Diaqua­(ethyl­enediamine)(N,N,N',N'-tetra­methyl­ethylenediamine)nickel(II) dichloride dihydrate

In the title compound, [Ni(C₂H₈N₂)(C₆H₁₆N₂)(H₂O)₂]Cl₂·2H₂O, the Ni^II ion, located on a twofold axis, is coordinated by four N atoms of the ethyl­enediamine and N,N,N',N'-tetra­methyl­ethylenediamine ligands and two water mol­ecules in a distorted octa­hedral geometry. Hydrogen bonds between ethyl­enediamine, water mol­ecules and chloride ions help to construct a three-dimensional supra­molecular architecture.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.009 Å
• R factor = 0.038
• wR factor = 0.112
• Data-to-parameter ratio = 17.5

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for         N2

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   2 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
   1 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

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Computing details

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

Diaqua(ethylenediamine)(N,N,N',N'-tetramethylethylenediamine)nickel(II) dichloride dihydrate

Crystal data

[Ni(C2H8N2)(C6H16N2)(H2O)2]Cl2·2H2O	F(000) = 808
Mr = 377.99	Dx = 1.395 Mg m^−3
Orthorhombic, Pbcn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2ab	Cell parameters from 3938 reflections
a = 15.005 (4) Å	θ = 2.5–28.2°
b = 9.591 (3) Å	µ = 1.39 mm^−1
c = 12.505 (3) Å	T = 298 K
V = 1799.6 (9) Å^3	Block, blue
Z = 4	0.35 × 0.33 × 0.21 mm

Data collection

Bruker SMART CCD area-detector diffractometer	1593 independent reflections
Radiation source: fine-focus sealed tube	1303 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.028
φ and ω scans	θmax = 25.0°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Bruker, 1998)	h = −8→17
Tmin = 0.629, Tmax = 0.744	k = −11→11
8632 measured reflections	l = −14→14

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.038	H-atom parameters constrained
wR(F^2) = 0.112	w = 1/[σ^2(Fo^2) + (0.0503P)^2 + 3.0865P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
1593 reflections	Δρmax = 0.77 e Å^−3
91 parameters	Δρmin = −0.89 e Å^−3
3 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0173 (16)

Special details

Experimental. The IUCr checkCIF software suggested the possibility of lattice centering or cell halving. But we were unable to see any evidence for these from the reflection data.

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
Ni1	0.5000	0.69497 (6)	0.7500	0.0262 (3)
Cl1	0.84573 (8)	0.34314 (12)	0.47700 (10)	0.0538 (4)
N1	0.5918 (2)	0.8592 (4)	0.7363 (3)	0.0407 (8)
H1A	0.6238	0.8666	0.7968	0.049*
H1B	0.6295	0.8425	0.6818	0.049*
N2	0.5960 (2)	0.5270 (3)	0.7387 (3)	0.0373 (8)
O1	0.51356 (17)	0.7004 (3)	0.9207 (2)	0.0370 (7)
H5	0.5612	0.7395	0.9421	0.055*
H6	0.4714	0.7435	0.9518	0.055*
O2	0.8352 (2)	0.6691 (4)	0.4835 (4)	0.0774 (13)
H7	0.8299	0.5809	0.4839	0.116*
H8	0.7831	0.7040	0.4826	0.116*
C1	0.5423 (4)	0.9892 (5)	0.7168 (5)	0.0602 (13)
H1C	0.5275	0.9967	0.6415	0.072*
H1D	0.5790	1.0687	0.7360	0.072*
C2	0.5491 (4)	0.4059 (5)	0.7612 (6)	0.101 (3)
H2A	0.5575	0.3845	0.8363	0.121*
H2B	0.5758	0.3306	0.7205	0.121*
C3	0.6655 (4)	0.5337 (7)	0.8172 (5)	0.092 (2)
H3A	0.6397	0.5463	0.8868	0.138*
H3B	0.7042	0.6107	0.8014	0.138*
H3C	0.6991	0.4485	0.8160	0.138*
C4	0.6345 (4)	0.5086 (6)	0.6346 (4)	0.0802 (19)
H4A	0.6725	0.4280	0.6350	0.120*
H4B	0.6689	0.5895	0.6163	0.120*
H4C	0.5879	0.4958	0.5829	0.120*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0255 (4)	0.0248 (4)	0.0284 (4)	0.000	−0.0009 (3)	0.000
Cl1	0.0490 (7)	0.0515 (7)	0.0610 (7)	0.0052 (5)	−0.0167 (5)	0.0009 (5)
N1	0.0393 (19)	0.0419 (19)	0.0409 (19)	−0.0104 (16)	0.0011 (15)	−0.0019 (15)
N2	0.0401 (18)	0.0324 (18)	0.0393 (18)	0.0097 (15)	−0.0030 (14)	−0.0025 (14)
O1	0.0352 (15)	0.0413 (16)	0.0344 (15)	0.0023 (12)	−0.0029 (12)	−0.0030 (12)
O2	0.047 (2)	0.049 (2)	0.137 (4)	−0.0015 (16)	0.024 (2)	0.021 (2)
C1	0.082 (4)	0.032 (2)	0.067 (3)	−0.012 (3)	0.015 (3)	0.003 (2)
C2	0.071 (4)	0.037 (3)	0.196 (9)	0.019 (3)	0.003 (5)	0.012 (4)
C3	0.081 (4)	0.115 (5)	0.080 (4)	0.062 (4)	−0.042 (3)	−0.036 (4)
C4	0.099 (4)	0.084 (4)	0.057 (3)	0.052 (4)	0.021 (3)	0.001 (3)

