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In the title complex, [Ni3(C9H3O6)(C9H23N3)3(H2O)3](ClO4)3·4.25H2O, the three NiII centres are bridged by a benzene-1,3,5-tricarboxyl­ate(3−) anion (btc). Each of the metal centres is coordinated by three N atoms of a tridentate N,N,N′,N′′,N′′-penta­methyl­diethylenetriamine ligand (pmdien), two O atoms of the btc ligand and one water mol­ecule in a distorted octa­hedral geometry. The secondary structure is stabilized by a variety of O—H...O hydrogen bonds and C—H...O inter­actions that serve to connect the complex cations, perchlorate anions and water solvent mol­ecules. Variability of intermolecular contacts stabilizing the crystal structure leads to disorder of part of O atoms of two perchlorate anions between two positions with occupancies 0.632 (5) and 0.337 (7).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807051938/tk2201sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807051938/tk2201Isup2.hkl
Contains datablock I

CCDC reference: 667252

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.005 Å
  • Disorder in solvent or counterion
  • R factor = 0.041
  • wR factor = 0.096
  • Data-to-parameter ratio = 12.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT214_ALERT_2_B Atom O89A (Anion/Solvent) ADP max/min Ratio 5.40 oblat PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.66 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.11 Ratio PLAT417_ALERT_2_B Short Inter D-H..H-D H6W .. H51W .. 1.97 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O87 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl3 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl3A PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 27.00 Perc.
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 26
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 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 2 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

The molecular structure of the title complex, (I), is depicted in Fig. 1. The structure comprises a trinuclear NiII trication, three perchlorate anions and 4.25 crystal water molecules of crystallization. The three NiII metal centres are bridged by a benzene-1,3,5-tricarboxylate(3-) anion (btc). The atoms forming the Ni3(btc) moiety deviate from planarity with dihedral angles between the central aromatic ring and the peripheral 4-membered C–O–Ni–O rings being in the range 3.2 (9)° to 8.1 (5)° for the rings containing Ni3 and Ni1 atoms, respectively (Brandenburg, 2006). Each of NiII cations is positioned at the vertex of an equilateral triangle with the Ni···Ni distances being 9.5197 (6) Å for Ni1···Ni2, 8.9876 (6) Å for Ni1···Ni3, and 9.6056 (5) Å for Ni2···Ni3. The geometry of the Ni centre is distorted octahedral. The degree of deformation can be seen from interatomic parameters around the Ni atom which differ significantly, e.g. Ni—Obtc bond lengths are in the range of 2.036 (2) to 2.493 (2) Å, whilst Ni—O(water) distances are similar and vary from 2.041 (2) to 2.079 (3) Å. For comparison, the Ni···Ni separations in the recently published polynuclear Ni complex involving the Ni3(btc) moiety are 9.236 (4), 9.236 (6) and 9.294 (6) Å, and Ni—O bond lengths of a bidentate coordinated carboxylate group vary from 2.110 (8) to 2.130 (8) Å (Chen et al., 2005).

To date, only 19 X-ray structures involving the M3(btc) moiety, where M represents any transition metal, are included in the CSD (Cambridge Structural Database, Version 5.28.1; Allen, 2002), e.g. Gd (Daiguebonne et al., 1998), Co (Livage et al., 2001), In (Lin et al., 2005), Nd (Wang et al., 2004), Ni (Chen et al., 2005), Sm (Daiguebonne et al., 2002) and Er (Daiguebonne et al., 2000).

The secondary structure of (I) is stabilized by a variety of O—H···O hydrogen bonds (Table 1, Fig. 2) and C—H···O interactions (Fig. 3), connecting the complex cations, perchlorate anions and water molecules.

Related literature top

For related literature, see: Chen et al. (2005); Allen (2002); Daiguebonne et al. (1998, 2000, 2002); Kopel et al. (2007); Lin et al. (2005); Livage et al. (2001); Wang et al. (2004).

Experimental top

The title complex, (I), was prepared by a recently described method (Kopel et al., 2007). Crystals suitable for X-ray analysis were obtained by recrystallization of (I) from water.

Refinement top

Some atoms of perchlorate anions (namely O atoms O77, O78 and O79 bonded to Cl2, and O atoms O86, O88 and O89 bonded to Cl3) were refined as disordered between two positions [the site occupancy factors was refined to 0.632 (5) and 0.337 (7)]. C-bound H-atoms were included in the riding model approximation with C–H distances of 0.95 - 0.99 Å (CH2), and with Uiso(H) = 1.2Ueq(CH2) or 1.5Ueq(Cmethyl). The O-bound H atoms were refined, with the O—H distances restrained to 0.95 (2) Å and with Uiso(H) values of 1.5Ueq(Owater); distances are given in Table 1. The maximum and minimum residual electron denisty peaks were located in the neighbourhood of disordered perchlorate anions with distances 1.33 and 0.84 Å, respectively from the O88A and Cl2 atoms.

Structure description top

The molecular structure of the title complex, (I), is depicted in Fig. 1. The structure comprises a trinuclear NiII trication, three perchlorate anions and 4.25 crystal water molecules of crystallization. The three NiII metal centres are bridged by a benzene-1,3,5-tricarboxylate(3-) anion (btc). The atoms forming the Ni3(btc) moiety deviate from planarity with dihedral angles between the central aromatic ring and the peripheral 4-membered C–O–Ni–O rings being in the range 3.2 (9)° to 8.1 (5)° for the rings containing Ni3 and Ni1 atoms, respectively (Brandenburg, 2006). Each of NiII cations is positioned at the vertex of an equilateral triangle with the Ni···Ni distances being 9.5197 (6) Å for Ni1···Ni2, 8.9876 (6) Å for Ni1···Ni3, and 9.6056 (5) Å for Ni2···Ni3. The geometry of the Ni centre is distorted octahedral. The degree of deformation can be seen from interatomic parameters around the Ni atom which differ significantly, e.g. Ni—Obtc bond lengths are in the range of 2.036 (2) to 2.493 (2) Å, whilst Ni—O(water) distances are similar and vary from 2.041 (2) to 2.079 (3) Å. For comparison, the Ni···Ni separations in the recently published polynuclear Ni complex involving the Ni3(btc) moiety are 9.236 (4), 9.236 (6) and 9.294 (6) Å, and Ni—O bond lengths of a bidentate coordinated carboxylate group vary from 2.110 (8) to 2.130 (8) Å (Chen et al., 2005).

To date, only 19 X-ray structures involving the M3(btc) moiety, where M represents any transition metal, are included in the CSD (Cambridge Structural Database, Version 5.28.1; Allen, 2002), e.g. Gd (Daiguebonne et al., 1998), Co (Livage et al., 2001), In (Lin et al., 2005), Nd (Wang et al., 2004), Ni (Chen et al., 2005), Sm (Daiguebonne et al., 2002) and Er (Daiguebonne et al., 2000).

The secondary structure of (I) is stabilized by a variety of O—H···O hydrogen bonds (Table 1, Fig. 2) and C—H···O interactions (Fig. 3), connecting the complex cations, perchlorate anions and water molecules.

