Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807051938/tk2201sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807051938/tk2201Isup2.hkl |
CCDC reference: 667252
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (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
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).
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.
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.
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).
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).
[Ni3(C9H3O6)(C9H23N3)3(H2O)3](ClO4)3·4.25H2O | F(000) = 2810 |
Mr = 1332.12 | Dx = 1.520 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 25991 reflections |
a = 11.7409 (2) Å | θ = 2.6–32.0° |
b = 30.6727 (5) Å | µ = 1.18 mm−1 |
c = 16.9590 (4) Å | T = 100 K |
β = 107.633 (2)° | Prism, dark-green |
V = 5820.41 (19) Å3 | 0.30 × 0.30 × 0.25 mm |
Z = 4 |
Oxford Diffraction Xcalibur2 + CCD diffractometer | 10209 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 8075 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
Detector resolution: 8.3611 pixels mm-1 | θmax = 25.1°, θmin = 2.6° |
ω scans | h = −13→13 |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006) | k = −35→28 |
Tmin = 0.655, Tmax = 0.740 | l = −20→20 |
27090 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.096 | H 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 parameters | Δρmax = 1.01 e Å−3 |
26 restraints | Δρmin = −1.02 e Å−3 |
[Ni3(C9H3O6)(C9H23N3)3(H2O)3](ClO4)3·4.25H2O | V = 5820.41 (19) Å3 |
Mr = 1332.12 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.7409 (2) Å | µ = 1.18 mm−1 |
b = 30.6727 (5) Å | T = 100 K |
c = 16.9590 (4) Å | 0.30 × 0.30 × 0.25 mm |
β = 107.633 (2)° |
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 = 0.740 | Rint = 0.025 |
27090 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 26 restraints |
wR(F2) = 0.096 | H 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 | Δρmax = 1.01 e Å−3 |
799 parameters | Δρmin = −1.02 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.18931 (4) | 0.372432 (13) | 0.49777 (2) | 0.01350 (10) | |
Ni2 | 0.24189 (4) | 0.612514 (14) | 0.15475 (2) | 0.01464 (10) | |
Ni3 | 0.57687 (4) | 0.611801 (13) | 0.74650 (2) | 0.01328 (10) | |
O1 | 0.2105 (2) | 0.42302 (7) | 0.41337 (13) | 0.0167 (5) | |
O2 | 0.2956 (2) | 0.42913 (7) | 0.54701 (13) | 0.0167 (5) | |
O3 | 0.3311 (2) | 0.34306 (8) | 0.47357 (15) | 0.0201 (5) | |
H3V | 0.371 (3) | 0.3184 (9) | 0.497 (2) | 0.030* | |
H3W | 0.386 (3) | 0.3588 (11) | 0.455 (2) | 0.030* | |
O4 | 0.2287 (2) | 0.55024 (7) | 0.22527 (13) | 0.0221 (5) | |
O5 | 0.3051 (2) | 0.61172 (7) | 0.28366 (13) | 0.0202 (5) | |
O6 | 0.4100 (2) | 0.59180 (10) | 0.15492 (16) | 0.0314 (6) | |
H6V | 0.460 (3) | 0.5804 (14) | 0.2039 (18) | 0.047* | |
H6W | 0.462 (3) | 0.6017 (14) | 0.128 (3) | 0.047* | |
O7 | 0.5043 (2) | 0.62186 (7) | 0.59350 (14) | 0.0201 (5) | |
O8 | 0.4838 (2) | 0.56524 (8) | 0.66740 (13) | 0.0208 (5) | |
O9 | 0.7360 (2) | 0.59170 (8) | 0.73098 (14) | 0.0179 (5) | |
H9V | 0.741 (3) | 0.5875 (12) | 0.6791 (14) | 0.027* | |
H9W | 0.789 (3) | 0.5725 (10) | 0.764 (2) | 0.027* | |
N1 | 0.2254 (3) | 0.34506 (9) | 0.61657 (17) | 0.0187 (6) | |
N2 | 0.0337 (2) | 0.39932 (9) | 0.51974 (16) | 0.0165 (6) | |
N3 | 0.0646 (2) | 0.33156 (9) | 0.41396 (16) | 0.0163 (6) | |
N4 | 0.2765 (3) | 0.68067 (10) | 0.15369 (19) | 0.0262 (7) | |
N5 | 0.0659 (2) | 0.63192 (9) | 0.14337 (17) | 0.0201 (6) | |
N6 | 0.1648 (3) | 0.59061 (10) | 0.02995 (17) | 0.0217 (6) | |
N7 | 0.5875 (2) | 0.57154 (9) | 0.84912 (16) | 0.0184 (6) | |
N8 | 0.4263 (2) | 0.63958 (9) | 0.77056 (16) | 0.0184 (6) | |
N9 | 0.6533 (2) | 0.67424 (9) | 0.78328 (16) | 0.0168 (6) | |
C1 | 0.3081 (3) | 0.49073 (10) | 0.46320 (19) | 0.0135 (7) | |
C2 | 0.2790 (3) | 0.50910 (11) | 0.38461 (19) | 0.0155 (7) | |
H2 | 0.2363 | 0.4924 | 0.3378 | 0.019* | |
C3 | 0.3123 (3) | 0.55197 (11) | 0.37416 (19) | 0.0158 (7) | |
C4 | 0.3748 (3) | 0.57623 (10) | 0.44331 (19) | 0.0148 (7) | |
H4 | 0.3982 | 0.6053 | 0.4365 | 0.018* | |
C5 | 0.4032 (3) | 0.55825 (10) | 0.52214 (19) | 0.0151 (7) | |
C6 | 0.3696 (3) | 0.51542 (10) | 0.53177 (19) | 0.0151 (7) | |
H6 | 0.3889 | 0.5030 | 0.5855 | 0.018* | |
C7 | 0.2709 (3) | 0.44529 (10) | 0.47542 (19) | 0.0142 (7) | |
C8 | 0.2798 (3) | 0.57222 (11) | 0.2895 (2) | 0.0181 (7) | |
C9 | 0.4679 (3) | 0.58317 (11) | 0.59844 (19) | 0.0163 (7) | |
C10 | 0.1662 (3) | 0.37705 (12) | 0.6569 (2) | 0.0225 (8) | |
H10A | 0.2098 | 0.4051 | 0.6643 | 0.027* | |
H10B | 0.1679 | 0.3662 | 0.7122 | 0.027* | |
C11 | 0.0378 (3) | 0.38396 (12) | 0.6041 (2) | 0.0218 (8) | |
H11A | −0.0070 | 0.3563 | 0.5996 | 0.026* | |
H11B | −0.0008 | 0.4058 | 0.6306 | 0.026* | |
C12 | −0.0713 (3) | 0.38080 (11) | 0.4570 (2) | 0.0229 (8) | |
H12A | −0.0898 | 0.3985 | 0.4058 | 0.027* | |
H12B | −0.1415 | 0.3818 | 0.4778 | 0.027* | |
C13 | −0.0470 (3) | 0.33401 (11) | 0.4378 (2) | 0.0202 (7) | |
H13A | −0.0391 | 0.3156 | 0.4871 | 0.024* | |
H13B | −0.1149 | 0.3229 | 0.3921 | 0.024* | |
C14 | 0.1844 (3) | 0.30049 (12) | 0.6262 (2) | 0.0266 (8) | |
H14A | 0.2016 | 0.2938 | 0.6852 | 0.040* | |
H14B | 0.2262 | 0.2796 | 0.6010 | 0.040* | |
