Literature DB >> 21202214

Tetra-kis(μ(3)-2-{[1,1-bis-(hydroxy-meth-yl)-2-oxidoeth-yl]imino-meth-yl}-6-methoxy-phenol-ato)tetra-nickel(II) tetra-hydrate.

Yujing Guo¹, Lianzhi Li, Yan Liu, Jianfang Dong, Daqi Wang.

Abstract

The title complex, [Ni(4)(C(12)H(15)NO(4))(4)]·4H(2)O, has crystal-lographic fourfold inversion symmetry, with each Ni(II) ion coordinated in a slightly distorted square-pyramidal coordination environment and forming an Ni(4)O(4) cubane-like core. In the crystal structure, inter-molecular O-H⋯O hydrogen bonds connect complex and water mol-ecules to form a three-dimensional network. The O atom of one of the unique hydroxy-methyl groups is disordered over two sites, with the ratio of occupancies being approximately 0.79:0.21.

Entities: CellLine Chemical Disease Species

Year: 2008 PMID： 21202214 PMCID： PMC2961190 DOI： 10.1107/S1600536808009872

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For related literature, see: Dong, Li, Xu & Wang (2007 ▶); Dong, Li, Xu, Cui & Wang (2007 ▶); Koikawa et al. (2005 ▶); Mishtu et al. (2002 ▶); Nihei et al. (2003 ▶).

Experimental

Crystal data

[Ni4(C12H15NO4)4]·4H2O M = 1319.90 Tetragonal, a = 18.754 (2) Å c = 15.4395 (15) Å V = 5430.3 (10) Å3 Z = 4 Mo Kα radiation μ = 1.45 mm−1 T = 298 (2) K 0.30 × 0.29 × 0.28 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.670, T max = 0.686 11110 measured reflections 2399 independent reflections 1840 reflections with I > 2σ(I) R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.066 wR(F 2) = 0.194 S = 1.08 2399 reflections 186 parameters H-atom parameters constrained Δρmax = 1.23 e Å−3 Δρmin = −0.70 e Å−3 Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808009872/lh2612sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808009872/lh2612Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ni₄(C₁₂H₁₅NO₄)₄]·4H₂O	Z = 4
M_r = 1319.90	F₀₀₀ = 2752
Tetragonal, I4₁/a	D_x = 1.614 Mg m⁻³
Hall symbol: -I 4ad	Mo Kα radiation λ = 0.71073 Å
a = 18.754 (2) Å	Cell parameters from 3768 reflections
b = 18.754 (2) Å	θ = 2.2–25.2º
c = 15.4395 (15) Å	µ = 1.45 mm⁻¹
α = 90º	T = 298 (2) K
β = 90º	Block, green
γ = 90º	0.30 × 0.29 × 0.28 mm
V = 5430.3 (10) Å³

Bruker SMART CCD area-detector diffractometer	2399 independent reflections
Radiation source: fine-focus sealed tube	1840 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.034
T = 298(2) K	θ_max = 25.0º
φ and ω scans	θ_min = 1.7º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −22→22
T_min = 0.670, T_max = 0.686	k = −22→15
11110 measured reflections	l = −9→18

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.066	H-atom parameters constrained
wR(F²) = 0.194	w = 1/[σ²(F_o²) + (0.0801P)² + 60.7787P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max = 0.001
2399 reflections	Δρ_max = 1.23 e Å⁻³
186 parameters	Δρ_min = −0.70 e Å⁻³
Primary atom site location: structure-invariant direct methods	Extinction correction: none

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.

