# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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#  from this site to visualise CIF-encoded structures and 
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data_dw1253

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H48 Li2 N4 Ni O4, 0.667(C7 H8)'
_chemical_formula_sum            'C40.67 H53.33 Li2 N4 Ni O4'
_chemical_formula_weight         734.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   20.0120(6)
_cell_length_b                   20.0120(6)
_cell_length_c                   8.1348(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2821.36(14)
_cell_formula_units_Z            3
_cell_measurement_temperature    120(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            orange-red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1174
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8723
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 The toluene solvate molecules are disordered across the -2 position.
 For the refinement, they were modelled with bond constraints and a 
 common isotropic displacement parameter for the C atoms.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_reflns_number            15927
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3334
_reflns_number_gt                2164
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick 2008)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3334
_refine_ls_number_parameters     242
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1135
_refine_ls_wR_factor_gt          0.1098
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.0000 0.5000 0.5000 0.02781(19) Uani 1 2 d S . .
Li1 Li 1.0102(3) 0.5884(3) 0.7368(6) 0.0398(12) Uani 1 1 d . . .
N1 N 0.97119(15) 0.57592(14) 0.4954(3) 0.0311(6) Uani 1 1 d . . .
H1 H 0.9262(14) 0.5600(13) 0.474(3) 0.010(7) Uiso 1 1 d . . .
N2 N 1.09271(13) 0.57716(14) 0.5989(3) 0.0300(6) Uani 1 1 d . . .
H2 H 1.1205(16) 0.5566(15) 0.637(3) 0.033(8) Uiso 1 1 d . . .
C1 C 1.01753(16) 0.64960(16) 0.4338(3) 0.0284(7) Uani 1 1 d . . .
C2 C 1.10048(15) 0.68601(15) 0.4449(3) 0.0267(7) Uani 1 1 d . . .
C3 C 1.13703(15) 0.64834(15) 0.5230(3) 0.0276(7) Uani 1 1 d . . .
C4 C 1.21775(16) 0.68639(16) 0.5251(3) 0.0312(7) Uani 1 1 d . . .
H4 H 1.2430 0.6624 0.5765 0.037 Uiso 1 1 calc R . .
C5 C 1.26181(17) 0.75891(17) 0.4532(3) 0.0359(7) Uani 1 1 d . . .
H5 H 1.3165 0.7826 0.4535 0.043 Uiso 1 1 calc R . .
C6 C 1.22816(17) 0.79635(17) 0.3826(3) 0.0350(7) Uani 1 1 d . . .
H6 H 1.2594 0.8459 0.3354 0.042 Uiso 1 1 calc R . .
C7 C 1.14670(16) 0.76165(16) 0.3793(3) 0.0306(7) Uani 1 1 d . . .
C8 C 1.11107(18) 0.80076(17) 0.3114(3) 0.0379(8) Uani 1 1 d . . .
H8 H 1.1420 0.8515 0.2692 0.046 Uiso 1 1 calc R . .
C9 C 1.03231(19) 0.76645(17) 0.3057(3) 0.0400(8) Uani 1 1 d . . .
H9 H 1.0089 0.7938 0.2615 0.048 Uiso 1 1 calc R . .
C10 C 0.98621(17) 0.69137(17) 0.3647(3) 0.0359(7) Uani 1 1 d . . .
H10 H 0.9317 0.6681 0.3573 0.043 Uiso 1 1 calc R . .
O1 O 0.93529(11) 0.51829(11) 0.8943(2) 0.0378(5) Uani 1 1 d . . .
C11 C 0.91250(19) 0.53912(19) 1.0444(3) 0.0466(8) Uani 1 1 d . . .
H11A H 0.9281 0.5945 1.0447 0.056 Uiso 1 1 calc R . .
H11B H 0.9356 0.5281 1.1410 0.056 Uiso 1 1 calc R . .
C12 C 0.82547(19) 0.4888(2) 1.0451(4) 0.0549(10) Uani 1 1 d . . .
H12A H 0.8010 0.5118 0.9774 0.066 Uiso 1 1 calc R . .
H12B H 0.8047 0.4807 1.1583 0.066 Uiso 1 1 calc R . .
C13 C 0.81292(19) 0.4139(2) 0.9706(4) 0.0607(10) Uani 1 1 d . . .
H13A H 0.8077 0.3770 1.0575 0.073 Uiso 1 1 calc R . .
H13B H 0.7660 0.3899 0.9012 0.073 Uiso 1 1 calc R . .
C14 C 0.88373(19) 0.43712(19) 0.8690(4) 0.0517(9) Uani 1 1 d . . .
H14A H 0.9088 0.4074 0.9030 0.062 Uiso 1 1 calc R . .
H14B H 0.8698 0.4266 0.7513 0.062 Uiso 1 1 calc R . .
O2 O 1.04596(11) 0.68779(11) 0.8372(2) 0.0395(5) Uani 1 1 d . . .
C21 C 1.0109(2) 0.7341(2) 0.8114(4) 0.0602(10) Uani 1 1 d . . .
H21A H 0.9774 0.7298 0.9052 0.072 Uiso 1 1 calc R . .
H21B H 0.9799 0.7189 0.7093 0.072 Uiso 1 1 calc R . .
C22 C 1.0800(4) 0.8159(3) 0.7977(8) 0.1152(18) Uani 1 1 d U . .
H22A H 1.0872 0.8333 0.6819 0.138 Uiso 1 1 calc R . .
H22B H 1.0710 0.8518 0.8648 0.138 Uiso 1 1 calc R . .
C23 C 1.1435(3) 0.8153(3) 0.8516(7) 0.137(3) Uani 1 1 d . . .
H23A H 1.1645 0.8488 0.9496 0.164 Uiso 1 1 calc R . .
H23B H 1.1836 0.8356 0.7649 0.164 Uiso 1 1 calc R . .
C24 C 1.1234(2) 0.7379(3) 0.8925(4) 0.0676(12) Uani 1 1 d . . .
H24A H 1.1269 0.7328 1.0128 0.081 Uiso 1 1 calc R . .
H24B H 1.1592 0.7242 0.8380 0.081 Uiso 1 1 calc R . .
C31 C 0.9691(12) 1.0093(11) 0.5160(18) 0.065(2) Uiso 0.17 1 d PGD A -1
C32 C 1.0479(11) 1.0608(15) 0.505(3) 0.065(2) Uiso 0.17 1 d PGD A -1
C33 C 1.0993(15) 1.033(2) 0.496(3) 0.065(2) Uiso 0.17 1 d PGD A -1
C34 C 1.072(2) 0.954(2) 0.497(3) 0.065(2) Uiso 0.17 1 d PGD A -1
C35 C 0.993(2) 0.9028(17) 0.508(3) 0.065(2) Uiso 0.17 1 d PGD A -1
C36 C 0.9417(17) 0.9303(12) 0.518(2) 0.065(2) Uiso 0.17 1 d PGD A -1
C37 C 0.9177(10) 1.0368(10) 0.525(2) 0.065(2) Uiso 0.17 1 d PD A -1
C41 C 0.9409(10) 0.9568(15) 1.002(4) 0.115(5) Uiso 0.17 1 d PGD B -1
C42 C 0.9991(9) 0.941(2) 0.959(5) 0.115(5) Uiso 0.17 1 d PGD B -1
C43 C 1.0758(9) 1.000(3) 0.964(6) 0.115(5) Uiso 0.17 1 d PGD B -1
C44 C 1.0943(13) 1.074(2) 1.013(6) 0.115(5) Uiso 0.17 1 d PGD B -1
C45 C 1.0362(19) 1.0892(16) 1.056(4) 0.115(5) Uiso 0.17 1 d PGD B -1
C46 C 0.9594(16) 1.0307(13) 1.050(4) 0.115(5) Uiso 0.17 1 d PGD B -1
C47 C 0.8642(9) 0.8983(13) 0.997(4) 0.115(5) Uiso 0.17 1 d PD B -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0216(3) 0.0262(3) 0.0316(3) -0.0012(2) 0.0016(2) 0.0090(3)
Li1 0.038(3) 0.043(3) 0.038(3) 0.005(2) 0.009(2) 0.020(3)
N1 0.0166(14) 0.0326(16) 0.0397(15) -0.0002(11) -0.0004(11) 0.0089(13)
N2 0.0276(14) 0.0304(15) 0.0308(13) 0.0019(10) -0.0019(11) 0.0134(13)
C1 0.0281(17) 0.0282(17) 0.0272(14) -0.0048(12) 0.0006(12) 0.0127(15)
C2 0.0277(17) 0.0283(17) 0.0227(14) -0.0059(12) -0.0005(12) 0.0130(14)
C3 0.0267(17) 0.0259(16) 0.0254(14) -0.0054(12) 0.0021(12) 0.0094(14)
C4 0.0266(17) 0.0293(17) 0.0364(16) -0.0059(13) -0.0037(13) 0.0129(15)
C5 0.0219(17) 0.0319(19) 0.0428(18) -0.0074(14) 0.0011(13) 0.0051(15)
C6 0.0326(19) 0.0259(17) 0.0374(17) 0.0008(13) 0.0023(13) 0.0077(15)
C7 0.0306(18) 0.0285(17) 0.0266(15) -0.0049(12) -0.0003(12) 0.0102(15)
C8 0.042(2) 0.0272(17) 0.0380(17) 0.0023(13) -0.0002(14) 0.0123(16)
C9 0.046(2) 0.0345(19) 0.0428(18) -0.0001(14) -0.0049(15) 0.0223(17)
C10 0.0301(18) 0.0348(19) 0.0415(17) -0.0008(14) -0.0036(14) 0.0152(16)
O1 0.0388(13) 0.0380(13) 0.0331(11) 0.0006(9) 0.0095(9) 0.0165(11)
C11 0.060(2) 0.044(2) 0.0352(17) -0.0010(15) 0.0133(15) 0.0259(19)
C12 0.052(2) 0.080(3) 0.047(2) 0.0145(18) 0.0154(17) 0.045(2)
C13 0.039(2) 0.062(3) 0.064(2) -0.0059(19) 0.0085(18) 0.012(2)
C14 0.050(2) 0.041(2) 0.052(2) -0.0037(16) 0.0120(16) 0.0133(19)
O2 0.0308(12) 0.0352(13) 0.0468(12) -0.0050(9) 0.0009(9) 0.0121(10)
C21 0.058(2) 0.075(3) 0.062(2) -0.0225(19) -0.0096(18) 0.044(2)
C22 0.144(4) 0.061(3) 0.140(4) -0.010(3) -0.025(3) 0.051(3)
C23 0.114(5) 0.085(4) 0.093(4) 0.026(3) -0.008(3) -0.039(4)
C24 0.042(2) 0.102(4) 0.058(2) -0.045(2) -0.0128(18) 0.036(2)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.876(2) 4_766 ?
Ni1 N1 1.876(2) . ?
Ni1 N2 1.900(2) . ?
Ni1 N2 1.900(2) 4_766 ?
Ni1 Li1 2.554(5) . ?
Ni1 Li1 2.554(5) 4_766 ?
Li1 O2 1.927(5) . ?
