Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Andrews, Phil'
'MacLellan, Jonathan G.'
'Mulvey, Robert E.'
'Nichols, Peter J.'

_publ_contact_author_name     	'Dr Phil Andrews'  
_publ_contact_author_address 
;
School of Chemistry
Monash University
PO Box 23
Clayton
Melbourne
Vic.
3800
AUSTRALIA
;

_publ_contact_author_email       'P.ANDREWS@SCI.MONASH.EDU.AU'

_publ_section_title		
;
New Homo- and Hetero-Alkali Metal Alkoxide Cages; 
Crystal Structures of
[Me2N(CH2)2OLi]8 and [{Me2N(CH2)2O}12Li8K6]O
;

data_jon1 

_database_code_CSD	175465


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C32 H80 Li8 N8 O8' 
_chemical_formula_weight          760.56 

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' 

_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    C2/c 

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                    18.571(4) 
_cell_length_b                    13.243(3) 
_cell_length_c                    19.467(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.30(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      4767.1(16) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.060 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1664 
_exptl_absorpt_coefficient_mu     0.072 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             34585 
_diffrn_reflns_av_R_equivalents   0.0679 
_diffrn_reflns_av_sigmaI/netI     0.0435 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        24 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          2.75 
_diffrn_reflns_theta_max          28.30 
_reflns_number_total              5885 
_reflns_number_gt                 4267 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 

_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^+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_extinction_coef        ? 
_refine_ls_number_reflns          5885 
_refine_ls_number_parameters      261 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0738 
_refine_ls_R_factor_gt            0.0483 
_refine_ls_wR_factor_ref          0.1604 
_refine_ls_wR_factor_gt           0.1447 
_refine_ls_goodness_of_fit_ref    1.077 
_refine_ls_restrained_S_all       1.077 
_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 
O3 O 0.11542(4) 0.11515(6) 0.25385(4) 0.0228(2) Uani 1 1 d . . . 
O4 O 0.01980(5) -0.01795(6) 0.32509(4) 0.0241(2) Uani 1 1 d . . . 
C9 C 0.18894(7) 0.11978(11) 0.27542(7) 0.0316(3) Uani 1 1 d . . . 
H24 H 0.2028 0.1898 0.2829 0.038 Uiso 1 1 calc R . . 
H23 H 0.2162 0.0932 0.2393 0.038 Uiso 1 1 calc R . . 
C10 C 0.20830(7) 0.06086(11) 0.34115(7) 0.0317(3) Uani 1 1 d . . . 
H11A H 0.1988 -0.0102 0.3325 0.038 Uiso 1 1 calc R . . 
H11B H 0.2596 0.0685 0.3547 0.038 Uiso 1 1 calc R . . 
C13 C 0.00715(8) -0.09113(11) 0.37307(7) 0.0324(3) Uani 1 1 d . . . 
H32 H -0.0150 -0.0600 0.4110 0.039 Uiso 1 1 calc R . . 
H31 H 0.0529 -0.1201 0.3913 0.039 Uiso 1 1 calc R . . 
C14 C -0.04208(8) -0.17521(10) 0.34236(8) 0.0337(3) Uani 1 1 d . . . 
H33 H -0.0164 -0.2140 0.3101 0.040 Uiso 1 1 calc R . . 
H34 H -0.0537 -0.2203 0.3790 0.040 Uiso 1 1 calc R . . 
Li1 Li 0.06235(12) 0.11396(16) 0.33830(11) 0.0246(5) Uani 1 1 d . . . 
O1 O 0.00714(5) 0.22764(6) 0.36216(4) 0.0234(2) Uani 1 1 d . . . 
N3 N 0.16716(6) 0.09472(8) 0.39809(5) 0.0266(3) Uani 1 1 d . . . 
N4 N -0.10941(6) -0.13630(8) 0.30660(6) 0.0282(3) Uani 1 1 d . . . 
C12 C 0.17306(10) 0.02066(14) 0.45347(8) 0.0474(4) Uani 1 1 d . . . 
H28 H 0.2222 0.0178 0.4736 0.071 Uiso 1 1 calc R . . 
H30 H 0.1589 -0.0445 0.4353 0.071 Uiso 1 1 calc R . . 
H29 H 0.1420 0.0398 0.4881 0.071 Uiso 1 1 calc R . . 
C11 C 0.19286(10) 0.19180(13) 0.42382(10) 0.0496(4) Uani 1 1 d . . . 
H26 H 0.1665 0.2115 0.4618 0.074 Uiso 1 1 calc R . . 
H25 H 0.1858 0.2411 0.3877 0.074 Uiso 1 1 calc R . . 
H27 H 0.2434 0.1872 0.4391 0.074 Uiso 1 1 calc R . . 
C16 C -0.15865(9) -0.10125(12) 0.35571(9) 0.0415(4) Uani 1 1 d . . . 
H39 H -0.1716 -0.1569 0.3837 0.062 Uiso 1 1 calc R . . 
H38 H -0.2014 -0.0739 0.3311 0.062 Uiso 1 1 calc R . . 
H40 H -0.1353 -0.0499 0.3846 0.062 Uiso 1 1 calc R . . 
N1 N -0.13978(6) 0.23839(8) 0.39808(6) 0.0269(3) Uani 1 1 d . . . 
C1 C -0.00698(8) 0.22941(11) 0.43106(7) 0.0313(3) Uani 1 1 d . . . 
H22 H -0.0031 0.2983 0.4479 0.038 Uiso 1 1 calc R . . 
H21 H 0.0293 0.1895 0.4579 0.038 Uiso 1 1 calc R . . 
C2 C -0.08165(8) 0.18858(11) 0.44214(7) 0.0316(3) Uani 1 1 d . . . 
H3 H -0.0828 0.1167 0.4326 0.038 Uiso 1 1 calc R . . 
H4 H -0.0903 0.1979 0.4901 0.038 Uiso 1 1 calc R . . 
C15 C -0.14506(9) -0.21416(12) 0.26235(9) 0.0430(4) Uani 1 1 d . . . 
H36 H -0.1540 -0.2725 0.2896 0.064 Uiso 1 1 calc R . . 
H35 H -0.1145 -0.2326 0.2272 0.064 Uiso 1 1 calc R . . 
H37 H -0.1901 -0.1885 0.2411 0.064 Uiso 1 1 calc R . . 
C3 C -0.20812(8) 0.18594(12) 0.40400(8) 0.0373(4) Uani 1 1 d . . . 
H8 H -0.2195 0.1878 0.4511 0.056 Uiso 1 1 calc R . . 
H10 H -0.2038 0.1170 0.3896 0.056 Uiso 1 1 calc R . . 
H9 H -0.2459 0.2186 0.3752 0.056 Uiso 1 1 calc R . . 
C4 C -0.14751(10) 0.34438(11) 0.41753(8) 0.0405(4) Uani 1 1 d . . . 
H6 H -0.1877 0.3737 0.3900 0.061 Uiso 1 1 calc R . . 
H5 H -0.1041 0.3804 0.4100 0.061 Uiso 1 1 calc R . . 
H7 H -0.1558 0.3485 0.4654 0.061 Uiso 1 1 calc R . . 
Li3 Li 0.08615(12) 0.22773(16) 0.19701(11) 0.0252(5) Uani 1 1 d . . . 
N2 N 0.07208(6) 0.48010(8) 0.36161(6) 0.0294(3) Uani 1 1 d . . . 
C6 C 0.10257(9) 0.51635(11) 0.29889(7) 0.0343(3) Uani 1 1 d . . . 
H14 H 0.1423 0.5621 0.3120 0.041 Uiso 1 1 calc R . . 
H13 H 0.0658 0.5538 0.2709 0.041 Uiso 1 1 calc R . . 
C5 C 0.12992(8) 0.43021(11) 0.25595(8) 0.0338(3) Uani 1 1 d . . . 
H12 H 0.1478 0.4579 0.2146 0.041 Uiso 1 1 calc R . . 
H11 H 0.1700 0.3969 0.2823 0.041 Uiso 1 1 calc R . . 
C7 C 0.12999(9) 0.45645(12) 0.41545(8) 0.0435(4) Uani 1 1 d . . . 
H16 H 0.1564 0.5169 0.4284 0.065 Uiso 1 1 calc R . . 
H15 H 0.1621 0.4077 0.3983 0.065 Uiso 1 1 calc R . . 
H17 H 0.1094 0.4292 0.4550 0.065 Uiso 1 1 calc R . . 
C8 C 0.02553(10) 0.55689(13) 0.38831(9) 0.0462(4) Uani 1 1 d . . . 
H19 H 0.0066 0.5322 0.4293 0.069 Uiso 1 1 calc R . . 
H20 H -0.0137 0.5719 0.3542 0.069 Uiso 1 1 calc R . . 
H18 H 0.0531 0.6171 0.3990 0.069 Uiso 1 1 calc R . . 
O2 O 0.07658(5) 0.35980(6) 0.23719(4) 0.0248(2) Uani 1 1 d . . . 
Li2 Li 0.01768(12) 0.35036(16) 0.31413(11) 0.0266(5) Uani 1 1 d . . . 
Li4 Li 0.06521(12) -0.00922(16) 0.24008(11) 0.0257(5) Uani 1 1 d . . . 

