Tetra­aqua­bis(4-carboxy­phenoxy­acetato)­magnesium(II)

Gao, S.; Li, J.-R.; Huo, L.-H.; Liu, J.-W.; Gu, C.-S.

doi:10.1107/S1600536803028757

Tetraaquabis(4-carboxyphenoxyacetato)magnesium(II)

S. Gao, J.-R. Li, L.-H. Huo, J.-W. Liu and C.-S. Gu

The title complex, [Mg(C₉H₇O₅)₂(H₂O)₄], is a neutral mononuclear molecule consisting of an Mg^II ion, two 4-carboxyphenoxyacetate ligands and four coordinated water molecules. The Mg^II atom lies on an inversion center and is six-coordinate, with two O atoms of two trans 4-CPOAH^- ligands and four water molecules. A supramolecular network structure is formed by intermolecular hydrogen bonds.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803028757/cf6309sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536803028757/cf6309Isup2.hkl Contains datablock I

CCDC reference: 223314

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
R factor = 0.054
wR factor = 0.139
Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.94

Alert level C
REFLT03_ALERT_3_C  Reflection count < 95% complete
           From the CIF: _diffrn_reflns_theta_max           27.48
           From the CIF: _diffrn_reflns_theta_full           0.00
           From the CIF: _reflns_number_total               2244
           TEST2: Reflns within _diffrn_reflns_theta_max
           Count of symmetry unique reflns         2383
           Completeness (_total/calc)             94.17%
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low ....       0.94
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Mg1    -   O2W      =       5.06 su
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       2.13
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          4

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97.

Tetraaquabis(4-carboxyphenoxyacetato)magnesium(II) top

Crystal data top

[Mg(C₉H₇O₅)₂(H₂O)₄]	Z = 1
M_r = 486.67	F(000) = 254
Triclinic, P1	D_x = 1.562 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 4.922 (1) Å	Cell parameters from 4564 reflections
b = 5.755 (1) Å	θ = 3.3–27.6°
c = 18.432 (4) Å	µ = 0.16 mm⁻¹
α = 94.13 (3)°	T = 293 K
β = 91.95 (3)°	Prism, colorless
γ = 96.13 (3)°	0.30 × 0.28 × 0.26 mm
V = 517.3 (2) Å³

Data collection top

Rigaku R-AXIS RAPID diffractometer	2244 independent reflections
Radiation source: fine-focus sealed tube	1609 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.034
Detector resolution: 10.000 pixels mm^-1	θ_max = 27.5°, θ_min = 3.3°
ω scans	h = −6→6
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −7→7
T_min = 0.953, T_max = 0.959	l = −23→23
4618 measured reflections

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)] = 0.054	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.139	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0717P)² + 0.1746P] where P = (F_o² + 2F_c²)/3
2244 reflections	(Δ/σ)_max < 0.001
167 parameters	Δρ_max = 0.34 e Å⁻³
4 restraints	Δρ_min = −0.24 e Å⁻³

Special details top

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.

