# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Dominic S. Wright'
_publ_contact_author_address     
;
Department of Chemistry
University of Cambridge
Lensfield Road
Cambridge
CB2 1EW
UNITED KINGDOM
;

_publ_contact_author_email       DSW1000@CAM.AC.UK

_publ_section_title              
;
Direct Synthesis of the 1,2,3-[C6H4P...P...P]- Anion,
Isoelectronic with the Indenyl Anion [C6H4CH...CH...CH]-
;
loop_
_publ_author_name
'Dominic S. Wright'
'Felipe Garcia'
'Robert J. Less'
'M. McPartlin'
'Vesal Naseri'
'J. Rawson'
;
M.S.Tomas
;

# Attachment '2.cif'

# Attachment 'compound2.CIF'

data_dw0752
_database_code_depnum_ccdc_archive 'CCDC 668765'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C16 H32 Li O8), Sb11'
_chemical_formula_sum            'C48 H96 Li3 O24 Sb11'
_chemical_formula_weight         2417.32

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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           rhombohedral
_symmetry_space_group_name_H-M   R3

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'

_cell_length_a                   21.138(2)
_cell_length_b                   21.138(2)
_cell_length_c                   32.330(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12510.2(18)
_cell_formula_units_Z            6
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    4653
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      22.46

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6876
_exptl_absorpt_coefficient_mu    3.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
Poor (small, poorly diffracting) crystals. Poor data. The Sb11 units
conform to space group R-3 but no solution for the crown ether moities
could be obtained in this setting. Common, isotropic displacement
parameters were assigned to the Li, O and C atoms. The crown ether
moieties were heavily disordered and were modeled as isotropic mixtures
with substantial restraints applied. The difficulty with the disordered
crown ether results in considerable uncertainty in the bond distances
and angles associated with these moieties and so the model should only
be considered for connectivity purposes, and not for the geometric
parameters.
;

