Literature DB >> 21578107

Hexaaqua-magnesium(II) bis-{[N-(4-meth-oxy-2-oxidobenzyl-idene)glycyl-glycinato(3-)]cuprate(II)} hexa-hydrate.

Jiaxun Jiang¹, Yao Lu, Limin Yuan, Wenlong Liu.

Abstract

In the title complex, [Mg(H(2)O)(6)][Cu(C(12)H(11)N(2)O(5))](2)·6H(2)O, the Cu(II) atoms lie at the center of the square plane of triple negatively charged O,N,N',O'-tetra-dentate Schiff base ligands, which are coordinated by one phenolate O atom, one imine N atom, one deprotonated amide N atom and one carboxyl-ate O atom. The Mg(II) center, which sits on an inversion center, is coordinated by six aqua ligands and exhibits a slightly distorted octa-hedral conformation. The asymmetric unit consists of an [N-(4-meth-oxy-2-oxidobenzyl-idene)glycyl-glycinato]cuprate(II) anion, one half of an [Mg(H(2)O)(6)](2+) cation and three free water mol-ecules. The cations and anions form columns by O-H⋯O hydrogen bonds.

Entities: CellLine Chemical Disease Species

Year: 2009 PMID： 21578107 PMCID： PMC2971438 DOI： 10.1107/S1600536809040872

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

Related literature

For structures of Schiff base analogues, see: Gupta et al. (2009 ▶); Vigato et al. (2007 ▶). For structures of Schiff base heteronuclear complexes, see: Jiang et al. (2009 ▶); Sakamoto et al. (2001 ▶); Vigato & Tamburini (2008 ▶); Zhang et al. (2008 ▶).

Experimental

Crystal data

[Mg(H2O)6][Cu(C12H11N2O5)]2·6H2O M = 894.04 Triclinic, a = 7.8606 (14) Å b = 10.933 (2) Å c = 11.539 (2) Å α = 76.650 (2)° β = 76.685 (2)° γ = 80.737 (2)° V = 932.8 (3) Å3 Z = 1 Mo Kα radiation μ = 1.25 mm−1 T = 296 K 0.30 × 0.28 × 0.25 mm

Data collection

Bruker SMART APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ▶) T min = 0.696, T max = 0.736 6808 measured reflections 3262 independent reflections 2836 reflections with I > 2σ(I) R int = 0.084

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.097 S = 1.04 3262 reflections 278 parameters 18 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.76 e Å−3 Δρmin = −0.57 e Å−3 Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT-Plus (Bruker, 2003 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809040872/zq2010sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809040872/zq2010Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Mg(H₂O)₆][Cu(C₁₂H₁₁N₂O₅)]₂·6H₂O	Z = 1
M_r = 894.04	F(000) = 464
Triclinic, P1	D_x = 1.592 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.8606 (14) Å	Cell parameters from 7186 reflections
b = 10.933 (2) Å	θ = 1.0–28.3°
c = 11.539 (2) Å	µ = 1.25 mm⁻¹
α = 76.650 (2)°	T = 296 K
β = 76.685 (2)°	Block, violet
γ = 80.737 (2)°	0.30 × 0.28 × 0.25 mm
V = 932.8 (3) Å³

Bruker SMART APEX CCD diffractometer	2836 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.084
φ and ω scans	θ_max = 25.0°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −9→9
T_min = 0.696, T_max = 0.736	k = −12→12
6808 measured reflections	l = −13→13
3262 independent reflections

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.097	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ²(F_o²) + (0.0593P)²] where P = (F_o² + 2F_c²)/3
3262 reflections	(Δ/σ)_max = 0.001
278 parameters	Δρ_max = 0.76 e Å⁻³
18 restraints	Δρ_min = −0.57 e Å⁻³

