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


data_stl04

_database_code_CSD	189782


_journal_coden_Cambridge      186


loop_
_publ_author_name
'William Clegg'
'Stephen T. Liddle'

_publ_contact_author_name     	'Prof William Clegg'  
_publ_contact_author_address 
;
Deparrtment of Chemistry
University of Newcastle
Newcastle upon Tyne
NE1 7RU
UNITED KINGDOM
;

_publ_contact_author_email       'W.CKEGG@NEWCASTLE.AC.UK'

_publ_requested_journal       'Dalton Transactions'


_publ_section_title		
;
Synthesis and structure of the novel octanuclear
lithium aryloxide cluster [(hmqLi)8(THF)4] (hmq =
2-hydroxy-4-methylquinoline monoanion): formation of a rare four-rung
intercepted Li-O ladder
;

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C112 H128 Li8 N8 O16'
_chemical_formula_weight          1897.74

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            triclinic
_symmetry_space_group_name_H-M    P-1

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

_cell_length_a                    12.5281(14)
_cell_length_b                    13.7330(15)
_cell_length_c                    16.4814(18)
_cell_angle_alpha                 77.117(2)
_cell_angle_beta                  68.609(2)
_cell_angle_gamma                 83.432(3)
_cell_volume                      2572.1(5)
_cell_formula_units_Z             1
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     4751
_cell_measurement_theta_min       2.55
_cell_measurement_theta_max       28.18

_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.42
_exptl_crystal_size_mid           0.22
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.225
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1008
_exptl_absorpt_coefficient_mu     0.080
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.6223
_exptl_absorpt_correction_T_max   0.9549
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       160(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   'Siemens SMART CCD diffractometer'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             11076
_diffrn_reflns_av_R_equivalents   0.0612
_diffrn_reflns_av_sigmaI/netI     0.2169
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          2.13
_diffrn_reflns_theta_max          25.00
_reflns_number_total              8406
_reflns_number_gt                 3257
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Siemens SMART'
_computing_cell_refinement        'local programs'
_computing_data_reduction         'Siemens SAINT'
_computing_structure_solution     'Siemens SHELXTL'
_computing_structure_refinement   'Siemens SHELXTL'
_computing_molecular_graphics     'Siemens SHELXTL'
_computing_publication_material   'SHELXTL and local programs'