H14C | 0.0981 | 0.2984 | 0.5989 | 0.040* | |
C15 | 0.3560 (3) | 0.34564 (13) | 0.6598 (2) | 0.0260 (8) | |
H15A | 0.3897 | 0.3734 | 0.6489 | 0.039* | |
H15B | 0.3944 | 0.3216 | 0.6394 | 0.039* | |
H15C | 0.3700 | 0.3423 | 0.7194 | 0.039* | |
C16 | 0.0250 (3) | 0.44741 (11) | 0.5169 (2) | 0.0251 (8) | |
H16A | 0.0267 | 0.4578 | 0.4627 | 0.038* | |
H16B | 0.0926 | 0.4599 | 0.5601 | 0.038* | |
H16C | −0.0500 | 0.4564 | 0.5262 | 0.038* | |
C17 | 0.0983 (3) | 0.28511 (11) | 0.4114 (2) | 0.0228 (8) | |
H17A | 0.1048 | 0.2713 | 0.4647 | 0.034* | |
H17B | 0.1754 | 0.2832 | 0.4003 | 0.034* | |
H17C | 0.0371 | 0.2701 | 0.3674 | 0.034* | |
C18 | 0.0431 (3) | 0.34967 (11) | 0.3294 (2) | 0.0204 (7) | |
H18A | −0.0186 | 0.3324 | 0.2898 | 0.031* | |
H18B | 0.1173 | 0.3485 | 0.3144 | 0.031* | |
H18C | 0.0165 | 0.3800 | 0.3283 | 0.031* | |
C20 | 0.1797 (4) | 0.69925 (13) | 0.1802 (3) | 0.0408 (11) | |
H20A | 0.1777 | 0.7312 | 0.1720 | 0.049* | |
H20B | 0.1947 | 0.6935 | 0.2399 | 0.049* | |
C21 | 0.0620 (4) | 0.68036 (13) | 0.1327 (3) | 0.0348 (10) | |
H21A | 0.0439 | 0.6877 | 0.0733 | 0.042* | |
H21B | −0.0018 | 0.6928 | 0.1529 | 0.042* | |
C22 | −0.0135 (3) | 0.61055 (14) | 0.0689 (2) | 0.0284 (9) | |
H22A | −0.0902 | 0.6266 | 0.0501 | 0.034* | |
H22B | −0.0306 | 0.5804 | 0.0828 | 0.034* | |
C23 | 0.0423 (3) | 0.60938 (13) | 0.0003 (2) | 0.0275 (8) | |
H23A | −0.0077 | 0.5915 | −0.0459 | 0.033* | |
H23B | 0.0462 | 0.6393 | −0.0205 | 0.033* | |
C24 | 0.3929 (4) | 0.69117 (15) | 0.2159 (3) | 0.0495 (13) | |
H24A | 0.4008 | 0.7229 | 0.2228 | 0.074* | |
H24B | 0.4582 | 0.6799 | 0.1969 | 0.074* | |
H24C | 0.3964 | 0.6776 | 0.2689 | 0.074* | |
C25 | 0.2803 (4) | 0.70070 (15) | 0.0757 (3) | 0.0484 (12) | |
H25A | 0.2038 | 0.6959 | 0.0329 | 0.073* | |
H25B | 0.3447 | 0.6874 | 0.0583 | 0.073* | |
H25C | 0.2949 | 0.7321 | 0.0839 | 0.073* | |
C26 | 0.0262 (4) | 0.62113 (16) | 0.2159 (3) | 0.0404 (11) | |
H26A | −0.0572 | 0.6301 | 0.2052 | 0.061* | |
H26B | 0.0765 | 0.6365 | 0.2647 | 0.061* | |
H26C | 0.0329 | 0.5896 | 0.2257 | 0.061* | |
C27 | 0.1576 (5) | 0.54266 (14) | 0.0316 (2) | 0.0452 (12) | |
H27A | 0.1102 | 0.5339 | 0.0676 | 0.068* | |
H27B | 0.2383 | 0.5305 | 0.0529 | 0.068* | |
H27C | 0.1196 | 0.5318 | −0.0245 | 0.068* | |
C28 | 0.2286 (4) | 0.60271 (17) | −0.0305 (2) | 0.0434 (12) | |
H28A | 0.3105 | 0.5915 | −0.0114 | 0.065* | |
H28B | 0.2304 | 0.6345 | −0.0352 | 0.065* | |
H28C | 0.1868 | 0.5901 | −0.0846 | 0.065* | |
C30 | 0.4667 (3) | 0.57526 (13) | 0.8598 (2) | 0.0298 (9) | |
H30A | 0.4687 | 0.5637 | 0.9147 | 0.036* | |
H30B | 0.4090 | 0.5577 | 0.8170 | 0.036* | |
C31 | 0.4271 (3) | 0.62195 (13) | 0.8527 (2) | 0.0299 (9) | |
H31A | 0.3460 | 0.6240 | 0.8587 | 0.036* | |
H31B | 0.4822 | 0.6393 | 0.8974 | 0.036* | |
C32 | 0.4437 (3) | 0.68742 (12) | 0.7751 (2) | 0.0258 (8) | |
H32A | 0.3910 | 0.7006 | 0.8044 | 0.031* | |
H32B | 0.4214 | 0.6997 | 0.7185 | 0.031* | |
C33 | 0.5721 (3) | 0.69852 (12) | 0.8200 (2) | 0.0248 (8) | |
H33A | 0.5847 | 0.7303 | 0.8161 | 0.030* | |
H33B | 0.5904 | 0.6908 | 0.8793 | 0.030* | |
C34 | 0.6044 (4) | 0.52518 (12) | 0.8308 (2) | 0.0280 (9) | |
H34A | 0.6860 | 0.5208 | 0.8285 | 0.042* | |
H34B | 0.5473 | 0.5173 | 0.7774 | 0.042* | |
H34C | 0.5910 | 0.5068 | 0.8744 | 0.042* | |
C35 | 0.6812 (3) | 0.58291 (12) | 0.9259 (2) | 0.0274 (8) | |
H35A | 0.6694 | 0.6130 | 0.9415 | 0.041* | |
H35B | 0.7597 | 0.5803 | 0.9172 | 0.041* | |
H35C | 0.6770 | 0.5631 | 0.9702 | 0.041* | |
C36 | 0.3111 (3) | 0.62924 (13) | 0.7090 (2) | 0.0284 (9) | |
H36A | 0.2462 | 0.6427 | 0.7257 | 0.043* | |
H36B | 0.2999 | 0.5976 | 0.7056 | 0.043* | |
H36C | 0.3103 | 0.6406 | 0.6549 | 0.043* | |
C37 | 0.6541 (3) | 0.69661 (11) | 0.7058 (2) | 0.0222 (8) | |
H37A | 0.5724 | 0.6982 | 0.6680 | 0.033* | |
H37B | 0.7045 | 0.6803 | 0.6795 | 0.033* | |
H37C | 0.6860 | 0.7262 | 0.7187 | 0.033* | |
C38 | 0.7766 (3) | 0.67569 (12) | 0.8407 (2) | 0.0217 (8) | |
H38A | 0.8290 | 0.6578 | 0.8185 | 0.033* | |
H38B | 0.7772 | 0.6644 | 0.8948 | 0.033* | |
H38C | 0.8053 | 0.7059 | 0.8467 | 0.033* | |
Cl1 | 0.10417 (9) | 0.75444 (3) | 0.36681 (5) | 0.0291 (2) | |
O96 | 0.0428 (3) | 0.77425 (12) | 0.4183 (2) | 0.0558 (10) | |
O97 | 0.1431 (3) | 0.71176 (11) | 0.4000 (2) | 0.0516 (9) | |
O98 | 0.0216 (3) | 0.74819 (11) | 0.28622 (17) | 0.0551 (9) | |
O99 | 0.2026 (3) | 0.78013 (11) | 0.3648 (2) | 0.0599 (10) | |
Cl2 | 0.15471 (10) | 0.50855 (3) | 0.74728 (8) | 0.0448 (3) | |
O76 | 0.1141 (3) | 0.54718 (10) | 0.7734 (2) | 0.0553 (9) | |
O77 | 0.2529 (6) | 0.4881 (2) | 0.7936 (4) | 0.0741 (18) | 0.632 (5) |
O78 | 0.1822 (5) | 0.52275 (18) | 0.6676 (3) | 0.0445 (12) | 0.632 (5) |
O79 | 0.0522 (10) | 0.4811 (3) | 0.7122 (4) | 0.056 (3) | 0.632 (5) |
O77A | 0.2363 (10) | 0.4990 (4) | 0.8379 (6) | 0.0741 (18) | 0.368 (5) |
O78A | 0.2408 (8) | 0.5090 (3) | 0.7093 (6) | 0.0445 (12) | 0.368 (5) |
O79A | 0.0760 (19) | 0.4731 (6) | 0.7436 (9) | 0.056 (3) | 0.368 (5) |
O87 | 0.2731 (3) | 0.13286 (13) | 0.3765 (3) | 0.0711 (11) | |
Cl3 | 0.3567 (2) | 0.16715 (9) | 0.40985 (12) | 0.0277 (6) | 0.663 (7) |
O86 | 0.3186 (6) | 0.18374 (16) | 0.4762 (3) | 0.0439 (15) | 0.663 (7) |
O88 | 0.4662 (4) | 0.14462 (16) | 0.4400 (3) | 0.0447 (15) | 0.663 (7) |