Li1 O1 1.937(5) . ?
Li1 N1 2.081(5) . ?
Li1 N2 2.100(5) . ?
Li1 C1 2.723(5) . ?
N1 C1 1.385(3) . ?
N1 H1 0.81(2) . ?
N2 C3 1.391(3) . ?
N2 H2 0.89(3) . ?
C1 C10 1.390(4) . ?
C1 C2 1.444(4) . ?
C2 C7 1.425(4) . ?
C2 C3 1.435(4) . ?
C3 C4 1.400(4) . ?
C4 C5 1.395(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.360(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.417(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.408(4) . ?
C8 C9 1.369(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.397(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
O1 C11 1.437(3) . ?
O1 C14 1.438(3) . ?
C11 C12 1.514(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.516(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.499(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O2 C21 1.430(4) . ?
O2 C24 1.434(4) . ?
C21 C22 1.530(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.348(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.432(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C31 C37 1.3903(11) . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C41 C47 1.3897(12) . ?
C41 C42 1.3900 . ?
C41 C46 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 179.998(1) 4_766 . ?
N1 Ni1 N2 94.54(11) 4_766 . ?
N1 Ni1 N2 85.46(11) . . ?
N1 Ni1 N2 85.46(11) 4_766 4_766 ?
N1 Ni1 N2 94.54(11) . 4_766 ?
N2 Ni1 N2 180.0 . 4_766 ?
N1 Ni1 Li1 126.56(13) 4_766 . ?
N1 Ni1 Li1 53.43(13) . . ?
N2 Ni1 Li1 53.86(13) . . ?
N2 Ni1 Li1 126.14(13) 4_766 . ?
N1 Ni1 Li1 53.44(13) 4_766 4_766 ?
N1 Ni1 Li1 126.57(13) . 4_766 ?
N2 Ni1 Li1 126.14(13) . 4_766 ?
N2 Ni1 Li1 53.86(13) 4_766 4_766 ?
Li1 Ni1 Li1 180.0(2) . 4_766 ?
O2 Li1 O1 102.8(2) . . ?
O2 Li1 N1 116.6(3) . . ?
O1 Li1 N1 115.4(3) . . ?
O2 Li1 N2 115.5(3) . . ?
O1 Li1 N2 129.9(3) . . ?
N1 Li1 N2 75.58(18) . . ?
O2 Li1 Ni1 153.5(2) . . ?
O1 Li1 Ni1 103.4(2) . . ?
N1 Li1 Ni1 46.36(12) . . ?
N2 Li1 Ni1 46.95(12) . . ?
O2 Li1 C1 90.6(2) . . ?
O1 Li1 C1 140.6(3) . . ?
N1 Li1 C1 29.87(11) . . ?
N2 Li1 C1 72.31(16) . . ?
Ni1 Li1 C1 66.20(13) . . ?
C1 N1 Ni1 123.8(2) . . ?
C1 N1 Li1 101.7(2) . . ?
Ni1 N1 Li1 80.20(17) . . ?
C1 N1 H1 111.3(17) . . ?
Ni1 N1 H1 114.7(17) . . ?
Li1 N1 H1 121.5(16) . . ?
C3 N2 Ni1 120.52(18) . . ?
C3 N2 Li1 105.1(2) . . ?
Ni1 N2 Li1 79.19(17) . . ?
C3 N2 H2 113.5(17) . . ?
Ni1 N2 H2 110.5(17) . . ?
Li1 N2 H2 124.7(17) . . ?
N1 C1 C10 121.6(3) . . ?
N1 C1 C2 120.2(3) . . ?
C10 C1 C2 118.2(3) . . ?
N1 C1 Li1 48.47(17) . . ?
C10 C1 Li1 134.2(2) . . ?
C2 C1 Li1 87.75(19) . . ?
C7 C2 C3 119.6(2) . . ?
C7 C2 C1 119.0(2) . . ?
C3 C2 C1 121.5(2) . . ?
N2 C3 C4 121.5(2) . . ?
N2 C3 C2 120.2(2) . . ?
C4 C3 C2 118.2(2) . . ?
C5 C4 C3 121.2(3) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C6 C5 C4 121.4(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 120.9(3) . . ?
C8 C7 C2 119.8(3) . . ?
C6 C7 C2 119.3(3) . . ?
C9 C8 C7 120.7(3) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 120.2(3) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C1 C10 C9 122.1(3) . . ?
C1 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C11 O1 C14 107.2(2) . . ?
C11 O1 Li1 126.5(2) . . ?
C14 O1 Li1 125.6(2) . . ?
O1 C11 C12 103.7(2) . . ?
O1 C11 H11A 111.0 . . ?
C12 C11 H11A 111.0 . . ?
O1 C11 H11B 111.0 . . ?
C12 C11 H11B 111.0 . . ?
H11A C11 H11B 109.0 . . ?
C11 C12 C13 102.9(3) . . ?
C11 C12 H12A 111.2 . . ?
C13 C12 H12A 111.2 . . ?
C11 C12 H12B 111.2 . . ?
C13 C12 H12B 111.2 . . ?
H12A C12 H12B 109.1 . . ?
C14 C13 C12 104.5(3) . . ?
C14 C13 H13A 110.9 . . ?
C12 C13 H13A 110.9 . . ?
C14 C13 H13B 110.9 . . ?
C12 C13 H13B 110.9 . . ?
H13A C13 H13B 108.9 . . ?
O1 C14 C13 107.7(3) . . ?
O1 C14 H14A 110.2 . . ?
C13 C14 H14A 110.2 . . ?
O1 C14 H14B 110.2 . . ?
C13 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
C21 O2 C24 107.6(3) . . ?
C21 O2 Li1 123.8(2) . . ?
C24 O2 Li1 124.7(2) . . ?
O2 C21 C22 103.3(3) . . ?
O2 C21 H21A 111.1 . . ?
C22 C21 H21A 111.1 . . ?
O2 C21 H21B 111.1 . . ?
C22 C21 H21B 111.1 . . ?
H21A C21 H21B 109.1 . . ?
C23 C22 C21 108.6(4) . . ?
C23 C22 H22A 110.0 . . ?
C21 C22 H22A 110.0 . . ?
C23 C22 H22B 110.0 . . ?
C21 C22 H22B 110.0 . . ?
H22A C22 H22B 108.3 . . ?
C22 C23 C24 109.2(4) . . ?
C22 C23 H23A 109.8 . . ?
C24 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 108.3 . . ?
C23 C24 O2 107.7(4) . . ?
C23 C24 H24A 110.2 . . ?
O2 C24 H24A 110.2 . . ?
C23 C24 H24B 110.2 . . ?
O2 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
C32 C31 C36 120.0 . . ?
C32 C31 C37 120.0 . . ?
C36 C31 C37 120.0 . . ?
C31 C32 C33 120.0 . . ?
C32 C33 C34 120.0 . . ?
C33 C34 C35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C31 120.0 . . ?
C47 C41 C42 120.0 . . ?
C47 C41 C46 120.0 . . ?
C42 C41 C46 120.0 . . ?
C43 C42 C41 120.0 . . ?
C42 C43 C44 120.0 . . ?
C43 C44 C45 120.0 . . ?
C46 C45 C44 120.0 . . ?
C45 C46 C41 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 943106'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw1245

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H66 Li3 N6 O6 V, 2(C4 H8 O)'
_chemical_formula_sum            'C62 H82 Li3 N6 O8 V'
_chemical_formula_weight         1111.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.7117(6)
_cell_length_b                   14.1550(4)
_cell_length_c                   18.9518(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.140(1)
_cell_angle_gamma                90.00
_cell_volume                     6024.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2368
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 The thf solvate molecule is disordered.  For the refinement, this was
 modelled as two 1/2 weight molecules with bond length constraints and a
 common isotropic displacement parameter for the C and O atoms (JED).
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_reflns_number            21086
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.64
_diffrn_reflns_theta_max         26.38
_reflns_number_total             6087
_reflns_number_gt                3812
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+4.0268P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6087
_refine_ls_number_parameters     351
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.2060
_refine_ls_wR_factor_gt          0.1828
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.0000 0.26760(5) 0.2500 0.0332(2) Uani 1 2 d S . .
O1 O -0.14461(10) 0.46133(17) 0.16598(13) 0.0466(6) Uani 1 1 d . . .
O2 O -0.13393(9) 0.37439(18) 0.31077(13) 0.0460(6) Uani 1 1 d . . .
O3 O -0.06445(11) -0.01800(18) 0.19575(15) 0.0508(6) Uani 1 1 d . . .
Li1 Li -0.0953(2) 0.3682(4) 0.2446(3) 0.0411(13) Uani 1 1 d . . .
Li2 Li 0.0000 0.0739(6) 0.2500 0.050(2) Uani 1 2 d S . .
N1 N -0.00191(11) 0.37610(18) 0.32068(15) 0.0346(6) Uani 1 1 d . . .
N2 N -0.08998(11) 0.24630(18) 0.18400(16) 0.0363(6) Uani 1 1 d . . .
N3 N -0.00746(12) 0.16937(19) 0.32720(17) 0.0401(7) Uani 1 1 d . . .
C1 C 0.00547(12) 0.4725(2) 0.32040(18) 0.0351(7) Uani 1 1 d . . .
C2 C 0.0000 0.5219(3) 0.2500 0.0350(10) Uani 1 2 d S . .
C3 C 0.0000 0.6228(3) 0.2500 0.0414(11) Uani 1 2 d S . .
C4 C 0.00900(14) 0.6729(2) 0.3198(2) 0.0461(9) Uani 1 1 d . . .
H4A H 0.0091 0.7400 0.3197 0.055 Uiso 1 1 calc R . .
C5 C 0.01748(14) 0.6252(3) 0.3874(2) 0.0457(9) Uani 1 1 d . . .
H5A H 0.0245 0.6594 0.4343 0.055 Uiso 1 1 calc R . .
C6 C 0.01586(14) 0.5274(2) 0.3879(2) 0.0409(8) Uani 1 1 d . . .
H6A H 0.0220 0.4962 0.4357 0.049 Uiso 1 1 calc R . .
C7 C -0.17093(16) 0.4515(3) 0.0802(2) 0.0538(10) Uani 1 1 d . . .
H7A H -0.1888 0.3880 0.0626 0.065 Uiso 1 1 calc R . .
H7B H -0.1409 0.4612 0.0625 0.065 Uiso 1 1 calc R . .
C8 C -0.21806(18) 0.5271(3) 0.0464(2) 0.0639(11) Uani 1 1 d . . .
H8A H -0.2262 0.5471 -0.0081 0.077 Uiso 1 1 calc R . .
H8B H -0.2556 0.5054 0.0436 0.077 Uiso 1 1 calc R . .
C9 C -0.1901(2) 0.6052(3) 0.1067(3) 0.0762(13) Uani 1 1 d . . .
H9A H -0.2209 0.6459 0.1082 0.091 Uiso 1 1 calc R . .
H9B H -0.1642 0.6448 0.0935 0.091 Uiso 1 1 calc R . .
C10 C -0.15426(16) 0.5553(3) 0.1856(2) 0.0538(10) Uani 1 1 d . . .
