Download citation
Download citation
link to html
In the title compound, [Zn(C3H10N2)3]Cl2·2H2O, a complex three-dimensional network of N—H...O, N—H...Cl and O—H...Cl hydrogen bonds helps to establish the crystal packing.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807014766/fj2009sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807014766/fj2009Isup2.hkl
Contains datablock I

CCDC reference: 647203

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.042
  • wR factor = 0.102
  • Data-to-parameter ratio = 21.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99 PLAT230_ALERT_2_C Hirshfeld Test Diff for N1 - C1 .. 5.63 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn1 - N3 .. 5.80 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn1 - N4 .. 7.92 su PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT420_ALERT_2_C D-H Without Acceptor N2 - H3 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N4 - H13 ... ?
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 30.03 From the CIF: _reflns_number_total 3984 Count of symmetry unique reflns 2832 Completeness (_total/calc) 140.68% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1152 Fraction of Friedel pairs measured 0.407 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT792_ALERT_1_G Check the Absolute Configuration of C2 = ... S PLAT792_ALERT_1_G Check the Absolute Configuration of C5 = ... S PLAT792_ALERT_1_G Check the Absolute Configuration of C8 = ... S
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 6 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 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 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Tris(propane-1,2-diamine-κ2N,N')zinc(II) dichloride dihydrate top
Crystal data top
[Zn(C3H10N2)3]Cl2·2H2OF(000) = 840
Mr = 394.69Dx = 1.356 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2ycCell parameters from 2649 reflections
a = 12.6384 (9) Åθ = 2.4–25.3°
b = 17.2427 (12) ŵ = 1.56 mm1
c = 8.8721 (6) ÅT = 293 K
β = 90.777 (1)°Block, colourless
V = 1933.2 (2) Å30.37 × 0.18 × 0.17 mm
Z = 4
Data collection top
Bruker SMART1000 CCD
diffractometer
3984 independent reflections
Radiation source: fine-focus sealed tube3019 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ω scansθmax = 30.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Bruker, 1999)
h = 1710
Tmin = 0.597, Tmax = 0.778k = 2423
8264 measured reflectionsl = 1210
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difmap and geom