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 
O3 0.0181(4) 0.0250(4) 0.0253(4) 0.0020(4) 0.0015(3) -0.0015(3) 
O4 0.0246(5) 0.0235(4) 0.0241(5) 0.0048(3) 0.0016(4) -0.0032(3) 
C9 0.0210(7) 0.0448(8) 0.0291(7) 0.0027(6) 0.0025(5) -0.0017(6) 
C10 0.0238(7) 0.0366(7) 0.0342(7) -0.0010(6) 0.0006(6) 0.0039(6) 
C13 0.0307(7) 0.0346(7) 0.0311(7) 0.0109(6) -0.0022(6) -0.0068(6) 
C14 0.0327(8) 0.0259(7) 0.0430(8) 0.0083(6) 0.0059(6) -0.0023(6) 
Li1 0.0245(11) 0.0244(10) 0.0248(10) 0.0009(9) 0.0016(9) -0.0022(8) 
O1 0.0239(5) 0.0249(4) 0.0216(4) 0.0003(4) 0.0035(4) 0.0004(3) 
N3 0.0261(6) 0.0281(6) 0.0250(6) 0.0002(4) -0.0008(5) -0.0016(4) 
N4 0.0242(6) 0.0256(6) 0.0351(6) -0.0032(5) 0.0045(5) -0.0057(5) 
C12 0.0447(10) 0.0602(11) 0.0363(8) 0.0158(8) -0.0021(7) 0.0001(8) 
C11 0.0430(10) 0.0456(9) 0.0602(11) -0.0208(8) 0.0057(8) -0.0101(8) 
C16 0.0373(8) 0.0406(9) 0.0486(9) -0.0050(7) 0.0150(7) -0.0031(7) 
N1 0.0270(6) 0.0279(6) 0.0269(6) 0.0002(4) 0.0075(5) 0.0026(5) 
C1 0.0289(7) 0.0425(8) 0.0226(7) 0.0003(6) 0.0022(5) 0.0013(6) 
C2 0.0324(8) 0.0396(8) 0.0235(7) 0.0072(6) 0.0068(6) 0.0022(6) 
C15 0.0382(9) 0.0383(8) 0.0531(10) -0.0116(7) 0.0076(7) -0.0146(7) 
C3 0.0296(8) 0.0460(9) 0.0379(8) 0.0023(7) 0.0110(6) -0.0009(7) 
C4 0.0521(10) 0.0318(8) 0.0396(8) -0.0041(6) 0.0144(7) 0.0060(7) 
Li3 0.0261(11) 0.0243(10) 0.0253(11) 0.0015(9) 0.0031(9) 0.0014(9) 
N2 0.0335(6) 0.0256(6) 0.0286(6) -0.0041(5) 0.0001(5) 0.0016(5) 
C6 0.0418(8) 0.0267(7) 0.0340(7) -0.0023(6) 0.0013(6) -0.0095(6) 
C5 0.0289(7) 0.0377(8) 0.0359(7) -0.0075(6) 0.0086(6) -0.0108(6) 
C7 0.0495(10) 0.0391(8) 0.0396(8) -0.0015(7) -0.0077(7) 0.0037(7) 
C8 0.0514(10) 0.0416(9) 0.0448(9) -0.0130(7) 0.0003(8) 0.0115(8) 
O2 0.0235(5) 0.0232(4) 0.0280(5) -0.0029(4) 0.0043(4) -0.0057(4) 
Li2 0.0283(12) 0.0239(11) 0.0275(11) -0.0015(9) 0.0020(9) -0.0015(9) 
Li4 0.0227(11) 0.0260(10) 0.0282(11) 0.0007(9) 0.0020(9) 0.0008(9) 

