Crystal structure of di-μ-hydroxido-bis{[N,N′-bis­(2,6-di­methyl­phen­yl)pentane-2,4-diiminato(1–)]zinc}

Goodner, J.A.; Powers, B.J.; Powell, D.R.; Yang, L.

doi:10.1107/S160053681401736X

metal-organic compounds

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ISSN: 2056-9890

Volume 70| Part 9| September 2014| Pages m320-m321

doi:10.1107/S160053681401736X

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Crystal structure of di-μ-hydroxido-bis{[N,N′-bis(2,6-dimethylphenyl)pentane-2,4-diiminato(1–)]zinc}

Joshua A. Goodner,^a Brandon J. Powers,^a Douglas R. Powell ^b and Lei Yang ^a ^*

^aDepartment of Chemistry, University of Central Arkansas, 201 Donaghey Avenue, Conway, AR 72035, USA, and ^bDepartment of Chemistry and Biochemistry, University of Oklahoma, Norman, OK 73019, USA
^*Correspondence e-mail: lyang@uca.edu

Edited by M. Weil, Vienna University of Technology, Austria (Received 14 July 2014; accepted 28 July 2014; online 6 August 2014)

The title compound, [Zn₂(C₂₁H₂₅N₂)₂(OH)₂], is a binuclear zinc complex formed by two bidentate β-diketiminate (nacnac) ligands and two μ-hydroxide O atoms, bridging two mononuclear units into a centrosymmetric dimeric unit. Each Zn²⁺ cation is coordinated by two N-donor atoms from the nacnac ligand and two O-donor atoms of hydroxide anions to give a distorted tetrahedral coordination environment. The Zn—O bond lengths are 1.9643 (13) and 2.0022 (14) Å, and the two Zn—N bond lengths are 1.9696 (14) and 1.9823 (14) Å. The distance between the two Zn²⁺ cations in the dimer is 2.9420 (4) Å. Although hydroxide groups are present in the complex, no classical hydrogen-bonding interations are observed because of the bulky β-diketiminate ligands.

Keywords: crystal structure; zinc; hydroxide bridging ligand; β-diketiminate ligand.

CCDC reference: 1013307

1. Related literature

For similar compounds with a [Zn₂(OH)₂] diamond core structure supported by β-diketiminate ligands, see: Cheng et al. (2001 ); Chisholm et al. (2002 ); Gondzik et al. (2014 ); Schulz et al. (2011 ). For the geometry index of four-coordinated metal cations, see: Yang et al. (2007 ).

2. Experimental

2.1. Crystal data

[Zn₂(C₂₁H₂₅N₂)₂(OH)₂]
M_r = 775.61
Monoclinic, P 2₁ /n
a = 12.8736 (4) Å
b = 8.7682 (3) Å
c = 17.4530 (5) Å
β = 105.222 (2)°
V = 1900.95 (10) Å³
Z = 2
Mo Kα radiation
μ = 1.30 mm⁻¹
T = 100 K
0.46 × 0.23 × 0.23 mm

2.2. Data collection

Bruker APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.586, T_max = 0.754
22627 measured reflections
3730 independent reflections
3576 reflections with I > 2σ(I)
R_int = 0.016

2.3. Refinement

R[F² > 2σ(F²)] = 0.029
wR(F²) = 0.079
S = 0.99
3730 reflections
230 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.06 e Å⁻³
Δρ_min = −0.25 e Å⁻³

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL2012 (Sheldrick, 2008); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXL2012 (Sheldrick, 2008).

Supporting information

CCDC reference: 1013307

Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S160053681401736X/wm5037sup1.cif

Supporting information file. DOI: 10.1107/S160053681401736X/wm5037Isup2.docx

Structure factors: contains datablock I. DOI: 10.1107/S160053681401736X/wm5037Isup3.hkl

Supporting information file. DOI: 10.1107/S160053681401736X/wm5037Isup5.cdx

checkCIF report

Synthesis and crystallization top

The complex was synthesized from the reaction of water with the [Zn(Et)(N,N'-bis(2,6-dimethylphenyl)pentane-2,4-diiminato)] complex in Et₂O. The solvent was removed under vacuum after the reaction, and a white powder was collected. Recrystallization of the white powder in saturated Et₂O at 253 K led to the formation of colorless crystals.

