Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807027687/hb2431sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807027687/hb2431Isup2.hkl |
CCDC reference: 654729
Key indicators
- Single-crystal X-ray study
- T = 291 K
- Mean (C-C) = 0.005 Å
- R factor = 0.064
- wR factor = 0.129
- Data-to-parameter ratio = 15.2
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 500 Deg. PLAT340_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 5
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 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 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
1 mmol of magnesium perchlorate was added to a solution of quinaldine acid (2 mmol) in 10 ml of 95% methanol. The mixture was stirred for 3 h at refluxing temperature and cooled. Clear blocks of (I) were obtained after one week as the solvents slowly evaporated.
The H atoms were placed geometrically (C—H = 0.93—0.96 Å, O—H = 0.85–0.96 Å) and refined as riding with Uiso(H) = 1.2Ueq(carrier) or 1.5Ueq(methyl C).
As part of our ongoing studies of the coordination chemistry of magnesium(II) (Tai et al., 2007), we now report the synthesis and structure of the title compound, (I), (Fig. 1).
In the molecule of (I), The Mg(II) center (site symmetry 1) is six-coordinate with two O donor of H2O, four O, N donor of two quinaldine anions (Table 1). Intermolecular O—H···O hydrogen bonds help to consolidate the crystal packing (Table 2).
For a related structure, see: Tai et al. (2007).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. The molecular structure of (I) showing 30% displacement ellipsoids (arbitrary spheres for the H atoms). |
[Mg(C10H6NO2)2(H2O)2]·2H2O·2CH4O | Z = 1 |
Mr = 504.77 | F(000) = 266 |
Triclinic, P1 | Dx = 1.344 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.129 (3) Å | Cell parameters from 318 reflections |
b = 9.038 (3) Å | θ = 2.4–19.2° |
c = 10.846 (4) Å | µ = 0.13 mm−1 |
α = 75.677 (5)° | T = 291 K |
β = 74.138 (5)° | Block, colourless |
γ = 70.160 (5)° | 0.30 × 0.26 × 0.24 mm |
V = 623.0 (4) Å3 |
Bruker SMART APEX CCD area-detector diffractometer | 2445 independent reflections |
Radiation source: sealed tube | 1640 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.062 |
ω scans | θmax = 26.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −8→8 |
Tmin = 0.96, Tmax = 0.97 | k = −10→11 |
5796 measured reflections | l = −13→13 |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.129 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.04P)2 + 0.11P] where P = (Fo2 + 2Fc2)/3 |
2445 reflections | (Δ/σ)max < 0.001 |
161 parameters | Δρmax = 0.22 e Å−3 |
0 restraints | Δρmin = −0.23 e Å−3 |
[Mg(C10H6NO2)2(H2O)2]·2H2O·2CH4O | γ = 70.160 (5)° |