For related literature, see: Chen et al. (2005); Allen (2002); Daiguebonne et al. (1998, 2000, 2002); Kopel et al. (2007); Lin et al. (2005); Livage et al. (2001); Wang et al. (2004).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title complex (I). The non-H atoms are drawn as 50% probability displacement ellipsoids. The disordered parts of the perchlorate anions have been omitted for clarity. The H-atoms are shown as short solid lines.
[Figure 2] Fig. 2. Part of the crystal structure of (I), showing the formation of O—H···O hydrogen bonds [Symmetry codes: (i) -x + 1, -y + 1, -z + 1; (ii) -x, -y + 1, -z + 1]. Some of disordered perchlorate atoms and H-atoms not involved in hydrogen bonding are omitted for clarity.
[Figure 3] Fig. 3. Part of the crystal structure of (I), showing the formation of C—H···O contacts [Symmetry codes: (i) -x + 1, -y + 1, -z + 1; (ii) -x, -y + 1, -z + 1; (iii) 1 - x, -1/2 + y, 3/2 - z, (iv) x, 1/2 - y, -1/2 + z; (v) x, 1/2 - y, 1/2 + z; (vi) 1 - x, 1/2 + y, 3/2 - z; (vii) -x, 1/2 + y, 1/2 - z]. Some of disordered perchlorate atoms and H-atoms not involved in hydrogen bonding are omitted for clarity.
3-Benzene-1,3,5-tricarboxylato)tris[aqua(N,N,N',N'',N''- pentamethyldiethylenetriamine)nickel(II)] tris(perchlorate) 4.25-hydrate top
Crystal data top
[Ni3(C9H3O6)(C9H23N3)3(H2O)3](ClO4)3·4.25H2OF(000) = 2810
Mr = 1332.12Dx = 1.520 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25991 reflections
a = 11.7409 (2) Åθ = 2.6–32.0°
b = 30.6727 (5) ŵ = 1.18 mm1
c = 16.9590 (4) ÅT = 100 K
β = 107.633 (2)°Prism, dark-green
V = 5820.41 (19) Å30.30 × 0.30 × 0.25 mm
Z = 4
Data collection top
Oxford Diffraction Xcalibur2 + CCD
diffractometer
10209 independent reflections
Radiation source: Enhance (Mo) X-ray Source8075 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
Detector resolution: 8.3611 pixels mm-1θmax = 25.1°, θmin = 2.6°
ω scansh = 1313
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2006)
k = 3528
Tmin = 0.655, Tmax = 0.740l = 2020
27090 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.03P)2 + 15P]
where P = (Fo2 + 2Fc2)/3
10209 reflections(Δ/σ)max = 0.002
799 parametersΔρmax = 1.01 e Å3
26 restraintsΔρmin = 1.02 e Å3
Crystal data top
[Ni3(C9H3O6)(C9H23N3)3(H2O)3](ClO4)3·4.25H2OV = 5820.41 (19) Å3
Mr = 1332.12Z = 4
Monoclinic, P21/cMo Kα radiation
a = 11.7409 (2) ŵ = 1.18 mm1
b = 30.6727 (5) ÅT = 100 K
c = 16.9590 (4) Å0.30 × 0.30 × 0.25 mm
β = 107.633 (2)°
Data collection top
Oxford Diffraction Xcalibur2 + CCD
diffractometer
10209 independent reflections
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2006)
8075 reflections with I > 2σ(I)
Tmin = 0.655, Tmax = 0.740Rint = 0.025
27090 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04126 restraints
wR(F2) = 0.096H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.03P)2 + 15P]
where P = (Fo2 + 2Fc2)/3
10209 reflectionsΔρmax = 1.01 e Å3
799 parametersΔρmin = 1.02 e Å3
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*/UeqOcc. (<1)
Ni10.18931 (4)0.372432 (13)0.49777 (2)0.01350 (10)
Ni20.24189 (4)0.612514 (14)0.15475 (2)0.01464 (10)
Ni30.57687 (4)0.611801 (13)0.74650 (2)0.01328 (10)
O10.2105 (2)0.42302 (7)0.41337 (13)0.0167 (5)
O20.2956 (2)0.42913 (7)0.54701 (13)0.0167 (5)
O30.3311 (2)0.34306 (8)0.47357 (15)0.0201 (5)
H3V0.371 (3)0.3184 (9)0.497 (2)0.030*
H3W0.386 (3)0.3588 (11)0.455 (2)0.030*
O40.2287 (2)0.55024 (7)0.22527 (13)0.0221 (5)
O50.3051 (2)0.61172 (7)0.28366 (13)0.0202 (5)
O60.4100 (2)0.59180 (10)0.15492 (16)0.0314 (6)
H6V0.460 (3)0.5804 (14)0.2039 (18)0.047*
H6W0.462 (3)0.6017 (14)0.128 (3)0.047*
O70.5043 (2)0.62186 (7)0.59350 (14)0.0201 (5)
O80.4838 (2)0.56524 (8)0.66740 (13)0.0208 (5)
O90.7360 (2)0.59170 (8)0.73098 (14)0.0179 (5)
H9V0.741 (3)0.5875 (12)0.6791 (14)0.027*
H9W0.789 (3)0.5725 (10)0.764 (2)0.027*
N10.2254 (3)0.34506 (9)0.61657 (17)0.0187 (6)
N20.0337 (2)0.39932 (9)0.51974 (16)0.0165 (6)
N30.0646 (2)0.33156 (9)0.41396 (16)0.0163 (6)
N40.2765 (3)0.68067 (10)0.15369 (19)0.0262 (7)
N50.0659 (2)0.63192 (9)0.14337 (17)0.0201 (6)
N60.1648 (3)0.59061 (10)0.02995 (17)0.0217 (6)
N70.5875 (2)0.57154 (9)0.84912 (16)0.0184 (6)
N80.4263 (2)0.63958 (9)0.77056 (16)0.0184 (6)
N90.6533 (2)0.67424 (9)0.78328 (16)0.0168 (6)
C10.3081 (3)0.49073 (10)0.46320 (19)0.0135 (7)
C20.2790 (3)0.50910 (11)0.38461 (19)0.0155 (7)
H20.23630.49240.33780.019*
C30.3123 (3)0.55197 (11)0.37416 (19)0.0158 (7)
C40.3748 (3)0.57623 (10)0.44331 (19)0.0148 (7)
H40.39820.60530.43650.018*
C50.4032 (3)0.55825 (10)0.52214 (19)0.0151 (7)
C60.3696 (3)0.51542 (10)0.53177 (19)0.0151 (7)
H60.38890.50300.58550.018*
C70.2709 (3)0.44529 (10)0.47542 (19)0.0142 (7)
C80.2798 (3)0.57222 (11)0.2895 (2)0.0181 (7)
C90.4679 (3)0.58317 (11)0.59844 (19)0.0163 (7)
C100.1662 (3)0.37705 (12)0.6569 (2)0.0225 (8)
H10A0.20980.40510.66430.027*
