Hexa­aqua­nickel(II) dichloride bis­(hexa­methyl­enetetr­amine) tetrahydrate

In the title compound, [Ni(H₂O)₆]Cl₂·2C₆H₁₂N₄·4H₂O, the Ni^II atom lies on a center of inversion, and is coordinated by six O atoms from six water mol­ecules, in a slightly distorted octahedral geometry. In the crystal structure, O, N and Cl atoms act as acceptors (A) to form intermolecular O—H...A hydrogen bonds, giving a three-dimensional network.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](Ni-O) = 0.002 Å
• R factor = 0.031
• wR factor = 0.089
• Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.98

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        Ni1
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .      49.00 A   3  

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   3 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

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Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

(I)

Crystal data

[Ni(H2O)6]Cl2·2C6H12N4·4H2O	Z = 1
Mr = 590.14	F(000) = 314
Triclinic, P1	Dx = 1.411 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.330 (6) Å	Cell parameters from 2777 reflections
b = 9.411 (6) Å	θ = 2.5–26.3°
c = 9.446 (6) Å	µ = 0.95 mm^−1
α = 119.551 (7)°	T = 293 K
β = 94.192 (8)°	Block, blue
γ = 100.990 (8)°	0.46 × 0.32 × 0.18 mm
V = 694.6 (8) Å^3

Data collection

Bruker SMART-CCD area-detector diffractometer	2418 independent reflections
Radiation source: fine-focus sealed tube	2216 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
φ and ω scans	θmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→11
Tmin = 0.670, Tmax = 0.848	k = −10→11
3644 measured reflections	l = −11→10

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)] = 0.031	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.089	w = 1/[σ^2(Fo^2) + (0.0606P)^2 + 0.0662P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
2418 reflections	Δρmax = 0.35 e Å^−3
204 parameters	Δρmin = −0.49 e Å^−3
0 restraints	Extinction correction: SHELXTL (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.059 (5)

