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The title complex, [Ni(C4H12N2)2(H2O)2]Cl2·2H2O, consists of two chloride ions, two water molecules and a complex dication. The nickel(II) center is pseudo-octahedral six-coordinate, with a trans geometry and is located on an inversion center. The coordinated water molecule hydrogen bonds to two chloride ions, as does the uncoordinated water molecule. The uncoordinated water molecule also accepts a hydrogen bond from one of the secondary amines.
Supporting information
CCDC reference: 620708
Key indicators
- Single-crystal X-ray study
- T = 110 K
- Mean (C-C) = 0.003 Å
- R factor = 0.042
- wR factor = 0.072
- Data-to-parameter ratio = 22.0
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.20 Ratio
| Author Response: see _publ_section_exptl_refinement. One methyl
group is disordered, so one set of H atoms has
a small Ueq producing a small Ueq(min).
|
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT245_ALERT_2_C U(iso) H7 Smaller than U(eq) C3 by ... 0.01 AngSq
PLAT245_ALERT_2_C U(iso) H8 Smaller than U(eq) C3 by ... 0.01 AngSq
PLAT245_ALERT_2_C U(iso) H9 Smaller than U(eq) C3 by ... 0.01 AngSq
1 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
3 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
Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: TEXSAN for Windows (Molecular Structure Corporation, 1999); molecular graphics: PROGRAM? (Reference?); software used to prepare material for publication: TEXSAN for Windows.
trans-Diaquabis(
N,
N'-dimethylethane-1,2-diamine-
κ2N,
N')nickel(II) dichloride dihydrate
top
Crystal data top
[Ni(C4H12N2)2(H2O)2]Cl2·2H2O | F(000) = 404.00 |
Mr = 377.97 | Dx = 1.395 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2530 reflections |
a = 8.7402 (15) Å | θ = 2.5–30.8° |
b = 12.788 (3) Å | µ = 1.39 mm−1 |
c = 9.011 (2) Å | T = 110 K |
β = 116.703 (13)° | Plate fragment, light purple |
V = 899.7 (3) Å3 | 0.30 × 0.15 × 0.10 mm |
Z = 2 | |
Data collection top
Nonius KappaCCD (with an Oxford Cryosystem Cryostream coller) diffractometer | 2774 independent reflections |
Radiation source: fine-focus sealed tube | 1978 reflections with I > 3.00σ(I) |
Graphite monochromator | Rint = 0.031 |
ω scans with κ offsets | θmax = 30.8°, θmin = 2.7° |
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997) | h = −12→12 |
Tmin = 0.734, Tmax = 0.874 | k = −17→18 |
13820 measured reflections | l = −12→12 |
Refinement top
Refinement on F2 | 0 constraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.042 | Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo) + 0.0004|Fo|2] |
wR(F2) = 0.072 | (Δ/σ)max = 0.0003 |
S = 0.96 | Δρmax = 0.36 e Å−3 |
1978 reflections | Δρmin = −0.42 e Å−3 |
90 parameters | Extinction correction: Zachariasen (1967), equ(3) Acta Cryst.(1968) A24, p213. |
5 restraints | Extinction coefficient: 0.0000015 (3) |
Special details top
Refinement. Refinement of F2. The weighted R-factor wR and goodness
of fit are based on F2, conventional R-factors R are