Refinement top

The positions of hydrogen atoms bonded to carbon atoms were initially determined by geometrical considerations and refined by using a riding model. The hydrogen atom bonded to the oxygen atom was located in a difference map, and its position was refined independently. Hydrogen atom displacement parameters were set to 1.2U_eq (1.5 for methyl) of the respective parent atom.

Related literature top

For similar compounds with a [Zn₂(OH)₂] diamond core structure supported by β-diketimine ligands, see: Cheng et al. (2001); Chisholm et al. (2002); Gondzik et al. (2014); Schulz et al. (2011). For the geometry index of four-coordinated metal cations, see: Yang et al. (2007).

Computing details top

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXL2012 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL2012 (Sheldrick, 2008).

Figures top

Fig. 1. The molecular structure of the title complex. Anisotropic displacement ellipsoids were drawn at the 30% probability level. Hydrogen atoms, except for the two oxygen donor atoms, have been omitted for clarity. [Symmetry code A: -x+2, -y+2, -z+2.]

Di-µ-hydroxido-bis{[N,N'-bis(2,6-dimethylphenyl)pentane-2,4-diiminato(1-)]zinc} top

Crystal data top

[Zn₂(C₂₁H₂₅N₂)₂(OH)₂]	F(000) = 816
M_r = 775.61	D_x = 1.355 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 12.8736 (4) Å	Cell parameters from 7335 reflections
b = 8.7682 (3) Å	θ = 2.3–28.3°
c = 17.4530 (5) Å	µ = 1.30 mm⁻¹
β = 105.222 (2)°	T = 100 K
V = 1900.95 (10) Å³	Block, colorless
Z = 2	0.46 × 0.23 × 0.23 mm

Data collection top

Bruker APEX CCD diffractometer	3576 reflections with I > 2σ(I)
ϕ and ω scans	R_int = 0.016
Absorption correction: multi-scan (SADABS; Bruker, 2007)	θ_max = 26.0°, θ_min = 1.8°
T_min = 0.586, T_max = 0.754	h = −15→15
22627 measured reflections	k = −10→10
3730 independent reflections	l = −21→21

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.029	Hydrogen site location: mixed
wR(F²) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	w = 1/[σ²(F_o²) + (0.050P)² + 1.390P] where P = (F_o² + 2F_c²)/3
3730 reflections	(Δ/σ)_max = 0.002
230 parameters	Δρ_max = 1.06 e Å⁻³
0 restraints	Δρ_min = −0.25 e Å⁻³

Crystal data top

[Zn₂(C₂₁H₂₅N₂)₂(OH)₂]	V = 1900.95 (10) Å³
M_r = 775.61	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 12.8736 (4) Å	µ = 1.30 mm⁻¹
b = 8.7682 (3) Å	T = 100 K
c = 17.4530 (5) Å	0.46 × 0.23 × 0.23 mm
β = 105.222 (2)°