_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^)+(0.0990P)^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      SHELXL
_refine_ls_extinction_coef        0.0042(11)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          8406
_refine_ls_number_parameters      654
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2139
_refine_ls_R_factor_gt            0.0784
_refine_ls_wR_factor_ref          0.2221
_refine_ls_wR_factor_gt           0.1676
_refine_ls_goodness_of_fit_ref    0.910
_refine_ls_restrained_S_all       0.910
_refine_ls_shift/su_max           0.012
_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
Li1 Li 0.6010(8) 0.6548(7) 0.6338(6) 0.029(2) Uani 1 1 d . . .
Li2 Li 0.7622(8) 0.5956(7) 0.4629(6) 0.027(2) Uani 1 1 d . . .
Li3 Li 0.5475(8) 0.6967(7) 0.4685(6) 0.030(2) Uani 1 1 d . . .
Li4 Li 0.4089(8) 0.5530(7) 0.5013(6) 0.031(2) Uani 1 1 d . . .
O1 O 0.6721(3) 0.7129(3) 0.5029(2) 0.0246(9) Uani 1 1 d . . .
N1 N 0.7152(4) 0.7800(3) 0.5992(3) 0.0247(11) Uani 1 1 d . . .
C1 C 0.7119(4) 0.7890(4) 0.5182(3) 0.0221(13) Uani 1 1 d . . .
C2 C 0.7502(4) 0.8758(4) 0.4506(4) 0.0264(14) Uani 1 1 d . . .
H2 H 0.7455 0.8795 0.3937 0.032 Uiso 1 1 calc R . .
C3 C 0.7931(5) 0.9529(4) 0.4666(4) 0.0325(15) Uani 1 1 d . . .
C4 C 0.8312(6) 1.0459(5) 0.3956(4) 0.055(2) Uani 1 1 d . . .
H4A H 0.8223 1.0373 0.3409 0.083 Uiso 1 1 calc R . .
H4B H 0.9119 1.0567 0.3838 0.083 Uiso 1 1 calc R . .
H4C H 0.7840 1.1037 0.4159 0.083 Uiso 1 1 calc R . .
C5 C 0.8033(5) 0.9436(4) 0.5514(4) 0.0315(15) Uani 1 1 d . . .
C6 C 0.8515(5) 1.0171(5) 0.5742(5) 0.0447(17) Uani 1 1 d . . .
H6 H 0.8798 1.0760 0.5316 0.054 Uiso 1 1 calc R . .
C7 C 0.8579(5) 1.0043(5) 0.6561(5) 0.052(2) Uani 1 1 d . . .
H7 H 0.8897 1.0550 0.6704 0.062 Uiso 1 1 calc R . .
C8 C 0.8185(5) 0.9180(5) 0.7205(5) 0.0508(19) Uani 1 1 d . . .
H8 H 0.8245 0.9101 0.7774 0.061 Uiso 1 1 calc R . .
C9 C 0.7711(5) 0.8446(5) 0.7006(4) 0.0426(17) Uani 1 1 d . . .
H9 H 0.7443 0.7859 0.7440 0.051 Uiso 1 1 calc R . .
C10 C 0.7624(4) 0.8565(4) 0.6154(4) 0.0265(14) Uani 1 1 d . . .
O2 O 0.4142(3) 0.6509(3) 0.5640(2) 0.0280(9) Uani 1 1 d . . .
N2 N 0.4304(4) 0.7064(3) 0.6795(3) 0.0230(11) Uani 1 1 d . . .
C11 C 0.3660(5) 0.6809(4) 0.6384(3) 0.0245(13) Uani 1 1 d . . .
C12 C 0.2426(5) 0.6866(4) 0.6769(3) 0.0277(14) Uani 1 1 d . . .
H12 H 0.1988 0.6666 0.6474 0.033 Uiso 1 1 calc R . .
C13 C 0.1875(4) 0.7192(4) 0.7532(3) 0.0269(14) Uani 1 1 d . . .
C14 C 0.0569(5) 0.7233(5) 0.7939(4) 0.0461(18) Uani 1 1 d . . .
H14A H 0.0249 0.6970 0.7573 0.069 Uiso 1 1 calc R . .
H14B H 0.0294 0.7927 0.7963 0.069 Uiso 1 1 calc R . .
H14C H 0.0326 0.6828 0.8541 0.069 Uiso 1 1 calc R . .
C15 C 0.2549(5) 0.7499(4) 0.7967(3) 0.0255(14) Uani 1 1 d . . .
C16 C 0.2072(5) 0.7872(4) 0.8763(4) 0.0383(16) Uani 1 1 d . . .
H16 H 0.1262 0.7911 0.9043 0.046 Uiso 1 1 calc R . .
C17 C 0.2755(6) 0.8178(5) 0.9140(4) 0.0473(18) Uani 1 1 d . . .
