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In the title compound, [PdII(C3H2O4)(C3H10N2)], the PdII atom adopts a distorted cis-square-planar geometry. The ligands form two six-membered chelate rings, with propane-1,3-diamine adopting a chair conformation and the malonato ligand a boat conformation. The crystal packing is stabilized by a network of N—H...O and C—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807004199/sj2210sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807004199/sj2210Isup2.hkl
Contains datablock I

CCDC reference: 636810

Key indicators

  • Single-crystal X-ray study
  • T = 123 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.016
  • wR factor = 0.043
  • Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT148_ALERT_3_B su on the a - Axis is Too Large (x 1000) . 5 Ang. PLAT148_ALERT_3_B su on the b - Axis is Too Large (x 1000) . 10 Ang.
Alert level C PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 3 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

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2005) and CRYSTALS (Betteridge et al., 2003); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: CrystalStructure.

(Malonato-κ2O:O')(propane-1,3-diamine-κ2N:N')palladium(II) top
Crystal data top
[Pd(C3H2O4)(C3H10N2)]Z = 2
Mr = 282.60F(000) = 280.00
Triclinic, P1Dx = 2.183 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.7107 Å
a = 4.430 (5) ÅCell parameters from 4173 reflections
b = 8.94 (1) Åθ = 3.4–27.5°
c = 11.40 (1) ŵ = 2.14 mm1
α = 106.93 (3)°T = 123 K
β = 90.83 (4)°Needle, colorless
γ = 95.03 (4)°0.50 × 0.05 × 0.05 mm
V = 429.9 (8) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
1889 reflections with F2 > 2σ(F2)
Detector resolution: 10.00 pixels mm-1Rint = 0.018
ω scansθmax = 27.5°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 55
Tmin = 0.574, Tmax = 0.898k = 1111
4252 measured reflectionsl = 1414
1958 independent reflections
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.016 w = 1/[σ2(Fo2) + (0.0242P)2 + 0.1199P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.043(Δ/σ)max < 0.001
S = 1.09Δρmax = 0.46 e Å3
1958 reflectionsΔρmin = 0.89 e Å3
119 parameters
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 using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd10.35023 (3)0.968883 (13)0.244399 (10)0.00850 (6)
O10.1297 (3)1.07758 (15)0.14101 (11)0.0123 (2)
O20.1441 (3)1.26866 (16)0.13242 (12)0.0194 (3)
O30.1240 (3)1.07096 (15)0.39429 (11)0.0124 (2)
O40.1469 (3)1.26194 (16)0.49075 (12)0.0188 (3)
N10.5509 (3)0.85836 (18)0.08874 (13)0.0114 (3)
H1A0.44030.86710.02470.014*
H1B0.73450.91010.08860.014*
N20.5457 (4)0.85110 (18)0.34821 (13)0.0114 (3)
H2A0.72900.90200.37590.014*
H2B0.43280.85720.41410.014*
C10.5925 (4)0.6901 (2)0.06755 (15)0.0128 (3)
H1C0.70290.65350.00660.015*
H1D0.39500.63040.05480.015*
C20.7629 (4)0.6588 (2)0.17344 (16)0.0132 (3)
H2C0.81580.55140.14760.016*
H2D0.95050.72730.19180.016*
C30.5878 (4)0.6832 (2)0.28991 (16)0.0133 (3)
H3A0.39070.62340.27060.016*
H3B0.69600.64380.34750.016*
