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The crystal structures of (1,5,9,13,20-penta­methyl-3,7,­11,­15,­18,­22-hexa­aza­bi­cyclo­[7.7.7]­tri­cosane-κ6NN′,­N′′,­N′′′,­N′′′′,­N′′′′′)­nickel­(II) di­perchlor­ate–x(water) (x = 0.530), [Ni(C22H48N6)]­(ClO4)2.­0.530H2O, and (1,5,9,­13,­20-penta­methyl-3,7,­11,­15,­18,­22-hexa­aza­bi­cyclo­[7.7.7]­tri­cosane-κ6NN′,­N′′,­N′′′,­N′′′′,­N′′′′′)­zinc­(II) di­per­chlor­ate–x(water) (x = 0.608), [Zn(C22H48N6)]­(ClO4)2.­0.608H2O, are isomorphic and each is described as an intergrowth of four substructures, consistent with different modulations of an idealized parent structure of space group C2/c. Two substructures correspond to alternative orientations of a C1 structure for which x = 0 in the general formula [M(C22H48N6)](ClO4)2.xH2O, and two substructures correspond to alternative origins of a P21/n structure for which x = 1. Twinning also occurs. An analysis of the pseudosymmetry, a description of the refinement and a description of the refined structures are presented. The MN6 coordination geometry is essentially octahedral, in contrast to the trigonal-prismatic geometry observed for the CdII and HgII complexes of the same ligand.

Supporting information

cif

Crystallographic Information File (CIF)
Contains datablocks global, Zn, Ni

hkl

Structure factor file (CIF format)
Contains datablock Ni

hkl

Structure factor file (CIF format)
Contains datablock Zn

CCDC references: 131806; 131807

Computing details top

Data collection: PHILIPS PW1100/20 software for Zn; MSC/AFC Diffractometer Control Software for Ni. For both compounds, cell refinement: PHILIPS PW1100/20 software; data reduction: XTAL_DIFDAT_ADSORB_SORTRF_ADDREF; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: RAELS96 (Rae, 1996); molecular graphics: ORTEPII (Johnson, 1976).

(Zn) top
Crystal data top
[Zn(C22H48N6)](ClO4)2.xH2ODx = 1.41 Mg m3
Monoclinic, C2/cCu Kα radiation, λ = 1.5418 Å
a = 10.191 (5) ÅCell parameters from 25 reflections
b = 17.678 (8) Åθ = 31.9–38.6°
c = 17.754 (9) ŵ = 3.15 mm1
β = 99.42 (2)°T = 295 K
V = 3155 (3) Å3Block, colourless
Z = 40.26 × 0.20 × 0.16 mm
F(000) = 1425.1
Data collection top
Philips PW1100/20 4-circle
diffractometer
2255 reflections with > 3σ(I)
Radiation source: fine-focus sealed tubeθmax = 64.0°, θmin = 3.0°
Graphite monochromatorh = 1111
ω/2θ scank = 020
Absorption correction: analytical (de meulenaer & Tompa, 1965)l = 020
Tmin = 0.567, Tmax = 0.7253 standard reflections every 90 min
2798 measured reflections intensity decay: 7.1%
2798 independent reflections
Refinement top
Refinement on F62 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.054Secondary atom site location: difference Fourier map
wR(F2) = 0.090Hydrogen site location: inferred from neighbouring sites
S = 1.73H-atom parameters not refined
2255 reflectionsCalculated w = 1/[σ2(Fo) + (0.04Fo)2]
254 parameters(Δ/σ)max = 0.29
Special details top

Experimental. The structure also contains 0.608 H2O per formula moiety because the crystal was a four component intergrowth. A water is associated with 2 components of monoclinic P 21/n symmetry. The other two components have a C centred triclinic symmetry C1.

The structure has four intergrowth components, each formed as a modulation of C2/c, using 4 of the 8 equivalent positions. Component 1, C1, positions 1,3,5,7. Component 2, C1, positions 2,4,6,8. Component 3, P21/n, positions 1,3,6,8. Component 4, P21/n, positions 2,4,5,7. Equal populations of components 3 and 4 makes symmetry of average C1. Reflection data was not merged because of triclinic diffraction symmetry.

Populations of the 4 components were 0.299 (6), 0.093 (6), 0.304 (4) 0.304 (4) respectively. Atomic coordinates for cation were the same for components 1 and 3. anions A and B belong to component 1. Anions C and D belong to component 3. Anion C is constrained to be related to A by symmetry operation -x + 1, y, -z + 1/2. In subsequent tables ' indicates an atom obtained by the transformation -x + 1, y, -z + 1/2. Thus anion C is the same as A' and C' is the same as A. Consequently anion C is excluded from the list. Crystal was a 0.466 (10): 0.534 twin.

Geometry. Anion C is the same as anion A'. Atoms marked ' are obtained from unprimed atoms by operation -x + 1,y,-z + 1/2. A l l e.s.d.'s are estimated using the full covariance matrix of the least squares problem and are thus conditional on the assumption that the various restraints and constraints are appropriate.

Refinement. Extensive constraints and restraints used since there are four component structures and the h+k odd data was unobserved. Parent symmetry of C2/c was used to constrain thermal motion and TLX rigid body models were used to constrain exactly tetrahedral anions. Anion has approximate 3 symmetry and differences in so related bonds were restrained to approach zero. More detail is in associated paper