H17 H 0.2421 0.8433 0.9671 0.057 Uiso 1 1 calc R . .
C18 C 0.3941(6) 0.8111(4) 0.8736(4) 0.0395(17) Uani 1 1 d . . .
H18 H 0.4417 0.8323 0.8995 0.047 Uiso 1 1 calc R . .
C19 C 0.4432(5) 0.7741(4) 0.7968(3) 0.0303(14) Uani 1 1 d . . .
H19 H 0.5244 0.7695 0.7705 0.036 Uiso 1 1 calc R . .
C20 C 0.3746(5) 0.7429(4) 0.7567(3) 0.0269(14) Uani 1 1 d . . .
O3 O 0.6918(3) 0.4812(3) 0.5489(2) 0.0235(9) Uani 1 1 d . . .
N3 N 0.6589(3) 0.5143(3) 0.6852(3) 0.0198(11) Uani 1 1 d . . .
C21 C 0.6780(4) 0.4483(4) 0.6321(4) 0.0210(13) Uani 1 1 d . . .
C22 C 0.6839(4) 0.3436(4) 0.6650(3) 0.0232(13) Uani 1 1 d . . .
H22 H 0.6945 0.2992 0.6257 0.028 Uiso 1 1 calc R . .
C23 C 0.6748(4) 0.3048(4) 0.7506(3) 0.0242(13) Uani 1 1 d . . .
C24 C 0.6824(6) 0.1946(4) 0.7847(4) 0.0444(18) Uani 1 1 d . . .
H24A H 0.6914 0.1588 0.7373 0.067 Uiso 1 1 calc R . .
H24B H 0.6122 0.1742 0.8350 0.067 Uiso 1 1 calc R . .
H24C H 0.7486 0.1788 0.8042 0.067 Uiso 1 1 calc R . .
C25 C 0.6608(4) 0.3745(4) 0.8077(3) 0.0234(13) Uani 1 1 d . . .
C26 C 0.6528(5) 0.3452(4) 0.8976(3) 0.0304(15) Uani 1 1 d . . .
H26 H 0.6573 0.2761 0.9224 0.036 Uiso 1 1 calc R . .
C27 C 0.6388(5) 0.4140(5) 0.9494(4) 0.0321(15) Uani 1 1 d . . .
H27 H 0.6350 0.3928 1.0093 0.038 Uiso 1 1 calc R . .
C28 C 0.6301(5) 0.5156(5) 0.9140(4) 0.0339(15) Uani 1 1 d . . .
H28 H 0.6195 0.5634 0.9503 0.041 Uiso 1 1 calc R . .
C29 C 0.6369(5) 0.5471(4) 0.8273(3) 0.0282(14) Uani 1 1 d . . .
H29 H 0.6318 0.6165 0.8039 0.034 Uiso 1 1 calc R . .
C30 C 0.6513(4) 0.4769(4) 0.7724(3) 0.0192(12) Uani 1 1 d . . .
O4 O 0.5691(3) 0.5792(2) 0.4189(2) 0.0209(9) Uani 1 1 d . . .
N4 N 0.7607(3) 0.5730(3) 0.3422(3) 0.0202(10) Uani 1 1 d . . .
C31 C 0.6532(4) 0.5728(4) 0.3443(3) 0.0222(13) Uani 1 1 d . . .
C32 C 0.6303(5) 0.5613(4) 0.2678(3) 0.0236(13) Uani 1 1 d . . .
H32 H 0.5528 0.5599 0.2719 0.028 Uiso 1 1 calc R . .
C33 C 0.7144(4) 0.5525(4) 0.1905(3) 0.0244(13) Uani 1 1 d . . .
C34 C 0.6897(5) 0.5320(5) 0.1135(3) 0.0388(16) Uani 1 1 d . . .
H34A H 0.6067 0.5369 0.1264 0.058 Uiso 1 1 calc R . .
H34B H 0.7188 0.4646 0.1039 0.058 Uiso 1 1 calc R . .
H34C H 0.7275 0.5811 0.0600 0.058 Uiso 1 1 calc R . .
C35 C 0.8315(4) 0.5544(4) 0.1865(3) 0.0250(13) Uani 1 1 d . . .
C36 C 0.9280(5) 0.5468(5) 0.1100(4) 0.0355(16) Uani 1 1 d . . .
H36 H 0.9171 0.5427 0.0567 0.043 Uiso 1 1 calc R . .
C37 C 1.0376(5) 0.5451(5) 0.1104(4) 0.0470(18) Uani 1 1 d . . .
H37 H 1.1018 0.5410 0.0579 0.056 Uiso 1 1 calc R . .
C38 C 1.0538(5) 0.5495(5) 0.1895(4) 0.0394(17) Uani 1 1 d . . .
H38 H 1.1293 0.5468 0.1908 0.047 Uiso 1 1 calc R . .
C39 C 0.9618(5) 0.5576(4) 0.2643(4) 0.0316(15) Uani 1 1 d . . .
H39 H 0.9743 0.5597 0.3173 0.038 Uiso 1 1 calc R . .
C40 C 0.8487(4) 0.5630(4) 0.2649(3) 0.0245(13) Uani 1 1 d . . .
O5 O 0.9137(3) 0.6193(3) 0.4704(2) 0.0285(10) Uani 1 1 d . . .
C41 C 0.9926(5) 0.6961(4) 0.4160(4) 0.0399(16) Uani 1 1 d . . .