_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 
O3 C9 1.3922(16) . ? 
O3 Li4 1.899(2) . ? 
O3 Li3 1.906(2) . ? 
O3 Li1 1.994(2) . ? 
O4 C13 1.3810(16) . ? 
O4 Li1 1.925(2) . ? 
O4 Li4 1.929(2) . ? 
O4 Li4 1.935(2) 2 ? 
C9 C10 1.513(2) . ? 
C10 N3 1.4731(18) . ? 
C13 C14 1.527(2) . ? 
C13 Li4 2.700(3) 2 ? 
C14 N4 1.4673(19) . ? 
C14 Li4 2.732(3) 2 ? 
Li1 O1 1.903(2) . ? 
Li1 N3 2.189(2) . ? 
Li1 Li4 3.152(3) 2 ? 
Li1 Li3 3.162(3) 2 ? 
O1 C1 1.3904(16) . ? 
O1 Li2 1.894(2) . ? 
O1 Li3 1.990(2) 2 ? 
N3 C11 1.4448(19) . ? 
N3 C12 1.4541(19) . ? 
N4 C16 1.4585(19) . ? 
N4 C15 1.4622(18) . ? 
N4 Li4 2.114(2) 2 ? 
N1 C3 1.4606(18) . ? 
N1 C4 1.4644(18) . ? 
N1 C2 1.4714(18) . ? 
N1 Li3 2.186(3) 2 ? 
C1 C2 1.522(2) . ? 
C1 Li3 2.775(3) 2 ? 
C2 Li3 2.752(3) 2 ? 
Li3 O2 1.931(2) . ? 
Li3 O1 1.990(2) 2 ? 
Li3 N1 2.186(3) 2 ? 
Li3 Li2 2.515(3) 2 ? 
Li3 C2 2.752(3) 2 ? 
Li3 C1 2.775(3) 2 ? 
Li3 Li1 3.162(3) 2 ? 
N2 C8 1.4610(19) . ? 
N2 C7 1.4646(19) . ? 
N2 C6 1.4730(19) . ? 
N2 Li2 2.157(2) . ? 
C6 C5 1.529(2) . ? 
C5 O2 1.3846(16) . ? 
O2 Li2 1.938(2) 2 ? 
O2 Li2 1.939(2) . ? 
Li2 O2 1.938(2) 2 ? 
Li2 Li3 2.515(3) 2 ? 
Li2 Li2 2.523(4) 2 ? 
Li4 O4 1.935(2) 2 ? 
Li4 N4 2.114(2) 2 ? 
Li4 Li4 2.488(4) 2 ? 
Li4 C13 2.700(3) 2 ? 
Li4 C14 2.732(3) 2 ? 
Li4 Li1 3.152(3) 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 
C9 O3 Li4 122.39(10) . . ? 
C9 O3 Li3 111.10(10) . . ? 
Li4 O3 Li3 119.11(10) . . ? 
C9 O3 Li1 107.30(10) . . ? 
Li4 O3 Li1 80.55(9) . . ? 
Li3 O3 Li1 110.41(10) . . ? 
C13 O4 Li1 129.78(10) . . ? 
C13 O4 Li4 137.51(11) . . ? 
Li1 O4 Li4 81.58(10) . . ? 
C13 O4 Li4 107.81(10) . 2 ? 
Li1 O4 Li4 109.47(10) . 2 ? 
Li4 O4 Li4 80.14(11) . 2 ? 
O3 C9 C10 112.47(11) . . ? 
N3 C10 C9 112.33(11) . . ? 
O4 C13 C14 112.33(11) . . ? 
O4 C13 Li4 43.04(7) . 2 ? 
C14 C13 Li4 74.85(9) . 2 ? 
N4 C14 C13 112.52(11) . . ? 
N4 C14 Li4 50.05(8) . 2 ? 
C13 C14 Li4 72.50(9) . 2 ? 
O1 Li1 O4 121.80(12) . . ? 
O1 Li1 O3 120.90(11) . . ? 
O4 Li1 O3 97.19(10) . . ? 
O1 Li1 N3 115.78(10) . . ? 
O4 Li1 N3 107.42(10) . . ? 
O3 Li1 N3 87.50(9) . . ? 
O1 Li1 Li4 97.46(9) . 2 ? 
O4 Li1 Li4 35.38(6) . 2 ? 
O3 Li1 Li4 90.66(9) . 2 ? 
N3 Li1 Li4 142.09(10) . 2 ? 
O1 Li1 Li3 36.62(6) . 2 ? 
O4 Li1 Li3 93.69(9) . 2 ? 
O3 Li1 Li3 107.74(9) . 2 ? 
N3 Li1 Li3 152.39(10) . 2 ? 
Li4 Li1 Li3 62.61(7) 2 2 ? 
C1 O1 Li2 119.94(11) . . ? 
C1 O1 Li1 113.74(10) . . ? 
Li2 O1 Li1 118.41(11) . . ? 
C1 O1 Li3 109.06(10) . 2 ? 
Li2 O1 Li3 80.67(9) . 2 ? 
Li1 O1 Li3 108.61(10) . 2 ? 
C11 N3 C12 110.07(13) . . ? 
C11 N3 C10 110.73(12) . . ? 
C12 N3 C10 110.11(12) . . ? 
C11 N3 Li1 109.27(11) . . ? 
C12 N3 Li1 118.38(11) . . ? 
C10 N3 Li1 97.63(9) . . ? 
C16 N4 C15 109.48(12) . . ? 
C16 N4 C14 111.04(12) . . ? 
C15 N4 C14 110.58(11) . . ? 
C16 N4 Li4 108.68(11) . 2 ? 
C15 N4 Li4 118.73(11) . 2 ? 
C14 N4 Li4 97.80(10) . 2 ? 
C3 N1 C4 109.19(12) . . ? 
C3 N1 C2 109.69(11) . . ? 
C4 N1 C2 111.29(12) . . ? 
C3 N1 Li3 120.21(11) . 2 ? 
C4 N1 Li3 110.12(10) . 2 ? 
C2 N1 Li3 95.60(10) . 2 ? 
O1 C1 C2 112.72(11) . . ? 
O1 C1 Li3 42.67(7) . 2 ? 
C2 C1 Li3 73.17(9) . 2 ? 
N1 C2 C1 112.77(11) . . ? 
N1 C2 Li3 52.24(8) . 2 ? 
C1 C2 Li3 74.86(9) . 2 ? 
O3 Li3 O2 120.36(12) . . ? 
O3 Li3 O1 121.47(12) . 2 ? 
O2 Li3 O1 97.31(10) . 2 ? 
O3 Li3 N1 114.48(11) . 2 ? 
O2 Li3 N1 110.53(10) . 2 ? 
O1 Li3 N1 87.15(9) 2 2 ? 
O3 Li3 Li2 136.94(13) . 2 ? 
O2 Li3 Li2 49.58(8) . 2 ? 
O1 Li3 Li2 48.00(7) 2 2 ? 
N1 Li3 Li2 106.91(10) 2 2 ? 
O3 Li3 C2 113.91(10) . 2 ? 
O2 Li3 C2 125.02(10) . 2 ? 
O1 Li3 C2 58.96(7) 2 2 ? 
N1 Li3 C2 32.15(5) 2 2 ? 
Li2 Li3 C2 94.78(9) 2 2 ? 
O3 Li3 C1 128.83(10) . 2 ? 
O2 Li3 C1 107.21(9) . 2 ? 
O1 Li3 C1 28.27(5) 2 2 ? 
N1 Li3 C1 58.92(7) 2 2 ? 
Li2 Li3 C1 65.10(8) 2 2 ? 
C2 Li3 C1 31.97(5) 2 2 ? 
O3 Li3 Li1 87.12(9) . 2 ? 
O2 Li3 Li1 114.12(10) . 2 ? 
O1 Li3 Li1 34.78(6) 2 2 ? 
N1 Li3 Li1 107.64(9) 2 2 ? 
Li2 Li3 Li1 69.06(8) 2 2 ? 
C2 Li3 Li1 75.50(7) 2 2 ? 
C1 Li3 Li1 55.21(6) 2 2 ? 
C8 N2 C7 108.29(12) . . ? 
C8 N2 C6 110.70(12) . . ? 
C7 N2 C6 110.48(12) . . ? 
C8 N2 Li2 115.96(12) . . ? 
C7 N2 Li2 114.84(11) . . ? 
C6 N2 Li2 96.03(10) . . ? 
N2 C6 C5 112.51(12) . . ? 
O2 C5 C6 112.40(12) . . ? 
C5 O2 Li3 128.79(11) . . ? 
C5 O2 Li2 140.32(11) . 2 ? 
Li3 O2 Li2 81.09(10) . 2 ? 
C5 O2 Li2 106.30(10) . . ? 
Li3 O2 Li2 109.52(10) . . ? 
Li2 O2 Li2 81.20(10) 2 . ? 
O1 Li2 O2 100.39(10) . 2 ? 
O1 Li2 O2 121.88(12) . . ? 
O2 Li2 O2 98.32(10) 2 . ? 
O1 Li2 N2 122.51(11) . . ? 
O2 Li2 N2 122.31(11) 2 . ? 
O2 Li2 N2 90.25(10) . . ? 
O1 Li2 Li3 51.33(8) . 2 ? 
O2 Li2 Li3 49.33(7) 2 2 ? 
O2 Li2 Li3 117.25(11) . 2 ? 
N2 Li2 Li3 151.18(12) . 2 ? 
O1 Li2 Li2 117.34(8) . 2 ? 
O2 Li2 Li2 49.41(8) 2 2 ? 
O2 Li2 Li2 49.39(8) . 2 ? 
N2 Li2 Li2 119.53(8) . 2 ? 
Li3 Li2 Li2 77.71(10) 2 2 ? 
O3 Li4 O4 100.30(10) . . ? 
O3 Li4 O4 120.29(12) . 2 ? 
O4 Li4 O4 99.44(10) . 2 ? 
O3 Li4 N4 123.08(12) . 2 ? 
O4 Li4 N4 122.61(11) . 2 ? 
O4 Li4 N4 89.79(9) 2 2 ? 
O3 Li4 Li4 116.77(8) . 2 ? 
O4 Li4 Li4 50.04(8) . 2 ? 
O4 Li4 Li4 49.82(8) 2 2 ? 
N4 Li4 Li4 119.28(8) 2 2 ? 
O3 Li4 C13 131.64(11) . 2 ? 
O4 Li4 C13 116.86(10) . 2 ? 
O4 Li4 C13 29.15(5) 2 2 ? 
N4 Li4 C13 60.87(7) 2 2 ? 
Li4 Li4 C13 73.03(10) 2 2 ? 
O3 Li4 C14 145.99(12) . 2 ? 
O4 Li4 C14 113.47(10) . 2 ? 
O4 Li4 C14 59.49(7) 2 2 ? 
N4 Li4 C14 32.15(5) 2 2 ? 
Li4 Li4 C14 89.35(8) 2 2 ? 
C13 Li4 C14 32.65(5) 2 2 ? 
O3 Li4 Li1 87.52(9) . 2 ? 
O4 Li4 Li1 94.46(9) . 2 ? 
O4 Li4 Li1 35.15(6) 2 2 ? 
N4 Li4 Li1 120.54(10) 2 2 ? 
Li4 Li4 Li1 51.40(8) 2 2 ? 
C13 Li4 Li1 61.16(7) 2 2 ? 
C14 Li4 Li1 93.53(8) 2 2 ? 

