Ni(Glu)

Crystal submitted by:

Crystal submitted on:

Data collected on:

Structure solved by:

Table 1 Crystal data and structure refinement for Ni(Glu)
Identification code	Ni(Glu)
Empirical formula	C₅H₁₁NNiO₆
Formula weight	239.86
Temperature/K	100.0
Crystal system	Orthorhombic
Space group	P2₁2₁2₁
a/Å, b/Å, c/Å	7.1385(14), 10.343(2), 11.135(2)
α/°, β/°, γ/°	90.00, 90.00, 90.00
Volume/Å³	822.2(3)
Z	4
ρ_calcmg/mm³	1.938
m/mm^‑1	2.359
F(000)	496
Crystal size/mm³	0.1 × 0.1 × 0.1
Theta range for data collection	2.69 to 27.92°
Index ranges	-8 ≤ h ≤ 9, -13 ≤ k ≤ 13, -12 ≤ l ≤ 14
Reflections collected	4322
Independent reflections	1858[R(int) = 0.0364]
Data/restraints/parameters	1858/0/162
Goodness-of-fit on F²	0.785
Final R indexes [I>2σ (I)]	R₁ = 0.0257, wR₂ = 0.0363
Final R indexes [all data]	R₁ = 0.0305, wR₂ = 0.0368
Largest diff. peak/hole / e Å^-3	0.483/-0.381

Table 2 Atomic Coordinates (Å×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for Ni(Glu). U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
Ni1	8919.6(5)	4344.1(3)	390.9(3)	9.11(8)
O1	10225(2)	2599.9(16)	229.3(17)	9(4)
O5W	7983(3)	6179.3(18)	307(2)	17(5)
O3	14964(2)	5351.1(17)	-2921.7(15)	10.9(4)
C5	13490(4)	4773(2)	-3286(2)	11.8(7)
O2	6452(2)	3740.1(15)	1138.2(15)	12.1(4)
O4	13188(2)	4659.7(15)	-4410(16)	13.1(5)
N1	8205(4)	3929(2)	-1363(2)	11.1(6)
C1	10408(4)	2187(2)	-832(2)	9(6)
C2	9341(4)	2849(2)	-1846(2)	9.9(7)
C4	12178(4)	4239(3)	-2345(2)	12.7(6)
C3	10701(4)	3323(3)	-2821(3)	11.4(7)
O6W	4618(3)	6493(2)	-763(2)	14(5)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for Ni(Glu). The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+...+2hka×b×U₁₂]
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
Ni1	8.31(16)	10.18(14)	8.83(15)	-0.08(17)	0.05(17)	-0.32(16)
O1	9.6(10)	10.8(9)	6.7(10)	0.1(9)	-1(9)	3.2(7)
O5W	10.2(11)	12.1(10)	28.8(13)	-0.5(11)	-6.6(12)	-0.1(8)
O3	8.9(11)	15.8(11)	7.9(9)	-0.3(8)	-0.9(8)	-3.7(8)
C5	11.9(18)	9.5(13)	14.1(16)	1.2(11)	1.5(12)	4.1(11)
O2	11(11)	11.9(9)	13.3(10)	-1.8(8)	0.7(9)	-1.5(8)
O4	11.5(10)	16.1(10)	11.8(11)	0(8)	0.6(8)	-0.7(7)
N1	11.3(14)	11.5(13)	10.6(14)	3.9(11)	-0.3(11)	3.7(10)
C1	7.1(14)	5.3(13)	14.5(15)	0(11)	0.5(12)	-2.8(11)
C2	7.7(17)	8.3(14)	13.8(16)	-2.9(12)	-0.4(12)	-2.5(11)
C4	11.1(15)	16.1(16)	11.1(14)	0.4(14)	-1.3(12)	-3.3(14)
C3	10(18)	16.3(15)	7.9(14)	2.4(13)	-0.4(12)	-0.6(12)
O6W	14.5(12)	14.5(11)	13.1(13)	0.6(10)	1.2(10)	-1.9(9)

Table 4 Bond Lengths for Ni(Glu).
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Ni1	O1	2.0386(17)	C5	O4²	1.276(3)
Ni1	O5W	2.0147(19)	C5	C4	1.510(4)
Ni1	O3¹	2.0651(17)	O2	C1	1.261(3)
Ni1	O2	2.0460(18)	O4	Ni1	2.3181(16)
Ni1	O4¹	2.3181(16)	N1	C2³	1.482(3)
Ni1	N1	2.064(2)	C1	O2	1.261(3)
O1	C1	1.264(3)	C1	C2	1.524(4)
O3	Ni1	2.0650(17)	C2	C3	1.537(3)
O3	C5	1.276(3)	C4	C3⁴	1.514(4)