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.102 w = 1/[σ2(Fo2) + (0.0534P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.97(Δ/σ)max = 0.002
3984 reflectionsΔρmax = 0.45 e Å3
185 parametersΔρmin = 0.28 e Å3
2 restraintsAbsolute structure: Flack (1983), 1152 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.190 (17)
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
Zn10.15068 (4)0.19751 (2)0.16002 (4)0.03674 (12)
N10.2977 (4)0.2017 (2)0.0287 (5)0.0523 (12)
H10.28240.20080.07060.063*
H20.33370.24550.04970.063*
N20.2455 (3)0.1092 (3)0.2807 (5)0.0500 (11)
H30.23810.11440.38090.060*
H40.22420.06120.25390.060*
C10.3615 (4)0.1335 (3)0.0708 (6)0.0542 (13)
H50.43410.14110.03980.065*
H60.33400.08790.01960.065*
C20.3585 (4)0.1213 (3)0.2385 (6)0.0504 (12)
H70.38490.16830.28870.061*
C30.4280 (5)0.0527 (4)0.2868 (8)0.0848 (19)
H80.42060.04400.39300.127*
H90.50060.06400.26520.127*
H100.40630.00710.23250.127*
N30.0868 (4)0.3017 (2)0.0502 (5)0.0497 (11)
H110.10830.30400.04600.060*
H120.01560.30050.05020.060*
N40.2025 (4)0.2872 (2)0.3223 (5)0.0489 (11)
H130.19750.26930.41730.059*
H140.27030.30040.30590.059*
C40.1260 (4)0.3713 (3)0.1354 (6)0.0572 (14)
H150.19530.38570.09930.069*
H160.07830.41450.11750.069*
C50.1327 (4)0.3549 (3)0.3001 (5)0.0512 (11)
H170.06180.33950.33190.061*
C60.1649 (5)0.4231 (3)0.3949 (7)0.0716 (16)
H180.16800.40800.49900.107*
H190.11410.46410.38200.107*
H200.23330.44100.36440.107*
N50.0764 (4)0.1135 (3)0.0091 (5)0.0530 (11)
H210.07410.13240.08540.064*
H220.11440.06930.00870.064*
N60.0037 (4)0.1724 (3)0.2831 (5)0.0504 (11)
H230.01750.16970.38280.060*
H240.04390.21050.26690.060*
C70.0327 (5)0.0973 (3)0.0612 (6)0.0571 (14)
H250.05530.04710.02320.069*
H260.08050.13620.02020.069*
C80.0395 (4)0.0975 (3)0.2286 (6)0.0507 (12)
H270.00640.05610.26750.061*
C90.1489 (5)0.0813 (4)0.2779 (8)0.0782 (17)
H280.15180.08400.38590.117*
H290.16950.03040.24520.117*
H300.19630.11900.23470.117*
Cl10.44920 (12)0.35064 (9)0.16614 (16)0.0630 (4)
Cl20.82637 (11)0.31616 (9)0.14336 (16)0.0610 (4)
O10.6597 (4)0.4532 (2)0.1305 (5)0.0809 (14)
H310.60060.42510.14040.097*
H320.70730.41430.13410.097*
O20.6187 (4)0.2166 (2)0.2024 (5)0.0843 (13)
H330.57010.25460.19220.101*
H340.67770.24450.18590.101*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0343 (2)0.0407 (2)0.0352 (2)0.0012 (3)0.00068 (15)0.0019 (3)
N10.048 (3)0.072 (3)0.036 (2)0.004 (2)0.0045 (18)0.0002 (19)
N20.052 (3)0.057 (3)0.041 (2)0.006 (2)0.0018 (19)0.0009 (18)