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ni1	0.40964 (4)	0.72996 (4)	1.05945 (5)	0.0374 (3)
N1	0.3971 (4)	0.6819 (3)	0.9486 (4)	0.0575 (16)
O1	0.3327 (2)	0.7952 (2)	1.0412 (3)	0.0480 (11)
O2	0.2316 (3)	0.8868 (4)	1.0480 (5)	0.097 (2)
O3	0.4952 (2)	0.6720 (2)	1.0675 (3)	0.0435 (10)
O4	0.3704 (5)	0.5372 (4)	0.9346 (5)	0.079 (2)	0.791 (10)
H4	0.3533	0.5023	0.9103	0.119*	0.791 (10)
O4'	0.3587 (16)	0.5547 (15)	0.836 (2)	0.079 (2)	0.209 (10)
H4'	0.3562	0.5134	0.8190	0.119*	0.209 (10)
O5	0.4819 (5)	0.6865 (5)	0.7848 (5)	0.120 (3)
H5	0.4383	0.6853	0.7893	0.181*
O6	0.3380 (3)	0.6042 (3)	0.0986 (4)	0.0729 (16)
H6A	0.3733	0.5978	0.1322	0.088*
H6B	0.3472	0.5846	0.0503	0.088*
C1	0.3427 (4)	0.6889 (4)	0.9010 (5)	0.061 (2)
H1	0.3392	0.6586	0.8535	0.073*
C2	0.2852 (4)	0.7394 (4)	0.9132 (5)	0.0529 (18)
C3	0.2839 (3)	0.7900 (4)	0.9815 (4)	0.0476 (16)
C4	0.2269 (4)	0.8386 (5)	0.9823 (5)	0.067 (2)
C5	0.1712 (5)	0.8344 (6)	0.9218 (6)	0.078 (3)
H5A	0.1334	0.8664	0.9245	0.094*
C6	0.1727 (5)	0.7834 (6)	0.8595 (6)	0.078 (3)
H6	0.1354	0.7800	0.8201	0.094*
C7	0.2279 (4)	0.7377 (5)	0.8544 (6)	0.068 (2)
H7	0.2281	0.7038	0.8104	0.081*
C8	0.1829 (7)	0.9466 (7)	1.0493 (9)	0.130 (5)
H8A	0.1797	0.9668	0.9923	0.195*
H8B	0.2001	0.9820	1.0891	0.195*
H8C	0.1366	0.9306	1.0675	0.195*
C9	0.4572 (5)	0.6290 (5)	0.9262 (6)	0.075 (3)
C10	0.4932 (4)	0.6144 (4)	1.0099 (4)	0.0523 (17)
H10A	0.4691	0.5749	1.0380	0.063*
H10B	0.5418	0.5995	0.9981	0.063*
C11	0.4273 (5)	0.5654 (5)	0.8832 (6)	0.073 (2)
H11A	0.4096	0.5781	0.8262	0.088*	0.791 (10)
H11B	0.4642	0.5296	0.8762	0.088*	0.791 (10)
H11C	0.4635	0.5509	0.8420	0.088*	0.209 (10)
H11D	0.4276	0.5290	0.9279	0.088*	0.209 (10)
C12	0.5136 (5)	0.6631 (6)	0.8640 (6)	0.085 (3)
H12A	0.5359	0.7033	0.8927	0.101*
H12B	0.5504	0.6283	0.8514	0.101*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0427 (5)	0.0358 (5)	0.0337 (5)	0.0002 (3)	−0.0072 (3)	−0.0007 (3)
N1	0.080 (4)	0.046 (3)	0.046 (3)	0.015 (3)	−0.022 (3)	−0.009 (3)
O1	0.045 (3)	0.055 (3)	0.043 (2)	0.008 (2)	−0.009 (2)	−0.005 (2)
O2	0.070 (4)	0.125 (6)	0.095 (5)	0.048 (4)	−0.010 (4)	−0.019 (4)
O3	0.056 (3)	0.039 (2)	0.036 (2)	0.010 (2)	−0.008 (2)	−0.0013 (19)
O4	0.094 (6)	0.059 (4)	0.086 (5)	0.007 (4)	−0.005 (5)	−0.030 (4)
O4'	0.094 (6)	0.059 (4)	0.086 (5)	0.007 (4)	−0.005 (5)	−0.030 (4)
O5	0.111 (6)	0.189 (8)	0.061 (4)	0.038 (6)	0.005 (4)	0.011 (5)
O6	0.053 (3)	0.096 (4)	0.070 (4)	−0.001 (3)	0.011 (3)	−0.003 (3)
C1	0.079 (5)	0.056 (4)	0.048 (4)	0.006 (4)	−0.022 (4)	−0.007 (3)
C2	0.055 (4)	0.059 (4)	0.045 (4)	−0.010 (3)	−0.013 (3)	0.007 (3)
C3	0.039 (4)	0.059 (4)	0.044 (4)	−0.001 (3)	−0.002 (3)	0.014 (3)
C4	0.049 (4)	0.093 (6)	0.058 (5)	0.010 (4)	−0.001 (4)	0.002 (5)
C5	0.050 (5)	0.110 (8)	0.075 (6)	0.014 (5)	−0.004 (4)	0.010 (6)
C6	0.060 (5)	0.106 (7)	0.069 (6)	−0.008 (5)	−0.018 (4)	0.007 (5)
C7	0.064 (5)	0.081 (6)	0.058 (5)	−0.011 (4)	−0.025 (4)	0.005 (4)
C8	0.105 (9)	0.148 (12)	0.137 (12)	0.064 (9)	−0.013 (8)	−0.026 (9)
C9	0.088 (6)	0.076 (6)	0.061 (5)	0.035 (5)	−0.005 (5)	−0.016 (4)
C10	0.054 (4)	0.060 (4)	0.043 (4)	0.010 (3)	−0.001 (3)	−0.013 (3)
C11	0.081 (6)	0.076 (6)	0.061 (5)	0.016 (5)	−0.007 (5)	−0.031 (5)
C12	0.085 (7)	0.104 (8)	0.065 (6)	0.024 (6)	0.001 (5)	−0.002 (5)