H10A H -0.1158 0.5879 0.2186 0.065 Uiso 1 1 calc R . .
H10B H -0.1762 0.5536 0.2164 0.065 Uiso 1 1 calc R . .
C11 C -0.19633(14) 0.3527(3) 0.2764(2) 0.0468(9) Uani 1 1 d . . .
H11A H -0.2067 0.2965 0.2410 0.056 Uiso 1 1 calc R . .
H11B H -0.2209 0.4066 0.2441 0.056 Uiso 1 1 calc R . .
C12 C -0.20666(18) 0.3337(4) 0.3465(3) 0.0694(12) Uani 1 1 d . . .
H12A H -0.2432 0.3658 0.3389 0.083 Uiso 1 1 calc R . .
H12B H -0.2106 0.2650 0.3527 0.083 Uiso 1 1 calc R . .
C13 C -0.1536(2) 0.3720(6) 0.4174(3) 0.115(2) Uani 1 1 d . . .
H13A H -0.1605 0.4382 0.4276 0.138 Uiso 1 1 calc R . .
H13B H -0.1438 0.3339 0.4661 0.138 Uiso 1 1 calc R . .
C14 C -0.10574(17) 0.3668(3) 0.3972(2) 0.0590(11) Uani 1 1 d . . .
H14A H -0.0771 0.4191 0.4232 0.071 Uiso 1 1 calc R . .
H14B H -0.0842 0.3060 0.4156 0.071 Uiso 1 1 calc R . .
C15 C -0.13078(14) 0.1909(2) 0.1932(2) 0.0384(8) Uani 1 1 d . . .
C16 C -0.18852(15) 0.1785(3) 0.1284(2) 0.0479(9) Uani 1 1 d . . .
H16A H -0.1976 0.2021 0.0767 0.057 Uiso 1 1 calc R . .
C17 C -0.23276(16) 0.1330(3) 0.1371(3) 0.0542(10) Uani 1 1 d . . .
H17A H -0.2713 0.1253 0.0917 0.065 Uiso 1 1 calc R . .
C18 C -0.22122(17) 0.0997(3) 0.2100(3) 0.0645(12) Uani 1 1 d . . .
H18A H -0.2526 0.0719 0.2158 0.077 Uiso 1 1 calc R . .
C19 C -0.16336(17) 0.1050(3) 0.2784(3) 0.0540(10) Uani 1 1 d . . .
C20 C -0.1513(2) 0.0677(3) 0.3535(3) 0.0753(14) Uani 1 1 d . . .
H20A H -0.1825 0.0404 0.3598 0.090 Uiso 1 1 calc R . .
C21 C -0.0949(2) 0.0706(3) 0.4176(3) 0.0763(14) Uani 1 1 d . . .
H21A H -0.0877 0.0478 0.4687 0.092 Uiso 1 1 calc R . .
C22 C -0.04740(19) 0.1066(3) 0.4092(3) 0.0588(10) Uani 1 1 d . . .
H22A H -0.0084 0.1059 0.4544 0.071 Uiso 1 1 calc R . .
C23 C -0.05606(16) 0.1432(2) 0.3363(2) 0.0449(8) Uani 1 1 d . . .
C24 C -0.11599(15) 0.1486(2) 0.2694(2) 0.0446(9) Uani 1 1 d . . .
C25 C -0.08041(18) -0.0829(3) 0.2397(2) 0.0550(10) Uani 1 1 d . . .
H25A H -0.0962 -0.0485 0.2707 0.066 Uiso 1 1 calc R . .
H25B H -0.0452 -0.1199 0.2779 0.066 Uiso 1 1 calc R . .
C26 C -0.1268(2) -0.1466(5) 0.1792(4) 0.107(2) Uani 1 1 d . . .
H26A H -0.1659 -0.1346 0.1759 0.129 Uiso 1 1 calc R . .
H26B H -0.1159 -0.2136 0.1938 0.129 Uiso 1 1 calc R . .
C27 C -0.1291(2) -0.1237(4) 0.1004(3) 0.0886(17) Uani 1 1 d . . .
H27A H -0.1705 -0.1265 0.0551 0.106 Uiso 1 1 calc R . .
H27B H -0.1040 -0.1678 0.0894 0.106 Uiso 1 1 calc R . .
C28 C -0.1051(3) -0.0250(4) 0.1132(3) 0.0936(18) Uani 1 1 d . . .
H28A H -0.0850 -0.0134 0.0807 0.112 Uiso 1 1 calc R . .
H28B H -0.1376 0.0217 0.0974 0.112 Uiso 1 1 calc R . .
O51 O 0.1179(3) 0.2345(5) 0.5029(4) 0.0587(6) Uiso 0.465(6) 1 d PD A 1
C52 C 0.1538(6) 0.1720(9) 0.5615(8) 0.0587(6) Uiso 0.465(6) 1 d PD A 1
H52A H 0.1940 0.1723 0.5666 0.070 Uiso 0.465(6) 1 calc PR A 1
H52B H 0.1373 0.1075 0.5463 0.070 Uiso 0.465(6) 1 calc PR A 1
C53 C 0.1582(4) 0.1994(7) 0.6421(5) 0.0587(6) Uiso 0.465(6) 1 d PD A 1
H53A H 0.1432 0.1476 0.6623 0.070 Uiso 0.465(6) 1 calc PR A 1
H53B H 0.2002 0.2123 0.6827 0.070 Uiso 0.465(6) 1 calc PR A 1
C54 C 0.1229(4) 0.2822(6) 0.6281(5) 0.0587(6) Uiso 0.465(6) 1 d PD A 1
H54A H 0.1479 0.3398 0.6464 0.070 Uiso 0.465(6) 1 calc PR A 1
H54B H 0.0986 0.2783 0.6555 0.070 Uiso 0.465(6) 1 calc PR A 1
C55 C 0.0820(4) 0.2810(7) 0.5323(5) 0.0587(6) Uiso 0.465(6) 1 d PD A 1
H55A H 0.0448 0.2455 0.5164 0.070 Uiso 0.465(6) 1 calc PR A 1
H55B H 0.0718 0.3461 0.5107 0.070 Uiso 0.465(6) 1 calc PR A 1
O51' O 0.1273(3) 0.2653(4) 0.5119(4) 0.0587(6) Uiso 0.535(6) 1 d PD A 2
C52' C 0.1601(5) 0.1830(8) 0.5629(7) 0.0587(6) Uiso 0.535(6) 1 d PD A 2
H52C H 0.2037 0.1925 0.5879 0.070 Uiso 0.535(6) 1 calc PR A 2
H52D H 0.1492 0.1242 0.5306 0.070 Uiso 0.535(6) 1 calc PR A 2
C53' C 0.1406(4) 0.1789(6) 0.6272(5) 0.0587(6) Uiso 0.535(6) 1 d PD A 2
H53C H 0.1324 0.1124 0.6349 0.070 Uiso 0.535(6) 1 calc PR A 2
H53D H 0.1734 0.2021 0.6792 0.070 Uiso 0.535(6) 1 calc PR A 2
C54' C 0.0941(3) 0.2285(6) 0.6074(5) 0.0587(6) Uiso 0.535(6) 1 d PD A 2
H54C H 0.0947 0.2565 0.6557 0.070 Uiso 0.535(6) 1 calc PR A 2
H54D H 0.0576 0.1900 0.5779 0.070 Uiso 0.535(6) 1 calc PR A 2
C55' C 0.0980(4) 0.3143(6) 0.5465(5) 0.0587(6) Uiso 0.535(6) 1 d PD A 2
H55C H 0.0579 0.3354 0.5051 0.070 Uiso 0.535(6) 1 calc PR A 2
H55D H 0.1214 0.3694 0.5781 0.070 Uiso 0.535(6) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0356(4) 0.0323(4) 0.0373(4) 0.000 0.0222(3) 0.000
O1 0.0496(13) 0.0462(15) 0.0400(13) -0.0023(11) 0.0187(11) 0.0052(10)
O2 0.0412(13) 0.0612(17) 0.0380(13) -0.0049(11) 0.0212(10) -0.0011(11)
O3 0.0582(15) 0.0500(16) 0.0514(15) 0.0025(12) 0.0324(13) -0.0022(12)
Li1 0.041(3) 0.047(3) 0.041(3) -0.002(2) 0.024(2) 0.004(2)
Li2 0.059(5) 0.039(5) 0.068(6) 0.000 0.042(5) 0.000
N1 0.0360(14) 0.0327(16) 0.0373(14) -0.0004(11) 0.0194(11) 0.0001(10)
N2 0.0359(14) 0.0355(16) 0.0437(16) -0.0028(12) 0.0242(12) -0.0008(10)
N3 0.0480(16) 0.0360(16) 0.0497(16) 0.0034(13) 0.0343(13) 0.0015(12)
C1 0.0287(15) 0.042(2) 0.0343(17) -0.0020(14) 0.0152(13) 0.0040(13)
C2 0.027(2) 0.038(3) 0.039(2) 0.000 0.0147(18) 0.000
C3 0.034(2) 0.038(3) 0.051(3) 0.000 0.020(2) 0.000
C4 0.0409(18) 0.0308(19) 0.061(2) -0.0066(17) 0.0201(16) 0.0000(14)
C5 0.0446(19) 0.045(2) 0.045(2) -0.0117(17) 0.0194(16) 0.0016(15)
C6 0.0427(18) 0.044(2) 0.0343(18) -0.0018(15) 0.0172(14) 0.0043(14)
C7 0.052(2) 0.062(3) 0.039(2) -0.0015(17) 0.0156(17) 0.0054(18)
C8 0.061(2) 0.064(3) 0.057(2) 0.011(2) 0.022(2) 0.009(2)
C9 0.095(3) 0.057(3) 0.067(3) 0.007(2) 0.032(3) 0.017(2)
C10 0.048(2) 0.046(2) 0.068(3) -0.0098(19) 0.0283(19) 0.0038(16)
C11 0.0400(19) 0.051(2) 0.053(2) -0.0069(17) 0.0251(16) 0.0019(15)
C12 0.058(2) 0.094(4) 0.071(3) -0.001(3) 0.042(2) -0.005(2)
C13 0.061(3) 0.231(8) 0.060(3) -0.004(4) 0.036(3) -0.008(4)
C14 0.052(2) 0.088(3) 0.039(2) -0.005(2) 0.0231(17) -0.003(2)
C15 0.0445(19) 0.0296(17) 0.054(2) -0.0068(15) 0.0340(17) -0.0010(13)
C16 0.047(2) 0.046(2) 0.057(2) -0.0137(18) 0.0303(18) -0.0064(15)
C17 0.045(2) 0.047(2) 0.077(3) -0.016(2) 0.0349(19) -0.0115(16)
C18 0.051(2) 0.045(2) 0.118(4) -0.005(2) 0.057(3) -0.0053(17)
C19 0.061(2) 0.037(2) 0.087(3) 0.007(2) 0.054(2) 0.0022(17)
C20 0.074(3) 0.070(3) 0.116(4) 0.034(3) 0.072(3) 0.015(2)
C21 0.099(4) 0.072(3) 0.095(4) 0.037(3) 0.077(3) 0.020(3)
C22 0.070(3) 0.055(2) 0.070(3) 0.022(2) 0.049(2) 0.0146(19)
C23 0.061(2) 0.0326(19) 0.057(2) 0.0043(16) 0.0413(19) 0.0047(15)
C24 0.049(2) 0.0323(18) 0.069(2) 0.0005(17) 0.0419(19) 0.0031(15)
C25 0.069(2) 0.041(2) 0.067(3) 0.0015(19) 0.043(2) -0.0024(18)
C26 0.082(4) 0.143(6) 0.107(4) -0.044(4) 0.053(3) -0.062(4)
C27 0.081(3) 0.071(3) 0.068(3) -0.018(3) 0.000(2) 0.020(3)
C28 0.148(5) 0.060(3) 0.051(3) -0.002(2) 0.031(3) 0.020(3)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N2 2.047(2) . ?