_diffrn_ambient_temperature      180(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            2555
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.84
_diffrn_reflns_theta_max         22.80
_reflns_number_total             2023
_reflns_number_gt                1568
_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^)+(0.0653P)^2^+1065.7550P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_number_reflns         2023
_refine_ls_number_parameters     109
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.1975
_refine_ls_wR_factor_gt          0.1768
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.002
_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
Sb1 Sb 0.0000 1.0000 0.53259(17) 0.0523(17) Uani 1 3 d S . .
Sb2 Sb 0.0000 1.0000 0.38616(17) 0.0543(18) Uani 1 3 d S . .
Sb3 Sb 0.0301(2) 0.8975(2) 0.49504(11) 0.0637(12) Uani 1 1 d . . .
Sb4 Sb -0.0565(2) 0.8619(2) 0.42334(11) 0.0678(12) Uani 1 1 d . . .
Sb5 Sb -0.1847(2) 0.8366(3) 0.45932(12) 0.0817(16) Uani 1 1 d . . .
Sb6 Sb 0.6667 1.3333 0.38737(17) 0.0552(18) Uani 1 3 d S . .
Sb7 Sb 0.6667 1.3333 0.24037(17) 0.0570(18) Uani 1 3 d S . .
Sb8 Sb 0.5336(2) 1.2328(2) 0.34955(12) 0.0705(13) Uani 1 1 d . . .
Sb9 Sb 0.5822(2) 1.1957(2) 0.27814(11) 0.0724(13) Uani 1 1 d . . .
Sb0 Sb 0.6833(3) 1.1670(3) 0.31305(13) 0.0870(17) Uani 1 1 d . . .
Li1 Li 0.011(6) 0.594(6) 0.472(3) 0.08(2) Uiso 1 1 d . . .
O11 O 0.173(2) 0.696(2) 0.4535(10) 0.098(6) Uiso 0.70 1 d PG A 1
O12 O 0.073(2) 0.7209(19) 0.4961(12) 0.098(6) Uiso 0.70 1 d PG A 1
O13 O 0.0016(17) 0.582(2) 0.5301(12) 0.098(6) Uiso 0.70 1 d PG A 1
O14 O 0.099(2) 0.5579(18) 0.4873(13) 0.098(6) Uiso 0.70 1 d PG A 1
C11 C 0.189(2) 0.7679(19) 0.4635(14) 0.102(4) Uiso 0.70 1 d PG A 1
H11A H 0.1735 0.7880 0.4402 0.122 Uiso 0.70 1 calc PR A 1
H11B H 0.2418 0.7996 0.4674 0.122 Uiso 0.70 1 calc PR A 1
C12 C 0.149(2) 0.7690(15) 0.5022(13) 0.102(4) Uiso 0.70 1 d PG A 1
H12A H 0.1667 0.7526 0.5262 0.122 Uiso 0.70 1 calc PR A 1
H12B H 0.1592 0.8191 0.5078 0.122 Uiso 0.70 1 calc PR A 1
C13 C 0.031(2) 0.705(2) 0.5335(14) 0.102(4) Uiso 0.70 1 d PG A 1
H13A H -0.0199 0.6905 0.5267 0.122 Uiso 0.70 1 calc PR A 1
H13B H 0.0517 0.7491 0.5511 0.122 Uiso 0.70 1 calc PR A 1
C14 C 0.033(2) 0.644(2) 0.5568(10) 0.102(4) Uiso 0.70 1 d PG A 1
H14A H 0.0833 0.6580 0.5642 0.122 Uiso 0.70 1 calc PR A 1
H14B H 0.0035 0.6332 0.5826 0.122 Uiso 0.70 1 calc PR A 1
C15 C 0.017(2) 0.526(2) 0.5430(14) 0.102(4) Uiso 0.70 1 d PG A 1
H15A H -0.0190 0.4790 0.5301 0.122 Uiso 0.70 1 calc PR A 1
H15B H 0.0113 0.5201 0.5734 0.122 Uiso 0.70 1 calc PR A 1
C16 C 0.093(3) 0.545(2) 0.5309(13) 0.102(4) Uiso 0.70 1 d PG A 1
H16A H 0.1294 0.5888 0.5459 0.122 Uiso 0.70 1 calc PR A 1
H16B H 0.1013 0.5038 0.5377 0.122 Uiso 0.70 1 calc PR A 1
C17 C 0.172(3) 0.589(2) 0.4724(15) 0.102(4) Uiso 0.70 1 d PG A 1
H17A H 0.1716 0.5753 0.4430 0.122 Uiso 0.70 1 calc PR A 1
H17B H 0.1982 0.5681 0.4883 0.122 Uiso 0.70 1 calc PR A 1
C18 C 0.2134(19) 0.671(2) 0.4766(13) 0.102(4) Uiso 0.70 1 d PG A 1
H18A H 0.2164 0.6850 0.5061 0.122 Uiso 0.70 1 calc PR A 1
H18B H 0.2635 0.6917 0.4655 0.122 Uiso 0.70 1 calc PR A 1
O21 O 0.0572(17) 0.560(2) 0.3975(11) 0.102(4) Uiso 0.70 1 d PG A 1
O22 O 0.039(2) 0.6801(15) 0.4073(13) 0.102(4) Uiso 0.70 1 d PG A 1
O23 O -0.079(2) 0.604(2) 0.4606(11) 0.102(4) Uiso 0.70 1 d PG A 1
O24 O -0.059(2) 0.4850(17) 0.4512(10) 0.102(4) Uiso 0.70 1 d PG A 1
C21 C 0.084(2) 0.617(2) 0.3674(12) 0.102(4) Uiso 0.70 1 d PG A 1
H21A H 0.0831 0.5966 0.3397 0.122 Uiso 0.70 1 calc PR A 1
H21B H 0.1356 0.6536 0.3738 0.122 Uiso 0.70 1 calc PR A 1
C22 C 0.039(2) 0.655(2) 0.3664(11) 0.102(4) Uiso 0.70 1 d PG A 1
H22A H 0.0610 0.6961 0.3468 0.122 Uiso 0.70 1 calc PR A 1
H22B H -0.0111 0.6199 0.3575 0.122 Uiso 0.70 1 calc PR A 1
C23 C -0.015(3) 0.6998(17) 0.4135(15) 0.102(4) Uiso 0.70 1 d PG A 1
H23A H -0.0193 0.7241 0.3882 0.122 Uiso 0.70 1 calc PR A 1
H23B H -0.0004 0.7351 0.4366 0.122 Uiso 0.70 1 calc PR A 1
C24 C -0.088(2) 0.634(2) 0.4231(13) 0.102(4) Uiso 0.70 1 d PG A 1
H24A H -0.1259 0.6486 0.4266 0.122 Uiso 0.70 1 calc PR A 1
H24B H -0.1038 0.5978 0.4004 0.122 Uiso 0.70 1 calc PR A 1
C25 C -0.1371(19) 0.531(2) 0.4685(12) 0.102(4) Uiso 0.70 1 d PG A 1
H25A H -0.1845 0.5276 0.4624 0.122 Uiso 0.70 1 calc PR A 1
H25B H -0.1367 0.5194 0.4982 0.122 Uiso 0.70 1 calc PR A 1
C26 C -0.1293(17) 0.4759(17) 0.4426(12) 0.102(4) Uiso 0.70 1 d PG A 1
H26A H -0.1681 0.4258 0.4497 0.122 Uiso 0.70 1 calc PR A 1
H26B H -0.1334 0.4844 0.4128 0.122 Uiso 0.70 1 calc PR A 1
C27 C -0.038(2) 0.4477(17) 0.4222(13) 0.102(4) Uiso 0.70 1 d PG A 1
H27A H -0.0813 0.4006 0.4144 0.122 Uiso 0.70 1 calc PR A 1
H27B H -0.0018 0.4372 0.4351 0.122 Uiso 0.70 1 calc PR A 1
C28 C -0.005(2) 0.4940(19) 0.3840(11) 0.102(4) Uiso 0.70 1 d PG A 1
H28A H 0.0090 0.4682 0.3638 0.122 Uiso 0.70 1 calc PR A 1
H28B H -0.0413 0.5045 0.3707 0.122 Uiso 0.70 1 calc PR A 1
O11' O 0.140(5) 0.646(5) 0.478(2) 0.098(6) Uiso 0.30 1 d PG A 2
O12' O 0.077(6) 0.729(4) 0.502(3) 0.098(6) Uiso 0.30 1 d PG A 2
O13' O -0.017(4) 0.610(5) 0.549(3) 0.098(6) Uiso 0.30 1 d PG A 2
O14' O 0.044(5) 0.528(4) 0.526(3) 0.098(6) Uiso 0.30 1 d PG A 2
C11' C 0.185(4) 0.716(5) 0.496(3) 0.102(4) Uiso 0.30 1 d PG A 2
H11C H 0.2344 0.7393 0.4842 0.122 Uiso 0.30 1 calc PR A 2
H11D H 0.1886 0.7122 0.5264 0.122 Uiso 0.30 1 calc PR A 2
C12' C 0.150(6) 0.763(4) 0.487(3) 0.102(4) Uiso 0.30 1 d PG A 2
H12C H 0.1798 0.8112 0.4999 0.122 Uiso 0.30 1 calc PR A 2
H12D H 0.1502 0.7696 0.4567 0.122 Uiso 0.30 1 calc PR A 2
C13' C 0.071(6) 0.739(4) 0.545(3) 0.102(4) Uiso 0.30 1 d PG A 2
H13C H 0.0791 0.7887 0.5508 0.122 Uiso 0.30 1 calc PR A 2
H13D H 0.1083 0.7332 0.5609 0.122 Uiso 0.30 1 calc PR A 2
C14' C -0.005(5) 0.681(6) 0.558(3) 0.102(4) Uiso 0.30 1 d PG A 2
H14C H -0.0117 0.6855 0.5875 0.122 Uiso 0.30 1 calc PR A 2
H14D H -0.0409 0.6895 0.5424 0.122 Uiso 0.30 1 calc PR A 2
C15' C 0.007(5) 0.581(5) 0.581(2) 0.102(4) Uiso 0.30 1 d PG A 2
H15C H -0.0254 0.5686 0.6054 0.122 Uiso 0.30 1 calc PR A 2
H15D H 0.0574 0.6163 0.5892 0.122 Uiso 0.30 1 calc PR A 2
C16' C 0.003(5) 0.512(4) 0.564(3) 0.102(4) Uiso 0.30 1 d PG A 2
H16C H 0.0229 0.4924 0.5847 0.122 Uiso 0.30 1 calc PR A 2
H16D H -0.0484 0.4752 0.5586 0.122 Uiso 0.30 1 calc PR A 2
C17' C 0.121(5) 0.561(5) 0.533(3) 0.102(4) Uiso 0.30 1 d PG A 2
H17C H 0.1336 0.5236 0.5426 0.122 Uiso 0.30 1 calc PR A 2
H17D H 0.1375 0.5993 0.5544 0.122 Uiso 0.30 1 calc PR A 2
C18' C 0.157(5) 0.592(6) 0.492(3) 0.102(4) Uiso 0.30 1 d PG A 2
H18C H 0.2111 0.6154 0.4956 0.122 Uiso 0.30 1 calc PR A 2
H18D H 0.1414 0.5530 0.4717 0.122 Uiso 0.30 1 calc PR A 2
O21' O 0.044(4) 0.553(5) 0.423(3) 0.102(4) Uiso 0.30 1 d PG A 2
O22' O 0.020(4) 0.671(4) 0.414(3) 0.102(4) Uiso 0.30 1 d PG A 2
O23' O -0.117(4) 0.593(5) 0.449(3) 0.102(4) Uiso 0.30 1 d PG A 2
O24' O -0.092(4) 0.477(4) 0.459(3) 0.102(4) Uiso 0.30 1 d PG A 2
C21' C 0.046(4) 0.582(5) 0.382(3) 0.102(4) Uiso 0.30 1 d PG A 2
H21C H -0.0032 0.5558 0.3697 0.122 Uiso 0.30 1 calc PR A 2
H21D H 0.0806 0.5766 0.3643 0.122 Uiso 0.30 1 calc PR A 2
C22' C 0.070(4) 0.662(5) 0.388(3) 0.102(4) Uiso 0.30 1 d PG A 2
H22C H 0.1186 0.6866 0.4016 0.122 Uiso 0.30 1 calc PR A 2
H22D H 0.0738 0.6844 0.3612 0.122 Uiso 0.30 1 calc PR A 2
C23' C -0.042(5) 0.663(5) 0.391(3) 0.102(4) Uiso 0.30 1 d PG A 2
H23C H -0.0612 0.6205 0.3725 0.122 Uiso 0.30 1 calc PR A 2
H23D H -0.0274 0.7075 0.3742 0.122 Uiso 0.30 1 calc PR A 2
C24' C -0.099(5) 0.654(5) 0.422(3) 0.102(4) Uiso 0.30 1 d PG A 2
H24C H -0.0803 0.6988 0.4391 0.122 Uiso 0.30 1 calc PR A 2
H24D H -0.1433 0.6459 0.4077 0.122 Uiso 0.30 1 calc PR A 2
C25' C -0.167(3) 0.524(5) 0.431(3) 0.102(4) Uiso 0.30 1 d PG A 2
H25C H -0.1513 0.5210 0.4025 0.122 Uiso 0.30 1 calc PR A 2
H25D H -0.2167 0.5165 0.4301 0.122 Uiso 0.30 1 calc PR A 2
C26' C -0.164(4) 0.467(5) 0.458(3) 0.102(4) Uiso 0.30 1 d PG A 2
H26C H -0.1802 0.4700 0.4865 0.122 Uiso 0.30 1 calc PR A 2
H26D H -0.1986 0.4175 0.4471 0.122 Uiso 0.30 1 calc PR A 2