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
Mg1	0.5000	1.0000	0.5000	0.0274 (3)
Cu1	0.53658 (3)	0.70272 (3)	0.98705 (2)	0.02798 (13)
C1	0.7984 (3)	0.5135 (2)	0.8983 (2)	0.0278 (5)
C2	0.9093 (3)	0.4662 (2)	0.8009 (2)	0.0318 (5)
H2	0.9106	0.5116	0.7219	0.038*
C3	1.0174 (3)	0.3528 (2)	0.8201 (3)	0.0338 (6)
C4	1.0200 (3)	0.2837 (2)	0.9381 (3)	0.0378 (6)
H4	1.0947	0.2089	0.9510	0.045*
C5	0.9110 (3)	0.3276 (2)	1.0342 (3)	0.0357 (6)
H5	0.9120	0.2808	1.1124	0.043*
C6	0.7962 (3)	0.4422 (2)	1.0192 (2)	0.0297 (5)
C7	0.6919 (3)	0.4804 (2)	1.1269 (2)	0.0311 (5)
H7	0.7045	0.4283	1.2012	0.037*
C8	0.4821 (3)	0.6142 (3)	1.2436 (2)	0.0354 (6)
H8A	0.5625	0.6201	1.2940	0.043*
H8B	0.4077	0.5488	1.2875	0.043*
C9	0.3683 (3)	0.7412 (2)	1.2172 (2)	0.0289 (5)
C10	0.2895 (3)	0.9088 (2)	1.0529 (2)	0.0319 (5)
H10A	0.3256	0.9790	1.0762	0.038*
H10B	0.1642	0.9065	1.0844	0.038*
C11	0.3290 (3)	0.9256 (2)	0.9147 (2)	0.0308 (5)
C12	1.1256 (4)	0.3610 (3)	0.6070 (3)	0.0504 (7)
H12A	1.0081	0.3695	0.5930	0.076*
H12B	1.2029	0.3108	0.5540	0.076*
H12C	1.1643	0.4432	0.5911	0.076*
N1	0.5819 (3)	0.58115 (19)	1.12892 (18)	0.0301 (4)
N2	0.3860 (3)	0.79083 (19)	1.10172 (18)	0.0315 (5)
O1	0.6989 (2)	0.62339 (15)	0.87217 (15)	0.0315 (4)
O3	0.4460 (2)	0.84413 (16)	0.86727 (15)	0.0352 (4)
O4	0.2500 (2)	1.01549 (17)	0.85495 (16)	0.0434 (5)
O2	0.2727 (2)	0.78645 (17)	1.30527 (15)	0.0370 (4)
O5	1.1276 (2)	0.30083 (17)	0.73004 (18)	0.0458 (5)
O6	0.4664 (2)	1.10040 (18)	0.63586 (15)	0.0376 (4)
H6A	0.553 (3)	1.120 (3)	0.656 (3)	0.056*
H6B	0.394 (3)	1.077 (3)	0.702 (2)	0.056*
O7	0.2365 (2)	1.0350 (2)	0.49409 (17)	0.0423 (5)
H7A	0.159 (4)	1.017 (3)	0.557 (2)	0.063*
H7B	0.194 (4)	1.096 (2)	0.448 (2)	0.063*
O8	0.4514 (3)	0.83655 (18)	0.62765 (16)	0.0423 (5)
H8C	0.393 (4)	0.785 (3)	0.616 (3)	0.063*
H8D	0.442 (5)	0.836 (3)	0.7002 (18)	0.063*
O9	0.8995 (3)	0.7896 (2)	0.68699 (18)	0.0479 (5)
H9A	0.908 (5)	0.855 (2)	0.712 (3)	0.072*
H9B	0.837 (4)	0.742 (3)	0.737 (3)	0.072*
O10	1.0000 (3)	0.9857 (2)	0.28950 (19)	0.0462 (5)
H10C	1.072 (4)	0.922 (2)	0.298 (3)	0.069*
H10D	0.934 (4)	0.984 (3)	0.246 (3)	0.069*
O11	0.2361 (3)	0.6905 (2)	0.56744 (19)	0.0483 (5)
H11A	0.145 (3)	0.724 (3)	0.602 (3)	0.072*
H11B	0.249 (4)	0.708 (3)	0.4918 (16)	0.072*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg1	0.0289 (6)	0.0339 (6)	0.0190 (5)	−0.0054 (4)	−0.0024 (4)	−0.0058 (4)
Cu1	0.03038 (19)	0.03127 (19)	0.01925 (18)	0.00204 (12)	−0.00343 (12)	−0.00437 (12)
C1	0.0263 (11)	0.0252 (11)	0.0331 (13)	−0.0035 (9)	−0.0082 (10)	−0.0054 (10)
C2	0.0310 (12)	0.0309 (12)	0.0332 (14)	−0.0027 (10)	−0.0070 (10)	−0.0061 (10)
C3	0.0276 (12)	0.0311 (12)	0.0450 (15)	−0.0024 (10)	−0.0071 (11)	−0.0135 (11)
C4	0.0351 (13)	0.0284 (12)	0.0506 (17)	0.0032 (10)	−0.0149 (12)	−0.0075 (11)
C5	0.0374 (13)	0.0292 (12)	0.0409 (15)	−0.0032 (10)	−0.0161 (12)	−0.0003 (11)
C6	0.0287 (12)	0.0280 (12)	0.0338 (13)	−0.0039 (9)	−0.0105 (10)	−0.0042 (10)
C7	0.0321 (12)	0.0335 (13)	0.0275 (13)	−0.0082 (10)	−0.0113 (10)	0.0023 (10)
C8	0.0336 (13)	0.0496 (15)	0.0211 (12)	−0.0027 (11)	−0.0070 (10)	−0.0031 (11)
C9	0.0267 (11)	0.0408 (13)	0.0230 (12)	−0.0097 (10)	−0.0048 (9)	−0.0104 (10)
C10	0.0386 (13)	0.0327 (13)	0.0226 (12)	−0.0009 (10)	−0.0006 (10)	−0.0096 (10)
C11	0.0338 (13)	0.0300 (12)	0.0263 (13)	−0.0012 (10)	−0.0015 (10)	−0.0070 (10)
C12	0.0512 (17)	0.0503 (17)	0.0473 (18)	0.0053 (13)	−0.0041 (14)	−0.0182 (14)
N1	0.0284 (10)	0.0366 (11)	0.0248 (10)	−0.0029 (8)	−0.0071 (8)	−0.0038 (8)
N2	0.0365 (11)	0.0345 (11)	0.0217 (10)	−0.0004 (9)	−0.0042 (9)	−0.0062 (8)
O1	0.0340 (9)	0.0305 (8)	0.0250 (9)	0.0041 (7)	−0.0038 (7)	−0.0033 (7)
O3	0.0448 (10)	0.0347 (9)	0.0193 (9)	0.0084 (7)	−0.0018 (7)	−0.0053 (7)
O4	0.0514 (11)	0.0391 (10)	0.0290 (10)	0.0146 (8)	−0.0035 (8)	−0.0040 (8)
O2	0.0370 (9)	0.0524 (11)	0.0215 (9)	−0.0036 (8)	−0.0024 (7)	−0.0116 (8)
O5	0.0446 (11)	0.0409 (10)	0.0486 (12)	0.0102 (8)	−0.0060 (9)	−0.0161 (9)
O6	0.0400 (10)	0.0481 (11)	0.0269 (9)	−0.0122 (8)	0.0019 (8)	−0.0154 (8)
O7	0.0303 (9)	0.0610 (12)	0.0288 (10)	−0.0006 (8)	−0.0027 (8)	−0.0019 (9)
O8	0.0591 (12)	0.0455 (11)	0.0240 (9)	−0.0185 (9)	−0.0083 (9)	−0.0016 (8)
O9	0.0487 (12)	0.0496 (12)	0.0385 (12)	−0.0082 (9)	−0.0032 (9)	0.0015 (9)
O10	0.0365 (11)	0.0617 (13)	0.0366 (11)	0.0040 (9)	−0.0026 (8)	−0.0140 (10)
O11	0.0530 (12)	0.0529 (12)	0.0393 (12)	−0.0108 (10)	−0.0093 (10)	−0.0067 (10)