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
Ni1	0.5000	0.5000	0.5000	0.02892 (16)
O1	0.3831 (2)	0.6342 (2)	0.4429 (2)	0.0450 (4)
H1	0.380 (3)	0.723 (4)	0.510 (4)	0.053 (8)*
H2	0.305 (3)	0.595 (3)	0.369 (4)	0.059 (8)*
O2	0.6415 (2)	0.5275 (2)	0.3532 (2)	0.0520 (4)
H3	0.632 (4)	0.579 (4)	0.314 (4)	0.076 (10)*
H4	0.684 (4)	0.456 (4)	0.288 (4)	0.080 (10)*
O3	0.6186 (2)	0.7235 (2)	0.69897 (19)	0.0515 (4)
H5	0.613 (3)	0.746 (4)	0.797 (4)	0.065 (8)*
H6	0.671 (3)	0.790 (4)	0.699 (4)	0.059 (9)*
N1	0.6580 (2)	1.0478 (2)	0.3272 (2)	0.0379 (4)
N2	0.6660 (2)	0.7597 (2)	0.2449 (2)	0.0391 (4)
N3	0.88469 (19)	0.9576 (2)	0.2560 (2)	0.0402 (4)
N4	0.6640 (2)	0.8457 (2)	0.0398 (2)	0.0390 (4)
C1	0.6077 (2)	0.9045 (3)	0.3516 (3)	0.0411 (5)
H11	0.4998	0.8690	0.3268	0.041 (6)*
H12	0.6407	0.9410	0.4669	0.049 (6)*
C2	0.8220 (2)	1.0986 (3)	0.3625 (3)	0.0435 (5)
H13	0.8582	1.1379	0.4780	0.055 (7)*
H14	0.8561	1.1918	0.3451	0.044 (6)*
C3	0.6057 (2)	0.9880 (3)	0.1507 (3)	0.0403 (5)
H15	0.4977	0.9528	0.1249	0.041 (6)*
H16	0.6374	1.0805	0.1317	0.036 (5)*
C4	0.8296 (2)	0.8163 (3)	0.2823 (3)	0.0433 (5)
H17	0.8691	0.7222	0.2120	0.048 (6)*
H18	0.8656	0.8519	0.3968	0.038 (6)*
C5	0.8272 (2)	0.9006 (3)	0.0816 (3)	0.0435 (5)
H19	0.8614	0.9925	0.0623	0.046 (6)*
H20	0.8668	0.8075	0.0093	0.042 (6)*
C6	0.6137 (2)	0.7066 (3)	0.0710 (3)	0.0410 (5)
H21	0.5057	0.6698	0.0448	0.045 (6)*
H22	0.6510	0.6113	−0.0013	0.050 (6)*
Cl1	0.81052 (7)	0.32527 (8)	0.06497 (8)	0.0593 (2)
O4	0.1488 (3)	0.5523 (4)	0.2005 (3)	0.0813 (7)
H7	0.165 (5)	0.585 (5)	0.129 (6)	0.114 (15)*
H8	0.068 (5)	0.496 (6)	0.174 (5)	0.106 (16)*
O5	0.8033 (2)	0.9976 (2)	0.7221 (2)	0.0518 (4)
H9	0.889 (4)	1.002 (4)	0.732 (4)	0.061 (9)*
H10	0.800 (4)	1.078 (5)	0.812 (5)	0.089 (12)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0391 (2)	0.0253 (2)	0.0249 (2)	0.01100 (14)	0.00910 (14)	0.01362 (15)
O1	0.0572 (10)	0.0356 (9)	0.0394 (8)	0.0216 (7)	0.0015 (7)	0.0153 (7)
O2	0.0749 (12)	0.0528 (10)	0.0612 (10)	0.0366 (9)	0.0443 (9)	0.0426 (9)
O3	0.0754 (12)	0.0348 (9)	0.0287 (8)	−0.0069 (8)	0.0047 (7)	0.0131 (7)
N1	0.0456 (10)	0.0344 (9)	0.0338 (8)	0.0174 (7)	0.0070 (7)	0.0154 (7)
N2	0.0481 (10)	0.0385 (9)	0.0441 (9)	0.0191 (8)	0.0193 (8)	0.0272 (8)
N3	0.0405 (9)	0.0386 (9)	0.0393 (9)	0.0119 (7)	0.0089 (7)	0.0180 (8)
N4	0.0471 (10)	0.0366 (9)	0.0311 (8)	0.0058 (7)	0.0076 (7)	0.0176 (7)
C1	0.0472 (12)	0.0502 (12)	0.0377 (10)	0.0228 (10)	0.0187 (9)	0.0266 (10)
C2	0.0469 (12)	0.0343 (11)	0.0383 (10)	0.0107 (9)	0.0014 (9)	0.0116 (9)
C3	0.0458 (12)	0.0390 (11)	0.0407 (10)	0.0100 (9)	0.0029 (9)	0.0251 (9)
C4	0.0505 (12)	0.0461 (12)	0.0468 (11)	0.0258 (10)	0.0171 (10)	0.0283 (10)
C5	0.0529 (13)	0.0410 (12)	0.0389 (11)	0.0093 (9)	0.0180 (9)	0.0222 (10)
C6	0.0479 (12)	0.0314 (10)	0.0408 (10)	0.0069 (9)	0.0133 (9)	0.0171 (9)
Cl1	0.0655 (4)	0.0484 (4)	0.0601 (4)	0.0163 (3)	0.0287 (3)	0.0226 (3)
O4	0.0682 (15)	0.0957 (17)	0.0812 (15)	0.0066 (13)	−0.0120 (12)	0.0552 (14)
O5	0.0442 (10)	0.0488 (10)	0.0489 (10)	0.0023 (7)	0.0079 (8)	0.0191 (9)

Geometric parameters (Å, º)