Ni1—O1	1.912 (4)	C2—C7	1.408 (10)
Ni1—O3	1.941 (4)	C2—C3	1.419 (10)
Ni1—N1	1.949 (6)	C3—C4	1.405 (11)
Ni1—O3ⁱ	1.970 (4)	C4—C5	1.403 (12)
Ni1—O3ⁱⁱ	2.565 (5)	C5—C6	1.357 (13)
N1—C1	1.265 (9)	C5—H5A	0.9300
N1—C9	1.541 (10)	C6—C7	1.345 (13)
O1—C3	1.303 (8)	C6—H6	0.9300
O2—C4	1.362 (11)	C7—H7	0.9300
O2—C8	1.446 (12)	C8—H8A	0.9600
O3—C10	1.400 (8)	C8—H8B	0.9600
O3—Ni1ⁱⁱⁱ	1.970 (4)	C8—H8C	0.9600
O4—C11	1.430 (12)	C9—C11	1.475 (13)
O4—H4	0.8200	C9—C10	1.484 (11)
O4—H11D	1.0883	C9—C12	1.565 (14)
O4'—C11	1.49 (3)	C10—H10A	0.9700
O4'—H4'	0.8200	C10—H10B	0.9700
O5—C12	1.429 (12)	C11—H11A	0.9700
O5—H5	0.8200	C11—H11B	0.9700
O6—H6A	0.8500	C11—H11C	0.9698
O6—H6B	0.8499	C11—H11D	0.9699
C1—C2	1.447 (11)	C12—H12A	0.9700
C1—H1	0.9300	C12—H12B	0.9700

O1—Ni1—O3	172.2 (2)	O2—C8—H8A	109.5
O1—Ni1—N1	94.3 (2)	O2—C8—H8B	109.5
O3—Ni1—N1	84.1 (2)	H8A—C8—H8B	109.5
O1—Ni1—O3ⁱ	94.57 (19)	O2—C8—H8C	109.5
O3—Ni1—O3ⁱ	88.47 (19)	H8A—C8—H8C	109.5
N1—Ni1—O3ⁱ	166.1 (2)	H8B—C8—H8C	109.5
O1—Ni1—O3ⁱⁱ	94.23 (17)	C11—C9—C10	114.6 (8)
O3—Ni1—O3ⁱⁱ	79.80 (17)	C11—C9—N1	110.2 (8)
N1—Ni1—O3ⁱⁱ	117.2 (2)	C10—C9—N1	104.9 (6)
O3ⁱ—Ni1—O3ⁱⁱ	72.63 (17)	C11—C9—C12	108.1 (8)
C1—N1—C9	121.7 (6)	C10—C9—C12	107.5 (8)
C1—N1—Ni1	124.1 (6)	N1—C9—C12	111.6 (7)
C9—N1—Ni1	114.0 (5)	O3—C10—C9	115.0 (6)
C3—O1—Ni1	125.9 (4)	O3—C10—H10A	108.5
C4—O2—C8	119.0 (8)	C9—C10—H10A	108.5
C10—O3—Ni1	111.7 (4)	O3—C10—H10B	108.5
C10—O3—Ni1ⁱⁱⁱ	121.9 (4)	C9—C10—H10B	108.5
Ni1—O3—Ni1ⁱⁱⁱ	108.9 (2)	H10A—C10—H10B	107.5
C11—O4—H4	109.5	O4—C11—C9	109.4 (7)
H4—O4—H11D	103.2	O4—C11—O4'	65.0 (13)
C11—O4'—H4'	109.5	C9—C11—O4'	130.9 (13)
C12—O5—H5	109.5	O4—C11—H11A	109.8
H6A—O6—H6B	108.4	C9—C11—H11A	109.8
N1—C1—C2	126.4 (7)	O4'—C11—H11A	45.3
N1—C1—H1	116.8	O4—C11—H11B	109.8
C2—C1—H1	116.8	C9—C11—H11B	109.8
C7—C2—C3	118.8 (7)	O4'—C11—H11B	117.9
C7—C2—C1	118.0 (7)	H11A—C11—H11B	108.2
C3—C2—C1	123.1 (6)	O4—C11—H11C	141.6
O1—C3—C4	118.7 (7)	C9—C11—H11C	104.8
O1—C3—C2	124.4 (6)	O4'—C11—H11C	104.3
C4—C3—C2	116.9 (7)	H11A—C11—H11C	73.3
O2—C4—C5	125.6 (8)	O4—C11—H11D	49.5
O2—C4—C3	112.8 (7)	C9—C11—H11D	104.3
C5—C4—C3	121.6 (9)	O4'—C11—H11D	104.9
C6—C5—C4	119.7 (9)	H11A—C11—H11D	145.1
C6—C5—H5A	120.1	H11B—C11—H11D	65.7
C4—C5—H5A	120.1	H11C—C11—H11D	105.4
C7—C6—C5	120.5 (8)	O5—C12—C9	111.7 (8)
C7—C6—H6	119.8	O5—C12—H12A	109.3
C5—C6—H6	119.8	C9—C12—H12A	109.3
C6—C7—C2	122.3 (9)	O5—C12—H12B	109.3
C6—C7—H7	118.9	C9—C12—H12B	109.3
C2—C7—H7	118.9	H12A—C12—H12B	107.9