based on F. R-factors based on F2 are statistically about
twice as large as those based on F. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni1 | 0.5000 | 0.5000 | 0.5000 | 0.01018 (8) | |
Cl1 | 0.75579 (6) | 0.29715 (3) | 0.99295 (5) | 0.01708 (11) | |
O1 | 0.5687 (2) | 0.34897 (9) | 0.6114 (2) | 0.0151 (3) | |
O2 | 0.1179 (2) | 0.69451 (13) | 0.6066 (2) | 0.0366 (5) | |
N1 | 0.4107 (2) | 0.55682 (12) | 0.6653 (2) | 0.0143 (4) | |
N2 | 0.7396 (2) | 0.55849 (11) | 0.6787 (2) | 0.0148 (4) | |
C1 | 0.5448 (3) | 0.6287 (1) | 0.7800 (2) | 0.0200 (5) | |
C2 | 0.7200 (2) | 0.5815 (1) | 0.8303 (2) | 0.0185 (4) | |
C3 | 0.3590 (2) | 0.4796 (2) | 0.7566 (3) | 0.0191 (5) | |
C4 | 0.8969 (2) | 0.4970 (2) | 0.7186 (3) | 0.0216 (5) | |
H1 | 0.3127 | 0.5983 | 0.6019 | 0.017* | |
H2 | 0.7554 | 0.6240 | 0.6377 | 0.018* | |
H3 | 0.5369 | 0.6937 | 0.7258 | 0.024* | |
H4 | 0.5285 | 0.6397 | 0.8762 | 0.024* | |
H5 | 0.7307 | 0.5187 | 0.8905 | 0.022* | |
H6 | 0.8059 | 0.6295 | 0.8981 | 0.022* | |
H7 | 0.3200 | 0.4175 | 0.6926 | 0.005* | 0.21 (2) |
H8 | 0.4546 | 0.4635 | 0.8597 | 0.005* | 0.21 |
H9 | 0.2697 | 0.5078 | 0.7770 | 0.005* | 0.21 |
H10 | 0.9147 | 0.4915 | 0.6224 | 0.026* | |
H11 | 0.9922 | 0.5311 | 0.8044 | 0.026* | |
H12 | 0.8846 | 0.4291 | 0.7545 | 0.026* | |
H13 | 0.6330 | 0.3424 | 0.7270 | 0.018* | |
H14 | 0.4795 | 0.2990 | 0.5698 | 0.018* | |
H15 | 0.0142 | 0.7224 | 0.5688 | 0.044* | |
H16 | 0.1454 | 0.6965 | 0.7136 | 0.044* | |
H17 | 0.4510 | 0.4324 | 0.8144 | 0.018* | 0.79 |
H18 | 0.3314 | 0.5148 | 0.8343 | 0.018* | 0.79 |
H19 | 0.2620 | 0.4416 | 0.6807 | 0.018* | 0.79 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0097 (2) | 0.0101 (2) | 0.0096 (2) | 0.00031 (12) | 0.00333 (12) | 0.00015 (12) |
Cl1 | 0.0175 (2) | 0.0149 (2) | 0.0143 (2) | 0.0033 (2) | 0.0032 (2) | 0.0003 (2) |
O1 | 0.0153 (6) | 0.0132 (6) | 0.0130 (6) | −0.0019 (5) | 0.0030 (5) | 0.0013 (5) |
O2 | 0.0378 (9) | 0.0513 (11) | 0.0230 (8) | 0.0266 (8) | 0.0157 (7) | 0.0109 (8) |
N1 | 0.0150 (7) | 0.0151 (7) | 0.0135 (7) | 0.0029 (6) | 0.0070 (6) | 0.0019 (6) |
N2 | 0.0144 (7) | 0.0130 (7) | 0.0145 (8) | −0.0016 (6) | 0.0043 (6) | 0.0021 (6) |
C1 | 0.0296 (10) | 0.0144 (9) | 0.0157 (9) | 0.0018 (8) | 0.0100 (8) | −0.0031 (8) |
C2 | 0.0206 (9) | 0.0173 (9) | 0.0119 (9) | −0.0055 (8) | 0.0021 (7) | −0.0017 (7) |
C3 | 0.0223 (9) | 0.0206 (10) | 0.0191 (10) | 0.0032 (8) | 0.0136 (8) | 0.0032 (8) |
C4 | 0.0130 (8) | 0.0244 (10) | 0.0229 (10) | 0.0001 (8) | 0.0040 (7) | 0.0038 (8) |
Geometric parameters (Å, º) top
Ni1—O1 | 2.135 (1) | N1—H1 | 0.950 |
Ni1—O1i | 2.135 (1) | N2—H2 | 0.950 |
Ni1—N1 | 2.098 (2) | C1—H3 | 0.950 |
Ni1—N1i | 2.098 (2) | C1—H4 | 0.950 |
Ni1—N2 | 2.123 (1) | C2—H5 | 0.950 |
Ni1—N2i | 2.123 (1) | C2—H6 | 0.950 |
N1—C1 | 1.482 (2) | C3—H7 | 0.950 |
N1—C3 | 1.480 (3) | C3—H8 | 0.952 |
N2—C2 | 1.481 (3) | C3—H9 | 0.950 |
N2—C4 | 1.480 (3) | C3—H17 | 0.952 |
C1—C2 | 1.514 (3) | C3—H18 | 0.951 |
O1—H13 | 0.939 | C3—H19 | 0.949 |
O1—H14 | 0.946 | C4—H10 | 0.950 |