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zn0.5005 (2)0.1568 (1)0.2552 (1)0.043 (1)0.604 (4)
C10.8091 (6)0.1506 (3)0.0856 (4)0.084 (2)0.604 (4)
C20.7066 (5)0.1529 (2)0.1412 (3)0.059 (1)0.604 (4)
C30.2953 (5)0.1619 (2)0.3732 (3)0.059 (1)0.604 (4)
C40.1979 (6)0.1638 (3)0.4317 (4)0.084 (2)0.604 (4)
C110.6538 (5)0.2337 (3)0.1399 (3)0.065 (2)0.604 (4)
N120.5206 (5)0.2388 (2)0.1648 (2)0.057 (1)0.604 (4)
C130.4833 (7)0.3201 (3)0.1721 (4)0.075 (2)0.604 (4)
C140.5238 (7)0.3528 (2)0.2510 (4)0.082 (2)0.604 (4)
C14a0.5108 (19)0.4389 (3)0.2465 (7)0.150 (3)0.604 (4)
C150.4413 (7)0.3234 (3)0.3080 (4)0.075 (2)0.604 (4)
N160.4810 (6)0.2462 (2)0.3386 (2)0.057 (1)0.604 (4)
C170.3988 (5)0.2232 (3)0.3975 (3)0.065 (2)0.604 (4)
C210.7811 (5)0.1308 (3)0.2196 (3)0.058 (1)0.604 (4)
N220.7183 (3)0.1582 (3)0.2851 (3)0.048 (1)0.604 (4)
C230.7872 (6)0.1234 (4)0.3579 (3)0.069 (2)0.604 (4)
C240.7283 (4)0.0494 (3)0.3784 (3)0.072 (2)0.604 (4)
C24a0.8269 (6)0.0109 (6)0.4408 (5)0.115 (2)0.604 (4)
C250.5971 (5)0.0582 (4)0.4064 (3)0.069 (1)0.604 (4)
N260.4812 (4)0.0737 (3)0.3446 (3)0.056 (1)0.604 (4)
C270.3560 (5)0.0828 (3)0.3778 (3)0.063 (2)0.604 (4)
C310.5978 (5)0.0962 (3)0.1112 (3)0.063 (2)0.604 (4)
N320.5185 (5)0.0692 (2)0.1698 (3)0.056 (1)0.604 (4)
C330.3964 (5)0.0289 (3)0.1314 (4)0.069 (1)0.604 (4)
C340.2751 (5)0.0786 (3)0.1123 (3)0.072 (2)0.604 (4)
C34a0.1725 (6)0.0372 (6)0.0542 (5)0.115 (2)0.604 (4)
C350.2105 (6)0.1000 (4)0.1800 (3)0.069 (2)0.604 (4)
N360.2823 (3)0.1608 (3)0.2293 (3)0.048 (1)0.604 (4)
C370.2123 (5)0.1779 (3)0.2953 (3)0.058 (1)0.604 (4)
ClA0.9053 (4)0.3531 (1)0.3671 (2)0.139 (5)0.604 (4)
O1A0.8938 (11)0.2835 (3)0.3319 (6)0.232 (8)0.604 (4)
O2A0.8153 (10)0.3581 (7)0.4168 (6)0.413 (19)0.604 (4)
O3A1.0322 (7)0.3615 (5)0.4068 (6)0.255 (8)0.604 (4)
O4A0.8801 (11)0.4091 (4)0.3129 (5)0.257 (6)0.604 (4)
ClB0.0648 (7)0.3414 (4)0.1140 (7)0.25 (2)0.301 (4)
O1B0.1150 (17)0.2949 (10)0.1739 (11)0.155 (14)0.301 (4)
O2B0.053 (2)0.3014 (11)0.0467 (10)0.56 (3)0.301 (4)
O3B0.0584 (11)0.3676 (10)0.1239 (15)0.80 (7)0.301 (4)
O4B0.1493 (12)0.4017 (7)0.1114 (13)0.154 (19)0.301 (4)
ClD0.8646 (6)0.3186 (3)0.4248 (3)0.140 (9)0.303 (4)
O1D0.8836 (14)0.2933 (7)0.3541 (5)0.194 (15)0.303 (4)
O2D0.8968 (12)0.3941 (4)0.4320 (7)0.107 (6)0.303 (4)
O3D0.7335 (9)0.3089 (8)0.4324 (8)0.254 (15)0.303 (4)
O4D0.9444 (15)0.2781 (6)0.4806 (7)0.33 (2)0.303 (4)
Ow0.6423 (19)0.0780 (7)0.2429 (12)0.176 (6)0.303 (4)
Zn'0.4995 (2)0.15680.2448 (1)0.0430.396 (4)
C1'0.1909 (6)0.1506 (3)0.4144 (4)0.084 (2)0.396 (4)
C2'0.2934 (5)0.1529 (2)0.3588 (3)0.059 (1)0.396 (4)
C3'0.7047 (5)0.1619 (2)0.1268 (3)0.059 (1)0.396 (4)
C4'0.8021 (6)0.1638 (3)0.0683 (4)0.084 (2)0.396 (4)
C11'0.3462 (5)0.2337 (3)0.3601 (3)0.065 (2)0.396 (4)
N12'0.4794 (5)0.2388 (2)0.3352 (2)0.057 (1)0.396 (4)
C13'0.5167 (7)0.3201 (3)0.3279 (4)0.075 (2)0.396 (4)
C14'0.4762 (7)0.3528 (2)0.2490 (4)0.082 (2)0.396 (4)
C14a'0.4892 (19)0.4389 (3)0.2535 (7)0.150 (3)0.396 (4)
C15'0.5587 (7)0.3234 (3)0.1920 (4)0.075 (2)0.396 (4)
N16'0.5190 (6)0.2462 (2)0.1614 (2)0.057 (1)0.396 (4)
C17'0.6012 (5)0.2232 (3)0.1025 (3)0.065 (2)0.396 (4)
C21'0.2189 (5)0.1308 (3)0.2804 (3)0.058 (1)0.396 (4)
N22'0.2817 (3)0.1582 (3)0.2149 (3)0.048 (1)0.396 (4)
C23'0.2128 (6)0.1234 (4)0.1421 (3)0.069 (2)0.396 (4)
C24'0.2717 (4)0.0494 (3)0.1216 (3)0.072 (2)0.396 (4)
C24a'0.1731 (6)0.0109 (6)0.0592 (5)0.115 (2)0.396 (4)
C25'0.4029 (5)0.0582 (4)0.0936 (3)0.069 (1)0.396 (4)
N26'0.5188 (4)0.0737 (3)0.1554 (3)0.056 (1)0.396 (4)
C27'0.6440 (5)0.0828 (3)0.1222 (3)0.063 (2)0.396 (4)
C31'0.4022 (5)0.0962 (3)0.3888 (3)0.063 (2)0.396 (4)
N32'0.4815 (5)0.0692 (2)0.3302 (3)0.056 (1)0.396 (4)
C33'0.6036 (5)0.0289 (3)0.3686 (4)0.069 (1)0.396 (4)
C34'0.7249 (5)0.0786 (3)0.3877 (3)0.072 (2)0.396 (4)
C34a'0.8275 (6)0.0372 (6)0.4458 (5)0.115 (2)0.396 (4)
C35'0.7895 (6)0.1000 (4)0.3200 (3)0.069 (2)0.396 (4)
N36'0.7177 (3)0.1608 (3)0.2707 (3)0.048 (1)0.396 (4)
C37'0.7877 (5)0.1779 (3)0.2047 (3)0.058 (1)0.396 (4)
ClA'0.0947 (4)0.3531 (1)0.1329 (2)0.139 (6)0.396 (4)
O1A'0.1062 (11)0.2835 (3)0.1681 (6)0.232 (5)0.396 (4)
O2A'0.1847 (10)0.3581 (7)0.0832 (6)0.41 (2)0.396 (4)
O3A'0.0322 (7)0.3615 (5)0.0932 (6)0.255 (9)0.396 (4)
O4A'0.1199 (11)0.4091 (4)0.1871 (5)0.257 (10)0.396 (4)
ClB'0.9352 (7)0.3414 (4)0.3860 (7)0.247 (13)0.094 (5)
O1B'0.8850 (17)0.2949 (10)0.3261 (11)0.155 (15)0.094 (5)
O2B'0.947 (2)0.3014 (11)0.4533 (10)0.56 (5)0.094 (5)
O3B'1.0584 (11)0.3676 (10)0.3761 (15)0.80 (4)0.094 (5)
O4B'0.8507 (12)0.4017 (7)0.3886 (13)0.154 (11)0.094 (5)
ClD'0.1354 (6)0.3186 (3)0.0752 (3)0.120 (7)0.303 (4)
O1D'0.1164 (14)0.2933 (7)0.1459 (5)0.150 (9)0.303 (4)
O2D'0.1032 (12)0.3941 (4)0.0680 (7)0.138 (8)0.303 (4)
O3D'0.2665 (9)0.3089 (8)0.0676 (8)0.219 (12)0.303 (4)
O4D'0.0556 (15)0.2781 (6)0.0194 (7)0.296 (16)0.303 (4)
Ow'0.3577 (19)0.0780 (7)0.2571 (12)0.176 (6)0.303 (4)
H1C10.84650.09840.08470.0840.604
H2C10.76430.16490.03320.0840.604
H3C10.88270.18720.10320.0840.604
H1C40.12780.12440.41810.0840.604
H2C40.24800.15350.48400.0840.604
H3C40.15530.21490.43080.0840.604
H1C110.71850.26530.17500.0650.604
H2C110.64590.25380.08670.0650.604
H1C130.38440.32450.15810.0750.604
H2C130.52680.35050.13560.0750.604
H1C140.61910.33970.26940.0820.604
H1C14a0.56520.45890.20880.1500.604
H2C14a0.41540.45290.22980.1500.604
H3C14a0.54330.46130.29790.1500.604
H1C150.36050.30990.27040.0750.604
H2C150.41360.34650.35430.0750.604
H1C170.35120.26910.41180.0650.604
H2C170.46060.20420.44320.0650.604
H1C210.78620.07430.22220.0580.604
H2C210.87300.15220.22530.0580.604
H1C230.78300.16010.40030.0690.604
H2C230.88220.11440.35280.0690.604
H1C240.71460.01620.33220.0720.604
H1C24a0.91440.00470.42290.1150.604
H2C24a0.83900.04260.48800.1150.604
H3C24a0.79190.04000.45230.1150.604
H1C250.60910.10990.42940.0690.604
H2C250.55220.02490.44000.0690.604
H1C270.37610.06830.43290.0630.604
H2C270.28810.04740.35020.0630.604
H1C310.53560.12080.06880.0630.604
H2C310.64050.05140.09090.0630.604
H1C330.37530.01240.16610.0690.604
H2C330.41620.00630.08280.0690.604
H1C340.30170.12610.08810.0720.604
H1C34a0.21390.02260.00900.1150.604
H2C34a0.14180.00930.07820.1150.604
H3C34a0.09490.07120.03750.1150.604
H1C350.23790.05510.21310.0690.604
H2C350.11680.11390.18390.0690.604
H1C370.12990.14640.29000.0580.604
H2C370.18760.23270.29310.0580.604
H1N120.45710.22030.11960.0570.604
H1N220.74200.21310.28990.0480.604
H1N320.57450.02880.19860.0560.604
H1N160.57290.25290.36770.0570.604
H1N260.46780.02470.31630.0560.604
H1N360.26490.20710.19670.0480.604
H1C1'0.15350.09840.41530.0840.604
H2C1'0.23570.16490.46680.0840.604
H3C1'0.11730.18720.39680.0840.604
H1C4'0.87220.12440.08190.0840.604
H2C4'0.75200.15350.01600.0840.604
H3C4'0.84470.21490.06920.0840.604
H1C11'0.28150.26530.32500.0650.604
H2C11'0.35410.25380.41330.0650.604
H1C13'0.61560.32450.34190.0750.604
H2C13'0.47320.35050.36440.0750.604
H1C14'0.38090.33970.23060.0820.604
H1C14a'0.43480.45890.29120.1500.604
H2C14a'0.58460.45290.27020.1500.604
H3C14a'0.45670.46130.20210.1500.604
H1C15'0.63950.30990.22960.0750.604
H2C15'0.58640.34650.14570.0750.604
H1C17'0.64880.26910.08820.0650.604
H2C17'0.53940.20420.05680.0650.604
H1C21'0.21380.07430.27780.0580.604
H2C21'0.12700.15220.27470.0580.604
H1C23'0.21700.16010.09970.0690.396
H2C23'0.11780.11440.14720.0690.396
H1C24'0.28540.01620.16780.0720.396
H1C24a'0.08560.00470.07710.1150.396
H2C24a'0.16100.04260.01200.1150.396
H3C24a'0.20810.04000.04770.1150.396
H1C25'0.39090.10990.07060.0690.396
H2C25'0.44780.02490.06000.0690.396
H1C27'0.62390.06830.06710.0630.396
H2C27'0.71190.04740.14980.0630.396
H1C31'0.46440.12080.43120.0630.396
H2C31'0.35950.05140.40910.0630.396
H1C33'0.62470.01240.33390.0690.396
H2C33'0.58380.00630.41720.0690.396
H1C34'0.69830.12610.41190.0720.396
H1C34a'0.78610.02260.49100.1150.396
H2C34a'0.85820.00930.42180.1150.396