H10B0.16790.36620.71220.027*
C110.0378 (3)0.38396 (12)0.6041 (2)0.0218 (8)
H11A0.00700.35630.59960.026*
H11B0.00080.40580.63060.026*
C120.0713 (3)0.38080 (11)0.4570 (2)0.0229 (8)
H12A0.08980.39850.40580.027*
H12B0.14150.38180.47780.027*
C130.0470 (3)0.33401 (11)0.4378 (2)0.0202 (7)
H13A0.03910.31560.48710.024*
H13B0.11490.32290.39210.024*
C140.1844 (3)0.30049 (12)0.6262 (2)0.0266 (8)
H14A0.20160.29380.68520.040*
H14B0.22620.27960.60100.040*
H14C0.09810.29840.59890.040*
C150.3560 (3)0.34564 (13)0.6598 (2)0.0260 (8)
H15A0.38970.37340.64890.039*
H15B0.39440.32160.63940.039*
H15C0.37000.34230.71940.039*
C160.0250 (3)0.44741 (11)0.5169 (2)0.0251 (8)
H16A0.02670.45780.46270.038*
H16B0.09260.45990.56010.038*
H16C0.05000.45640.52620.038*
C170.0983 (3)0.28511 (11)0.4114 (2)0.0228 (8)
H17A0.10480.27130.46470.034*
H17B0.17540.28320.40030.034*
H17C0.03710.27010.36740.034*
C180.0431 (3)0.34967 (11)0.3294 (2)0.0204 (7)
H18A0.01860.33240.28980.031*
H18B0.11730.34850.31440.031*
H18C0.01650.38000.32830.031*
C200.1797 (4)0.69925 (13)0.1802 (3)0.0408 (11)
H20A0.17770.73120.17200.049*
H20B0.19470.69350.23990.049*
C210.0620 (4)0.68036 (13)0.1327 (3)0.0348 (10)
H21A0.04390.68770.07330.042*
H21B0.00180.69280.15290.042*
C220.0135 (3)0.61055 (14)0.0689 (2)0.0284 (9)
H22A0.09020.62660.05010.034*
H22B0.03060.58040.08280.034*
C230.0423 (3)0.60938 (13)0.0003 (2)0.0275 (8)
H23A0.00770.59150.04590.033*
H23B0.04620.63930.02050.033*
C240.3929 (4)0.69117 (15)0.2159 (3)0.0495 (13)
H24A0.40080.72290.22280.074*
H24B0.45820.67990.19690.074*
H24C0.39640.67760.26890.074*
C250.2803 (4)0.70070 (15)0.0757 (3)0.0484 (12)
H25A0.20380.69590.03290.073*
H25B0.34470.68740.05830.073*
H25C0.29490.73210.08390.073*
C260.0262 (4)0.62113 (16)0.2159 (3)0.0404 (11)
H26A0.05720.63010.20520.061*
H26B0.07650.63650.26470.061*
H26C0.03290.58960.22570.061*
C270.1576 (5)0.54266 (14)0.0316 (2)0.0452 (12)
H27A0.11020.53390.06760.068*
H27B0.23830.53050.05290.068*
H27C0.11960.53180.02450.068*
C280.2286 (4)0.60271 (17)0.0305 (2)0.0434 (12)
H28A0.31050.59150.01140.065*
H28B0.23040.63450.03520.065*
H28C0.18680.59010.08460.065*
C300.4667 (3)0.57526 (13)0.8598 (2)0.0298 (9)
H30A0.46870.56370.91470.036*
H30B0.40900.55770.81700.036*
C310.4271 (3)0.62195 (13)0.8527 (2)0.0299 (9)
H31A0.34600.62400.85870.036*
H31B0.48220.63930.89740.036*
C320.4437 (3)0.68742 (12)0.7751 (2)0.0258 (8)
H32A0.39100.70060.80440.031*
H32B0.42140.69970.71850.031*
C330.5721 (3)0.69852 (12)0.8200 (2)0.0248 (8)
H33A0.58470.73030.81610.030*
H33B0.59040.69080.87930.030*
C340.6044 (4)0.52518 (12)0.8308 (2)0.0280 (9)
H34A0.68600.52080.82850.042*
H34B0.54730.51730.77740.042*
H34C0.59100.50680.87440.042*
C350.6812 (3)0.58291 (12)0.9259 (2)0.0274 (8)
H35A0.66940.61300.94150.041*
H35B0.75970.58030.91720.041*
H35C0.67700.56310.97020.041*
C360.3111 (3)0.62924 (13)0.7090 (2)0.0284 (9)
H36A0.24620.64270.72570.043*
H36B0.29990.59760.70560.043*
H36C0.31030.64060.65490.043*
C370.6541 (3)0.69661 (11)0.7058 (2)0.0222 (8)
H37A0.57240.69820.66800.033*
H37B0.70450.68030.67950.033*
H37C0.68600.72620.71870.033*
C380.7766 (3)0.67569 (12)0.8407 (2)0.0217 (8)
H38A0.82900.65780.81850.033*
H38B0.77720.66440.89480.033*
H38C0.80530.70590.84670.033*
Cl10.10417 (9)0.75444 (3)0.36681 (5)0.0291 (2)
O960.0428 (3)0.77425 (12)0.4183 (2)0.0558 (10)
O970.1431 (3)0.71176 (11)0.4000 (2)0.0516 (9)
O980.0216 (3)0.74819 (11)0.28622 (17)0.0551 (9)
O990.2026 (3)0.78013 (11)0.3648 (2)0.0599 (10)
Cl20.15471 (10)0.50855 (3)0.74728 (8)0.0448 (3)
O760.1141 (3)0.54718 (10)0.7734 (2)0.0553 (9)
O770.2529 (6)0.4881 (2)0.7936 (4)0.0741 (18)0.632 (5)
O780.1822 (5)0.52275 (18)0.6676 (3)0.0445 (12)0.632 (5)
O790.0522 (10)0.4811 (3)0.7122 (4)0.056 (3)0.632 (5)
O77A0.2363 (10)0.4990 (4)0.8379 (6)0.0741 (18)0.368 (5)
O78A0.2408 (8)0.5090 (3)0.7093 (6)0.0445 (12)0.368 (5)
O79A0.0760 (19)0.4731 (6)0.7436 (9)0.056 (3)0.368 (5)
O870.2731 (3)0.13286 (13)0.3765 (3)0.0711 (11)
Cl30.3567 (2)0.16715 (9)0.40985 (12)0.0277 (6)0.663 (7)
O860.3186 (6)0.18374 (16)0.4762 (3)0.0439 (15)0.663 (7)
O880.4662 (4)0.14462 (16)0.4400 (3)0.0447 (15)0.663 (7)
O890.3589 (7)0.1989 (2)0.3509 (4)0.065 (2)0.663 (7)
Cl3A0.3081 (7)0.17759 (15)0.4139 (3)0.0338 (13)0.337 (7)
O86A0.2359 (11)0.1898 (4)0.4636 (6)0.048 (3)0.337 (7)
O88A0.4306 (10)0.1809 (4)0.4639 (7)0.065 (4)0.337 (7)
O89A0.2786 (15)0.2004 (6)0.3427 (7)0.082 (5)0.337 (7)
O510.5580 (8)0.5631 (3)0.0792 (5)0.0141 (18)*0.25
H51W0.603 (10)0.589 (2)0.092 (8)0.021*0.25
H51V0.600 (10)0.537 (2)0.099 (8)0.021*0.25
O520.4498 (3)0.26949 (10)0.5315 (2)0.0464 (8)
H52V0.532 (2)0.2783 (17)0.551 (3)0.070*
H52W0.437 (5)0.2448 (12)0.497 (3)0.070*
O530.3673 (3)0.69819 (11)0.5254 (2)0.0527 (9)
H53V0.301 (4)0.6950 (18)0.473 (2)0.079*
H53W0.390 (5)0.6671 (8)0.536 (3)0.079*
O540.4280 (2)0.45053 (9)0.71672 (17)0.0337 (7)
H54V0.396 (4)0.4442 (15)0.6605 (14)0.051*
H54W0.372 (3)0.4644 (14)0.737 (3)0.051*