C27' C -0.076(5) 0.445(4) 0.425(3) 0.102(4) Uiso 0.30 1 d PG A 2
H27C H -0.0922 0.4581 0.3987 0.122 Uiso 0.30 1 calc PR A 2
H27D H -0.1027 0.3915 0.4275 0.122 Uiso 0.30 1 calc PR A 2
C28' C 0.005(5) 0.475(5) 0.424(4) 0.102(4) Uiso 0.30 1 d PG A 2
H28C H 0.0192 0.4586 0.4495 0.122 Uiso 0.30 1 calc PR A 2
H28D H 0.0179 0.4554 0.4000 0.122 Uiso 0.30 1 calc PR A 2
Li2 Li 0.2467(12) 0.9281(12) 0.2822(6) 0.08(2) Uiso 1 1 d G B 2
O31 O 0.2527(17) 0.9754(16) 0.2154(7) 0.098(6) Uiso 0.65 1 d PG B 1
O32 O 0.3749(12) 0.9905(15) 0.2569(9) 0.098(6) Uiso 0.65 1 d PG B 1
O33 O 0.2861(16) 0.8476(14) 0.2809(9) 0.098(6) Uiso 0.65 1 d PG B 1
O34 O 0.1657(15) 0.8311(14) 0.2397(8) 0.098(6) Uiso 0.65 1 d PG B 1
C31 C 0.3191(19) 0.9989(17) 0.1931(7) 0.102(4) Uiso 0.65 1 d PG B 1
H31A H 0.3236 1.0328 0.1707 0.122 Uiso 0.65 1 calc PR B 1
H31B H 0.3195 0.9564 0.1806 0.122 Uiso 0.65 1 calc PR B 1
C32 C 0.3816(16) 1.0368(16) 0.2232(9) 0.102(4) Uiso 0.65 1 d PG B 1
H32A H 0.4282 1.0520 0.2085 0.122 Uiso 0.65 1 calc PR B 1
H32B H 0.3828 1.0813 0.2339 0.122 Uiso 0.65 1 calc PR B 1
C33 C 0.3977(14) 0.9388(19) 0.2480(10) 0.102(4) Uiso 0.65 1 d PG B 1
H33A H 0.4516 0.9626 0.2489 0.122 Uiso 0.65 1 calc PR B 1
H33B H 0.3806 0.9172 0.2203 0.122 Uiso 0.65 1 calc PR B 1
C34 C 0.3638(17) 0.8808(19) 0.2811(10) 0.102(4) Uiso 0.65 1 d PG B 1
H34A H 0.3775 0.8429 0.2762 0.122 Uiso 0.65 1 calc PR B 1
H34B H 0.3829 0.9029 0.3085 0.122 Uiso 0.65 1 calc PR B 1
C35 C 0.251(2) 0.7885(14) 0.2522(10) 0.102(4) Uiso 0.65 1 d PG B 1
H35A H 0.2551 0.7461 0.2617 0.122 Uiso 0.65 1 calc PR B 1
H35B H 0.2744 0.8036 0.2246 0.122 Uiso 0.65 1 calc PR B 1
C36 C 0.1722(18) 0.7687(12) 0.2499(10) 0.102(4) Uiso 0.65 1 d PG B 1
H36A H 0.1469 0.7304 0.2286 0.122 Uiso 0.65 1 calc PR B 1
H36B H 0.1483 0.7487 0.2768 0.122 Uiso 0.65 1 calc PR B 1
C37 C 0.1756(18) 0.8486(18) 0.1966(8) 0.102(4) Uiso 0.65 1 d PG B 1
H37A H 0.1314 0.8142 0.1808 0.122 Uiso 0.65 1 calc PR B 1
H37B H 0.2178 0.8457 0.1857 0.122 Uiso 0.65 1 calc PR B 1
C38 C 0.1889(19) 0.925(2) 0.1926(7) 0.102(4) Uiso 0.65 1 d PG B 1
H38A H 0.1955 0.9394 0.1630 0.122 Uiso 0.65 1 calc PR B 1
H38B H 0.1460 0.9271 0.2031 0.122 Uiso 0.65 1 calc PR B 1
O41 O 0.1385(14) 0.9424(18) 0.2840(9) 0.102(4) Uiso 0.65 1 d PG B 1
O42 O 0.2842(16) 1.0516(12) 0.2956(9) 0.102(4) Uiso 0.65 1 d PG B 1
O43 O 0.3119(16) 0.9623(17) 0.3454(7) 0.102(4) Uiso 0.65 1 d PG B 1
O44 O 0.1683(15) 0.8533(15) 0.3331(8) 0.102(4) Uiso 0.65 1 d PG B 1
C41 C 0.1551(18) 1.0107(19) 0.3021(10) 0.102(4) Uiso 0.65 1 d PG B 1
H41A H 0.1577 1.0084 0.3326 0.122 Uiso 0.65 1 calc PR B 1
H41B H 0.1170 1.0231 0.2950 0.122 Uiso 0.65 1 calc PR B 1
C42 C 0.228(2) 1.0671(16) 0.2848(10) 0.102(4) Uiso 0.65 1 d PG B 1
H42A H 0.2245 1.0683 0.2543 0.122 Uiso 0.65 1 calc PR B 1
H42B H 0.2407 1.1159 0.2955 0.122 Uiso 0.65 1 calc PR B 1
C43 C 0.3134(18) 1.0768(15) 0.3359(9) 0.102(4) Uiso 0.65 1 d PG B 1
H43A H 0.2734 1.0642 0.3560 0.122 Uiso 0.65 1 calc PR B 1
H43B H 0.3457 1.1305 0.3358 0.122 Uiso 0.65 1 calc PR B 1
C44 C 0.3560(16) 1.0399(18) 0.3477(9) 0.102(4) Uiso 0.65 1 d PG B 1
H44A H 0.3984 1.0565 0.3289 0.122 Uiso 0.65 1 calc PR B 1
H44B H 0.3749 1.0542 0.3762 0.122 Uiso 0.65 1 calc PR B 1
C45 C 0.265(2) 0.930(2) 0.3804(6) 0.102(4) Uiso 0.65 1 d PG B 1
H45A H 0.2401 0.9581 0.3874 0.122 Uiso 0.65 1 calc PR B 1
H45B H 0.2933 0.9303 0.4047 0.122 Uiso 0.65 1 calc PR B 1
C46 C 0.210(2) 0.8530(18) 0.3682(7) 0.102(4) Uiso 0.65 1 d PG B 1
H46A H 0.2349 0.8257 0.3614 0.122 Uiso 0.65 1 calc PR B 1
H46B H 0.1761 0.8281 0.3916 0.122 Uiso 0.65 1 calc PR B 1
C47 C 0.1089(15) 0.8637(18) 0.3441(9) 0.102(4) Uiso 0.65 1 d PG B 1
H47A H 0.1253 0.9047 0.3639 0.122 Uiso 0.65 1 calc PR B 1
H47B H 0.0694 0.8190 0.3572 0.122 Uiso 0.65 1 calc PR B 1
C48 C 0.0816(13) 0.880(2) 0.3049(11) 0.102(4) Uiso 0.65 1 d PG B 1
H48A H 0.0619 0.8375 0.2863 0.122 Uiso 0.65 1 calc PR B 1
H48B H 0.0415 0.8901 0.3116 0.122 Uiso 0.65 1 calc PR B 1
O31' O 0.279(3) 0.995(3) 0.2178(13) 0.098(6) Uiso 0.35 1 d PG B 2
O32' O 0.366(2) 0.966(3) 0.2678(17) 0.098(6) Uiso 0.35 1 d PG B 2
O33' O 0.261(3) 0.823(3) 0.2823(17) 0.098(6) Uiso 0.35 1 d PG B 2
O34' O 0.171(3) 0.851(3) 0.2323(15) 0.098(6) Uiso 0.35 1 d PG B 2
C31' C 0.357(3) 1.038(3) 0.2148(17) 0.102(4) Uiso 0.35 1 d PG B 2
H31C H 0.3744 1.0811 0.2330 0.122 Uiso 0.35 1 calc PR B 2
H31D H 0.3705 1.0552 0.1860 0.122 Uiso 0.35 1 calc PR B 2
C32' C 0.392(3) 0.994(3) 0.2273(19) 0.102(4) Uiso 0.35 1 d PG B 2
H32C H 0.3790 0.9536 0.2075 0.122 Uiso 0.35 1 calc PR B 2
H32D H 0.4460 1.0256 0.2275 0.122 Uiso 0.35 1 calc PR B 2
C33' C 0.385(3) 0.913(4) 0.281(2) 0.102(4) Uiso 0.35 1 d PG B 2
H33C H 0.3871 0.9128 0.3114 0.122 Uiso 0.35 1 calc PR B 2
H33D H 0.4337 0.9263 0.2699 0.122 Uiso 0.35 1 calc PR B 2
C34' C 0.329(4) 0.838(4) 0.266(2) 0.102(4) Uiso 0.35 1 d PG B 2
H34C H 0.3278 0.8362 0.2352 0.122 Uiso 0.35 1 calc PR B 2
H34D H 0.3421 0.8010 0.2757 0.122 Uiso 0.35 1 calc PR B 2
C35' C 0.199(4) 0.766(2) 0.2620(19) 0.102(4) Uiso 0.35 1 d PG B 2
H35C H 0.1561 0.7464 0.2807 0.122 Uiso 0.35 1 calc PR B 2
H35D H 0.2083 0.7252 0.2558 0.122 Uiso 0.35 1 calc PR B 2
C36' C 0.182(4) 0.792(3) 0.2224(18) 0.102(4) Uiso 0.35 1 d PG B 2
H36C H 0.2226 0.8074 0.2026 0.122 Uiso 0.35 1 calc PR B 2
H36D H 0.1370 0.7516 0.2096 0.122 Uiso 0.35 1 calc PR B 2
C37' C 0.170(3) 0.891(4) 0.1965(14) 0.102(4) Uiso 0.35 1 d PG B 2
H37C H 0.1422 0.9163 0.2028 0.122 Uiso 0.35 1 calc PR B 2
H37D H 0.1448 0.8566 0.1735 0.122 Uiso 0.35 1 calc PR B 2
C38' C 0.246(4) 0.946(4) 0.1835(12) 0.102(4) Uiso 0.35 1 d PG B 2
H38C H 0.2741 0.9217 0.1766 0.122 Uiso 0.35 1 calc PR B 2
H38D H 0.2450 0.9735 0.1589 0.122 Uiso 0.35 1 calc PR B 2
O41' O 0.159(3) 0.973(3) 0.2778(17) 0.102(4) Uiso 0.35 1 d PG B 2
O42' O 0.148(3) 0.854(3) 0.3220(16) 0.102(4) Uiso 0.35 1 d PG B 2
O43' O 0.289(3) 0.936(3) 0.3507(13) 0.102(4) Uiso 0.35 1 d PG B 2
O44' O 0.301(3) 1.053(2) 0.3061(15) 0.102(4) Uiso 0.35 1 d PG B 2
C41' C 0.104(3) 0.939(4) 0.309(2) 0.102(4) Uiso 0.35 1 d PG B 2
H41C H 0.0601 0.9421 0.3021 0.122 Uiso 0.35 1 calc PR B 2
H41D H 0.1231 0.9632 0.3362 0.122 Uiso 0.35 1 calc PR B 2
C42' C 0.086(2) 0.860(4) 0.311(2) 0.102(4) Uiso 0.35 1 d PG B 2
H42C H 0.0465 0.8338 0.3314 0.122 Uiso 0.35 1 calc PR B 2
H42D H 0.0675 0.8373 0.2836 0.122 Uiso 0.35 1 calc PR B 2
C43' C 0.160(3) 0.858(3) 0.3655(15) 0.102(4) Uiso 0.35 1 d PG B 2
H43C H 0.1243 0.8119 0.3789 0.122 Uiso 0.35 1 calc PR B 2
H43D H 0.1552 0.8985 0.3777 0.122 Uiso 0.35 1 calc PR B 2
C44' C 0.237(4) 0.872(3) 0.3720(14) 0.102(4) Uiso 0.35 1 d PG B 2
H44C H 0.2478 0.8774 0.4020 0.122 Uiso 0.35 1 calc PR B 2
H44D H 0.2395 0.8291 0.3620 0.122 Uiso 0.35 1 calc PR B 2
C45' C 0.308(3) 1.002(3) 0.3718(14) 0.102(4) Uiso 0.35 1 d PG B 2
H45C H 0.3394 1.0094 0.3959 0.122 Uiso 0.35 1 calc PR B 2
H45D H 0.2628 1.0015 0.3817 0.122 Uiso 0.35 1 calc PR B 2
C46' C 0.347(3) 1.063(3) 0.3408(17) 0.102(4) Uiso 0.35 1 d PG B 2
H46C H 0.3618 1.1108 0.3540 0.122 Uiso 0.35 1 calc PR B 2
H46D H 0.3919 1.0637 0.3312 0.122 Uiso 0.35 1 calc PR B 2
C47' C 0.252(4) 1.081(3) 0.3133(18) 0.102(4) Uiso 0.35 1 d PG B 2
H47C H 0.2797 1.1347 0.3128 0.122 Uiso 0.35 1 calc PR B 2
H47D H 0.2287 1.0642 0.3406 0.122 Uiso 0.35 1 calc PR B 2
C48' C 0.196(4) 1.051(3) 0.2793(19) 0.102(4) Uiso 0.35 1 d PG B 2
H48C H 0.1602 1.0677 0.2841 0.122 Uiso 0.35 1 calc PR B 2
H48D H 0.2202 1.0712 0.2524 0.122 Uiso 0.35 1 calc PR B 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
Sb1 0.058(3) 0.058(3) 0.042(4) 0.000 0.000 0.0288(15)
Sb2 0.060(3) 0.060(3) 0.042(4) 0.000 0.000 0.0302(16)
Sb3 0.084(3) 0.064(3) 0.057(2) -0.0016(17) -0.0114(19) 0.048(3)
Sb4 0.090(4) 0.049(3) 0.058(3) -0.0143(17) -0.018(2) 0.031(3)
Sb5 0.060(3) 0.071(3) 0.068(3) 0.0147(19) -0.015(2) -0.001(3)
Sb6 0.064(3) 0.064(3) 0.037(4) 0.000 0.000 0.0322(16)
Sb7 0.066(3) 0.066(3) 0.040(4) 0.000 0.000 0.0328(16)
Sb8 0.057(3) 0.073(3) 0.061(2) -0.0005(19) 0.0099(18) 0.017(3)
Sb9 0.083(3) 0.055(3) 0.055(2) -0.0103(18) 0.0011(19) 0.017(3)
Sb0 0.146(5) 0.081(4) 0.065(3) 0.010(2) 0.021(3) 0.080(4)

