mer-Bis(diethyl­enetriamine)zinc(II) dichloride monohydrate

In the title compound, [Zn(C₄H₁₃N₃)₂]Cl₂·H₂O, the Zn^II atom is coordinated by six N atoms from two diethyl­enetriamine ligands in a distorted octa­hedral geometry. The complex cation is the mer isomer.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.041
• wR factor = 0.081
• Data-to-parameter ratio = 17.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT420_ALERT_2_C D-H Without Acceptor       N4     -   H4A    ...          ?
PLAT420_ALERT_2_C D-H Without Acceptor       N4     -   H4B    ...          ?
PLAT480_ALERT_4_C Long H...A H-Bond Reported H4B    ..  CL1     ..       2.95 Ang.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   4 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1999); software used to prepare material for publication: SHELXTL/PC.

mer-Bis(diethylenetriamine)zinc(II) dichloride monohydrate

Crystal data

[Zn(C4H13N3)2]Cl2·H2O	F(000) = 760
Mr = 360.63	Dx = 1.486 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1897 reflections
a = 13.436 (4) Å	θ = 2.8–22.9°
b = 8.811 (2) Å	µ = 1.86 mm^−1
c = 13.924 (4) Å	T = 298 K
β = 102.030 (4)°	Block, colourless
V = 1612.2 (8) Å^3	0.20 × 0.20 × 0.10 mm
Z = 4

Data collection

SMART 1K CCD area-detector diffractometer	2862 independent reflections
Radiation source: fine-focus sealed tube	2166 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.037
φ and ω scans	θmax = 25.1°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→16
Tmin = 0.708, Tmax = 0.836	k = −9→10
7671 measured reflections	l = −8→16

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.081	H-atom parameters constrained
S = 0.95	w = 1/[σ^2(Fo^2) + (0.0324P)^2] where P = (Fo^2 + 2Fc^2)/3
2862 reflections	(Δ/σ)max < 0.001
163 parameters	Δρmax = 0.48 e Å^−3
3 restraints	Δρmin = −0.36 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.76137 (3)	0.38861 (4)	0.56388 (3)	0.03289 (14)
N1	0.6110 (2)	0.3313 (3)	0.5853 (2)	0.0420 (8)
H1A	0.5951	0.3897	0.6330	0.063*
H1B	0.5647	0.3482	0.5296	0.063*
N2	0.77669 (19)	0.1469 (3)	0.5768 (2)	0.0355 (7)
H2	0.8088	0.1244	0.6394	0.053*
N3	0.91525 (19)	0.3559 (3)	0.5305 (2)	0.0394 (8)
H3A	0.9162	0.3922	0.4703	0.059*
H3B	0.9622	0.4064	0.5745	0.059*
N4	0.8318 (2)	0.4504 (3)	0.7170 (2)	0.0531 (9)
H4A	0.7993	0.4028	0.7588	0.080*
H4B	0.8975	0.4215	0.7309	0.080*
N5	0.74671 (19)	0.6301 (3)	0.5564 (2)	0.0361 (7)
H5	0.6857	0.6553	0.5706	0.054*
N6	0.7032 (2)	0.4188 (3)	0.4027 (2)	0.0368 (7)