H41A H 0.9547 0.7494 0.3835 0.048 Uiso 1 1 calc R . .
H41B H 1.0594 0.6680 0.3722 0.048 Uiso 1 1 calc R . .
C42 C 1.0304(5) 0.7374(5) 0.4788(4) 0.0432(17) Uani 1 1 d . . .
H42A H 1.1087 0.7634 0.4491 0.052 Uiso 1 1 calc R . .
H42B H 0.9766 0.7910 0.5034 0.052 Uiso 1 1 calc R . .
C43 C 1.0273(5) 0.6458(5) 0.5500(4) 0.0403(17) Uani 1 1 d . . .
H43A H 1.0190 0.6643 0.6067 0.048 Uiso 1 1 calc R . .
H43B H 1.0974 0.6027 0.5316 0.048 Uiso 1 1 calc R . .
C44 C 0.9220(4) 0.5944(4) 0.5579(3) 0.0295(14) Uani 1 1 d . . .
H44A H 0.9307 0.5212 0.5766 0.035 Uiso 1 1 calc R . .
H44B H 0.8525 0.6190 0.6021 0.035 Uiso 1 1 calc R . .
O6 O 0.5163(4) 0.8183(3) 0.3933(3) 0.0430(11) Uani 1 1 d . . .
C45 C 0.4657(7) 0.9052(5) 0.4316(5) 0.064(2) Uani 1 1 d . . .
H45A H 0.4874 0.9057 0.4835 0.077 Uiso 1 1 calc R . .
H45B H 0.3810 0.9057 0.4509 0.077 Uiso 1 1 calc R . .
C46 C 0.5124(6) 0.9941(5) 0.3589(5) 0.057(2) Uani 1 1 d . . .
H46A H 0.4582 1.0527 0.3657 0.069 Uiso 1 1 calc R . .
H46B H 0.5874 1.0124 0.3573 0.069 Uiso 1 1 calc R . .
C47 C 0.5243(8) 0.9555(5) 0.2787(5) 0.081(3) Uani 1 1 d . . .
H47A H 0.5837 0.9916 0.2256 0.097 Uiso 1 1 calc R . .
H47B H 0.4507 0.9633 0.2680 0.097 Uiso 1 1 calc R . .
C48 C 0.5593(6) 0.8457(5) 0.2988(4) 0.053(2) Uani 1 1 d . . .
H48A H 0.5251 0.8053 0.2724 0.064 Uiso 1 1 calc R . .
H48B H 0.6438 0.8360 0.2752 0.064 Uiso 1 1 calc R . .
O7 O 0.0868(7) 0.9022(7) 1.1205(7) 0.169(4) Uani 1 1 d . . .
C49 C -0.0036(12) 0.9714(10) 1.1506(10) 0.182(7) Uani 1 1 d . . .
H49A H 0.0100 1.0359 1.1078 0.218 Uiso 1 1 calc R . .
H49B H -0.0073 0.9831 1.2087 0.218 Uiso 1 1 calc R . .
C50 C -0.1083(11) 0.9334(8) 1.1593(9) 0.142(5) Uani 1 1 d . . .
H50A H -0.1308 0.9631 1.1072 0.170 Uiso 1 1 calc R . .
H50B H -0.1704 0.9474 1.2137 0.170 Uiso 1 1 calc R . .
C51 C -0.0845(11) 0.8252(8) 1.1650(11) 0.169(6) Uani 1 1 d . . .
H51A H -0.1256 0.7885 1.2258 0.202 Uiso 1 1 calc R . .
H51B H -0.1096 0.8013 1.1226 0.202 Uiso 1 1 calc R . .
C52 C 0.0350(12) 0.8101(8) 1.1436(8) 0.151(5) Uani 1 1 d . . .
H52A H 0.0516 0.7682 1.1952 0.181 Uiso 1 1 calc R . .
H52B H 0.0667 0.7745 1.0932 0.181 Uiso 1 1 calc R . .
O8 O 0.7937(13) 0.8687(16) 0.9520(10) 0.298(7) Uani 1 1 d . . .
C53 C 0.6800(17) 0.9342(11) 1.0105(14) 0.243(11) Uani 1 1 d . . .
H53A H 0.6652 0.9174 1.0751 0.291 Uiso 1 1 calc R . .
H53B H 0.6863 1.0073 0.9887 0.291 Uiso 1 1 calc R . .
C54 C 0.5939(16) 0.8911(13) 0.9853(12) 0.223(8) Uani 1 1 d . . .
H54A H 0.5134 0.9044 1.0221 0.267 Uiso 1 1 calc R . .
H54B H 0.6050 0.9108 0.9213 0.267 Uiso 1 1 calc R . .
C55 C 0.6363(12) 0.7898(10) 1.0103(15) 0.269(12) Uani 1 1 d . . .
H55A H 0.5917 0.7629 1.0733 0.323 Uiso 1 1 calc R . .
H55B H 0.6239 0.7469 0.9738 0.323 Uiso 1 1 calc R . .
C56 C 0.7392(18) 0.7858(12) 1.0003(17) 0.315(17) Uani 1 1 d . . .
H56A H 0.7770 0.7289 0.9713 0.378 Uiso 1 1 calc R . .
H56B H 0.7469 0.7727 1.0596 0.378 Uiso 1 1 calc R . .