_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
Sb1 Sb3 2.821(5) 3_465 ?
Sb1 Sb3 2.821(5) 2_675 ?
Sb1 Sb3 2.821(5) . ?
Sb2 Sb4 2.811(5) 2_675 ?
Sb2 Sb4 2.811(5) . ?
Sb2 Sb4 2.811(5) 3_465 ?
Sb3 Sb5 2.717(7) 2_675 ?
Sb3 Sb4 2.813(5) . ?
Sb4 Sb5 2.744(7) . ?
Sb5 Sb3 2.717(7) 3_465 ?
Sb6 Sb8 2.818(5) 2_775 ?
Sb6 Sb8 2.818(5) . ?
Sb6 Sb8 2.818(5) 3_575 ?
Sb7 Sb9 2.819(5) 2_775 ?
Sb7 Sb9 2.819(5) . ?
Sb7 Sb9 2.819(5) 3_575 ?
Sb8 Sb0 2.742(7) 3_575 ?
Sb8 Sb9 2.793(6) . ?
Sb9 Sb0 2.742(7) . ?
Sb0 Sb8 2.742(7) 2_775 ?
Li1 O13 1.89(10) . ?
Li1 O23 2.06(11) . ?
Li1 O21' 2.09(13) . ?
Li1 O24 2.12(12) . ?
Li1 O24' 2.36(14) . ?
Li1 O11' 2.38(14) . ?
Li1 O14 2.39(11) . ?
Li1 O22' 2.44(13) . ?
Li1 O12 2.46(12) . ?
Li1 O14' 2.55(13) . ?
Li1 O13' 2.61(13) . ?
Li1 O22 2.64(11) . ?
O11 C11 1.4235 . ?
O11 C18 1.4270 . ?
O12 C12 1.4272 . ?
O12 C13 1.4354 . ?
O13 C15 1.4303 . ?
O13 C14 1.4303 . ?
O14 C17 1.4276 . ?
O14 C16 1.4307 . ?
C11 C12 1.5072 . ?
C13 C14 1.5006 . ?
C15 C16 1.5064 . ?
C17 C18 1.5103 . ?
O21 C21 1.4277 . ?
O21 C28 1.4322 . ?
O22 C23 1.4248 . ?
O22 C22 1.4274 . ?
O23 C25 1.4283 . ?
O23 C24 1.4302 . ?
O24 C26 1.4264 . ?
O24 C27 1.4319 . ?
C21 C22 1.5055 . ?
C23 C24 1.5082 . ?
C25 C26 1.5073 . ?
C27 C28 1.5114 . ?
O11' C11' 1.4271(11) . ?
O11' C18' 1.4357 . ?
O12' C12' 1.4235(10) . ?
O12' C13' 1.4266 . ?
O13' C14' 1.4275 . ?
O13' C15' 1.4303 . ?
O14' C16' 1.4302 . ?
O14' C17' 1.4305 . ?
C11' C12' 1.5069 . ?
C13' C14' 1.5103(12) . ?
C15' C16' 1.5062 . ?
C17' C18' 1.5004 . ?
O21' C28' 1.4281 . ?
O21' C21' 1.4303 . ?
O22' C22' 1.4249 . ?
O22' C23' 1.4271 . ?
O23' C24' 1.4278 . ?
O23' C25' 1.4322 . ?
O24' C27' 1.4263 . ?
O24' C26' 1.4321 . ?
C21' C22' 1.5080 . ?
C23' C24' 1.5057 . ?
C25' C26' 1.5112 . ?
C27' C28' 1.5073 . ?
Li2 O42' 2.28(5) . ?
Li2 O32' 2.28(5) . ?
Li2 O34' 2.28(5) . ?
Li2 O43' 2.37(5) . ?
Li2 O33' 2.39(5) . ?
Li2 O31' 2.42(5) . ?
Li2 O44' 2.42(5) . ?
Li2 O41' 2.49(5) . ?
O31 C31 1.4273 . ?
O31 C38 1.4358 . ?
O32 C32 1.4235 . ?
O32 C33 1.4267 . ?
O33 C34 1.4275 . ?
O33 C35 1.4303 . ?
O34 C36 1.4303 . ?
O34 C37 1.4306 . ?
C31 C32 1.5071 . ?
C33 C34 1.5103 . ?
C35 C36 1.5062 . ?
C37 C38 1.5006 . ?
O41 C48 1.4284 . ?
O41 C41 1.4304 . ?
O42 C42 1.4248 . ?
O42 C43 1.4274 . ?
O43 C44 1.4277 . ?
O43 C45 1.4321 . ?
O44 C47 1.4260 . ?
O44 C46 1.4321 . ?
C41 C42 1.5082 . ?
C43 C44 1.5055 . ?
C45 C46 1.5112 . ?
C47 C48 1.5072 . ?
O31' C31' 1.4301 . ?
O31' C38' 1.4305 . ?
O32' C33' 1.4275 . ?
O32' C32' 1.4305 . ?
O33' C35' 1.4236 . ?
O33' C34' 1.4267 . ?
O34' C36' 1.4272 . ?
O34' C37' 1.4358 . ?
C31' C32' 1.5065 . ?
C33' C34' 1.5102 . ?
C35' C36' 1.5069 . ?
C37' C38' 1.5005 . ?
O41' C48' 1.4282 . ?
O41' C41' 1.4303 . ?
O42' C42' 1.4247 . ?
O42' C43' 1.4274 . ?
O43' C44' 1.4277 . ?
O43' C45' 1.4323 . ?
O44' C47' 1.4265 . ?
O44' C46' 1.4320 . ?
C41' C42' 1.5080 . ?
C43' C44' 1.5055 . ?
C45' C46' 1.5113 . ?
C47' C48' 1.5074 . ?