O550.1060 (2)0.46955 (8)0.18374 (15)0.0240 (5)
H55V0.137 (3)0.4963 (8)0.202 (2)0.036*
H55W0.038 (2)0.4686 (14)0.199 (2)0.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0180 (2)0.0101 (2)0.0119 (2)0.00242 (17)0.00381 (17)0.00048 (16)
Ni20.0188 (2)0.0142 (2)0.0104 (2)0.00220 (17)0.00359 (17)0.00279 (16)
Ni30.0161 (2)0.0127 (2)0.0099 (2)0.00199 (17)0.00225 (16)0.00155 (16)
O10.0238 (12)0.0128 (12)0.0123 (11)0.0053 (10)0.0037 (10)0.0014 (9)
O20.0246 (13)0.0132 (12)0.0112 (11)0.0036 (10)0.0039 (10)0.0011 (9)
O30.0223 (13)0.0155 (13)0.0257 (13)0.0018 (10)0.0122 (11)0.0044 (10)
O40.0358 (14)0.0153 (12)0.0109 (11)0.0004 (11)0.0005 (11)0.0007 (10)
O50.0328 (14)0.0124 (12)0.0131 (11)0.0000 (10)0.0034 (10)0.0019 (9)
O60.0211 (14)0.0443 (17)0.0267 (14)0.0087 (12)0.0041 (11)0.0030 (13)
O70.0254 (13)0.0146 (13)0.0226 (12)0.0069 (10)0.0105 (11)0.0053 (10)
O80.0296 (14)0.0193 (13)0.0104 (11)0.0080 (10)0.0016 (10)0.0031 (9)
O90.0208 (13)0.0183 (13)0.0154 (12)0.0037 (10)0.0068 (10)0.0008 (10)
N10.0251 (16)0.0163 (15)0.0151 (14)0.0008 (12)0.0070 (12)0.0020 (11)
N20.0189 (15)0.0126 (15)0.0167 (14)0.0003 (11)0.0034 (12)0.0011 (11)
N30.0191 (14)0.0117 (14)0.0170 (14)0.0033 (11)0.0038 (12)0.0007 (11)
N40.0261 (17)0.0185 (16)0.0258 (16)0.0022 (13)0.0046 (13)0.0096 (13)
N50.0206 (15)0.0230 (16)0.0175 (14)0.0028 (12)0.0069 (12)0.0005 (12)
N60.0240 (16)0.0279 (17)0.0138 (14)0.0045 (13)0.0065 (12)0.0012 (12)
N70.0230 (15)0.0180 (15)0.0127 (14)0.0021 (12)0.0032 (12)0.0010 (11)
N80.0165 (14)0.0236 (16)0.0145 (14)0.0029 (12)0.0039 (12)0.0032 (12)
N90.0191 (14)0.0140 (15)0.0161 (14)0.0001 (11)0.0035 (12)0.0034 (11)
C10.0143 (16)0.0117 (16)0.0143 (16)0.0014 (13)0.0042 (13)0.0005 (13)
C20.0213 (17)0.0146 (17)0.0101 (15)0.0013 (14)0.0038 (13)0.0022 (13)
C30.0219 (18)0.0137 (17)0.0116 (16)0.0030 (14)0.0046 (14)0.0016 (13)
C40.0216 (17)0.0084 (16)0.0158 (16)0.0014 (13)0.0076 (14)0.0009 (13)
C50.0183 (17)0.0146 (17)0.0125 (16)0.0009 (13)0.0046 (13)0.0000 (13)
C60.0203 (17)0.0149 (17)0.0106 (15)0.0016 (13)0.0053 (14)0.0005 (13)
C70.0154 (16)0.0132 (17)0.0145 (16)0.0009 (13)0.0052 (13)0.0024 (13)
C80.0236 (18)0.0140 (18)0.0163 (17)0.0028 (14)0.0057 (14)0.0007 (14)
C90.0191 (17)0.0152 (18)0.0161 (17)0.0017 (14)0.0073 (14)0.0041 (14)
C100.030 (2)0.025 (2)0.0146 (17)0.0001 (16)0.0100 (15)0.0005 (14)
C110.0272 (19)0.0227 (19)0.0183 (17)0.0015 (15)0.0109 (15)0.0001 (14)
C120.0186 (18)0.024 (2)0.0247 (19)0.0020 (15)0.0049 (15)0.0004 (15)
C130.0163 (17)0.0210 (19)0.0219 (18)0.0054 (14)0.0035 (14)0.0005 (14)
C140.034 (2)0.0173 (19)0.027 (2)0.0006 (16)0.0073 (17)0.0093 (15)
C150.027 (2)0.029 (2)0.0185 (18)0.0030 (16)0.0013 (15)0.0048 (15)
C160.032 (2)0.0138 (19)0.031 (2)0.0033 (15)0.0111 (17)0.0008 (15)
C170.0269 (19)0.0135 (18)0.0262 (19)0.0031 (15)0.0052 (16)0.0031 (15)
C180.0249 (19)0.0186 (19)0.0161 (17)0.0031 (15)0.0040 (15)0.0021 (14)
C200.050 (3)0.017 (2)0.051 (3)0.0067 (19)0.010 (2)0.0016 (19)
C210.030 (2)0.027 (2)0.040 (2)0.0135 (17)0.0000 (19)0.0060 (18)
C220.0180 (18)0.038 (2)0.027 (2)0.0028 (17)0.0040 (16)0.0086 (17)
C230.0215 (19)0.036 (2)0.0207 (18)0.0013 (17)0.0002 (15)0.0027 (16)
C240.048 (3)0.030 (2)0.049 (3)0.013 (2)0.017 (2)0.012 (2)
C250.051 (3)0.042 (3)0.047 (3)0.011 (2)0.007 (2)0.023 (2)
C260.033 (2)0.065 (3)0.030 (2)0.002 (2)0.0186 (19)0.003 (2)
C270.073 (3)0.031 (2)0.021 (2)0.009 (2)0.001 (2)0.0075 (18)
C280.040 (2)0.075 (3)0.018 (2)0.002 (2)0.0127 (18)0.001 (2)
C300.027 (2)0.040 (2)0.025 (2)0.0009 (17)0.0116 (17)0.0117 (17)
C310.028 (2)0.044 (3)0.0229 (19)0.0101 (18)0.0154 (16)0.0111 (17)
C320.028 (2)0.023 (2)0.027 (2)0.0094 (16)0.0104 (17)0.0009 (16)
C330.033 (2)0.0173 (19)0.0248 (19)0.0051 (16)0.0089 (17)0.0048 (15)
C340.041 (2)0.0175 (19)0.0221 (19)0.0022 (17)0.0050 (17)0.0033 (15)
C350.035 (2)0.027 (2)0.0151 (17)0.0016 (17)0.0003 (16)0.0011 (15)
C360.0153 (18)0.036 (2)0.030 (2)0.0010 (16)0.0017 (16)0.0052 (17)
C370.029 (2)0.0155 (18)0.0209 (18)0.0055 (15)0.0062 (16)0.0012 (14)
C380.0187 (18)0.0194 (19)0.0239 (18)0.0036 (14)0.0018 (15)0.0054 (15)
Cl10.0371 (5)0.0292 (5)0.0210 (4)0.0014 (4)0.0090 (4)0.0033 (4)
O960.0341 (17)0.080 (3)0.053 (2)0.0077 (17)0.0141 (15)0.0404 (19)
O970.0434 (19)0.046 (2)0.060 (2)0.0035 (15)0.0082 (16)0.0241 (16)
O980.081 (2)0.056 (2)0.0203 (15)0.0005 (18)0.0030 (16)0.0032 (14)
O990.060 (2)0.050 (2)0.085 (3)0.0138 (17)0.043 (2)0.0031 (19)
Cl20.0406 (6)0.0256 (6)0.0790 (8)0.0072 (5)0.0345 (6)0.0163 (5)
O760.054 (2)0.0355 (19)0.085 (3)0.0025 (15)0.0348 (19)0.0224 (17)
O770.072 (4)0.082 (4)0.077 (5)0.038 (3)0.035 (3)0.019 (4)
O780.049 (3)0.052 (3)0.040 (3)0.008 (2)0.023 (2)0.002 (2)
O790.081 (5)0.046 (4)0.057 (6)0.043 (4)0.047 (5)0.025 (4)
O77A0.072 (4)0.082 (4)0.077 (5)0.038 (3)0.035 (3)0.019 (4)
O78A0.049 (3)0.052 (3)0.040 (3)0.008 (2)0.023 (2)0.002 (2)
O79A0.081 (5)0.046 (4)0.057 (6)0.043 (4)0.047 (5)0.025 (4)