Mr = 504.77 | V = 623.0 (4) Å3 |
Triclinic, P1 | Z = 1 |
a = 7.129 (3) Å | Mo Kα radiation |
b = 9.038 (3) Å | µ = 0.13 mm−1 |
c = 10.846 (4) Å | T = 291 K |
α = 75.677 (5)° | 0.30 × 0.26 × 0.24 mm |
β = 74.138 (5)° |
Bruker SMART APEX CCD area-detector diffractometer | 2445 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 1640 reflections with I > 2σ(I) |
Tmin = 0.96, Tmax = 0.97 | Rint = 0.062 |
5796 measured reflections |
R[F2 > 2σ(F2)] = 0.064 | 0 restraints |
wR(F2) = 0.129 | H-atom parameters constrained |
S = 1.09 | Δρmax = 0.22 e Å−3 |
2445 reflections | Δρmin = −0.23 e Å−3 |
161 parameters |
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 | Uiso*/Ueq | ||
C1 | 0.5400 (4) | 0.3602 (3) | 0.8444 (3) | 0.0447 (6) | |
C2 | 0.3913 (5) | 0.3680 (4) | 0.7786 (3) | 0.0512 (7) | |
H2 | 0.3326 | 0.2854 | 0.7970 | 0.061* | |
C3 | 0.3347 (4) | 0.4995 (4) | 0.6868 (3) | 0.0482 (7) | |
H3 | 0.2357 | 0.5062 | 0.6432 | 0.058* | |
C4 | 0.4245 (4) | 0.6259 (3) | 0.6570 (3) | 0.0440 (6) | |
H4 | 0.3873 | 0.7135 | 0.5931 | 0.053* | |
C5 | 0.5670 (4) | 0.6163 (4) | 0.7241 (3) | 0.0470 (7) | |
H5 | 0.6230 | 0.7001 | 0.7077 | 0.056* | |
C6 | 0.6292 (4) | 0.4820 (4) | 0.8172 (3) | 0.0500 (7) | |
C7 | 0.7774 (4) | 0.4703 (3) | 0.8849 (3) | 0.0456 (6) | |
H7 | 0.8385 | 0.5512 | 0.8680 | 0.055* | |
C8 | 0.8292 (4) | 0.3384 (4) | 0.9753 (3) | 0.0482 (7) | |
H8 | 0.9266 | 0.3279 | 1.0215 | 0.058* | |
C9 | 0.7375 (4) | 0.2212 (4) | 0.9980 (3) | 0.0472 (7) | |
C10 | 0.7840 (5) | 0.0708 (3) | 1.0976 (3) | 0.0484 (7) | |
C11 | 0.9682 (5) | 0.7515 (4) | 0.4226 (3) | 0.0585 (9) | |
H11A | 1.0915 | 0.7807 | 0.4051 | 0.088* | |
H11B | 0.9838 | 0.6788 | 0.3667 | 0.088* | |
H11C | 0.9400 | 0.7010 | 0.5117 | 0.088* | |
Mg1 | 0.5000 | 0.0000 | 1.0000 | 0.0406 (3) | |
N1 | 0.5957 (4) | 0.2269 (3) | 0.9335 (2) | 0.0507 (6) | |
O1 | 0.7001 (3) | −0.0334 (2) | 1.10861 (17) | 0.0459 (5) | |
O2 | 0.9058 (3) | 0.0623 (2) | 1.16859 (17) | 0.0451 (5) | |
O3 | 0.7270 (3) | −0.0998 (2) | 0.85156 (18) | 0.0528 (5) | |
H3A | 0.8505 | −0.0769 | 0.8482 | 0.063* | |
H3B | 0.6846 | −0.0546 | 0.7702 | 0.063* | |
O4 | 0.6256 (3) | 0.0316 (2) | 0.61644 (17) | 0.0432 (5) | |
H4A | 0.7206 | −0.0108 | 0.5575 | 0.052* | |
H4B | 0.5156 | 0.0148 | 0.6157 | 0.052* | |
O5 | 0.8078 (3) | 0.8873 (2) | 0.39970 (17) | 0.0445 (5) | |
H5C | 0.8589 | 0.9636 | 0.3320 | 0.053* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0443 (15) | 0.0422 (16) | 0.0441 (14) | 0.0006 (13) | −0.0151 (12) | −0.0135 (11) |
C2 | 0.0641 (19) | 0.0474 (18) | 0.0474 (15) | −0.0157 (15) | −0.0168 (14) | −0.0127 (13) |
C3 | 0.0423 (15) | 0.0540 (18) | 0.0483 (14) | −0.0087 (14) | −0.0147 (12) | −0.0101 (13) |
C4 | 0.0476 (15) | 0.0444 (16) | 0.0441 (13) | −0.0105 (13) | −0.0143 (12) | −0.0135 (12) |