Data collection top

Bruker APEX CCD diffractometer	3730 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	3576 reflections with I > 2σ(I)
T_min = 0.586, T_max = 0.754	R_int = 0.016
22627 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	0 restraints
wR(F²) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	Δρ_max = 1.06 e Å⁻³
3730 reflections	Δρ_min = −0.25 e Å⁻³
230 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Zn1	0.95859 (2)	0.92266 (2)	0.92324 (2)	0.02197 (9)
N1	1.01789 (11)	0.88907 (16)	0.83143 (8)	0.0201 (3)
N2	0.81321 (11)	0.83790 (17)	0.87559 (8)	0.0228 (3)
O1	0.96361 (10)	1.13369 (16)	0.96789 (7)	0.0259 (3)
H1	0.9667 (18)	1.209 (3)	0.9400 (15)	0.038 (7)*
C3	0.95099 (13)	0.87215 (19)	0.75919 (10)	0.0210 (3)
C4	0.83960 (13)	0.8525 (2)	0.74383 (10)	0.0223 (3)
H4	0.8007	0.8593	0.6896	0.027*
C5	0.77700 (13)	0.8241 (2)	0.79754 (10)	0.0225 (3)
C6	0.99662 (14)	0.8736 (2)	0.68752 (10)	0.0262 (4)
H6A	1.0405	0.9654	0.6889	0.039*
H6B	0.9375	0.8735	0.6389	0.039*
H6C	1.0414	0.7829	0.6884	0.039*
C7	0.66271 (13)	0.7706 (2)	0.76132 (10)	0.0267 (4)
H7A	0.6537	0.6674	0.7802	0.040*
H7B	0.6483	0.7698	0.7033	0.040*
H7C	0.6123	0.8399	0.7770	0.040*
C8	0.74730 (13)	0.7795 (2)	0.92370 (10)	0.0241 (4)
C9	0.76109 (14)	0.6264 (2)	0.94808 (10)	0.0259 (4)
C10	0.69362 (16)	0.5658 (2)	0.99114 (11)	0.0305 (4)
H10	0.7011	0.4621	1.0074	0.037*
C11	0.61560 (15)	0.6562 (3)	1.01037 (11)	0.0335 (4)
H11	0.5684	0.6135	1.0383	0.040*
C12	0.60651 (14)	0.8085 (3)	0.98893 (11)	0.0333 (4)
H12	0.5541	0.8698	1.0037	0.040*
C13	0.67270 (14)	0.8742 (2)	0.94604 (11)	0.0294 (4)
C14	0.84837 (15)	0.5304 (2)	0.92859 (12)	0.0309 (4)
H14A	0.8418	0.4248	0.9451	0.046*
H14B	0.9191	0.5707	0.9568	0.046*
H14C	0.8408	0.5334	0.8712	0.046*
C15	0.66482 (18)	1.0416 (3)	0.92477 (14)	0.0394 (5)
H15A	0.7365	1.0880	0.9413	0.059*
H15B	0.6168	1.0925	0.9520	0.059*
H15C	0.6360	1.0530	0.8672	0.059*
C16	1.13079 (13)	0.8705 (2)	0.83836 (9)	0.0205 (3)
C17	1.17176 (14)	0.7214 (2)	0.84038 (10)	0.0238 (3)
C18	1.28096 (14)	0.7028 (2)	0.84487 (11)	0.0281 (4)
H18	1.3101	0.6030	0.8463	0.034*
C19	1.34732 (14)	0.8281 (2)	0.84731 (11)	0.0290 (4)
H19	1.4212	0.8140	0.8494	0.035*
C20	1.30597 (14)	0.9738 (2)	0.84663 (10)	0.0277 (4)
H20	1.3522	1.0591	0.8488	0.033*
C21	1.19747 (14)	0.9978 (2)	0.84288 (10)	0.0228 (3)
C22	1.09984 (17)	0.5850 (2)	0.83697 (13)	0.0314 (4)
H22A	1.0652	0.5902	0.8806	0.047*
H22B	1.1429	0.4916	0.8419	0.047*
H22C	1.0446	0.5843	0.7862	0.047*
C23	1.15467 (15)	1.1575 (2)	0.84357 (11)	0.0285 (4)
H23A	1.0852	1.1661	0.8038	0.043*
H23B	1.2058	1.2301	0.8311	0.043*
H23C	1.1452	1.1803	0.8963	0.043*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.01621 (12)	0.03297 (14)	0.01712 (12)	0.00048 (7)	0.00511 (8)	−0.00413 (7)
N1	0.0170 (7)	0.0258 (7)	0.0179 (7)	0.0004 (5)	0.0054 (5)	−0.0020 (5)
N2	0.0172 (6)	0.0314 (8)	0.0201 (7)	0.0002 (6)	0.0056 (5)	0.0005 (6)
O1	0.0264 (6)	0.0323 (7)	0.0186 (6)	0.0012 (5)	0.0052 (5)	−0.0017 (5)
C3	0.0231 (8)	0.0214 (8)	0.0196 (8)	0.0010 (6)	0.0074 (6)	−0.0003 (6)
C4	0.0212 (8)	0.0272 (9)	0.0179 (8)	0.0000 (6)	0.0039 (6)	0.0015 (6)
C5	0.0190 (8)	0.0248 (8)	0.0226 (8)	0.0014 (6)	0.0037 (6)	0.0023 (7)
C6	0.0239 (8)	0.0366 (10)	0.0191 (8)	−0.0015 (7)	0.0073 (7)	−0.0002 (7)
C7	0.0204 (8)	0.0353 (10)	0.0227 (8)	−0.0037 (7)	0.0028 (7)	0.0038 (7)
C8	0.0164 (7)	0.0375 (10)	0.0177 (8)	−0.0011 (7)	0.0033 (6)	0.0005 (7)
C9	0.0215 (8)	0.0347 (9)	0.0201 (8)	−0.0020 (7)	0.0029 (7)	−0.0022 (7)
C10	0.0296 (10)	0.0388 (11)	0.0216 (9)	−0.0083 (8)	0.0040 (7)	0.0017 (7)
C11	0.0255 (9)	0.0542 (13)	0.0217 (9)	−0.0101 (9)	0.0081 (7)	−0.0004 (8)
C12	0.0205 (8)	0.0561 (13)	0.0243 (9)	0.0028 (8)	0.0078 (7)	−0.0023 (8)
C13	0.0208 (8)	0.0431 (11)	0.0242 (9)	0.0042 (8)	0.0057 (7)	0.0024 (8)
C14	0.0295 (9)	0.0311 (10)	0.0318 (10)	0.0015 (8)	0.0077 (8)	−0.0006 (8)
C15	0.0364 (11)	0.0441 (12)	0.0418 (12)	0.0127 (9)	0.0177 (9)	0.0040 (10)
C16	0.0187 (8)	0.0280 (9)	0.0157 (7)	0.0011 (6)	0.0062 (6)	−0.0011 (6)
C17	0.0251 (8)	0.0276 (9)	0.0204 (8)	0.0023 (7)	0.0087 (6)	−0.0009 (7)
C18	0.0274 (9)	0.0340 (10)	0.0248 (9)	0.0089 (7)	0.0102 (7)	0.0017 (7)
C19	0.0185 (8)	0.0461 (11)	0.0235 (9)	0.0032 (7)	0.0071 (7)	−0.0007 (8)
C20	0.0220 (8)	0.0392 (10)	0.0226 (9)	−0.0064 (7)	0.0072 (7)	−0.0025 (8)
C21	0.0243 (8)	0.0281 (9)	0.0167 (8)	−0.0002 (7)	0.0066 (6)	−0.0006 (6)
C22	0.0341 (10)	0.0249 (9)	0.0386 (11)	0.0014 (7)	0.0154 (9)	−0.0015 (7)
C23	0.0315 (9)	0.0258 (9)	0.0296 (9)	−0.0016 (7)	0.0104 (7)	−0.0007 (7)

