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In the title compound, [Ni(H2O)6]Cl2·2C6H12N4·4H2O, the NiII 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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803020269/lh6108sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803020269/lh6108Isup2.hkl
Contains datablock I

CCDC reference: 225679

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

Computing details top

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) top
Crystal data top
[Ni(H2O)6]Cl2·2C6H12N4·4H2OZ = 1
Mr = 590.14F(000) = 314
Triclinic, P1Dx = 1.411 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.330 (6) ÅCell parameters from 2777 reflections
b = 9.411 (6) Åθ = 2.5–26.3°
c = 9.446 (6) ŵ = 0.95 mm1
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) Å3
Data collection top
Bruker SMART-CCD area-detector
diffractometer
2418 independent reflections
Radiation source: fine-focus sealed tube2216 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
φ and ω scansθmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 911
Tmin = 0.670, Tmax = 0.848k = 1011
3644 measured reflectionsl = 1110
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.031H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.089 w = 1/[σ2(Fo2) + (0.0606P)2 + 0.0662P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
2418 reflectionsΔρmax = 0.35 e Å3
204 parametersΔρmin = 0.49 e Å3
0 restraintsExtinction correction: SHELXTL (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.059 (5)
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
Ni10.50000.50000.50000.02892 (16)
O10.3831 (2)0.6342 (2)0.4429 (2)0.0450 (4)
H10.380 (3)0.723 (4)0.510 (4)0.053 (8)*
H20.305 (3)0.595 (3)0.369 (4)0.059 (8)*
O20.6415 (2)0.5275 (2)0.3532 (2)0.0520 (4)
H30.632 (4)0.579 (4)0.314 (4)0.076 (10)*
H40.684 (4)0.456 (4)0.288 (4)0.080 (10)*
O30.6186 (2)0.7235 (2)0.69897 (19)0.0515 (4)
H50.613 (3)0.746 (4)0.797 (4)0.065 (8)*
H60.671 (3)0.790 (4)0.699 (4)0.059 (9)*
N10.6580 (2)1.0478 (2)0.3272 (2)0.0379 (4)
N20.6660 (2)0.7597 (2)0.2449 (2)0.0391 (4)
N30.88469 (19)0.9576 (2)0.2560 (2)0.0402 (4)
N40.6640 (2)0.8457 (2)0.0398 (2)0.0390 (4)
C10.6077 (2)0.9045 (3)0.3516 (3)0.0411 (5)
H110.49980.86900.32680.041 (6)*
H120.64070.94100.46690.049 (6)*
C20.8220 (2)1.0986 (3)0.3625 (3)0.0435 (5)
H130.85821.13790.47800.055 (7)*
H140.85611.19180.34510.044 (6)*
C30.6057 (2)0.9880 (3)0.1507 (3)0.0403 (5)
H150.49770.95280.12490.041 (6)*
H160.63741.08050.13170.036 (5)*
C40.8296 (2)0.8163 (3)0.2823 (3)0.0433 (5)
H170.86910.72220.21200.048 (6)*
H180.86560.85190.39680.038 (6)*
C50.8272 (2)0.9006 (3)0.0816 (3)0.0435 (5)
H190.86140.99250.06230.046 (6)*
H200.86680.80750.00930.042 (6)*
C60.6137 (2)0.7066 (3)0.0710 (3)0.0410 (5)
H210.50570.66980.04480.045 (6)*
H220.65100.61130.00130.050 (6)*
Cl10.81052 (7)0.32527 (8)0.06497 (8)0.0593 (2)
O40.1488 (3)0.5523 (4)0.2005 (3)0.0813 (7)
H70.165 (5)0.585 (5)0.129 (6)0.114 (15)*
H80.068 (5)0.496 (6)0.174 (5)0.106 (16)*
O50.8033 (2)0.9976 (2)0.7221 (2)0.0518 (4)
H90.889 (4)1.002 (4)0.732 (4)0.061 (9)*
H100.800 (4)1.078 (5)0.812 (5)0.089 (12)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0391 (2)0.0253 (2)0.0249 (2)0.01100 (14)0.00910 (14)0.01362 (15)
O10.0572 (10)0.0356 (9)0.0394 (8)0.0216 (7)0.0015 (7)0.0153 (7)
O20.0749 (12)0.0528 (10)0.0612 (10)0.0366 (9)0.0443 (9)0.0426 (9)
O30.0754 (12)0.0348 (9)0.0287 (8)0.0069 (8)0.0047 (7)0.0131 (7)