O89 | 0.3589 (7) | 0.1989 (2) | 0.3509 (4) | 0.065 (2) | 0.663 (7) |
Cl3A | 0.3081 (7) | 0.17759 (15) | 0.4139 (3) | 0.0338 (13) | 0.337 (7) |
O86A | 0.2359 (11) | 0.1898 (4) | 0.4636 (6) | 0.048 (3) | 0.337 (7) |
O88A | 0.4306 (10) | 0.1809 (4) | 0.4639 (7) | 0.065 (4) | 0.337 (7) |
O89A | 0.2786 (15) | 0.2004 (6) | 0.3427 (7) | 0.082 (5) | 0.337 (7) |
O51 | 0.5580 (8) | 0.5631 (3) | 0.0792 (5) | 0.0141 (18)* | 0.25 |
H51W | 0.603 (10) | 0.589 (2) | 0.092 (8) | 0.021* | 0.25 |
H51V | 0.600 (10) | 0.537 (2) | 0.099 (8) | 0.021* | 0.25 |
O52 | 0.4498 (3) | 0.26949 (10) | 0.5315 (2) | 0.0464 (8) | |
H52V | 0.532 (2) | 0.2783 (17) | 0.551 (3) | 0.070* | |
H52W | 0.437 (5) | 0.2448 (12) | 0.497 (3) | 0.070* | |
O53 | 0.3673 (3) | 0.69819 (11) | 0.5254 (2) | 0.0527 (9) | |
H53V | 0.301 (4) | 0.6950 (18) | 0.473 (2) | 0.079* | |
H53W | 0.390 (5) | 0.6671 (8) | 0.536 (3) | 0.079* | |
O54 | 0.4280 (2) | 0.45053 (9) | 0.71672 (17) | 0.0337 (7) | |
H54V | 0.396 (4) | 0.4442 (15) | 0.6605 (14) | 0.051* | |
H54W | 0.372 (3) | 0.4644 (14) | 0.737 (3) | 0.051* | |
O55 | 0.1060 (2) | 0.46955 (8) | 0.18374 (15) | 0.0240 (5) | |
H55V | 0.137 (3) | 0.4963 (8) | 0.202 (2) | 0.036* | |
H55W | 0.038 (2) | 0.4686 (14) | 0.199 (2) | 0.036* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0180 (2) | 0.0101 (2) | 0.0119 (2) | −0.00242 (17) | 0.00381 (17) | 0.00048 (16) |
Ni2 | 0.0188 (2) | 0.0142 (2) | 0.0104 (2) | 0.00220 (17) | 0.00359 (17) | 0.00279 (16) |
Ni3 | 0.0161 (2) | 0.0127 (2) | 0.0099 (2) | −0.00199 (17) | 0.00225 (16) | −0.00155 (16) |
O1 | 0.0238 (12) | 0.0128 (12) | 0.0123 (11) | −0.0053 (10) | 0.0037 (10) | −0.0014 (9) |
O2 | 0.0246 (13) | 0.0132 (12) | 0.0112 (11) | −0.0036 (10) | 0.0039 (10) | 0.0011 (9) |
O3 | 0.0223 (13) | 0.0155 (13) | 0.0257 (13) | 0.0018 (10) | 0.0122 (11) | 0.0044 (10) |
O4 | 0.0358 (14) | 0.0153 (12) | 0.0109 (11) | 0.0004 (11) | 0.0005 (11) | 0.0007 (10) |
O5 | 0.0328 (14) | 0.0124 (12) | 0.0131 (11) | 0.0000 (10) | 0.0034 (10) | 0.0019 (9) |
O6 | 0.0211 (14) | 0.0443 (17) | 0.0267 (14) | 0.0087 (12) | 0.0041 (11) | 0.0030 (13) |
O7 | 0.0254 (13) | 0.0146 (13) | 0.0226 (12) | −0.0069 (10) | 0.0105 (11) | −0.0053 (10) |
O8 | 0.0296 (14) | 0.0193 (13) | 0.0104 (11) | −0.0080 (10) | 0.0016 (10) | −0.0031 (9) |
O9 | 0.0208 (13) | 0.0183 (13) | 0.0154 (12) | 0.0037 (10) | 0.0068 (10) | −0.0008 (10) |
N1 | 0.0251 (16) | 0.0163 (15) | 0.0151 (14) | 0.0008 (12) | 0.0070 (12) | 0.0020 (11) |
N2 | 0.0189 (15) | 0.0126 (15) | 0.0167 (14) | 0.0003 (11) | 0.0034 (12) | 0.0011 (11) |
N3 | 0.0191 (14) | 0.0117 (14) | 0.0170 (14) | −0.0033 (11) | 0.0038 (12) | −0.0007 (11) |
N4 | 0.0261 (17) | 0.0185 (16) | 0.0258 (16) | −0.0022 (13) | −0.0046 (13) | 0.0096 (13) |
N5 | 0.0206 (15) | 0.0230 (16) | 0.0175 (14) | 0.0028 (12) | 0.0069 (12) | 0.0005 (12) |
N6 | 0.0240 (16) | 0.0279 (17) | 0.0138 (14) | 0.0045 (13) | 0.0065 (12) | 0.0012 (12) |
N7 | 0.0230 (15) | 0.0180 (15) | 0.0127 (14) | 0.0021 (12) | 0.0032 (12) | 0.0010 (11) |
N8 | 0.0165 (14) | 0.0236 (16) | 0.0145 (14) | 0.0029 (12) | 0.0039 (12) | 0.0032 (12) |
N9 | 0.0191 (14) | 0.0140 (15) | 0.0161 (14) | 0.0001 (11) | 0.0035 (12) | −0.0034 (11) |
C1 | 0.0143 (16) | 0.0117 (16) | 0.0143 (16) | −0.0014 (13) | 0.0042 (13) | −0.0005 (13) |
C2 | 0.0213 (17) | 0.0146 (17) | 0.0101 (15) | 0.0013 (14) | 0.0038 (13) | −0.0022 (13) |
C3 | 0.0219 (18) | 0.0137 (17) | 0.0116 (16) | 0.0030 (14) | 0.0046 (14) | 0.0016 (13) |
C4 | 0.0216 (17) | 0.0084 (16) | 0.0158 (16) | −0.0014 (13) | 0.0076 (14) | −0.0009 (13) |
C5 | 0.0183 (17) | 0.0146 (17) | 0.0125 (16) | −0.0009 (13) | 0.0046 (13) | 0.0000 (13) |
C6 | 0.0203 (17) | 0.0149 (17) | 0.0106 (15) | −0.0016 (13) | 0.0053 (14) | 0.0005 (13) |
C7 | 0.0154 (16) | 0.0132 (17) | 0.0145 (16) | −0.0009 (13) | 0.0052 (13) | −0.0024 (13) |
C8 | 0.0236 (18) | 0.0140 (18) | 0.0163 (17) | 0.0028 (14) | 0.0057 (14) | −0.0007 (14) |
C9 | 0.0191 (17) | 0.0152 (18) | 0.0161 (17) | −0.0017 (14) | 0.0073 (14) | −0.0041 (14) |
C10 | 0.030 (2) | 0.025 (2) | 0.0146 (17) | −0.0001 (16) | 0.0100 (15) | 0.0005 (14) |
C11 | 0.0272 (19) | 0.0227 (19) | 0.0183 (17) | −0.0015 (15) | 0.0109 (15) | 0.0001 (14) |
C12 | 0.0186 (18) | 0.024 (2) | 0.0247 (19) | −0.0020 (15) | 0.0049 (15) | −0.0004 (15) |
C13 | 0.0163 (17) | 0.0210 (19) | 0.0219 (18) | −0.0054 (14) | 0.0035 (14) | 0.0005 (14) |
C14 | 0.034 (2) | 0.0173 (19) | 0.027 (2) | 0.0006 (16) | 0.0073 (17) | 0.0093 (15) |
C15 | 0.027 (2) | 0.029 (2) | 0.0185 (18) | 0.0030 (16) | 0.0013 (15) | 0.0048 (15) |
C16 | 0.032 (2) | 0.0138 (19) | 0.031 (2) | 0.0033 (15) | 0.0111 (17) | 0.0008 (15) |
C17 | 0.0269 (19) | 0.0135 (18) | 0.0262 (19) | −0.0031 (15) | 0.0052 (16) | −0.0031 (15) |
C18 | 0.0249 (19) | 0.0186 (19) | 0.0161 (17) | −0.0031 (15) | 0.0040 (15) | −0.0021 (14) |
C20 | 0.050 (3) | 0.017 (2) | 0.051 (3) | 0.0067 (19) | 0.010 (2) | −0.0016 (19) |
C21 | 0.030 (2) | 0.027 (2) | 0.040 (2) | 0.0135 (17) | 0.0000 (19) | −0.0060 (18) |
C22 | 0.0180 (18) | 0.038 (2) | 0.027 (2) | −0.0028 (17) | 0.0040 (16) | −0.0086 (17) |
C23 | 0.0215 (19) | 0.036 (2) | 0.0207 (18) | 0.0013 (17) | 0.0002 (15) | −0.0027 (16) |
C24 | 0.048 (3) | 0.030 (2) | 0.049 (3) | −0.013 (2) | −0.017 (2) | 0.012 (2) |