Mg1—O7ⁱ	2.0591 (18)	C8—H8A	0.9700
Mg1—O7	2.0591 (18)	C8—H8B	0.9700
Mg1—O6	2.0598 (17)	C9—O2	1.266 (3)
Mg1—O6ⁱ	2.0599 (17)	C9—N2	1.302 (3)
Mg1—O8	2.0625 (18)	C10—N2	1.451 (3)
Mg1—O8ⁱ	2.0626 (18)	C10—C11	1.526 (3)
Cu1—O1	1.8797 (17)	C10—H10A	0.9700
Cu1—N2	1.892 (2)	C10—H10B	0.9700
Cu1—N1	1.920 (2)	C11—O4	1.231 (3)
Cu1—O3	1.9799 (16)	C11—O3	1.292 (3)
C1—O1	1.336 (3)	C12—O5	1.422 (4)
C1—C2	1.401 (3)	C12—H12A	0.9600
C1—C6	1.430 (3)	C12—H12B	0.9600
C2—C3	1.389 (3)	C12—H12C	0.9600
C2—H2	0.9300	O6—H6A	0.840 (17)
C3—O5	1.361 (3)	O6—H6B	0.851 (17)
C3—C4	1.400 (4)	O7—H7A	0.840 (17)
C4—C5	1.368 (4)	O7—H7B	0.833 (17)
C4—H4	0.9300	O8—H8C	0.831 (17)
C5—C6	1.422 (3)	O8—H8D	0.822 (17)
C5—H5	0.9300	O9—H9A	0.848 (18)
C6—C7	1.432 (4)	O9—H9B	0.810 (18)
C7—N1	1.288 (3)	O10—H10C	0.826 (18)
C7—H7	0.9300	O10—H10D	0.810 (17)
C8—N1	1.466 (3)	O11—H11A	0.813 (18)
C8—C9	1.533 (3)	O11—H11B	0.835 (18)