_diffrn_measured_fraction_theta_max    0.992 
_diffrn_reflns_theta_full              28.30 
_diffrn_measured_fraction_theta_full   0.992 
_refine_diff_density_max    0.243 
_refine_diff_density_min   -0.220 
_refine_diff_density_rms    0.042 

data_jon2 

_database_code_CSD	175466


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C60 H140 K6 Li8 N12 O15' 
_chemical_formula_weight          1559.96 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'K'  'K'   0.2009   0.2494 
'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' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'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' 

_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-y, x-y, z' 
'-x+y, -x, z' 
'x+2/3, y+1/3, z+1/3' 
'-y+2/3, x-y+1/3, z+1/3' 
'-x+y+2/3, -x+1/3, z+1/3' 
'x+1/3, y+2/3, z+2/3' 
'-y+1/3, x-y+2/3, z+2/3' 
'-x+y+1/3, -x+2/3, z+2/3' 
'-x, -y, -z' 
'y, -x+y, -z' 
'x-y, x, -z' 
'-x+2/3, -y+1/3, -z+1/3' 
'y+2/3, -x+y+1/3, -z+1/3' 
'x-y+2/3, x+1/3, -z+1/3' 
'-x+1/3, -y+2/3, -z+2/3' 
'y+1/3, -x+y+2/3, -z+2/3' 
'x-y+1/3, x+2/3, -z+2/3' 