C25 | 0.051 (3) | 0.042 (3) | 0.047 (3) | −0.011 (2) | 0.007 (2) | 0.023 (2) |
C26 | 0.033 (2) | 0.065 (3) | 0.030 (2) | 0.002 (2) | 0.0186 (19) | 0.003 (2) |
C27 | 0.073 (3) | 0.031 (2) | 0.021 (2) | 0.009 (2) | −0.001 (2) | −0.0075 (18) |
C28 | 0.040 (2) | 0.075 (3) | 0.018 (2) | −0.002 (2) | 0.0127 (18) | −0.001 (2) |
C30 | 0.027 (2) | 0.040 (2) | 0.025 (2) | 0.0009 (17) | 0.0116 (17) | 0.0117 (17) |
C31 | 0.028 (2) | 0.044 (3) | 0.0229 (19) | 0.0101 (18) | 0.0154 (16) | 0.0111 (17) |
C32 | 0.028 (2) | 0.023 (2) | 0.027 (2) | 0.0094 (16) | 0.0104 (17) | −0.0009 (16) |
C33 | 0.033 (2) | 0.0173 (19) | 0.0248 (19) | 0.0051 (16) | 0.0089 (17) | −0.0048 (15) |
C34 | 0.041 (2) | 0.0175 (19) | 0.0221 (19) | −0.0022 (17) | 0.0050 (17) | 0.0033 (15) |
C35 | 0.035 (2) | 0.027 (2) | 0.0151 (17) | −0.0016 (17) | −0.0003 (16) | −0.0011 (15) |
C36 | 0.0153 (18) | 0.036 (2) | 0.030 (2) | −0.0010 (16) | 0.0017 (16) | 0.0052 (17) |
C37 | 0.029 (2) | 0.0155 (18) | 0.0209 (18) | −0.0055 (15) | 0.0062 (16) | −0.0012 (14) |
C38 | 0.0187 (18) | 0.0194 (19) | 0.0239 (18) | −0.0036 (14) | 0.0018 (15) | −0.0054 (15) |
Cl1 | 0.0371 (5) | 0.0292 (5) | 0.0210 (4) | −0.0014 (4) | 0.0090 (4) | −0.0033 (4) |
O96 | 0.0341 (17) | 0.080 (3) | 0.053 (2) | −0.0077 (17) | 0.0141 (15) | −0.0404 (19) |
O97 | 0.0434 (19) | 0.046 (2) | 0.060 (2) | 0.0035 (15) | 0.0082 (16) | 0.0241 (16) |
O98 | 0.081 (2) | 0.056 (2) | 0.0203 (15) | −0.0005 (18) | 0.0030 (16) | −0.0032 (14) |
O99 | 0.060 (2) | 0.050 (2) | 0.085 (3) | −0.0138 (17) | 0.043 (2) | −0.0031 (19) |
Cl2 | 0.0406 (6) | 0.0256 (6) | 0.0790 (8) | −0.0072 (5) | 0.0345 (6) | −0.0163 (5) |
O76 | 0.054 (2) | 0.0355 (19) | 0.085 (3) | −0.0025 (15) | 0.0348 (19) | −0.0224 (17) |
O77 | 0.072 (4) | 0.082 (4) | 0.077 (5) | 0.038 (3) | 0.035 (3) | 0.019 (4) |
O78 | 0.049 (3) | 0.052 (3) | 0.040 (3) | −0.008 (2) | 0.023 (2) | 0.002 (2) |
O79 | 0.081 (5) | 0.046 (4) | 0.057 (6) | −0.043 (4) | 0.047 (5) | −0.025 (4) |
O77A | 0.072 (4) | 0.082 (4) | 0.077 (5) | 0.038 (3) | 0.035 (3) | 0.019 (4) |
O78A | 0.049 (3) | 0.052 (3) | 0.040 (3) | −0.008 (2) | 0.023 (2) | 0.002 (2) |
O79A | 0.081 (5) | 0.046 (4) | 0.057 (6) | −0.043 (4) | 0.047 (5) | −0.025 (4) |
O87 | 0.057 (2) | 0.070 (3) | 0.079 (3) | −0.018 (2) | 0.011 (2) | −0.024 (2) |
Cl3 | 0.0230 (11) | 0.0480 (13) | 0.0128 (8) | 0.0034 (9) | 0.0065 (8) | 0.0075 (8) |
O86 | 0.071 (5) | 0.048 (3) | 0.021 (3) | 0.021 (3) | 0.025 (3) | 0.005 (2) |
O88 | 0.044 (3) | 0.055 (3) | 0.038 (3) | 0.015 (2) | 0.017 (2) | 0.008 (2) |
O89 | 0.095 (5) | 0.060 (4) | 0.057 (4) | 0.017 (4) | 0.048 (4) | 0.028 (3) |
Cl3A | 0.047 (3) | 0.029 (2) | 0.023 (2) | 0.000 (2) | 0.008 (2) | 0.0031 (14) |
O86A | 0.044 (7) | 0.058 (7) | 0.037 (6) | 0.005 (5) | 0.007 (5) | 0.001 (5) |
O88A | 0.053 (7) | 0.079 (9) | 0.070 (8) | 0.000 (6) | 0.030 (7) | −0.029 (6) |
O89A | 0.086 (10) | 0.142 (13) | 0.018 (5) | 0.006 (10) | 0.015 (7) | 0.039 (6) |
O52 | 0.066 (2) | 0.0275 (17) | 0.050 (2) | 0.0073 (16) | 0.0249 (18) | 0.0089 (14) |
O53 | 0.053 (2) | 0.0406 (19) | 0.055 (2) | 0.0109 (16) | 0.0022 (17) | −0.0007 (16) |
O54 | 0.0326 (16) | 0.0237 (15) | 0.0336 (16) | 0.0035 (12) | −0.0068 (13) | −0.0040 (12) |
O55 | 0.0247 (14) | 0.0230 (14) | 0.0229 (13) | 0.0022 (11) | 0.0053 (11) | −0.0030 (11) |
Ni1—O3 | 2.041 (2) | C16—H16B | 0.9800 |
Ni1—N1 | 2.104 (3) | C16—H16C | 0.9800 |
Ni1—N3 | 2.115 (3) | C17—H17A | 0.9800 |
Ni1—N2 | 2.138 (3) | C17—H17B | 0.9800 |
Ni1—O2 | 2.156 (2) | C17—H17C | 0.9800 |
Ni1—O1 | 2.176 (2) | C18—H18A | 0.9800 |
Ni1—C7 | 2.505 (3) | C18—H18B | 0.9800 |
Ni2—O6 | 2.072 (3) | C18—H18C | 0.9800 |
Ni2—O5 | 2.085 (2) | C20—C21 | 1.490 (6) |
Ni2—N5 | 2.102 (3) | C20—H20A | 0.9900 |
Ni2—N4 | 2.131 (3) | C20—H20B | 0.9900 |
Ni2—N6 | 2.142 (3) | C21—H21A | 0.9900 |
Ni2—O4 | 2.284 (2) | C21—H21B | 0.9900 |
Ni2—C8 | 2.517 (3) | C22—C23 | 1.497 (5) |
Ni3—O8 | 2.036 (2) | C22—H22A | 0.9900 |
Ni3—O9 | 2.059 (2) | C22—H22B | 0.9900 |
Ni3—N7 | 2.107 (3) | C23—H23A | 0.9900 |
Ni3—N8 | 2.111 (3) | C23—H23B | 0.9900 |
Ni3—N9 | 2.127 (3) | C24—H24A | 0.9800 |
O1—C7 | 1.275 (4) | C24—H24B | 0.9800 |
O2—C7 | 1.261 (4) | C24—H24C | 0.9800 |
O3—H3V | 0.915 (19) | C25—H25A | 0.9800 |
O3—H3W | 0.93 (4) | C25—H25B | 0.9800 |
O4—C8 | 1.267 (4) | C25—H25C | 0.9800 |
O5—C8 | 1.259 (4) | C26—H26A | 0.9800 |
O6—H6V | 0.930 (19) | C26—H26B | 0.9800 |
O6—H6W | 0.91 (2) | C26—H26C | 0.9800 |
O7—C9 | 1.273 (4) | C27—H27A | 0.9800 |
O8—C9 | 1.254 (4) | C27—H27B | 0.9800 |
O9—H9V | 0.908 (19) | C27—H27C | 0.9800 |
O9—H9W | 0.913 (19) | C28—H28A | 0.9800 |
N1—C14 | 1.475 (4) | C28—H28B | 0.9800 |
N1—C10 | 1.484 (4) | C28—H28C | 0.9800 |
N1—C15 | 1.485 (4) | C30—C31 | 1.499 (5) |
N2—C12 | 1.477 (4) | C30—H30A | 0.9900 |
N2—C16 | 1.479 (4) | C30—H30B | 0.9900 |
N2—C11 | 1.493 (4) | C31—H31A | 0.9900 |
N3—C17 | 1.483 (4) | C31—H31B | 0.9900 |
N3—C13 | 1.486 (4) | C32—C33 | 1.508 (5) |
N3—C18 | 1.486 (4) | C32—H32A | 0.9900 |
N4—C20 | 1.459 (5) | C32—H32B | 0.9900 |
N4—C25 | 1.471 (5) | C33—H33A | 0.9900 |
N4—C24 | 1.487 (5) | C33—H33B | 0.9900 |
N5—C22 | 1.477 (4) | C34—H34A | 0.9800 |
N5—C26 | 1.479 (5) | C34—H34B | 0.9800 |
N5—C21 | 1.496 (5) | C34—H34C | 0.9800 |
N6—C27 | 1.474 (5) | C35—H35A | 0.9800 |