H3C34a'0.90510.07120.46250.1150.396
H1C35'0.76210.05510.28690.0690.396
H2C35'0.88320.11390.31610.0690.396
H1C37'0.87010.14640.21000.0580.396
H2C37'0.81240.23270.20690.0580.396
H1N12'0.54290.22030.38040.0570.396
H1N22'0.25800.21310.21010.0480.396
H1N32'0.42550.02880.30140.0560.396
H1N16'0.42710.25290.13230.0570.396
H1N26'0.53220.02470.18370.0560.396
H1N36'0.73510.20710.30330.0480.396
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn0.0410.0360.049 (1)0.0000.0020.000
C10.072 (3)0.116 (4)0.073 (4)0.008 (4)0.035 (2)0.006 (5)
C20.050 (2)0.074 (2)0.055 (2)0.003 (3)0.017 (2)0.006 (3)
C30.050 (2)0.074 (2)0.055 (2)0.003 (3)0.017 (2)0.006 (3)
C40.072 (3)0.116 (4)0.073 (4)0.008 (4)0.035 (2)0.006 (5)
C110.062 (4)0.069 (3)0.065 (4)0.008 (3)0.016 (3)0.012 (3)
N120.054 (2)0.054 (2)0.062 (2)0.002 (1)0.011 (1)0.012 (1)
C130.079 (4)0.045 (2)0.106 (5)0.009 (3)0.027 (4)0.022 (2)
C140.070 (6)0.039 (3)0.142 (6)0.0000.038 (6)0.000
C14a0.156 (7)0.038 (3)0.283 (8)0.0000.113 (8)0.000
C150.079 (4)0.045 (2)0.106 (5)0.009 (3)0.027 (4)0.022 (2)
N160.054 (2)0.054 (2)0.062 (2)0.002 (1)0.011 (1)0.012 (1)
C170.062 (4)0.069 (3)0.065 (4)0.008 (3)0.016 (3)0.012 (3)
C210.046 (2)0.064 (3)0.066 (3)0.000 (3)0.017 (2)0.001 (3)
N220.041 (1)0.054 (1)0.048 (2)0.001 (1)0.001 (1)0.001 (1)
C230.050 (2)0.079 (4)0.075 (5)0.003 (2)0.003 (3)0.019 (3)
C240.058 (2)0.081 (5)0.076 (3)0.025 (3)0.008 (2)0.031 (3)
C24a0.078 (3)0.154 (5)0.110 (4)0.039 (3)0.005 (3)0.068 (4)
C250.065 (3)0.062 (3)0.076 (4)0.008 (2)0.002 (3)0.025 (2)
N260.050 (1)0.048 (1)0.072 (2)0.003 (1)0.009 (1)0.013 (1)
C270.052 (4)0.072 (3)0.069 (3)0.000 (3)0.016 (3)0.018 (2)
C310.052 (4)0.072 (3)0.069 (3)0.000 (3)0.016 (3)0.018 (2)
N320.050 (1)0.048 (1)0.072 (2)0.003 (1)0.009 (1)0.013 (1)
C330.065 (3)0.062 (3)0.076 (4)0.008 (2)0.002 (3)0.025 (2)
C340.058 (2)0.081 (5)0.076 (3)0.025 (3)0.008 (2)0.031 (3)
C34a0.078 (3)0.154 (5)0.110 (4)0.039 (3)0.005 (3)0.068 (4)
C350.050 (2)0.079 (4)0.075 (5)0.003 (2)0.003 (3)0.019 (3)
N360.041 (1)0.054 (1)0.048 (2)0.001 (1)0.001 (1)0.001 (1)
C370.046 (2)0.064 (3)0.066 (3)0.000 (3)0.017 (2)0.001 (3)
ClA0.216 (5)0.072 (4)0.099 (7)0.014 (2)0.067 (3)0.009 (4)
O1A0.337 (11)0.076 (9)0.225 (10)0.033 (4)0.122 (7)0.044 (6)
O2A0.444 (17)0.53 (3)0.286 (17)0.116 (17)0.133 (17)0.010 (15)
O3A0.308 (8)0.170 (9)0.212 (12)0.098 (8)0.183 (9)0.042 (8)
O4A0.262 (13)0.121 (5)0.327 (16)0.039 (5)0.131 (9)0.121 (9)
ClB0.060 (11)0.163 (16)0.49 (4)0.031 (5)0.050 (11)0.22 (2)
O1B0.094 (13)0.114 (17)0.26 (3)0.004 (8)0.043 (11)0.09 (2)
O2B0.76 (5)0.40 (4)0.36 (5)0.43 (4)0.39 (3)0.19 (3)
O3B0.113 (11)0.47 (5)1.85 (10)0.149 (14)0.30 (2)0.81 (7)
O4B0.071 (13)0.068 (14)0.32 (4)0.008 (5)0.020 (10)0.077 (19)
ClD0.183 (11)0.093 (10)0.121 (9)0.017 (5)0.041 (6)0.020 (8)
O1D0.197 (19)0.176 (14)0.195 (13)0.027 (11)0.009 (12)0.119 (13)
O2D0.125 (9)0.089 (8)0.084 (8)0.001 (6)0.048 (6)0.020 (7)
O3D0.255 (15)0.27 (3)0.25 (3)0.153 (17)0.067 (15)0.127 (18)
O4D0.50 (4)0.134 (15)0.27 (2)0.032 (12)0.16 (2)0.055 (13)
Ow0.181 (13)0.065 (7)0.258 (17)0.013 (8)0.029 (15)0.012 (10)
Zn'0.0410.0360.049 (1)0.0000.0020.000
C1'0.072 (3)0.116 (4)0.073 (4)0.008 (4)0.035 (2)0.006 (5)
C2'0.050 (2)0.074 (2)0.055 (2)0.003 (3)0.017 (2)0.006 (3)
C3'0.050 (2)0.074 (2)0.055 (2)0.003 (3)0.017 (2)0.006 (3)
C4'0.072 (3)0.116 (4)0.073 (4)0.008 (4)0.035 (2)0.006 (5)
C11'0.062 (4)0.069 (3)0.065 (4)0.008 (3)0.016 (3)0.012 (3)
N12'0.054 (2)0.054 (2)0.062 (2)0.002 (1)0.011 (1)0.012 (1)
C13'0.079 (4)0.045 (2)0.106 (5)0.009 (3)0.027 (4)0.022 (2)
C14'0.070 (6)0.039 (3)0.142 (6)0.0000.038 (6)0.000
C14a'0.156 (7)0.038 (3)0.283 (8)0.0000.113 (8)0.000
C15'0.079 (4)0.045 (2)0.106 (5)0.009 (3)0.027 (4)0.022 (2)
N16'0.054 (2)0.054 (2)0.062 (2)0.002 (1)0.011 (1)0.012 (1)
C17'0.062 (4)0.069 (3)0.065 (4)0.008 (3)0.016 (3)0.012 (3)
C21'0.046 (2)0.064 (3)0.066 (3)0.000 (3)0.017 (2)0.001 (3)
N22'0.041 (1)0.054 (1)0.048 (2)0.001 (1)0.001 (1)0.001 (1)
C23'0.050 (2)0.079 (4)0.075 (5)0.003 (2)0.003 (3)0.019 (3)
C24'0.058 (2)0.081 (5)0.076 (3)0.025 (3)0.008 (2)0.031 (3)
C24a'0.078 (3)0.154 (5)0.110 (4)0.039 (3)0.005 (3)0.068 (4)
C25'0.065 (3)0.062 (3)0.076 (4)0.008 (2)0.002 (3)0.025 (2)
N26'0.050 (1)0.048 (1)0.072 (2)0.003 (1)0.009 (1)0.013 (1)
C27'0.052 (4)0.072 (3)0.069 (3)0.000 (3)0.016 (3)0.018 (2)
C31'0.052 (4)0.072 (3)0.069 (3)0.000 (3)0.016 (3)0.018 (2)
N32'0.050 (1)0.048 (1)0.072 (2)0.003 (1)0.009 (1)0.013 (1)
C33'0.065 (3)0.062 (3)0.076 (4)0.008 (2)0.002 (3)0.025 (2)
C34'0.058 (2)0.081 (5)0.076 (3)0.025 (3)0.008 (2)0.031 (3)
C34a'0.078 (3)0.154 (5)0.110 (4)0.039 (3)0.005 (3)0.068 (4)
C35'0.050 (2)0.079 (4)0.075 (5)0.003 (2)0.003 (3)0.019 (3)
N36'0.041 (1)0.054 (1)0.048 (2)0.001 (1)0.001 (1)0.001 (1)
C37'0.046 (2)0.064 (3)0.066 (3)0.000 (3)0.017 (2)0.001 (3)
ClA'0.216 (5)0.072 (4)0.099 (7)0.014 (2)0.067 (3)0.009 (4)
O1A'0.337 (11)0.076 (9)0.225 (10)0.033 (4)0.122 (7)0.044 (6)
O2A'0.444 (17)0.53 (3)0.286 (17)0.116 (17)0.133 (17)0.010 (15)
O3A'0.308 (8)0.170 (9)0.212 (12)0.098 (8)0.183 (9)0.042 (8)
O4A'0.262 (13)0.121 (5)0.327 (16)0.039 (5)0.131 (9)0.121 (9)
ClB'0.060 (11)0.163 (16)0.49 (4)0.031 (5)0.050 (11)0.22 (2)
O1B'0.094 (13)0.114 (17)0.26 (3)0.004 (8)0.043 (11)0.09 (2)
O2B'0.76 (5)0.40 (4)0.36 (5)0.43 (4)0.39 (3)0.19 (3)
O3B'0.113 (11)0.47 (5)1.85 (10)0.149 (14)0.30 (2)0.81 (7)
O4B'0.071 (13)0.068 (14)0.32 (4)0.008 (5)0.020 (10)0.077 (19)
ClD'0.183 (11)0.093 (10)0.121 (9)0.017 (5)0.041 (6)0.020 (8)
O1D'0.197 (19)0.176 (14)0.195 (13)0.027 (11)0.009 (12)0.119 (13)
O2D'0.125 (9)0.089 (8)0.084 (8)0.001 (6)0.048 (6)0.020 (7)
O3D'0.255 (15)0.27 (3)0.25 (3)0.153 (17)0.067 (15)0.127 (18)
O4D'0.50 (4)0.134 (15)0.27 (2)0.032 (12)0.16 (2)0.055 (13)
Ow'0.181 (13)0.065 (7)0.258 (17)0.013 (8)0.029 (15)0.012 (10)
H1C10.0720.1160.0730.0080.0350.006
H2C10.0720.1160.0730.0080.0350.006
H3C10.0720.1160.0730.0080.0350.006
H1C40.0720.1160.0730.0080.0350.006
H2C40.0720.1160.0730.0080.0350.006
H3C40.0720.1160.0730.0080.0350.006
H1C110.0620.0690.0650.0080.0160.012
H2C110.0620.0690.0650.0080.0160.012
H1C130.0790.0450.1060.0090.0270.022
H2C130.0790.0450.1060.0090.0270.022
H1C140.0700.0390.1420.0000.0380.000
H1C14a0.1560.0380.2830.0000.1130.000
H2C14a0.1560.0380.2830.0000.1130.000
H3C14a0.1560.0380.2830.0000.1130.000
H1C150.0790.0450.1060.0090.0270.022
H2C150.0790.0450.1060.0090.0270.022
H1C170.0620.0690.0650.0080.0160.012
H2C170.0620.0690.0650.0080.0160.012
H1C210.0460.0640.0660.0000.0170.001
H2C210.0460.0640.0660.0000.0170.001
H1C230.0500.0790.0750.0030.0030.019
H2C230.0500.0790.0750.0030.0030.019
H1C240.0580.0810.0760.0250.0080.031
H1C24a0.0780.1540.1100.0390.0050.068
H2C24a0.0780.1540.1100.0390.0050.068
H3C24a0.0780.1540.1100.0390.0050.068
H1C250.0650.0620.0760.0080.0020.025
H2C250.0650.0620.0760.0080.0020.025
H1C270.0520.0720.0690.0000.0160.018
H2C270.0520.0720.0690.0000.0160.018
H1C310.0520.0720.0690.0000.0160.018
H2C310.0520.0720.0690.0000.0160.018
H1C330.0650.0620.0760.0080.0020.025
H2C330.0650.0620.0760.0080.0020.025
H1C340.0580.0810.0760.0250.0080.031
H1C34a0.0780.1540.1100.0390.0050.068
H2C34a0.0780.1540.1100.0390.0050.068
H3C34a0.0780.1540.1100.0390.0050.068
H1C350.0500.0790.0750.0030.0030.019
H2C350.0500.0790.0750.0030.0030.019
H1C370.0460.0640.0660.0000.0170.001
H2C370.0460.0640.0660.0000.0170.001
H1N120.0540.0540.0620.0020.0110.012
H1N220.0410.0540.0480.0010.0010.001
H1N320.0500.0480.0720.0030.0090.013
H1N160.0540.0540.0620.0020.0110.012
H1N260.0500.0480.0720.0030.0090.013
H1N360.0410.0540.0480.0010.0010.001
H1C1'0.0720.1160.0730.0080.0350.006
H2C1'0.0720.1160.0730.0080.0350.006
H3C1'0.0720.1160.0730.0080.0350.006
H1C4'0.0720.1160.0730.0080.0350.006
H2C4'0.0720.1160.0730.0080.0350.006
H3C4'0.0720.1160.0730.0080.0350.006
H1C11'0.0620.0690.0650.0080.0160.012
H2C11'0.0620.0690.0650.0080.0160.012
H1C13'0.0790.0450.1060.0090.0270.022