¹2+X,1+Y,+Z; ²2+X,1+Y,-1+Z; ³-1/2-X,-Y,1/2+Z; ⁴1/2-X,-Y,1/2+Z

Table 5 Bond Angles for Ni(Glu).
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
O1	Ni1	O3	92.23(7)	O2	Ni1	O4	149.74(7)
O1	Ni1	O2	99.17(7)	O2	Ni1	N1	96.23(9)
O1	Ni1	O4	89.69(6)	O2	C1	O1	124.8(2)
O1	Ni1	N1	81.11(8)	O2	C1	C2	115.9(2)
O1	C1	C2¹	119.3(2)	O4	C5	O3	119.6(2)
O5W	Ni1	O1	168.94(9)	O4	C5	C4¹	122.8(2)
O5W	Ni1	O3¹	91.52(8)	N1	Ni1	O3¹	171.18(9)
O5W	Ni1	O2	91.19(8)	N1	Ni1	O4	113.77(8)
O5W	Ni1	O4	83.18(8)	N1³	C2	C1	110.1(2)
O5W	Ni1	N1	94.01(10)	N1³	C2	C3	111.2(2)
O3	Ni1	O4¹	60.09(6)	C1	O1	Ni1	115.38(16)
O3	C5	C4	117.5(2)	C1	O2	Ni1¹	129.13(17)
C5	O3	Ni1¹	95.77(16)	C1	C2	C3¹	110.5(2)
C5	O4	Ni1	84.40(15)	C2	N1	Ni1	111.42(17)
C5¹	C4	C3¹	114.7(2)	C4	C3	C2	113.1(2)
O2	Ni1	O3²	90.51(7)

¹2+X,1+Y,+Z; ²2+X,1+Y,-1+Z; ³1/2-X,-Y,1/2+Z; ⁴-1/2-X,-Y,1/2+Z

Table 6 Hydrogen Bonds for Ni(Glu).
D	H	A	d(D-H)/Å	d(H-A)/Å	d(D-A)/Å	D-H-A/°
O5W	H5WA	O6W	0.79(3)	1.92(3)	2.701(3)	173(3)
O5W	H5WB	O6W¹	0.82(3)	1.92(3)	2.723(3)	165(3)
O6W	H6WA	O4²	0.70(3)	2.09(3)	2.776(3)	167(3)
O6W	H6WB	O3³	0.81(3)	1.89(3)	2.689(3)	170(3)

¹1/2-X,1-Y,1/2+Z; ²1+X,1+Y,+Z; ³-1/2+X,1/2-Y,-Z

Table 7 Torsion Angles for Ni(Glu).
A	B	C	D	Angle/˚
Ni1	O1	C1	O2¹	166.73(19)
Ni1	O1	C1	C2	-12.0(3)
Ni1²	O3	C5	O4	-3.6(2)
Ni1²	O3	C5	C4	175.9(2)
Ni1	N1	C2	C1	11.7(3)
Ni1	N1	C2	C3	-111.2(2)
O1	Ni1	O2	C1³	-46.5(2)
O1	Ni1	N1	C2	-13.81(17)
O1	C1	C2	N1	-0.1(3)
O1	C1	C2	C3	123.2(3)
O5W	Ni1	O1	C1	-49.9(5)
O5W	Ni1	O2	C1³	129.6(2)
O5W	Ni1	N1	C2	156.19(18)
O3⁴	Ni1	O1	C1	-159.62(19)
O3⁴	Ni1	O2	C1³	-138.8(2)
O3⁴	Ni1	N1	C2	27.5(7)
O3	C5	O4	Ni1²	3.2(2)
O3	C5	C4	C3	-167.3(2)
C5	C4	C3	C2	-177.4(2)
O2	Ni1	O1	C1	109.50(19)
O2	Ni1	N1	C2	-112.16(18)
O2¹	C1	C2	N1	-178.9(2)
O2¹	C1	C2	C3	-55.7(3)
O4⁴	Ni1	O1	C1	-99.57(19)
O4⁴	Ni1	O2	C1³	-151.91(18)
O4⁴	Ni1	N1	C2	71.89(19)
O4	C5	C4	C3	12.2(4)
N1	Ni1	O1	C1	14.56(19)
N1	Ni1	O2	C1³	35.5(2)
N1	C2	C3	C4	65.2(3)
C1	C2	C3	C4	-57.4(3)
C4	C5	O4	Ni1²	-176.3(2)

¹1/2-X,-Y,1/2+Z; ²2+X,1+Y,-1+Z; ³-1/2-X,-Y,1/2+Z; ⁴2+X,1+Y,+Z

Table 8 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for Ni(Glu).
Atom	x	y	z	U(eq)
H3B	11310(3)	2490(2)	-3217(18)	3(6)
H3A	9950(4)	3710(3)	-3410(2)	17(8)
H5WA	7010(4)	6340(2)	0(2)	18(10)
H6WA	4040(4)	6140(2)	-380(2)	11(9)
H1B	8090(3)	4540(2)	-1810(2)	3(8)
H4A	11660(3)	5040(2)	-1890(2)	20(8)
H1A	6890(4)	3680(2)	-1200(2)	14(8)
H6WB	4690(5)	6070(3)	-1370(3)	50(14)
H5WB	8640(5)	6810(3)	470(3)	61(12)
H4B	13000(4)	3770(2)	-1660(2)	25(8)
H2	8580(3)	2233(19)	-2230(2)	0(6)

[RSC Journal Format]

Experimental

Single crystals of C₅H₁₁NNiO₆ [Ni(Glu)] were recrystallised from [solvents] mounted in inert oil and transferred to the cold gas stream of the diffractometer.

Crystal structure determination of [Ni(Glu)]

Crystal Data. C₅H₁₁NNiO₆, M =239.86, Orthorhombic, a = 7.1385(14) Å, b = 10.343(2) Å, c = 11.135(2) Å, U = 822.2(3) Å³, T = 100.0, space group P2₁2₁2₁ (no. 19), Z = 4, μ(Mo-Kα) = 2.359, 4322 reflections measured, 1858 unique (R_int = 0.0364) which were used in all calculations. The final wR(F₂) was 0.0368 (all data).

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