Ni4	106.1 (8)
Ni1^xv—Zr6—D2^xv	83.8 (5)	Zr1^iv—D18—Zr5^xviii	118.1 (7)
Ni1^xv—Zr6—D2^iv	115.8 (6)	Zr1^iv—D18—Zr5^iv	122.3 (7)
Ni1^xv—Zr6—D5	83.6 (5)	Zr1^iv—D18—Ni1	103.4 (7)
Ni1^xv—Zr6—D6^iv	78.3 (4)	Zr5^xviii—D18—Zr5^iv	106.8 (6)
Ni1^xv—Zr6—D7^iv	88.2 (6)	Zr5^xviii—D18—Ni1	102.5 (7)
Ni1^xv—Zr6—D13^iv	145.5 (6)	Zr5^iv—D18—Ni1	100.0 (8)
Ni1^xv—Zr6—D17^iv	124.9 (6)

Symmetry codes: (i) −x+1, −y+2, −z; (ii) x, y, z−1; (iii) −x+1, −y+2, −z+1; (iv) −x+1, −y+1, −z+1; (v) x, y+1, z; (vi) −x+2, −y+1, −z+2; (vii) −x+1, −y+1, −z+2; (viii) x+1, y, z; (ix) −x+2, −y+1, −z+1; (x) x, y, z+1; (xi) −x, −y+2, −z; (xii) −x, −y+1, −z+1; (xiii) −x, −y+2, −z+1; (xiv) x−1, y, z−1; (xv) x−1, y, z; (xvi) −x, −y+1, −z; (xvii) x−1, y+1, z; (xviii) x, y−1, z; (xix) x+1, y−1, z; (xx) −x+1, −y, −z+1; (xxi) x+1, y, z+1; (xxii) x+1, y, z−1; (xxiii) −x, −y, −z+1; (xxiv) −x, −y, −z; (xxv) x−1, y, z+1.