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
Li1 0.026(6) 0.034(6) 0.033(5) -0.005(5) -0.018(4) 0.001(5)
Li2 0.026(5) 0.038(6) 0.025(5) -0.007(4) -0.012(4) -0.011(5)
Li3 0.024(5) 0.028(6) 0.039(6) -0.005(5) -0.015(5) 0.001(4)
Li4 0.030(6) 0.044(6) 0.022(5) -0.013(5) -0.010(4) 0.001(5)
O1 0.018(2) 0.026(2) 0.032(2) -0.0096(18) -0.0094(17) -0.0020(17)
N1 0.022(3) 0.025(3) 0.028(3) -0.010(2) -0.009(2) 0.003(2)
C1 0.010(3) 0.023(3) 0.031(3) -0.010(3) -0.004(2) 0.008(3)
C2 0.018(3) 0.024(3) 0.031(3) 0.001(3) -0.006(3) 0.002(3)
C3 0.018(3) 0.030(4) 0.044(4) -0.002(3) -0.007(3) 0.001(3)
C4 0.042(4) 0.041(4) 0.072(5) 0.002(4) -0.012(4) -0.009(3)
C5 0.021(3) 0.027(4) 0.045(4) -0.014(3) -0.007(3) 0.004(3)
C6 0.030(4) 0.038(4) 0.070(5) -0.024(4) -0.014(3) 0.001(3)
C7 0.035(4) 0.051(5) 0.082(6) -0.039(4) -0.020(4) -0.003(4)
C8 0.036(4) 0.065(5) 0.069(5) -0.039(4) -0.026(4) 0.004(4)
C9 0.038(4) 0.050(4) 0.047(4) -0.019(3) -0.019(3) 0.002(3)
C10 0.013(3) 0.033(4) 0.037(3) -0.020(3) -0.007(3) 0.004(3)
O2 0.024(2) 0.037(2) 0.023(2) -0.0125(19) -0.0032(17) -0.0040(18)
N2 0.017(3) 0.028(3) 0.024(2) -0.006(2) -0.007(2) -0.001(2)
C11 0.024(3) 0.027(3) 0.024(3) -0.007(3) -0.008(3) -0.004(3)
C12 0.022(3) 0.029(4) 0.032(3) -0.006(3) -0.011(3) 0.003(3)
C13 0.014(3) 0.037(4) 0.026(3) -0.011(3) -0.001(3) 0.005(3)
C14 0.020(4) 0.068(5) 0.047(4) -0.020(4) -0.002(3) 0.000(3)
C15 0.027(3) 0.025(3) 0.019(3) -0.005(3) -0.004(3) 0.006(3)
C16 0.036(4) 0.042(4) 0.034(4) -0.009(3) -0.013(3) 0.011(3)
C17 0.063(5) 0.050(5) 0.028(4) -0.013(3) -0.014(4) 0.008(4)
C18 0.062(5) 0.035(4) 0.028(4) -0.006(3) -0.024(3) -0.002(4)
C19 0.034(4) 0.033(4) 0.028(3) -0.003(3) -0.017(3) -0.002(3)
C20 0.037(4) 0.023(3) 0.020(3) -0.004(3) -0.010(3) 0.001(3)
O3 0.020(2) 0.033(2) 0.018(2) -0.0031(18) -0.0076(16) -0.0030(17)
N3 0.014(2) 0.029(3) 0.019(2) -0.002(2) -0.0112(19) -0.001(2)
C21 0.005(3) 0.032(4) 0.026(3) -0.005(3) -0.005(2) -0.004(2)
C22 0.021(3) 0.027(4) 0.022(3) -0.010(3) -0.006(2) 0.007(3)
C23 0.017(3) 0.028(4) 0.024(3) 0.002(3) -0.008(2) 0.003(3)
C24 0.068(5) 0.032(4) 0.036(4) -0.005(3) -0.025(4) 0.008(3)
C25 0.020(3) 0.031(4) 0.022(3) -0.002(3) -0.012(2) 0.003(3)
C26 0.031(4) 0.032(4) 0.024(3) 0.007(3) -0.011(3) -0.002(3)