O870.057 (2)0.070 (3)0.079 (3)0.018 (2)0.011 (2)0.024 (2)
Cl30.0230 (11)0.0480 (13)0.0128 (8)0.0034 (9)0.0065 (8)0.0075 (8)
O860.071 (5)0.048 (3)0.021 (3)0.021 (3)0.025 (3)0.005 (2)
O880.044 (3)0.055 (3)0.038 (3)0.015 (2)0.017 (2)0.008 (2)
O890.095 (5)0.060 (4)0.057 (4)0.017 (4)0.048 (4)0.028 (3)
Cl3A0.047 (3)0.029 (2)0.023 (2)0.000 (2)0.008 (2)0.0031 (14)
O86A0.044 (7)0.058 (7)0.037 (6)0.005 (5)0.007 (5)0.001 (5)
O88A0.053 (7)0.079 (9)0.070 (8)0.000 (6)0.030 (7)0.029 (6)
O89A0.086 (10)0.142 (13)0.018 (5)0.006 (10)0.015 (7)0.039 (6)
O520.066 (2)0.0275 (17)0.050 (2)0.0073 (16)0.0249 (18)0.0089 (14)
O530.053 (2)0.0406 (19)0.055 (2)0.0109 (16)0.0022 (17)0.0007 (16)
O540.0326 (16)0.0237 (15)0.0336 (16)0.0035 (12)0.0068 (13)0.0040 (12)
O550.0247 (14)0.0230 (14)0.0229 (13)0.0022 (11)0.0053 (11)0.0030 (11)
Geometric parameters (Å, º) top
Ni1—O32.041 (2)C16—H16B0.9800
Ni1—N12.104 (3)C16—H16C0.9800
Ni1—N32.115 (3)C17—H17A0.9800
Ni1—N22.138 (3)C17—H17B0.9800
Ni1—O22.156 (2)C17—H17C0.9800
Ni1—O12.176 (2)C18—H18A0.9800
Ni1—C72.505 (3)C18—H18B0.9800
Ni2—O62.072 (3)C18—H18C0.9800
Ni2—O52.085 (2)C20—C211.490 (6)
Ni2—N52.102 (3)C20—H20A0.9900
Ni2—N42.131 (3)C20—H20B0.9900
Ni2—N62.142 (3)C21—H21A0.9900
Ni2—O42.284 (2)C21—H21B0.9900
Ni2—C82.517 (3)C22—C231.497 (5)
Ni3—O82.036 (2)C22—H22A0.9900
Ni3—O92.059 (2)C22—H22B0.9900
Ni3—N72.107 (3)C23—H23A0.9900
Ni3—N82.111 (3)C23—H23B0.9900
Ni3—N92.127 (3)C24—H24A0.9800
O1—C71.275 (4)C24—H24B0.9800
O2—C71.261 (4)C24—H24C0.9800
O3—H3V0.915 (19)C25—H25A0.9800
O3—H3W0.93 (4)C25—H25B0.9800
O4—C81.267 (4)C25—H25C0.9800
O5—C81.259 (4)C26—H26A0.9800
O6—H6V0.930 (19)C26—H26B0.9800
O6—H6W0.91 (2)C26—H26C0.9800
O7—C91.273 (4)C27—H27A0.9800
O8—C91.254 (4)C27—H27B0.9800
O9—H9V0.908 (19)C27—H27C0.9800
O9—H9W0.913 (19)C28—H28A0.9800
N1—C141.475 (4)C28—H28B0.9800
N1—C101.484 (4)C28—H28C0.9800
N1—C151.485 (4)C30—C311.499 (5)
N2—C121.477 (4)C30—H30A0.9900
N2—C161.479 (4)C30—H30B0.9900
N2—C111.493 (4)C31—H31A0.9900
N3—C171.483 (4)C31—H31B0.9900
N3—C131.486 (4)C32—C331.508 (5)
N3—C181.486 (4)C32—H32A0.9900
N4—C201.459 (5)C32—H32B0.9900
N4—C251.471 (5)C33—H33A0.9900
N4—C241.487 (5)C33—H33B0.9900
N5—C221.477 (4)C34—H34A0.9800
N5—C261.479 (5)C34—H34B0.9800
N5—C211.496 (5)C34—H34C0.9800
N6—C271.474 (5)C35—H35A0.9800
N6—C281.488 (5)C35—H35B0.9800
N6—C231.488 (4)C35—H35C0.9800
N7—C351.470 (4)C36—H36A0.9800
N7—C341.481 (4)C36—H36B0.9800
N7—C301.487 (5)C36—H36C0.9800
N8—C361.471 (4)C37—H37A0.9800
N8—C321.480 (5)C37—H37B0.9800
N8—C311.491 (4)C37—H37C0.9800
N9—C381.481 (4)C38—H38A0.9800
N9—C371.485 (4)C38—H38B0.9800
N9—C331.487 (4)C38—H38C0.9800
C1—C21.391 (4)Cl1—O991.408 (3)
C1—C61.392 (4)Cl1—O961.426 (3)
C1—C71.494 (4)Cl1—O981.429 (3)
C2—C31.398 (5)Cl1—O971.444 (3)
C2—H20.9500Cl2—O771.338 (6)
C3—C41.395 (4)Cl2—O78A1.353 (8)
C3—C81.503 (4)Cl2—O761.398 (3)
C4—C51.390 (4)Cl2—O79A1.416 (12)
C4—H40.9500Cl2—O791.440 (7)
C5—C61.395 (4)Cl2—O781.544 (5)
C5—C91.497 (4)Cl2—O77A1.573 (10)
C6—H60.9500O87—Cl31.433 (4)
C10—C111.518 (5)O87—Cl3A1.515 (6)
C10—H10A0.9900Cl3—O891.401 (6)
C10—H10B0.9900Cl3—O881.411 (5)
C11—H11A0.9900Cl3—O861.425 (5)
C11—H11B0.9900Cl3A—O89A1.348 (12)
C12—C131.517 (5)Cl3A—O86A1.414 (12)
C12—H12A0.9900Cl3A—O88A1.435 (13)
C12—H12B0.9900O51—H51W0.94 (2)
C13—H13A0.9900O51—H51V0.94 (2)
C13—H13B0.9900O52—H52V0.95 (2)
C14—H14A0.9800O52—H52W0.95 (2)
C14—H14B0.9800O53—H53V1.00 (2)
C14—H14C0.9800O53—H53W0.99 (2)
C15—H15A0.9800O54—H54V0.933 (19)
C15—H15B0.9800O54—H54W0.92 (2)
C15—H15C0.9800O55—H55V0.914 (19)
C16—H16A0.9800O55—H55W0.909 (19)
O3—Ni1—N194.38 (10)N1—C14—H14B109.5
O3—Ni1—N392.53 (10)H14A—C14—H14B109.5
N1—Ni1—N3107.73 (11)N1—C14—H14C109.5
O3—Ni1—N2176.07 (10)H14A—C14—H14C109.5
N1—Ni1—N285.52 (11)H14B—C14—H14C109.5
N3—Ni1—N283.77 (10)N1—C15—H15A109.5
O3—Ni1—O291.26 (9)N1—C15—H15B109.5
N1—Ni1—O291.48 (10)H15A—C15—H15B109.5
N3—Ni1—O2160.05 (9)N1—C15—H15C109.5
N2—Ni1—O292.66 (9)H15A—C15—H15C109.5
O3—Ni1—O185.40 (9)H15B—C15—H15C109.5
N1—Ni1—O1152.20 (10)N2—C16—H16A109.5
N3—Ni1—O1100.04 (9)N2—C16—H16B109.5
N2—Ni1—O196.52 (9)H16A—C16—H16B109.5
O2—Ni1—O160.76 (8)N2—C16—H16C109.5
O3—Ni1—C789.48 (10)H16A—C16—H16C109.5
N1—Ni1—C7121.70 (11)H16B—C16—H16C109.5
N3—Ni1—C7130.21 (10)N3—C17—H17A109.5
N2—Ni1—C793.91 (10)N3—C17—H17B109.5
O2—Ni1—C730.23 (9)H17A—C17—H17B109.5
O1—Ni1—C730.59 (9)N3—C17—H17C109.5
O6—Ni2—O587.62 (10)H17A—C17—H17C109.5
O6—Ni2—N5174.88 (11)H17B—C17—H17C109.5
O5—Ni2—N597.32 (10)N3—C18—H18A109.5
O6—Ni2—N496.70 (12)N3—C18—H18B109.5
O5—Ni2—N490.69 (10)H18A—C18—H18B109.5
N5—Ni2—N484.62 (12)N3—C18—H18C109.5
O6—Ni2—N691.28 (11)H18A—C18—H18C109.5
O5—Ni2—N6160.36 (10)H18B—C18—H18C109.5
N5—Ni2—N683.61 (11)N4—C20—C21111.3 (3)
N4—Ni2—N6108.90 (11)N4—C20—H20A109.4
O6—Ni2—O487.62 (10)C21—C20—H20A109.4
O5—Ni2—O460.02 (8)N4—C20—H20B109.4
N5—Ni2—O493.68 (10)C21—C20—H20B109.4
N4—Ni2—O4150.28 (10)H20A—C20—H20B108.0