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
Sb3 Sb1 Sb3 102.84(16) 3_465 2_675 ?
Sb3 Sb1 Sb3 102.84(16) 3_465 . ?
Sb3 Sb1 Sb3 102.84(16) 2_675 . ?
Sb4 Sb2 Sb4 103.05(15) 2_675 . ?
Sb4 Sb2 Sb4 103.05(15) 2_675 3_465 ?
Sb4 Sb2 Sb4 103.05(15) . 3_465 ?
Sb5 Sb3 Sb4 98.58(18) 2_675 . ?
Sb5 Sb3 Sb1 104.97(17) 2_675 . ?
Sb4 Sb3 Sb1 101.11(18) . . ?
Sb5 Sb4 Sb2 104.45(18) . . ?
Sb5 Sb4 Sb3 98.64(18) . . ?
Sb2 Sb4 Sb3 101.14(18) . . ?
Sb3 Sb5 Sb4 97.44(16) 3_465 . ?
Sb8 Sb6 Sb8 102.57(16) 2_775 . ?
Sb8 Sb6 Sb8 102.57(16) 2_775 3_575 ?
Sb8 Sb6 Sb8 102.57(16) . 3_575 ?
Sb9 Sb7 Sb9 102.62(16) 2_775 . ?
Sb9 Sb7 Sb9 102.62(16) 2_775 3_575 ?
Sb9 Sb7 Sb9 102.62(16) . 3_575 ?
Sb0 Sb8 Sb9 98.04(18) 3_575 . ?
Sb0 Sb8 Sb6 105.15(18) 3_575 . ?
Sb9 Sb8 Sb6 101.65(19) . . ?
Sb0 Sb9 Sb8 99.13(18) . . ?
Sb0 Sb9 Sb7 104.17(18) . . ?
Sb8 Sb9 Sb7 101.57(19) . . ?
Sb8 Sb0 Sb9 97.02(17) 2_775 . ?
O13 Li1 O23 99(5) . . ?
O13 Li1 O21' 138(6) . . ?
O23 Li1 O21' 115(5) . . ?
O13 Li1 O24 102(5) . . ?
O23 Li1 O24 83(4) . . ?
O21' Li1 O24 61(4) . . ?
O13 Li1 O24' 93(5) . . ?
O23 Li1 O24' 70(4) . . ?
O21' Li1 O24' 76(4) . . ?
O13 Li1 O11' 90(5) . . ?
O23 Li1 O11' 151(6) . . ?
O21' Li1 O11' 74(4) . . ?
O24 Li1 O11' 123(5) . . ?
O24' Li1 O11' 138(6) . . ?
O13 Li1 O14 79(4) . . ?
O23 Li1 O14 169(6) . . ?
O21' Li1 O14 63(4) . . ?
O24 Li1 O14 88(4) . . ?
O24' Li1 O14 100(5) . . ?
O13 Li1 O22' 145(6) . . ?
O23 Li1 O22' 64(4) . . ?
O21' Li1 O22' 76(4) . . ?
O24 Li1 O22' 105(5) . . ?
O24' Li1 O22' 106(5) . . ?
O11' Li1 O22' 94(5) . . ?
O14 Li1 O22' 124(5) . . ?
O13 Li1 O12 78(4) . . ?
O23 Li1 O12 88(4) . . ?
O21' Li1 O12 126(6) . . ?
O24 Li1 O12 170(5) . . ?
O24' Li1 O12 154(5) . . ?
O11' Li1 O12 67(4) . . ?
O14 Li1 O12 102(4) . . ?
O22' Li1 O12 72(4) . . ?
O23 Li1 O14' 135(5) . . ?
O21' Li1 O14' 93(5) . . ?
O24 Li1 O14' 82(4) . . ?
O24' Li1 O14' 85(4) . . ?
O11' Li1 O14' 68(3) . . ?
O22' Li1 O14' 162(6) . . ?
O12 Li1 O14' 104(4) . . ?
O23 Li1 O13' 83(4) . . ?
O21' Li1 O13' 157(6) . . ?
O24 Li1 O13' 111(5) . . ?
O24' Li1 O13' 99(5) . . ?
O11' Li1 O13' 98(4) . . ?
O14 Li1 O13' 97(4) . . ?
O22' Li1 O13' 126(5) . . ?
O12 Li1 O13' 66(3) . . ?
O14' Li1 O13' 64(3) . . ?
O13 Li1 O22 148(6) . . ?
O23 Li1 O22 72(3) . . ?
O21' Li1 O22 71(4) . . ?
O24 Li1 O22 107(4) . . ?
O24' Li1 O22 111(4) . . ?
O11' Li1 O22 86(4) . . ?
O14 Li1 O22 116(4) . . ?
O12 Li1 O22 71(3) . . ?
O14' Li1 O22 153(5) . . ?
O13' Li1 O22 130(5) . . ?
C11 O11 C18 114.6 . . ?
C12 O12 C13 113.2 . . ?
C12 O12 Li1 128(3) . . ?
C13 O12 Li1 95(3) . . ?
C15 O13 C14 113.3 . . ?
C15 O13 Li1 110(3) . . ?
C14 O13 Li1 121(4) . . ?
C17 O14 C16 113.3 . . ?
C17 O14 Li1 129(3) . . ?
C16 O14 Li1 105(3) . . ?
O11 C11 C12 111.6 . . ?
O12 C12 C11 107.9 . . ?
O12 C13 C14 110.7 . . ?
O13 C14 C13 106.7 . . ?
O13 C15 C16 111.1 . . ?
C16 C15 Li1 88(2) . . ?
O14 C16 C15 106.9 . . ?
O14 C17 C18 111.1 . . ?
O11 C18 C17 106.0 . . ?
C21 O21 C28 113.7 . . ?
C23 O22 C22 113.1 . . ?
C23 O22 Li1 99(2) . . ?
C22 O22 Li1 121(2) . . ?
C25 O23 C24 113.6 . . ?
C25 O23 Li1 101(3) . . ?
C24 O23 Li1 122(3) . . ?
C26 O24 C27 112.7 . . ?
C26 O24 Li1 109(3) . . ?
C27 O24 Li1 124(3) . . ?
O21 C21 C22 111.5 . . ?
O22 C22 C21 107.3 . . ?
O22 C23 C24 111.6 . . ?
O23 C24 C23 106.4 . . ?
O23 C25 C26 111.6 . . ?
C26 C25 Li1 82(2) . . ?
O24 C26 C25 107.1 . . ?
O24 C27 C28 110.3 . . ?
O21 C28 C27 106.5 . . ?
C11' O11' C18' 113.21(7) . . ?
C11' O11' Li1 122(4) . . ?
C18' O11' Li1 110(4) . . ?
C12' O12' C13' 114.62(9) . . ?
C12' O12' Li1 105(3) . . ?
C13' O12' Li1 118(3) . . ?
C14' O13' C15' 113.3 . . ?
C14' O13' Li1 114(3) . . ?
C15' O13' Li1 119(3) . . ?
C16' O14' C17' 113.3 . . ?
C16' O14' Li1 114(3) . . ?
C17' O14' Li1 113(3) . . ?
O11' C11' C12' 107.92(8) . . ?
O12' C12' C11' 111.6 . . ?
O12' C13' C14' 106.04(13) . . ?
O13' C14' C13' 111.0 . . ?
O13' C15' C16' 107.0 . . ?
O14' C16' C15' 111.06(6) . . ?
O14' C17' C18' 106.7 . . ?
O11' C18' C17' 110.7 . . ?
C28' O21' C21' 113.6 . . ?
C28' O21' Li1 109(4) . . ?
C21' O21' Li1 117(4) . . ?
C22' O22' C23' 113.1 . . ?
C22' O22' Li1 99(3) . . ?
C23' O22' Li1 124(3) . . ?
C24' O23' C25' 113.7 . . ?
C27' O24' C26' 112.7 . . ?
C27' O24' Li1 109(3) . . ?
C26' O24' Li1 122(3) . . ?
O21' C21' C22' 106.4 . . ?
O22' C22' C21' 111.6 . . ?
O22' C23' C24' 107.3 . . ?
O23' C24' C23' 111.5 . . ?
O23' C25' C26' 106.5 . . ?
O24' C26' C25' 110.3 . . ?
O24' C27' C28' 107.1 . . ?
O21' C28' C27' 111.6 . . ?
O42' Li2 O32' 146(2) . . ?
O42' Li2 O34' 80.5(18) . . ?
O32' Li2 O34' 111(2) . . ?
O42' Li2 O43' 72.9(15) . . ?
O32' Li2 O43' 81.5(17) . . ?
O34' Li2 O43' 145(2) . . ?
O42' Li2 O33' 82.0(17) . . ?
O32' Li2 O33' 72.3(16) . . ?
O34' Li2 O33' 73.0(16) . . ?
O43' Li2 O33' 80.9(16) . . ?
O42' Li2 O31' 141(2) . . ?
O32' Li2 O31' 71.3(15) . . ?
O34' Li2 O31' 72.3(15) . . ?
O43' Li2 O31' 141(2) . . ?
O33' Li2 O31' 114(2) . . ?
O42' Li2 O44' 110(2) . . ?
O32' Li2 O44' 81.1(17) . . ?
O34' Li2 O44' 141(2) . . ?
O43' Li2 O44' 70.8(15) . . ?
O33' Li2 O44' 144(2) . . ?
O31' Li2 O44' 78.3(16) . . ?
O42' Li2 O41' 71.9(15) . . ?
O32' Li2 O41' 140(2) . . ?
O34' Li2 O41' 80.7(17) . . ?
O43' Li2 O41' 111(2) . . ?
O33' Li2 O41' 146(2) . . ?
O31' Li2 O41' 76.8(15) . . ?
O44' Li2 O41' 68.7(14) . . ?
C31 O31 C38 113.2 . . ?
C32 O32 C33 114.6 . . ?
C34 O33 C35 113.3 . . ?
C36 O34 C37 113.3 . . ?
O31 C31 C32 107.9 . . ?
O32 C32 C31 111.6 . . ?
O32 C33 C34 106.0 . . ?
O33 C34 C33 111.0 . . ?
O33 C35 C36 107.0 . . ?
O34 C36 C35 111.1 . . ?
O34 C37 C38 106.7 . . ?
O31 C38 C37 110.7 . . ?
C48 O41 C41 113.6 . . ?
C42 O42 C43 113.1 . . ?
C44 O43 C45 113.7 . . ?
C47 O44 C46 112.7 . . ?
O41 C41 C42 106.4 . . ?
O42 C42 C41 111.6 . . ?
O42 C43 C44 107.3 . . ?
O43 C44 C43 111.5 . . ?
O43 C45 C46 106.5 . . ?
O44 C46 C45 110.2 . . ?
O44 C47 C48 107.2 . . ?
O41 C48 C47 111.6 . . ?
C31' O31' C38' 113.3 . . ?
C31' O31' Li2 109.1(13) . . ?
C38' O31' Li2 110.8(13) . . ?
C33' O32' C32' 113.3 . . ?
C33' O32' Li2 111.0(13) . . ?
C32' O32' Li2 117.7(13) . . ?
C35' O33' C34' 114.6 . . ?
C35' O33' Li2 107.5(13) . . ?
C34' O33' Li2 112.5(13) . . ?
C36' O34' C37' 113.2 . . ?
C36' O34' Li2 115.0(14) . . ?
C37' O34' Li2 111.4(13) . . ?
O31' C31' C32' 111.1 . . ?
O32' C32' C31' 106.9 . . ?
O32' C33' C34' 111.1 . . ?
O33' C34' C33' 106.0 . . ?
O33' C35' C36' 111.6 . . ?
O34' C36' C35' 107.9 . . ?
O34' C37' C38' 110.7 . . ?
O31' C38' C37' 106.7 . . ?
C48' O41' C41' 113.6 . . ?
C48' O41' Li2 110.6(13) . . ?
C41' O41' Li2 109.4(12) . . ?
C42' O42' C43' 113.1 . . ?
C42' O42' Li2 111.5(13) . . ?
C43' O42' Li2 116.0(13) . . ?
C44' O43' C45' 113.7 . . ?
C44' O43' Li2 107.3(13) . . ?
C45' O43' Li2 114.8(13) . . ?
C47' O44' C46' 112.7 . . ?
C47' O44' Li2 116.9(13) . . ?
C46' O44' Li2 109.2(12) . . ?
O41' C41' C42' 106.4 . . ?
O43' C44' C43' 111.5 . . ?
O43' C45' C46' 106.5 . . ?
O44' C46' C45' 110.25(7) . . ?
O44' C47' C48' 107.2 . . ?
O41' C48' C47' 111.6 . . ?