Geometric parameters (Å, º) top

Zn1—O1ⁱ	1.9643 (13)	C11—H11	0.9500
Zn1—N1	1.9696 (14)	C12—C13	1.397 (3)
Zn1—N2	1.9823 (14)	C12—H12	0.9500
Zn1—O1	2.0022 (14)	C13—C15	1.511 (3)
N1—C3	1.335 (2)	C14—H14A	0.9800
N1—C16	1.436 (2)	C14—H14B	0.9800
N2—C5	1.324 (2)	C14—H14C	0.9800
N2—C8	1.436 (2)	C15—H15A	0.9800
O1—H1	0.83 (3)	C15—H15B	0.9800
C3—C4	1.398 (2)	C15—H15C	0.9800
C3—C6	1.515 (2)	C16—C21	1.398 (2)
C4—C5	1.410 (2)	C16—C17	1.407 (2)
C4—H4	0.9500	C17—C18	1.397 (2)
C5—C7	1.515 (2)	C17—C22	1.504 (3)
C6—H6A	0.9800	C18—C19	1.386 (3)
C6—H6B	0.9800	C18—H18	0.9500
C6—H6C	0.9800	C19—C20	1.383 (3)
C7—H7A	0.9800	C19—H19	0.9500
C7—H7B	0.9800	C20—C21	1.397 (2)
C7—H7C	0.9800	C20—H20	0.9500
C8—C13	1.400 (3)	C21—C23	1.506 (3)
C8—C9	1.406 (3)	C22—H22A	0.9800
C9—C10	1.394 (3)	C22—H22B	0.9800
C9—C14	1.512 (3)	C22—H22C	0.9800
C10—C11	1.388 (3)	C23—H23A	0.9800
C10—H10	0.9500	C23—H23B	0.9800
C11—C12	1.383 (3)	C23—H23C	0.9800

