rudi001

Table 1 Crystal data and structure refinement for rudi001.

Identification code	rudi001
Empirical formula	C14H20B22Cl22N6Ni
Formula weight	1348.79
Temperature/K	100.00
Crystal system	orthorhombic
Space group	Pnma
a/Å	10.3212(3)
b/Å	13.0627(3)
c/Å	20.4914(5)
α/°	90
β/°	90
γ/°	90
Volume/Å3	2762.71(12)
Z	2
ρcalcg/cm3	1.621
μ/mm‑1	10.516
F(000)	1316.0
Crystal size/mm3	0.259 × 0.149 × 0.132
Radiation	CuKα (λ = 1.54178)
2Θ range for data collection/°	9.594 to 149.166
Index ranges	-12 ≤ h ≤ 12, -16 ≤ k ≤ 16, -25 ≤ l ≤ 25
Reflections collected	35499
Independent reflections	2943 [Rint = 0.0506, Rsigma = 0.0225]
Data/restraints/parameters	2943/148/236
Goodness-of-fit on F2	1.206
Final R indexes [I>=2σ (I)]	R1 = 0.0417, wR2 = 0.1159
Final R indexes [all data]	R1 = 0.0429, wR2 = 0.1166
Largest diff. peak/hole / e Å-3	2.29/-0.44

Experimental

Single crystals of C₁₄H₂₀B₂₂Cl₂₂N₆Ni [rudi001] were []. A suitable crystal was selected and [] on a Bruker Venture Photon III diffractometer. The crystal was kept at 100.00 K during data collection. Using Olex2 [1], the structure was solved with the XS [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.

1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
2. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [rudi001]

Crystal Data for C₁₄H₂₀B₂₂Cl₂₂N₆Ni (M =1348.79 g/mol): orthorhombic, space group Pnma (no. 62), a = 10.3212(3) Å, b = 13.0627(3) Å, c = 20.4914(5) Å, V = 2762.71(12) Å³, Z = 2, T = 100.00 K, μ(CuKα) = 10.516 mm^-1, Dcalc = 1.621 g/cm³, 35499 reflections measured (9.594° ≤ 2Θ ≤ 149.166°), 2943 unique (R_int = 0.0506, R_sigma = 0.0225) which were used in all calculations. The final R₁ was 0.0417 (I > 2σ(I)) and wR₂ was 0.1166 (all data).

Refinement model description

Number of restraints - 148, number of constraints - unknown.

Details:

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Ni1-N4 ≈ Ni1-N1 ≈ Ni1-N3 ≈ Ni1-N2
 with sigma of 0.002
 N4-C7 ≈ N1-C1 ≈ N3-C5 ≈ N2-C3
 with sigma of 0.002
 C2-C1 ≈ C8-C7 ≈ C4-C3 ≈ C6-C5
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Ni1 ≈ C7 ≈ C8 ≈ N4 ≈ N1 ≈ C1 ≈ N2 ≈ C3 ≈ C4
≈ N3 ≈ C5 ≈ C6: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Uanis(C2) ≈ Ueq, Uanis(N1) ≈ Ueq, Uanis(Ni1) ≈ Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Ni1, C2, C1, N1, C8, C7, N4, N2, C3, C4, N3, C5, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Ni1(0.25) N1(0.25) N2(0.5) N3(0.25) N4(0.5) C1(0.25) C2(0.25)
 H2A(0.25) H2B(0.25) H2C(0.25) C3(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
 C5(0.25) C6(0.25) H6A(0.25) H6B(0.25) H6C(0.25) C7(0.5) C8(0.5) H8A(0.5)
 H8B(0.5) H8C(0.5)
6.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
6.b Boron cage BH refined with riding coordinates:
 C9(H9)

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