O7ⁱ—Mg1—O7	179.999 (1)	C9—C8—H8A	109.7
O7ⁱ—Mg1—O6	88.05 (8)	N1—C8—H8B	109.7
O7—Mg1—O6	91.95 (8)	C9—C8—H8B	109.7
O7ⁱ—Mg1—O6ⁱ	91.95 (8)	H8A—C8—H8B	108.2
O7—Mg1—O6ⁱ	88.05 (8)	O2—C9—N2	127.6 (2)
O6—Mg1—O6ⁱ	180.0	O2—C9—C8	119.1 (2)
O7ⁱ—Mg1—O8	90.55 (8)	N2—C9—C8	113.2 (2)
O7—Mg1—O8	89.45 (8)	N2—C10—C11	107.92 (19)
O6—Mg1—O8	90.60 (8)	N2—C10—H10A	110.1
O6ⁱ—Mg1—O8	89.40 (8)	C11—C10—H10A	110.1
O7ⁱ—Mg1—O8ⁱ	89.45 (8)	N2—C10—H10B	110.1
O7—Mg1—O8ⁱ	90.55 (8)	C11—C10—H10B	110.1
O6—Mg1—O8ⁱ	89.40 (8)	H10A—C10—H10B	108.4
O6ⁱ—Mg1—O8ⁱ	90.60 (8)	O4—C11—O3	123.8 (2)
O8—Mg1—O8ⁱ	180.000 (1)	O4—C11—C10	118.8 (2)
O1—Cu1—N2	175.66 (8)	O3—C11—C10	117.4 (2)
O1—Cu1—N1	96.90 (8)	O5—C12—H12A	109.5
N2—Cu1—N1	83.79 (9)	O5—C12—H12B	109.5
O1—Cu1—O3	95.95 (7)	H12A—C12—H12B	109.5
N2—Cu1—O3	83.51 (8)	O5—C12—H12C	109.5
N1—Cu1—O3	167.03 (8)	H12A—C12—H12C	109.5
O1—C1—C2	117.5 (2)	H12B—C12—H12C	109.5
O1—C1—C6	123.6 (2)	C7—N1—C8	121.6 (2)
C2—C1—C6	118.9 (2)	C7—N1—Cu1	124.53 (18)
C3—C2—C1	121.2 (2)	C8—N1—Cu1	113.87 (16)
C3—C2—H2	119.4	C9—N2—C10	124.0 (2)
C1—C2—H2	119.4	C9—N2—Cu1	119.48 (17)
O5—C3—C2	124.4 (2)	C10—N2—Cu1	116.46 (15)
O5—C3—C4	115.0 (2)	C1—O1—Cu1	125.02 (15)
C2—C3—C4	120.6 (2)	C11—O3—Cu1	114.46 (15)
C5—C4—C3	119.0 (2)	C3—O5—C12	118.7 (2)
C5—C4—H4	120.5	Mg1—O6—H6A	121 (2)
C3—C4—H4	120.5	Mg1—O6—H6B	118 (2)
C4—C5—C6	122.6 (2)	H6A—O6—H6B	106 (2)
C4—C5—H5	118.7	Mg1—O7—H7A	121 (2)
C6—C5—H5	118.7	Mg1—O7—H7B	124 (2)
C5—C6—C1	117.7 (2)	H7A—O7—H7B	108 (2)
C5—C6—C7	117.5 (2)	Mg1—O8—H8C	121 (2)
C1—C6—C7	124.7 (2)	Mg1—O8—H8D	120 (2)
N1—C7—C6	125.1 (2)	H8C—O8—H8D	112 (3)
N1—C7—H7	117.4	H9A—O9—H9B	113 (3)
C6—C7—H7	117.4	H10C—O10—H10D	114 (3)
N1—C8—C9	109.61 (19)	H11A—O11—H11B	114 (3)
N1—C8—H8A	109.7