V1 N2 2.047(2) 2 ?
V1 N1 2.054(3) . ?
V1 N1 2.054(3) 2 ?
V1 N3 2.094(3) 2 ?
V1 N3 2.094(3) . ?
V1 Li2 2.741(9) . ?
V1 Li1 2.792(5) . ?
V1 Li1 2.792(5) 2 ?
O1 C7 1.432(4) . ?
O1 C10 1.435(4) . ?
O1 Li1 1.931(6) . ?
O2 C14 1.437(4) . ?
O2 C11 1.440(4) . ?
O2 Li1 1.945(6) . ?
O3 C28 1.399(5) . ?
O3 C25 1.427(4) . ?
O3 Li2 1.959(6) . ?
Li1 N2 2.113(6) . ?
Li1 N1 2.117(6) . ?
Li1 C15 2.685(7) . ?
Li1 C1 2.707(6) . ?
Li2 O3 1.959(6) 2 ?
Li2 N3 2.068(6) . ?
Li2 N3 2.068(6) 2 ?
N1 C1 1.378(4) . ?
N2 C15 1.387(4) . ?
N3 C23 1.393(4) . ?
C1 C6 1.407(4) . ?
C1 C2 1.451(4) . ?
C2 C3 1.428(7) . ?
C2 C1 1.451(4) 2 ?
C3 C4 1.417(4) . ?
C3 C4 1.417(4) 2 ?
C4 C5 1.368(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.384(5) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 C8 1.507(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.498(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.498(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.500(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.475(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.457(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.403(5) . ?
C15 C24 1.434(5) . ?
C16 C17 1.385(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.349(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.422(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.403(6) . ?
C19 C24 1.448(5) . ?
C20 C21 1.365(7) . ?
C20 H20A 0.9500 . ?
C21 C22 1.401(6) . ?
C21 H21A 0.9500 . ?
C22 C23 1.387(5) . ?
C22 H22A 0.9500 . ?
C23 C24 1.444(5) . ?
C25 C26 1.490(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.500(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.500(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
O51 C52 1.367(13) . ?
O51 C55 1.447(10) . ?
C52 C53 1.526(13) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.427(11) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.594(10) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
O51' C55' 1.398(9) . ?
O51' C52' 1.486(12) . ?
C52' C53' 1.528(11) . ?
C52' H52C 0.9900 . ?
C52' H52D 0.9900 . ?
C53' C54' 1.275(9) . ?
C53' H53C 0.9900 . ?
C53' H53D 0.9900 . ?
C54' C55' 1.712(10) . ?
C54' H54C 0.9900 . ?
C54' H54D 0.9900 . ?
C55' H55C 0.9900 . ?
C55' H55D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 V1 N2 163.06(15) . 2 ?
N2 V1 N1 97.46(10) . . ?
N2 V1 N1 95.19(10) 2 . ?
N2 V1 N1 95.19(10) . 2 ?
N2 V1 N1 97.46(10) 2 2 ?
N1 V1 N1 83.22(15) . 2 ?
N2 V1 N3 86.33(10) . 2 ?
N2 V1 N3 82.43(10) 2 2 ?
N1 V1 N3 172.56(10) . 2 ?
N1 V1 N3 90.08(10) 2 2 ?
N2 V1 N3 82.43(10) . . ?
N2 V1 N3 86.34(10) 2 . ?
N1 V1 N3 90.08(10) . . ?
N1 V1 N3 172.56(10) 2 . ?
N3 V1 N3 96.78(15) 2 . ?
N2 V1 Li2 81.53(7) . . ?
N2 V1 Li2 81.53(7) 2 . ?
N1 V1 Li2 138.39(7) . . ?
N1 V1 Li2 138.39(7) 2 . ?
N3 V1 Li2 48.39(7) 2 . ?
N3 V1 Li2 48.39(7) . . ?
N2 V1 Li1 48.88(13) . . ?
N2 V1 Li1 143.89(13) 2 . ?
N1 V1 Li1 48.95(13) . . ?
N1 V1 Li1 83.92(14) 2 . ?
N3 V1 Li1 133.67(13) 2 . ?
N3 V1 Li1 89.24(14) . . ?
Li2 V1 Li1 120.66(12) . . ?
N2 V1 Li1 143.89(13) . 2 ?
N2 V1 Li1 48.88(13) 2 2 ?
N1 V1 Li1 83.92(14) . 2 ?
N1 V1 Li1 48.95(13) 2 2 ?
N3 V1 Li1 89.24(14) 2 2 ?
N3 V1 Li1 133.67(13) . 2 ?
Li2 V1 Li1 120.66(12) . 2 ?
Li1 V1 Li1 118.7(2) . 2 ?
C7 O1 C10 109.8(3) . . ?
C7 O1 Li1 125.4(3) . . ?
C10 O1 Li1 124.4(3) . . ?
C14 O2 C11 109.4(3) . . ?
C14 O2 Li1 126.8(3) . . ?
C11 O2 Li1 120.4(2) . . ?
C28 O3 C25 109.7(3) . . ?
C28 O3 Li2 127.9(3) . . ?
C25 O3 Li2 122.1(2) . . ?
O1 Li1 O2 96.7(2) . . ?
O1 Li1 N2 109.3(3) . . ?
O2 Li1 N2 125.2(3) . . ?
O1 Li1 N1 126.2(3) . . ?
O2 Li1 N1 109.0(3) . . ?
N2 Li1 N1 93.5(2) . . ?
O1 Li1 C15 112.2(3) . . ?
O2 Li1 C15 94.9(2) . . ?
N2 Li1 C15 30.75(12) . . ?
N1 Li1 C15 111.7(2) . . ?
O1 Li1 C1 97.8(2) . . ?
O2 Li1 C1 106.9(2) . . ?
N2 Li1 C1 115.8(2) . . ?
N1 Li1 C1 30.15(12) . . ?
C15 Li1 C1 140.4(2) . . ?
O1 Li1 V1 127.7(2) . . ?
O2 Li1 V1 135.6(3) . . ?
N2 Li1 V1 46.85(12) . . ?
N1 Li1 V1 47.04(12) . . ?
C15 Li1 V1 70.98(15) . . ?
C1 Li1 V1 70.31(14) . . ?
O3 Li2 O3 96.7(4) . 2 ?
O3 Li2 N3 117.33(10) . . ?
O3 Li2 N3 114.14(10) 2 . ?
O3 Li2 N3 114.14(10) . 2 ?
O3 Li2 N3 117.33(10) 2 2 ?
N3 Li2 N3 98.4(4) . 2 ?
O3 Li2 V1 131.6(2) . . ?
O3 Li2 V1 131.6(2) 2 . ?
N3 Li2 V1 49.21(19) . . ?
N3 Li2 V1 49.21(19) 2 . ?
C1 N1 V1 133.7(2) . . ?
C1 N1 Li1 99.4(2) . . ?
V1 N1 Li1 84.01(17) . . ?
C15 N2 V1 134.9(2) . . ?
C15 N2 Li1 98.1(2) . . ?
V1 N2 Li1 84.27(17) . . ?
C23 N3 Li2 108.2(2) . . ?
C23 N3 V1 131.1(2) . . ?
Li2 N3 V1 82.4(2) . . ?
N1 C1 C6 120.6(3) . . ?
N1 C1 C2 121.9(3) . . ?
C6 C1 C2 117.4(3) . . ?
N1 C1 Li1 50.49(18) . . ?
C6 C1 Li1 119.5(2) . . ?
C2 C1 Li1 97.8(2) . . ?
C3 C2 C1 118.8(2) . . ?
C3 C2 C1 118.8(2) . 2 ?
C1 C2 C1 122.4(4) . 2 ?
C4 C3 C4 119.9(5) . 2 ?
C4 C3 C2 120.0(2) . . ?
C4 C3 C2 120.0(2) 2 . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 H5A 119.7 . . ?
C6 C5 H5A 119.7 . . ?
C5 C6 C1 122.6(3) . . ?
C5 C6 H6A 118.7 . . ?
C1 C6 H6A 118.7 . . ?
O1 C7 C8 104.5(3) . . ?
O1 C7 H7A 110.8 . . ?
C8 C7 H7A 110.8 . . ?
O1 C7 H7B 110.8 . . ?
C8 C7 H7B 110.8 . . ?
H7A C7 H7B 108.9 . . ?
C9 C8 C7 102.3(3) . . ?
C9 C8 H8A 111.3 . . ?
C7 C8 H8A 111.3 . . ?
C9 C8 H8B 111.3 . . ?
C7 C8 H8B 111.3 . . ?
H8A C8 H8B 109.2 . . ?
C8 C9 C10 104.3(4) . . ?
C8 C9 H9A 110.9 . . ?
C10 C9 H9A 110.9 . . ?
C8 C9 H9B 110.9 . . ?
C10 C9 H9B 110.9 . . ?
H9A C9 H9B 108.9 . . ?
O1 C10 C9 106.2(3) . . ?
O1 C10 H10A 110.5 . . ?
C9 C10 H10A 110.5 . . ?
O1 C10 H10B 110.5 . . ?
C9 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
O2 C11 C12 106.0(3) . . ?
O2 C11 H11A 110.5 . . ?
C12 C11 H11A 110.5 . . ?
O2 C11 H11B 110.5 . . ?
C12 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
C13 C12 C11 104.9(3) . . ?
C13 C12 H12A 110.8 . . ?
C11 C12 H12A 110.8 . . ?
C13 C12 H12B 110.8 . . ?
C11 C12 H12B 110.8 . . ?
H12A C12 H12B 108.8 . . ?
C14 C13 C12 105.5(4) . . ?
C14 C13 H13A 110.6 . . ?
C12 C13 H13A 110.6 . . ?
C14 C13 H13B 110.6 . . ?
C12 C13 H13B 110.6 . . ?
H13A C13 H13B 108.8 . . ?
O2 C14 C13 105.9(3) . . ?
O2 C14 H14A 110.6 . . ?
C13 C14 H14A 110.6 . . ?
O2 C14 H14B 110.6 . . ?
C13 C14 H14B 110.6 . . ?
H14A C14 H14B 108.7 . . ?
N2 C15 C16 120.3(3) . . ?
N2 C15 C24 121.1(3) . . ?