N6—Ni2—O4100.35 (10)C20—C21—N5109.3 (3)
O6—Ni2—C886.66 (11)C20—C21—H21A109.8
O5—Ni2—C829.91 (10)N5—C21—H21A109.8
N5—Ni2—C896.95 (11)C20—C21—H21B109.8
N4—Ni2—C8120.52 (11)N5—C21—H21B109.8
N6—Ni2—C8130.45 (11)H21A—C21—H21B108.3
O4—Ni2—C830.12 (9)N5—C22—C23111.3 (3)
O8—Ni3—O991.85 (10)N5—C22—H22A109.4
O8—Ni3—N791.07 (10)C23—C22—H22A109.4
O9—Ni3—N795.81 (10)N5—C22—H22B109.4
O8—Ni3—N895.56 (10)C23—C22—H22B109.4
O9—Ni3—N8172.46 (10)H22A—C22—H22B108.0
N7—Ni3—N885.43 (11)N6—C23—C22110.6 (3)
O8—Ni3—N9156.85 (10)N6—C23—H23A109.5
O9—Ni3—N989.35 (10)C22—C23—H23A109.5
N7—Ni3—N9111.81 (11)N6—C23—H23B109.5
N8—Ni3—N983.30 (11)C22—C23—H23B109.5
C7—O1—Ni189.13 (18)H23A—C23—H23B108.1
C7—O2—Ni190.36 (18)N4—C24—H24A109.5
Ni1—O3—H3V128 (2)N4—C24—H24B109.5
Ni1—O3—H3W122 (2)H24A—C24—H24B109.5
H3V—O3—H3W105 (3)N4—C24—H24C109.5
C8—O4—Ni285.16 (19)H24A—C24—H24C109.5
C8—O5—Ni294.38 (19)H24B—C24—H24C109.5
Ni2—O6—H6V118 (3)N4—C25—H25A109.5
Ni2—O6—H6W132 (3)N4—C25—H25B109.5
H6V—O6—H6W103 (4)H25A—C25—H25B109.5
C9—O8—Ni3101.9 (2)N4—C25—H25C109.5
Ni3—O9—H9V119 (2)H25A—C25—H25C109.5
Ni3—O9—H9W126 (2)H25B—C25—H25C109.5
H9V—O9—H9W106 (3)N5—C26—H26A109.5
C14—N1—C10110.3 (3)N5—C26—H26B109.5
C14—N1—C15106.2 (3)H26A—C26—H26B109.5
C10—N1—C15108.8 (3)N5—C26—H26C109.5
C14—N1—Ni1119.9 (2)H26A—C26—H26C109.5
C10—N1—Ni1101.01 (19)H26B—C26—H26C109.5
C15—N1—Ni1110.2 (2)N6—C27—H27A109.5
C12—N2—C16109.1 (3)N6—C27—H27B109.5
C12—N2—C11110.3 (3)H27A—C27—H27B109.5
C16—N2—C11109.1 (3)N6—C27—H27C109.5
C12—N2—Ni1107.3 (2)H27A—C27—H27C109.5
C16—N2—Ni1115.7 (2)H27B—C27—H27C109.5
C11—N2—Ni1105.3 (2)N6—C28—H28A109.5
C17—N3—C13108.8 (3)N6—C28—H28B109.5
C17—N3—C18107.4 (3)H28A—C28—H28B109.5
C13—N3—C18109.8 (3)N6—C28—H28C109.5
C17—N3—Ni1116.9 (2)H28A—C28—H28C109.5
C13—N3—Ni1105.96 (19)H28B—C28—H28C109.5
C18—N3—Ni1107.90 (19)N7—C30—C31110.3 (3)
C20—N4—C25110.6 (3)N7—C30—H30A109.6
C20—N4—C24109.3 (3)C31—C30—H30A109.6
C25—N4—C24106.0 (3)N7—C30—H30B109.6
C20—N4—Ni2102.2 (2)C31—C30—H30B109.6
C25—N4—Ni2118.4 (3)H30A—C30—H30B108.1
C24—N4—Ni2110.1 (2)N8—C31—C30109.6 (3)
C22—N5—C26109.6 (3)N8—C31—H31A109.7
C22—N5—C21110.4 (3)C30—C31—H31A109.7
C26—N5—C21108.5 (3)N8—C31—H31B109.7
C22—N5—Ni2107.5 (2)C30—C31—H31B109.7
C26—N5—Ni2114.2 (2)H31A—C31—H31B108.2
C21—N5—Ni2106.6 (2)N8—C32—C33110.6 (3)
C27—N6—C28107.8 (3)N8—C32—H32A109.5
C27—N6—C23109.7 (3)C33—C32—H32A109.5
C28—N6—C23107.9 (3)N8—C32—H32B109.5
C27—N6—Ni2107.6 (2)C33—C32—H32B109.5
C28—N6—Ni2116.9 (2)H32A—C32—H32B108.1
C23—N6—Ni2106.7 (2)N9—C33—C32110.2 (3)
C35—N7—C34107.6 (3)N9—C33—H33A109.6
C35—N7—C30111.1 (3)C32—C33—H33A109.6
C34—N7—C30107.0 (3)N9—C33—H33B109.6
C35—N7—Ni3115.7 (2)C32—C33—H33B109.6
C34—N7—Ni3111.6 (2)H33A—C33—H33B108.1
C30—N7—Ni3103.6 (2)N7—C34—H34A109.5
C36—N8—C32109.5 (3)N7—C34—H34B109.5
C36—N8—C31109.2 (3)H34A—C34—H34B109.5
C32—N8—C31110.4 (3)N7—C34—H34C109.5
C36—N8—Ni3114.8 (2)H34A—C34—H34C109.5
C32—N8—Ni3107.4 (2)H34B—C34—H34C109.5
C31—N8—Ni3105.4 (2)N7—C35—H35A109.5
C38—N9—C37107.5 (3)N7—C35—H35B109.5
C38—N9—C33109.5 (3)H35A—C35—H35B109.5
C37—N9—C33108.4 (3)N7—C35—H35C109.5
C38—N9—Ni3117.5 (2)H35A—C35—H35C109.5
C37—N9—Ni3105.77 (19)H35B—C35—H35C109.5
C33—N9—Ni3107.9 (2)N8—C36—H36A109.5
C2—C1—C6119.6 (3)N8—C36—H36B109.5
C2—C1—C7120.9 (3)H36A—C36—H36B109.5
C6—C1—C7119.4 (3)N8—C36—H36C109.5
C1—C2—C3120.4 (3)H36A—C36—H36C109.5
C1—C2—H2119.8H36B—C36—H36C109.5
C3—C2—H2119.8N9—C37—H37A109.5
C4—C3—C2119.4 (3)N9—C37—H37B109.5
C4—C3—C8119.9 (3)H37A—C37—H37B109.5
C2—C3—C8120.6 (3)N9—C37—H37C109.5
C5—C4—C3120.6 (3)H37A—C37—H37C109.5
C5—C4—H4119.7H37B—C37—H37C109.5
C3—C4—H4119.7N9—C38—H38A109.5
C4—C5—C6119.5 (3)N9—C38—H38B109.5
C4—C5—C9122.7 (3)H38A—C38—H38B109.5
C6—C5—C9117.8 (3)N9—C38—H38C109.5
C1—C6—C5120.5 (3)H38A—C38—H38C109.5
C1—C6—H6119.7H38B—C38—H38C109.5
C5—C6—H6119.7O99—Cl1—O96110.4 (2)
O2—C7—O1119.5 (3)O99—Cl1—O98112.1 (2)
O2—C7—C1120.6 (3)O96—Cl1—O98108.7 (2)
O1—C7—C1119.9 (3)O99—Cl1—O97110.6 (2)
O2—C7—Ni159.41 (16)O96—Cl1—O97107.9 (2)
O1—C7—Ni160.28 (16)O98—Cl1—O97107.1 (2)
C1—C7—Ni1174.1 (2)O77—Cl2—O78A69.5 (5)
O5—C8—O4120.4 (3)O77—Cl2—O76121.8 (4)
O5—C8—C3118.4 (3)O78A—Cl2—O76121.1 (4)
O4—C8—C3121.2 (3)O77—Cl2—O79A95.8 (10)
O5—C8—Ni255.70 (16)O78A—Cl2—O79A124.0 (10)
O4—C8—Ni264.72 (17)O76—Cl2—O79A112.6 (11)
C3—C8—Ni2173.7 (2)O77—Cl2—O79115.7 (6)
O8—C9—O7120.8 (3)O78A—Cl2—O79117.4 (6)
O8—C9—C5118.4 (3)O76—Cl2—O79107.7 (6)
O7—C9—C5120.8 (3)O77—Cl2—O78106.0 (4)
N1—C10—C11109.9 (3)O76—Cl2—O78102.7 (3)
N1—C10—H10A109.7O79A—Cl2—O78119.0 (7)
C11—C10—H10A109.7O79—Cl2—O7899.9 (4)
N1—C10—H10B109.7O78A—Cl2—O77A98.4 (6)
C11—C10—H10B109.7O76—Cl2—O77A90.8 (5)
H10A—C10—H10B108.2O79A—Cl2—O77A95.5 (8)
N2—C11—C10110.3 (3)O79—Cl2—O77A118.7 (6)
N2—C11—H11A109.6O78—Cl2—O77A132.9 (5)
C10—C11—H11A109.6O89—Cl3—O88112.8 (4)
N2—C11—H11B109.6O89—Cl3—O86113.2 (4)
C10—C11—H11B109.6O88—Cl3—O86111.0 (3)
H11A—C11—H11B108.1O89—Cl3—O87112.7 (4)