C60.0247 (4)1.2072 (2)0.40964 (15)0.0114 (3)
C50.1312 (4)1.3001 (2)0.32211 (15)0.0130 (3)
H5A0.05031.40150.34600.016*
H5B0.35081.31810.32800.016*
C40.0279 (4)1.2125 (2)0.18947 (15)0.0119 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.00930 (8)0.00899 (8)0.00757 (8)0.00094 (5)0.00011 (5)0.00297 (5)
O10.0155 (6)0.0124 (6)0.0099 (6)0.0037 (5)0.0009 (5)0.0040 (5)
O20.0255 (7)0.0190 (7)0.0161 (6)0.0079 (6)0.0028 (5)0.0073 (5)
O30.0147 (6)0.0143 (6)0.0095 (6)0.0032 (5)0.0026 (5)0.0047 (5)
O40.0221 (7)0.0193 (7)0.0163 (7)0.0067 (6)0.0077 (5)0.0055 (5)
N10.0131 (7)0.0113 (7)0.0100 (7)0.0017 (6)0.0009 (5)0.0034 (5)
N20.0132 (7)0.0125 (7)0.0096 (7)0.0024 (6)0.0003 (5)0.0043 (5)
C10.0162 (9)0.0103 (8)0.0118 (8)0.0022 (7)0.0013 (6)0.0027 (6)
C20.0122 (8)0.0106 (8)0.0164 (9)0.0028 (6)0.0001 (6)0.0027 (6)
C30.0160 (9)0.0114 (8)0.0136 (8)0.0017 (7)0.0014 (7)0.0054 (6)
C60.0120 (8)0.0129 (8)0.0088 (8)0.0004 (6)0.0022 (6)0.0031 (6)
C50.0160 (8)0.0108 (8)0.0123 (8)0.0001 (7)0.0008 (6)0.0038 (6)
C40.0129 (8)0.0116 (8)0.0119 (8)0.0002 (6)0.0026 (6)0.0049 (6)
Geometric parameters (Å, º) top
Pd1—N12.024 (2)N2—H2B0.9000
Pd1—N22.029 (2)C1—C21.521 (3)
Pd1—O12.0225 (18)C1—H1C0.9700
Pd1—O32.015 (2)C1—H1D0.9700
O1—C41.296 (2)C2—C31.518 (3)
O2—C41.224 (2)C2—H2C0.9700
O3—C61.296 (3)C2—H2D0.9700
O4—C61.223 (2)C3—H3A0.9700
N1—C11.481 (3)C3—H3B0.9700
N1—H1A0.9000C6—C51.529 (3)
N1—H1B0.9000C5—C41.529 (3)
N2—C31.484 (3)C5—H5A0.9700
N2—H2A0.9000C5—H5B0.9700
O1—Pd1—N186.42 (9)H1C—C1—H1D107.8
O1—Pd1—N2176.25 (5)C3—C2—C1114.40 (16)
O3—Pd1—N1176.18 (5)C3—C2—H2C108.7
O3—Pd1—N286.67 (9)C1—C2—H2C108.7
O3—Pd1—O192.08 (9)C3—C2—H2D108.7
N1—Pd1—N294.60 (9)C1—C2—H2D108.7
C4—O1—Pd1121.31 (12)H2C—C2—H2D107.6
C6—O3—Pd1121.25 (11)N2—C3—C2112.16 (15)
C1—N1—Pd1117.27 (11)N2—C3—H3A109.2
C1—N1—H1A108.0C2—C3—H3A109.2
Pd1—N1—H1A108.0N2—C3—H3B109.2
C1—N1—H1B108.0C2—C3—H3B109.2
Pd1—N1—H1B108.0H3A—C3—H3B107.9
H1A—N1—H1B107.2O4—C6—O3122.34 (16)
C3—N2—Pd1117.84 (12)O4—C6—C5120.12 (17)
C3—N2—H2A107.8O3—C6—C5117.54 (16)
Pd1—N2—H2A107.8C4—C5—C6111.33 (16)
C3—N2—H2B107.8C4—C5—H5A109.4
Pd1—N2—H2B107.8C6—C5—H5A109.4
H2A—N2—H2B107.2C4—C5—H5B109.4
N1—C1—C2113.04 (15)C6—C5—H5B109.4
N1—C1—H1C109.0H5A—C5—H5B108.0
C2—C1—H1C109.0O2—C4—O1121.97 (17)
N1—C1—H1D109.0O2—C4—C5120.81 (17)
C2—C1—H1D109.0O1—C4—C5117.22 (16)
Pd1—N1—C1—C254.76 (19)O1—Pd1—N1—C1140.02 (13)
Pd1—N2—C3—C254.82 (19)O3—Pd1—N2—C3139.66 (14)
N1—Pd1—N2—C336.73 (14)Pd1—O3—C6—O4169.98 (13)
N1—C1—C2—C369.1 (2)Pd1—O3—C6—C510.3 (2)
N2—Pd1—N1—C136.36 (14)O4—C6—C5—C4118.12 (19)
C1—C2—C3—N268.7 (2)O3—C6—C5—C462.2 (2)
O3—Pd1—O1—C428.41 (13)Pd1—O1—C4—O2168.81 (13)
N1—Pd1—O1—C4155.11 (14)Pd1—O1—C4—C511.1 (2)
O1—Pd1—O3—C628.80 (13)C6—C5—C4—O2117.4 (2)
N2—Pd1—O3—C6154.75 (14)C6—C5—C4—O162.5 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O2i0.902.192.956 (3)143
N1—H1B···O1ii0.902.163.027 (4)163
N2—H2A···O3ii0.902.183.030 (4)158
N2—H2B···O4iii0.902.102.894 (3)147
C2—H2C···O2iv0.972.513.445 (4)163
Symmetry codes: (i) x, y+2, z; (ii) x+1, y, z; (iii) x, y+2, z+1; (iv) x+1, y1, z.
 

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