C5 | 0.0383 (14) | 0.0620 (19) | 0.0444 (14) | −0.0137 (14) | −0.0107 (12) | −0.0146 (13) |
C6 | 0.0438 (15) | 0.0514 (19) | 0.0509 (15) | −0.0001 (14) | −0.0141 (13) | −0.0164 (13) |
C7 | 0.0433 (15) | 0.0423 (16) | 0.0506 (15) | −0.0120 (13) | −0.0018 (12) | −0.0165 (12) |
C8 | 0.0446 (15) | 0.0575 (19) | 0.0473 (14) | −0.0140 (14) | −0.0119 (12) | −0.0161 (13) |
C9 | 0.0476 (15) | 0.0444 (16) | 0.0489 (15) | −0.0035 (13) | −0.0131 (13) | −0.0176 (12) |
C10 | 0.0576 (17) | 0.0386 (16) | 0.0513 (15) | −0.0138 (14) | −0.0089 (14) | −0.0149 (12) |
C11 | 0.0489 (17) | 0.0486 (18) | 0.0517 (16) | −0.0107 (14) | 0.0080 (14) | 0.0128 (13) |
Mg1 | 0.0534 (8) | 0.0355 (7) | 0.0402 (6) | −0.0157 (6) | −0.0123 (6) | −0.0125 (5) |
N1 | 0.0550 (14) | 0.0517 (15) | 0.0441 (12) | −0.0065 (12) | −0.0148 (11) | −0.0133 (11) |
O1 | 0.0380 (10) | 0.0565 (13) | 0.0477 (10) | −0.0136 (9) | −0.0126 (8) | −0.0129 (9) |
O2 | 0.0419 (10) | 0.0483 (11) | 0.0493 (10) | −0.0215 (9) | 0.0089 (9) | −0.0242 (8) |
O3 | 0.0614 (13) | 0.0532 (13) | 0.0464 (10) | −0.0149 (11) | −0.0122 (9) | −0.0142 (9) |
O4 | 0.0439 (10) | 0.0482 (12) | 0.0465 (10) | −0.0193 (9) | −0.0060 (8) | −0.0195 (8) |
O5 | 0.0475 (10) | 0.0436 (11) | 0.0446 (10) | −0.0091 (9) | −0.0108 (8) | −0.0158 (8) |
C1—N1 | 1.361 (4) | C10—O1 | 1.244 (3) |
C1—C6 | 1.384 (4) | C10—O2 | 1.283 (3) |
C1—C2 | 1.406 (4) | C10—Mg1 | 2.831 (3) |
C2—C3 | 1.370 (4) | C11—O5 | 1.389 (3) |
C2—H2 | 0.9300 | C11—H11A | 0.9600 |
C3—C4 | 1.422 (4) | C11—H11B | 0.9600 |
C3—H3 | 0.9300 | C11—H11C | 0.9600 |
C4—C5 | 1.373 (4) | Mg1—O1 | 1.9913 (17) |
C4—H4 | 0.9300 | Mg1—O1i | 1.9913 (17) |
C5—C6 | 1.401 (4) | Mg1—O3i | 2.081 (2) |
C5—H5 | 0.9300 | Mg1—O3 | 2.081 (2) |
C6—C7 | 1.406 (4) | Mg1—N1 | 2.267 (3) |
C7—C8 | 1.357 (4) | Mg1—N1i | 2.267 (3) |
C7—H7 | 0.9300 | O3—H3A | 0.9600 |
C8—C9 | 1.366 (4) | O3—H3B | 0.9600 |
C8—H8 | 0.9300 | O4—H4A | 0.8500 |
C9—N1 | 1.360 (4) | O4—H4B | 0.8500 |
C9—C10 | 1.513 (4) | O5—H5C | 0.9599 |
N1—C1—C6 | 121.5 (3) | C9—C10—Mg1 | 82.07 (17) |
N1—C1—C2 | 117.4 (3) | O5—C11—H11A | 109.5 |
C6—C1—C2 | 121.1 (3) | O5—C11—H11B | 109.5 |
C3—C2—C1 | 118.7 (3) | H11A—C11—H11B | 109.5 |
C3—C2—H2 | 120.6 | O5—C11—H11C | 109.5 |
C1—C2—H2 | 120.6 | H11A—C11—H11C | 109.5 |
C2—C3—C4 | 121.2 (3) | H11B—C11—H11C | 109.5 |
C2—C3—H3 | 119.4 | O1—Mg1—O1i | 180.0 |
C4—C3—H3 | 119.4 | O1—Mg1—O3i | 87.67 (8) |
C5—C4—C3 | 118.9 (3) | O1i—Mg1—O3i | 92.33 (8) |
C5—C4—H4 | 120.6 | O1—Mg1—O3 | 92.33 (8) |
C3—C4—H4 | 120.6 | O1i—Mg1—O3 | 87.67 (8) |
C4—C5—C6 | 120.9 (3) | O3i—Mg1—O3 | 180.0 |
C4—C5—H5 | 119.5 | O1—Mg1—N1 | 76.97 (8) |
C6—C5—H5 | 119.5 | O1i—Mg1—N1 | 103.03 (8) |
C1—C6—C5 | 119.2 (3) | O3i—Mg1—N1 | 90.70 (8) |