_cell_length_a                    14.895(2) 
_cell_length_b                    14.895(2) 
_cell_length_c                    36.505(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      7014(2) 
_cell_formula_units_Z             3 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.108 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2526 
_exptl_absorpt_coefficient_mu     0.334 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             26025 
_diffrn_reflns_av_R_equivalents   0.0774 
_diffrn_reflns_av_sigmaI/netI     0.0689 
_diffrn_reflns_limit_h_min        -19 
_diffrn_reflns_limit_h_max        19 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -45 
_diffrn_reflns_limit_l_max        46 
_diffrn_reflns_theta_min          3.21 
_diffrn_reflns_theta_max          28.27 
_reflns_number_total              3848 
_reflns_number_gt                 1600 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_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^)+(0.1777P)^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_extinction_coef        ? 
_refine_ls_number_reflns          3848 
_refine_ls_number_parameters      184 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1899 
_refine_ls_R_factor_gt            0.0844 
_refine_ls_wR_factor_ref          0.3012 
_refine_ls_wR_factor_gt           0.2358 
_refine_ls_goodness_of_fit_ref    0.970 
_refine_ls_restrained_S_all       0.970 
_refine_ls_shift/su_max           0.003 
_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 
K1 K 0.11802(7) 0.88202(7) 0.05906(2) 0.0833(5) Uani 1 1 d . . . 
O1 O 0.0003(2) 0.7754(2) 0.00000(7) 0.0856(8) Uani 1 1 d . C . 
O2 O 0.1497(2) 1.0745(2) 0.07528(7) 0.0856(8) Uani 1 1 d . . . 
N2 N 0.2433(5) 0.9769(4) 0.12193(15) 0.1424(19) Uani 1 1 d . . . 
N1 N 0.0971(5) 0.6830(4) 0.04812(15) 0.143(2) Uani 1 1 d . . . 
C5 C 0.2103(5) 1.1196(4) 0.10475(15) 0.1123(16) Uani 1 1 d . . . 
H5A H 0.1664 1.1011 0.1263 0.135 Uiso 1 1 calc R A 1 
H5B H 0.2437 1.1942 0.1019 0.135 Uiso 1 1 calc R A 1 
C7 C 0.3443(8) 0.9953(13) 0.1182(3) 0.292(8) Uani 1 1 d . C . 
H7A H 0.3825 1.0265 0.1402 0.439 Uiso 1 1 calc R . . 
H7B H 0.3772 1.0411 0.0979 0.439 Uiso 1 1 calc R . . 
H7C H 0.3426 0.9309 0.1139 0.439 Uiso 1 1 calc R . . 
C8 C 0.2016(10) 0.9231(12) 0.1548(2) 0.282(7) Uani 1 1 d . C . 
H8A H 0.2569 0.9354 0.1713 0.423 Uiso 1 1 calc R . . 
H8B H 0.1607 0.8502 0.1498 0.423 Uiso 1 1 calc R . . 
H8C H 0.1586 0.9468 0.1658 0.423 Uiso 1 1 calc R . . 
C1 C -0.0102(4) 0.6796(4) -0.00492(14) 0.1099(15) Uani 1 1 d . . . 
H1A H 0.0444 0.6863 -0.0211 0.132 Uiso 1 1 calc R B 1 
H1B H -0.0759 0.6352 -0.0169 0.132 Uiso 1 1 calc R B 1 
C4 C 0.0488(13) 0.6157(9) 0.0782(4) 0.310(9) Uani 1 1 d . C . 
H4A H 0.0755 0.6535 0.1007 0.465 Uiso 1 1 calc R . . 
H4B H 0.0628 0.5595 0.0773 0.465 Uiso 1 1 calc R . . 
H4C H -0.0247 0.5887 0.0771 0.465 Uiso 1 1 calc R . . 
C3 C 0.1916(9) 0.6870(8) 0.0412(5) 0.288(8) Uani 1 1 d . C . 
H3A H 0.2226 0.6845 0.0639 0.432 Uiso 1 1 calc R . . 
H3B H 0.2373 0.7502 0.0285 0.432 Uiso 1 1 calc R . . 
H3C H 0.1796 0.6289 0.0263 0.432 Uiso 1 1 calc R . . 
C6 C 0.2913(8) 1.0918(10) 0.1114(3) 0.117(3) Uani 0.50 1 d P C 1 
H6A H 0.3367 1.1347 0.1309 0.140 Uiso 0.50 1 calc PR C 1 
H6B H 0.3328 1.1054 0.0894 0.140 Uiso 0.50 1 calc PR C 1 
C6A C 0.2022(10) 1.0467(10) 0.1336(3) 0.126(4) Uani 0.50 1 d P C 2 
H6C H 0.1301 1.0043 0.1406 0.152 Uiso 0.50 1 calc PR C 2 
H6D H 0.2403 1.0859 0.1550 0.152 Uiso 0.50 1 calc PR C 2 
O3 O 0.0000 1.0000 0.0000 0.198(6) Uani 1 6 d S . . 
Li1 Li 0.0928(6) 0.9078(6) -0.02266(17) 0.0872(17) Uani 1 1 d . . . 
Li2 Li 0.0000 1.0000 0.0700(3) 0.088(3) Uani 1 3 d S . . 
C2 C -0.0058(10) 0.6275(8) 0.0301(4) 0.123(4) Uani 0.50 1 d P C 1 
H2A H -0.0579 0.6239 0.0470 0.147 Uiso 0.50 1 calc PR C 1 
H2B H -0.0224 0.5572 0.0247 0.147 Uiso 0.50 1 calc PR C 1 
C2A C 0.0802(10) 0.6714(8) 0.0067(3) 0.120(3) Uani 0.50 1 d P C 2 
H2C H 0.1417 0.7247 -0.0055 0.144 Uiso 0.50 1 calc PR C 2 
H2D H 0.0703 0.6046 -0.0008 0.144 Uiso 0.50 1 calc PR C 2 
C11 C 0.050(3) 1.050(3) 0.2265(10) 0.44(3) Uani 0.67 1 d P . . 
O4 O 0.0000 1.0000 0.2776(7) 0.64(5) Uani 1 3 d S . . 
C10 C 0.073(3) 1.004(5) 0.2592(6) 0.34(2) Uani 0.67 1 d P . . 
C9 C 0.2712(16) 0.639(5) 0.1446(6) 0.334(15) Uani 0.67 1 d P . . 

