Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The title compound, [PdCl2(C12H20N2O2)], consists of discrete complex mol­ecules. The palladium center is in a square-planar geometry coordinated by two chloro anions and two N-donor atoms, with mean Pd-Cl and Pd-N bond distances of 2.278 (1) and 2.029 (2) Å, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804029290/rz6016sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804029290/rz6016Isup2.hkl
Contains datablock I

CCDC reference: 258698

Key indicators

  • Single-crystal X-ray study
  • T = 301 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.025
  • wR factor = 0.060
  • Data-to-parameter ratio = 18.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pd1 - N2 .. 5.60 su PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for C7 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C12 PLAT480_ALERT_4_C Long H...A H-Bond Reported H13A .. N2 .. 2.73 Ang.
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 26.37 From the CIF: _reflns_number_total 3239 Count of symmetry unique reflns 1709 Completeness (_total/calc) 189.53% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1530 Fraction of Friedel pairs measured 0.895 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2001); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

Dichloro[(4S,4'S)-4,4'-diisopropyl-2,2'-bi-1,3-oxazoline]palladium(II) top
Crystal data top
[PdCl2(C12H20N2O2)]F(000) = 404
Mr = 401.60Dx = 1.661 Mg m3
Monoclinic, P21Melting point: 253. K
Hall symbol: P 2ybMo Kα radiation, λ = 0.71073 Å
a = 6.3388 (13) ÅCell parameters from 3272 reflections
b = 12.790 (3) Åθ = 3.2–26.3°
c = 10.196 (2) ŵ = 1.49 mm1
β = 103.74 (3)°T = 301 K
V = 803.0 (3) Å3Prism, brown
Z = 20.54 × 0.20 × 0.18 mm
Data collection top
Oxford Diffraction Xcalibur CCD
diffractometer
3239 independent reflections
Radiation source: fine-focus sealed tube3120 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
Rotation method data acquisition using 'ω scans'θmax = 26.4°, θmin = 4.1°
Absorption correction: analytical
face-indexed (CrysAlis RED; Oxford Diffraction, 2003)
h = 47
Tmin = 0.501, Tmax = 0.776k = 1515
5523 measured reflectionsl = 1212
Refinement top
Refinement on F2 w = 1/[σ2(Fo2) + (0.0239P)2 + 0.6348P]
where P = (Fo2 + 2Fc2)/3
Least-squares matrix: full(Δ/σ)max = 0.001
R[F2 > 2σ(F2)] = 0.026Δρmax = 0.85 e Å3
wR(F2) = 0.060Δρmin = 0.56 e Å3
S = 1.08Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
3239 reflectionsExtinction coefficient: 0.0084 (12)
173 parametersAbsolute structure: Flack (1983), 1967 Friedel pairs
1 restraintAbsolute structure parameter: 0.05 (3)
H-atom parameters constrained
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C30.8624 (7)0.0047 (3)0.6334 (4)0.0526 (9)
C41.0034 (7)0.0152 (3)0.7672 (4)0.0501 (9)
C60.5761 (7)0.0742 (4)0.4872 (4)0.0580 (12)
H6A0.42430.05210.47330.070*