Geometric parameters (Å, º)

Ni1—N1	2.099 (3)	O2—H7	0.85
Ni1—N1^i	2.099 (3)	O2—H8	0.85
Ni1—O1	2.145 (3)	C1—C1^i	1.518 (10)
Ni1—O1^i	2.145 (3)	C1—H1C	0.97
Ni1—N2^i	2.166 (3)	C1—H1D	0.97
Ni1—N2	2.166 (3)	C2—C2^i	1.500 (12)
N1—C1	1.472 (6)	C2—H2A	0.97
N1—H1A	0.90	C2—H2B	0.97
N1—H1B	0.90	C3—H3A	0.96
N2—C2	1.387 (6)	C3—H3B	0.96
N2—C3	1.433 (6)	C3—H3C	0.96
N2—C4	1.435 (6)	C4—H4A	0.96
O1—H5	0.85	C4—H4B	0.96
O1—H6	0.85	C4—H4C	0.96
N1—Ni1—N1^i	82.8 (2)	Ni1—O1—H6	113.4
N1—Ni1—O1	90.06 (12)	H5—O1—H6	105.4
N1^i—Ni1—O1	87.85 (11)	H7—O2—H8	107.7
N1—Ni1—O1^i	87.85 (12)	N1—C1—C1^i	109.3 (3)
N1^i—Ni1—O1^i	90.06 (12)	N1—C1—H1C	109.8
O1—Ni1—O1^i	177.21 (15)	C1^i—C1—H1C	109.8
N1—Ni1—N2^i	178.84 (13)	N1—C1—H1D	109.8
N1^i—Ni1—N2^i	96.68 (14)	C1^i—C1—H1D	109.8
O1—Ni1—N2^i	90.93 (11)	H1C—C1—H1D	108.3
O1^i—Ni1—N2^i	91.15 (11)	N2—C2—C2^i	117.5 (4)
N1—Ni1—N2	96.68 (14)	N2—C2—H2A	107.9
N1^i—Ni1—N2	178.84 (13)	C2^i—C2—H2A	107.9
O1—Ni1—N2	91.15 (11)	N2—C2—H2B	107.9
O1^i—Ni1—N2	90.93 (11)	C2^i—C2—H2B	107.9
N2^i—Ni1—N2	83.90 (19)	H2A—C2—H2B	107.2
C1—N1—Ni1	108.6 (3)	N2—C3—H3A	109.5
C1—N1—H1A	110.0	N2—C3—H3B	109.5
Ni1—N1—H1A	110.0	H3A—C3—H3B	109.5
C1—N1—H1B	110.0	N2—C3—H3C	109.5
Ni1—N1—H1B	110.0	H3A—C3—H3C	109.5
H1A—N1—H1B	108.3	H3B—C3—H3C	109.5
C2—N2—C3	105.5 (4)	N2—C4—H4A	109.5
C2—N2—C4	106.6 (4)	N2—C4—H4B	109.5
C3—N2—C4	109.5 (4)	H4A—C4—H4B	109.5
C2—N2—Ni1	105.8 (3)	N2—C4—H4C	109.5
C3—N2—Ni1	114.0 (3)	H4A—C4—H4C	109.5
C4—N2—Ni1	114.8 (3)	H4B—C4—H4C	109.5
Ni1—O1—H5	113.9
N1^i—Ni1—N1—C1	−13.8 (2)	O1^i—Ni1—N2—C3	144.4 (4)
O1—Ni1—N1—C1	−101.7 (3)	N2^i—Ni1—N2—C3	−124.6 (4)
O1^i—Ni1—N1—C1	76.5 (3)	N1—Ni1—N2—C4	−70.9 (4)
N2—Ni1—N1—C1	167.2 (3)	O1—Ni1—N2—C4	−161.1 (4)
N1—Ni1—N2—C2	171.9 (4)	O1^i—Ni1—N2—C4	17.0 (4)
O1—Ni1—N2—C2	81.7 (4)	N2^i—Ni1—N2—C4	108.1 (4)
O1^i—Ni1—N2—C2	−100.1 (4)	Ni1—N1—C1—C1^i	38.6 (6)
N2^i—Ni1—N2—C2	−9.1 (3)	C3—N2—C2—C2^i	147.2 (8)
N1—Ni1—N2—C3	56.5 (4)	C4—N2—C2—C2^i	−96.4 (8)
O1—Ni1—N2—C3	−33.7 (4)	Ni1—N2—C2—C2^i	26.1 (9)

Symmetry code: (i) −x+1, y, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H7···Cl1	0.85	2.29	3.132 (4)	168
O2—H8···Cl1^ii	0.85	2.35	3.188 (4)	168
O1—H6···Cl1^iii	0.85	2.29	3.139 (3)	173
O1—H5···O2^iv	0.85	1.86	2.707 (4)	177
N1—H1B···Cl1^ii	0.90	2.59	3.378 (4)	147
N1—H1A···O2^iv	0.90	2.44	3.291 (6)	158

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