C16 C15 C24 118.5(3) . . ?
N2 C15 Li1 51.19(18) . . ?
C16 C15 Li1 117.6(3) . . ?
C24 C15 Li1 98.5(2) . . ?
C17 C16 C15 122.4(4) . . ?
C17 C16 H16A 118.8 . . ?
C15 C16 H16A 118.8 . . ?
C18 C17 C16 120.0(4) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C19 121.8(3) . . ?
C17 C18 H18A 119.1 . . ?
C19 C18 H18A 119.1 . . ?
C20 C19 C18 121.4(4) . . ?
C20 C19 C24 119.8(4) . . ?
C18 C19 C24 118.8(4) . . ?
C21 C20 C19 120.4(4) . . ?
C21 C20 H20A 119.8 . . ?
C19 C20 H20A 119.8 . . ?
C20 C21 C22 121.1(4) . . ?
C20 C21 H21A 119.5 . . ?
C22 C21 H21A 119.5 . . ?
C23 C22 C21 121.5(4) . . ?
C23 C22 H22A 119.3 . . ?
C21 C22 H22A 119.3 . . ?
C22 C23 N3 120.3(3) . . ?
C22 C23 C24 118.7(3) . . ?
N3 C23 C24 121.0(3) . . ?
C15 C24 C23 123.6(3) . . ?
C15 C24 C19 118.1(3) . . ?
C23 C24 C19 118.2(3) . . ?
O3 C25 C26 106.9(4) . . ?
O3 C25 H25A 110.3 . . ?
C26 C25 H25A 110.3 . . ?
O3 C25 H25B 110.3 . . ?
C26 C25 H25B 110.3 . . ?
H25A C25 H25B 108.6 . . ?
C25 C26 C27 105.3(4) . . ?
C25 C26 H26A 110.7 . . ?
C27 C26 H26A 110.7 . . ?
C25 C26 H26B 110.7 . . ?
C27 C26 H26B 110.7 . . ?
H26A C26 H26B 108.8 . . ?
C26 C27 C28 103.1(4) . . ?
C26 C27 H27A 111.1 . . ?
C28 C27 H27A 111.1 . . ?
C26 C27 H27B 111.1 . . ?
C28 C27 H27B 111.1 . . ?
H27A C27 H27B 109.1 . . ?
O3 C28 C27 105.7(4) . . ?
O3 C28 H28A 110.6 . . ?
C27 C28 H28A 110.6 . . ?
O3 C28 H28B 110.6 . . ?
C27 C28 H28B 110.6 . . ?
H28A C28 H28B 108.7 . . ?
C52 O51 C55 106.7(7) . . ?
O51 C52 C53 109.9(9) . . ?
O51 C52 H52A 109.7 . . ?
C53 C52 H52A 109.7 . . ?
O51 C52 H52B 109.7 . . ?
C53 C52 H52B 109.7 . . ?
H52A C52 H52B 108.2 . . ?
C54 C53 C52 107.0(7) . . ?
C54 C53 H53A 110.3 . . ?
C52 C53 H53A 110.3 . . ?
C54 C53 H53B 110.3 . . ?
C52 C53 H53B 110.3 . . ?
H53A C53 H53B 108.6 . . ?
C53 C54 C55 102.1(6) . . ?
C53 C54 H54A 111.3 . . ?
C55 C54 H54A 111.3 . . ?
C53 C54 H54B 111.3 . . ?
C55 C54 H54B 111.3 . . ?
H54A C54 H54B 109.2 . . ?
O51 C55 C54 104.6(6) . . ?
O51 C55 H55A 110.8 . . ?
C54 C55 H55A 110.8 . . ?
O51 C55 H55B 110.8 . . ?
C54 C55 H55B 110.8 . . ?
H55A C55 H55B 108.9 . . ?
C55' O51' C52' 110.4(6) . . ?
O51' C52' C53' 104.2(7) . . ?
O51' C52' H52C 110.9 . . ?
C53' C52' H52C 110.9 . . ?
O51' C52' H52D 110.9 . . ?
C53' C52' H52D 110.9 . . ?
H52C C52' H52D 108.9 . . ?
C54' C53' C52' 111.7(7) . . ?
C54' C53' H53C 109.3 . . ?
C52' C53' H53C 109.3 . . ?
C54' C53' H53D 109.3 . . ?
C52' C53' H53D 109.3 . . ?
H53C C53' H53D 107.9 . . ?
C53' C54' C55' 103.5(6) . . ?
C53' C54' H54C 111.1 . . ?
C55' C54' H54C 111.1 . . ?
C53' C54' H54D 111.1 . . ?
C55' C54' H54D 111.1 . . ?
H54C C54' H54D 109.0 . . ?
O51' C55' C54' 100.7(5) . . ?
O51' C55' H55C 111.6 . . ?
C54' C55' H55C 111.6 . . ?
O51' C55' H55D 111.6 . . ?
C54' C55' H55D 111.6 . . ?
H55C C55' H55D 109.4 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 943107'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p21

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
; 
 'C36 H36 N12 Ni6, C40 H41 Li N12 O Ni6 2-,
  2(C16 H32 Li O4 1+), 5(C4 H8 O)'
;
_chemical_formula_sum            'C128 H181 Li3 N24 Ni12 O14'
_chemical_formula_weight         3005.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.2275(3)
_cell_length_b                   17.0537(7)
_cell_length_c                   16.5692(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.948(3)
_cell_angle_gamma                90.00
_cell_volume                     3717.5(2)
_cell_formula_units_Z            1

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1574
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 The data were rather diffuse and of limited resolution due to the
 superimposition of complexes 5a and 5b2-. Therefore the data were 
 truncated at 0.92\%A. Ligands and thf molecules were treated 
 with similar distance and similar U restraints during the refinement. 
 However, the diffuse character of the electron density did not allow 
 the refinement of disordered atoms over split positions. All atoms 
 were refined isotropically, except Ni atoms which were treated 
 anisotropically. Hydrogen atoms were not considered in the refinement. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_measurement_device_type  'Beamline I19, Diamond Light Source'
_diffrn_measurement_method       /w-scans
_diffrn_reflns_number            27906
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_sigmaI/netI    0.1202
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         22.75
_reflns_number_total             10066
_reflns_number_gt                4604
_reflns_threshold_expression     >2sigma(I)

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(8)
_refine_ls_number_reflns         10066
_refine_ls_number_parameters     396
_refine_ls_number_restraints     1070
_refine_ls_R_factor_all          0.2344
_refine_ls_R_factor_gt           0.1384
_refine_ls_wR_factor_ref         0.3662
_refine_ls_wR_factor_gt          0.3256
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.76388(17) 0.0932(4) 0.12874(14) 0.0887(9) Uani 1 1 d . . .
Ni2 Ni 0.70468(17) 0.0907(4) 0.36140(14) 0.0976(10) Uani 1 1 d . . .
Ni3 Ni 0.8353(2) 0.1750(3) 0.2702(2) 0.0891(13) Uani 1 1 d . . .
Ni4 Ni 0.8377(3) 0.0100(3) 0.2687(3) 0.0962(14) Uani 1 1 d . . .
Ni5 Ni 0.6306(3) 0.1701(4) 0.2192(3) 0.1233(17) Uani 1 1 d . . .
Ni6 Ni 0.6332(6) 0.0184(4) 0.2210(4) 0.177(3) Uani 1 1 d . . .
N11 N 0.8647(13) 0.1662(8) 0.1566(10) 0.065(5) Uiso 1 1 d DU . .
C11 C 0.8405(19) 0.2397(10) 0.1227(13) 0.090(8) Uiso 1 1 d DU . .
C12 C 0.881(2) 0.2682(12) 0.0516(14) 0.097(9) Uiso 1 1 d DU . .
C13 C 0.854(2) 0.3466(12) 0.0240(14) 0.101(8) Uiso 1 1 d DU . .
C14 C 0.793(3) 0.3905(15) 0.0701(18) 0.149(12) Uiso 1 1 d DU . .
C15 C 0.757(3) 0.3650(13) 0.1458(17) 0.126(11) Uiso 1 1 d DU . .
C16 C 0.779(2) 0.2868(12) 0.1695(16) 0.116(10) Uiso 1 1 d DU . .
N12 N 0.7403(14) 0.2495(11) 0.2352(11) 0.078(6) Uiso 1 1 d DU . .
N21 N 0.8637(17) 0.0060(10) 0.1567(13) 0.087(7) Uiso 1 1 d DU . .
C21 C 0.851(2) -0.0694(11) 0.1290(14) 0.097(9) Uiso 1 1 d DU . .
C22 C 0.892(2) -0.0994(14) 0.0599(16) 0.118(11) Uiso 1 1 d DU . .
C23 C 0.880(3) -0.1821(15) 0.045(2) 0.150(13) Uiso 1 1 d DU . .
C24 C 0.811(3) -0.2283(15) 0.082(2) 0.168(15) Uiso 1 1 d DU . .
C25 C 0.759(3) -0.1961(15) 0.146(2) 0.173(16) Uiso 1 1 d DU . .
C26 C 0.782(2) -0.1164(13) 0.1679(16) 0.120(10) Uiso 1 1 d DU . .
N22 N 0.7543(17) -0.0871(13) 0.2404(12) 0.110(9) Uiso 1 1 d DU . .
N31 N 0.6672(13) 0.0025(10) 0.1003(11) 0.082(6) Uiso 1 1 d DU . .
C31 C 0.5915(16) 0.0399(10) 0.0506(15) 0.098(8) Uiso 1 1 d DU . .
C32 C 0.514(2) -0.0054(12) 0.005(2) 0.140(12) Uiso 1 1 d DU . .
C33 C 0.4368(19) 0.0441(15) -0.0366(19) 0.135(11) Uiso 1 1 d DU . .
C34 C 0.4460(14) 0.1243(12) -0.0478(12) 0.078(7) Uiso 1 1 d DU . .
C35 C 0.5136(15) 0.1697(11) 0.0063(13) 0.086(7) Uiso 1 1 d DU . .
C36 C 0.5849(12) 0.1213(9) 0.0546(11) 0.065(6) Uiso 1 1 d DU . .
N32 N 0.6605(11) 0.1564(9) 0.1048(9) 0.061(5) Uiso 1 1 d DU . .
N41 N 0.9318(10) 0.0868(14) 0.2962(7) 0.079(4) Uiso 1 1 d DU . .
C41 C 0.9605(11) 0.0964(15) 0.3773(8) 0.079(5) Uiso 1 1 d DU . .
C42 C 1.0556(14) 0.0677(15) 0.4112(11) 0.114(9) Uiso 1 1 d DU . .
C43 C 1.0761(15) 0.0779(16) 0.4973(11) 0.104(7) Uiso 1 1 d DU . .
C44 C 1.0139(17) 0.1268(15) 0.5372(12) 0.123(9) Uiso 1 1 d DU . .
C45 C 0.9160(17) 0.1561(16) 0.5032(11) 0.119(9) Uiso 1 1 d DU . .
C46 C 0.8911(13) 0.1367(13) 0.4200(10) 0.089(7) Uiso 1 1 d DU . .
