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The reaction of magnesium(II) nitrate hexa­hydrate with the proton-transfer compound (pipzH2)(pydc) [pipz is piperazine and pydcH2 is pyridine-2,6-dicarboxylic acid] in aqueous solution leads to the formation of the title compound, [Mg(C7H3O4)(H2O)3]·2H2O. The piperazinium cation is not incorporated in this crystal structure. The MgII atom has a distorted octa­hedral coordination environment. There are many inter­molecular O—H...O hydrogen bonds involving the (pydc)2− species and water mol­ecules in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680701937X/pr2003sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680701937X/pr2003Isup2.hkl
Contains datablock I

CCDC reference: 646591

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.001 Å
  • R factor = 0.027
  • wR factor = 0.079
  • Data-to-parameter ratio = 17.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H6A .. H8B .. 2.06 Ang.
Alert level C PLAT048_ALERT_1_C MoietyFormula Not Given ........................ ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mg1 - N1 .. 5.78 su PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 1 O7 -MG1 -N1 -C2 152.90 0.40 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6 O7 -MG1 -N1 -C6 -24.40 0.50 1.555 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 0 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: XSCANS (Bruker, 1998); cell refinement: XSCANS; data reduction: SAINT-Plus (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXTL.

Triaqua(pyridine-2,6-dicarboxylato)magnesium(II) dihydrate top
Crystal data top
[Mg(C7H3O4)(H2O)3]·2H2OF(000) = 584
Mr = 279.49Dx = 1.592 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.9229 (7) ÅCell parameters from 17671 reflections
b = 9.9459 (8) Åθ = 2.5–27.6°
c = 13.2508 (10) ŵ = 0.19 mm1
β = 97.383 (4)°T = 150 K
V = 1166.21 (16) Å3Block, colourless
Z = 40.22 × 0.19 × 0.17 mm
Data collection top
Bruker APEXII
diffractometer
2780 independent reflections
Radiation source: fine-focus sealed tube2596 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
Detector resolution: 100 pixels mm-1θmax = 27.9°, θmin = 2.6°
ω scansh = 1111
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997a)
k = 1313
Tmin = 0.879, Tmax = 0.968l = 1717
27484 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0426P)2 + 0.5028P]
where P = (Fo2 + 2Fc2)/3
2780 reflections(Δ/σ)max = 0.001
163 parametersΔρmax = 0.36 e Å3
0 restraintsΔρmin = 0.33 e Å3
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
xyzUiso*/Ueq
Mg10.94555 (4)0.77757 (3)0.72778 (2)0.01190 (10)
N10.96732 (10)0.75754 (8)0.57207 (6)0.01214 (17)