H6A	0.7521	0.3956	0.3697	0.055*
H6B	0.6494	0.3577	0.3815	0.055*
O1	0.6146 (2)	0.0398 (3)	0.2982 (2)	0.0701 (9)
H30	0.5698	0.0957	0.3131	0.084*
H31	0.5875	−0.0366	0.2677	0.084*
C1	0.6095 (3)	0.1704 (4)	0.6129 (3)	0.0488 (10)
H1C	0.5402	0.1325	0.5969	0.073*
H1D	0.6345	0.1596	0.6831	0.073*
C2	0.6748 (2)	0.0801 (4)	0.5590 (3)	0.0439 (10)
H2A	0.6788	−0.0243	0.5816	0.066*
H2B	0.6454	0.0807	0.4892	0.066*
C3	0.8421 (3)	0.1010 (4)	0.5111 (3)	0.0460 (10)
H3C	0.8080	0.1184	0.4435	0.069*
H3D	0.8577	−0.0063	0.5193	0.069*
C4	0.9385 (3)	0.1922 (4)	0.5350 (3)	0.0512 (11)
H4C	0.9759	0.1662	0.6003	0.077*
H4D	0.9810	0.1681	0.4886	0.077*
C5	0.8245 (3)	0.6154 (4)	0.7281 (3)	0.0495 (10)
H5A	0.8807	0.6508	0.7785	0.074*
H5B	0.7616	0.6402	0.7484	0.074*
C6	0.8269 (3)	0.6931 (4)	0.6330 (3)	0.0461 (10)
H6C	0.8165	0.8013	0.6392	0.069*
H6D	0.8927	0.6778	0.6161	0.069*
C10	0.7458 (3)	0.6781 (4)	0.4555 (3)	0.0456 (10)
H7A	0.8136	0.6695	0.4421	0.068*
H7B	0.7244	0.7832	0.4466	0.068*
C11	0.6732 (3)	0.5782 (4)	0.3867 (3)	0.0461 (10)
H8A	0.6048	0.5921	0.3976	0.069*
H8B	0.6732	0.6063	0.3193	0.069*
Cl1	0.90783 (7)	0.05033 (12)	0.79676 (7)	0.0513 (3)
Cl2	0.53831 (6)	0.77924 (11)	0.14035 (8)	0.0512 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0343 (2)	0.0320 (2)	0.0324 (3)	−0.00201 (19)	0.00711 (19)	−0.0008 (2)
N1	0.0400 (18)	0.0450 (19)	0.045 (2)	−0.0024 (14)	0.0185 (16)	−0.0060 (16)
N2	0.0322 (17)	0.0355 (17)	0.0367 (19)	−0.0024 (13)	0.0020 (15)	0.0061 (14)
N3	0.0336 (16)	0.0434 (19)	0.0409 (19)	−0.0063 (13)	0.0071 (15)	0.0009 (15)
N4	0.069 (2)	0.055 (2)	0.0331 (19)	−0.0067 (17)	0.0054 (18)	−0.0009 (16)
N5	0.0287 (16)	0.0367 (18)	0.0429 (19)	0.0012 (13)	0.0078 (15)	−0.0055 (15)
N6	0.0330 (16)	0.0431 (19)	0.0336 (18)	−0.0031 (13)	0.0050 (14)	0.0010 (15)
O1	0.0710 (19)	0.079 (2)	0.066 (2)	0.0001 (16)	0.0269 (18)	−0.0177 (17)
C1	0.043 (2)	0.058 (3)	0.049 (3)	−0.0112 (19)	0.016 (2)	0.009 (2)
C2	0.044 (2)	0.035 (2)	0.053 (3)	−0.0067 (17)	0.013 (2)	0.0037 (19)
C3	0.048 (2)	0.036 (2)	0.057 (3)	0.0027 (18)	0.018 (2)	0.001 (2)
C4	0.036 (2)	0.052 (3)	0.067 (3)	0.0093 (19)	0.015 (2)	0.007 (2)
C5	0.044 (2)	0.061 (3)	0.042 (3)	−0.005 (2)	0.004 (2)	−0.021 (2)
C6	0.041 (2)	0.038 (2)	0.056 (3)	−0.0077 (18)	0.003 (2)	−0.010 (2)
C10	0.051 (2)	0.036 (2)	0.050 (3)	0.0004 (18)	0.011 (2)	0.006 (2)
C11	0.041 (2)	0.053 (3)	0.041 (2)	0.0059 (18)	0.002 (2)	0.010 (2)
Cl1	0.0411 (5)	0.0748 (7)	0.0380 (6)	0.0032 (5)	0.0079 (5)	0.0054 (5)
Cl2	0.0392 (5)	0.0555 (6)	0.0575 (7)	0.0002 (5)	0.0067 (5)	0.0053 (5)