H2C13'0.0790.0450.1060.0090.0270.022
H1C14'0.0700.0390.1420.0000.0380.000
H1C14a'0.1560.0380.2830.0000.1130.000
H2C14a'0.1560.0380.2830.0000.1130.000
H3C14a'0.1560.0380.2830.0000.1130.000
H1C15'0.0790.0450.1060.0090.0270.022
H2C15'0.0790.0450.1060.0090.0270.022
H1C17'0.0620.0690.0650.0080.0160.012
H2C17'0.0620.0690.0650.0080.0160.012
H1C21'0.0460.0640.0660.0000.0170.001
H2C21'0.0460.0640.0660.0000.0170.001
H1C23'0.0500.0790.0750.0030.0030.019
H2C23'0.0500.0790.0750.0030.0030.019
H1C24'0.0580.0810.0760.0250.0080.031
H1C24a'0.0780.1540.1100.0390.0050.068
H2C24a'0.0780.1540.1100.0390.0050.068
H3C24a'0.0780.1540.1100.0390.0050.068
H1C25'0.0650.0620.0760.0080.0020.025
H2C25'0.0650.0620.0760.0080.0020.025
H1C27'0.0520.0720.0690.0000.0160.018
H2C27'0.0520.0720.0690.0000.0160.018
H1C31'0.0520.0720.0690.0000.0160.018
H2C31'0.0520.0720.0690.0000.0160.018
H1C33'0.0650.0620.0760.0080.0020.025
H2C33'0.0650.0620.0760.0080.0020.025
H1C34'0.0580.0810.0760.0250.0080.031
H1C34a'0.0780.1540.1100.0390.0050.068
H2C34a'0.0780.1540.1100.0390.0050.068
H3C34a'0.0780.1540.1100.0390.0050.068
H1C35'0.0500.0790.0750.0030.0030.019
H2C35'0.0500.0790.0750.0030.0030.019
H1C37'0.0460.0640.0660.0000.0170.001
H2C37'0.0460.0640.0660.0000.0170.001
H1N12'0.0540.0540.0620.0020.0110.012
H1N22'0.0410.0540.0480.0010.0010.001
H1N32'0.0500.0480.0720.0030.0090.013
H1N16'0.0540.0540.0620.0020.0110.012
H1N26'0.0500.0480.0720.0030.0090.013
H1N36'0.0410.0540.0480.0010.0010.001
Geometric parameters (Å, º) top
Zn—N122.196 (2)Zn—N162.196 (2)
Zn—N222.196 (2)Zn—N262.196 (2)
Zn—N322.196 (2)Zn—N362.196 (2)
C1—C21.549 (6)C3—C41.549 (6)
C2—C111.524 (3)C2—C211.524 (3)
C11—N121.497 (4)C21—N221.497 (4)
N12—C131.498 (4)N22—C231.497 (4)
C13—C141.509 (4)C23—C241.509 (4)
C14—C14a1.529 (5)C24—C24a1.529 (5)
C14—C151.509 (4)C24—C251.509 (4)
C15—N161.500 (4)C25—N261.500 (4)
C3—C171.524 (3)C3—C271.524 (3)
N16—C171.499 (4)N26—C271.499 (4)
C2—C311.524 (3)ClA—O1A1.376 (3)
C31—N321.497 (4)N22—O1A2.882 (9)
N32—C331.497 (4)N36—O1B2.990 (14)
C33—C341.509 (4)N36—O1C2.909 (8)
C34—C34a1.529 (5)N22—O1D3.060 (12)
C34—C351.509 (4)N16—O3D3.037 (11)
C35—N361.500 (4)N32—Ow3.083 (15)
C3—C371.524 (3)O4Ci—Ow3.13 (2)
N36—C371.499 (4)O1Dii—Ow2.84 (2)
N12—Zn—N1692.7 (1)Zn—N26—C27113.3 (3)
N12—Zn—N2287.6 (2)C25—N26—C27110.5 (3)
N12—Zn—N26179.3 (2)C3—C27—N26116.2 (5)
N12—Zn—N3286.2 (2)C2—C31—N32114.3 (5)
N12—Zn—N3692.2 (2)Zn—N32—C31111.7 (3)
N16—Zn—N2291.6 (2)Zn—N32—C33119.5 (3)
N16—Zn—N2688.0 (2)C31—N32—C33109.8 (3)
N16—Zn—N32178.8 (2)N32—C33—C34114.5 (3)
N16—Zn—N3685.3 (2)C33—C34—C34a108.5 (3)
N22—Zn—N2692.2 (2)C33—C34—C35114.5 (5)
N22—Zn—N3288.8 (2)C34a—C34—C35108.5 (2)
N22—Zn—N36176.9 (1)C34—C35—N36114.2 (3)
N26—Zn—N3293.1 (1)Zn—N36—C35118.6 (3)
N26—Zn—N3688.0 (2)Zn—N36—C37116.0 (3)
N32—Zn—N3694.3 (2)C35—N36—C37110.6 (3)
C1—C2—C11106.8 (3)C3—C37—N36114.1 (4)
C1—C2—C21106.7 (3)N22—O1A—ClA145.1 (7)
C1—C2—C31106.7 (3)C21—N22—O1A98.5 (4)
C11—C2—C21112.1 (3)C23—N22—O1A83.4 (3)
C11—C2—C31112.0 (3)Zn—N22—O1A129.3 (3)
C21—C2—C31112.0 (3)N36—O1B—ClB148.0 (12)
C4—C3—C17106.5 (3)C35—N36—O1B100.3 (5)
C4—C3—C27106.4 (3)C37—N36—O1B77.2 (5)
C4—C3—C37106.4 (3)Zn—N36—O1B126.7 (4)
C17—C3—C27112.3 (3)N36—O1C—ClC146.9 (7)
C17—C3—C37112.3 (3)C35—N36—O1C96.0 (4)
C27—C3—C37112.3 (3)C37—N36—O1C78.4 (3)
C2—C11—N12112.8 (4)Zn—N36—O1C130.1 (3)
Zn—N12—C11111.9 (3)N22—O1D—ClD117.9 (6)
Zn—N12—C13121.0 (3)C21—N22—O1D106.6 (3)
C11—N12—C13109.8 (3)C23—N22—O1D79.9 (4)
N12—C13—C14114.4 (3)Zn—N22—O1D125.0 (3)
C13—C14—C14a108.9 (3)N16—O3D—ClD137.8 (7)
C13—C14—C15113.1 (5)C15—N16—O3D91.2 (5)
C14a—C14—C15108.9 (3)C17—N16—O3D103.7 (4)
C14—C15—N16114.2 (3)Zn—N16—O3D118.1 (3)
Zn—N16—C15117.3 (4)C31—N32—Ow109.4 (5)
Zn—N16—C17113.4 (3)C33—N32—Ow92.5 (4)
C15—N16—C17110.6 (3)Zn—N32—Ow112.3 (4)
C3—C17—N16115.8 (5)N32—Ow—O4Ci84.9 (5)
C2—C21—N22114.5 (4)N32—Ow—O1Dii115.4 (7)
Zn—N22—C21110.6 (3)O4Ci—Ow—O1Dii100.5 (6)
Zn—N22—C23121.2 (3)Ow—O1Dii—ClDii106.2 (8)
C21—N22—C23109.8 (3)Ow—O4Ci—ClCi104.8 (6)
N22—C23—C24114.5 (3)N12—Zn—C252.6 (1)
C23—C24—C24a108.7 (3)N22—Zn—C253.2 (1)
C23—C24—C25113.5 (5)N32—Zn—C253.2 (1)
C24a—C24—C25108.7 (2)N16—Zn—C352.9 (1)
C24—C25—N26114.3 (3)N26—Zn—C353.0 (1)
Zn—N26—C25119.9 (3)N36—Zn—C352.2 (1)
N12—C2—C3—N1660.4 (2)N12—C11—C2—C3140.9 (6)
N22—C2—C3—N2661.2 (2)N22—C21—C2—C1157.0 (4)
N32—C2—C3—N3660.4 (2)N22—C21—C2—C1140.4 (6)
C11—N12—Zn—N16116.3 (3)N22—C21—C2—C3186.5 (5)
C13—N12—Zn—N1615.5 (5)N32—C31—C2—C1158.5 (4)
C11—N12—Zn—N2224.8 (3)N32—C31—C2—C1184.9 (5)
C13—N12—Zn—N22107.1 (4)N32—C31—C2—C2142.0 (6)
C11—N12—Zn—N3264.2 (3)N16—C17—C3—C4196.0 (3)
C13—N12—Zn—N32164.0 (4)N16—C17—C3—C2779.8 (5)
C11—N12—Zn—N36158.3 (3)N16—C17—C3—C3747.9 (5)
C13—N12—Zn—N3669.8 (4)N26—C27—C3—C4197.6 (4)
C15—N16—Zn—N1219.8 (5)N26—C27—C3—C1746.3 (6)
C17—N16—Zn—N12150.7 (3)N26—C27—C3—C3781.5 (5)
C15—N16—Zn—N22107.5 (4)N36—C37—C3—C4193.4 (4)
C17—N16—Zn—N22121.6 (3)N36—C37—C3—C1777.3 (5)
C15—N16—Zn—N26199.6 (4)N36—C37—C3—C2750.5 (5)
C17—N16—Zn—N2629.4 (3)Zn—N12—C11—C235.4 (5)
C15—N16—Zn—N3672.2 (4)C13—N12—C11—C2172.6 (4)
C17—N16—Zn—N3658.7 (3)C14—C13—N12—Zn40.5 (6)
C21—N22—Zn—N1261.8 (3)C14—C13—N12—C1192.2 (6)
C23—N22—Zn—N12192.3 (4)C14a—C14—C13—N12166.6 (7)
C21—N22—Zn—N16154.4 (3)C15—C14—C13—N1272.2 (6)
C23—N22—Zn—N1675.1 (4)N16—C15—C14—C1379.3 (7)
C21—N22—Zn—N26117.5 (3)N16—C15—C14—C14a159.4 (8)
C23—N22—Zn—N2613.0 (4)Zn—N16—C15—C1450.6 (8)
C21—N22—Zn—N3224.5 (3)C17—N16—C15—C14182.9 (5)
C23—N22—Zn—N32106.1 (4)C3—C17—N16—Zn26.4 (5)
C25—N26—Zn—N1676.8 (5)C3—C17—N16—C15107.8 (5)
C27—N26—Zn—N1656.6 (3)Zn—N22—C21—C235.1 (4)
C25—N26—Zn—N2214.7 (4)C23—N22—C21—C2171.4 (3)
C27—N26—Zn—N22148.1 (3)C24—C23—N22—Zn40.5 (6)
C25—N26—Zn—N32103.7 (4)C24—C23—N22—C2190.3 (6)
C27—N26—Zn—N32122.9 (3)C24a—C24—C23—N22165.6 (5)
C25—N26—Zn—N36197.8 (4)C25—C24—C23—N2273.3 (5)
C27—N26—Zn—N3628.7 (3)N26—C25—C24—C2376.0 (6)
C31—N32—Zn—N1227.8 (3)N26—C25—C24—C24a197.1 (6)
C33—N32—Zn—N12102.2 (4)Zn—N26—C25—C2444.5 (7)
C31—N32—Zn—N2259.9 (3)C27—N26—C25—C24179.1 (5)
C33—N32—Zn—N22189.9 (4)C3—C27—N26—Zn25.7 (5)
C31—N32—Zn—N26152.0 (3)C3—C27—N26—C25112.1 (5)
C33—N32—Zn—N2677.9 (4)Zn—N32—C31—C231.9 (5)
C31—N32—Zn—N36119.8 (3)C33—N32—C31—C2166.8 (3)
C33—N32—Zn—N3610.3 (4)C34—C33—N32—Zn38.7 (6)
C35—N36—Zn—N1298.1 (4)C34—C33—N32—C3192.2 (6)
C37—N36—Zn—N12126.5 (3)C34a—C34—C33—N32163.7 (5)
C35—N36—Zn—N16190.7 (4)C35—C34—C33—N3274.9 (5)
C37—N36—Zn—N1634.0 (3)N36—C35—C34—C3377.0 (6)
C35—N36—Zn—N2681.2 (4)N36—C35—C34—C34a161.6 (6)
C37—N36—Zn—N2654.2 (4)Zn—N36—C35—C3441.9 (7)
C35—N36—Zn—N3211.8 (4)C37—N36—C35—C34179.4 (5)
C37—N36—Zn—N32147.2 (4)C3—C37—N36—Zn21.1 (5)
N12—C11—C2—C1202.6 (4)C3—C37—N36—C35117.7 (5)
N12—C11—C2—C2186.0 (5)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+3/2, y1/2, z+1/2.
(Ni) top
Crystal data top
[Ni(C22H48N6)](ClO4)2.xH2ODx = 1.42 Mg m3
Monoclinic, C2/cCu Kα radiation, λ = 1.5418 Å
a = 10.177 (1) ÅCell parameters from 25 reflections
b = 17.648 (2) Åθ = 31.9–39.5°
c = 17.605 (2) ŵ = 2.96 mm1
β = 99.70 (1)°T = 295 K
V = 3117 (1) Å3Block, pink
Z = 40.24 × 0.18 × 0.14 mm
F(000) = 1404.1
Data collection top
Rigaku AFC6R 4-circle
diffractometer
4104 reflections with > 3σ(I)
Radiation source: rotating anodeθmax = 60.5°, θmin = 3.0°
Graphite monochromatorh = 1111
ω/2θ scank = 200
Absorption correction: analytical (de meulenaer & Tompa, 1965)l = 2020
Tmin = 0.629, Tmax = 0.7333 standard reflections every 150 reflections
9441 measured reflections intensity decay: 4.6%
9441 independent reflections
Refinement top
Refinement on F62 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.074Secondary atom site location: difference Fourier map
wR(F2) = 0.137Hydrogen site location: inferred from neighbouring sites
S = 1.91H-atom parameters not refined
4104 reflectionsCalculated w = 1/[σ2(Fo) + (0.04Fo)2]
269 parameters(Δ/σ)max = 0.32
Special details top