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 
K1 0.0846(7) 0.0857(7) 0.0866(7) 0.0052(4) -0.0044(4) 0.0477(5) 
O1 0.0903(18) 0.0802(17) 0.0879(17) -0.0018(13) -0.0025(13) 0.0440(14) 
O2 0.0857(17) 0.0836(17) 0.0856(16) -0.0065(13) -0.0068(14) 0.0408(14) 
N2 0.181(5) 0.128(4) 0.147(4) -0.027(3) -0.069(4) 0.099(4) 
N1 0.196(5) 0.116(4) 0.150(4) -0.024(3) -0.067(4) 0.104(4) 
C5 0.130(4) 0.109(4) 0.099(3) -0.002(3) -0.018(3) 0.061(3) 
C7 0.151(8) 0.47(2) 0.270(12) -0.093(14) -0.078(8) 0.164(12) 
C8 0.263(13) 0.337(16) 0.125(6) 0.049(8) -0.031(7) 0.060(11) 
C1 0.121(4) 0.101(4) 0.119(4) -0.009(3) -0.015(3) 0.064(3) 
C4 0.44(2) 0.185(9) 0.355(16) 0.140(11) 0.196(16) 0.197(13) 
C3 0.200(10) 0.193(10) 0.53(2) 0.023(12) 0.062(13) 0.142(9) 
C6 0.088(6) 0.149(10) 0.099(6) -0.023(6) -0.022(5) 0.048(7) 
C6A 0.113(8) 0.138(9) 0.116(8) -0.042(7) -0.043(7) 0.053(7) 
O3 0.203(9) 0.203(9) 0.189(12) 0.000 0.000 0.101(4) 
Li1 0.085(4) 0.090(4) 0.083(4) 0.002(3) -0.004(3) 0.041(4) 
Li2 0.083(4) 0.083(4) 0.100(7) 0.000 0.000 0.041(2) 
C2 0.141(10) 0.073(6) 0.161(10) 0.003(6) 0.014(8) 0.059(6) 
C2A 0.142(10) 0.078(6) 0.144(9) 0.001(6) 0.019(8) 0.058(6) 
C11 0.36(5) 0.26(4) 0.63(6) 0.19(4) 0.33(6) 0.10(2) 
O4 0.88(7) 0.88(7) 0.15(2) 0.000 0.000 0.44(4) 
C10 0.30(3) 0.69(7) 0.20(2) 0.05(3) 0.00(2) 0.37(4) 
C9 0.25(2) 0.37(4) 0.35(3) -0.02(6) -0.164(19) 0.13(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 
K1 O2 2.727(3) . ? 
K1 O1 2.731(3) . ? 
K1 O1 2.735(3) 12_665 ? 
K1 O2 2.738(3) 3_465 ? 
K1 N2 2.848(5) . ? 
K1 N1 2.850(4) . ? 
K1 Li1 3.073(7) 11_455 ? 
K1 Li1 3.080(7) 12_665 ? 
K1 C5 3.173(5) 3_465 ? 
K1 C1 3.176(5) 12_665 ? 
O1 C1 1.369(6) . ? 
O1 Li1 1.934(7) 11_455 ? 
O1 Li1 1.937(7) . ? 
O1 K1 2.735(3) 11_455 ? 
O2 C5 1.349(6) . ? 
O2 Li2 1.941(3) . ? 
O2 Li1 1.974(7) 12_665 ? 
O2 K1 2.738(3) 2_675 ? 
N2 C7 1.394(11) . ? 
N2 C8 1.404(11) . ? 
N2 C6A 1.508(14) . ? 
N2 C6 1.538(14) . ? 
N1 C3 1.402(11) . ? 
N1 C4 1.417(10) . ? 
N1 C2 1.482(13) . ? 
N1 C2A 1.527(13) . ? 
C5 C6A 1.473(14) . ? 
C5 C6 1.478(12) . ? 
C5 K1 3.173(5) 2_675 ? 
C1 C2A 1.474(13) . ? 
C1 C2 1.514(12) . ? 
C1 K1 3.176(5) 11_455 ? 
O3 Li1 2.526(8) 12_665 ? 
O3 Li1 2.526(8) 3_465 ? 
O3 Li1 2.526(7) 11_455 ? 
O3 Li1 2.526(7) 2_675 ? 
O3 Li1 2.526(7) . ? 
O3 Li1 2.526(7) 10_575 ? 
O3 Li2 2.554(12) . ? 
O3 Li2 2.554(12) 10_575 ? 
Li1 O1 1.934(7) 12_665 ? 
Li1 O2 1.974(7) 11_455 ? 
Li1 Li1 2.904(9) 12_665 ? 
Li1 Li1 2.904(9) 11_455 ? 
Li1 Li2 2.946(10) 10_575 ? 
Li1 K1 3.073(7) 12_665 ? 
Li1 K1 3.080(7) 11_455 ? 
Li2 O2 1.941(3) 3_465 ? 
Li2 O2 1.941(3) 2_675 ? 
Li2 Li1 2.946(10) 11_455 ? 
Li2 Li1 2.946(10) 12_665 ? 
Li2 Li1 2.946(10) 10_575 ? 
Li2 K1 3.0701(19) 3_465 ? 
Li2 K1 3.0701(19) 2_675 ? 
C11 C11 1.29(4) 3_465 ? 
C11 C11 1.29(4) 2_675 ? 
C11 C10 1.50(5) . ? 
C11 C10 1.54(5) 2_675 ? 
O4 C10 1.25(2) 3_465 ? 
O4 C10 1.25(2) . ? 
O4 C10 1.25(2) 2_675 ? 
C10 C11 1.54(5) 3_465 ? 
C10 C10 1.82(4) 3_465 ? 
C10 C10 1.82(4) 2_675 ? 
C9 C9 1.39(3) 3_565 ? 
C9 C9 1.39(3) 2_665 ? 
C9 C9 1.80(3) 15 ? 
C9 C9 1.80(3) 14_455 ? 