Geometric parameters (Å, º)

Zn1—N1	2.162 (3)	C3—H3D	0.9700
Zn1—N2	2.144 (3)	N4—C5	1.467 (4)
Zn1—N3	2.230 (3)	N4—H4A	0.9000
Zn1—N4	2.212 (3)	N4—H4B	0.9000
Zn1—N5	2.137 (3)	C10—C11	1.502 (5)
Zn1—N6	2.233 (3)	C10—H7A	0.9700
N2—C3	1.452 (4)	C10—H7B	0.9700
N2—C2	1.463 (4)	C5—C6	1.497 (5)
N2—H2	0.9100	C5—H5A	0.9700
N6—C11	1.466 (4)	C5—H5B	0.9700
N6—H6A	0.9000	C1—C2	1.497 (5)
N6—H6B	0.9000	C1—H1C	0.9700
N1—C1	1.470 (4)	C1—H1D	0.9700
N1—H1A	0.9000	C6—H6C	0.9700
N1—H1B	0.9000	C6—H6D	0.9700
N3—C4	1.475 (4)	C2—H2A	0.9700
N3—H3A	0.9000	C2—H2B	0.9700
N3—H3B	0.9000	C4—H4C	0.9700
N5—C6	1.459 (4)	C4—H4D	0.9700
N5—C10	1.464 (4)	C11—H8A	0.9700
N5—H5	0.9100	C11—H8B	0.9700
C3—C4	1.502 (5)	O1—H30	0.8367
C3—H3C	0.9700	O1—H31	0.8375
N1—Zn1—N2	80.36 (10)	H3C—C3—H3D	108.3
N1—Zn1—N3	158.71 (11)	C5—N4—Zn1	108.7 (2)
N1—Zn1—N4	98.55 (12)	C5—N4—H4A	110.0
N1—Zn1—N5	99.21 (10)	Zn1—N4—H4A	110.0
N1—Zn1—N6	91.43 (11)	C5—N4—H4B	110.0
N2—Zn1—N3	79.17 (10)	Zn1—N4—H4B	110.0
N2—Zn1—N4	98.59 (11)	H4A—N4—H4B	108.3
N2—Zn1—N5	178.02 (11)	N5—C10—C11	108.5 (3)
N2—Zn1—N6	102.12 (10)	N5—C10—H7A	110.0
N3—Zn1—N4	90.22 (11)	C11—C10—H7A	110.0
N3—Zn1—N5	101.44 (10)	N5—C10—H7B	110.0
N3—Zn1—N6	87.22 (10)	C11—C10—H7B	110.0
N4—Zn1—N5	79.55 (11)	H7A—C10—H7B	108.4
N4—Zn1—N6	158.25 (11)	N4—C5—C6	110.3 (3)
N5—Zn1—N6	79.80 (10)	N4—C5—H5A	109.6
C3—N2—C2	116.7 (3)	C6—C5—H5A	109.6
C3—N2—Zn1	106.5 (2)	N4—C5—H5B	109.6
C2—N2—Zn1	108.4 (2)	C6—C5—H5B	109.6
C3—N2—H2	108.3	H5A—C5—H5B	108.1
C2—N2—H2	108.3	N1—C1—C2	109.8 (3)
Zn1—N2—H2	108.3	N1—C1—H1C	109.7
C11—N6—Zn1	107.1 (2)	C2—C1—H1C	109.7
C11—N6—H6A	110.3	N1—C1—H1D	109.7
Zn1—N6—H6A	110.3	C2—C1—H1D	109.7
C11—N6—H6B	110.3	H1C—C1—H1D	108.2
Zn1—N6—H6B	110.3	N5—C6—C5	108.9 (3)
H6A—N6—H6B	108.5	N5—C6—H6C	109.9
C1—N1—Zn1	109.0 (2)	C5—C6—H6C	109.9
C1—N1—H1A	109.9	N5—C6—H6D	109.9
Zn1—N1—H1A	109.9	C5—C6—H6D	109.9
C1—N1—H1B	109.9	H6C—C6—H6D	108.3
Zn1—N1—H1B	109.9	N2—C2—C1	109.1 (3)
H1A—N1—H1B	108.3	N2—C2—H2A	109.9
C4—N3—Zn1	108.39 (19)	C1—C2—H2A	109.9
C4—N3—H3A	110.0	N2—C2—H2B	109.9
Zn1—N3—H3A	110.0	C1—C2—H2B	109.9
C4—N3—H3B	110.0	H2A—C2—H2B	108.3
Zn1—N3—H3B	110.0	N3—C4—C3	110.4 (3)
H3A—N3—H3B	108.4	N3—C4—H4C	109.6
C6—N5—C10	116.7 (3)	C3—C4—H4C	109.6
C6—N5—Zn1	107.3 (2)	N3—C4—H4D	109.6
C10—N5—Zn1	108.5 (2)	C3—C4—H4D	109.6
C6—N5—H5	108.1	H4C—C4—H4D	108.1
C10—N5—H5	108.1	N6—C11—C10	110.0 (3)
Zn1—N5—H5	108.1	N6—C11—H8A	109.7
N2—C3—C4	108.6 (3)	C10—C11—H8A	109.7
N2—C3—H3C	110.0	N6—C11—H8B	109.7
C4—C3—H3C	110.0	C10—C11—H8B	109.7
N2—C3—H3D	110.0	H8A—C11—H8B	108.2
C4—C3—H3D	110.0	H30—O1—H31	109.8

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O1^i	0.90	2.34	3.166 (4)	152
N1—H1B···Cl2^ii	0.90	2.55	3.388 (3)	155
N2—H2···Cl1	0.91	2.40	3.311 (3)	174
N3—H3A···Cl1^iii	0.90	2.45	3.339 (3)	171
N3—H3B···Cl1^iv	0.90	2.56	3.462 (3)	178
N4—H4B···Cl1^iv	0.90	2.95	3.651 (3)	136
N5—H5···Cl2^v	0.91	2.45	3.348 (3)	169
N6—H6A···Cl1^iii	0.90	2.55	3.391 (3)	155
N6—H6B···Cl2^ii	0.90	2.57	3.404 (3)	154
O1—H30···Cl2^ii	0.84	2.35	3.184 (3)	172
O1—H31···Cl2^vi	0.84	2.39	3.196 (3)	161

Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x+1, y−1/2, −z+1/2; (iii) x, −y+1/2, z−1/2; (iv) −x+2, y+1/2, −z+3/2; (v) x, −y+3/2, z+1/2; (vi) x, y−1, z.