C10.053 (3)0.057 (3)0.053 (3)0.014 (3)0.008 (2)0.002 (2)
C20.033 (3)0.060 (3)0.059 (3)0.011 (2)0.003 (2)0.002 (2)
C30.062 (4)0.099 (5)0.093 (5)0.026 (3)0.012 (3)0.017 (4)
N30.048 (3)0.069 (3)0.032 (2)0.005 (2)0.0008 (18)0.0057 (18)
N40.053 (3)0.056 (2)0.038 (2)0.0064 (18)0.0002 (19)0.0080 (17)
C40.064 (4)0.040 (2)0.069 (4)0.001 (2)0.002 (3)0.013 (2)
C50.049 (3)0.052 (3)0.053 (3)0.006 (2)0.004 (2)0.001 (2)
C60.077 (4)0.053 (3)0.084 (4)0.007 (3)0.012 (3)0.009 (3)
N50.056 (3)0.063 (3)0.039 (2)0.002 (2)0.006 (2)0.0029 (19)
N60.051 (3)0.057 (3)0.043 (2)0.002 (2)0.0037 (19)0.0064 (19)
C70.052 (4)0.065 (3)0.053 (3)0.011 (3)0.009 (2)0.007 (2)
C80.049 (3)0.049 (3)0.054 (3)0.013 (2)0.001 (2)0.007 (2)
C90.058 (4)0.092 (4)0.085 (4)0.025 (3)0.014 (3)0.010 (3)
Cl10.0502 (8)0.0807 (10)0.0579 (8)0.0081 (7)0.0025 (6)0.0049 (7)
Cl20.0456 (8)0.0802 (9)0.0573 (8)0.0112 (6)0.0017 (6)0.0096 (7)
O10.070 (3)0.0533 (19)0.120 (4)0.004 (2)0.011 (3)0.006 (2)
O20.074 (3)0.075 (3)0.104 (4)0.004 (2)0.008 (2)0.004 (2)
Geometric parameters (Å, º) top
Zn1—N52.177 (4)C4—C51.489 (7)
Zn1—N32.193 (4)C4—H150.9700
Zn1—N42.206 (4)C4—H160.9700
Zn1—N22.207 (4)C5—C61.499 (7)
Zn1—N12.207 (5)C5—H170.9800
Zn1—N62.211 (4)C6—H180.9600
N1—C11.472 (6)C6—H190.9600
N1—H10.9000C6—H200.9600
N1—H20.9000N5—C71.487 (7)
N2—C21.496 (6)N5—H210.9000
N2—H30.9000N5—H220.9000
N2—H40.9000N6—C81.480 (6)
C1—C21.504 (7)N6—H230.9000
C1—H50.9700N6—H240.9000
C1—H60.9700C7—C81.488 (7)
C2—C31.531 (7)C7—H250.9700
C2—H70.9800C7—H260.9700
C3—H80.9600C8—C91.484 (8)
C3—H90.9600C8—H270.9800
C3—H100.9600C9—H280.9600
N3—C41.498 (6)C9—H290.9600
N3—H110.9000C9—H300.9600
N3—H120.9000O1—H310.8954
N4—C51.476 (6)O1—H320.9005
N4—H130.9000O2—H330.9009
N4—H140.9000O2—H340.9006
N5—Zn1—N396.84 (17)C5—N4—H14110.3
N5—Zn1—N4171.74 (19)Zn1—N4—H14110.3
N3—Zn1—N479.63 (16)H13—N4—H14108.5
N5—Zn1—N293.77 (14)C5—C4—N3111.0 (4)
N3—Zn1—N2167.30 (18)C5—C4—H15109.4
N4—Zn1—N290.72 (17)N3—C4—H15109.4
N5—Zn1—N193.22 (16)C5—C4—H16109.4
N3—Zn1—N192.65 (17)N3—C4—H16109.4
N4—Zn1—N194.40 (17)H15—C4—H16108.0
N2—Zn1—N179.79 (17)N4—C5—C4107.9 (4)
N5—Zn1—N679.36 (17)N4—C5—C6112.8 (4)
N3—Zn1—N694.20 (18)C4—C5—C6114.4 (4)
N4—Zn1—N693.38 (17)N4—C5—H17107.1
N2—Zn1—N694.59 (16)C4—C5—H17107.1
N1—Zn1—N6170.44 (16)C6—C5—H17107.1
C1—N1—Zn1107.6 (3)C5—C6—H18109.5
C1—N1—H1110.2C5—C6—H19109.5
Zn1—N1—H1110.2H18—C6—H19109.5
C1—N1—H2110.2C5—C6—H20109.5
Zn1—N1—H2110.2H18—C6—H20109.5
H1—N1—H2108.5H19—C6—H20109.5
C2—N2—Zn1107.2 (3)C7—N5—Zn1109.1 (3)
C2—N2—H3110.3C7—N5—H21109.9