N42 N 0.8036(11) 0.1669(11) 0.3764(10) 0.073(5) Uiso 1 1 d DU . .
N51 N 0.5194(9) 0.0946(14) 0.2096(7) 0.073(4) Uiso 1 1 d DU . .
C51 C 0.4596(11) 0.1058(13) 0.2732(9) 0.080(6) Uiso 1 1 d DU . .
C52 C 0.3605(12) 0.0734(13) 0.2730(10) 0.089(7) Uiso 1 1 d DU . .
C53 C 0.3044(13) 0.0865(19) 0.3410(12) 0.106(7) Uiso 1 1 d DU . .
C54 C 0.3497(16) 0.1300(16) 0.4037(14) 0.126(10) Uiso 1 1 d DU . .
C55 C 0.4531(15) 0.1576(15) 0.4091(12) 0.111(8) Uiso 1 1 d DU . .
C56 C 0.5092(11) 0.1405(12) 0.3434(10) 0.077(6) Uiso 1 1 d DU . .
N52 N 0.6090(11) 0.1647(11) 0.3384(10) 0.074(5) Uiso 1 1 d DU . .
N61 N 0.8027(13) -0.0068(11) 0.3887(13) 0.092(7) Uiso 1 1 d DU . .
C61 C 0.7470(14) -0.0733(12) 0.4077(17) 0.119(9) Uiso 1 1 d DU . .
C62 C 0.7936(19) -0.1392(16) 0.450(2) 0.160(12) Uiso 1 1 d DU . .
C63 C 0.730(2) -0.200(2) 0.477(3) 0.228(18) Uiso 1 1 d DU . .
C64 C 0.628(2) -0.2015(15) 0.445(2) 0.173(14) Uiso 1 1 d DU . .
C65 C 0.5790(18) -0.1341(15) 0.406(2) 0.146(11) Uiso 1 1 d DU . .
C66 C 0.6418(13) -0.0708(11) 0.3862(15) 0.101(8) Uiso 1 1 d DU . .
N62 N 0.6068(13) -0.0061(11) 0.3411(12) 0.090(7) Uiso 1 1 d DU . .
Li1 Li 0.244(6) -0.269(5) 0.245(4) 0.17(2) Uiso 1 1 d . . .
O1 O 0.085(3) -0.165(2) 0.2280(19) 0.276(16) Uiso 1 1 d DU . .
C110 C 0.055(4) -0.1056(17) 0.282(3) 0.27(2) Uiso 1 1 d DU . .
C120 C 0.025(3) -0.150(3) 0.351(2) 0.185(15) Uiso 1 1 d DU . .
C130 C 0.003(3) -0.222(3) 0.317(3) 0.252(19) Uiso 1 1 d DU . .
C140 C 0.100(3) -0.2334(18) 0.280(2) 0.171(14) Uiso 1 1 d DU . .
O2 O 0.333(2) -0.1971(16) 0.218(2) 0.202(11) Uiso 1 1 d DU . .
C210 C 0.352(3) -0.171(3) 0.1395(19) 0.207(17) Uiso 1 1 d DU . .
C220 C 0.413(4) -0.099(2) 0.149(3) 0.232(19) Uiso 1 1 d DU . .
C230 C 0.473(3) -0.115(3) 0.219(3) 0.25(2) Uiso 1 1 d DU . .
C240 C 0.392(4) -0.141(3) 0.267(2) 0.28(2) Uiso 1 1 d DU . .
O3 O 0.209(2) -0.3355(16) 0.1674(16) 0.186(10) Uiso 1 1 d DU . .
C310 C 0.234(3) -0.357(3) 0.089(2) 0.207(16) Uiso 1 1 d DU . .
C320 C 0.167(5) -0.425(3) 0.070(3) 0.37(3) Uiso 1 1 d DU . .
C330 C 0.077(4) -0.392(4) 0.082(3) 0.31(2) Uiso 1 1 d DU . .
C340 C 0.102(3) -0.349(4) 0.157(3) 0.31(2) Uiso 1 1 d DU . .
O4 O 0.286(2) -0.342(2) 0.330(2) 0.235(13) Uiso 1 1 d DU . .
C410 C 0.309(5) -0.310(3) 0.411(3) 0.33(2) Uiso 1 1 d DU . .
C420 C 0.395(4) -0.361(5) 0.439(3) 0.34(3) Uiso 1 1 d DU . .
C430 C 0.366(5) -0.433(3) 0.413(4) 0.31(2) Uiso 1 1 d DU . .
C440 C 0.273(4) -0.421(2) 0.358(3) 0.31(2) Uiso 1 1 d DU . .
O5 O 1.0848(16) 0.0881(19) 0.1448(14) 0.185(8) Uiso 1 1 d DU . .
C510 C 1.137(3) 0.1622(18) 0.146(2) 0.173(13) Uiso 1 1 d DU . .
C520 C 1.227(2) 0.154(2) 0.103(2) 0.160(12) Uiso 1 1 d DU . .
C530 C 1.214(2) 0.088(3) 0.0591(19) 0.185(12) Uiso 1 1 d DU . .
C540 C 1.113(3) 0.060(2) 0.068(2) 0.27(2) Uiso 1 1 d DU . .
O6 O 0.510(3) 0.2895(19) 0.182(2) 0.233(14) Uiso 1 1 d DU . .
C610 C 0.534(3) 0.369(3) 0.207(3) 0.28(2) Uiso 1 1 d DU . .
C620 C 0.439(4) 0.413(2) 0.189(3) 0.225(19) Uiso 1 1 d DU . .
C630 C 0.389(3) 0.373(3) 0.127(4) 0.28(2) Uiso 1 1 d DU . .
C640 C 0.463(4) 0.316(3) 0.103(2) 0.30(2) Uiso 1 1 d DU . .
O7 O 0.643(5) 0.303(4) 0.421(6) 0.53(3) Uiso 1 1 d DU . .
C710 C 0.635(7) 0.376(6) 0.462(5) 0.50(4) Uiso 1 1 d DU . .
C720 C 0.738(9) 0.409(4) 0.464(6) 0.45(4) Uiso 1 1 d DU . .
C730 C 0.771(5) 0.386(6) 0.393(8) 0.44(4) Uiso 1 1 d DU . .
C740 C 0.690(9) 0.336(6) 0.354(3) 0.53(4) Uiso 1 1 d DU . .
Li2 Li 0.9582(14) 0.0858(13) 0.1869(11) 0.12(10) Uiso 0.13 1 d PD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0613(14) 0.141(2) 0.0649(14) 0.006(3) 0.0136(11) 0.000(3)
Ni2 0.0577(14) 0.171(3) 0.0651(15) -0.004(3) 0.0121(11) -0.017(3)
Ni3 0.050(2) 0.148(4) 0.070(3) 0.001(3) 0.0084(18) 0.002(2)
Ni4 0.061(2) 0.145(4) 0.084(3) -0.014(3) 0.017(2) -0.004(2)
Ni5 0.070(2) 0.196(5) 0.104(3) 0.017(4) 0.011(2) -0.020(3)
Ni6 0.174(6) 0.195(6) 0.162(6) 0.003(5) 0.026(5) -0.045(5)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N32 1.754(15) . ?
Ni1 N11 1.847(18) . ?
Ni1 N21 2.01(2) . ?
Ni1 N31 2.031(18) . ?
Ni1 Li2 2.653(19) . ?
Ni1 Ni6 2.737(7) . ?
Ni1 Ni5 2.762(6) . ?
Ni1 Ni4 2.806(5) . ?
Ni1 Ni3 2.807(5) . ?
Ni2 N52 1.800(18) . ?
Ni2 N42 1.843(18) . ?
Ni2 N62 2.10(2) . ?
Ni2 N61 2.13(2) . ?
Ni2 Ni6 2.715(8) . ?
Ni2 Ni5 2.805(6) . ?
Ni2 Ni3 2.806(5) . ?
Ni2 Ni4 2.813(5) . ?
Ni3 N12 1.837(18) . ?
Ni3 N42 1.856(17) . ?
Ni3 N11 1.969(17) . ?
Ni3 N41 1.99(2) . ?
Ni3 Li2 2.71(2) . ?
Ni3 Ni5 2.753(5) . ?
Ni3 Ni4 2.815(4) . ?
Ni4 N41 1.83(2) . ?
Ni4 N21 1.92(2) . ?
Ni4 N22 2.02(2) . ?
Ni4 N61 2.11(2) . ?
Ni4 Li2 2.55(2) . ?
Ni4 Ni6 2.742(9) . ?
Ni5 N51 1.949(18) . ?
Ni5 N12 1.98(2) . ?
Ni5 N32 1.991(17) . ?
Ni5 N52 2.026(18) . ?
Ni5 Ni6 2.587(7) . ?
Ni6 N51 1.983(19) . ?
Ni6 N62 2.10(2) . ?
Ni6 N31 2.11(2) . ?
Ni6 N22 2.41(2) . ?
N11 C11 1.397(13) . ?
N11 Li2 1.879(16) . ?
C11 C16 1.427(16) . ?
C11 C12 1.429(14) . ?
C12 C13 1.447(15) . ?
C13 C14 1.387(19) . ?
C14 C15 1.450(16) . ?
C15 C16 1.412(15) . ?
C16 N12 1.403(14) . ?
N21 C21 1.371(13) . ?
N21 Li2 1.880(16) . ?
C21 C26 1.410(16) . ?
C21 C22 1.417(15) . ?
C22 C23 1.439(16) . ?
C23 C24 1.390(19) . ?
C24 C25 1.431(16) . ?
C25 C26 1.431(15) . ?
C26 N22 1.388(14) . ?
N31 C31 1.384(13) . ?
C31 C36 1.393(16) . ?
C31 C32 1.434(15) . ?
C32 C33 1.445(16) . ?
C33 C34 1.386(18) . ?
C34 C35 1.427(15) . ?
C35 C36 1.433(14) . ?
C36 N32 1.370(12) . ?
N41 C41 1.367(12) . ?
N41 Li2 1.880(16) . ?
C41 C46 1.398(16) . ?
C41 C42 1.410(14) . ?
C42 C43 1.435(15) . ?
C43 C44 1.387(19) . ?
C44 C45 1.446(15) . ?
C45 C46 1.422(15) . ?
C46 N42 1.397(13) . ?
N51 C51 1.395(13) . ?
C51 C56 1.404(16) . ?
C51 C52 1.423(14) . ?
C52 C53 1.430(15) . ?
C53 C54 1.363(19) . ?
C54 C55 1.440(15) . ?
C55 C56 1.412(15) . ?
C56 N52 1.393(13) . ?
N61 C61 1.405(14) . ?
C61 C66 1.401(17) . ?
C61 C62 1.432(15) . ?
C62 C63 1.437(16) . ?
C63 C64 1.40(2) . ?
C64 C65 1.434(16) . ?
C65 C66 1.422(15) . ?
C66 N62 1.385(14) . ?
Li1 O3 1.75(8) . ?
Li1 O2 1.79(8) . ?
Li1 O4 1.92(8) . ?
Li1 C140 2.13(8) . ?
Li1 C340 2.64(9) . ?
O1 C110 1.436(19) . ?