O2—H15 | 0.887 | C4—H11 | 0.950 |
O2—H16 | 0.882 | C4—H12 | 0.950 |
| | | |
Cl1···O1ii | 3.080 (1) | O2···N1 | 2.952 (2) |
Cl1···O1 | 3.144 (2) | O2···C3 | 3.356 (3) |
Cl1···O2iii | 3.250 (2) | O2···C1 | 3.439 (3) |
Cl1···O2iv | 3.266 (2) | O2···C1vi | 3.534 (3) |
Cl1···N2v | 3.430 (2) | O2···C4vii | 3.589 (3) |
| | | |
O1—Ni1—O1i | 180.00 | C2—N2—H2 | 106.33 |
O1—Ni1—N1 | 95.46 (6) | C4—N2—H2 | 106.33 |
O1—Ni1—N1i | 84.54 (6) | N1—C1—H3 | 109.41 |
O1—Ni1—N2 | 89.37 (5) | N1—C1—H4 | 109.41 |
O1—Ni1—N2i | 90.63 (5) | C2—C1—H3 | 109.41 |
O1i—Ni1—N1 | 84.54 (6) | C2—C1—H4 | 109.41 |
O1i—Ni1—N1i | 95.46 (6) | H3—C1—H4 | 109.46 |
O1i—Ni1—N2 | 90.63 (5) | N2—C2—H5 | 109.61 |
O1i—Ni1—N2i | 89.37 (5) | N2—C2—H6 | 109.61 |
N1—Ni1—N1i | 180.00 | C1—C2—H5 | 109.61 |
N1—Ni1—N2 | 83.92 (6) | C1—C2—H6 | 109.62 |
N1—Ni1—N2i | 96.08 (6) | H5—C2—H6 | 109.46 |
N1i—Ni1—N2 | 96.08 (6) | N1—C3—H7 | 109.68 |
N1i—Ni1—N2i | 83.92 (6) | N1—C3—H8 | 109.46 |
N2—Ni1—N2i | 180.00 | N1—C3—H9 | 109.67 |
Ni1—N1—C1 | 106.3 (1) | N1—C3—H17 | 109.49 |
Ni1—N1—C3 | 117.9 (1) | N1—C3—H18 | 109.58 |
C1—N1—C3 | 111.7 (1) | N1—C3—H19 | 109.74 |
Ni1—N2—C2 | 106.6 (1) | H7—C3—H8 | 109.26 |
Ni1—N2—C4 | 119.3 (1) | H7—C3—H9 | 109.47 |
C2—N2—C4 | 111.2 (1) | H8—C3—H9 | 109.29 |
N1—C1—C2 | 109.7 (2) | H17—C3—H18 | 109.23 |
N2—C2—C1 | 108.9 (1) | H17—C3—H19 | 109.34 |
Ni1—O1—H13 | 120.31 | H18—C3—H19 | 109.45 |
Ni1—O1—H14 | 114.71 | N2—C4—H10 | 109.47 |
H13—O1—H14 | 110.77 | N2—C4—H11 | 109.47 |
H15—O2—H16 | 97.91 | N2—C4—H12 | 109.47 |
Ni1—N1—H1 | 106.80 | H10—C4—H11 | 109.47 |
C1—N1—H1 | 106.80 | H10—C4—H12 | 109.47 |
C3—N1—H1 | 106.80 | H11—C4—H12 | 109.47 |
Ni1—N2—H2 | 106.33 | | |
| | | |
Ni1—N1—C1—C2 | −42.2 (2) | N1—Ni1—N2—C2 | 13.1 (1) |
Ni1—N1i—C1i—C2i | 42.2 (2) | N1—Ni1—N2—C4 | 140.0 (2) |
Ni1—N2—C2—C1 | −39.5 (2) | N1—Ni1—N2i—C2i | 166.9 (1) |
Ni1—N2i—C2i—C1i | 39.5 (2) | N1—Ni1—N2i—C4i | 40.0 (2) |
O1—Ni1—N1—C1 | 104.5 (1) | N1—C1—C2—N2 | 56.4 (2) |
O1—Ni1—N1—C3 | −21.6 (1) | N2—Ni1—N1—C1 | 15.7 (1) |
O1—Ni1—N1i—C1i | 75.5 (1) | N2—Ni1—N1—C3 | −110.4 (1) |
O1—Ni1—N1i—C3i | −158.4 (1) | N2—Ni1—N1i—C1i | 164.3 (1) |
O1—Ni1—N2—C2 | −82.4 (1) | N2—Ni1—N1i—C3i | −69.6 (1) |
O1—Ni1—N2—C4 | 44.4 (2) | C1—C2—N2—C4 | −171.0 (1) |
O1—Ni1—N2i—C2i | −97.6 (1) | C2—C1—N1—C3 | 87.6 (2) |
O1—Ni1—N2i—C4i | 135.6 (2) | | |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1/2, −y+1/2, z+1/2; (iii) −x+1/2, y−1/2, −z+3/2; (iv) −x+1, −y+1, −z+2; (v) −x+3/2, y−1/2, −z+3/2; (vi) x−1/2, −y+3/2, z−1/2; (vii) x−1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H13···Cl1 | 0.94 | 2.22 | 3.144 (2) | 168 |
O1—H14···Cl1viii | 0.95 | 2.14 | 3.080 (1) | 170 |
O2—H15···Cl1ix | 0.89 | 2.37 | 3.250 (2) | 172 |
O2—H16···Cl1iv | 0.88 | 2.39 | 3.266 (2) | 175 |
N1—H1···O2 | 0.95 | 2.12 | 2.952 (2) | 146 |
N2—H2···Cl1x | 0.95 | 2.49 | 3.430 (2) | 170 |
Symmetry codes: (iv) −x+1, −y+1, −z+2; (viii) x−1/2, −y+1/2, z−1/2; (ix) −x+1/2, y+1/2, −z+3/2; (x) −x+3/2, y+1/2, −z+3/2. |
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