Zn1—N2—H3110.3Zn1—N5—H21109.9
C2—N2—H4110.3C7—N5—H22109.9
Zn1—N2—H4110.3Zn1—N5—H22109.9
H3—N2—H4108.5H21—N5—H22108.3
N1—C1—C2109.9 (4)C8—N6—Zn1108.5 (3)
N1—C1—H5109.7C8—N6—H23110.0
C2—C1—H5109.7Zn1—N6—H23110.0
N1—C1—H6109.7C8—N6—H24110.0
C2—C1—H6109.7Zn1—N6—H24110.0
H5—C1—H6108.2H23—N6—H24108.4
N2—C2—C1107.7 (4)N5—C7—C8112.1 (4)
N2—C2—C3111.5 (5)N5—C7—H25109.2
C1—C2—C3111.3 (5)C8—C7—H25109.2
N2—C2—H7108.8N5—C7—H26109.2
C1—C2—H7108.8C8—C7—H26109.2
C3—C2—H7108.8H25—C7—H26107.9
C2—C3—H8109.5N6—C8—C9114.1 (5)
C2—C3—H9109.5N6—C8—C7107.6 (4)
H8—C3—H9109.5C9—C8—C7111.1 (5)
C2—C3—H10109.5N6—C8—H27107.9
H8—C3—H10109.5C9—C8—H27107.9
H9—C3—H10109.5C7—C8—H27107.9
C4—N3—Zn1108.3 (3)C8—C9—H28109.5
C4—N3—H11110.0C8—C9—H29109.5
Zn1—N3—H11110.0H28—C9—H29109.5
C4—N3—H12110.0C8—C9—H30109.5
Zn1—N3—H12110.0H28—C9—H30109.5
H11—N3—H12108.4H29—C9—H30109.5
C5—N4—Zn1107.2 (3)H31—O1—H3298.8
C5—N4—H13110.3H33—O2—H3499.3
Zn1—N4—H13110.3
N5—Zn1—N1—C180.2 (4)N1—Zn1—N4—C5114.0 (3)
N3—Zn1—N1—C1177.2 (3)N6—Zn1—N4—C571.6 (3)
N4—Zn1—N1—C1103.0 (3)Zn1—N3—C4—C535.8 (5)
N2—Zn1—N1—C113.1 (4)Zn1—N4—C5—C447.8 (4)
N5—Zn1—N2—C2109.9 (3)Zn1—N4—C5—C6175.2 (4)
N3—Zn1—N2—C236.8 (9)N3—C4—C5—N457.1 (6)
N4—Zn1—N2—C277.0 (3)N3—C4—C5—C6176.5 (4)
N1—Zn1—N2—C217.4 (3)N3—Zn1—N5—C784.8 (4)
N6—Zn1—N2—C2170.4 (3)N2—Zn1—N5—C7102.1 (4)
Zn1—N1—C1—C242.3 (5)N1—Zn1—N5—C7177.9 (4)
Zn1—N2—C2—C144.8 (4)N6—Zn1—N5—C78.2 (3)
Zn1—N2—C2—C3167.2 (4)N5—Zn1—N6—C819.8 (3)
N1—C1—C2—N259.8 (6)N3—Zn1—N6—C8116.0 (3)
N1—C1—C2—C3177.7 (5)N4—Zn1—N6—C8164.2 (3)
N5—Zn1—N3—C4179.4 (3)N2—Zn1—N6—C873.2 (3)
N4—Zn1—N3—C46.9 (3)Zn1—N5—C7—C836.0 (5)
N2—Zn1—N3—C434.1 (10)Zn1—N6—C8—C9168.0 (4)
N1—Zn1—N3—C487.0 (4)Zn1—N6—C8—C744.2 (5)
N6—Zn1—N3—C499.6 (3)N5—C7—C8—N654.4 (6)
N3—Zn1—N4—C522.1 (3)N5—C7—C8—C9180.0 (5)
N2—Zn1—N4—C5166.2 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···Cl2i0.902.623.457 (5)155
N1—H2···Cl10.902.543.419 (5)166
N2—H3···Cl2ii0.902.833.601 (5)144
N2—H4···O1iii0.902.303.185 (6)166
N3—H11···O2i0.902.273.133 (6)162
N3—H12···Cl2iv0.902.563.414 (5)160
N4—H14···Cl10.902.733.599 (5)162
N5—H21···Cl1i0.902.713.477 (5)144
N5—H22···O1iii0.902.343.143 (6)148
N6—H23···Cl1ii0.902.693.499 (5)150
N6—H24···Cl2iv0.902.683.553 (5)165
O1—H31···Cl10.902.323.214 (5)179
O1—H32···Cl20.902.273.166 (5)180
O2—H33···Cl10.902.263.164 (5)180
O2—H34···Cl20.902.293.186 (5)180
Symmetry codes: (i) x1/2, y+1/2, z1/2; (ii) x1/2, y+1/2, z+1/2; (iii) x1/2, y1/2, z; (iv) x1, y, z.
 

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