N2—C12—C13110.4 (3)O88—Cl3—O87102.9 (3)
N2—C12—H12A109.6O86—Cl3—O87103.4 (3)
C13—C12—H12A109.6O89A—Cl3A—O86A111.0 (9)
N2—C12—H12B109.6O89A—Cl3A—O88A115.6 (9)
C13—C12—H12B109.6O86A—Cl3A—O88A107.7 (7)
H12A—C12—H12B108.1O89A—Cl3A—O8797.5 (8)
N3—C13—C12110.2 (3)O86A—Cl3A—O87110.8 (6)
N3—C13—H13A109.6O88A—Cl3A—O87114.0 (6)
C12—C13—H13A109.6H51W—O51—H51V116 (10)
N3—C13—H13B109.6H52V—O52—H52W113 (5)
C12—C13—H13B109.6H53V—O53—H53W100 (4)
H13A—C13—H13B108.1H54V—O54—H54W111 (4)
N1—C14—H14A109.5H55V—O55—H55W103 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3V···O520.92 (2)1.77 (2)2.677 (4)173 (4)
O3—H3W···O7i0.93 (4)1.83 (2)2.742 (3)167 (4)
O6—H6W···O510.91 (2)1.99 (4)2.607 (9)124 (4)
O6—H6V···O54i0.93 (2)1.83 (2)2.745 (4)166 (4)
O9—H9V···O1i0.91 (2)1.85 (2)2.743 (3)166 (3)
O9—H9W···O55i0.91 (2)1.82 (2)2.727 (3)171 (4)
O52—H52V···O53i0.95 (2)2.13 (5)2.789 (5)125 (4)
O53—H53W···O70.99 (2)1.97 (3)2.877 (4)151 (5)
O53—H53V···O971.00 (2)1.96 (3)2.869 (5)151 (5)
O54—H54V···O20.93 (2)1.98 (2)2.902 (3)167 (4)
O55—H55V···O40.91 (2)1.95 (2)2.843 (3)166 (4)
O55—H55W···O76ii0.91 (2)2.04 (2)2.934 (4)168 (4)
C2—H2···O550.952.693.607 (4)162
C6—H6···O540.952.673.601 (4)166
C10—H10A···O540.992.813.697 (5)149
C11—H11B···O790.992.673.477 (11)139
C11—H11B···O79A0.992.783.56 (2)136
C15—H15A···O540.982.613.392 (5)137
C15—H15B···O520.982.663.585 (5)159
C16—H16B···O780.982.643.526 (6)150
C16—H16B···O790.982.843.396 (9)117
C17—H17A···O86A0.982.943.327 (12)105
C20—H20B···O980.992.923.310 (6)105
C21—H21B···O980.992.773.476 (5)128
C27—H27A···O550.982.803.605 (5)140
C28—H28A···O510.982.983.941 (10)169
C30—H30B···O770.992.763.603 (9)143
C30—H30B···O77A0.992.823.513 (15)128
C30—H30B···O78A0.992.693.677 (11)175
C34—H34B···O540.982.523.293 (5)136
C36—H36B···O780.982.663.579 (6)157
C36—H36B···O78A0.982.813.783 (11)171
C37—H37A···O530.982.853.803 (5)164
C34—H34A···O55i0.982.533.487 (5)165
C37—H37C···O89i0.982.573.337 (7)136
C37—H37C···O89Ai0.982.573.417 (16)145
C25—H25B···O88iii0.982.573.518 (7)162
C25—H25B···O88Aiii0.982.783.704 (12)157
C24—H24B···O88iii0.982.933.797 (7)148
C24—H24B···O89iii0.982.583.439 (9)146
C15—H15C···O89Aiv0.982.933.762 (15)143
C14—H14A···O89Aiv0.982.553.498 (12)162
C15—H15C···O89iv0.982.603.508 (7)154
C14—H14A···O89iv0.982.873.739 (8)149
C10—H10B···O87iv0.992.683.564 (5)148
C11—H11A···O97ii0.992.633.612 (5)172
C12—H12A···O78ii0.992.793.646 (7)145
C16—H16A···O78ii0.982.833.462 (7)123
C26—H26C···O79ii0.982.723.580 (8)146
C26—H26C···O79Aii0.982.453.276 (14)142
C14—H14C···O96ii0.982.743.423 (5)127
C14—H14C···O97ii0.982.863.754 (5)153
C18—H18C···O76ii0.982.953.809 (5)147
C13—H13A···O97ii0.992.703.562 (5)146
C17—H17C···O98v0.982.573.411 (5)143
C18—H18A···O98v0.982.883.634 (5)134
C21—H21A···O96vi0.992.873.836 (5)165
C23—H23B···O96vi0.992.843.832 (5)177
C25—H25C···O53vi0.982.613.452 (5)145
C25—H25A···O96vi0.982.443.314 (5)148
C25—H25A···O99vi0.982.943.464 (6)115
C22—H22A···O86Avii0.992.553.488 (12)158
C21—H21B···O86Avii0.992.863.395 (13)115
C26—H26A···O87vii0.982.493.405 (6)154
C22—H22A···O87vii0.992.803.512 (5)130
C28—H28C···O76viii0.982.653.614 (5)169
C35—H35C···O51ix0.982.633.390 (9)134
C30—H30A···O51ix0.992.673.565 (9)151
C33—H33B···O52x0.992.963.397 (5)108
C33—H33B···O86x0.992.373.333 (6)164
C35—H35A···O86x0.982.563.510 (6)163
C35—H35A···O86Ax0.982.883.756 (12)149
C33—H33B···O86Ax0.992.823.689 (11)147
C33—H33B···O88Ax0.992.763.715 (12)162
C33—H33B···O52x0.992.963.397 (5)108
C38—H38B···O86x0.982.813.614 (6)140
C38—H38B···O86Ax0.982.573.395 (10)141
C31—H31B···O86x0.992.983.960 (7)170
C31—H31B···O88x0.992.643.427 (6)136
C31—H31B···O88Ax0.992.603.548 (14)161
C32—H32A···O99xi0.992.773.731 (5)165
C38—H38C···O96xii0.982.753.371 (5)122
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x+1, y+1/2, z+1/2; (iv) x, y+1/2, z+1/2; (v) x, y1/2, z+1/2; (vi) x, y+3/2, z1/2; (vii) x, y+1/2, z+1/2; (viii) x, y, z1; (ix) x, y, z+1; (x) x+1, y+1/2, z+3/2; (xi) x, y+3/2, z+1/2; (xii) x+1, y+3/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Ni3(C9H3O6)(C9H23N3)3(H2O)3](ClO4)3·4.25H2O
Mr1332.12
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)11.7409 (2), 30.6727 (5), 16.9590 (4)
β (°) 107.633 (2)
V3)5820.41 (19)
Z4
Radiation typeMo Kα
µ (mm1)1.18
Crystal size (mm)0.30 × 0.30 × 0.25
Data collection
DiffractometerOxford Diffraction Xcalibur2 + CCD
Absorption correctionMulti-scan
(CrysAlis RED; Oxford Diffraction, 2006)
Tmin, Tmax0.655, 0.740
No. of measured, independent and
observed [I > 2σ(I)] reflections
27090, 10209, 8075
Rint0.025
(sin θ/λ)max1)0.597
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.096, 1.01
No. of reflections10209
No. of parameters799
No. of restraints26
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
w = 1/[σ2(Fo2) + (0.03P)2 + 15P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.01, 1.02

Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2006).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3V···O520.915 (19)1.77 (2)2.677 (4)173 (4)
O3—H3W···O7i0.93 (4)1.83 (2)2.742 (3)167 (4)
O6—H6W···O510.91 (2)1.99 (4)2.607 (9)124 (4)
O6—H6V···O54i0.930 (19)1.83 (2)2.745 (4)166 (4)
O9—H9V···O1i0.908 (19)1.85 (2)2.743 (3)166 (3)
O9—H9W···O55i0.913 (19)1.82 (2)2.727 (3)171 (4)
O52—H52V···O53i0.95 (2)2.13 (5)2.789 (5)125 (4)
O53—H53W···O70.99 (2)1.97 (3)2.877 (4)151 (5)
O53—H53V···O971.00 (2)1.96 (3)2.869 (5)151 (5)
O54—H54V···O20.933 (19)1.98 (2)2.902 (3)167 (4)
O55—H55V···O40.914 (19)1.95 (2)2.843 (3)166 (4)
O55—H55W···O76ii0.909 (19)2.04 (2)2.934 (4)168 (4)
C2—H2···O550.952.693.607 (4)162.4
C6—H6···O540.952.673.601 (4)166.4
C10—H10A···O540.992.813.697 (5)149.0
C11—H11B···O790.992.673.477 (11)139.1
C11—H11B···O79A0.992.783.56 (2)135.9
C15—H15A···O540.982.613.392 (5)137.0
C15—H15B···O520.982.663.585 (5)158.6
C16—H16B···O780.982.643.526 (6)149.9
C16—H16B···O790.982.843.396 (9)116.7
C17—H17A···O86A0.982.943.327 (12)104.7
C20—H20B···O980.992.923.310 (6)104.5
C21—H21B···O980.992.773.476 (5)128.3
C27—H27A···O550.982.803.605 (5)140.0
C28—H28A···O510.982.983.941 (10)168.8
C30—H30B···O770.992.763.603 (9)143.4
C30—H30B···O77A0.992.823.513 (15)127.9
C30—H30B···O78A0.992.693.677 (11)175.1
C34—H34B···O540.982.523.293 (5)135.9
C36—H36B···O780.982.663.579 (6)157.3
C36—H36B···O78A0.982.813.783 (11)170.8
C37—H37A···O530.982.853.803 (5)164.4
C34—H34A···O55i0.982.533.487 (5)165.3
C37—H37C···O89i0.982.573.337 (7)135.6
C37—H37C···O89Ai0.982.573.417 (16)144.9
C25—H25B···O88iii0.982.573.518 (7)162.0
C25—H25B···O88Aiii0.982.783.704 (12)157.1
C24—H24B···O88iii0.982.933.797 (7)147.6
C24—H24B···O89iii0.982.583.439 (9)146.3
C15—H15C···O89Aiv0.982.933.762 (15)143.1
C14—H14A···O89Aiv0.982.553.498 (12)162.0
C15—H15C···O89iv0.982.603.508 (7)154.2
C14—H14A···O89iv0.982.873.739 (8)148.9
C10—H10B···O87iv0.992.683.564 (5)148.3
C11—H11A···O97ii0.992.633.612 (5)171.9
C12—H12A···O78ii0.992.793.646 (7)145.0
C16—H16A···O78ii0.982.833.462 (7)122.9
C26—H26C···O79ii0.982.723.580 (8)146.1
C26—H26C···O79Aii0.982.453.276 (14)142.0
C14—H14C···O96ii0.982.743.423 (5)127.4
C14—H14C···O97ii0.982.863.754 (5)152.7
C18—H18C···O76ii0.982.953.809 (5)146.7
C13—H13A···O97ii0.992.703.562 (5)146.1
C17—H17C···O98v0.982.573.411 (5)143.4
C18—H18A···O98v0.982.883.634 (5)134.1
C21—H21A···O96vi0.992.873.836 (5)164.5
C23—H23B···O96vi0.992.843.832 (5)176.6
C25—H25C···O53vi0.982.613.452 (5)144.5
C25—H25A···O96vi0.982.443.314 (5)148.1
C25—H25A···O99vi0.982.943.464 (6)114.5
C22—H22A···O86Avii0.992.553.488 (12)157.9
C21—H21B···O86Avii0.992.863.395 (13)114.7
C26—H26A···O87vii0.982.493.405 (6)154.4
C22—H22A···O87vii0.992.803.512 (5)129.6
C28—H28C···O76viii0.982.653.614 (5)168.6
C35—H35C···O51ix0.982.633.390 (9)134.3
C30—H30A···O51ix0.992.673.565 (9)151.3
C33—H33B···O52x0.992.963.397 (5)107.8
C33—H33B···O86x0.992.373.333 (6)164.4
C35—H35A···O86x0.982.563.510 (6)162.7
C35—H35A···O86Ax0.982.883.756 (12)149.1
C33—H33B···O86Ax0.992.823.689 (11)146.5
C33—H33B···O88Ax0.992.763.715 (12)161.5
C33—H33B···O52x0.992.963.397 (5)107.8
C38—H38B···O86x0.982.813.614 (6)139.8
C38—H38B···O86Ax0.982.573.395 (10)141.4
C31—H31B···O86x0.992.983.960 (7)170.1
C31—H31B···O88x0.992.643.427 (6)136.2
C31—H31B···O88Ax0.992.603.548 (14)160.8
C32—H32A···O99xi0.992.773.731 (5)164.5
C38—H38C···O96xii0.982.753.371 (5)121.7
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x+1, y+1/2, z+1/2; (iv) x, y+1/2, z+1/2; (v) x, y1/2, z+1/2; (vi) x, y+3/2, z1/2; (vii) x, y+1/2, z+1/2; (viii) x, y, z1; (ix) x, y, z+1; (x) x+1, y+1/2, z+3/2; (xi) x, y+3/2, z+1/2; (xii) x+1, y+3/2, z+1/2.
 

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