O1 C140 1.44(2) . ?
C110 C120 1.47(2) . ?
C120 C130 1.36(3) . ?
C130 C140 1.50(2) . ?
O2 C210 1.42(2) . ?
O2 C240 1.43(2) . ?
C210 C220 1.46(2) . ?
C220 C230 1.36(3) . ?
C230 C240 1.48(2) . ?
O3 C310 1.42(2) . ?
O3 C340 1.43(2) . ?
C310 C320 1.48(2) . ?
C320 C330 1.36(3) . ?
C330 C340 1.46(2) . ?
O4 C440 1.44(2) . ?
O4 C410 1.45(2) . ?
C410 C420 1.48(2) . ?
C420 C430 1.35(3) . ?
C430 C440 1.47(2) . ?
O5 C540 1.44(2) . ?
O5 C510 1.44(2) . ?
O5 Li2 1.879(14) . ?
C510 C520 1.45(2) . ?
C520 C530 1.34(3) . ?
C530 C540 1.44(2) . ?
O6 C610 1.44(2) . ?
O6 C640 1.45(2) . ?
C610 C620 1.46(2) . ?
C620 C630 1.35(3) . ?
C630 C640 1.47(2) . ?
O7 C740 1.44(2) . ?
O7 C710 1.45(2) . ?
C710 C720 1.47(2) . ?
C720 C730 1.35(3) . ?
C730 C740 1.46(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N32 Ni1 N11 99.7(7) . . ?
N32 Ni1 N21 170.0(7) . . ?
N11 Ni1 N21 90.0(6) . . ?
N32 Ni1 N31 87.6(6) . . ?
N11 Ni1 N31 172.7(7) . . ?
N21 Ni1 N31 82.7(7) . . ?
N32 Ni1 Li2 144.5(7) . . ?
N11 Ni1 Li2 45.1(4) . . ?
N21 Ni1 Li2 45.0(4) . . ?
N31 Ni1 Li2 127.7(7) . . ?
N32 Ni1 Ni6 83.7(6) . . ?
N11 Ni1 Ni6 131.0(5) . . ?
N21 Ni1 Ni6 88.0(6) . . ?
N31 Ni1 Ni6 49.9(6) . . ?
Li2 Ni1 Ni6 114.8(5) . . ?
N32 Ni1 Ni5 45.9(5) . . ?
N11 Ni1 Ni5 91.7(5) . . ?
N21 Ni1 Ni5 131.9(6) . . ?
N31 Ni1 Ni5 93.8(5) . . ?
Li2 Ni1 Ni5 118.3(4) . . ?
Ni6 Ni1 Ni5 56.12(15) . . ?
N32 Ni1 Ni4 134.0(5) . . ?
N11 Ni1 Ni4 87.4(5) . . ?
N21 Ni1 Ni4 43.2(6) . . ?
N31 Ni1 Ni4 87.9(5) . . ?
Li2 Ni1 Ni4 55.6(4) . . ?
Ni6 Ni1 Ni4 59.3(2) . . ?
Ni5 Ni1 Ni4 88.78(14) . . ?
N32 Ni1 Ni3 94.0(5) . . ?
N11 Ni1 Ni3 44.3(5) . . ?
N21 Ni1 Ni3 91.1(6) . . ?
N31 Ni1 Ni3 136.2(6) . . ?
Li2 Ni1 Ni3 59.4(4) . . ?
Ni6 Ni1 Ni3 86.70(18) . . ?
Ni5 Ni1 Ni3 59.25(14) . . ?
Ni4 Ni1 Ni3 60.20(10) . . ?
N52 Ni2 N42 90.5(7) . . ?
N52 Ni2 N62 96.2(6) . . ?
N42 Ni2 N62 172.7(7) . . ?
N52 Ni2 N61 172.9(7) . . ?
N42 Ni2 N61 96.6(6) . . ?
N62 Ni2 N61 76.8(7) . . ?
N52 Ni2 Ni6 87.8(5) . . ?
N42 Ni2 Ni6 128.0(5) . . ?
N62 Ni2 Ni6 49.7(6) . . ?
N61 Ni2 Ni6 88.7(6) . . ?
N52 Ni2 Ni5 46.1(5) . . ?
N42 Ni2 Ni5 87.4(5) . . ?
N62 Ni2 Ni5 95.1(5) . . ?
N61 Ni2 Ni5 135.1(6) . . ?
Ni6 Ni2 Ni5 55.87(15) . . ?
N52 Ni2 Ni3 89.1(5) . . ?
N42 Ni2 Ni3 40.8(5) . . ?
N62 Ni2 Ni3 136.0(6) . . ?
N61 Ni2 Ni3 96.9(5) . . ?
Ni6 Ni2 Ni3 87.15(17) . . ?
Ni5 Ni2 Ni3 58.76(14) . . ?
N52 Ni2 Ni4 133.9(5) . . ?
N42 Ni2 Ni4 86.7(5) . . ?
N62 Ni2 Ni4 86.5(6) . . ?
N61 Ni2 Ni4 48.1(6) . . ?
Ni6 Ni2 Ni4 59.5(2) . . ?
Ni5 Ni2 Ni4 87.79(15) . . ?
Ni3 Ni2 Ni4 60.12(10) . . ?
N12 Ni3 N42 97.9(7) . . ?
N12 Ni3 N11 87.0(7) . . ?
N42 Ni3 N11 171.2(8) . . ?
N12 Ni3 N41 173.0(8) . . ?
N42 Ni3 N41 86.6(6) . . ?
N11 Ni3 N41 87.8(6) . . ?
N12 Ni3 Li2 130.9(7) . . ?
N42 Ni3 Li2 130.4(6) . . ?
N11 Ni3 Li2 43.9(4) . . ?
N41 Ni3 Li2 43.9(4) . . ?
N12 Ni3 Ni5 46.0(6) . . ?
N42 Ni3 Ni5 88.7(5) . . ?
N11 Ni3 Ni5 89.4(6) . . ?
N41 Ni3 Ni5 129.2(6) . . ?
Li2 Ni3 Ni5 116.7(4) . . ?
N12 Ni3 Ni2 94.9(5) . . ?
N42 Ni3 Ni2 40.5(6) . . ?
N11 Ni3 Ni2 132.0(5) . . ?
N41 Ni3 Ni2 85.0(5) . . ?
Li2 Ni3 Ni2 115.0(5) . . ?
Ni5 Ni3 Ni2 60.59(14) . . ?
N12 Ni3 Ni1 85.4(6) . . ?
N42 Ni3 Ni1 131.7(6) . . ?
N11 Ni3 Ni1 41.0(5) . . ?
N41 Ni3 Ni1 87.6(5) . . ?
Li2 Ni3 Ni1 57.5(4) . . ?
Ni5 Ni3 Ni1 59.55(15) . . ?
Ni2 Ni3 Ni1 91.26(16) . . ?
N12 Ni3 Ni4 134.1(7) . . ?
N42 Ni3 Ni4 86.5(6) . . ?
N11 Ni3 Ni4 84.9(5) . . ?
N41 Ni3 Ni4 40.4(6) . . ?
Li2 Ni3 Ni4 54.9(5) . . ?
Ni5 Ni3 Ni4 88.8(2) . . ?
Ni2 Ni3 Ni4 60.05(17) . . ?
Ni1 Ni3 Ni4 59.89(17) . . ?
N41 Ni4 N21 94.7(7) . . ?
N41 Ni4 N22 170.3(9) . . ?
N21 Ni4 N22 84.0(7) . . ?
N41 Ni4 N61 94.2(6) . . ?
N21 Ni4 N61 169.8(7) . . ?
N22 Ni4 N61 86.5(7) . . ?
N41 Ni4 Li2 47.4(5) . . ?
N21 Ni4 Li2 47.2(5) . . ?
N22 Ni4 Li2 130.5(7) . . ?
N61 Ni4 Li2 141.4(7) . . ?
N41 Ni4 Ni6 131.2(6) . . ?
N21 Ni4 Ni6 89.6(7) . . ?
N22 Ni4 Ni6 58.5(7) . . ?
N61 Ni4 Ni6 88.4(5) . . ?
Li2 Ni4 Ni6 118.2(5) . . ?
N41 Ni4 Ni1 90.8(6) . . ?
N21 Ni4 Ni1 45.7(7) . . ?
N22 Ni4 Ni1 95.0(7) . . ?
N61 Ni4 Ni1 139.2(5) . . ?
Li2 Ni4 Ni1 59.2(4) . . ?
Ni6 Ni4 Ni1 59.11(18) . . ?
N41 Ni4 Ni2 87.8(5) . . ?
N21 Ni4 Ni2 136.8(7) . . ?
N22 Ni4 Ni2 99.8(6) . . ?
N61 Ni4 Ni2 48.7(5) . . ?
Li2 Ni4 Ni2 120.2(5) . . ?
Ni6 Ni4 Ni2 58.49(18) . . ?
Ni1 Ni4 Ni2 91.15(16) . . ?
N41 Ni4 Ni3 44.8(6) . . ?
N21 Ni4 Ni3 92.7(5) . . ?
N22 Ni4 Ni3 144.7(7) . . ?
N61 Ni4 Ni3 97.1(6) . . ?
Li2 Ni4 Ni3 60.4(5) . . ?
Ni6 Ni4 Ni3 86.5(2) . . ?
Ni1 Ni4 Ni3 59.92(17) . . ?
Ni2 Ni4 Ni3 59.83(17) . . ?
N51 Ni5 N12 176.4(7) . . ?
N51 Ni5 N32 93.9(6) . . ?
N12 Ni5 N32 89.5(6) . . ?
N51 Ni5 N52 82.4(6) . . ?
N12 Ni5 N52 94.4(7) . . ?
N32 Ni5 N52 170.0(7) . . ?
N51 Ni5 Ni6 49.4(6) . . ?
N12 Ni5 Ni6 132.2(6) . . ?
N32 Ni5 Ni6 83.7(5) . . ?
N52 Ni5 Ni6 86.9(6) . . ?
N51 Ni5 Ni3 139.1(6) . . ?
N12 Ni5 Ni3 41.8(5) . . ?
N32 Ni5 Ni3 90.5(4) . . ?
N52 Ni5 Ni3 86.3(4) . . ?
Ni6 Ni5 Ni3 90.9(3) . . ?
N51 Ni5 Ni1 99.2(5) . . ?
N12 Ni5 Ni1 84.1(5) . . ?
N32 Ni5 Ni1 39.3(4) . . ?
N52 Ni5 Ni1 132.0(6) . . ?
Ni6 Ni5 Ni1 61.5(2) . . ?
Ni3 Ni5 Ni1 61.19(14) . . ?
N51 Ni5 Ni2 86.8(5) . . ?
N12 Ni5 Ni2 91.7(5) . . ?
N32 Ni5 Ni2 131.1(5) . . ?
N52 Ni5 Ni2 39.8(5) . . ?
Ni6 Ni5 Ni2 60.3(2) . . ?
Ni3 Ni5 Ni2 60.65(14) . . ?
Ni1 Ni5 Ni2 92.25(18) . . ?
N51 Ni6 N62 91.2(7) . . ?