Ni1—O3^i	2.0227 (18)	N3—C4	1.476 (3)
Ni1—O3	2.0227 (18)	N4—C5	1.467 (3)
Ni1—O1	2.0460 (17)	N4—C3	1.471 (3)
Ni1—O1^i	2.0460 (17)	N4—C6	1.478 (3)
Ni1—O2	2.0554 (18)	C1—H11	0.9700
Ni1—O2^i	2.0554 (18)	C1—H12	0.9700
O1—H1	0.77 (3)	C2—H13	0.9700
O1—H2	0.85 (3)	C2—H14	0.9700
O2—H3	0.76 (4)	C3—H15	0.9700
O2—H4	0.84 (4)	C3—H16	0.9700
O3—H5	0.85 (3)	C4—H17	0.9700
O3—H6	0.71 (3)	C4—H18	0.9700
N1—C2	1.474 (3)	C5—H19	0.9700
N1—C1	1.474 (3)	C5—H20	0.9700
N1—C3	1.479 (3)	C6—H21	0.9700
N2—C4	1.472 (3)	C6—H22	0.9700
N2—C6	1.472 (3)	O4—H7	0.88 (5)
N2—C1	1.475 (3)	O4—H8	0.77 (5)
N3—C5	1.476 (3)	O5—H9	0.79 (3)
N3—C2	1.476 (3)	O5—H10	0.82 (4)
O3^i—Ni1—O3	180.000 (1)	N1—C1—H11	109.2
O3^i—Ni1—O1	92.61 (9)	N2—C1—H11	109.2
O3—Ni1—O1	87.39 (9)	N1—C1—H12	109.2
O3^i—Ni1—O1^i	87.39 (9)	N2—C1—H12	109.2
O3—Ni1—O1^i	92.61 (9)	H11—C1—H12	107.9
O1—Ni1—O1^i	180.000 (1)	N1—C2—N3	111.96 (16)
O3^i—Ni1—O2	89.24 (9)	N1—C2—H13	109.2
O3—Ni1—O2	90.76 (9)	N3—C2—H13	109.2
O1—Ni1—O2	86.66 (8)	N1—C2—H14	109.2
O1^i—Ni1—O2	93.34 (8)	N3—C2—H14	109.2
O3^i—Ni1—O2^i	90.76 (9)	H13—C2—H14	107.9
O3—Ni1—O2^i	89.24 (9)	N4—C3—N1	111.71 (16)
O1—Ni1—O2^i	93.34 (8)	N4—C3—H15	109.3
O1^i—Ni1—O2^i	86.66 (8)	N1—C3—H15	109.3
O2—Ni1—O2^i	180.000 (1)	N4—C3—H16	109.3
Ni1—O1—H1	121 (2)	N1—C3—H16	109.3
Ni1—O1—H2	127.3 (18)	H15—C3—H16	107.9
H1—O1—H2	106 (3)	N2—C4—N3	112.02 (16)
Ni1—O2—H3	121 (3)	N2—C4—H17	109.2
Ni1—O2—H4	127 (2)	N3—C4—H17	109.2
H3—O2—H4	104 (3)	N2—C4—H18	109.2
Ni1—O3—H5	121 (2)	N3—C4—H18	109.2
Ni1—O3—H6	127 (2)	H17—C4—H18	107.9
H5—O3—H6	112 (3)	N4—C5—N3	112.04 (16)
C2—N1—C1	108.67 (15)	N4—C5—H19	109.2
C2—N1—C3	108.16 (17)	N3—C5—H19	109.2
C1—N1—C3	107.79 (16)	N4—C5—H20	109.2
C4—N2—C6	108.33 (16)	N3—C5—H20	109.2
C4—N2—C1	108.53 (17)	H19—C5—H20	107.9
C6—N2—C1	108.04 (16)	N2—C6—N4	111.60 (16)
C5—N3—C2	107.84 (17)	N2—C6—H21	109.3
C5—N3—C4	108.05 (16)	N4—C6—H21	109.3
C2—N3—C4	108.34 (17)	N2—C6—H22	109.3
C5—N4—C3	108.55 (16)	N4—C6—H22	109.3
C5—N4—C6	108.52 (16)	H21—C6—H22	108.0
C3—N4—C6	108.11 (17)	H7—O4—H8	109 (4)
N1—C1—N2	111.89 (16)	H9—O5—H10	102 (3)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···N1^ii	0.77 (3)	2.06 (3)	2.823 (3)	172 (3)
O1—H2···O4	0.85 (3)	1.90 (3)	2.739 (3)	166 (3)
O2—H3···N2	0.76 (4)	2.08 (4)	2.814 (3)	164 (3)
O2—H4···Cl1	0.84 (4)	2.39 (4)	3.191 (2)	158 (3)
O3—H5···N4^iii	0.85 (3)	1.98 (3)	2.799 (3)	161 (3)
O3—H6···O5	0.71 (3)	2.00 (3)	2.714 (3)	172 (3)
O4—H7···Cl1^iv	0.88 (5)	2.37 (5)	3.253 (3)	176 (4)
O4—H8···Cl1^v	0.77 (5)	2.44 (5)	3.210 (3)	173 (4)
O5—H9···N3^vi	0.79 (3)	2.05 (3)	2.838 (3)	170 (3)
O5—H10···Cl1^vii	0.82 (4)	2.35 (4)	3.168 (3)	174 (3)

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