_diffrn_measured_fraction_theta_max 0.488
_diffrn_reflns_theta_full        22.80
_diffrn_measured_fraction_theta_full 0.488
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.141


data_dw0753
_database_code_depnum_ccdc_archive 'CCDC 668766'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H36 Li O8 P3'
_chemical_formula_sum            'C22 H36 Li O8 P3'
_chemical_formula_weight         528.36

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'
P P 0.1023 0.0942 '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           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.7916(2)
_cell_length_b                   8.35170(10)
_cell_length_c                   26.4267(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.3460(10)
_cell_angle_gamma                90.00
_cell_volume                     2595.02(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    34715
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      31.51

_exptl_crystal_description       ?
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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            16782
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.69
_diffrn_reflns_theta_max         31.51
_reflns_number_total             8012
_reflns_number_gt                6868
_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^)+(0.0407P)^2^+1.0364P] 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_extinction_coef       ?
_refine_ls_number_reflns         8012
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0986
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_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 0.68600(18) 0.3303(3) 0.37812(9) 0.0268(4) Uani 1 1 d . . .
P1 P 0.29941(3) 0.58506(4) 0.054781(13) 0.02541(8) Uani 1 1 d . . .
O1 O 0.79329(7) 0.38758(11) 0.30873(4) 0.02585(18) Uani 1 1 d . . .
O2 O 0.77982(8) 0.59593(12) 0.39028(4) 0.0288(2) Uani 1 1 d . . .
O3 O 0.79904(7) 0.32610(10) 0.45012(4) 0.02320(17) Uani 1 1 d . . .
O4 O 0.81473(7) 0.11930(11) 0.37055(4) 0.02415(17) Uani 1 1 d . . .
O5 O 0.58385(7) 0.16674(10) 0.31265(4) 0.02449(18) Uani 1 1 d . . .
O6 O 0.56244(7) 0.49714(11) 0.32719(4) 0.02382(17) Uani 1 1 d . . .
O7 O 0.58562(7) 0.13414(10) 0.41688(4) 0.02347(17) Uani 1 1 d . . .
O8 O 0.56077(7) 0.46040(10) 0.43093(4) 0.02252(17) Uani 1 1 d . . .
C1 C 0.87123(11) 0.51829(17) 0.31484(6) 0.0292(3) Uani 1 1 d . . .
H1A H 0.8912 0.5571 0.2813 0.035 Uiso 1 1 calc R . .
H1B H 0.9419 0.4835 0.3344 0.035 Uiso 1 1 calc R . .
P2 P 0.29438(3) 0.40053(4) 0.161903(13) 0.02310(7) Uani 1 1 d . . .
C2 C 0.81483(11) 0.64992(16) 0.34275(6) 0.0298(3) Uani 1 1 d . . .
H2A H 0.8686 0.7403 0.3485 0.036 Uiso 1 1 calc R . .
H2B H 0.7477 0.6894 0.3216 0.036 Uiso 1 1 calc R . .
P3 P 0.29129(3) 0.35314(4) 0.084229(14) 0.02784(8) Uani 1 1 d . . .
C3 C 0.82606(11) 0.48122(16) 0.47019(5) 0.0265(2) Uani 1 1 d . . .
H3A H 0.8851 0.4714 0.4987 0.032 Uiso 1 1 calc R . .
H3B H 0.7575 0.5290 0.4835 0.032 Uiso 1 1 calc R . .
C4 C 0.86864(11) 0.58940(16) 0.43005(6) 0.0291(3) Uani 1 1 d . . .
H4A H 0.8850 0.6977 0.4440 0.035 Uiso 1 1 calc R . .
H4B H 0.9391 0.5455 0.4173 0.035 Uiso 1 1 calc R . .
C5 C 0.84494(10) 0.24274(17) 0.29269(5) 0.0263(2) Uani 1 1 d . . .
H5A H 0.9021 0.2686 0.2683 0.032 Uiso 1 1 calc R . .
H5B H 0.7862 0.1735 0.2752 0.032 Uiso 1 1 calc R . .
C6 C 0.90148(10) 0.15446(16) 0.33729(5) 0.0245(2) Uani 1 1 d . . .
H6A H 0.9366 0.0543 0.3260 0.029 Uiso 1 1 calc R . .
H6B H 0.9615 0.2216 0.3548 0.029 Uiso 1 1 calc R . .
C7 C 0.85886(10) 0.07539(15) 0.42055(5) 0.0257(2) Uani 1 1 d . . .
H7A H 0.9249 0.0033 0.4183 0.031 Uiso 1 1 calc R . .
H7B H 0.7999 0.0166 0.4378 0.031 Uiso 1 1 calc R . .
C9 C 0.89497(10) 0.22110(15) 0.45125(5) 0.0241(2) Uani 1 1 d . . .
H9A H 0.9188 0.1903 0.4866 0.029 Uiso 1 1 calc R . .
H9B H 0.9597 0.2746 0.4365 0.029 Uiso 1 1 calc R . .
C13 C 0.48836(10) 0.25081(16) 0.28911(5) 0.0259(2) Uani 1 1 d . . .
H13A H 0.4246 0.2505 0.3114 0.031 Uiso 1 1 calc R . .
H13B H 0.4625 0.1998 0.2564 0.031 Uiso 1 1 calc R . .
C14 C 0.55486(10) 0.01859(14) 0.33545(5) 0.0255(2) Uani 1 1 d . . .
H14A H 0.6239 -0.0485 0.3409 0.031 Uiso 1 1 calc R . .
H14B H 0.4995 -0.0396 0.3122 0.031 Uiso 1 1 calc R . .
C15 C 0.46951(10) 0.56246(15) 0.35208(5) 0.0257(2) Uani 1 1 d . . .
H15A H 0.4062 0.4844 0.3516 0.031 Uiso 1 1 calc R . .
H15B H 0.4414 0.6614 0.3347 0.031 Uiso 1 1 calc R . .
C16 C 0.52769(10) 0.41963(16) 0.28049(5) 0.0247(2) Uani 1 1 d . . .
H16A H 0.5921 0.4176 0.2586 0.030 Uiso 1 1 calc R . .
H16B H 0.4650 0.4812 0.2627 0.030 Uiso 1 1 calc R . .
C17 C 0.47792(10) 0.35324(15) 0.44864(5) 0.0229(2) Uani 1 1 d . . .
H17A H 0.4153 0.3361 0.4221 0.027 Uiso 1 1 calc R . .
H17B H 0.4455 0.3974 0.4792 0.027 Uiso 1 1 calc R . .
C18 C 0.51283(10) 0.59903(14) 0.40596(5) 0.0250(2) Uani 1 1 d . . .
H18A H 0.5713 0.6841 0.4059 0.030 Uiso 1 1 calc R . .
H18B H 0.4494 0.6394 0.4249 0.030 Uiso 1 1 calc R . .
C19 C 0.50437(10) 0.04506(14) 0.38550(5) 0.0247(2) Uani 1 1 d . . .
H19A H 0.4321 0.1054 0.3804 0.030 Uiso 1 1 calc R . .
H19B H 0.4886 -0.0589 0.4016 0.030 Uiso 1 1 calc R . .
C20 C 0.53915(10) 0.19773(15) 0.46117(5) 0.0241(2) Uani 1 1 d . . .
H20A H 0.6011 0.2164 0.4879 0.029 Uiso 1 1 calc R . .
H20B H 0.4854 0.1196 0.4742 0.029 Uiso 1 1 calc R . .
C25 C 0.32748(10) 0.94855(14) 0.15764(6) 0.0257(2) Uani 1 1 d . . .
H25A H 0.3364 1.0616 0.1570 0.031 Uiso 1 1 calc R . .
C26 C 0.32357(10) 0.86846(15) 0.20440(5) 0.0242(2) Uani 1 1 d . . .
H26A H 0.3292 0.9275 0.2352 0.029 Uiso 1 1 calc R . .
C27 C 0.31153(9) 0.70472(14) 0.20535(5) 0.0204(2) Uani 1 1 d . . .
H27A H 0.3079 0.6521 0.2370 0.024 Uiso 1 1 calc R . .
C28 C 0.31853(10) 0.86419(14) 0.11312(5) 0.0231(2) Uani 1 1 d . . .
H28A H 0.3198 0.9202 0.0819 0.028 Uiso 1 1 calc R . .
C29 C 0.30443(9) 0.61261(13) 0.16016(4) 0.01807(19) Uani 1 1 d . . .
C30 C 0.30737(9) 0.69419(14) 0.11255(4) 0.0191(2) 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
Li1 0.0235(10) 0.0298(10) 0.0271(12) 0.0012(9) 0.0013(8) -0.0005(8)
P1 0.02567(15) 0.03134(16) 0.01946(15) -0.00011(12) 0.00334(11) -0.00188(12)
O1 0.0175(4) 0.0302(4) 0.0301(5) -0.0008(4) 0.0029(3) 0.0003(3)
O2 0.0217(4) 0.0380(5) 0.0265(5) 0.0027(4) -0.0001(3) 0.0004(4)
O3 0.0182(4) 0.0252(4) 0.0261(4) -0.0027(3) 0.0009(3) 0.0017(3)
O4 0.0178(4) 0.0312(4) 0.0234(4) -0.0017(4) 0.0013(3) 0.0003(3)
O5 0.0158(3) 0.0242(4) 0.0333(5) 0.0029(4) 0.0008(3) 0.0012(3)
O6 0.0176(4) 0.0271(4) 0.0270(5) -0.0022(4) 0.0027(3) 0.0018(3)
O7 0.0190(4) 0.0222(4) 0.0292(5) -0.0025(3) 0.0022(3) 0.0009(3)
O8 0.0181(4) 0.0203(4) 0.0292(5) 0.0021(3) 0.0019(3) 0.0011(3)
C1 0.0208(5) 0.0349(6) 0.0324(7) 0.0067(5) 0.0058(5) -0.0042(5)
P2 0.02737(15) 0.01746(13) 0.02439(16) 0.00176(11) 0.00137(11) -0.00129(11)
C2 0.0281(6) 0.0269(6) 0.0344(7) 0.0083(5) 0.0023(5) -0.0010(5)
P3 0.03066(16) 0.02596(15) 0.02707(18) -0.00575(13) 0.00334(12) -0.00211(12)
C3 0.0243(5) 0.0324(6) 0.0225(6) -0.0088(5) -0.0006(4) 0.0010(5)
C4 0.0248(6) 0.0292(6) 0.0322(7) -0.0033(5) -0.0043(5) -0.0033(5)
C5 0.0205(5) 0.0376(6) 0.0212(6) -0.0071(5) 0.0033(4) 0.0019(5)
C6 0.0179(5) 0.0315(6) 0.0245(6) -0.0064(5) 0.0043(4) 0.0027(4)
C7 0.0229(5) 0.0247(5) 0.0291(6) 0.0043(5) -0.0003(4) 0.0037(4)
C9 0.0197(5) 0.0296(6) 0.0225(6) 0.0024(5) -0.0006(4) 0.0041(4)
C13 0.0172(5) 0.0291(6) 0.0308(7) -0.0030(5) -0.0032(4) 0.0022(4)
C14 0.0235(5) 0.0183(5) 0.0351(7) -0.0045(5) 0.0042(5) -0.0004(4)
C15 0.0195(5) 0.0253(5) 0.0323(7) 0.0020(5) 0.0019(4) 0.0075(4)
C16 0.0214(5) 0.0320(6) 0.0203(5) 0.0042(5) -0.0007(4) 0.0032(4)
C17 0.0194(5) 0.0258(5) 0.0241(6) -0.0026(5) 0.0059(4) -0.0011(4)
C18 0.0241(5) 0.0191(5) 0.0320(7) -0.0020(5) 0.0027(4) 0.0057(4)
C19 0.0221(5) 0.0169(5) 0.0356(7) -0.0024(5) 0.0042(5) -0.0034(4)
C20 0.0240(5) 0.0275(5) 0.0209(6) 0.0040(5) 0.0025(4) -0.0001(4)
C25 0.0189(5) 0.0172(5) 0.0406(7) 0.0012(5) 0.0004(5) 0.0006(4)
C26 0.0184(5) 0.0237(5) 0.0300(6) -0.0071(5) -0.0003(4) 0.0009(4)
C27 0.0165(4) 0.0233(5) 0.0211(5) 0.0000(4) 0.0004(4) 0.0011(4)
C28 0.0176(5) 0.0220(5) 0.0297(6) 0.0072(5) 0.0010(4) 0.0003(4)
C29 0.0149(4) 0.0177(4) 0.0215(5) 0.0013(4) 0.0008(4) 0.0000(3)
C30 0.0146(4) 0.0220(5) 0.0206(5) 0.0015(4) 0.0010(4) -0.0006(4)