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

	x	y	z	U_iso*/U_eq
Mg1	0.5000	0.5000	0.0000	0.0256 (3)
O1W	0.7673 (4)	0.3553 (3)	0.07109 (10)	0.0344 (4)
H1WB	0.879 (7)	0.440 (6)	0.0971 (18)	0.081 (13)*
H1WA	0.715 (8)	0.246 (5)	0.0960 (19)	0.079 (13)*
O2W	0.7674 (4)	0.7976 (3)	0.00269 (10)	0.0363 (4)
H2WB	0.740 (8)	0.862 (6)	0.0430 (13)	0.077 (12)*
H2WA	0.929 (4)	0.783 (7)	−0.003 (2)	0.077 (12)*
O1	0.2970 (3)	0.6407 (3)	0.08755 (8)	0.0341 (4)
O2	0.5835 (3)	0.9494 (3)	0.13240 (9)	0.0362 (4)
O3	0.0146 (3)	0.6346 (3)	0.20545 (9)	0.0364 (4)
O4	−0.8875 (4)	0.3524 (4)	0.42565 (10)	0.0498 (5)
O5	−0.7329 (4)	0.7041 (4)	0.47962 (10)	0.0514 (6)
H12	−0.8582	0.6703	0.5065	0.077*
C1	0.3743 (5)	0.8047 (4)	0.13468 (12)	0.0285 (5)
C2	0.2055 (5)	0.8371 (4)	0.20142 (12)	0.0320 (5)
H2A	0.3247	0.8601	0.2449	0.038*
H2B	0.1088	0.9746	0.1983	0.038*
C3	−0.1532 (5)	0.6267 (5)	0.26359 (12)	0.0316 (5)
C4	−0.3264 (5)	0.4205 (5)	0.26426 (13)	0.0394 (6)
H4A	−0.3197	0.3008	0.2279	0.047*
C5	−0.5090 (5)	0.3937 (5)	0.31916 (14)	0.0406 (6)
H5A	−0.6245	0.2550	0.3197	0.049*
C6	−0.5217 (5)	0.5718 (5)	0.37346 (12)	0.0335 (6)
C7	−0.3443 (5)	0.7764 (5)	0.37298 (13)	0.0363 (6)
H7A	−0.3493	0.8951	0.4097	0.044*
C8	−0.1598 (5)	0.8053 (5)	0.31825 (13)	0.0350 (6)
H8A	−0.0418	0.9427	0.3181	0.042*
C9	−0.7268 (5)	0.5403 (5)	0.43020 (13)	0.0370 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg1	0.0229 (5)	0.0286 (6)	0.0244 (5)	−0.0009 (4)	0.0065 (4)	−0.0013 (4)
O1W	0.0332 (9)	0.0356 (11)	0.0329 (10)	−0.0036 (8)	0.0003 (7)	0.0035 (8)
O2W	0.0292 (9)	0.0374 (11)	0.0411 (11)	−0.0021 (8)	0.0112 (8)	−0.0026 (8)
O1	0.0316 (9)	0.0405 (10)	0.0283 (9)	−0.0017 (7)	0.0072 (7)	−0.0059 (7)
O2	0.0359 (9)	0.0374 (10)	0.0327 (9)	−0.0076 (8)	0.0070 (7)	−0.0004 (7)
O3	0.0343 (9)	0.0418 (11)	0.0302 (9)	−0.0078 (8)	0.0134 (7)	−0.0046 (7)
O4	0.0464 (11)	0.0569 (13)	0.0432 (11)	−0.0103 (10)	0.0197 (9)	−0.0003 (9)
O5	0.0486 (11)	0.0645 (14)	0.0383 (10)	−0.0057 (10)	0.0231 (9)	−0.0077 (9)
C1	0.0304 (11)	0.0325 (13)	0.0233 (11)	0.0033 (10)	0.0028 (9)	0.0048 (9)
C2	0.0314 (12)	0.0355 (14)	0.0275 (12)	−0.0023 (10)	0.0060 (9)	−0.0025 (9)
C3	0.0310 (12)	0.0412 (15)	0.0226 (11)	0.0034 (10)	0.0056 (9)	0.0002 (9)
C4	0.0431 (14)	0.0421 (16)	0.0302 (13)	−0.0058 (12)	0.0127 (11)	−0.0066 (10)
C5	0.0412 (14)	0.0425 (16)	0.0350 (13)	−0.0095 (12)	0.0113 (11)	−0.0013 (11)
C6	0.0309 (12)	0.0421 (15)	0.0264 (12)	−0.0003 (11)	0.0060 (9)	0.0003 (10)
C7	0.0353 (13)	0.0454 (16)	0.0268 (12)	0.0009 (11)	0.0084 (10)	−0.0052 (10)
C8	0.0333 (13)	0.0381 (15)	0.0320 (12)	−0.0033 (11)	0.0093 (10)	−0.0008 (10)
C9	0.0346 (13)	0.0505 (17)	0.0258 (12)	0.0019 (12)	0.0078 (10)	0.0025 (11)

Geometric parameters (Å, º) top

Mg1—O2Wⁱ	2.042 (2)	O5—C9	1.266 (3)
Mg1—O2W	2.042 (2)	O5—H12	0.820
Mg1—O1	2.086 (2)	C1—C2	1.519 (3)
Mg1—O1ⁱ	2.086 (2)	C2—H2A	0.970
Mg1—O1Wⁱ	2.101 (2)	C2—H2B	0.970
Mg1—O1W	2.101 (2)	C3—C4	1.386 (4)
Mg1—H2WB	2.35 (3)	C3—C8	1.390 (3)
O1W—H1WB	0.81 (2)	C4—C5	1.382 (3)
O1W—H1WA	0.83 (2)	C4—H4A	0.930
O2W—H2WB	0.83 (2)	C5—C6	1.388 (4)
O2W—H2WA	0.82 (2)	C5—H5A	0.930
O1—C1	1.254 (3)	C6—C7	1.390 (4)
O2—C1	1.257 (3)	C6—C9	1.485 (3)
O3—C3	1.376 (3)	C7—C8	1.387 (3)
O3—C2	1.424 (3)	C7—H7A	0.930
O4—C9	1.266 (3)	C8—H8A	0.930