C1—C2—C3—C4	176.2 (7)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···N1	0.82	2.58	2.988 (9)	112
O4—H4···O6^iv	0.82	1.94	2.714 (8)	157
O4'—H4'···O6^iv	0.82	1.96	2.68 (3)	148
O6—H6A···O1^v	0.85	1.95	2.803 (7)	180
O6—H6B···O4^vi	0.85	2.04	2.892 (9)	180

Ni1—O1	1.912 (4)
Ni1—O3	1.941 (4)
Ni1—N1	1.949 (6)
Ni1—O3ⁱ	1.970 (4)
Ni1—O3ⁱⁱ	2.565 (5)

O1—Ni1—O3	172.2 (2)
O1—Ni1—N1	94.3 (2)
O3—Ni1—N1	84.1 (2)
O1—Ni1—O3ⁱ	94.57 (19)
O3—Ni1—O3ⁱ	88.47 (19)
N1—Ni1—O3ⁱ	166.1 (2)
O1—Ni1—O3ⁱⁱ	94.23 (17)
O3—Ni1—O3ⁱⁱ	79.80 (17)
N1—Ni1—O3ⁱⁱ	117.2 (2)
O3ⁱ—Ni1—O3ⁱⁱ	72.63 (17)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5⋯N1	0.82	2.58	2.988 (9)	112
O4—H4⋯O6ⁱⁱⁱ	0.82	1.94	2.714 (8)	157
O4′—H4′⋯O6ⁱⁱⁱ	0.82	1.96	2.68 (3)	148
O6—H6A⋯O1^iv	0.85	1.95	2.803 (7)	180
O6—H6B⋯O4^v	0.85	2.04	2.892 (9)	180

Symmetry codes: (iii) ; (iv) ; (v) .

1 in total

1. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

1 in total

2 in total

1. Tetra-kis(μ3-2-{[1,1-bis-(hy-droxy-meth-yl)-2-oxidoeth-yl]imino-meth-yl}-6-nitro-pheno-lato)tetra-copper(II).

Authors: Eduard N Chygorin; Yuri O Smal; Vladimir N Kokozay; Irina V Omelchenko
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2014-01-18

2. Crystal structure of tetra-kis-(μ3-2-{[1,1-bis-(hy-droxy-meth-yl)-2-oxidoeth-yl]imino-meth-yl}-6-meth-oxy-phenolato)tetra-kis-[aqua-copper(II)]: a redetermination at 200 K.

Authors: Elena A Buvaylo; Olga Yu Vassilyeva; Brian W Skelton
Journal: Acta Crystallogr E Crystallogr Commun Date: 2015-09-26

2 in total