N10.0456 (10)0.0344 (9)0.0338 (8)0.0174 (7)0.0070 (7)0.0154 (7)
N20.0481 (10)0.0385 (9)0.0441 (9)0.0191 (8)0.0193 (8)0.0272 (8)
N30.0405 (9)0.0386 (9)0.0393 (9)0.0119 (7)0.0089 (7)0.0180 (8)
N40.0471 (10)0.0366 (9)0.0311 (8)0.0058 (7)0.0076 (7)0.0176 (7)
C10.0472 (12)0.0502 (12)0.0377 (10)0.0228 (10)0.0187 (9)0.0266 (10)
C20.0469 (12)0.0343 (11)0.0383 (10)0.0107 (9)0.0014 (9)0.0116 (9)
C30.0458 (12)0.0390 (11)0.0407 (10)0.0100 (9)0.0029 (9)0.0251 (9)
C40.0505 (12)0.0461 (12)0.0468 (11)0.0258 (10)0.0171 (10)0.0283 (10)
C50.0529 (13)0.0410 (12)0.0389 (11)0.0093 (9)0.0180 (9)0.0222 (10)
C60.0479 (12)0.0314 (10)0.0408 (10)0.0069 (9)0.0133 (9)0.0171 (9)
Cl10.0655 (4)0.0484 (4)0.0601 (4)0.0163 (3)0.0287 (3)0.0226 (3)
O40.0682 (15)0.0957 (17)0.0812 (15)0.0066 (13)0.0120 (12)0.0552 (14)
O50.0442 (10)0.0488 (10)0.0489 (10)0.0023 (7)0.0079 (8)0.0191 (9)
Geometric parameters (Å, º) top
Ni1—O3i2.0227 (18)N3—C41.476 (3)
Ni1—O32.0227 (18)N4—C51.467 (3)
Ni1—O12.0460 (17)N4—C31.471 (3)
Ni1—O1i2.0460 (17)N4—C61.478 (3)
Ni1—O22.0554 (18)C1—H110.9700
Ni1—O2i2.0554 (18)C1—H120.9700
O1—H10.77 (3)C2—H130.9700
O1—H20.85 (3)C2—H140.9700
O2—H30.76 (4)C3—H150.9700
O2—H40.84 (4)C3—H160.9700
O3—H50.85 (3)C4—H170.9700
O3—H60.71 (3)C4—H180.9700
N1—C21.474 (3)C5—H190.9700
N1—C11.474 (3)C5—H200.9700
N1—C31.479 (3)C6—H210.9700
N2—C41.472 (3)C6—H220.9700
N2—C61.472 (3)O4—H70.88 (5)
N2—C11.475 (3)O4—H80.77 (5)
N3—C51.476 (3)O5—H90.79 (3)
N3—C21.476 (3)O5—H100.82 (4)
O3i—Ni1—O3180.000 (1)N1—C1—H11109.2
O3i—Ni1—O192.61 (9)N2—C1—H11109.2
O3—Ni1—O187.39 (9)N1—C1—H12109.2
O3i—Ni1—O1i87.39 (9)N2—C1—H12109.2
O3—Ni1—O1i92.61 (9)H11—C1—H12107.9
O1—Ni1—O1i180.000 (1)N1—C2—N3111.96 (16)
O3i—Ni1—O289.24 (9)N1—C2—H13109.2
O3—Ni1—O290.76 (9)N3—C2—H13109.2
O1—Ni1—O286.66 (8)N1—C2—H14109.2
O1i—Ni1—O293.34 (8)N3—C2—H14109.2
O3i—Ni1—O2i90.76 (9)H13—C2—H14107.9
O3—Ni1—O2i89.24 (9)N4—C3—N1111.71 (16)
O1—Ni1—O2i93.34 (8)N4—C3—H15109.3
O1i—Ni1—O2i86.66 (8)N1—C3—H15109.3
O2—Ni1—O2i180.000 (1)N4—C3—H16109.3
Ni1—O1—H1121 (2)N1—C3—H16109.3
Ni1—O1—H2127.3 (18)H15—C3—H16107.9
H1—O1—H2106 (3)N2—C4—N3112.02 (16)
Ni1—O2—H3121 (3)N2—C4—H17109.2
Ni1—O2—H4127 (2)N3—C4—H17109.2
H3—O2—H4104 (3)N2—C4—H18109.2
Ni1—O3—H5121 (2)N3—C4—H18109.2
Ni1—O3—H6127 (2)H17—C4—H18107.9
H5—O3—H6112 (3)N4—C5—N3112.04 (16)
C2—N1—C1108.67 (15)N4—C5—H19109.2
C2—N1—C3108.16 (17)N3—C5—H19109.2
C1—N1—C3107.79 (16)N4—C5—H20109.2
C4—N2—C6108.33 (16)N3—C5—H20109.2
C4—N2—C1108.53 (17)H19—C5—H20107.9
C6—N2—C1108.04 (16)N2—C6—N4111.60 (16)
C5—N3—C2107.84 (17)N2—C6—H21109.3
C5—N3—C4108.05 (16)N4—C6—H21109.3
C2—N3—C4108.34 (17)N2—C6—H22109.3
C5—N4—C3108.55 (16)N4—C6—H22109.3
C5—N4—C6108.52 (16)H21—C6—H22108.0
C3—N4—C6108.11 (17)H7—O4—H8109 (4)
N1—C1—N2111.89 (16)H9—O5—H10102 (3)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···N1ii0.77 (3)2.06 (3)2.823 (3)172 (3)
O1—H2···O40.85 (3)1.90 (3)2.739 (3)166 (3)
O2—H3···N20.76 (4)2.08 (4)2.814 (3)164 (3)
O2—H4···Cl10.84 (4)2.39 (4)3.191 (2)158 (3)
O3—H5···N4iii0.85 (3)1.98 (3)2.799 (3)161 (3)
O3—H6···O50.71 (3)2.00 (3)2.714 (3)172 (3)
O4—H7···Cl1iv0.88 (5)2.37 (5)3.253 (3)176 (4)
O4—H8···Cl1v0.77 (5)2.44 (5)3.210 (3)173 (4)
O5—H9···N3vi0.79 (3)2.05 (3)2.838 (3)170 (3)
O5—H10···Cl1vii0.82 (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) x1, y, z; (vi) x+2, y+2, z+1; (vii) x, y+1, z+1.
 

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