O2Wⁱ—Mg1—O2W	180.0	O1—C1—O2	125.9 (2)
O2Wⁱ—Mg1—O1	89.31 (7)	O1—C1—C2	118.8 (2)
O2W—Mg1—O1	90.69 (7)	O2—C1—C2	115.3 (2)
O2Wⁱ—Mg1—O1ⁱ	90.69 (7)	O3—C2—C1	109.25 (18)
O2W—Mg1—O1ⁱ	89.31 (7)	O3—C2—H2A	109.8
O1—Mg1—O1ⁱ	180.0	C1—C2—H2A	109.8
O2Wⁱ—Mg1—O1Wⁱ	89.65 (8)	O3—C2—H2B	109.8
O2W—Mg1—O1Wⁱ	90.35 (8)	C1—C2—H2B	109.8
O1—Mg1—O1Wⁱ	88.90 (7)	H2A—C2—H2B	108.3
O1ⁱ—Mg1—O1Wⁱ	91.10 (7)	O3—C3—C4	114.3 (2)
O2Wⁱ—Mg1—O1W	90.35 (8)	O3—C3—C8	125.2 (2)
O2W—Mg1—O1W	89.65 (8)	C4—C3—C8	120.4 (2)
O1—Mg1—O1W	91.10 (7)	C5—C4—C3	119.7 (2)
O1ⁱ—Mg1—O1W	88.90 (7)	C5—C4—H4A	120.1
O1Wⁱ—Mg1—O1W	180.0	C3—C4—H4A	120.1
O2Wⁱ—Mg1—H2WB	159.8 (6)	C4—C5—C6	120.6 (3)
O2W—Mg1—H2WB	20.2 (6)	C4—C5—H5A	119.7
O1—Mg1—H2WB	71.2 (6)	C6—C5—H5A	119.7
O1ⁱ—Mg1—H2WB	108.8 (6)	C5—C6—C7	119.2 (2)
O1Wⁱ—Mg1—H2WB	95.0 (9)	C5—C6—C9	119.2 (2)
O1W—Mg1—H2WB	85.0 (9)	C7—C6—C9	121.6 (2)
Mg1—O1W—H1WB	120 (3)	C8—C7—C6	120.7 (2)
Mg1—O1W—H1WA	122 (3)	C8—C7—H7A	119.6
H1WB—O1W—H1WA	105 (4)	C6—C7—H7A	119.6
Mg1—O2W—H2WB	102 (3)	C7—C8—C3	119.3 (2)
Mg1—O2W—H2WA	118 (3)	C7—C8—H8A	120.4
H2WB—O2W—H2WA	113 (4)	C3—C8—H8A	120.4
C1—O1—Mg1	130.59 (15)	O4—C9—O5	123.9 (2)
C3—O3—C2	118.3 (2)	O4—C9—C6	117.9 (2)
C9—O5—H12	109.5	O5—C9—C6	118.1 (2)

O2Wⁱ—Mg1—O1—C1	160.1 (2)	C3—C4—C5—C6	0.3 (4)
O2W—Mg1—O1—C1	−19.9 (2)	C4—C5—C6—C7	−1.3 (4)
O1Wⁱ—Mg1—O1—C1	−110.3 (2)	C4—C5—C6—C9	177.9 (3)
O1W—Mg1—O1—C1	69.7 (2)	C5—C6—C7—C8	1.3 (4)
Mg1—O1—C1—O2	12.5 (4)	C9—C6—C7—C8	−178.0 (2)
Mg1—O1—C1—C2	−167.42 (16)	C6—C7—C8—C3	−0.2 (4)
C3—O3—C2—C1	178.2 (2)	O3—C3—C8—C7	178.5 (2)
O1—C1—C2—O3	13.0 (3)	C4—C3—C8—C7	−0.9 (4)
O2—C1—C2—O3	−166.9 (2)	C5—C6—C9—O4	−1.6 (4)
C2—O3—C3—C4	−178.1 (2)	C7—C6—C9—O4	177.7 (2)
C2—O3—C3—C8	2.5 (4)	C5—C6—C9—O5	179.3 (3)
O3—C3—C4—C5	−178.6 (2)	C7—C6—C9—O5	−1.4 (4)
C8—C3—C4—C5	0.8 (4)

Symmetry code: (i) −x+1, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WB···O3ⁱⁱ	0.81 (2)	2.26 (2)	3.001 (3)	151 (4)
O1W—H1WB···O1ⁱⁱ	0.81 (2)	2.27 (3)	2.924 (3)	138 (4)
O1W—H1WA···O2ⁱⁱⁱ	0.83 (2)	1.94 (2)	2.748 (3)	166 (4)
O2W—H2WB···O2	0.83 (2)	1.90 (2)	2.704 (2)	164 (4)
O2W—H2WA···O1W^iv	0.82 (2)	2.17 (3)	2.888 (3)	147 (4)
O5—H12···O4^v	0.82	1.80	2.612 (2)	169

Symmetry codes: (ii) x+1, y, z; (iii) x, y−1, z; (iv) −x+2, −y+1, −z; (v) −x−2, −y+1, −z+1.

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

Tetra­aqua­bis(4-carboxy­phenoxy­acetato)­magnesium(II)

Supporting information

Key indicators

checkCIF/PLATON results

Tetraaquabis(4-carboxyphenoxyacetato)magnesium(II)