N51 Ni6 N31 103.2(6) . . ?
N62 Ni6 N31 161.0(8) . . ?
N51 Ni6 N22 171.9(8) . . ?
N62 Ni6 N22 84.2(7) . . ?
N31 Ni6 N22 80.0(6) . . ?
N51 Ni6 Ni5 48.3(6) . . ?
N62 Ni6 Ni5 101.9(6) . . ?
N31 Ni6 Ni5 97.0(5) . . ?
N22 Ni6 Ni5 139.2(6) . . ?
N51 Ni6 Ni2 88.7(5) . . ?
N62 Ni6 Ni2 49.8(6) . . ?
N31 Ni6 Ni2 141.3(6) . . ?
N22 Ni6 Ni2 93.3(6) . . ?
Ni5 Ni6 Ni2 63.8(2) . . ?
N51 Ni6 Ni1 99.1(6) . . ?
N62 Ni6 Ni1 143.0(6) . . ?
N31 Ni6 Ni1 47.4(5) . . ?
N22 Ni6 Ni1 88.5(5) . . ?
Ni5 Ni6 Ni1 62.4(2) . . ?
Ni2 Ni6 Ni1 94.8(2) . . ?
N51 Ni6 Ni4 141.1(6) . . ?
N62 Ni6 Ni4 88.4(5) . . ?
N31 Ni6 Ni4 88.1(5) . . ?
N22 Ni6 Ni4 45.6(5) . . ?
Ni5 Ni6 Ni4 93.9(3) . . ?
Ni2 Ni6 Ni4 62.05(19) . . ?
Ni1 Ni6 Ni4 61.61(19) . . ?
C11 N11 Ni1 112.0(16) . . ?
C11 N11 Li2 151.5(17) . . ?
Ni1 N11 Li2 90.8(9) . . ?
C11 N11 Ni3 104.8(11) . . ?
Ni1 N11 Ni3 94.7(7) . . ?
Li2 N11 Ni3 89.4(9) . . ?
N11 C11 C16 113.9(12) . . ?
N11 C11 C12 123.2(14) . . ?
C16 C11 C12 122.7(13) . . ?
C11 C12 C13 118.2(14) . . ?
C14 C13 C12 117.7(15) . . ?
C13 C14 C15 124.9(16) . . ?
C16 C15 C14 116.7(15) . . ?
N12 C16 C15 124.3(15) . . ?
N12 C16 C11 116.2(13) . . ?
C15 C16 C11 119.4(13) . . ?
C16 N12 Ni3 105.3(13) . . ?
C16 N12 Ni5 121.9(19) . . ?
Ni3 N12 Ni5 92.1(8) . . ?
C21 N21 Li2 146(2) . . ?
C21 N21 Ni4 109.1(13) . . ?
Li2 N21 Ni4 84.1(9) . . ?
C21 N21 Ni1 124.0(19) . . ?
Li2 N21 Ni1 85.9(9) . . ?
Ni4 N21 Ni1 91.0(8) . . ?
N21 C21 C26 116.4(13) . . ?
N21 C21 C22 124.2(15) . . ?
C26 C21 C22 119.1(13) . . ?
C21 C22 C23 116.4(16) . . ?
C24 C23 C22 123.3(17) . . ?
C23 C24 C25 119.6(16) . . ?
C24 C25 C26 116.5(16) . . ?
N22 C26 C21 115.6(14) . . ?
N22 C26 C25 119.4(16) . . ?
C21 C26 C25 123.6(14) . . ?
C26 N22 Ni4 107.9(12) . . ?
C26 N22 Ni6 112.8(19) . . ?
Ni4 N22 Ni6 76.0(8) . . ?
C31 N31 Ni1 100.7(11) . . ?
C31 N31 Ni6 107.0(16) . . ?
Ni1 N31 Ni6 82.7(7) . . ?
N31 C31 C36 118.4(13) . . ?
N31 C31 C32 119.8(15) . . ?
C36 C31 C32 121.1(13) . . ?
C31 C32 C33 111.6(14) . . ?
C34 C33 C32 125.0(17) . . ?
C33 C34 C35 120.6(16) . . ?
C34 C35 C36 111.8(13) . . ?
N32 C36 C31 114.8(12) . . ?
N32 C36 C35 119.0(13) . . ?
C31 C36 C35 126.0(13) . . ?
C36 N32 Ni1 111.8(10) . . ?
C36 N32 Ni5 115.1(13) . . ?
Ni1 N32 Ni5 94.8(7) . . ?
C41 N41 Ni4 116.2(16) . . ?
C41 N41 Li2 152.6(14) . . ?
Ni4 N41 Li2 86.7(9) . . ?
C41 N41 Ni3 103.2(13) . . ?
Ni4 N41 Ni3 94.7(6) . . ?
Li2 N41 Ni3 88.7(9) . . ?
N41 C41 C46 115.2(12) . . ?
N41 C41 C42 119.7(13) . . ?
C46 C41 C42 125.0(12) . . ?
C41 C42 C43 115.0(14) . . ?
C44 C43 C42 119.1(15) . . ?
C43 C44 C45 124.9(15) . . ?
C46 C45 C44 114.0(14) . . ?
N42 C46 C41 118.2(12) . . ?
N42 C46 C45 120.8(14) . . ?
C41 C46 C45 120.5(12) . . ?
C46 N42 Ni2 110.4(15) . . ?
C46 N42 Ni3 105.2(11) . . ?
Ni2 N42 Ni3 98.7(8) . . ?
C51 N51 Ni5 109.2(12) . . ?
C51 N51 Ni6 120.1(14) . . ?
Ni5 N51 Ni6 82.3(5) . . ?
N51 C51 C56 115.5(11) . . ?
N51 C51 C52 122.6(13) . . ?
C56 C51 C52 121.1(11) . . ?
C51 C52 C53 119.3(13) . . ?
C54 C53 C52 117.6(14) . . ?
C53 C54 C55 124.4(15) . . ?
C56 C55 C54 117.1(14) . . ?
N52 C56 C51 116.1(12) . . ?
N52 C56 C55 124.2(14) . . ?
C51 C56 C55 119.2(12) . . ?
C56 N52 Ni2 115.4(15) . . ?
C56 N52 Ni5 107.5(11) . . ?
Ni2 N52 Ni5 94.1(7) . . ?
C61 N61 Ni4 119.5(18) . . ?
C61 N61 Ni2 110.9(12) . . ?
Ni4 N61 Ni2 83.2(7) . . ?
C66 C61 N61 116.6(13) . . ?
C66 C61 C62 121.0(14) . . ?
N61 C61 C62 122.3(16) . . ?
C61 C62 C63 118.7(17) . . ?
C64 C63 C62 117.9(18) . . ?
C63 C64 C65 121.7(18) . . ?
C66 C65 C64 117.8(16) . . ?
N62 C66 C61 115.4(13) . . ?
N62 C66 C65 124.0(15) . . ?
C61 C66 C65 120.4(14) . . ?
C66 N62 Ni6 126.3(17) . . ?
C66 N62 Ni2 111.9(12) . . ?
Ni6 N62 Ni2 80.5(7) . . ?
O3 Li1 O2 113(4) . . ?
O3 Li1 O4 99(4) . . ?
O2 Li1 O4 119(4) . . ?
O3 Li1 C140 102(4) . . ?
O2 Li1 C140 121(4) . . ?
O4 Li1 C140 101(4) . . ?
O3 Li1 C340 30.2(18) . . ?
O2 Li1 C340 132(4) . . ?
O4 Li1 C340 102(4) . . ?
C140 Li1 C340 72(3) . . ?
C110 O1 C140 103.5(18) . . ?
O1 C110 C120 103.5(14) . . ?
C130 C120 C110 101.7(18) . . ?
C120 C130 C140 97.9(18) . . ?
O1 C140 C130 94.0(18) . . ?
O1 C140 Li1 98(3) . . ?
C130 C140 Li1 168(3) . . ?
C210 O2 C240 100.0(19) . . ?
C210 O2 Li1 129(4) . . ?
C240 O2 Li1 130(4) . . ?
O2 C210 C220 108.4(18) . . ?
C230 C220 C210 101.2(19) . . ?
C220 C230 C240 97.3(19) . . ?
O2 C240 C230 106(2) . . ?
C310 O3 C340 100(2) . . ?
C310 O3 Li1 141(4) . . ?
C340 O3 Li1 112(4) . . ?
O3 C310 C320 102(2) . . ?
C330 C320 C310 99(2) . . ?
C320 C330 C340 102.1(19) . . ?
O3 C340 C330 108.5(17) . . ?
O3 C340 Li1 38(2) . . ?
C330 C340 Li1 145(3) . . ?
C440 O4 C410 95(2) . . ?
C440 O4 Li1 144(4) . . ?
C410 O4 Li1 116(4) . . ?
O4 C410 C420 98(2) . . ?
C430 C420 C410 104.5(19) . . ?
C420 C430 C440 105.2(16) . . ?
O4 C440 C430 102(2) . . ?
C540 O5 C510 98(2) . . ?
C540 O5 Li2 130(2) . . ?
C510 O5 Li2 117(2) . . ?
O5 C510 C520 108.8(17) . . ?
C530 C520 C510 106.6(15) . . ?
C520 C530 C540 106.4(16) . . ?
O5 C540 C530 108.2(18) . . ?
C610 O6 C640 92(2) . . ?
O6 C610 C620 105(2) . . ?
C630 C620 C610 104.1(16) . . ?
C620 C630 C640 104.2(18) . . ?
O6 C640 C630 102(2) . . ?
C740 O7 C710 94(2) . . ?
O7 C710 C720 103(2) . . ?
C730 C720 C710 104.9(19) . . ?
C720 C730 C740 105.6(17) . . ?
O7 C740 C730 104(2) . . ?
N11 Li2 O5 118.2(15) . . ?
N11 Li2 N41 93.9(12) . . ?
O5 Li2 N41 128.2(13) . . ?
N11 Li2 N21 93.2(10) . . ?
O5 Li2 N21 120.7(16) . . ?
N41 Li2 N21 94.5(12) . . ?
N11 Li2 Ni4 94.7(9) . . ?
O5 Li2 Ni4 147.0(14) . . ?
N41 Li2 Ni4 45.9(7) . . ?
N21 Li2 Ni4 48.6(8) . . ?
N11 Li2 Ni1 44.1(7) . . ?
O5 Li2 Ni1 137.0(11) . . ?
N41 Li2 Ni1 94.6(8) . . ?
N21 Li2 Ni1 49.1(8) . . ?
Ni4 Li2 Ni1 65.3(5) . . ?
N11 Li2 Ni3 46.6(7) . . ?
O5 Li2 Ni3 141.5(15) . . ?
N41 Li2 Ni3 47.3(7) . . ?
N21 Li2 Ni3 97.1(9) . . ?
Ni4 Li2 Ni3 64.7(4) . . ?
Ni1 Li2 Ni3 63.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.923
_diffrn_reflns_theta_full        22.75
_diffrn_measured_fraction_theta_full 0.923
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.187
_database_code_depnum_ccdc_archive 'CCDC 943108'