N6—C28 | 1.488 (5) | C35—H35B | 0.9800 |
N6—C23 | 1.488 (4) | C35—H35C | 0.9800 |
N7—C35 | 1.470 (4) | C36—H36A | 0.9800 |
N7—C34 | 1.481 (4) | C36—H36B | 0.9800 |
N7—C30 | 1.487 (5) | C36—H36C | 0.9800 |
N8—C36 | 1.471 (4) | C37—H37A | 0.9800 |
N8—C32 | 1.480 (5) | C37—H37B | 0.9800 |
N8—C31 | 1.491 (4) | C37—H37C | 0.9800 |
N9—C38 | 1.481 (4) | C38—H38A | 0.9800 |
N9—C37 | 1.485 (4) | C38—H38B | 0.9800 |
N9—C33 | 1.487 (4) | C38—H38C | 0.9800 |
C1—C2 | 1.391 (4) | Cl1—O99 | 1.408 (3) |
C1—C6 | 1.392 (4) | Cl1—O96 | 1.426 (3) |
C1—C7 | 1.494 (4) | Cl1—O98 | 1.429 (3) |
C2—C3 | 1.398 (5) | Cl1—O97 | 1.444 (3) |
C2—H2 | 0.9500 | Cl2—O77 | 1.338 (6) |
C3—C4 | 1.395 (4) | Cl2—O78A | 1.353 (8) |
C3—C8 | 1.503 (4) | Cl2—O76 | 1.398 (3) |
C4—C5 | 1.390 (4) | Cl2—O79A | 1.416 (12) |
C4—H4 | 0.9500 | Cl2—O79 | 1.440 (7) |
C5—C6 | 1.395 (4) | Cl2—O78 | 1.544 (5) |
C5—C9 | 1.497 (4) | Cl2—O77A | 1.573 (10) |
C6—H6 | 0.9500 | O87—Cl3 | 1.433 (4) |
C10—C11 | 1.518 (5) | O87—Cl3A | 1.515 (6) |
C10—H10A | 0.9900 | Cl3—O89 | 1.401 (6) |
C10—H10B | 0.9900 | Cl3—O88 | 1.411 (5) |
C11—H11A | 0.9900 | Cl3—O86 | 1.425 (5) |
C11—H11B | 0.9900 | Cl3A—O89A | 1.348 (12) |
C12—C13 | 1.517 (5) | Cl3A—O86A | 1.414 (12) |
C12—H12A | 0.9900 | Cl3A—O88A | 1.435 (13) |
C12—H12B | 0.9900 | O51—H51W | 0.94 (2) |
C13—H13A | 0.9900 | O51—H51V | 0.94 (2) |
C13—H13B | 0.9900 | O52—H52V | 0.95 (2) |
C14—H14A | 0.9800 | O52—H52W | 0.95 (2) |
C14—H14B | 0.9800 | O53—H53V | 1.00 (2) |
C14—H14C | 0.9800 | O53—H53W | 0.99 (2) |
C15—H15A | 0.9800 | O54—H54V | 0.933 (19) |
C15—H15B | 0.9800 | O54—H54W | 0.92 (2) |
C15—H15C | 0.9800 | O55—H55V | 0.914 (19) |
C16—H16A | 0.9800 | O55—H55W | 0.909 (19) |
O3—Ni1—N1 | 94.38 (10) | N1—C14—H14B | 109.5 |
O3—Ni1—N3 | 92.53 (10) | H14A—C14—H14B | 109.5 |
N1—Ni1—N3 | 107.73 (11) | N1—C14—H14C | 109.5 |
O3—Ni1—N2 | 176.07 (10) | H14A—C14—H14C | 109.5 |
N1—Ni1—N2 | 85.52 (11) | H14B—C14—H14C | 109.5 |
N3—Ni1—N2 | 83.77 (10) | N1—C15—H15A | 109.5 |
O3—Ni1—O2 | 91.26 (9) | N1—C15—H15B | 109.5 |
N1—Ni1—O2 | 91.48 (10) | H15A—C15—H15B | 109.5 |
N3—Ni1—O2 | 160.05 (9) | N1—C15—H15C | 109.5 |
N2—Ni1—O2 | 92.66 (9) | H15A—C15—H15C | 109.5 |
O3—Ni1—O1 | 85.40 (9) | H15B—C15—H15C | 109.5 |
N1—Ni1—O1 | 152.20 (10) | N2—C16—H16A | 109.5 |
N3—Ni1—O1 | 100.04 (9) | N2—C16—H16B | 109.5 |
N2—Ni1—O1 | 96.52 (9) | H16A—C16—H16B | 109.5 |
O2—Ni1—O1 | 60.76 (8) | N2—C16—H16C | 109.5 |
O3—Ni1—C7 | 89.48 (10) | H16A—C16—H16C | 109.5 |
N1—Ni1—C7 | 121.70 (11) | H16B—C16—H16C | 109.5 |
N3—Ni1—C7 | 130.21 (10) | N3—C17—H17A | 109.5 |
N2—Ni1—C7 | 93.91 (10) | N3—C17—H17B | 109.5 |
O2—Ni1—C7 | 30.23 (9) | H17A—C17—H17B | 109.5 |
O1—Ni1—C7 | 30.59 (9) | N3—C17—H17C | 109.5 |
O6—Ni2—O5 | 87.62 (10) | H17A—C17—H17C | 109.5 |
O6—Ni2—N5 | 174.88 (11) | H17B—C17—H17C | 109.5 |
O5—Ni2—N5 | 97.32 (10) | N3—C18—H18A | 109.5 |
O6—Ni2—N4 | 96.70 (12) | N3—C18—H18B | 109.5 |
O5—Ni2—N4 | 90.69 (10) | H18A—C18—H18B | 109.5 |
N5—Ni2—N4 | 84.62 (12) | N3—C18—H18C | 109.5 |
O6—Ni2—N6 | 91.28 (11) | H18A—C18—H18C | 109.5 |
O5—Ni2—N6 | 160.36 (10) | H18B—C18—H18C | 109.5 |
N5—Ni2—N6 | 83.61 (11) | N4—C20—C21 | 111.3 (3) |
N4—Ni2—N6 | 108.90 (11) | N4—C20—H20A | 109.4 |
O6—Ni2—O4 | 87.62 (10) | C21—C20—H20A | 109.4 |
O5—Ni2—O4 | 60.02 (8) | N4—C20—H20B | 109.4 |
N5—Ni2—O4 | 93.68 (10) | C21—C20—H20B | 109.4 |
N4—Ni2—O4 | 150.28 (10) | H20A—C20—H20B | 108.0 |
N6—Ni2—O4 | 100.35 (10) | C20—C21—N5 | 109.3 (3) |
O6—Ni2—C8 | 86.66 (11) | C20—C21—H21A | 109.8 |
O5—Ni2—C8 | 29.91 (10) | N5—C21—H21A | 109.8 |
N5—Ni2—C8 | 96.95 (11) | C20—C21—H21B | 109.8 |
N4—Ni2—C8 | 120.52 (11) | N5—C21—H21B | 109.8 |
N6—Ni2—C8 | 130.45 (11) | H21A—C21—H21B | 108.3 |
O4—Ni2—C8 | 30.12 (9) | N5—C22—C23 | 111.3 (3) |
O8—Ni3—O9 | 91.85 (10) | N5—C22—H22A | 109.4 |
O8—Ni3—N7 | 91.07 (10) | C23—C22—H22A | 109.4 |
O9—Ni3—N7 | 95.81 (10) | N5—C22—H22B | 109.4 |
O8—Ni3—N8 | 95.56 (10) | C23—C22—H22B | 109.4 |
O9—Ni3—N8 | 172.46 (10) | H22A—C22—H22B | 108.0 |
N7—Ni3—N8 | 85.43 (11) | N6—C23—C22 | 110.6 (3) |
O8—Ni3—N9 | 156.85 (10) | N6—C23—H23A | 109.5 |
O9—Ni3—N9 | 89.35 (10) | C22—C23—H23A | 109.5 |
N7—Ni3—N9 | 111.81 (11) | N6—C23—H23B | 109.5 |
N8—Ni3—N9 | 83.30 (11) | C22—C23—H23B | 109.5 |
C7—O1—Ni1 | 89.13 (18) | H23A—C23—H23B | 108.1 |
C7—O2—Ni1 | 90.36 (18) | N4—C24—H24A | 109.5 |
Ni1—O3—H3V | 128 (2) | N4—C24—H24B | 109.5 |
Ni1—O3—H3W | 122 (2) | H24A—C24—H24B | 109.5 |
H3V—O3—H3W | 105 (3) | N4—C24—H24C | 109.5 |
C8—O4—Ni2 | 85.16 (19) | H24A—C24—H24C | 109.5 |
C8—O5—Ni2 | 94.38 (19) | H24B—C24—H24C | 109.5 |
Ni2—O6—H6V | 118 (3) | N4—C25—H25A | 109.5 |
Ni2—O6—H6W | 132 (3) | N4—C25—H25B | 109.5 |
H6V—O6—H6W | 103 (4) | H25A—C25—H25B | 109.5 |
C9—O8—Ni3 | 101.9 (2) | N4—C25—H25C | 109.5 |
Ni3—O9—H9V | 119 (2) | H25A—C25—H25C | 109.5 |
Ni3—O9—H9W | 126 (2) | H25B—C25—H25C | 109.5 |
H9V—O9—H9W | 106 (3) | N5—C26—H26A | 109.5 |
C14—N1—C10 | 110.3 (3) | N5—C26—H26B | 109.5 |
C14—N1—C15 | 106.2 (3) | H26A—C26—H26B | 109.5 |
C10—N1—C15 | 108.8 (3) | N5—C26—H26C | 109.5 |
C14—N1—Ni1 | 119.9 (2) | H26A—C26—H26C | 109.5 |
C10—N1—Ni1 | 101.01 (19) | H26B—C26—H26C | 109.5 |
C15—N1—Ni1 | 110.2 (2) | N6—C27—H27A | 109.5 |
C12—N2—C16 | 109.1 (3) | N6—C27—H27B | 109.5 |
C12—N2—C11 | 110.3 (3) | H27A—C27—H27B | 109.5 |