C27 0.029(4) 0.050(4) 0.021(3) -0.011(3) -0.012(3) 0.000(3)
C28 0.024(4) 0.052(5) 0.030(4) -0.017(3) -0.010(3) 0.000(3)
C29 0.031(4) 0.028(4) 0.028(3) -0.008(3) -0.012(3) 0.002(3)
C30 0.007(3) 0.029(4) 0.022(3) -0.005(3) -0.008(2) 0.006(2)
O4 0.015(2) 0.030(2) 0.0173(19) -0.0028(17) -0.0053(16) -0.0018(17)
N4 0.010(2) 0.032(3) 0.017(2) -0.005(2) -0.0040(19) 0.000(2)
C31 0.019(3) 0.021(3) 0.018(3) 0.000(2) 0.001(3) -0.002(3)
C32 0.019(3) 0.037(4) 0.018(3) -0.007(3) -0.010(3) -0.001(3)
C33 0.021(3) 0.039(4) 0.013(3) -0.003(3) -0.006(2) -0.004(3)
C34 0.027(4) 0.070(5) 0.026(3) -0.019(3) -0.013(3) 0.002(3)
C35 0.019(3) 0.037(4) 0.020(3) -0.011(3) -0.005(2) 0.000(3)
C36 0.019(3) 0.065(5) 0.024(3) -0.016(3) -0.005(3) -0.003(3)
C37 0.026(4) 0.083(5) 0.029(4) -0.028(4) 0.003(3) -0.001(4)
C38 0.015(3) 0.069(5) 0.036(4) -0.018(4) -0.009(3) 0.005(3)
C39 0.025(4) 0.047(4) 0.029(3) -0.013(3) -0.016(3) 0.003(3)
C40 0.020(3) 0.035(4) 0.020(3) -0.006(3) -0.009(3) -0.001(3)
O5 0.022(2) 0.036(2) 0.030(2) -0.0027(19) -0.0126(18) -0.0067(18)
C41 0.027(4) 0.043(4) 0.043(4) 0.000(3) -0.009(3) -0.001(3)
C42 0.022(4) 0.040(4) 0.063(4) -0.018(4) -0.002(3) -0.011(3)
C43 0.026(4) 0.057(5) 0.050(4) -0.025(4) -0.020(3) 0.002(3)
C44 0.015(3) 0.040(4) 0.033(3) -0.007(3) -0.008(3) 0.001(3)
O6 0.050(3) 0.035(3) 0.040(3) -0.002(2) -0.017(2) 0.010(2)
C45 0.068(6) 0.048(5) 0.062(5) -0.005(4) -0.017(4) 0.027(4)
C46 0.053(5) 0.043(5) 0.073(5) -0.007(4) -0.023(4) 0.008(4)
C47 0.134(9) 0.043(5) 0.071(6) 0.013(4) -0.054(6) -0.017(5)
C48 0.069(5) 0.050(5) 0.036(4) 0.003(4) -0.021(4) 0.000(4)
O7 0.098(7) 0.107(7) 0.257(11) -0.020(7) -0.021(7) 0.003(6)
C49 0.110(11) 0.153(12) 0.32(2) -0.163(14) -0.067(12) 0.042(10)
C50 0.119(11) 0.085(9) 0.252(16) -0.036(9) -0.103(11) 0.015(8)
C51 0.107(11) 0.073(9) 0.34(2) -0.013(10) -0.110(13) 0.010(8)
C52 0.126(12) 0.071(8) 0.174(12) 0.006(8) 0.030(9) -0.022(8)
O8 0.221(16) 0.37(2) 0.295(17) -0.005(17) -0.105(13) -0.064(17)
C53 0.191(18) 0.158(15) 0.43(3) -0.226(19) -0.079(19) 0.003(12)
C54 0.25(2) 0.158(15) 0.29(2) -0.045(15) -0.169(18) 0.111(16)
C55 0.062(9) 0.095(11) 0.57(4) -0.020(16) -0.043(15) 0.008(8)
C56 0.166(19) 0.146(14) 0.56(4) 0.20(2) -0.17(2) -0.110(14)