_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 O3 2.239(3) . ?
Li1 O7 2.306(2) . ?
Li1 O4 2.345(2) . ?
Li1 O1 2.354(3) . ?
Li1 O6 2.362(2) . ?
Li1 O8 2.371(2) . ?
Li1 O5 2.449(3) . ?
Li1 O2 2.489(3) . ?
P1 C30 1.7744(12) . ?
P1 P3 2.0923(5) . ?
O1 C1 1.4282(16) . ?
O1 C5 1.4329(16) . ?
O2 C2 1.4246(17) . ?
O2 C4 1.4275(16) . ?
O3 C3 1.4268(15) . ?
O3 C9 1.4298(14) . ?
O4 C7 1.4306(16) . ?
O4 C6 1.4288(14) . ?
O5 C14 1.4289(15) . ?
O5 C13 1.4289(14) . ?
O6 C16 1.4261(16) . ?
O6 C15 1.4283(14) . ?
O7 C19 1.4277(15) . ?
O7 C20 1.4315(15) . ?
O8 C18 1.4279(15) . ?
O8 C17 1.4296(14) . ?
C1 C2 1.506(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
P2 C29 1.7760(11) . ?
P2 P3 2.0881(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.508(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.5027(19) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C9 1.5061(19) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C13 C16 1.5070(18) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C19 1.5074(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C18 1.5072(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C20 1.5105(17) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C25 C28 1.3686(19) . ?
C25 C26 1.4090(19) . ?
C25 H25A 0.9500 . ?
C26 C27 1.3753(17) . ?
C26 H26A 0.9500 . ?
C27 C29 1.4177(16) . ?
C27 H27A 0.9500 . ?
C28 C30 1.4258(16) . ?
C28 H28A 0.9500 . ?
C29 C30 1.4335(16) . ?