C70.6989 (11)0.0028 (6)0.4158 (6)0.0863 (19)
H7B0.61230.06470.38650.104*
H7A0.73450.02980.33790.104*
C91.0929 (6)0.0129 (3)0.9909 (4)0.0470 (8)
H9A1.15870.04781.04370.056*
C101.2656 (6)0.0697 (3)0.9349 (5)0.0548 (10)
H10B1.40210.03190.95710.066*
H10A1.28950.13980.97180.066*
C120.5853 (10)0.1905 (5)0.4510 (5)0.0715 (14)
H12A0.54450.23060.52310.086*
C130.8087 (13)0.2245 (6)0.4458 (8)0.108 (3)
H13C0.80710.29750.42400.129*
H13B0.85600.18500.37800.129*
H13A0.90650.21270.53210.129*
C140.4183 (12)0.2131 (7)0.3228 (6)0.116 (3)
H14C0.42490.28570.30020.139*
H14B0.27640.19710.33520.139*
H14A0.44700.17090.25110.139*
C150.9770 (7)0.0807 (3)1.0766 (4)0.0529 (10)
H15A0.86270.03791.09960.064*
C160.8701 (8)0.1751 (4)1.0007 (5)0.0628 (11)
H16C0.79890.21481.05750.075*
H16B0.97810.21770.97480.075*
H16A0.76510.15290.92140.075*
C171.1344 (11)0.1118 (5)1.2083 (5)0.0894 (18)
H17C1.06020.15431.26060.107*
H17B1.18940.05011.25840.107*
H17A1.25290.15061.18870.107*
N20.6904 (5)0.0579 (3)0.6296 (3)0.0458 (7)
N50.9405 (5)0.0230 (2)0.8670 (3)0.0406 (6)
O80.8983 (7)0.0297 (3)0.5186 (4)0.0787 (11)
O111.1781 (5)0.0733 (2)0.7879 (3)0.0610 (8)
Cl10.64648 (18)0.14617 (8)1.02844 (10)0.0522 (2)
Cl20.32994 (17)0.18221 (10)0.72770 (12)0.0624 (3)
Pd10.65534 (3)0.10302 (3)0.81330 (2)0.03745 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C30.063 (2)0.052 (2)0.048 (2)0.0063 (19)0.0229 (19)0.0030 (17)
C40.049 (2)0.0397 (19)0.066 (3)0.0094 (16)0.0223 (19)0.0028 (18)
C60.058 (2)0.074 (4)0.0405 (19)0.005 (2)0.0085 (17)0.0034 (18)
C70.104 (5)0.105 (5)0.050 (3)0.013 (4)0.017 (3)0.021 (3)
C90.046 (2)0.0368 (18)0.054 (2)0.0040 (15)0.0050 (17)0.0011 (16)
C100.0393 (19)0.042 (2)0.081 (3)0.0000 (15)0.0118 (19)0.0133 (19)
C120.087 (4)0.085 (4)0.044 (2)0.016 (3)0.018 (2)0.009 (2)
C130.118 (6)0.115 (6)0.084 (5)0.018 (5)0.014 (4)0.042 (4)
C140.108 (5)0.176 (8)0.066 (4)0.054 (5)0.023 (4)0.043 (4)
C150.060 (2)0.054 (2)0.044 (2)0.0117 (18)0.0108 (18)0.0086 (17)
C160.058 (2)0.060 (3)0.071 (3)0.016 (2)0.018 (2)0.015 (2)
C170.110 (4)0.093 (4)0.053 (3)0.020 (4)0.005 (3)0.013 (3)
N20.0511 (17)0.0397 (14)0.0499 (18)0.0055 (13)0.0183 (14)0.0042 (14)
N50.0448 (16)0.0331 (13)0.0465 (16)0.0007 (12)0.0161 (13)0.0009 (12)
O80.092 (3)0.091 (3)0.059 (2)0.031 (2)0.0291 (19)0.0146 (18)
O110.0548 (17)0.0564 (18)0.075 (2)0.0188 (13)0.0225 (15)0.0025 (15)
Cl10.0663 (6)0.0457 (4)0.0503 (5)0.0012 (4)0.0251 (4)0.0076 (4)
Cl20.0508 (5)0.0761 (7)0.0633 (6)0.0216 (5)0.0194 (5)0.0091 (5)
Pd10.03997 (13)0.03336 (12)0.04285 (13)0.00128 (14)0.01742 (8)0.00101 (14)
Geometric parameters (Å, º) top
C3—N21.278 (5)C12—H12A0.9800
C3—O81.320 (5)C13—H13C0.9600
C3—C41.465 (6)C13—H13B0.9600
C4—N51.276 (5)C13—H13A0.9600
C4—O111.309 (5)C14—H14C0.9600
C6—N21.476 (5)C14—H14B0.9600
C6—C121.537 (8)C14—H14A0.9600
C6—C71.541 (7)C15—C161.505 (6)
C6—H6A0.9800C15—C171.523 (6)
C7—O81.478 (7)C15—H15A0.9800