C16—N2—C11 | 109.1 (3) | N6—C27—H27C | 109.5 |
C12—N2—Ni1 | 107.3 (2) | H27A—C27—H27C | 109.5 |
C16—N2—Ni1 | 115.7 (2) | H27B—C27—H27C | 109.5 |
C11—N2—Ni1 | 105.3 (2) | N6—C28—H28A | 109.5 |
C17—N3—C13 | 108.8 (3) | N6—C28—H28B | 109.5 |
C17—N3—C18 | 107.4 (3) | H28A—C28—H28B | 109.5 |
C13—N3—C18 | 109.8 (3) | N6—C28—H28C | 109.5 |
C17—N3—Ni1 | 116.9 (2) | H28A—C28—H28C | 109.5 |
C13—N3—Ni1 | 105.96 (19) | H28B—C28—H28C | 109.5 |
C18—N3—Ni1 | 107.90 (19) | N7—C30—C31 | 110.3 (3) |
C20—N4—C25 | 110.6 (3) | N7—C30—H30A | 109.6 |
C20—N4—C24 | 109.3 (3) | C31—C30—H30A | 109.6 |
C25—N4—C24 | 106.0 (3) | N7—C30—H30B | 109.6 |
C20—N4—Ni2 | 102.2 (2) | C31—C30—H30B | 109.6 |
C25—N4—Ni2 | 118.4 (3) | H30A—C30—H30B | 108.1 |
C24—N4—Ni2 | 110.1 (2) | N8—C31—C30 | 109.6 (3) |
C22—N5—C26 | 109.6 (3) | N8—C31—H31A | 109.7 |
C22—N5—C21 | 110.4 (3) | C30—C31—H31A | 109.7 |
C26—N5—C21 | 108.5 (3) | N8—C31—H31B | 109.7 |
C22—N5—Ni2 | 107.5 (2) | C30—C31—H31B | 109.7 |
C26—N5—Ni2 | 114.2 (2) | H31A—C31—H31B | 108.2 |
C21—N5—Ni2 | 106.6 (2) | N8—C32—C33 | 110.6 (3) |
C27—N6—C28 | 107.8 (3) | N8—C32—H32A | 109.5 |
C27—N6—C23 | 109.7 (3) | C33—C32—H32A | 109.5 |
C28—N6—C23 | 107.9 (3) | N8—C32—H32B | 109.5 |
C27—N6—Ni2 | 107.6 (2) | C33—C32—H32B | 109.5 |
C28—N6—Ni2 | 116.9 (2) | H32A—C32—H32B | 108.1 |
C23—N6—Ni2 | 106.7 (2) | N9—C33—C32 | 110.2 (3) |
C35—N7—C34 | 107.6 (3) | N9—C33—H33A | 109.6 |
C35—N7—C30 | 111.1 (3) | C32—C33—H33A | 109.6 |
C34—N7—C30 | 107.0 (3) | N9—C33—H33B | 109.6 |
C35—N7—Ni3 | 115.7 (2) | C32—C33—H33B | 109.6 |
C34—N7—Ni3 | 111.6 (2) | H33A—C33—H33B | 108.1 |
C30—N7—Ni3 | 103.6 (2) | N7—C34—H34A | 109.5 |
C36—N8—C32 | 109.5 (3) | N7—C34—H34B | 109.5 |
C36—N8—C31 | 109.2 (3) | H34A—C34—H34B | 109.5 |
C32—N8—C31 | 110.4 (3) | N7—C34—H34C | 109.5 |
C36—N8—Ni3 | 114.8 (2) | H34A—C34—H34C | 109.5 |
C32—N8—Ni3 | 107.4 (2) | H34B—C34—H34C | 109.5 |
C31—N8—Ni3 | 105.4 (2) | N7—C35—H35A | 109.5 |
C38—N9—C37 | 107.5 (3) | N7—C35—H35B | 109.5 |
C38—N9—C33 | 109.5 (3) | H35A—C35—H35B | 109.5 |
C37—N9—C33 | 108.4 (3) | N7—C35—H35C | 109.5 |
C38—N9—Ni3 | 117.5 (2) | H35A—C35—H35C | 109.5 |
C37—N9—Ni3 | 105.77 (19) | H35B—C35—H35C | 109.5 |
C33—N9—Ni3 | 107.9 (2) | N8—C36—H36A | 109.5 |
C2—C1—C6 | 119.6 (3) | N8—C36—H36B | 109.5 |
C2—C1—C7 | 120.9 (3) | H36A—C36—H36B | 109.5 |
C6—C1—C7 | 119.4 (3) | N8—C36—H36C | 109.5 |
C1—C2—C3 | 120.4 (3) | H36A—C36—H36C | 109.5 |
C1—C2—H2 | 119.8 | H36B—C36—H36C | 109.5 |
C3—C2—H2 | 119.8 | N9—C37—H37A | 109.5 |
C4—C3—C2 | 119.4 (3) | N9—C37—H37B | 109.5 |
C4—C3—C8 | 119.9 (3) | H37A—C37—H37B | 109.5 |
C2—C3—C8 | 120.6 (3) | N9—C37—H37C | 109.5 |
C5—C4—C3 | 120.6 (3) | H37A—C37—H37C | 109.5 |
C5—C4—H4 | 119.7 | H37B—C37—H37C | 109.5 |
C3—C4—H4 | 119.7 | N9—C38—H38A | 109.5 |
C4—C5—C6 | 119.5 (3) | N9—C38—H38B | 109.5 |
C4—C5—C9 | 122.7 (3) | H38A—C38—H38B | 109.5 |
C6—C5—C9 | 117.8 (3) | N9—C38—H38C | 109.5 |
C1—C6—C5 | 120.5 (3) | H38A—C38—H38C | 109.5 |
C1—C6—H6 | 119.7 | H38B—C38—H38C | 109.5 |
C5—C6—H6 | 119.7 | O99—Cl1—O96 | 110.4 (2) |
O2—C7—O1 | 119.5 (3) | O99—Cl1—O98 | 112.1 (2) |
O2—C7—C1 | 120.6 (3) | O96—Cl1—O98 | 108.7 (2) |
O1—C7—C1 | 119.9 (3) | O99—Cl1—O97 | 110.6 (2) |
O2—C7—Ni1 | 59.41 (16) | O96—Cl1—O97 | 107.9 (2) |
O1—C7—Ni1 | 60.28 (16) | O98—Cl1—O97 | 107.1 (2) |
C1—C7—Ni1 | 174.1 (2) | O77—Cl2—O78A | 69.5 (5) |
O5—C8—O4 | 120.4 (3) | O77—Cl2—O76 | 121.8 (4) |
O5—C8—C3 | 118.4 (3) | O78A—Cl2—O76 | 121.1 (4) |
O4—C8—C3 | 121.2 (3) | O77—Cl2—O79A | 95.8 (10) |
O5—C8—Ni2 | 55.70 (16) | O78A—Cl2—O79A | 124.0 (10) |
O4—C8—Ni2 | 64.72 (17) | O76—Cl2—O79A | 112.6 (11) |
C3—C8—Ni2 | 173.7 (2) | O77—Cl2—O79 | 115.7 (6) |
O8—C9—O7 | 120.8 (3) | O78A—Cl2—O79 | 117.4 (6) |
O8—C9—C5 | 118.4 (3) | O76—Cl2—O79 | 107.7 (6) |
O7—C9—C5 | 120.8 (3) | O77—Cl2—O78 | 106.0 (4) |
N1—C10—C11 | 109.9 (3) | O76—Cl2—O78 | 102.7 (3) |
N1—C10—H10A | 109.7 | O79A—Cl2—O78 | 119.0 (7) |
C11—C10—H10A | 109.7 | O79—Cl2—O78 | 99.9 (4) |
N1—C10—H10B | 109.7 | O78A—Cl2—O77A | 98.4 (6) |
C11—C10—H10B | 109.7 | O76—Cl2—O77A | 90.8 (5) |
H10A—C10—H10B | 108.2 | O79A—Cl2—O77A | 95.5 (8) |
N2—C11—C10 | 110.3 (3) | O79—Cl2—O77A | 118.7 (6) |
N2—C11—H11A | 109.6 | O78—Cl2—O77A | 132.9 (5) |
C10—C11—H11A | 109.6 | O89—Cl3—O88 | 112.8 (4) |
N2—C11—H11B | 109.6 | O89—Cl3—O86 | 113.2 (4) |
C10—C11—H11B | 109.6 | O88—Cl3—O86 | 111.0 (3) |
H11A—C11—H11B | 108.1 | O89—Cl3—O87 | 112.7 (4) |
N2—C12—C13 | 110.4 (3) | O88—Cl3—O87 | 102.9 (3) |
N2—C12—H12A | 109.6 | O86—Cl3—O87 | 103.4 (3) |
C13—C12—H12A | 109.6 | O89A—Cl3A—O86A | 111.0 (9) |
N2—C12—H12B | 109.6 | O89A—Cl3A—O88A | 115.6 (9) |
C13—C12—H12B | 109.6 | O86A—Cl3A—O88A | 107.7 (7) |
H12A—C12—H12B | 108.1 | O89A—Cl3A—O87 | 97.5 (8) |
N3—C13—C12 | 110.2 (3) | O86A—Cl3A—O87 | 110.8 (6) |
N3—C13—H13A | 109.6 | O88A—Cl3A—O87 | 114.0 (6) |
C12—C13—H13A | 109.6 | H51W—O51—H51V | 116 (10) |
N3—C13—H13B | 109.6 | H52V—O52—H52W | 113 (5) |
C12—C13—H13B | 109.6 | H53V—O53—H53W | 100 (4) |
H13A—C13—H13B | 108.1 | H54V—O54—H54W | 111 (4) |
N1—C14—H14A | 109.5 | H55V—O55—H55W | 103 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3V···O52 | 0.92 (2) | 1.77 (2) | 2.677 (4) | 173 (4) |
O3—H3W···O7i | 0.93 (4) | 1.83 (2) | 2.742 (3) | 167 (4) |