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 
O2 K1 O1 120.38(9) . . ? 
O2 K1 O1 75.82(8) . 12_665 ? 
O1 K1 O1 75.51(6) . 12_665 ? 
O2 K1 O2 75.46(11) . 3_465 ? 
O1 K1 O2 75.90(8) . 3_465 ? 
O1 K1 O2 120.29(9) 12_665 3_465 ? 
O2 K1 N2 65.01(11) . . ? 
O1 K1 N2 174.61(11) . . ? 
O1 K1 N2 106.84(16) 12_665 . ? 
O2 K1 N2 106.44(15) 3_465 . ? 
O2 K1 N1 174.44(11) . . ? 
O1 K1 N1 65.19(11) . . ? 
O1 K1 N1 106.58(15) 12_665 . ? 
O2 K1 N1 106.99(16) 3_465 . ? 
N2 K1 N1 109.43(14) . . ? 
O2 K1 Li1 92.75(15) . 11_455 ? 
O1 K1 Li1 38.37(14) . 11_455 ? 
O1 K1 Li1 92.22(14) 12_665 11_455 ? 
O2 K1 Li1 39.19(13) 3_465 11_455 ? 
N2 K1 Li1 144.92(18) . 11_455 ? 
N1 K1 Li1 92.17(18) . 11_455 ? 
O2 K1 Li1 39.16(13) . 12_665 ? 
O1 K1 Li1 92.21(14) . 12_665 ? 
O1 K1 Li1 38.35(14) 12_665 12_665 ? 
O2 K1 Li1 92.64(15) 3_465 12_665 ? 
N2 K1 Li1 92.52(17) . 12_665 ? 
N1 K1 Li1 144.21(17) . 12_665 ? 
Li1 K1 Li1 84.4(3) 11_455 12_665 ? 
O2 K1 C5 87.63(12) . 3_465 ? 
O1 K1 C5 87.58(13) . 3_465 ? 
O1 K1 C5 145.31(11) 12_665 3_465 ? 
O2 K1 C5 25.02(11) 3_465 3_465 ? 
N2 K1 C5 92.78(19) . 3_465 ? 
N1 K1 C5 92.81(18) . 3_465 ? 
Li1 K1 C5 57.85(15) 11_455 3_465 ? 
Li1 K1 C5 114.62(17) 12_665 3_465 ? 
O2 K1 C1 88.01(12) . 12_665 ? 
O1 K1 C1 87.54(12) . 12_665 ? 
O1 K1 C1 25.40(10) 12_665 12_665 ? 
O2 K1 C1 145.69(11) 3_465 12_665 ? 
N2 K1 C1 92.81(18) . 12_665 ? 
N1 K1 C1 92.33(17) . 12_665 ? 
Li1 K1 C1 114.20(15) 11_455 12_665 ? 
Li1 K1 C1 57.69(16) 12_665 12_665 ? 
C5 K1 C1 170.70(13) 3_465 12_665 ? 
C1 O1 Li1 130.3(4) . 11_455 ? 
C1 O1 Li1 131.1(4) . . ? 
Li1 O1 Li1 97.2(5) 11_455 . ? 
C1 O1 K1 114.5(3) . . ? 
Li1 O1 K1 80.4(2) 11_455 . ? 
Li1 O1 K1 79.8(2) . . ? 
C1 O1 K1 95.6(3) . 11_455 ? 
Li1 O1 K1 79.7(2) 11_455 11_455 ? 
Li1 O1 K1 80.5(2) . 11_455 ? 
K1 O1 K1 149.86(12) . 11_455 ? 
C5 O2 Li2 131.0(5) . . ? 
C5 O2 Li1 129.9(4) . 12_665 ? 
Li2 O2 Li1 97.6(4) . 12_665 ? 
C5 O2 K1 114.7(3) . . ? 
Li2 O2 K1 80.32(11) . . ? 
Li1 O2 K1 80.1(2) 12_665 . ? 
C5 O2 K1 95.8(3) . 2_675 ? 
Li2 O2 K1 80.04(11) . 2_675 ? 
Li1 O2 K1 79.6(2) 12_665 2_675 ? 
K1 O2 K1 149.47(11) . 2_675 ? 
C7 N2 C8 108.8(9) . . ? 
C7 N2 C6A 131.5(9) . . ? 
C8 N2 C6A 86.4(9) . . ? 
C7 N2 C6 84.3(9) . . ? 
C8 N2 C6 132.6(8) . . ? 
C6A N2 C6 55.0(7) . . ? 
C7 N2 K1 113.2(6) . . ? 
C8 N2 K1 114.3(6) . . ? 
C6A N2 K1 100.2(4) . . ? 
C6 N2 K1 100.0(4) . . ? 
C3 N1 C4 108.4(9) . . ? 
C3 N1 C2 132.9(9) . . ? 
C4 N1 C2 86.1(10) . . ? 
C3 N1 C2A 86.1(9) . . ? 
C4 N1 C2A 133.7(9) . . ? 
C2 N1 C2A 55.4(7) . . ? 
C3 N1 K1 113.3(6) . . ? 
C4 N1 K1 112.2(6) . . ? 
C2 N1 K1 100.7(4) . . ? 
C2A N1 K1 100.5(4) . . ? 
O2 C5 C6A 114.5(6) . . ? 
O2 C5 C6 115.3(6) . . ? 
C6A C5 C6 56.9(7) . . ? 
O2 C5 K1 59.2(2) . 2_675 ? 
C6A C5 K1 151.7(6) . 2_675 ? 
C6 C5 K1 151.2(6) . 2_675 ? 
O1 C1 C2A 114.6(5) . . ? 
O1 C1 C2 114.3(5) . . ? 
C2A C1 C2 55.9(7) . . ? 
O1 C1 K1 59.0(2) . 11_455 ? 
C2A C1 K1 151.2(6) . 11_455 ? 
C2 C1 K1 152.7(6) . 11_455 ? 
C5 C6 N2 111.2(8) . . ? 
C5 C6A N2 113.3(9) . . ? 
Li1 O3 Li1 180.0(2) 12_665 3_465 ? 
Li1 O3 Li1 109.82(14) 12_665 11_455 ? 
Li1 O3 Li1 70.18(14) 3_465 11_455 ? 
Li1 O3 Li1 70.18(14) 12_665 2_675 ? 
Li1 O3 Li1 109.82(14) 3_465 2_675 ? 
Li1 O3 Li1 180.0(3) 11_455 2_675 ? 
Li1 O3 Li1 70.18(14) 12_665 . ? 
Li1 O3 Li1 109.82(14) 3_465 . ? 
Li1 O3 Li1 70.18(14) 11_455 . ? 
Li1 O3 Li1 109.82(14) 2_675 . ? 
Li1 O3 Li1 109.82(14) 12_665 10_575 ? 
Li1 O3 Li1 70.18(14) 3_465 10_575 ? 
Li1 O3 Li1 109.82(14) 11_455 10_575 ? 
Li1 O3 Li1 70.18(14) 2_675 10_575 ? 
Li1 O3 Li1 180.0(3) . 10_575 ? 
Li1 O3 Li2 70.88(14) 12_665 . ? 
Li1 O3 Li2 109.12(14) 3_465 . ? 
Li1 O3 Li2 70.88(14) 11_455 . ? 
Li1 O3 Li2 109.12(14) 2_675 . ? 
Li1 O3 Li2 109.12(14) . . ? 
Li1 O3 Li2 70.88(14) 10_575 . ? 
Li1 O3 Li2 109.12(14) 12_665 10_575 ? 