Experimental. The structure also contains 0.530 H2O per formula moiety because the crystal was a four component intergrowth. A water is associated with 2 components of monoclinic P 21/n symmetry. The other two components have a C centred triclinic symmetry C1.

The structure has four intergrowth components, each formed as a modulation of C2/c, using 4 of the 8 equivalent positions. Component 1, C1, positions 1,3,5,7. Component 2, C1, positions 2,4,6,8. Component 3, P21/n, positions 1,3,6,8. Component 4, P21/n, positions 2,4,5,7. Unequal populations of components makes symmetry of average P1. Reflection data was not merged because of triclinic diffraction symmetry.

Populations of the 4 components were 0.299 (4), 0.171 (4), 0.306 (4) 0.224 (4) respectively. Only atoms of comonents 1 and 3 are listed. Atoms for components 2 and 4 are obtained using the transformation - x+1,y,-z+1/2. Anions A and B belong to component 1. Anions C and D and atom Ow belong to component 3. In tables indicates a cation atom of component 3. Crystal was a 0.635 (13) : 0.365 twin.

Geometry. All e.s.d.'s are estimated using the full covariance matrix of the least squares problem and are thus conditional on the assumption that the various restraints and constraints are appropriate.

Refinement. Extensive constraints and restraints used since there are four component structures and the h+k odd data was limited in quality. Parent symmetry of C2/c was used to constrain thermal motion and TLX rigid body models were used to constrain exactly tetrahedral anions. Anion has approximate 3 symmetry and differences in so related bonds were restrained to approach zero. More detail is in associated paper