O1ⁱ—Zn1—N1	122.77 (6)	C11—C12—C13	121.50 (18)
O1ⁱ—Zn1—N2	119.80 (6)	C11—C12—H12	119.2
N1—Zn1—N2	97.33 (6)	C13—C12—H12	119.2
O1ⁱ—Zn1—O1	84.25 (6)	C12—C13—C8	117.67 (19)
N1—Zn1—O1	118.36 (6)	C12—C13—C15	121.39 (18)
N2—Zn1—O1	116.11 (6)	C8—C13—C15	120.94 (17)
C3—N1—C16	117.04 (14)	C9—C14—H14A	109.5
C3—N1—Zn1	119.54 (11)	C9—C14—H14B	109.5
C16—N1—Zn1	123.26 (11)	H14A—C14—H14B	109.5
C5—N2—C8	117.81 (14)	C9—C14—H14C	109.5
C5—N2—Zn1	120.29 (11)	H14A—C14—H14C	109.5
C8—N2—Zn1	121.74 (11)	H14B—C14—H14C	109.5
Zn1ⁱ—O1—Zn1	95.75 (6)	C13—C15—H15A	109.5
Zn1ⁱ—O1—H1	132.7 (17)	C13—C15—H15B	109.5
Zn1—O1—H1	120.8 (17)	H15A—C15—H15B	109.5
N1—C3—C4	124.70 (15)	C13—C15—H15C	109.5
N1—C3—C6	118.99 (15)	H15A—C15—H15C	109.5
C4—C3—C6	116.30 (15)	H15B—C15—H15C	109.5
C3—C4—C5	129.11 (15)	C21—C16—C17	121.33 (15)
C3—C4—H4	115.4	C21—C16—N1	120.49 (15)
C5—C4—H4	115.4	C17—C16—N1	118.17 (15)
N2—C5—C4	124.02 (15)	C18—C17—C16	118.38 (16)
N2—C5—C7	119.89 (15)	C18—C17—C22	120.61 (17)
C4—C5—C7	116.07 (15)	C16—C17—C22	121.01 (15)
C3—C6—H6A	109.5	C19—C18—C17	120.81 (17)
C3—C6—H6B	109.5	C19—C18—H18	119.6
H6A—C6—H6B	109.5	C17—C18—H18	119.6
C3—C6—H6C	109.5	C20—C19—C18	119.98 (16)
H6A—C6—H6C	109.5	C20—C19—H19	120.0
H6B—C6—H6C	109.5	C18—C19—H19	120.0
C5—C7—H7A	109.5	C19—C20—C21	121.15 (18)
C5—C7—H7B	109.5	C19—C20—H20	119.4
H7A—C7—H7B	109.5	C21—C20—H20	119.4
C5—C7—H7C	109.5	C20—C21—C16	118.32 (17)
H7A—C7—H7C	109.5	C20—C21—C23	120.18 (17)
H7B—C7—H7C	109.5	C16—C21—C23	121.50 (16)
C13—C8—C9	121.56 (16)	C17—C22—H22A	109.5
C13—C8—N2	120.37 (17)	C17—C22—H22B	109.5
C9—C8—N2	118.06 (15)	H22A—C22—H22B	109.5
C10—C9—C8	118.67 (17)	C17—C22—H22C	109.5
C10—C9—C14	120.93 (18)	H22A—C22—H22C	109.5
C8—C9—C14	120.39 (16)	H22B—C22—H22C	109.5
C11—C10—C9	120.38 (19)	C21—C23—H23A	109.5
C11—C10—H10	119.8	C21—C23—H23B	109.5
C9—C10—H10	119.8	H23A—C23—H23B	109.5
C12—C11—C10	120.06 (17)	C21—C23—H23C	109.5
C12—C11—H11	120.0	H23A—C23—H23C	109.5
C10—C11—H11	120.0	H23B—C23—H23C	109.5