O6—H6W···O51 | 0.91 (2) | 1.99 (4) | 2.607 (9) | 124 (4) |
O6—H6V···O54i | 0.93 (2) | 1.83 (2) | 2.745 (4) | 166 (4) |
O9—H9V···O1i | 0.91 (2) | 1.85 (2) | 2.743 (3) | 166 (3) |
O9—H9W···O55i | 0.91 (2) | 1.82 (2) | 2.727 (3) | 171 (4) |
O52—H52V···O53i | 0.95 (2) | 2.13 (5) | 2.789 (5) | 125 (4) |
O53—H53W···O7 | 0.99 (2) | 1.97 (3) | 2.877 (4) | 151 (5) |
O53—H53V···O97 | 1.00 (2) | 1.96 (3) | 2.869 (5) | 151 (5) |
O54—H54V···O2 | 0.93 (2) | 1.98 (2) | 2.902 (3) | 167 (4) |
O55—H55V···O4 | 0.91 (2) | 1.95 (2) | 2.843 (3) | 166 (4) |
O55—H55W···O76ii | 0.91 (2) | 2.04 (2) | 2.934 (4) | 168 (4) |
C2—H2···O55 | 0.95 | 2.69 | 3.607 (4) | 162 |
C6—H6···O54 | 0.95 | 2.67 | 3.601 (4) | 166 |
C10—H10A···O54 | 0.99 | 2.81 | 3.697 (5) | 149 |
C11—H11B···O79 | 0.99 | 2.67 | 3.477 (11) | 139 |
C11—H11B···O79A | 0.99 | 2.78 | 3.56 (2) | 136 |
C15—H15A···O54 | 0.98 | 2.61 | 3.392 (5) | 137 |
C15—H15B···O52 | 0.98 | 2.66 | 3.585 (5) | 159 |
C16—H16B···O78 | 0.98 | 2.64 | 3.526 (6) | 150 |
C16—H16B···O79 | 0.98 | 2.84 | 3.396 (9) | 117 |
C17—H17A···O86A | 0.98 | 2.94 | 3.327 (12) | 105 |
C20—H20B···O98 | 0.99 | 2.92 | 3.310 (6) | 105 |
C21—H21B···O98 | 0.99 | 2.77 | 3.476 (5) | 128 |
C27—H27A···O55 | 0.98 | 2.80 | 3.605 (5) | 140 |
C28—H28A···O51 | 0.98 | 2.98 | 3.941 (10) | 169 |
C30—H30B···O77 | 0.99 | 2.76 | 3.603 (9) | 143 |
C30—H30B···O77A | 0.99 | 2.82 | 3.513 (15) | 128 |
C30—H30B···O78A | 0.99 | 2.69 | 3.677 (11) | 175 |
C34—H34B···O54 | 0.98 | 2.52 | 3.293 (5) | 136 |
C36—H36B···O78 | 0.98 | 2.66 | 3.579 (6) | 157 |
C36—H36B···O78A | 0.98 | 2.81 | 3.783 (11) | 171 |
C37—H37A···O53 | 0.98 | 2.85 | 3.803 (5) | 164 |
C34—H34A···O55i | 0.98 | 2.53 | 3.487 (5) | 165 |
C37—H37C···O89i | 0.98 | 2.57 | 3.337 (7) | 136 |
C37—H37C···O89Ai | 0.98 | 2.57 | 3.417 (16) | 145 |
C25—H25B···O88iii | 0.98 | 2.57 | 3.518 (7) | 162 |
C25—H25B···O88Aiii | 0.98 | 2.78 | 3.704 (12) | 157 |
C24—H24B···O88iii | 0.98 | 2.93 | 3.797 (7) | 148 |
C24—H24B···O89iii | 0.98 | 2.58 | 3.439 (9) | 146 |
C15—H15C···O89Aiv | 0.98 | 2.93 | 3.762 (15) | 143 |
C14—H14A···O89Aiv | 0.98 | 2.55 | 3.498 (12) | 162 |
C15—H15C···O89iv | 0.98 | 2.60 | 3.508 (7) | 154 |
C14—H14A···O89iv | 0.98 | 2.87 | 3.739 (8) | 149 |
C10—H10B···O87iv | 0.99 | 2.68 | 3.564 (5) | 148 |
C11—H11A···O97ii | 0.99 | 2.63 | 3.612 (5) | 172 |
C12—H12A···O78ii | 0.99 | 2.79 | 3.646 (7) | 145 |
C16—H16A···O78ii | 0.98 | 2.83 | 3.462 (7) | 123 |
C26—H26C···O79ii | 0.98 | 2.72 | 3.580 (8) | 146 |
C26—H26C···O79Aii | 0.98 | 2.45 | 3.276 (14) | 142 |
C14—H14C···O96ii | 0.98 | 2.74 | 3.423 (5) | 127 |
C14—H14C···O97ii | 0.98 | 2.86 | 3.754 (5) | 153 |
C18—H18C···O76ii | 0.98 | 2.95 | 3.809 (5) | 147 |
C13—H13A···O97ii | 0.99 | 2.70 | 3.562 (5) | 146 |
C17—H17C···O98v | 0.98 | 2.57 | 3.411 (5) | 143 |
C18—H18A···O98v | 0.98 | 2.88 | 3.634 (5) | 134 |
C21—H21A···O96vi | 0.99 | 2.87 | 3.836 (5) | 165 |
C23—H23B···O96vi | 0.99 | 2.84 | 3.832 (5) | 177 |
C25—H25C···O53vi | 0.98 | 2.61 | 3.452 (5) | 145 |
C25—H25A···O96vi | 0.98 | 2.44 | 3.314 (5) | 148 |
C25—H25A···O99vi | 0.98 | 2.94 | 3.464 (6) | 115 |
C22—H22A···O86Avii | 0.99 | 2.55 | 3.488 (12) | 158 |
C21—H21B···O86Avii | 0.99 | 2.86 | 3.395 (13) | 115 |
C26—H26A···O87vii | 0.98 | 2.49 | 3.405 (6) | 154 |
C22—H22A···O87vii | 0.99 | 2.80 | 3.512 (5) | 130 |
C28—H28C···O76viii | 0.98 | 2.65 | 3.614 (5) | 169 |
C35—H35C···O51ix | 0.98 | 2.63 | 3.390 (9) | 134 |
C30—H30A···O51ix | 0.99 | 2.67 | 3.565 (9) | 151 |
C33—H33B···O52x | 0.99 | 2.96 | 3.397 (5) | 108 |
C33—H33B···O86x | 0.99 | 2.37 | 3.333 (6) | 164 |
C35—H35A···O86x | 0.98 | 2.56 | 3.510 (6) | 163 |
C35—H35A···O86Ax | 0.98 | 2.88 | 3.756 (12) | 149 |
C33—H33B···O86Ax | 0.99 | 2.82 | 3.689 (11) | 147 |
C33—H33B···O88Ax | 0.99 | 2.76 | 3.715 (12) | 162 |
C33—H33B···O52x | 0.99 | 2.96 | 3.397 (5) | 108 |
C38—H38B···O86x | 0.98 | 2.81 | 3.614 (6) | 140 |
C38—H38B···O86Ax | 0.98 | 2.57 | 3.395 (10) | 141 |
C31—H31B···O86x | 0.99 | 2.98 | 3.960 (7) | 170 |
C31—H31B···O88x | 0.99 | 2.64 | 3.427 (6) | 136 |
C31—H31B···O88Ax | 0.99 | 2.60 | 3.548 (14) | 161 |
C32—H32A···O99xi | 0.99 | 2.77 | 3.731 (5) | 165 |
C38—H38C···O96xii | 0.98 | 2.75 | 3.371 (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, y−1/2, −z+1/2; (vi) x, −y+3/2, z−1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (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 |
Mr | 1332.12 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 100 |
a, b, c (Å) | 11.7409 (2), 30.6727 (5), 16.9590 (4) |
β (°) | 107.633 (2) |
V (Å3) | 5820.41 (19) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.18 |
Crystal size (mm) | 0.30 × 0.30 × 0.25 |
Data collection | |
Diffractometer | Oxford Diffraction Xcalibur2 + CCD |
Absorption correction | Multi-scan (CrysAlis RED; Oxford Diffraction, 2006) |
Tmin, Tmax | 0.655, 0.740 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 27090, 10209, 8075 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.597 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.096, 1.01 |
No. of reflections | 10209 |
No. of parameters | 799 |
No. of restraints | 26 |
H-atom treatment | H 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 Å−3) | 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).