Li1 O3 Li2 70.88(14) 3_465 10_575 ? 
Li1 O3 Li2 109.12(14) 11_455 10_575 ? 
Li1 O3 Li2 70.88(14) 2_675 10_575 ? 
Li1 O3 Li2 70.88(14) . 10_575 ? 
Li1 O3 Li2 109.12(14) 10_575 10_575 ? 
Li2 O3 Li2 180.0 . 10_575 ? 
O1 Li1 O1 119.7(3) 12_665 . ? 
O1 Li1 O2 118.8(4) 12_665 11_455 ? 
O1 Li1 O2 118.2(4) . 11_455 ? 
O1 Li1 O3 96.4(3) 12_665 . ? 
O1 Li1 O3 96.3(3) . . ? 
O2 Li1 O3 95.8(3) 11_455 . ? 
O1 Li1 Li1 41.4(3) 12_665 12_665 ? 
O1 Li1 Li1 118.7(4) . 12_665 ? 
O2 Li1 Li1 117.6(3) 11_455 12_665 ? 
O3 Li1 Li1 54.91(7) . 12_665 ? 
O1 Li1 Li1 118.7(4) 12_665 11_455 ? 
O1 Li1 Li1 41.4(3) . 11_455 ? 
O2 Li1 Li1 117.1(3) 11_455 11_455 ? 
O3 Li1 Li1 54.91(7) . 11_455 ? 
Li1 Li1 Li1 90.7(3) 12_665 11_455 ? 
O1 Li1 Li2 117.8(3) 12_665 10_575 ? 
O1 Li1 Li2 117.6(3) . 10_575 ? 
O2 Li1 Li2 40.8(2) 11_455 10_575 ? 
O3 Li1 Li2 55.0(2) . 10_575 ? 
Li1 Li1 Li2 90.1(2) 12_665 10_575 ? 
Li1 Li1 Li2 90.1(2) 11_455 10_575 ? 
O1 Li1 K1 61.2(2) 12_665 12_665 ? 
O1 Li1 K1 178.9(4) . 12_665 ? 
O2 Li1 K1 61.22(19) 11_455 12_665 ? 
O3 Li1 K1 82.9(2) . 12_665 ? 
Li1 Li1 K1 61.40(17) 12_665 12_665 ? 
Li1 Li1 K1 137.85(19) 11_455 12_665 ? 
Li2 Li1 K1 61.30(14) 10_575 12_665 ? 
O1 Li1 K1 178.9(4) 12_665 11_455 ? 
O1 Li1 K1 61.1(2) . 11_455 ? 
O2 Li1 K1 60.74(19) 11_455 11_455 ? 
O3 Li1 K1 82.8(2) . 11_455 ? 
Li1 Li1 K1 137.71(18) 12_665 11_455 ? 
Li1 Li1 K1 61.31(17) 11_455 11_455 ? 
Li2 Li1 K1 61.22(14) 10_575 11_455 ? 
K1 Li1 K1 118.0(2) 12_665 11_455 ? 
O2 Li2 O2 119.01(13) 3_465 . ? 
O2 Li2 O2 119.01(13) 3_465 2_675 ? 
O2 Li2 O2 119.01(13) . 2_675 ? 
O2 Li2 O3 95.7(4) 3_465 . ? 
O2 Li2 O3 95.7(4) . . ? 
O2 Li2 O3 95.7(4) 2_675 . ? 
O2 Li2 Li1 41.6(2) 3_465 11_455 ? 
O2 Li2 Li1 117.3(3) . 11_455 ? 
O2 Li2 Li1 117.7(3) 2_675 11_455 ? 
O3 Li2 Li1 54.1(2) . 11_455 ? 
O2 Li2 Li1 117.7(3) 3_465 12_665 ? 
O2 Li2 Li1 41.6(2) . 12_665 ? 
O2 Li2 Li1 117.3(3) 2_675 12_665 ? 
O3 Li2 Li1 54.1(2) . 12_665 ? 
Li1 Li2 Li1 89.1(3) 11_455 12_665 ? 
O2 Li2 Li1 117.3(3) 3_465 10_575 ? 
O2 Li2 Li1 117.7(3) . 10_575 ? 
O2 Li2 Li1 41.6(2) 2_675 10_575 ? 
O3 Li2 Li1 54.1(2) . 10_575 ? 
Li1 Li2 Li1 89.1(3) 11_455 10_575 ? 
Li1 Li2 Li1 89.1(3) 12_665 10_575 ? 
O2 Li2 K1 61.13(8) 3_465 3_465 ? 
O2 Li2 K1 178.3(6) . 3_465 ? 
O2 Li2 K1 61.45(8) 2_675 3_465 ? 
O3 Li2 K1 82.5(2) . 3_465 ? 
Li1 Li2 K1 61.55(17) 11_455 3_465 ? 
Li1 Li2 K1 136.7(4) 12_665 3_465 ? 
Li1 Li2 K1 61.38(17) 10_575 3_465 ? 
O2 Li2 K1 178.3(6) 3_465 2_675 ? 
O2 Li2 K1 61.45(8) . 2_675 ? 
O2 Li2 K1 61.13(8) 2_675 2_675 ? 
O3 Li2 K1 82.5(2) . 2_675 ? 
Li1 Li2 K1 136.7(4) 11_455 2_675 ? 
Li1 Li2 K1 61.38(17) 12_665 2_675 ? 
Li1 Li2 K1 61.55(17) 10_575 2_675 ? 
K1 Li2 K1 118.34(10) 3_465 2_675 ? 
N1 C2 C1 112.7(8) . . ? 
C1 C2A N1 112.5(8) . . ? 
C11 C11 C11 60.000(18) 3_465 2_675 ? 
C11 C11 C10 66(3) 3_465 . ? 
C11 C11 C10 101(2) 2_675 . ? 
C11 C11 C10 99(3) 3_465 2_675 ? 
C11 C11 C10 64(4) 2_675 2_675 ? 
C10 C11 C10 74(2) . 2_675 ? 
C10 O4 C10 94(2) 3_465 . ? 
C10 O4 C10 94(2) 3_465 2_675 ? 
C10 O4 C10 94(2) . 2_675 ? 
O4 C10 C11 93(3) . . ? 
O4 C10 C11 92(3) . 3_465 ? 
C11 C10 C11 50(2) . 3_465 ? 
O4 C10 C10 43.1(10) . 3_465 ? 
C11 C10 C10 80.3(15) . 3_465 ? 
C11 C10 C10 52(2) 3_465 3_465 ? 
O4 C10 C10 43.1(10) . 2_675 ? 
C11 C10 C10 54(2) . 2_675 ? 
C11 C10 C10 79.5(14) 3_465 2_675 ? 
C10 C10 C10 60.000(19) 3_465 2_675 ? 
C9 C9 C9 60.00(2) 3_565 2_665 ? 
C9 C9 C9 90.000(8) 3_565 15 ? 
C9 C9 C9 67.3(8) 2_665 15 ? 
C9 C9 C9 67.3(8) 3_565 14_455 ? 
C9 C9 C9 90.002(6) 2_665 14_455 ? 
C9 C9 C9 45.5(16) 15 14_455 ? 

_diffrn_measured_fraction_theta_max    0.989 
_diffrn_reflns_theta_full              28.27 
_diffrn_measured_fraction_theta_full   0.989 
_refine_diff_density_max    0.527 
_refine_diff_density_min   -0.333 
_refine_diff_density_rms    0.062