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6B···O4	0.85 (2)	1.91 (2)	2.755 (3)	175 (3)
O6—H6A···O2ⁱⁱ	0.84 (2)	2.02 (2)	2.836 (2)	165 (3)
O7—H7A···O10ⁱ	0.84 (2)	1.91 (2)	2.734 (3)	165 (3)
O7—H7B···O9ⁱ	0.83 (2)	1.96 (2)	2.776 (3)	166 (3)
O8—H8C···O11	0.83 (2)	1.98 (2)	2.797 (3)	169 (3)
O8—H8D···O3	0.82 (2)	1.96 (2)	2.775 (2)	173 (3)
O9—H9A···O10ⁱⁱⁱ	0.85 (2)	1.99 (2)	2.787 (3)	157 (3)
O9—H9B···O1	0.81 (2)	2.01 (2)	2.816 (3)	174 (4)
O10—H10C···O2^iv	0.83 (2)	1.99 (2)	2.805 (3)	171 (4)
O10—H10D···O4ⁱ	0.81 (2)	2.05 (2)	2.857 (3)	176 (4)
O11—H11A···O9^v	0.81 (2)	2.05 (2)	2.857 (3)	172 (4)
O11—H11B···O2^vi	0.84 (2)	2.10 (2)	2.927 (3)	170 (4)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H6B⋯O4	0.851 (17)	1.907 (18)	2.755 (3)	175 (3)
O6—H6A⋯O2ⁱ	0.840 (17)	2.016 (18)	2.836 (2)	165 (3)
O7—H7A⋯O10ⁱⁱ	0.840 (17)	1.91 (2)	2.734 (3)	165 (3)
O7—H7B⋯O9ⁱⁱ	0.833 (17)	1.959 (18)	2.776 (3)	166 (3)
O8—H8C⋯O11	0.831 (17)	1.978 (18)	2.797 (3)	169 (3)
O8—H8D⋯O3	0.822 (17)	1.957 (17)	2.775 (2)	173 (3)
O9—H9A⋯O10ⁱⁱⁱ	0.848 (18)	1.985 (19)	2.787 (3)	157 (3)
O9—H9B⋯O1	0.810 (18)	2.009 (19)	2.816 (3)	174 (4)
O10—H10C⋯O2^iv	0.826 (18)	1.986 (19)	2.805 (3)	171 (4)
O10—H10D⋯O4ⁱⁱ	0.810 (17)	2.049 (18)	2.857 (3)	176 (4)
O11—H11A⋯O9^v	0.813 (18)	2.050 (19)	2.857 (3)	172 (4)
O11—H11B⋯O2^vi	0.835 (18)	2.101 (19)	2.927 (3)	170 (4)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .

2 in total

1. A short history of SHELX.

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

2. Hexaaqua-cobalt(II) bis-{[N-(4-meth-oxy-2-oxidobenzyl-idene)glycylglycinato]nickel(II)} hexa-hydrate.

Authors: Jiaxun Jiang; Yao Lu; Limin Yuan; Wenlong Liu
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-07-18

2 in total