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3V···O52 | 0.915 (19) | 1.77 (2) | 2.677 (4) | 173 (4) |
O3—H3W···O7i | 0.93 (4) | 1.83 (2) | 2.742 (3) | 167 (4) |
O6—H6W···O51 | 0.91 (2) | 1.99 (4) | 2.607 (9) | 124 (4) |
O6—H6V···O54i | 0.930 (19) | 1.83 (2) | 2.745 (4) | 166 (4) |
O9—H9V···O1i | 0.908 (19) | 1.85 (2) | 2.743 (3) | 166 (3) |
O9—H9W···O55i | 0.913 (19) | 1.82 (2) | 2.727 (3) | 171 (4) |
O52—H52V···O53i | 0.95 (2) | 2.13 (5) | 2.789 (5) | 125 (4) |
O53—H53W···O7 | 0.99 (2) | 1.97 (3) | 2.877 (4) | 151 (5) |
O53—H53V···O97 | 1.00 (2) | 1.96 (3) | 2.869 (5) | 151 (5) |
O54—H54V···O2 | 0.933 (19) | 1.98 (2) | 2.902 (3) | 167 (4) |
O55—H55V···O4 | 0.914 (19) | 1.95 (2) | 2.843 (3) | 166 (4) |
O55—H55W···O76ii | 0.909 (19) | 2.04 (2) | 2.934 (4) | 168 (4) |
C2—H2···O55 | 0.95 | 2.69 | 3.607 (4) | 162.4 |
C6—H6···O54 | 0.95 | 2.67 | 3.601 (4) | 166.4 |
C10—H10A···O54 | 0.99 | 2.81 | 3.697 (5) | 149.0 |
C11—H11B···O79 | 0.99 | 2.67 | 3.477 (11) | 139.1 |
C11—H11B···O79A | 0.99 | 2.78 | 3.56 (2) | 135.9 |
C15—H15A···O54 | 0.98 | 2.61 | 3.392 (5) | 137.0 |
C15—H15B···O52 | 0.98 | 2.66 | 3.585 (5) | 158.6 |
C16—H16B···O78 | 0.98 | 2.64 | 3.526 (6) | 149.9 |
C16—H16B···O79 | 0.98 | 2.84 | 3.396 (9) | 116.7 |
C17—H17A···O86A | 0.98 | 2.94 | 3.327 (12) | 104.7 |
C20—H20B···O98 | 0.99 | 2.92 | 3.310 (6) | 104.5 |
C21—H21B···O98 | 0.99 | 2.77 | 3.476 (5) | 128.3 |
C27—H27A···O55 | 0.98 | 2.80 | 3.605 (5) | 140.0 |
C28—H28A···O51 | 0.98 | 2.98 | 3.941 (10) | 168.8 |
C30—H30B···O77 | 0.99 | 2.76 | 3.603 (9) | 143.4 |
C30—H30B···O77A | 0.99 | 2.82 | 3.513 (15) | 127.9 |
C30—H30B···O78A | 0.99 | 2.69 | 3.677 (11) | 175.1 |
C34—H34B···O54 | 0.98 | 2.52 | 3.293 (5) | 135.9 |
C36—H36B···O78 | 0.98 | 2.66 | 3.579 (6) | 157.3 |
C36—H36B···O78A | 0.98 | 2.81 | 3.783 (11) | 170.8 |
C37—H37A···O53 | 0.98 | 2.85 | 3.803 (5) | 164.4 |
C34—H34A···O55i | 0.98 | 2.53 | 3.487 (5) | 165.3 |
C37—H37C···O89i | 0.98 | 2.57 | 3.337 (7) | 135.6 |
C37—H37C···O89Ai | 0.98 | 2.57 | 3.417 (16) | 144.9 |
C25—H25B···O88iii | 0.98 | 2.57 | 3.518 (7) | 162.0 |
C25—H25B···O88Aiii | 0.98 | 2.78 | 3.704 (12) | 157.1 |
C24—H24B···O88iii | 0.98 | 2.93 | 3.797 (7) | 147.6 |
C24—H24B···O89iii | 0.98 | 2.58 | 3.439 (9) | 146.3 |
C15—H15C···O89Aiv | 0.98 | 2.93 | 3.762 (15) | 143.1 |
C14—H14A···O89Aiv | 0.98 | 2.55 | 3.498 (12) | 162.0 |
C15—H15C···O89iv | 0.98 | 2.60 | 3.508 (7) | 154.2 |
C14—H14A···O89iv | 0.98 | 2.87 | 3.739 (8) | 148.9 |
C10—H10B···O87iv | 0.99 | 2.68 | 3.564 (5) | 148.3 |
C11—H11A···O97ii | 0.99 | 2.63 | 3.612 (5) | 171.9 |
C12—H12A···O78ii | 0.99 | 2.79 | 3.646 (7) | 145.0 |
C16—H16A···O78ii | 0.98 | 2.83 | 3.462 (7) | 122.9 |
C26—H26C···O79ii | 0.98 | 2.72 | 3.580 (8) | 146.1 |
C26—H26C···O79Aii | 0.98 | 2.45 | 3.276 (14) | 142.0 |
C14—H14C···O96ii | 0.98 | 2.74 | 3.423 (5) | 127.4 |
C14—H14C···O97ii | 0.98 | 2.86 | 3.754 (5) | 152.7 |
C18—H18C···O76ii | 0.98 | 2.95 | 3.809 (5) | 146.7 |
C13—H13A···O97ii | 0.99 | 2.70 | 3.562 (5) | 146.1 |
C17—H17C···O98v | 0.98 | 2.57 | 3.411 (5) | 143.4 |
C18—H18A···O98v | 0.98 | 2.88 | 3.634 (5) | 134.1 |
C21—H21A···O96vi | 0.99 | 2.87 | 3.836 (5) | 164.5 |
C23—H23B···O96vi | 0.99 | 2.84 | 3.832 (5) | 176.6 |
C25—H25C···O53vi | 0.98 | 2.61 | 3.452 (5) | 144.5 |
C25—H25A···O96vi | 0.98 | 2.44 | 3.314 (5) | 148.1 |
C25—H25A···O99vi | 0.98 | 2.94 | 3.464 (6) | 114.5 |
C22—H22A···O86Avii | 0.99 | 2.55 | 3.488 (12) | 157.9 |
C21—H21B···O86Avii | 0.99 | 2.86 | 3.395 (13) | 114.7 |
C26—H26A···O87vii | 0.98 | 2.49 | 3.405 (6) | 154.4 |
C22—H22A···O87vii | 0.99 | 2.80 | 3.512 (5) | 129.6 |
C28—H28C···O76viii | 0.98 | 2.65 | 3.614 (5) | 168.6 |
C35—H35C···O51ix | 0.98 | 2.63 | 3.390 (9) | 134.3 |
C30—H30A···O51ix | 0.99 | 2.67 | 3.565 (9) | 151.3 |
C33—H33B···O52x | 0.99 | 2.96 | 3.397 (5) | 107.8 |
C33—H33B···O86x | 0.99 | 2.37 | 3.333 (6) | 164.4 |
C35—H35A···O86x | 0.98 | 2.56 | 3.510 (6) | 162.7 |
C35—H35A···O86Ax | 0.98 | 2.88 | 3.756 (12) | 149.1 |
C33—H33B···O86Ax | 0.99 | 2.82 | 3.689 (11) | 146.5 |
C33—H33B···O88Ax | 0.99 | 2.76 | 3.715 (12) | 161.5 |
C33—H33B···O52x | 0.99 | 2.96 | 3.397 (5) | 107.8 |
C38—H38B···O86x | 0.98 | 2.81 | 3.614 (6) | 139.8 |
C38—H38B···O86Ax | 0.98 | 2.57 | 3.395 (10) | 141.4 |
C31—H31B···O86x | 0.99 | 2.98 | 3.960 (7) | 170.1 |
C31—H31B···O88x | 0.99 | 2.64 | 3.427 (6) | 136.2 |
C31—H31B···O88Ax | 0.99 | 2.60 | 3.548 (14) | 160.8 |
C32—H32A···O99xi | 0.99 | 2.77 | 3.731 (5) | 164.5 |
C38—H38C···O96xii | 0.98 | 2.75 | 3.371 (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, y−1/2, −z+1/2; (vi) x, −y+3/2, z−1/2; (vii) −x, y+1/2, −z+1/2; (viii) x, y, z−1; (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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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.