C1—C6—C7 | 119.6 (3) | O3—Mg1—N1 | 89.30 (8) |
C5—C6—C7 | 121.2 (3) | O1—Mg1—N1i | 103.03 (8) |
C8—C7—C6 | 118.5 (3) | O1i—Mg1—N1i | 76.97 (8) |
C8—C7—H7 | 120.7 | O3i—Mg1—N1i | 89.30 (8) |
C6—C7—H7 | 120.7 | O3—Mg1—N1i | 90.70 (8) |
C7—C8—C9 | 119.6 (3) | N1—Mg1—N1i | 180.0 |
C7—C8—H8 | 120.2 | C9—N1—C1 | 117.0 (3) |
C9—C8—H8 | 120.2 | C9—N1—Mg1 | 110.26 (18) |
N1—C9—C8 | 123.7 (3) | C1—N1—Mg1 | 132.7 (2) |
N1—C9—C10 | 112.9 (3) | C10—O1—Mg1 | 120.38 (19) |
C8—C9—C10 | 123.3 (3) | Mg1—O3—H3A | 109.4 |
O1—C10—O2 | 124.2 (3) | Mg1—O3—H3B | 109.2 |
O1—C10—C9 | 119.4 (3) | H3A—O3—H3B | 109.5 |
O2—C10—C9 | 116.4 (3) | H4A—O4—H4B | 109.5 |
O2—C10—Mg1 | 161.3 (2) | C11—O5—H5C | 109.1 |
Symmetry code: (i) −x+1, −y, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3A···O2ii | 0.96 | 1.74 | 2.696 (3) | 171 |
O3—H3B···O4 | 0.96 | 1.76 | 2.713 (3) | 175 |
O4—H4A···O5iii | 0.85 | 1.99 | 2.759 (3) | 149 |
O4—H4B···O5iv | 0.85 | 2.21 | 2.968 (3) | 149 |
O5—H5C···O2v | 0.96 | 1.77 | 2.665 (3) | 153 |
Symmetry codes: (ii) −x+2, −y, −z+2; (iii) x, y−1, z; (iv) −x+1, −y+1, −z+1; (v) x, y+1, z−1. |
Experimental details
Crystal data | |
Chemical formula | [Mg(C10H6NO2)2(H2O)2]·2H2O·2CH4O |
Mr | 504.77 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 291 |
a, b, c (Å) | 7.129 (3), 9.038 (3), 10.846 (4) |
α, β, γ (°) | 75.677 (5), 74.138 (5), 70.160 (5) |
V (Å3) | 623.0 (4) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.13 |
Crystal size (mm) | 0.30 × 0.26 × 0.24 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.96, 0.97 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5796, 2445, 1640 |
Rint | 0.062 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.064, 0.129, 1.09 |
No. of reflections | 2445 |
No. of parameters | 161 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.22, −0.23 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXTL (Bruker, 2000), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3A···O2i | 0.96 | 1.74 | 2.696 (3) | 171 |
O3—H3B···O4 | 0.96 | 1.76 | 2.713 (3) | 175 |
O4—H4A···O5ii | 0.85 | 1.99 | 2.759 (3) | 149 |
O4—H4B···O5iii | 0.85 | 2.21 | 2.968 (3) | 149 |
O5—H5C···O2iv | 0.96 | 1.77 | 2.665 (3) | 153 |
Symmetry codes: (i) −x+2, −y, −z+2; (ii) x, y−1, z; (iii) −x+1, −y+1, −z+1; (iv) x, y+1, z−1. |
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As part of our ongoing studies of the coordination chemistry of magnesium(II) (Tai et al., 2007), we now report the synthesis and structure of the title compound, (I), (Fig. 1).
In the molecule of (I), The Mg(II) center (site symmetry 1) is six-coordinate with two O donor of H2O, four O, N donor of two quinaldine anions (Table 1). Intermolecular O—H···O hydrogen bonds help to consolidate the crystal packing (Table 2).