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni0.5038 (5)0.1588 (1)0.2506 (3)0.047 (1)0.299 (4)
C10.8115 (7)0.1517 (3)0.0825 (4)0.091 (2)0.299 (4)
C20.7099 (6)0.1541 (2)0.1378 (4)0.063 (1)0.299 (4)
C30.2996 (6)0.1635 (2)0.3697 (4)0.063 (1)0.299 (4)
C40.2026 (7)0.1656 (3)0.4276 (4)0.091 (2)0.299 (4)
C110.6535 (6)0.2340 (3)0.1366 (4)0.067 (1)0.299 (4)
N120.5219 (6)0.2387 (2)0.1618 (4)0.059 (1)0.299 (4)
C130.4795 (7)0.3186 (3)0.1690 (4)0.079 (2)0.299 (4)
C140.5272 (7)0.3529 (2)0.2469 (4)0.082 (2)0.299 (4)
C14a0.507 (2)0.4390 (3)0.2407 (7)0.141 (2)0.299 (4)
C150.4547 (8)0.3236 (3)0.3085 (4)0.079 (2)0.299 (4)
N160.4878 (6)0.2443 (2)0.3345 (3)0.059 (1)0.299 (4)
C170.4058 (6)0.2233 (3)0.3944 (4)0.067 (1)0.299 (4)
C210.7834 (6)0.1337 (3)0.2177 (4)0.064 (1)0.299 (4)
N220.7165 (5)0.1594 (3)0.2816 (3)0.052 (1)0.299 (4)
C230.7829 (6)0.1274 (3)0.3565 (4)0.073 (2)0.299 (4)
C240.7304 (6)0.0513 (3)0.3754 (4)0.080 (2)0.299 (4)
C24a0.8288 (7)0.0155 (6)0.4412 (6)0.130 (1)0.299 (4)
C250.5963 (6)0.0579 (4)0.3998 (4)0.079 (1)0.299 (4)
N260.4824 (6)0.0767 (3)0.3374 (4)0.061 (1)0.299 (4)
C270.3586 (6)0.0842 (3)0.3725 (4)0.074 (2)0.299 (4)
C310.6010 (6)0.0966 (3)0.1100 (4)0.074 (2)0.299 (4)
N320.5213 (6)0.0712 (2)0.1686 (4)0.061 (1)0.299 (4)
C330.3995 (6)0.0299 (3)0.1318 (4)0.079 (1)0.299 (4)
C340.2796 (6)0.0797 (3)0.1087 (4)0.080 (2)0.299 (4)
C34a0.1756 (7)0.0355 (5)0.0526 (6)0.130 (1)0.299 (4)
C350.2153 (6)0.1057 (4)0.1750 (4)0.073 (2)0.299 (4)
N360.2907 (5)0.1647 (3)0.2254 (4)0.052 (1)0.299 (4)
C370.2187 (6)0.1813 (3)0.2910 (4)0.064 (1)0.299 (4)
ClA0.9027 (9)0.3535 (3)0.3664 (3)0.144 (4)0.299 (4)
O1A0.891 (2)0.2826 (7)0.3321 (13)0.273 (7)0.299 (4)
O2A0.818 (2)0.3581 (14)0.4202 (11)0.417 (16)0.299 (4)
O3A1.0331 (12)0.3647 (12)0.4026 (12)0.240 (7)0.299 (4)
O4A0.869 (2)0.4088 (10)0.3105 (10)0.238 (6)0.299 (4)
ClB0.0678 (6)0.3433 (3)0.1148 (6)0.251 (15)0.299 (4)
O1B0.1135 (13)0.3019 (8)0.1809 (8)0.176 (10)0.299 (4)
O2B0.068 (2)0.2978 (8)0.0506 (8)0.53 (2)0.299 (4)
O3B0.0608 (8)0.3683 (8)0.1166 (12)0.72 (5)0.299 (4)
O4B0.1505 (10)0.4051 (5)0.1111 (10)0.190 (14)0.299 (4)
Ni"0.4986 (3)0.1585 (1)0.2589 (2)0.047 (1)0.306 (4)
C1"0.8069 (7)0.1511 (5)0.0913 (4)0.091 (2)0.306 (4)
C2"0.7052 (5)0.1536 (3)0.1464 (3)0.063 (1)0.306 (4)
C3"0.2940 (5)0.1636 (3)0.3777 (3)0.063 (1)0.306 (4)
C4"0.1968 (7)0.1658 (5)0.4355 (4)0.091 (2)0.306 (4)
C11"0.6480 (6)0.2334 (3)0.1445 (4)0.067 (1)0.306 (4)
N12"0.5162 (6)0.2379 (3)0.1695 (3)0.059 (1)0.306 (4)
C13"0.4730 (7)0.3178 (3)0.1761 (4)0.079 (2)0.306 (4)
C14"0.5202 (8)0.3527 (2)0.2537 (5)0.082 (2)0.306 (4)
C14a"0.499 (3)0.4387 (3)0.2468 (8)0.141 (2)0.306 (4)
C15"0.4477 (8)0.3237 (3)0.3155 (5)0.079 (2)0.306 (4)
N16"0.4815 (6)0.2446 (2)0.3421 (3)0.059 (1)0.306 (4)
C17"0.3996 (6)0.2238 (4)0.4021 (3)0.067 (1)0.306 (4)
C21"0.7787 (5)0.1339 (3)0.2264 (3)0.064 (1)0.306 (4)
N22"0.7113 (4)0.1599 (3)0.2901 (3)0.052 (1)0.306 (4)
C23"0.7778 (6)0.1286 (4)0.3653 (3)0.073 (2)0.306 (4)
C24"0.7259 (6)0.0525 (4)0.3847 (4)0.080 (2)0.306 (4)
C24a"0.8245 (8)0.0174 (7)0.4509 (6)0.130 (1)0.306 (4)
C25"0.5917 (6)0.0589 (4)0.4090 (4)0.079 (1)0.306 (4)
N26"0.4777 (6)0.0770 (3)0.3463 (3)0.061 (1)0.306 (4)
C27"0.3538 (6)0.0845 (4)0.3812 (4)0.074 (2)0.306 (4)
C31"0.5969 (6)0.0957 (4)0.1190 (4)0.074 (2)0.306 (4)
N32"0.5172 (6)0.0705 (3)0.1776 (3)0.061 (1)0.306 (4)
C33"0.3959 (6)0.0287 (3)0.1410 (4)0.079 (1)0.306 (4)
C34"0.2755 (6)0.0780 (4)0.1175 (4)0.080 (2)0.306 (4)
C34a"0.1721 (8)0.0331 (7)0.0616 (6)0.130 (1)0.306 (4)
C35"0.2108 (6)0.1042 (4)0.1835 (4)0.073 (2)0.306 (4)
N36"0.2855 (4)0.1638 (3)0.2335 (3)0.052 (1)0.306 (4)
C37"0.2131 (5)0.1807 (4)0.2989 (3)0.064 (1)0.306 (4)
ClC0.0909 (8)0.3542 (3)0.1323 (3)0.144 (5)0.306 (4)
O1C0.104 (2)0.2845 (6)0.1690 (11)0.268 (4)0.306 (4)
O2C0.1819 (18)0.3596 (12)0.0821 (10)0.407 (18)0.306 (4)
O3C0.0373 (11)0.3613 (11)0.0912 (11)0.250 (7)0.306 (4)
O4C0.115 (2)0.4115 (9)0.1867 (9)0.243 (7)0.306 (4)
ClD0.8649 (6)0.3201 (3)0.4266 (2)0.129 (6)0.306 (4)
O1D0.8875 (11)0.2915 (6)0.3566 (4)0.137 (5)0.306 (4)
O2D0.9043 (11)0.3953 (3)0.4332 (6)0.135 (5)0.306 (4)
O3D0.7302 (7)0.3149 (7)0.4305 (7)0.208 (9)0.306 (4)
O4D0.9375 (12)0.2786 (5)0.4862 (5)0.236 (15)0.306 (4)
Ow0.6538 (15)0.0784 (7)0.2480 (8)0.145 (4)0.306 (4)
H1C10.85000.09960.08240.0910.299
H2C10.76610.16500.02930.0910.299
H3C10.88450.18890.09990.0910.299
H1C40.13120.12680.41300.0910.299
H2C40.25210.15430.48040.0910.299
H3C40.16130.21700.42720.0910.299
H1C110.71780.26640.17160.0670.299
H2C110.64380.25390.08280.0670.299
H1C130.37980.32040.15870.0790.299
H2C130.51530.34960.12950.0790.299
H1C140.62450.34220.26230.0820.299
H1C14a0.55450.45950.19990.1410.299
H2C14a0.40950.45040.22690.1410.299
H3C14a0.54320.46310.29120.1410.299
H1C150.36240.31460.28000.0790.299
H2C150.44980.34670.35980.0790.299
H1C170.36050.27010.40890.0670.299
H2C170.46740.20370.44050.0670.299
H1C210.79250.07730.22080.0640.299
H2C210.87400.15730.22450.0640.299
H1C230.77010.16360.39830.0730.299
H2C230.88020.12210.35480.0730.299
H1C240.72240.01800.32890.0800.299
H1C24a0.91840.01090.42540.1300.299
H2C24a0.83600.04820.48810.1300.299
H3C24a0.79620.03590.45300.1300.299
H1C250.60150.10700.42850.0790.299
H2C250.55090.01920.42770.0790.299
H1C270.38060.06850.42770.0740.299
H2C270.28960.04930.34440.0740.299
H1C310.53850.11990.06630.0740.299
H2C310.64400.05100.09120.0740.299
H1C330.37730.00890.16900.0790.299
H2C330.41970.00400.08450.0790.299
H1C340.30710.12530.08150.0800.299
H1C34a0.21640.01770.00790.1300.299
H2C34a0.14450.00920.07960.1300.299
H3C34a0.09800.06920.03350.1300.299
H1C350.23160.06160.21110.0730.299
H2C350.12300.12550.17440.0730.299
H1C370.13530.15030.28410.0640.299
H2C370.19510.23640.28950.0640.299
H1N120.45840.21920.11640.0590.299
H1N220.73900.21460.28630.0520.299
H1N320.57770.03150.19890.0610.299
H1N160.58040.24840.36420.0590.299
H1N260.46740.02830.30760.0610.299
H1N360.27460.21150.19320.0520.299
H1C1"0.84590.09900.09160.0910.306
H2C1"0.76160.16390.03790.0910.306
H3C1"0.87960.18860.10840.0910.306
H1C4"0.12570.12680.42110.0910.306
H2C4"0.24620.15500.48840.0910.306
H3C4"0.15500.21720.43470.0910.306
H1C11"0.71190.26620.17930.0670.306
H2C11"0.63830.25290.09050.0670.306
H1C13"0.37330.31930.16560.0790.306
H2C13"0.50860.34860.13640.0790.306
H1C14"0.61760.34230.26930.0820.306
H1C14a"0.54660.45900.20590.1410.306
H2C14a"0.40150.44980.23280.1410.306
H3C14a"0.53500.46330.29720.1410.306
H1C15"0.35560.31420.28690.0790.306
H2C15"0.44240.34710.36660.0790.306
H1C17"0.35370.27060.41610.0670.306
H2C17"0.46120.20460.44840.0670.306
H1C21"0.78820.07760.23000.0640.306
H2C21"0.86900.15780.23320.0640.306
H1C23"0.76460.16510.40680.0730.306
H2C23"0.87510.12350.36380.0730.306
H1C24"0.71840.01880.33850.0800.306
H1C24a"0.91420.01290.43520.1300.306
H2C24a"0.83120.05050.49750.1300.306
H3C24a"0.79240.03400.46300.1300.306
H1C25"0.59630.10820.43730.0790.306
H2C25"0.54650.02030.43710.0790.306
H1C27"0.37580.06920.43660.0740.306
H2C27"0.28520.04920.35330.0740.306
H1C31"0.53430.11850.07510.0740.306
H2C31"0.64040.05000.10060.0740.306
H1C33"0.37390.00990.17850.0790.306
H2C33"0.41640.00250.09400.0790.306
H1C34"0.30260.12350.09000.0800.306
H1C34a"0.21330.01510.01710.1300.306
H2C34a"0.14130.01150.08900.1300.306
H3C34a"0.09420.06650.04220.1300.306
H1C35"0.22740.06050.21990.0730.306
H2C35"0.11830.12380.18260.0730.306
H1C37"0.13000.14940.29220.0640.306
H2C37"0.18900.23560.29690.0640.306
H1N12"0.45310.21800.12420.0590.306
H1N22"0.73320.21520.29440.0520.306
H1N32"0.57390.03120.20830.0610.306
H1N16"0.57400.24910.37180.0590.306
H1N26"0.46330.02840.31690.0610.306
H1N36"0.26910.21030.20090.0520.306
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0440.0380.058 (1)0.002 (1)0.0050.001 (1)
C10.076 (2)0.122 (4)0.082 (3)0.006 (3)0.037 (2)0.015 (4)
C20.056 (2)0.073 (2)0.065 (2)0.001 (2)0.020 (1)0.004 (2)
C30.056 (2)0.073 (2)0.065 (2)0.001 (2)0.020 (1)0.004 (2)
C40.076 (2)0.122 (4)0.082 (3)0.006 (3)0.037 (2)0.015 (4)
C110.064 (3)0.082 (3)0.057 (3)0.003 (2)0.015 (2)0.017 (2)
N120.056 (1)0.058 (1)0.065 (1)0.002 (1)0.011 (1)0.011 (1)
C130.084 (4)0.053 (2)0.103 (3)0.001 (3)0.026 (3)0.018 (2)
C140.071 (5)0.044 (2)0.138 (4)0.0000.040 (4)0.000
C14a0.154 (5)0.046 (3)0.245 (6)0.0000.098 (6)0.000
C150.084 (4)0.053 (2)0.103 (3)0.001 (3)0.026 (3)0.018 (2)
N160.056 (1)0.058 (1)0.065 (1)0.002 (1)0.011 (1)0.011 (1)
C170.064 (3)0.082 (3)0.057 (3)0.003 (2)0.015 (2)0.017 (2)
C210.050 (2)0.070 (3)0.076 (3)0.002 (2)0.020 (2)0.001 (2)
N220.046 (1)0.053 (1)0.054 (2)0.003 (1)0.002 (1)0.003 (1)
C230.057 (2)0.095 (3)0.062 (3)0.000 (2)0.004 (2)0.020 (2)
C240.065 (2)0.090 (4)0.083 (2)0.022 (2)0.008 (2)0.033 (2)
C24a0.086 (3)0.174 (4)0.126 (3)0.037 (3)0.006 (2)0.087 (3)
C250.073 (2)0.062 (3)0.104 (4)0.019 (2)0.019 (2)0.031 (2)
N260.055 (1)0.049 (1)0.081 (2)0.005 (1)0.013 (1)0.012 (1)
C270.071 (3)0.081 (3)0.073 (2)0.009 (2)0.026 (2)0.023 (2)
C310.071 (3)0.081 (3)0.073 (2)0.009 (2)0.026 (2)0.023 (2)
N320.055 (1)0.049 (1)0.081 (2)0.005 (1)0.013 (1)0.012 (1)
C330.073 (2)0.062 (3)0.104 (4)0.019 (2)0.019 (2)0.031 (2)
C340.065 (2)0.090 (4)0.083 (2)0.022 (2)0.008 (2)0.033 (2)
C34a0.086 (3)0.174 (4)0.126 (3)0.037 (3)0.006 (2)0.087 (3)
C350.057 (2)0.095 (3)0.062 (3)0.000 (2)0.004 (2)0.020 (2)
N360.046 (1)0.053 (1)0.054 (2)0.003 (1)0.002 (1)0.003 (1)
C370.050 (2)0.070 (3)0.076 (3)0.002 (2)0.020 (2)0.001 (2)
ClA0.222 (4)0.074 (4)0.104 (7)0.020 (2)0.067 (2)0.004 (4)
O1A0.337 (11)0.077 (8)0.331 (12)0.024 (3)0.160 (8)0.059 (6)
O2A0.436 (14)0.57 (3)0.264 (15)0.129 (15)0.115 (14)0.069 (13)
O3A0.285 (6)0.124 (7)0.238 (11)0.061 (5)0.169 (6)0.021 (7)
O4A0.238 (9)0.127 (5)0.293 (12)0.042 (4)0.112 (6)0.111 (7)
ClB0.091 (8)0.169 (14)0.46 (2)0.035 (5)0.037 (10)0.193 (17)
O1B0.101 (9)0.127 (14)0.308 (17)0.012 (6)0.058 (9)0.086 (14)
O2B0.74 (4)0.42 (3)0.33 (3)0.41 (3)0.23 (2)0.08 (2)
O3B0.087 (7)0.52 (4)1.56 (8)0.084 (9)0.139 (13)0.76 (5)
O4B0.087 (9)0.074 (12)0.41 (3)0.017 (5)0.031 (9)0.095 (16)
Ni"0.0440.0380.058 (1)0.002 (1)0.0050.001 (1)
C1"0.076 (2)0.122 (4)0.082 (3)0.006 (3)0.037 (2)0.015 (4)
C2"0.056 (2)0.073 (2)0.065 (2)0.001 (2)0.020 (1)0.004 (2)
C3"0.056 (2)0.073 (2)0.065 (2)0.001 (2)0.020 (1)0.004 (2)
C4"0.076 (2)0.122 (4)0.082 (3)0.006 (3)0.037 (2)0.015 (4)
C11"0.064 (3)0.082 (3)0.057 (3)0.003 (2)0.015 (2)0.017 (2)
N12"0.056 (1)0.058 (1)0.065 (1)0.002 (1)0.011 (1)0.011 (1)
C13"0.084 (4)0.053 (2)0.103 (3)0.001 (3)0.026 (3)0.018 (2)
C14"0.071 (5)0.044 (2)0.138 (4)0.0000.040 (4)0.000
C14a"0.154 (5)0.046 (3)0.245 (6)0.0000.098 (6)0.000
C15"0.084 (4)0.053 (2)0.103 (3)0.001 (3)0.026 (3)0.018 (2)
N16"0.056 (1)0.058 (1)0.065 (1)0.002 (1)0.011 (1)0.011 (1)
C17"0.064 (3)0.082 (3)0.057 (3)0.003 (2)0.015 (2)0.017 (2)
C21"0.050 (2)0.070 (3)0.076 (3)0.002 (2)0.020 (2)0.001 (2)
N22"0.046 (1)0.053 (1)0.054 (2)0.003 (1)0.002 (1)0.003 (1)
C23"0.057 (2)0.095 (3)0.062 (3)0.000 (2)0.004 (2)0.020 (2)
C24"0.065 (2)0.090 (4)0.083 (2)0.022 (2)0.008 (2)0.033 (2)
C24a"0.086 (3)0.174 (4)0.126 (3)0.037 (3)0.006 (2)0.087 (3)
C25"0.073 (2)0.062 (3)0.104 (4)0.019 (2)0.019 (2)0.031 (2)
N26"0.055 (1)0.049 (1)0.081 (2)0.005 (1)0.013 (1)0.012 (1)
C27"0.071 (3)0.081 (3)0.073 (2)0.009 (2)0.026 (2)0.023 (2)
C31"0.071 (3)0.081 (3)0.073 (2)0.009 (2)0.026 (2)0.023 (2)
N32"0.055 (1)0.049 (1)0.081 (2)0.005 (1)0.013 (1)0.012 (1)
C33"0.073 (2)0.062 (3)0.104 (4)0.019 (2)0.019 (2)0.031 (2)
C34"0.065 (2)0.090 (4)0.083 (2)0.022 (2)0.008 (2)0.033 (2)
C34a"0.086 (3)0.174 (4)0.126 (3)0.037 (3)0.006 (2)0.087 (3)
C35"0.057 (2)0.095 (3)0.062 (3)0.000 (2)0.004 (2)0.020 (2)
N36"0.046 (1)0.053 (1)0.054 (2)0.003 (1)0.002 (1)0.003 (1)
C37"0.050 (2)0.070 (3)0.076 (3)0.002 (2)0.020 (2)0.001 (2)
ClC0.223 (5)0.073 (6)0.102 (7)0.020 (2)0.069 (2)0.006 (4)
O1C0.337 (11)0.080 (4)0.314 (12)0.019 (4)0.152 (8)0.066 (5)
O2C0.428 (14)0.55 (3)0.262 (16)0.126 (14)0.109 (13)0.061 (13)
O3C0.298 (6)0.140 (9)0.236 (12)0.062 (6)0.178 (7)0.021 (8)
O4C0.239 (10)0.128 (8)0.307 (12)0.045 (4)0.112 (6)0.117 (7)
ClD0.179 (10)0.102 (5)0.088 (7)0.015 (3)0.033 (3)0.007 (6)
O1D0.175 (10)0.115 (5)0.103 (9)0.020 (4)0.024 (4)0.023 (6)
O2D0.168 (11)0.103 (4)0.115 (9)0.013 (4)0.033 (5)0.019 (5)
O3D0.211 (11)0.183 (15)0.235 (17)0.072 (7)0.049 (8)0.112 (12)
O4D0.40 (2)0.134 (9)0.118 (7)0.006 (12)0.106 (10)0.008 (9)
Ow0.166 (10)0.091 (8)0.161 (10)0.032 (7)0.025 (9)0.003 (7)
H1C10.0760.1220.0820.0060.0370.015
H2C10.0760.1220.0820.0060.0370.015
H3C10.0760.1220.0820.0060.0370.015
H1C40.0760.1220.0820.0060.0370.015
H2C40.0760.1220.0820.0060.0370.015
H3C40.0760.1220.0820.0060.0370.015
H1C110.0640.0820.0570.0030.0150.017
H2C110.0640.0820.0570.0030.0150.017
H1C130.0840.0530.1030.0010.0260.018
H2C130.0840.0530.1030.0010.0260.018
H1C140.0710.0440.1380.0000.0400.000
H1C14a0.1540.0460.2450.0000.0980.000
H2C14a0.1540.0460.2450.0000.0980.000
H3C14a0.1540.0460.2450.0000.0980.000
H1C150.0840.0530.1030.0010.0260.018
H2C150.0840.0530.1030.0010.0260.018
H1C170.0640.0820.0570.0030.0150.017
H2C170.0640.0820.0570.0030.0150.017
H1C210.0500.0700.0760.0020.0200.001
H2C210.0500.0700.0760.0020.0200.001
H1C230.0570.0950.0620.0000.0040.020
H2C230.0570.0950.0620.0000.0040.020
H1C240.0650.0900.0830.0220.0080.033
H1C24a0.0860.1740.1260.0370.0060.087
H2C24a0.0860.1740.1260.0370.0060.087
H3C24a0.0860.1740.1260.0370.0060.087
H1C250.0730.0620.1040.0190.0190.031
H2C250.0730.0620.1040.0190.0190.031
H1C270.0710.0810.0730.0090.0260.023
H2C270.0710.0810.0730.0090.0260.023
H1C310.0710.0810.0730.0090.0260.023
H2C310.0710.0810.0730.0090.0260.023
H1C330.0730.0620.1040.0190.0190.031
H2C330.0730.0620.1040.0190.0190.031
H1C340.0650.0900.0830.0220.0080.033
H1C34a0.0860.1740.1260.0370.0060.087
H2C34a0.0860.1740.1260.0370.0060.087
H3C34a0.0860.1740.1260.0370.0060.087
H1C350.0570.0950.0620.0000.0040.020
H2C350.0570.0950.0620.0000.0040.020
H1C370.0500.0700.0760.0020.0200.001
H2C370.0500.0700.0760.0020.0200.001
H1N120.0560.0580.0650.0020.0110.011
H1N220.0460.0530.0540.0030.0020.003
H1N320.0550.0490.0810.0050.0130.012
H1N160.0560.0580.0650.0020.0110.011
H1N260.0550.0490.0810.0050.0130.012
H1N360.0460.0530.0540.0030.0020.003
H1C1"0.0760.1220.0820.0060.0370.015
H2C1"0.0760.1220.0820.0060.0370.015
H3C1"0.0760.1220.0820.0060.0370.015
H1C4"0.0760.1220.0820.0060.0370.015
H2C4"0.0760.1220.0820.0060.0370.015
H3C4"0.0760.1220.0820.0060.0370.015
H1C11"0.0640.0820.0570.0030.0150.017
H2C11"0.0640.0820.0570.0030.0150.017
H1C13"0.0840.0530.1030.0010.0260.018
H2C13"0.0840.0530.1030.0010.0260.018
H1C14"0.0710.0440.1380.0000.0400.000
H1C14a"0.1540.0460.2450.0000.0980.000
H2C14a"0.1540.0460.2450.0000.0980.000
H3C14a"0.1540.0460.2450.0000.0980.000
H1C15"0.0840.0530.1030.0010.0260.018
H2C15"0.0840.0530.1030.0010.0260.018
H1C17"0.0640.0820.0570.0030.0150.017
H2C17"0.0640.0820.0570.0030.0150.017
H1C21"0.0500.0700.0760.0020.0200.001
H2C21"0.0500.0700.0760.0020.0200.001
H1C23"0.0570.0950.0620.0000.0040.020
H2C23"0.0570.0950.0620.0000.0040.020
H1C24"0.0650.0900.0830.0220.0080.033
H1C24a"0.0860.1740.1260.0370.0060.087
H2C24a"0.0860.1740.1260.0370.0060.087
H3C24a"0.0860.1740.1260.0370.0060.087
H1C25"0.0730.0620.1040.0190.0190.031
H2C25"0.0730.0620.1040.0190.0190.031
H1C27"0.0710.0810.0730.0090.0260.023
H2C27"0.0710.0810.0730.0090.0260.023
H1C31"0.0710.0810.0730.0090.0260.023
H2C31"0.0710.0810.0730.0090.0260.023
H1C33"0.0730.0620.1040.0190.0190.031
H2C33"0.0730.0620.1040.0190.0190.031
H1C34"0.0650.0900.0830.0220.0080.033
H1C34a"0.0860.1740.1260.0370.0060.087
H2C34a"0.0860.1740.1260.0370.0060.087
H3C34a"0.0860.1740.1260.0370.0060.087
H1C35"0.0570.0950.0620.0000.0040.020
H2C35"0.0570.0950.0620.0000.0040.020
H1C37"0.0500.0700.0760.0020.0200.001
H2C37"0.0500.0700.0760.0020.0200.001
H1N12"0.0560.0580.0650.0020.0110.011
H1N22"0.0460.0530.0540.0030.0020.003
H1N32"0.0550.0490.0810.0050.0130.012
H1N16"0.0560.0580.0650.0020.0110.011
H1N26"0.0550.0490.0810.0050.0130.012
H1N36"0.0460.0530.0540.0030.0020.003
Geometric parameters (Å, º) top
Ni—N122.136 (2)C24—C251.503 (3)
Ni—N162.137 (2)C25—N261.494 (4)
Ni—N222.142 (2)C3—C271.520 (3)
Ni—N262.143 (2)N26—C271.499 (4)
Ni—N322.143 (2)C2—C311.521 (3)
Ni—N362.141 (2)C31—N321.484 (4)
C1—C21.535 (5)N32—C331.488 (4)
C3—C41.535 (5)C33—C341.503 (3)
C2—C111.522 (3)C34—C34a1.534 (4)
C11—N121.483 (4)C34—C351.503 (3)
N12—C131.488 (4)C35—N361.494 (4)
C13—C141.503 (3)C3—C371.520 (3)
C14—C14a1.534 (4)N36—C371.497 (4)
C14—C151.503 (3)ClA—O1A1.386 (3)
C15—N161.493 (4)N22—O1A2.853 (15)
C3—C171.521 (3)N36—O1B3.042 (13)
N16—C171.498 (4)N36"—O1C2.919 (14)
C2—C211.520 (3)N22"—O1D3.044 (11)
C21—N221.482 (4)N16"—O3D3.007 (10)
N22—C231.488 (4)N32"—Ow3.129 (13)
C23—C241.503 (3)O4Ci—Ow3.14 (3)
C24—C24a1.534 (4)O1Dii—Ow2.929 (17)
N12—Ni—N1693.7 (1)Ni—N26—C27115.3 (3)
N12—Ni—N2288.6 (2)C25—N26—C27108.6 (3)
N12—Ni—N26178.4 (2)C3—C27—N26115.0 (4)
N12—Ni—N3287.4 (2)C2—C31—N32115.6 (4)
N12—Ni—N3691.5 (2)Ni—N32—C31111.5 (3)
N16—Ni—N2290.7 (2)Ni—N32—C33119.2 (3)
N16—Ni—N2687.5 (2)C31—N32—C33111.0 (3)
N16—Ni—N32178.7 (2)N32—C33—C34114.2 (3)
N16—Ni—N3685.2 (2)C33—C34—C34a108.5 (3)
N22—Ni—N2692.4 (1)C33—C34—C35114.1 (5)
N22—Ni—N3288.9 (2)C34a—C34—C35108.2 (3)
N22—Ni—N36175.9 (1)C34—C35—N36115.3 (3)
N26—Ni—N3291.3 (1)Ni—N36—C35119.3 (3)
N26—Ni—N3687.7 (2)Ni—N36—C37117.4 (3)
N32—Ni—N3695.3 (1)C35—N36—C37109.0 (3)
C1—C2—C11108.1 (3)C3—C37—N36113.7 (4)
C1—C2—C21107.5 (3)N22—O1A—ClA145.7 (13)
C1—C2—C31108.0 (3)C21—N22—O1A97.4 (5)
C11—C2—C21111.0 (3)C23—N22—O1A81.2 (5)
C11—C2—C31111.1 (3)Ni—N22—O1A129.3 (4)
C21—C2—C31110.9 (3)N36—O1B—ClB137.4 (9)
C4—C3—C17107.4 (3)C35—N36—O1B100.3 (4)
C4—C3—C27107.2 (3)C37—N36—O1B72.4 (4)
C4—C3—C37106.9 (3)Ni—N36—O1B128.9 (3)
C17—C3—C27111.8 (3)N36"—O1C—ClC146.7 (12)
C17—C3—C37111.6 (3)C35"—N36—O1C93.4 (5)
C27—C3—C37111.7 (3)C37"—N36—O1C78.1 (5)
C2—C11—N12113.9 (4)Ni"—N36"—O1C131.6 (4)
Ni—N12—C11112.1 (3)N22"—O1D—ClD116.4 (5)
Ni—N12—C13120.1 (3)C21"—N22"—O1D102.1 (3)
C11—N12—C13111.5 (3)C23"—N22"—O1D78.0 (3)
N12—C13—C14113.9 (3)Ni"—N22"—O1D127.7 (3)
C13—C14—C14a108.3 (4)N16"—O3D—ClD139.0 (5)
C13—C14—C15113.4 (4)C15"—N16"—O3D84.6 (4)
C14a—C14—C15108.4 (4)C17"—N16"—O3D104.8 (3)
C14—C15—N16115.5 (3)Ni"—N16"—O3D119.3 (3)
Ni—N16—C15119.4 (3)C31"—N32"—Ow105.6 (4)
Ni—N16—C17115.4 (3)C33"—N32"—Ow92.1 (4)
C15—N16—C17108.9 (3)Ni"—N32"—Ow115.3 (3)
C3—C17—N16115.0 (4)N32"—Ow—O4Ci80.6 (4)
C2—C21—N22114.4 (4)N32"—Ow—O1Dii113.7 (4)
Ni—N22—C21112.3 (3)O4Ci—Ow—O1Dii98.3 (6)
Ni—N22—C23120.8 (3)Ow—O1Dii—ClDii104.3 (6)
C21—N22—C23111.0 (3)Ow—O4Ci—ClCi103.5 (9)
N22—C23—C24114.2 (3)N12—Ni—C253.3 (1)
C23—C24—C24a108.9 (3)N22—Ni—C253.4 (1)
C23—C24—C25111.6 (5)N32—Ni—C253.9 (1)
C24a—C24—C25108.9 (3)N16—Ni—C352.7 (1)
C24—C25—N26115.9 (3)N26—Ni—C352.7 (1)
Ni—N26—C25121.0 (3)N36—Ni—C352.1 (1)
N12—C2—C3—N1662.1 (2)N12—C11—C2—C3139.4 (5)
N22—C2—C3—N2662.7 (2)N22—C21—C2—C1159.0 (4)
N32—C2—C3—N3662.4 (2)N22—C21—C2—C1141.0 (5)
C11—N12—Ni—N16115.6 (3)N22—C21—C2—C3183.1 (4)
C13—N12—Ni—N1618.4 (4)N32—C31—C2—C1159.5 (4)
C11—N12—Ni—N2225.0 (3)N32—C31—C2—C1182.1 (4)
C13—N12—Ni—N22109.0 (4)N32—C31—C2—C2141.9 (5)
C11—N12—Ni—N3263.9 (3)N16—C17—C3—C4195.6 (3)
C13—N12—Ni—N32162.1 (4)N16—C17—C3—C2778.3 (4)
C11—N12—Ni—N36159.2 (3)N16—C17—C3—C3747.6 (5)
C13—N12—Ni—N3666.9 (4)N26—C27—C3—C4196.5 (4)
C15—N16—Ni—N1216.9 (4)N26—C27—C3—C1746.1 (5)
C17—N16—Ni—N12149.6 (3)N26—C27—C3—C3779.7 (4)
C15—N16—Ni—N22105.5 (4)N36—C37—C3—C4193.0 (3)
C17—N16—Ni—N22121.8 (3)N36—C37—C3—C1775.9 (4)
C15—N16—Ni—N26197.9 (4)N36—C37—C3—C2750.1 (5)
C17—N16—Ni—N2629.4 (3)Ni—N12—C11—C234.8 (4)
C15—N16—Ni—N3674.2 (4)C13—N12—C11—C2172.8 (3)
C17—N16—Ni—N3658.5 (3)C14—C13—N12—Ni45.8 (5)
C21—N22—Ni—N1260.8 (3)C14—C13—N12—C1188.5 (5)
C23—N22—Ni—N12194.8 (4)C14a—C14—C13—N12166.4 (8)
C21—N22—Ni—N16154.5 (3)C15—C14—C13—N1273.2 (5)
C23—N22—Ni—N1671.4 (4)N16—C15—C14—C1372.6 (7)
C21—N22—Ni—N26118.0 (3)N16—C15—C14—C14a167.1 (9)
C23—N22—Ni—N2616.1 (4)Ni—N16—C15—C1443.5 (7)
C21—N22—Ni—N3226.7 (3)C17—N16—C15—C14178.9 (5)
C23—N22—Ni—N32107.4 (4)C3—C17—N16—Ni26.0 (4)
C25—N26—Ni—N1677.3 (4)C3—C17—N16—C15111.4 (4)
C27—N26—Ni—N1656.7 (3)Ni—N22—C21—C232.7 (4)
C25—N26—Ni—N2213.3 (4)C23—N22—C21—C2171.3 (3)
C27—N26—Ni—N22147.3 (3)C24—C23—N22—Ni46.4 (5)
C25—N26—Ni—N32102.2 (4)C24—C23—N22—C2188.2 (5)
C27—N26—Ni—N32123.8 (3)C24a—C24—C23—N22165.1 (5)
C25—N26—Ni—N36197.4 (4)C25—C24—C23—N2274.6 (5)
C27—N26—Ni—N3628.6 (3)N26—C25—C24—C2371.8 (6)
C31—N32—Ni—N1228.6 (3)N26—C25—C24—C24a192.1 (6)
C33—N32—Ni—N12102.9 (4)Ni—N26—C25—C2440.9 (6)
C31—N32—Ni—N2260.0 (3)C27—N26—C25—C24177.6 (5)
C33—N32—Ni—N22191.5 (4)C3—C27—N26—Ni25.6 (5)
C31—N32—Ni—N26152.4 (3)C3—C27—N26—C25113.8 (4)
C33—N32—Ni—N2676.2 (4)Ni—N32—C31—C231.2 (5)
C31—N32—Ni—N36119.8 (3)C33—N32—C31—C2166.7 (3)
C33—N32—Ni—N3611.6 (4)C34—C33—N32—Ni41.5 (6)
C35—N36—Ni—N1297.4 (4)C34—C33—N32—C3190.2 (5)
C37—N36—Ni—N12127.3 (3)C34a—C34—C33—N32164.3 (6)
C35—N36—Ni—N16191.0 (4)C35—C34—C33—N3275.0 (5)
C37—N36—Ni—N1633.6 (3)N36—C35—C34—C3373.1 (6)
C35—N36—Ni—N2681.3 (4)N36—C35—C34—C34a166.0 (6)
C37—N36—Ni—N2654.0 (3)Ni—N36—C35—C3438.0 (6)
C35—N36—Ni—N329.8 (4)C37—N36—C35—C34176.7 (4)
C37—N36—Ni—N32145.2 (3)C3—C37—N36—Ni21.2 (4)
N12—C11—C2—C1202.2 (4)C3—C37—N36—C35118.4 (4)
N12—C11—C2—C2184.6 (4)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+3/2, y1/2, z+1/2.
 
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