O10.79253 (8)0.61715 (7)0.67119 (6)0.01531 (16)
O20.70377 (10)0.49507 (8)0.53455 (6)0.02170 (18)
O31.25850 (9)0.99566 (8)0.58303 (6)0.01913 (17)
O41.10602 (8)0.92879 (8)0.69624 (6)0.01589 (16)
O50.76850 (8)0.91036 (8)0.70375 (6)0.01731 (17)
H5A0.68110.89140.65710.021*
H5B0.74380.98230.74580.021*
O61.11699 (9)0.64309 (8)0.76000 (6)0.02097 (18)
H6A1.19310.64520.71610.025*
H6B1.15670.59660.82010.025*
O70.94305 (10)0.80247 (9)0.87798 (6)0.02146 (18)
H7A0.98980.75510.93590.026*
H7B0.89300.87430.90710.026*
O80.63473 (9)0.37721 (8)0.34965 (6)0.01897 (17)
H8A0.65510.42730.41090.023*
H8B0.60210.44250.29930.023*
O90.51687 (9)0.83294 (8)0.56894 (6)0.02121 (18)
H9B0.47550.75890.60130.025*
H9A0.43750.89730.56220.025*
C10.78414 (11)0.58612 (10)0.57773 (8)0.0141 (2)
C20.88498 (11)0.66661 (10)0.51583 (7)0.01294 (19)
C30.89889 (12)0.64870 (11)0.41319 (8)0.0172 (2)
H30.83820.58500.37310.021*
C41.00462 (13)0.72714 (11)0.37116 (8)0.0177 (2)
H41.01710.71680.30150.021*
C51.09195 (12)0.82055 (11)0.43094 (8)0.0156 (2)
H51.16510.87400.40340.019*
C61.06856 (11)0.83301 (10)0.53218 (7)0.01238 (19)
C71.15228 (11)0.92801 (10)0.60956 (8)0.01370 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.01321 (17)0.01233 (17)0.01021 (17)0.00017 (11)0.00176 (12)0.00039 (11)
N10.0128 (4)0.0113 (4)0.0122 (4)0.0001 (3)0.0015 (3)0.0008 (3)
O10.0185 (3)0.0152 (3)0.0126 (3)0.0037 (3)0.0030 (3)0.0000 (3)
O20.0281 (4)0.0216 (4)0.0152 (4)0.0130 (3)0.0019 (3)0.0016 (3)
O30.0183 (4)0.0203 (4)0.0194 (4)0.0081 (3)0.0049 (3)0.0025 (3)
O40.0174 (3)0.0168 (3)0.0135 (3)0.0036 (3)0.0027 (3)0.0019 (3)
O50.0164 (3)0.0177 (4)0.0172 (4)0.0042 (3)0.0004 (3)0.0043 (3)
O60.0205 (4)0.0256 (4)0.0175 (4)0.0104 (3)0.0045 (3)0.0056 (3)
O70.0283 (4)0.0253 (4)0.0110 (3)0.0112 (3)0.0032 (3)0.0000 (3)
O80.0247 (4)0.0173 (4)0.0149 (4)0.0007 (3)0.0022 (3)0.0002 (3)
O90.0194 (4)0.0231 (4)0.0211 (4)0.0038 (3)0.0025 (3)0.0016 (3)
C10.0155 (4)0.0134 (4)0.0134 (4)0.0017 (3)0.0012 (3)0.0016 (3)
C20.0142 (4)0.0121 (4)0.0124 (4)0.0010 (3)0.0011 (3)0.0009 (3)
C30.0215 (5)0.0165 (5)0.0130 (5)0.0042 (4)0.0009 (4)0.0019 (4)
C40.0230 (5)0.0196 (5)0.0108 (4)0.0013 (4)0.0040 (4)0.0002 (4)
C50.0170 (5)0.0163 (5)0.0142 (5)0.0013 (4)0.0044 (4)0.0018 (4)
C60.0125 (4)0.0115 (4)0.0130 (4)0.0000 (3)0.0014 (3)0.0006 (3)
C70.0138 (4)0.0125 (4)0.0146 (4)0.0004 (3)0.0010 (3)0.0006 (3)
Geometric parameters (Å, º) top
Mg1—O72.0086 (8)O7—H7A0.9501
Mg1—O62.0356 (8)O7—H7B0.9500
Mg1—O52.0523 (8)O8—H8A0.9499
Mg1—N12.1065 (9)O8—H8B0.9501
Mg1—O42.1542 (8)O9—H9B0.9501
Mg1—O12.1700 (8)O9—H9A0.9500
N1—C21.3313 (13)C1—C21.5208 (14)
N1—C61.3347 (13)C2—C31.3929 (14)
O1—C11.2692 (13)C3—C41.3943 (15)
O2—C11.2475 (13)C3—H30.9500
O3—C71.2491 (13)C4—C51.3925 (15)