_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
Li1 O1 2.020(10) . ?
Li1 N1 2.205(10) . ?
Li1 N2 2.086(10) . ?
Li1 N3 2.090(10) . ?
Li2 O1 1.955(10) . ?
Li2 O3 1.915(9) . ?
Li2 N4 2.087(9) . ?
Li2 O5 2.013(9) . ?
Li3 O1 1.894(10) . ?
Li3 O2 1.883(10) . ?
Li3 O4 1.916(10) . ?
Li3 O6 1.938(10) . ?
Li4 O2 1.889(10) . ?
Li4 O3 1.888(9) 2_666 ?
Li4 O4 1.990(10) . ?
Li4 O4 2.046(10) 2_666 ?
O1 C1 1.317(6) . ?
N1 C1 1.329(6) . ?
N1 C10 1.380(6) . ?
C1 C2 1.429(7) . ?
C2 C3 1.357(7) . ?
C3 C4 1.514(8) . ?
C3 C5 1.424(8) . ?
C5 C6 1.415(8) . ?
C5 C10 1.411(8) . ?
C6 C7 1.353(9) . ?
C7 C8 1.402(9) . ?
C8 C9 1.379(8) . ?
C9 C10 1.420(8) . ?
O2 C11 1.291(6) . ?
N2 C11 1.342(6) . ?
N2 C20 1.384(6) . ?
C11 C12 1.441(7) . ?
C12 C13 1.343(7) . ?
C13 C14 1.525(7) . ?
C13 C15 1.435(7) . ?
C15 C16 1.414(7) . ?
C15 C20 1.402(7) . ?
C16 C17 1.372(8) . ?
C17 C18 1.390(9) . ?
C18 C19 1.373(7) . ?
C19 C20 1.409(7) . ?
O3 Li4 1.888(9) 2_666 ?
O3 C21 1.297(6) . ?
N3 C21 1.341(6) . ?
N3 C30 1.385(6) . ?
C21 Li4 2.790(10) 2_666 ?
C21 C22 1.423(7) . ?
C22 C23 1.360(7) . ?
C23 C24 1.497(7) . ?
C23 C25 1.442(7) . ?
C25 C26 1.414(7) . ?
C25 C30 1.406(7) . ?
C26 C27 1.366(7) . ?
C27 C28 1.395(8) . ?
C28 C29 1.372(7) . ?
C29 C30 1.418(7) . ?
O4 Li4 2.046(10) 2_666 ?
O4 C31 1.309(5) . ?
N4 C31 1.334(6) . ?
N4 C40 1.370(6) . ?
C31 Li4 2.640(10) 2_666 ?
C31 C32 1.435(7) . ?
C32 C33 1.346(7) . ?
C33 C34 1.500(7) . ?
C33 C35 1.446(7) . ?
C35 C36 1.408(7) . ?
C35 C40 1.418(7) . ?
C36 C37 1.373(8) . ?
C37 C38 1.405(7) . ?
C38 C39 1.362(7) . ?
C39 C40 1.407(7) . ?
O5 C41 1.437(6) . ?
O5 C44 1.447(6) . ?
C41 C42 1.517(7) . ?
C42 C43 1.509(8) . ?
C43 C44 1.517(7) . ?
O6 C45 1.447(7) . ?
O6 C48 1.425(7) . ?
C45 C46 1.506(9) . ?
C46 C47 1.483(9) . ?
C47 C48 1.520(9) . ?
O7 C49 1.409(12) . ?
O7 C52 1.400(11) . ?
C49 C50 1.413(14) . ?
C50 C51 1.470(12) . ?
C51 C52 1.409(14) . ?
O8 C53 1.69(2) . ?
O8 C56 1.332(17) . ?
C53 C54 1.504(18) . ?
C54 C55 1.457(16) . ?
C55 C56 1.235(17) . ?