C16—N1—C3—C4	165.14 (16)	C11—C12—C13—C8	1.5 (3)
Zn1—N1—C3—C4	−10.5 (2)	C11—C12—C13—C15	−178.18 (19)
C16—N1—C3—C6	−14.8 (2)	C9—C8—C13—C12	−4.5 (3)
Zn1—N1—C3—C6	169.60 (12)	N2—C8—C13—C12	176.31 (16)
N1—C3—C4—C5	−10.3 (3)	C9—C8—C13—C15	175.20 (17)
C6—C3—C4—C5	169.62 (18)	N2—C8—C13—C15	−4.0 (3)
C8—N2—C5—C4	−169.09 (16)	C3—N1—C16—C21	100.95 (19)
Zn1—N2—C5—C4	6.4 (2)	Zn1—N1—C16—C21	−83.61 (18)
C8—N2—C5—C7	9.1 (2)	C3—N1—C16—C17	−79.0 (2)
Zn1—N2—C5—C7	−175.34 (12)	Zn1—N1—C16—C17	96.43 (16)
C3—C4—C5—N2	12.6 (3)	C21—C16—C17—C18	−1.7 (2)
C3—C4—C5—C7	−165.64 (18)	N1—C16—C17—C18	178.23 (15)
C5—N2—C8—C13	−91.7 (2)	C21—C16—C17—C22	178.88 (17)
Zn1—N2—C8—C13	92.82 (17)	N1—C16—C17—C22	−1.2 (2)
C5—N2—C8—C9	89.03 (19)	C16—C17—C18—C19	0.0 (3)
Zn1—N2—C8—C9	−86.44 (18)	C22—C17—C18—C19	179.42 (17)
C13—C8—C9—C10	4.2 (3)	C17—C18—C19—C20	1.1 (3)
N2—C8—C9—C10	−176.53 (15)	C18—C19—C20—C21	−0.5 (3)
C13—C8—C9—C14	−175.09 (16)	C19—C20—C21—C16	−1.1 (3)
N2—C8—C9—C14	4.2 (2)	C19—C20—C21—C23	179.00 (16)
C8—C9—C10—C11	−0.9 (3)	C17—C16—C21—C20	2.3 (2)
C14—C9—C10—C11	178.37 (17)	N1—C16—C21—C20	−177.69 (15)
C9—C10—C11—C12	−2.0 (3)	C17—C16—C21—C23	−177.87 (16)
C10—C11—C12—C13	1.7 (3)	N1—C16—C21—C23	2.2 (2)

Symmetry code: (i) −x+2, −y+2, −z+2.

Experimental details

Crystal data
Chemical formula	[Zn₂(C₂₁H₂₅N₂)₂(OH)₂]
M_r	775.61
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	100
a, b, c (Å)	12.8736 (4), 8.7682 (3), 17.4530 (5)
β (°)	105.222 (2)
V (Å³)	1900.95 (10)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.30
Crystal size (mm)	0.46 × 0.23 × 0.23

Data collection
Diffractometer	Bruker APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.586, 0.754
No. of measured, independent and observed [I > 2σ(I)] reflections	22627, 3730, 3576
R_int	0.016
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.079, 0.99
No. of reflections	3730
No. of parameters	230
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.06, −0.25

Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXTL (Sheldrick, 2008), SHELXL2012 (Sheldrick, 2008).

Acknowledgements

The authors thank the National Science Foundation (grant No. CHE-0130835) and the University of Oklahoma for funds to purchase of the X-ray instrument and computers.

References

Bruker (2007). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Cheng, M., Moore, D., Reczek, J. J., Chamberlain, B. M., Lobkovsky, E. B. & Coates, G. W. (2001). J. Am. Chem. Soc. 123, 8738–8749. Web of Science CSD CrossRef PubMed CAS Google Scholar
Chisholm, M. H., Gallucci, J. & Phomphrai, K. (2002). Inorg. Chem. 41, 2785–2794. Web of Science CSD CrossRef PubMed CAS Google Scholar
Gondzik, S., Schulz, S. & Wölper, C. (2014). Chem. Commun. 50, 1189–1191. Web of Science CSD CrossRef CAS Google Scholar
Schulz, S., Spielmann, J., Bläser, D. & Wölper, C. (2011). Chem. Commun. 47, 2676–2678. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Yang, L., Wang, Z., Powell, D. R. & Houser, R. P. (2007). Dalton Trans. pp. 4439–4441. Google Scholar

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Volume 70| Part 9| September 2014| Pages m320-m321

doi:10.1107/S160053681401736X

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Crystal structure of di-μ-hydroxido-bis­{[N,N′-bis­­(2,6-di­methyl­phen­yl)pentane-2,4-diiminato(1–)]zinc}

1. Related literature

2. Experimental

2.1. Crystal data

2.2. Data collection

2.3. Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Crystal structure of di-μ-hydroxido-bis{[N,N′-bis(2,6-dimethylphenyl)pentane-2,4-diiminato(1–)]zinc}