O4—C71.2695 (13)C4—H40.9500
O5—H5A0.9500C5—C61.3895 (14)
O5—H5B0.9501C5—H50.9500
O6—H6A0.9500C6—C71.5183 (14)
O6—H6B0.9499
O7—Mg1—O688.68 (3)Mg1—O7—H7A132.8
O7—Mg1—O588.17 (3)Mg1—O7—H7B124.1
O6—Mg1—O5176.49 (4)H7A—O7—H7B103.0
O7—Mg1—N1175.10 (4)H8A—O8—H8B104.5
O6—Mg1—N188.96 (3)H9B—O9—H9A103.7
O5—Mg1—N194.30 (3)O2—C1—O1125.62 (9)
O7—Mg1—O4101.45 (4)O2—C1—C2118.68 (9)
O6—Mg1—O489.95 (3)O1—C1—C2115.68 (9)
O5—Mg1—O492.19 (3)N1—C2—C3121.43 (9)
N1—Mg1—O474.26 (3)N1—C2—C1112.21 (8)
O7—Mg1—O1110.27 (4)C3—C2—C1126.32 (9)
O6—Mg1—O190.68 (3)C2—C3—C4117.92 (9)
O5—Mg1—O188.96 (3)C2—C3—H3121.0
N1—Mg1—O174.05 (3)C4—C3—H3121.0
O4—Mg1—O1148.28 (3)C5—C4—C3120.26 (9)
C2—N1—C6120.88 (9)C5—C4—H4119.9
C2—N1—Mg1119.92 (7)C3—C4—H4119.9
C6—N1—Mg1119.14 (7)C6—C5—C4117.79 (9)
C1—O1—Mg1118.14 (6)C6—C5—H5121.1
C7—O4—Mg1118.21 (6)C4—C5—H5121.1
Mg1—O5—H5A121.6N1—C6—C5121.70 (9)
Mg1—O5—H5B128.7N1—C6—C7112.45 (8)
H5A—O5—H5B107.4C5—C6—C7125.85 (9)
Mg1—O6—H6A115.7O3—C7—O4126.73 (9)
Mg1—O6—H6B133.3O3—C7—C6118.06 (9)
H6A—O6—H6B107.8O4—C7—C6115.20 (9)
O7—Mg1—N1—C2152.9 (4)Mg1—N1—C2—C3178.60 (8)
O6—Mg1—N1—C291.71 (8)C6—N1—C2—C1176.44 (8)
O5—Mg1—N1—C286.98 (8)Mg1—N1—C2—C10.81 (11)
O4—Mg1—N1—C2178.05 (8)O2—C1—C2—N1178.23 (9)
O1—Mg1—N1—C20.71 (7)O1—C1—C2—N10.36 (13)
O7—Mg1—N1—C624.4 (5)O2—C1—C2—C30.56 (16)
O6—Mg1—N1—C685.58 (8)O1—C1—C2—C3178.03 (10)
O5—Mg1—N1—C695.72 (8)N1—C2—C3—C41.40 (16)
O4—Mg1—N1—C64.66 (7)C1—C2—C3—C4176.07 (10)
O1—Mg1—N1—C6176.59 (8)C2—C3—C4—C50.39 (16)
O7—Mg1—O1—C1178.05 (7)C3—C4—C5—C60.63 (16)
O6—Mg1—O1—C189.20 (8)C2—N1—C6—C50.26 (15)
O5—Mg1—O1—C194.29 (8)Mg1—N1—C6—C5177.53 (8)
N1—Mg1—O1—C10.48 (7)C2—N1—C6—C7178.83 (9)
O4—Mg1—O1—C11.80 (11)Mg1—N1—C6—C71.56 (11)
O7—Mg1—O4—C7169.71 (7)C4—C5—C6—N10.73 (15)
O6—Mg1—O4—C781.07 (8)C4—C5—C6—C7179.69 (9)
O5—Mg1—O4—C7101.72 (8)Mg1—O4—C7—O3169.87 (8)
N1—Mg1—O4—C77.87 (7)Mg1—O4—C7—C69.48 (11)
O1—Mg1—O4—C710.14 (11)N1—C6—C7—O3174.19 (9)
Mg1—O1—C1—O2178.70 (8)C5—C6—C7—O34.86 (15)
Mg1—O1—C1—C20.22 (12)N1—C6—C7—O45.23 (12)
C6—N1—C2—C31.36 (15)C5—C6—C7—O4175.73 (10)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5A···O90.951.852.7919 (11)173
O5—H5B···O1i0.951.792.7395 (10)177
O6—H6A···O8ii0.951.872.8084 (11)167
O6—H6B···O3iii0.951.732.6678 (11)171
O7—H7A···O9iv0.951.962.8674 (11)160
O7—H7B···O2i0.951.722.6683 (11)176
O8—H8A···O20.951.772.7145 (11)171
O8—H8B···O4v0.951.872.7905 (11)161
O9—H9B···O8vi0.951.842.7815 (11)170
O9—H9A···O3vii0.951.922.8424 (12)162
Symmetry codes: (i) x+3/2, y+1/2, z+3/2; (ii) x+2, y+1, z+1; (iii) x+5/2, y1/2, z+3/2; (iv) x+1/2, y+3/2, z+1/2; (v) x1/2, y+3/2, z1/2; (vi) x+1, y+1, z+1; (vii) x1, y, z.
 

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