C7—H7B0.9700C16—H16C0.9600
C7—H7A0.9700C16—H16B0.9600
C9—N51.469 (5)C16—H16A0.9600
C9—C101.532 (6)C17—H17C0.9600
C9—C151.536 (6)C17—H17B0.9600
C9—H9A0.9800C17—H17A0.9600
C10—O111.470 (6)N2—Pd12.022 (3)
C10—H10B0.9700N5—Pd12.036 (3)
C10—H10A0.9700Cl1—Pd12.2755 (10)
C12—C131.494 (9)Cl2—Pd12.2775 (12)
C12—C141.502 (8)
N2—C3—O8118.4 (4)H13C—C13—H13A109.5
N2—C3—C4116.6 (3)H13B—C13—H13A109.5
O8—C3—C4124.9 (4)C12—C14—H14C109.5
N5—C4—O11120.1 (4)C12—C14—H14B109.5
N5—C4—C3116.1 (3)H14C—C14—H14B109.5
O11—C4—C3123.7 (4)C12—C14—H14A109.5
N2—C6—C12109.6 (4)H14C—C14—H14A109.5
N2—C6—C7100.9 (4)H14B—C14—H14A109.5
C12—C6—C7116.9 (5)C16—C15—C17111.4 (4)
N2—C6—H6A109.7C16—C15—C9112.2 (4)
C12—C6—H6A109.7C17—C15—C9110.3 (4)
C7—C6—H6A109.7C16—C15—H15A107.6
O8—C7—C6104.9 (4)C17—C15—H15A107.6
O8—C7—H7B110.8C9—C15—H15A107.6
C6—C7—H7B110.8C15—C16—H16C109.5
O8—C7—H7A110.8C15—C16—H16B109.5
C6—C7—H7A110.8H16C—C16—H16B109.5
H7B—C7—H7A108.8C15—C16—H16A109.5
N5—C9—C10102.1 (3)H16C—C16—H16A109.5
N5—C9—C15111.1 (3)H16B—C16—H16A109.5
C10—C9—C15115.2 (3)C15—C17—H17C109.5
N5—C9—H9A109.4C15—C17—H17B109.5
C10—C9—H9A109.4H17C—C17—H17B109.5
C15—C9—H9A109.4C15—C17—H17A109.5
O11—C10—C9105.3 (3)H17C—C17—H17A109.5
O11—C10—H10B110.7H17B—C17—H17A109.5
C9—C10—H10B110.7C3—N2—C6108.7 (3)
O11—C10—H10A110.7C3—N2—Pd1113.9 (3)
C9—C10—H10A110.7C6—N2—Pd1137.3 (3)
H10B—C10—H10A108.8C4—N5—C9107.5 (3)
C13—C12—C14113.0 (6)C4—N5—Pd1113.8 (3)
C13—C12—C6112.3 (5)C9—N5—Pd1138.5 (2)
C14—C12—C6109.6 (6)C3—O8—C7104.6 (4)
C13—C12—H12A107.2C4—O11—C10104.3 (3)
C14—C12—H12A107.2N2—Pd1—N579.62 (13)
C6—C12—H12A107.2N2—Pd1—Cl1174.56 (10)
C12—C13—H13C109.5N5—Pd1—Cl194.94 (9)
C12—C13—H13B109.5N2—Pd1—Cl293.48 (10)
H13C—C13—H13B109.5N5—Pd1—Cl2172.80 (9)
C12—C13—H13A109.5Cl1—Pd1—Cl291.95 (5)
N2—C3—C4—N50.2 (6)C7—C6—N2—Pd1172.2 (4)
O8—C3—C4—N5178.8 (4)O11—C4—N5—C90.9 (5)
N2—C3—C4—O11175.9 (4)C3—C4—N5—C9175.3 (3)
O8—C3—C4—O112.7 (7)O11—C4—N5—Pd1176.3 (3)
N2—C6—C7—O815.0 (6)C3—C4—N5—Pd10.0 (4)
C12—C6—C7—O8103.7 (6)C10—C9—N5—C45.6 (4)
N5—C9—C10—O117.9 (4)C15—C9—N5—C4117.7 (4)
C15—C9—C10—O11112.5 (4)C10—C9—N5—Pd1179.2 (3)
N2—C6—C12—C1369.9 (6)C15—C9—N5—Pd155.9 (5)
C7—C6—C12—C1344.0 (6)N2—C3—O8—C76.4 (6)
N2—C6—C12—C14163.5 (4)C4—C3—O8—C7172.2 (5)
C7—C6—C12—C1482.5 (6)C6—C7—O8—C313.4 (6)
N5—C9—C15—C1658.6 (4)N5—C4—O11—C104.5 (5)
C10—C9—C15—C1656.9 (5)C3—C4—O11—C10179.5 (4)
N5—C9—C15—C17176.7 (4)C9—C10—O11—C47.6 (4)
C10—C9—C15—C1767.9 (5)C3—N2—Pd1—N50.2 (3)
O8—C3—N2—C64.1 (6)C6—N2—Pd1—N5175.9 (4)
C4—C3—N2—C6177.2 (4)C3—N2—Pd1—Cl2178.2 (3)
O8—C3—N2—Pd1179.0 (3)C6—N2—Pd1—Cl26.2 (4)
C4—C3—N2—Pd10.3 (5)C4—N5—Pd1—N20.1 (3)
C12—C6—N2—C3112.0 (4)C9—N5—Pd1—N2173.2 (4)
C7—C6—N2—C311.9 (5)C4—N5—Pd1—Cl1179.7 (3)
C12—C6—N2—Pd163.8 (6)C9—N5—Pd1—Cl16.9 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C13—H13A···N20.962.733.047 (9)100
C16—H16A···N50.962.632.960 (6)101
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds