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Acta Crystallogr Sect E Struct Rep Online. 2009 July 1; 65(Pt 7): m728.
Published online 2009 June 6. doi:  10.1107/S1600536809020662
PMCID: PMC2969409

Bis(5,5,7,12,12,14-hexa­methyl-1,4,8,11-tetra­azacyclo­tetra­decane-κ4 N)(μ-l-mal­ato-κ4 O 1,O 2:O 4,O 4′)dinickel(II) bis(perchlorate) monohydrate

Abstract

In the crystal structure of the title dinuclear compound, [Ni2(C4H4O5)(C16H36N4)2](ClO4)2·H2O, the bridg­ing di­car­box­yl­ate dianion O,O′-chelates to two Ni atoms, both of which are also chelated by the N-macrocylic ligand. The Ni atoms exhibit a distorted octa­hedral coordination. N—H(...)O and O—H(...)O hydrogen bonds link the cations and the uncoordinated water mol­ecules into a layer structure; the perchlorate anions occupy the space between adjacent layers, and are only weakly linked to the layers. One of the perchlorate anions is disordered over two sets of sites in a 3:2 ratio.

Related literature

For the nickel phthalate perchlorate hydrate derivative of the macrocycle, see: Ou & Zhang (2009 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-0m728-scheme1.jpg

Experimental

Crystal data

  • [Ni2(C4H4O5)(C16H36N4)2](ClO4)2·H2O
  • M r = 1035.38
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m728-efi1.jpg
  • a = 13.562 (2) Å
  • b = 18.984 (2) Å
  • c = 19.350 (3) Å
  • V = 4982 (1) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.93 mm−1
  • T = 293 K
  • 0.48 × 0.45 × 0.34 mm

Data collection

  • Bruker SMART area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.605, T max = 0.730
  • 42585 measured reflections
  • 10997 independent reflections
  • 7769 reflections with I > 2σ(I)
  • R int = 0.043

Refinement

  • R[F 2 > 2σ(F 2)] = 0.043
  • wR(F 2) = 0.123
  • S = 1.03
  • 10997 reflections
  • 647 parameters
  • 79 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.41 e Å−3
  • Δρmin = −0.38 e Å−3
  • Absolute structure: Flack (1983 [triangle]), 4936 Friedel pairs
  • Flack parameter: −0.01 (2)

Data collection: SMART (Bruker, 1999 [triangle]); cell refinement: SAINT-Plus (Bruker, 1999 [triangle]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2009 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809020662/xu2535sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809020662/xu2535Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Foundation for University Key Teachers of the Education Department of Hunan Province and the Key Subject Construction Project of Hunan Province, China (No. 2006–180).

supplementary crystallographic information

Experimental

L-Malic acid (0.13 g, 1 mmol) was neutralized with sodium hydroxide (0.08 g, 2 mmol) in water (10 ml). To this solution was added (5,5,7,12,12,14 -hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel perchlorate (0.54 g, 1 mmol) dissolved in acetonitrile (10 ml). The solution was left to stand at room temperature; blue crystals formed after several weeks.

Refinement

Carbon bound H-atoms were positioned geometrically and refined using the riding model, with C—H = 0.93 to 0.98 Å and U(H) set to 1.2–1.5 Ueq(C).

H atoms attached to the N– and O-atoms were located in difference Fourier maps and were refined with a distance restraint of N–H = O–H = 0.85±0.01 Å; their temperature factors were restrained to 1.5 times Ueq(N,O).

One of the two anions is disordered over two positions. The Cl–O distance was restrained to 1.45±0.01 Å and the O···O distance to 2.37±0.02 Å. The anisotropic temperature factors of the oxygen atoms were restrained to be nearly isotropic. The disorder refined to a 3:2 ratio.

Figures

Fig. 1.
Thermal ellipsoid plot (Barbour, 2001) of [Ni2(C16H36N4)2(C4H4O5)]2+2(ClO4)-.H2O showing displacement ellipsoids of the dinculear salt hydrate at the 50% probability level. H-atoms are drawn as spheres of arbitrary radii. The disorder in the perchlorate ...

Crystal data

[Ni2(C4H4O5)(C16H36N4)2](ClO4)2·H2OF(000) = 2208
Mr = 1035.38Dx = 1.381 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 1019 reflections
a = 13.562 (2) Åθ = 2.8–22.5°
b = 18.984 (2) ŵ = 0.93 mm1
c = 19.350 (3) ÅT = 293 K
V = 4982 (1) Å3Block, blue
Z = 40.48 × 0.45 × 0.34 mm

Data collection

Bruker SMART area-detector diffractometer10997 independent reflections
Radiation source: fine-focus sealed tube7769 reflections with I > 2σ(I)
graphiteRint = 0.043
[var phi] and ω scansθmax = 27.2°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −17→17
Tmin = 0.605, Tmax = 0.730k = −24→24
42585 measured reflectionsl = −24→24

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.123w = 1/[σ2(Fo2) + (0.066P)2 + 1.0201P] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
10997 reflectionsΔρmax = 0.41 e Å3
647 parametersΔρmin = −0.38 e Å3
79 restraintsAbsolute structure: Flack (Flack, 1983), 4936 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: −0.01 (2)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Ni10.12840 (5)0.77230 (3)0.82955 (3)0.03650 (16)
Ni20.54780 (5)0.96584 (3)0.76686 (3)0.04267 (17)
Cl10.82095 (12)0.87472 (8)0.96151 (9)0.0635 (4)
Cl20.2212 (4)0.9094 (3)0.5860 (2)0.0694 (15)0.603 (15)
Cl2'0.2343 (12)0.8981 (10)0.5917 (8)0.184 (9)0.397 (15)
O10.2141 (2)0.68426 (16)0.81902 (18)0.0410 (8)
O20.3574 (3)0.63875 (18)0.7861 (2)0.0589 (11)
O30.2686 (2)0.81315 (17)0.79792 (18)0.0430 (8)
H3O0.28010.85660.79640.052*
O40.4208 (3)0.89861 (18)0.7931 (2)0.0483 (9)
O50.5716 (3)0.85639 (19)0.7953 (2)0.0520 (9)
O60.8605 (4)0.8321 (3)0.9084 (3)0.1028 (18)
O70.8598 (5)0.9427 (3)0.9528 (4)0.120 (2)
O80.8508 (5)0.8471 (4)1.0255 (3)0.121 (2)
O90.7173 (3)0.8767 (3)0.9558 (3)0.0895 (16)
O100.1180 (7)0.9240 (9)0.6026 (8)0.145 (6)0.603 (15)
O110.2768 (10)0.8832 (8)0.6437 (6)0.130 (5)0.603 (15)
O120.2533 (11)0.9786 (6)0.5709 (8)0.159 (6)0.603 (15)
O130.2280 (19)0.8633 (11)0.5287 (9)0.254 (12)0.603 (15)
O10'0.237 (3)0.9458 (18)0.6497 (14)0.29 (2)0.397 (15)
O11'0.2788 (14)0.9246 (12)0.5304 (10)0.131 (8)0.397 (15)
O12'0.281 (2)0.8324 (15)0.6114 (19)0.30 (2)0.397 (15)
O13'0.1331 (14)0.8814 (14)0.5764 (12)0.153 (9)0.397 (15)
O1W0.7584 (7)0.7864 (6)0.7920 (5)0.147 (3)
H110.701 (5)0.800 (8)0.778 (7)0.221*
H120.762 (11)0.804 (8)0.833 (3)0.221*
N10.0790 (3)0.7848 (2)0.7234 (2)0.0475 (10)
H10.132 (3)0.796 (3)0.703 (3)0.071*
N20.0713 (3)0.8748 (2)0.8429 (2)0.0434 (10)
H20.015 (2)0.872 (3)0.861 (3)0.065*
N30.1520 (3)0.7656 (2)0.9405 (2)0.0411 (10)
H30.200 (5)0.736 (3)0.948 (3)0.062*
N40.0065 (3)0.7076 (2)0.8493 (2)0.0441 (10)
H4−0.042 (3)0.735 (3)0.851 (3)0.066*
N50.4683 (3)1.0599 (2)0.7605 (2)0.0481 (11)
H50.508 (4)1.092 (2)0.748 (3)0.072*
N60.5049 (4)0.9492 (3)0.6629 (2)0.0558 (12)
H60.454 (3)0.922 (3)0.661 (4)0.084*
N70.6895 (3)0.9928 (2)0.7340 (2)0.0421 (9)
H70.690 (4)1.0362 (10)0.723 (3)0.063*
N80.5986 (3)0.9947 (2)0.8667 (2)0.0456 (10)
H80.610 (5)0.9529 (14)0.880 (3)0.068*
C10.0142 (5)0.8480 (3)0.7268 (3)0.0592 (15)
H1A−0.04990.83490.74500.071*
H1B0.00480.86700.68070.071*
C20.0603 (5)0.9028 (3)0.7724 (3)0.0547 (14)
H2A0.12440.91580.75430.066*
H2B0.01920.94460.77330.066*
C30.1289 (5)0.9216 (3)0.8894 (3)0.0486 (12)
H3a0.19790.91960.87450.058*
C40.0963 (6)0.9980 (3)0.8861 (4)0.0730 (19)
H4A0.11471.01760.84220.109*
H4B0.12761.02410.92250.109*
H4C0.02601.00060.89140.109*
C50.1246 (4)0.8945 (3)0.9628 (3)0.0496 (13)
H5A0.05600.88490.97350.059*
H5B0.14540.93250.99300.059*
C60.1849 (4)0.8283 (3)0.9827 (3)0.0475 (13)
C70.2919 (4)0.8393 (4)0.9707 (3)0.0617 (16)
H7A0.30300.85020.92290.093*
H7B0.32720.79710.98260.093*
H7C0.31490.87750.99890.093*
C80.1688 (5)0.8155 (4)1.0609 (3)0.0663 (17)
H8A0.19660.77081.07360.099*
H8B0.09950.81541.07080.099*
H8C0.20040.85221.08680.099*
C90.0614 (4)0.7314 (3)0.9669 (3)0.0479 (12)
H9A0.00980.76630.97240.057*
H9B0.07440.71041.01170.057*
C100.0286 (4)0.6755 (3)0.9168 (3)0.0476 (13)
H10A0.08020.64050.91160.057*
H10B−0.02980.65210.93450.057*
C11−0.0160 (4)0.6528 (3)0.7949 (3)0.0508 (13)
H11A0.04400.62510.78710.061*
C12−0.0966 (6)0.6027 (4)0.8186 (4)0.081 (2)
H12A−0.11080.56970.78240.121*
H12B−0.15500.62910.82940.121*
H12C−0.07480.57780.85900.121*
C13−0.0437 (4)0.6878 (3)0.7277 (3)0.0582 (14)
H13A−0.09400.72250.73800.070*
H13B−0.07450.65220.69890.070*
C140.0346 (4)0.7242 (3)0.6839 (3)0.0547 (14)
C15−0.0159 (6)0.7498 (4)0.6154 (3)0.081 (2)
H15A−0.07420.77630.62640.122*
H15B−0.03360.70980.58780.122*
H15C0.02910.77910.59010.122*
C160.1187 (5)0.6740 (3)0.6648 (3)0.0664 (16)
H16A0.14910.65650.70610.100*
H16B0.16670.69880.63770.100*
H16C0.09290.63530.63850.100*
C170.4060 (5)1.0505 (4)0.6974 (3)0.0677 (18)
H17A0.35081.01980.70790.081*
H17B0.38011.09580.68280.081*
C180.4658 (5)1.0195 (3)0.6410 (3)0.0686 (18)
H18A0.52021.05060.62990.082*
H18B0.42551.01400.60000.082*
C190.5745 (6)0.9148 (4)0.6122 (3)0.073 (2)
C200.5342 (7)0.9181 (5)0.5379 (4)0.103 (3)
H20A0.53510.96600.52190.154*
H20B0.46770.90070.53710.154*
H20C0.57460.88970.50820.154*
C210.5837 (7)0.8374 (4)0.6313 (4)0.096 (3)
H21A0.60430.83330.67860.144*
H21B0.63160.81530.60190.144*
H21C0.52100.81460.62550.144*
C220.6739 (5)0.9521 (4)0.6130 (3)0.0643 (16)
H22A0.71340.93180.57630.077*
H22B0.66231.00090.60070.077*
C230.7364 (5)0.9517 (3)0.6780 (3)0.0576 (15)
H230.74380.90290.69360.069*
C240.8386 (5)0.9808 (5)0.6604 (4)0.083 (2)
H24A0.87500.98860.70220.124*
H24B0.83171.02460.63590.124*
H24C0.87320.94760.63190.124*
C250.7485 (4)0.9935 (3)0.7985 (3)0.0495 (13)
H25A0.81091.01690.79030.059*
H25B0.76210.94550.81290.059*
C260.6935 (4)1.0309 (3)0.8540 (3)0.0519 (13)
H26A0.73231.03140.89610.062*
H26B0.68141.07920.84020.062*
C270.5318 (4)1.0307 (3)0.9167 (3)0.0549 (13)
C280.4578 (5)0.9774 (3)0.9420 (3)0.0734 (18)
H28A0.42300.95790.90320.110*
H28B0.41181.00000.97250.110*
H28C0.49140.94050.96630.110*
C290.5892 (6)1.0587 (4)0.9801 (4)0.085 (2)
H29A0.63211.09630.96590.127*
H29B0.62761.02130.99980.127*
H29C0.54341.07601.01390.127*
C300.4802 (5)1.0937 (3)0.8827 (3)0.0613 (16)
H30A0.44241.11770.91820.074*
H30B0.53081.12620.86730.074*
C310.4119 (4)1.0802 (3)0.8222 (3)0.0563 (15)
H310.36821.04100.83450.068*
C320.3483 (6)1.1456 (5)0.8105 (5)0.098 (3)
H32A0.31251.14070.76790.147*
H32B0.38981.18650.80810.147*
H32C0.30261.15070.84800.147*
C330.3003 (4)0.6883 (2)0.7964 (3)0.0396 (11)
C340.3416 (3)0.7616 (2)0.7795 (3)0.0398 (11)
H340.35250.76430.72950.048*
C350.4385 (3)0.7751 (3)0.8153 (3)0.0430 (11)
H35A0.48580.73990.80060.052*
H35B0.42930.77000.86480.052*
C360.4800 (4)0.8474 (3)0.8008 (3)0.0435 (12)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ni10.0370 (3)0.0302 (3)0.0422 (3)0.0003 (3)0.0024 (3)−0.0010 (3)
Ni20.0445 (4)0.0362 (3)0.0472 (4)−0.0054 (3)−0.0047 (3)0.0082 (3)
Cl10.0550 (9)0.0606 (9)0.0750 (10)0.0010 (7)−0.0042 (8)0.0111 (8)
Cl20.065 (3)0.087 (3)0.056 (2)−0.024 (2)−0.0080 (18)0.0161 (18)
Cl2'0.131 (11)0.207 (17)0.213 (18)−0.036 (10)−0.047 (11)0.041 (14)
O10.0395 (19)0.0307 (16)0.053 (2)0.0006 (14)0.0074 (16)−0.0038 (15)
O20.048 (2)0.0317 (18)0.097 (3)0.0023 (17)0.015 (2)−0.0147 (19)
O30.0387 (18)0.0281 (16)0.062 (2)0.0007 (14)0.0060 (16)0.0005 (15)
O40.047 (2)0.0347 (18)0.063 (2)−0.0022 (16)−0.0028 (17)0.0084 (16)
O50.044 (2)0.042 (2)0.070 (2)−0.0066 (16)0.0000 (18)0.0012 (18)
O60.071 (3)0.131 (5)0.107 (4)0.019 (3)0.005 (3)−0.024 (4)
O70.099 (4)0.085 (4)0.175 (6)−0.032 (3)−0.040 (4)0.030 (4)
O80.140 (6)0.131 (5)0.090 (4)0.010 (5)−0.022 (4)0.038 (4)
O90.054 (3)0.081 (3)0.133 (5)0.011 (2)0.011 (3)0.016 (3)
O100.139 (9)0.161 (10)0.135 (9)−0.027 (8)−0.001 (7)0.032 (8)
O110.141 (9)0.141 (9)0.107 (8)−0.011 (7)−0.045 (7)0.047 (7)
O120.152 (9)0.151 (10)0.175 (11)−0.035 (8)−0.022 (8)0.048 (9)
O130.260 (16)0.253 (16)0.249 (15)0.024 (12)−0.024 (12)−0.043 (11)
O10'0.29 (3)0.29 (3)0.30 (3)−0.018 (13)0.009 (13)−0.009 (13)
O11'0.134 (11)0.146 (12)0.114 (11)−0.023 (9)0.038 (9)0.044 (9)
O12'0.31 (3)0.30 (3)0.29 (3)0.013 (13)0.002 (13)0.007 (13)
O13'0.144 (13)0.164 (13)0.152 (13)−0.055 (11)0.002 (10)0.011 (10)
O1W0.132 (6)0.163 (8)0.147 (7)0.045 (6)0.011 (5)−0.018 (6)
N10.048 (3)0.049 (3)0.045 (3)−0.001 (2)−0.004 (2)−0.002 (2)
N20.048 (3)0.0305 (19)0.051 (3)0.0031 (18)0.000 (2)−0.0006 (18)
N30.040 (2)0.042 (2)0.041 (2)0.0061 (19)0.0043 (18)−0.0029 (18)
N40.039 (2)0.037 (2)0.056 (3)−0.0009 (18)0.005 (2)−0.0022 (19)
N50.041 (2)0.041 (2)0.062 (3)−0.0029 (18)−0.004 (2)0.013 (2)
N60.066 (3)0.058 (3)0.043 (2)−0.023 (2)−0.010 (2)0.009 (2)
N70.045 (2)0.034 (2)0.047 (2)−0.0017 (18)0.001 (2)0.005 (2)
N80.051 (3)0.038 (2)0.048 (3)0.000 (2)−0.003 (2)0.003 (2)
C10.075 (4)0.047 (3)0.056 (3)0.010 (3)−0.013 (3)0.004 (3)
C20.070 (4)0.040 (3)0.054 (3)0.013 (3)−0.004 (3)0.007 (2)
C30.058 (3)0.037 (3)0.051 (3)0.002 (3)0.002 (3)−0.007 (2)
C40.111 (6)0.040 (3)0.067 (4)0.002 (3)0.005 (4)−0.011 (3)
C50.054 (3)0.047 (3)0.048 (3)0.003 (3)0.004 (3)−0.011 (2)
C60.058 (3)0.047 (3)0.038 (3)−0.002 (3)−0.003 (2)−0.009 (2)
C70.053 (3)0.074 (4)0.059 (4)−0.008 (3)−0.002 (3)−0.011 (3)
C80.090 (5)0.063 (4)0.046 (3)0.010 (3)0.002 (3)−0.004 (3)
C90.044 (3)0.050 (3)0.049 (3)0.006 (3)0.008 (2)0.000 (2)
C100.044 (3)0.042 (3)0.057 (3)−0.002 (2)0.011 (3)0.006 (2)
C110.049 (3)0.040 (3)0.062 (3)−0.005 (2)0.001 (3)−0.009 (3)
C120.085 (5)0.071 (4)0.086 (5)−0.036 (4)0.012 (4)−0.020 (4)
C130.052 (3)0.054 (3)0.068 (4)−0.006 (3)−0.009 (3)−0.015 (3)
C140.057 (3)0.056 (3)0.051 (3)−0.004 (3)−0.008 (3)−0.011 (3)
C150.107 (6)0.076 (5)0.061 (4)−0.005 (4)−0.021 (4)−0.008 (3)
C160.077 (4)0.062 (4)0.059 (4)0.002 (3)0.006 (4)−0.019 (3)
C170.056 (4)0.077 (4)0.070 (4)0.001 (3)−0.020 (3)0.026 (4)
C180.070 (4)0.073 (4)0.063 (4)−0.011 (3)−0.019 (3)0.029 (3)
C190.105 (6)0.072 (4)0.044 (3)−0.015 (4)0.003 (4)0.000 (3)
C200.124 (7)0.134 (7)0.050 (4)−0.035 (6)−0.009 (4)−0.011 (4)
C210.143 (8)0.068 (5)0.076 (5)−0.019 (5)0.015 (5)−0.012 (4)
C220.074 (4)0.070 (4)0.049 (3)−0.005 (3)0.009 (3)0.003 (3)
C230.074 (4)0.046 (3)0.053 (3)0.014 (3)0.006 (3)0.006 (3)
C240.063 (4)0.118 (6)0.067 (4)0.017 (4)0.007 (3)0.009 (4)
C250.040 (3)0.051 (3)0.058 (3)−0.003 (2)−0.004 (3)−0.003 (3)
C260.049 (3)0.048 (3)0.058 (3)−0.001 (3)−0.014 (3)−0.003 (3)
C270.065 (4)0.055 (3)0.045 (3)0.002 (3)−0.001 (3)−0.003 (3)
C280.090 (5)0.067 (4)0.063 (4)−0.002 (4)0.027 (4)0.003 (3)
C290.087 (5)0.100 (6)0.067 (4)0.012 (4)−0.004 (4)−0.022 (4)
C300.065 (4)0.047 (3)0.072 (4)−0.001 (3)0.005 (3)−0.006 (3)
C310.043 (3)0.048 (3)0.078 (4)−0.002 (2)−0.003 (3)0.007 (3)
C320.081 (5)0.104 (6)0.108 (6)0.040 (5)−0.005 (5)−0.005 (5)
C330.042 (3)0.030 (2)0.047 (3)0.001 (2)0.001 (2)−0.010 (2)
C340.039 (3)0.035 (2)0.045 (3)0.000 (2)0.005 (2)−0.002 (2)
C350.041 (3)0.033 (2)0.055 (3)0.001 (2)0.002 (2)0.005 (2)
C360.045 (3)0.037 (3)0.049 (3)−0.004 (2)0.001 (2)0.000 (2)

Geometric parameters (Å, °)

Ni1—O12.046 (3)C8—H8A0.9600
Ni1—N42.094 (4)C8—H8B0.9600
Ni1—N22.110 (4)C8—H8C0.9600
Ni1—O32.142 (3)C9—C101.505 (8)
Ni1—N12.174 (4)C9—H9A0.9700
Ni1—N32.173 (4)C9—H9B0.9700
Ni2—N72.087 (4)C10—H10A0.9700
Ni2—N52.090 (4)C10—H10B0.9700
Ni2—N62.117 (5)C11—C131.508 (8)
Ni2—N82.122 (5)C11—C121.519 (8)
Ni2—O52.174 (4)C11—H11A0.9800
Ni2—O42.203 (4)C12—H12A0.9600
Ni2—C362.516 (5)C12—H12B0.9600
Cl1—O81.405 (6)C12—H12C0.9600
Cl1—O71.405 (6)C13—C141.524 (9)
Cl1—O91.411 (5)C13—H13A0.9700
Cl1—O61.414 (6)C13—H13B0.9700
Cl2—O131.416 (10)C14—C161.531 (9)
Cl2—O111.435 (9)C14—C151.570 (9)
Cl2—O121.415 (10)C15—H15A0.9600
Cl2—O101.463 (10)C15—H15B0.9600
Cl2'—O12'1.446 (12)C15—H15C0.9600
Cl2'—O11'1.424 (11)C16—H16A0.9600
Cl2'—O10'1.443 (12)C16—H16B0.9600
Cl2'—O13'1.439 (12)C16—H16C0.9600
O1—C331.250 (6)C17—C181.481 (10)
O2—C331.234 (6)C17—H17A0.9700
O3—C341.438 (6)C17—H17B0.9700
O3—H3O0.8400C18—H18A0.9700
O4—C361.270 (6)C18—H18B0.9700
O5—C361.257 (6)C19—C221.523 (9)
O1W—H110.86 (9)C19—C211.522 (10)
O1W—H120.86 (9)C19—C201.540 (10)
N1—C11.489 (7)C20—H20A0.9600
N1—C141.506 (7)C20—H20B0.9600
N1—H10.85 (5)C20—H20C0.9600
N2—C21.471 (7)C21—H21A0.9600
N2—C31.487 (7)C21—H21B0.9600
N2—H20.84 (5)C21—H21C0.9600
N3—C91.480 (6)C22—C231.517 (8)
N3—C61.513 (7)C22—H22A0.9700
N3—H30.88 (6)C22—H22B0.9700
N4—C101.472 (7)C23—C241.531 (9)
N4—C111.511 (7)C23—H230.9800
N4—H40.85 (5)C24—H24A0.9600
N5—C311.471 (8)C24—H24B0.9600
N5—C171.494 (8)C24—H24C0.9600
N5—H50.85 (5)C25—C261.487 (8)
N6—C181.496 (8)C25—H25A0.9700
N6—C191.510 (9)C25—H25B0.9700
N6—H60.85 (5)C26—H26A0.9700
N7—C231.478 (7)C26—H26B0.9700
N7—C251.483 (7)C27—C281.508 (9)
N7—H70.85 (2)C27—C301.534 (8)
N8—C261.478 (7)C27—C291.547 (9)
N8—C271.491 (7)C28—H28A0.9600
N8—H80.85 (5)C28—H28B0.9600
C1—C21.501 (8)C28—H28C0.9600
C1—H1A0.9700C29—H29A0.9600
C1—H1B0.9700C29—H29B0.9600
C2—H2A0.9700C29—H29C0.9600
C2—H2B0.9700C30—C311.514 (9)
C3—C41.518 (7)C30—H30A0.9700
C3—C51.512 (7)C30—H30B0.9700
C3—H3a0.9800C31—C321.529 (9)
C4—H4A0.9600C31—H310.9800
C4—H4B0.9600C32—H32A0.9600
C4—H4C0.9600C32—H32B0.9600
C5—C61.548 (8)C32—H32C0.9600
C5—H5A0.9700C33—C341.536 (7)
C5—H5B0.9700C34—C351.507 (7)
C6—C71.484 (8)C34—H340.9800
C6—C81.548 (8)C35—C361.510 (7)
C7—H7A0.9600C35—H35A0.9700
C7—H7B0.9600C35—H35B0.9700
C7—H7C0.9600
O1—Ni1—N489.28 (15)C10—C9—H9B109.8
O1—Ni1—N2166.91 (15)H9A—C9—H9B108.2
N4—Ni1—N2103.22 (17)N4—C10—C9109.8 (4)
O1—Ni1—O376.30 (13)N4—C10—H10A109.7
N4—Ni1—O3164.72 (15)C9—C10—H10A109.7
N2—Ni1—O391.55 (15)N4—C10—H10B109.7
O1—Ni1—N199.79 (15)C9—C10—H10B109.7
N4—Ni1—N189.60 (17)H10A—C10—H10B108.2
N2—Ni1—N184.37 (17)C13—C11—N4110.4 (4)
O3—Ni1—N187.94 (16)C13—C11—C12110.9 (5)
O1—Ni1—N388.08 (15)N4—C11—C12111.5 (5)
N4—Ni1—N384.36 (17)C13—C11—H11A108.0
N2—Ni1—N389.29 (17)N4—C11—H11A108.0
O3—Ni1—N399.94 (15)C12—C11—H11A108.0
N1—Ni1—N3170.03 (16)C11—C12—H12A109.5
N7—Ni2—N5104.33 (16)C11—C12—H12B109.5
N7—Ni2—N690.01 (18)H12A—C12—H12B109.5
N5—Ni2—N685.9 (2)C11—C12—H12C109.5
N7—Ni2—N885.12 (18)H12A—C12—H12C109.5
N5—Ni2—N890.06 (18)H12B—C12—H12C109.5
N6—Ni2—N8172.74 (18)C11—C13—C14120.3 (5)
N7—Ni2—O5100.08 (15)C11—C13—H13A107.2
N5—Ni2—O5155.28 (16)C14—C13—H13A107.2
N6—Ni2—O598.00 (17)C11—C13—H13B107.2
N8—Ni2—O588.17 (16)C14—C13—H13B107.2
N7—Ni2—O4158.72 (15)H13A—C13—H13B106.9
N5—Ni2—O496.04 (15)N1—C14—C13110.1 (4)
N6—Ni2—O485.28 (16)N1—C14—C16107.4 (5)
N8—Ni2—O4101.17 (16)C13—C14—C16111.8 (5)
O5—Ni2—O460.25 (13)N1—C14—C15111.4 (5)
N7—Ni2—C36129.40 (16)C13—C14—C15107.8 (5)
N5—Ni2—C36126.19 (17)C16—C14—C15108.2 (5)
N6—Ni2—C3690.80 (17)C14—C15—H15A109.5
N8—Ni2—C3696.45 (17)C14—C15—H15B109.5
O5—Ni2—C3629.99 (15)H15A—C15—H15B109.5
O4—Ni2—C3630.30 (15)C14—C15—H15C109.5
O8—Cl1—O7110.0 (4)H15A—C15—H15C109.5
O8—Cl1—O9111.4 (4)H15B—C15—H15C109.5
O7—Cl1—O9109.9 (4)C14—C16—H16A109.5
O8—Cl1—O6108.5 (4)C14—C16—H16B109.5
O7—Cl1—O6107.2 (4)H16A—C16—H16B109.5
O9—Cl1—O6109.7 (4)C14—C16—H16C109.5
O13—Cl2—O11111.1 (11)H16A—C16—H16C109.5
O13—Cl2—O12113.1 (11)H16B—C16—H16C109.5
O11—Cl2—O12108.8 (8)C18—C17—N5109.8 (5)
O13—Cl2—O10110.5 (11)C18—C17—H17A109.7
O11—Cl2—O10113.5 (8)N5—C17—H17A109.7
O12—Cl2—O1099.4 (9)C18—C17—H17B109.7
O12'—Cl2'—O11'109.9 (16)N5—C17—H17B109.7
O12'—Cl2'—O10'108.9 (16)H17A—C17—H17B108.2
O11'—Cl2'—O10'114.5 (16)C17—C18—N6109.9 (5)
O12'—Cl2'—O13'106.2 (15)C17—C18—H18A109.7
O11'—Cl2'—O13'108.1 (13)N6—C18—H18A109.7
O10'—Cl2'—O13'108.9 (16)C17—C18—H18B109.7
C33—O1—Ni1121.1 (3)N6—C18—H18B109.7
C34—O3—Ni1115.8 (3)H18A—C18—H18B108.2
C34—O3—H3O122.1N6—C19—C22110.3 (5)
Ni1—O3—H3O122.1N6—C19—C21108.1 (6)
C36—O4—Ni288.6 (3)C22—C19—C21111.9 (7)
C36—O5—Ni290.2 (3)N6—C19—C20111.6 (7)
H11—O1W—H12103 (13)C22—C19—C20107.7 (6)
C1—N1—C14113.7 (4)C21—C19—C20107.2 (6)
C1—N1—Ni1103.2 (3)C19—C20—H20A109.5
C14—N1—Ni1121.2 (3)C19—C20—H20B109.5
C1—N1—H1109 (5)H20A—C20—H20B109.5
C14—N1—H1107 (5)C19—C20—H20C109.5
Ni1—N1—H1101 (5)H20A—C20—H20C109.5
C2—N2—C3113.5 (4)H20B—C20—H20C109.5
C2—N2—Ni1104.9 (3)C19—C21—H21A109.5
C3—N2—Ni1115.6 (3)C19—C21—H21B109.5
C2—N2—H2109 (4)H21A—C21—H21B109.5
C3—N2—H2105 (5)C19—C21—H21C109.5
Ni1—N2—H2109 (5)H21A—C21—H21C109.5
C9—N3—C6113.8 (4)H21B—C21—H21C109.5
C9—N3—Ni1104.2 (3)C23—C22—C19120.1 (5)
C6—N3—Ni1122.1 (3)C23—C22—H22A107.3
C9—N3—H3106 (4)C19—C22—H22A107.3
C6—N3—H3101 (4)C23—C22—H22B107.3
Ni1—N3—H3109 (4)C19—C22—H22B107.3
C10—N4—C11111.9 (4)H22A—C22—H22B106.9
C10—N4—Ni1104.2 (3)N7—C23—C22111.4 (5)
C11—N4—Ni1115.9 (3)N7—C23—C24111.3 (5)
C10—N4—H4112 (4)C22—C23—C24108.6 (5)
C11—N4—H4108 (4)N7—C23—H23108.5
Ni1—N4—H4105 (4)C22—C23—H23108.5
C31—N5—C17113.7 (5)C24—C23—H23108.5
C31—N5—Ni2116.4 (3)C23—C24—H24A109.5
C17—N5—Ni2103.8 (4)C23—C24—H24B109.5
C31—N5—H5112 (5)H24A—C24—H24B109.5
C17—N5—H5102 (5)C23—C24—H24C109.5
Ni2—N5—H5108 (5)H24A—C24—H24C109.5
C18—N6—C19115.0 (5)H24B—C24—H24C109.5
C18—N6—Ni2103.5 (4)N7—C25—C26109.9 (4)
C19—N6—Ni2120.7 (4)N7—C25—H25A109.7
C18—N6—H6104 (5)C26—C25—H25A109.7
C19—N6—H6103 (5)N7—C25—H25B109.7
Ni2—N6—H6110 (5)C26—C25—H25B109.7
C23—N7—C25112.9 (4)H25A—C25—H25B108.2
C23—N7—Ni2119.4 (3)N8—C26—C25109.5 (4)
C25—N7—Ni2104.0 (3)N8—C26—H26A109.8
C23—N7—H7109 (4)C25—C26—H26A109.8
C25—N7—H7101 (4)N8—C26—H26B109.8
Ni2—N7—H7108 (4)C25—C26—H26B109.8
C26—N8—C27115.0 (4)H26A—C26—H26B108.2
C26—N8—Ni2104.6 (3)N8—C27—C28107.9 (5)
C27—N8—Ni2120.8 (3)N8—C27—C30110.9 (4)
C26—N8—H8109 (5)C28—C27—C30111.0 (5)
C27—N8—H8110 (5)N8—C27—C29111.5 (5)
Ni2—N8—H895 (4)C28—C27—C29107.9 (5)
N1—C1—C2109.8 (5)C30—C27—C29107.6 (5)
N1—C1—H1A109.7C27—C28—H28A109.5
C2—C1—H1A109.7C27—C28—H28B109.5
N1—C1—H1B109.7H28A—C28—H28B109.5
C2—C1—H1B109.7C27—C28—H28C109.5
H1A—C1—H1B108.2H28A—C28—H28C109.5
N2—C2—C1109.7 (4)H28B—C28—H28C109.5
N2—C2—H2A109.7C27—C29—H29A109.5
C1—C2—H2A109.7C27—C29—H29B109.5
N2—C2—H2B109.7H29A—C29—H29B109.5
C1—C2—H2B109.7C27—C29—H29C109.5
H2A—C2—H2B108.2H29A—C29—H29C109.5
N2—C3—C4113.1 (5)H29B—C29—H29C109.5
N2—C3—C5110.2 (4)C31—C30—C27118.5 (5)
C4—C3—C5110.7 (5)C31—C30—H30A107.7
N2—C3—H3a107.5C27—C30—H30A107.7
C4—C3—H3a107.5C31—C30—H30B107.7
C5—C3—H3a107.5C27—C30—H30B107.7
C3—C4—H4A109.5H30A—C30—H30B107.1
C3—C4—H4B109.5N5—C31—C30110.8 (5)
H4A—C4—H4B109.5N5—C31—C32112.6 (6)
C3—C4—H4C109.5C30—C31—C32108.8 (6)
H4A—C4—H4C109.5N5—C31—H31108.2
H4B—C4—H4C109.5C30—C31—H31108.2
C3—C5—C6119.3 (4)C32—C31—H31108.2
C3—C5—H5A107.5C31—C32—H32A109.5
C6—C5—H5A107.5C31—C32—H32B109.5
C3—C5—H5B107.5H32A—C32—H32B109.5
C6—C5—H5B107.5C31—C32—H32C109.5
H5A—C5—H5B107.0H32A—C32—H32C109.5
C7—C6—N3108.3 (4)H32B—C32—H32C109.5
C7—C6—C8108.2 (5)O2—C33—O1126.6 (5)
N3—C6—C8111.2 (5)O2—C33—C34115.3 (4)
C7—C6—C5111.4 (5)O1—C33—C34118.1 (4)
N3—C6—C5110.4 (4)O3—C34—C35111.7 (4)
C8—C6—C5107.2 (5)O3—C34—C33108.2 (4)
C6—C7—H7A109.5C35—C34—C33112.0 (4)
C6—C7—H7B109.5O3—C34—H34108.2
H7A—C7—H7B109.5C35—C34—H34108.2
C6—C7—H7C109.5C33—C34—H34108.2
H7A—C7—H7C109.5C34—C35—C36113.2 (4)
H7B—C7—H7C109.5C34—C35—H35A108.9
C6—C8—H8A109.5C36—C35—H35A108.9
C6—C8—H8B109.5C34—C35—H35B108.9
H8A—C8—H8B109.5C36—C35—H35B108.9
C6—C8—H8C109.5H35A—C35—H35B107.7
H8A—C8—H8C109.5O5—C36—O4120.8 (5)
H8B—C8—H8C109.5O5—C36—C35120.5 (5)
N3—C9—C10109.4 (4)O4—C36—C35118.8 (4)
N3—C9—H9A109.8O5—C36—Ni259.8 (3)
C10—C9—H9A109.8O4—C36—Ni261.1 (2)
N3—C9—H9B109.8C35—C36—Ni2175.7 (4)
N4—Ni1—O1—C33170.1 (4)Ni1—N2—C2—C144.9 (5)
N2—Ni1—O1—C33−27.0 (9)N1—C1—C2—N2−61.4 (6)
O3—Ni1—O1—C33−4.8 (4)C2—N2—C3—C447.5 (7)
N1—Ni1—O1—C3380.6 (4)Ni1—N2—C3—C4168.7 (4)
N3—Ni1—O1—C33−105.5 (4)C2—N2—C3—C5171.9 (4)
O1—Ni1—O3—C346.3 (3)Ni1—N2—C3—C5−66.8 (5)
N4—Ni1—O3—C34−13.4 (8)N2—C3—C5—C674.0 (6)
N2—Ni1—O3—C34−178.7 (3)C4—C3—C5—C6−160.1 (5)
N1—Ni1—O3—C34−94.3 (3)C9—N3—C6—C7157.0 (5)
N3—Ni1—O3—C3491.8 (3)Ni1—N3—C6—C7−76.7 (5)
N7—Ni2—O4—C3621.9 (6)C9—N3—C6—C838.2 (6)
N5—Ni2—O4—C36−174.9 (3)Ni1—N3—C6—C8164.5 (4)
N6—Ni2—O4—C3699.7 (3)C9—N3—C6—C5−80.7 (5)
N8—Ni2—O4—C36−83.6 (3)Ni1—N3—C6—C545.5 (5)
O5—Ni2—O4—C36−2.3 (3)C3—C5—C6—C759.7 (7)
N7—Ni2—O5—C36−169.0 (3)C3—C5—C6—N3−60.8 (6)
N5—Ni2—O5—C3620.1 (6)C3—C5—C6—C8177.9 (5)
N6—Ni2—O5—C36−77.6 (3)C6—N3—C9—C10173.3 (4)
N8—Ni2—O5—C36106.3 (3)Ni1—N3—C9—C1038.1 (5)
O4—Ni2—O5—C362.3 (3)C11—N4—C10—C9173.7 (4)
O1—Ni1—N1—C1179.2 (3)Ni1—N4—C10—C947.8 (4)
N4—Ni1—N1—C190.0 (4)N3—C9—C10—N4−60.8 (5)
N2—Ni1—N1—C1−13.3 (3)C10—N4—C11—C13176.8 (4)
O3—Ni1—N1—C1−105.1 (4)Ni1—N4—C11—C13−63.9 (5)
O1—Ni1—N1—C1450.5 (4)C10—N4—C11—C1253.1 (6)
N4—Ni1—N1—C14−38.7 (4)Ni1—N4—C11—C12172.4 (4)
N2—Ni1—N1—C14−142.0 (4)N4—C11—C13—C1472.6 (6)
O3—Ni1—N1—C14126.3 (4)C12—C11—C13—C14−163.4 (5)
O1—Ni1—N2—C292.6 (7)C1—N1—C14—C13−76.0 (6)
N4—Ni1—N2—C2−104.9 (4)Ni1—N1—C14—C1347.9 (6)
O3—Ni1—N2—C271.1 (4)C1—N1—C14—C16162.0 (5)
N1—Ni1—N2—C2−16.7 (4)Ni1—N1—C14—C16−74.1 (5)
N3—Ni1—N2—C2171.0 (4)C1—N1—C14—C1543.6 (7)
O1—Ni1—N2—C3−33.1 (9)Ni1—N1—C14—C15167.5 (4)
N4—Ni1—N2—C3129.3 (4)C11—C13—C14—N1−62.5 (7)
O3—Ni1—N2—C3−54.7 (4)C11—C13—C14—C1656.9 (7)
N1—Ni1—N2—C3−142.4 (4)C11—C13—C14—C15175.7 (5)
N3—Ni1—N2—C345.3 (4)C31—N5—C17—C18−171.1 (5)
O1—Ni1—N3—C9−99.3 (3)Ni2—N5—C17—C18−43.8 (5)
N4—Ni1—N3—C9−9.8 (3)N5—C17—C18—N660.1 (7)
N2—Ni1—N3—C993.5 (3)C19—N6—C18—C17−174.9 (5)
O3—Ni1—N3—C9−175.0 (3)Ni2—N6—C18—C17−41.2 (5)
O1—Ni1—N3—C6130.3 (4)C18—N6—C19—C2273.4 (7)
N4—Ni1—N3—C6−140.3 (4)Ni2—N6—C19—C22−51.8 (6)
N2—Ni1—N3—C6−36.9 (4)C18—N6—C19—C21−164.0 (6)
O3—Ni1—N3—C654.5 (4)Ni2—N6—C19—C2170.8 (7)
O1—Ni1—N4—C1068.1 (3)C18—N6—C19—C20−46.3 (7)
N2—Ni1—N4—C10−108.0 (3)Ni2—N6—C19—C20−171.5 (5)
O3—Ni1—N4—C1087.2 (7)N6—C19—C22—C2363.5 (8)
N1—Ni1—N4—C10167.9 (3)C21—C19—C22—C23−56.9 (8)
N3—Ni1—N4—C10−20.1 (3)C20—C19—C22—C23−174.5 (7)
O1—Ni1—N4—C11−55.4 (4)C25—N7—C23—C22179.9 (5)
N2—Ni1—N4—C11128.6 (4)Ni2—N7—C23—C2257.2 (6)
O3—Ni1—N4—C11−36.2 (8)C25—N7—C23—C24−58.8 (6)
N1—Ni1—N4—C1144.5 (4)Ni2—N7—C23—C24178.6 (4)
N3—Ni1—N4—C11−143.5 (4)C19—C22—C23—N7−67.2 (7)
N7—Ni2—N5—C31−129.5 (4)C19—C22—C23—C24169.9 (6)
N6—Ni2—N5—C31141.5 (4)C23—N7—C25—C26−175.7 (4)
N8—Ni2—N5—C31−44.5 (4)Ni2—N7—C25—C26−44.9 (5)
O5—Ni2—N5—C3141.2 (6)C27—N8—C26—C25−174.6 (4)
O4—Ni2—N5—C3156.7 (4)Ni2—N8—C26—C25−39.8 (5)
C36—Ni2—N5—C3153.5 (4)N7—C25—C26—N859.7 (6)
N7—Ni2—N5—C17104.8 (4)C26—N8—C27—C28−161.0 (5)
N6—Ni2—N5—C1715.9 (4)Ni2—N8—C27—C2872.1 (5)
N8—Ni2—N5—C17−170.2 (4)C26—N8—C27—C3077.3 (6)
O5—Ni2—N5—C17−84.4 (5)Ni2—N8—C27—C30−49.7 (6)
O4—Ni2—N5—C17−68.9 (4)C26—N8—C27—C29−42.6 (7)
C36—Ni2—N5—C17−72.1 (4)Ni2—N8—C27—C29−169.5 (4)
N7—Ni2—N6—C18−91.2 (4)N8—C27—C30—C3162.6 (7)
N5—Ni2—N6—C1813.1 (4)C28—C27—C30—C31−57.4 (7)
O5—Ni2—N6—C18168.6 (4)C29—C27—C30—C31−175.2 (6)
O4—Ni2—N6—C18109.5 (4)C17—N5—C31—C30−176.0 (5)
C36—Ni2—N6—C18139.4 (4)Ni2—N5—C31—C3063.5 (5)
N7—Ni2—N6—C1939.1 (4)C17—N5—C31—C32−53.9 (7)
N5—Ni2—N6—C19143.5 (4)Ni2—N5—C31—C32−174.4 (5)
O5—Ni2—N6—C19−61.1 (4)C27—C30—C31—N5−71.3 (7)
O4—Ni2—N6—C19−120.1 (4)C27—C30—C31—C32164.3 (6)
C36—Ni2—N6—C19−90.3 (4)Ni1—O1—C33—O2−177.9 (4)
N5—Ni2—N7—C23−127.0 (4)Ni1—O1—C33—C342.5 (6)
N6—Ni2—N7—C23−41.2 (4)Ni1—O3—C34—C35−130.4 (3)
N8—Ni2—N7—C23144.2 (4)Ni1—O3—C34—C33−6.6 (5)
O5—Ni2—N7—C2357.0 (4)O2—C33—C34—O3−176.7 (4)
O4—Ni2—N7—C2335.8 (7)O1—C33—C34—O32.9 (6)
C36—Ni2—N7—C2349.9 (4)O2—C33—C34—C35−53.1 (6)
N5—Ni2—N7—C25106.1 (3)O1—C33—C34—C35126.5 (5)
N6—Ni2—N7—C25−168.1 (3)O3—C34—C35—C36−57.3 (5)
N8—Ni2—N7—C2517.3 (3)C33—C34—C35—C36−178.9 (4)
O5—Ni2—N7—C25−69.9 (3)Ni2—O5—C36—O4−4.0 (5)
O4—Ni2—N7—C25−91.1 (5)Ni2—O5—C36—C35175.0 (4)
C36—Ni2—N7—C25−77.0 (4)Ni2—O4—C36—O54.0 (5)
N7—Ni2—N8—C2611.9 (3)Ni2—O4—C36—C35−175.0 (4)
N5—Ni2—N8—C26−92.5 (3)C34—C35—C36—O5−144.5 (5)
O5—Ni2—N8—C26112.2 (3)C34—C35—C36—O434.5 (7)
O4—Ni2—N8—C26171.3 (3)N7—Ni2—C36—O514.0 (4)
C36—Ni2—N8—C26141.0 (3)N5—Ni2—C36—O5−169.7 (3)
N7—Ni2—N8—C27143.4 (4)N6—Ni2—C36—O5104.7 (3)
N5—Ni2—N8—C2739.1 (4)N8—Ni2—C36—O5−74.9 (3)
O5—Ni2—N8—C27−116.3 (4)O4—Ni2—C36—O5−176.1 (5)
O4—Ni2—N8—C27−57.1 (4)N7—Ni2—C36—O4−169.9 (3)
C36—Ni2—N8—C27−87.4 (4)N5—Ni2—C36—O46.3 (4)
C14—N1—C1—C2174.7 (5)N6—Ni2—C36—O4−79.2 (3)
Ni1—N1—C1—C241.5 (5)N8—Ni2—C36—O4101.1 (3)
C3—N2—C2—C1172.0 (5)O5—Ni2—C36—O4176.1 (5)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N2—H2···O6i0.84 (5)2.41 (2)3.230 (7)165 (6)
N5—H5···O2ii0.85 (5)2.14 (3)2.940 (6)158 (6)
N7—H7···O2ii0.85 (2)2.06 (2)2.869 (5)160 (6)
O1w—H11···O50.86 (9)2.09 (7)2.862 (9)149 (12)
O1w—H12···O60.86 (9)2.05 (8)2.784 (12)143 (13)

Symmetry codes: (i) x−1, y, z; (ii) −x+1, y+1/2, −z+3/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: XU2535).

References

  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–211.
  • Bruker (1999). SMART and SAINT-Plus Bruker AXS Inc, Madison, Wisconsin, USA.
  • Flack, H. D. (1983). Acta Cryst. A39, 876–881.
  • Ou, G.-C., Zhang, M. & Yuan, X.-Y. (2009). Acta Cryst. E65, m726. [PMC free article] [PubMed]
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Westrip, S. P. (2009). publCIF In preparation.

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