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
O1 Li1 N1 64.1(3) . . ?
O1 Li1 N2 108.9(4) . . ?
O1 Li1 N3 119.4(5) . . ?
N1 Li1 N2 109.5(4) . . ?
N1 Li1 N3 116.7(4) . . ?
N2 Li1 N3 123.4(5) . . ?
O1 Li2 O3 106.7(4) . . ?
O1 Li2 N4 114.6(5) . . ?
O1 Li2 O5 100.7(4) . . ?
O3 Li2 N4 105.2(4) . . ?
O3 Li2 O5 111.0(5) . . ?
N4 Li2 O5 118.1(5) . . ?
O1 Li3 O2 114.2(5) . . ?
O1 Li3 O4 111.6(5) . . ?
O1 Li3 O6 110.6(5) . . ?
O2 Li3 O4 93.7(4) . . ?
O2 Li3 O6 111.7(5) . . ?
O4 Li3 O6 114.3(5) . . ?
O2 Li4 O3 137.2(6) . 2_666 ?
O2 Li4 O4 91.1(4) . . ?
O2 Li4 O4 103.8(4) . 2_666 ?
O3 Li4 O4 115.9(4) 2_666 . ?
O3 Li4 O4 102.4(5) 2_666 2_666 ?
O4 Li4 O4 101.4(4) . 2_666 ?
Li1 O1 Li2 99.3(4) . . ?
Li1 O1 Li3 98.1(4) . . ?
Li1 O1 C1 92.5(4) . . ?
Li2 O1 Li3 96.1(4) . . ?
Li2 O1 C1 125.8(4) . . ?
Li3 O1 C1 134.4(4) . . ?
Li1 N1 C1 84.3(4) . . ?
Li1 N1 C10 155.7(4) . . ?
C1 N1 C10 117.4(5) . . ?
O1 C1 N1 116.4(5) . . ?
O1 C1 C2 121.2(5) . . ?
N1 C1 C2 122.3(5) . . ?
C1 C2 C3 120.7(5) . . ?
C2 C3 C4 120.7(6) . . ?
C2 C3 C5 118.4(5) . . ?
C4 C3 C5 120.9(6) . . ?
C3 C5 C6 123.4(6) . . ?
C3 C5 C10 117.8(5) . . ?
C6 C5 C10 118.8(6) . . ?
C5 C6 C7 120.6(6) . . ?
C6 C7 C8 121.5(6) . . ?
C7 C8 C9 119.6(7) . . ?
C8 C9 C10 120.1(6) . . ?
N1 C10 C5 123.2(5) . . ?
N1 C10 C9 117.4(5) . . ?
C5 C10 C9 119.4(5) . . ?
Li3 O2 Li4 87.7(4) . . ?
Li3 O2 C11 128.8(4) . . ?
Li4 O2 C11 143.3(4) . . ?
Li1 N2 C11 113.7(4) . . ?
Li1 N2 C20 126.8(4) . . ?
C11 N2 C20 117.8(5) . . ?
O2 C11 N2 120.2(5) . . ?
O2 C11 C12 119.4(5) . . ?
N2 C11 C12 120.4(5) . . ?
C11 C12 C13 122.2(5) . . ?
C12 C13 C14 121.6(5) . . ?
C12 C13 C15 118.3(5) . . ?
C14 C13 C15 120.2(5) . . ?
C13 C15 C16 123.7(5) . . ?
C13 C15 C20 117.4(5) . . ?
C16 C15 C20 118.9(5) . . ?
C15 C16 C17 121.3(6) . . ?
C16 C17 C18 119.4(6) . . ?
C17 C18 C19 120.7(6) . . ?
C18 C19 C20 120.8(6) . . ?
N2 C20 C15 123.8(5) . . ?
N2 C20 C19 117.3(5) . . ?
C15 C20 C19 118.9(5) . . ?
Li2 O3 Li4 101.3(4) . 2_666 ?
Li2 O3 C21 134.1(4) . . ?
Li4 O3 C21 121.2(4) 2_666 . ?
Li1 N3 C21 113.1(4) . . ?
Li1 N3 C30 127.3(4) . . ?
C21 N3 C30 117.4(4) . . ?
Li4 C21 O3 35.4(3) 2_666 . ?
Li4 C21 N3 129.8(4) 2_666 . ?
Li4 C21 C22 99.3(4) 2_666 . ?
O3 C21 N3 118.9(5) . . ?
O3 C21 C22 119.7(5) . . ?
N3 C21 C22 121.4(5) . . ?
C21 C22 C23 122.3(5) . . ?
C22 C23 C24 122.2(5) . . ?
C22 C23 C25 117.3(5) . . ?
C24 C23 C25 120.5(5) . . ?
C23 C25 C26 123.5(5) . . ?
C23 C25 C30 117.7(5) . . ?
C26 C25 C30 118.7(5) . . ?
C25 C26 C27 121.5(5) . . ?
C26 C27 C28 119.7(5) . . ?
C27 C28 C29 120.6(6) . . ?
C28 C29 C30 120.6(5) . . ?
N3 C30 C25 123.7(5) . . ?
N3 C30 C29 117.3(5) . . ?
C25 C30 C29 118.9(5) . . ?
Li3 O4 Li4 84.0(4) . . ?
Li3 O4 Li4 116.2(4) . 2_666 ?
Li3 O4 C31 120.1(4) . . ?
Li4 O4 Li4 78.6(4) . 2_666 ?
Li4 O4 C31 151.2(4) . . ?
Li4 O4 C31 101.5(4) 2_666 . ?
Li2 N4 C31 110.7(4) . . ?
Li2 N4 C40 131.0(4) . . ?
C31 N4 C40 118.3(4) . . ?
Li4 C31 O4 49.4(3) 2_666 . ?
Li4 C31 N4 92.1(4) 2_666 . ?
Li4 C31 C32 124.6(4) 2_666 . ?
O4 C31 N4 118.4(5) . . ?
O4 C31 C32 120.6(5) . . ?
N4 C31 C32 120.9(4) . . ?
C31 C32 C33 122.4(5) . . ?
C32 C33 C34 121.9(5) . . ?
C32 C33 C35 117.4(5) . . ?
C34 C33 C35 120.5(4) . . ?
C33 C35 C36 123.8(5) . . ?
C33 C35 C40 117.5(4) . . ?
C36 C35 C40 118.7(5) . . ?
C35 C36 C37 121.6(5) . . ?
C36 C37 C38 119.2(5) . . ?
C37 C38 C39 120.3(5) . . ?
C38 C39 C40 121.7(5) . . ?
N4 C40 C35 123.3(5) . . ?
N4 C40 C39 118.3(5) . . ?
C35 C40 C39 118.3(5) . . ?
Li2 O5 C41 127.6(4) . . ?
Li2 O5 C44 116.4(4) . . ?
C41 O5 C44 109.2(4) . . ?
O5 C41 C42 106.2(4) . . ?
C41 C42 C43 101.5(5) . . ?
C42 C43 C44 102.6(5) . . ?
O5 C44 C43 105.6(4) . . ?
Li3 O6 C45 119.6(4) . . ?
Li3 O6 C48 128.8(5) . . ?
C45 O6 C48 110.0(5) . . ?
O6 C45 C46 105.6(5) . . ?
C45 C46 C47 101.5(6) . . ?
C46 C47 C48 105.0(6) . . ?
O6 C48 C47 104.9(6) . . ?
C49 O7 C52 105.2(10) . . ?
O7 C49 C50 109.4(10) . . ?
C49 C50 C51 104.4(10) . . ?
C50 C51 C52 106.4(10) . . ?
O7 C52 C51 109.9(10) . . ?
C53 O8 C56 87.6(15) . . ?
O8 C53 C54 94.9(11) . . ?
C53 C54 C55 91.2(13) . . ?
C54 C55 C56 112.6(15) . . ?
O8 C56 C55 113.9(17) . . ?

_diffrn_measured_fraction_theta_max    0.927
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.927
_refine_diff_density_max    0.418
_refine_diff_density_min   -0.381
_refine_diff_density_rms    0.066