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
O3 Li1 O7 84.49(9) . . ?
O3 Li1 O4 73.32(7) . . ?
O7 Li1 O4 82.02(8) . . ?
O3 Li1 O1 110.16(9) . . ?
O7 Li1 O1 144.51(12) . . ?
O4 Li1 O1 72.33(7) . . ?
O3 Li1 O6 142.70(12) . . ?
O7 Li1 O6 110.91(9) . . ?
O4 Li1 O6 140.37(12) . . ?
O1 Li1 O6 77.36(8) . . ?
O3 Li1 O8 82.20(9) . . ?
O7 Li1 O8 72.58(7) . . ?
O4 Li1 O8 146.19(11) . . ?
O1 Li1 O8 139.54(11) . . ?
O6 Li1 O8 71.36(7) . . ?
O3 Li1 O5 145.17(11) . . ?
O7 Li1 O5 71.08(7) . . ?
O4 Li1 O5 78.88(8) . . ?
O1 Li1 O5 80.07(8) . . ?
O6 Li1 O5 71.17(7) . . ?
O8 Li1 O5 112.13(9) . . ?
O3 Li1 O2 70.99(7) . . ?
O7 Li1 O2 144.50(12) . . ?
O4 Li1 O2 113.37(9) . . ?
O1 Li1 O2 70.11(7) . . ?
O6 Li1 O2 78.28(8) . . ?
O8 Li1 O2 78.83(8) . . ?
O5 Li1 O2 141.14(11) . . ?
C30 P1 P3 99.00(4) . . ?
C1 O1 C5 113.23(9) . . ?
C1 O1 Li1 116.50(10) . . ?
C5 O1 Li1 108.94(9) . . ?
C2 O2 C4 114.57(10) . . ?
C2 O2 Li1 108.91(10) . . ?
C4 O2 Li1 110.80(9) . . ?
C3 O3 C9 113.26(9) . . ?
C3 O3 Li1 113.79(10) . . ?
C9 O3 Li1 116.53(9) . . ?
C7 O4 C6 113.18(9) . . ?
C7 O4 Li1 107.84(9) . . ?
C6 O4 Li1 113.35(9) . . ?
C14 O5 C13 113.78(9) . . ?
C14 O5 Li1 107.81(9) . . ?
C13 O5 Li1 111.26(9) . . ?
C16 O6 C15 113.07(9) . . ?
C16 O6 Li1 110.48(9) . . ?
C15 O6 Li1 115.12(9) . . ?
C19 O7 C20 112.74(9) . . ?
C19 O7 Li1 117.18(10) . . ?
C20 O7 Li1 109.91(9) . . ?
C18 O8 C17 113.73(9) . . ?
C18 O8 Li1 110.00(9) . . ?
C17 O8 Li1 112.18(9) . . ?
O1 C1 C2 108.00(10) . . ?
O1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
O1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
C29 P2 P3 99.19(4) . . ?
O2 C2 C1 111.64(11) . . ?
O2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
O2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
P2 P3 P1 101.084(19) . . ?
O3 C3 C4 111.06(11) . . ?
O3 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
O3 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O2 C4 C3 106.02(10) . . ?
O2 C4 H4A 110.5 . . ?
C3 C4 H4A 110.5 . . ?
O2 C4 H4B 110.5 . . ?
C3 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
O1 C5 C6 110.81(10) . . ?
O1 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O4 C6 C5 106.72(9) . . ?
O4 C6 H6A 110.4 . . ?
C5 C6 H6A 110.4 . . ?
O4 C6 H6B 110.4 . . ?
C5 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
O4 C7 C9 111.02(10) . . ?
O4 C7 H7A 109.4 . . ?
C9 C7 H7A 109.4 . . ?
O4 C7 H7B 109.4 . . ?
C9 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O3 C9 C7 107.06(9) . . ?
O3 C9 H9A 110.3 . . ?
C7 C9 H9A 110.3 . . ?
O3 C9 H9B 110.3 . . ?
C7 C9 H9B 110.3 . . ?
H9A C9 H9B 108.6 . . ?
O5 C13 C16 106.51(9) . . ?
O5 C13 H13A 110.4 . . ?
C16 C13 H13A 110.4 . . ?
O5 C13 H13B 110.4 . . ?
C16 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
O5 C14 C19 111.47(10) . . ?
O5 C14 H14A 109.3 . . ?
C19 C14 H14A 109.3 . . ?
O5 C14 H14B 109.3 . . ?
C19 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
O6 C15 C18 107.19(10) . . ?
O6 C15 H15A 110.3 . . ?
C18 C15 H15A 110.3 . . ?
O6 C15 H15B 110.3 . . ?
C18 C15 H15B 110.3 . . ?
H15A C15 H15B 108.5 . . ?
O6 C16 C13 111.43(10) . . ?
O6 C16 H16A 109.3 . . ?
C13 C16 H16A 109.3 . . ?
O6 C16 H16B 109.3 . . ?
C13 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
O8 C17 C20 106.43(9) . . ?
O8 C17 H17A 110.4 . . ?
C20 C17 H17A 110.4 . . ?
O8 C17 H17B 110.4 . . ?
C20 C17 H17B 110.4 . . ?
H17A C17 H17B 108.6 . . ?
O8 C18 C15 111.48(10) . . ?
O8 C18 H18A 109.3 . . ?
C15 C18 H18A 109.3 . . ?
O8 C18 H18B 109.3 . . ?
C15 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
O7 C19 C14 107.08(10) . . ?
O7 C19 H19A 110.3 . . ?
C14 C19 H19A 110.3 . . ?
O7 C19 H19B 110.3 . . ?
C14 C19 H19B 110.3 . . ?
H19A C19 H19B 108.6 . . ?
O7 C20 C17 110.25(10) . . ?
O7 C20 H20A 109.6 . . ?
C17 C20 H20A 109.6 . . ?
O7 C20 H20B 109.6 . . ?
C17 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C28 C25 C26 120.27(11) . . ?
C28 C25 H25A 119.9 . . ?
C26 C25 H25A 119.9 . . ?
C27 C26 C25 119.89(12) . . ?
C27 C26 H26A 120.1 . . ?
C25 C26 H26A 120.1 . . ?
C26 C27 C29 121.59(11) . . ?
C26 C27 H27A 119.2 . . ?
C29 C27 H27A 119.2 . . ?
C25 C28 C30 121.51(12) . . ?
C25 C28 H28A 119.2 . . ?
C30 C28 H28A 119.2 . . ?
C27 C29 C30 118.53(10) . . ?
C27 C29 P2 121.27(9) . . ?
C30 C29 P2 120.19(9) . . ?
C28 C30 C29 118.19(11) . . ?
C28 C30 P1 121.28(9) . . ?
C29 C30 P1 120.51(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Li1 O1 C1 -46.88(14) . . . . ?
O7 Li1 O1 C1 -156.67(17) . . . . ?
O4 Li1 O1 C1 -110.92(10) . . . . ?
O6 Li1 O1 C1 94.94(10) . . . . ?
O8 Li1 O1 C1 55.11(19) . . . . ?
O5 Li1 O1 C1 167.69(9) . . . . ?
O2 Li1 O1 C1 13.00(10) . . . . ?
O3 Li1 O1 C5 82.70(12) . . . . ?
O7 Li1 O1 C5 -27.1(2) . . . . ?
O4 Li1 O1 C5 18.66(9) . . . . ?
O6 Li1 O1 C5 -135.48(8) . . . . ?
O8 Li1 O1 C5 -175.31(15) . . . . ?
O5 Li1 O1 C5 -62.73(9) . . . . ?
O2 Li1 O1 C5 142.58(8) . . . . ?
O3 Li1 O2 C2 138.13(9) . . . . ?
O7 Li1 O2 C2 -173.02(17) . . . . ?
O4 Li1 O2 C2 76.78(12) . . . . ?
O1 Li1 O2 C2 17.31(9) . . . . ?
O6 Li1 O2 C2 -63.33(9) . . . . ?
O8 Li1 O2 C2 -136.36(9) . . . . ?
O5 Li1 O2 C2 -24.84(19) . . . . ?
O3 Li1 O2 C4 11.24(10) . . . . ?
O7 Li1 O2 C4 60.1(2) . . . . ?
O4 Li1 O2 C4 -50.10(14) . . . . ?
O1 Li1 O2 C4 -109.57(9) . . . . ?
O6 Li1 O2 C4 169.79(9) . . . . ?
O8 Li1 O2 C4 96.76(10) . . . . ?
O5 Li1 O2 C4 -151.72(15) . . . . ?
O7 Li1 O3 C3 -133.46(9) . . . . ?
O4 Li1 O3 C3 143.24(9) . . . . ?
O1 Li1 O3 C3 79.82(12) . . . . ?
O6 Li1 O3 C3 -15.7(2) . . . . ?
O8 Li1 O3 C3 -60.34(10) . . . . ?
O5 Li1 O3 C3 -178.30(17) . . . . ?
O2 Li1 O3 C3 20.48(10) . . . . ?
O7 Li1 O3 C9 91.91(10) . . . . ?
O4 Li1 O3 C9 8.62(10) . . . . ?
O1 Li1 O3 C9 -54.81(13) . . . . ?
O6 Li1 O3 C9 -150.37(16) . . . . ?
O8 Li1 O3 C9 165.03(8) . . . . ?
O5 Li1 O3 C9 47.1(2) . . . . ?
O2 Li1 O3 C9 -114.15(9) . . . . ?
O3 Li1 O4 C7 20.82(9) . . . . ?
O7 Li1 O4 C7 -65.79(9) . . . . ?
O1 Li1 O4 C7 139.04(8) . . . . ?
O6 Li1 O4 C7 -179.10(15) . . . . ?
O8 Li1 O4 C7 -24.6(2) . . . . ?
O5 Li1 O4 C7 -137.96(8) . . . . ?
O2 Li1 O4 C7 80.82(12) . . . . ?
O3 Li1 O4 C6 -105.29(9) . . . . ?
O7 Li1 O4 C6 168.11(8) . . . . ?
O1 Li1 O4 C6 12.94(10) . . . . ?
O6 Li1 O4 C6 54.79(19) . . . . ?
O8 Li1 O4 C6 -150.72(18) . . . . ?
O5 Li1 O4 C6 95.93(9) . . . . ?
O2 Li1 O4 C6 -45.28(13) . . . . ?
O3 Li1 O5 C14 28.7(2) . . . . ?
O7 Li1 O5 C14 -19.20(9) . . . . ?
O4 Li1 O5 C14 66.08(9) . . . . ?
O1 Li1 O5 C14 139.85(8) . . . . ?
O6 Li1 O5 C14 -140.24(8) . . . . ?
O8 Li1 O5 C14 -80.45(11) . . . . ?
O2 Li1 O5 C14 179.68(14) . . . . ?
O3 Li1 O5 C13 154.11(18) . . . . ?
O7 Li1 O5 C13 106.21(9) . . . . ?
O4 Li1 O5 C13 -168.51(9) . . . . ?
O1 Li1 O5 C13 -94.74(9) . . . . ?
O6 Li1 O5 C13 -14.82(10) . . . . ?
O8 Li1 O5 C13 44.96(13) . . . . ?
O2 Li1 O5 C13 -54.91(18) . . . . ?
O3 Li1 O6 C16 172.93(16) . . . . ?
O7 Li1 O6 C16 -77.69(12) . . . . ?
O4 Li1 O6 C16 25.51(19) . . . . ?
O1 Li1 O6 C16 66.17(9) . . . . ?
O8 Li1 O6 C16 -139.84(8) . . . . ?
O5 Li1 O6 C16 -17.50(9) . . . . ?
O2 Li1 O6 C16 138.13(8) . . . . ?
O3 Li1 O6 C15 -57.5(2) . . . . ?
O7 Li1 O6 C15 51.88(13) . . . . ?
O4 Li1 O6 C15 155.08(15) . . . . ?
O1 Li1 O6 C15 -164.26(9) . . . . ?
O8 Li1 O6 C15 -10.27(10) . . . . ?
O5 Li1 O6 C15 112.08(9) . . . . ?
O2 Li1 O6 C15 -92.29(9) . . . . ?
O3 Li1 O7 C19 -165.99(8) . . . . ?
O4 Li1 O7 C19 -92.11(9) . . . . ?
O1 Li1 O7 C19 -48.5(2) . . . . ?
O6 Li1 O7 C19 49.06(13) . . . . ?
O8 Li1 O7 C19 110.47(9) . . . . ?
O5 Li1 O7 C19 -11.19(10) . . . . ?
O2 Li1 O7 C19 148.34(16) . . . . ?
O3 Li1 O7 C20 63.61(10) . . . . ?
O4 Li1 O7 C20 137.49(8) . . . . ?
O1 Li1 O7 C20 -178.94(17) . . . . ?
O6 Li1 O7 C20 -81.34(12) . . . . ?
O8 Li1 O7 C20 -19.93(9) . . . . ?
O5 Li1 O7 C20 -141.59(8) . . . . ?
O2 Li1 O7 C20 17.9(2) . . . . ?
O3 Li1 O8 C18 133.53(9) . . . . ?
O7 Li1 O8 C18 -139.84(8) . . . . ?
O4 Li1 O8 C18 177.06(18) . . . . ?
O1 Li1 O8 C18 21.47(19) . . . . ?
O6 Li1 O8 C18 -19.79(9) . . . . ?
O5 Li1 O8 C18 -79.47(12) . . . . ?
O2 Li1 O8 C18 61.47(9) . . . . ?
O3 Li1 O8 C17 -98.82(9) . . . . ?
O7 Li1 O8 C17 -12.18(10) . . . . ?
O4 Li1 O8 C17 -55.3(2) . . . . ?
O1 Li1 O8 C17 149.13(15) . . . . ?
O6 Li1 O8 C17 107.87(9) . . . . ?
O5 Li1 O8 C17 48.19(13) . . . . ?
O2 Li1 O8 C17 -170.87(8) . . . . ?
C5 O1 C1 C2 -167.26(11) . . . . ?
Li1 O1 C1 C2 -39.76(14) . . . . ?
C4 O2 C2 C1 79.97(14) . . . . ?
Li1 O2 C2 C1 -44.73(13) . . . . ?
O1 C1 C2 O2 56.87(15) . . . . ?
C29 P2 P3 P1 -0.84(4) . . . . ?
C30 P1 P3 P2 1.12(4) . . . . ?
C9 O3 C3 C4 85.67(13) . . . . ?
Li1 O3 C3 C4 -50.46(13) . . . . ?
C2 O2 C4 C3 -161.53(11) . . . . ?
Li1 O2 C4 C3 -37.83(13) . . . . ?
O3 C3 C4 O2 58.47(13) . . . . ?
C1 O1 C5 C6 83.50(13) . . . . ?
Li1 O1 C5 C6 -47.86(12) . . . . ?
C7 O4 C6 C5 -163.83(10) . . . . ?
Li1 O4 C6 C5 -40.61(13) . . . . ?
O1 C5 C6 O4 59.75(13) . . . . ?
C6 O4 C7 C9 79.11(12) . . . . ?
Li1 O4 C7 C9 -47.10(12) . . . . ?
C3 O3 C9 C7 -169.73(11) . . . . ?
Li1 O3 C9 C7 -34.87(13) . . . . ?
O4 C7 C9 O3 54.87(13) . . . . ?
C14 O5 C13 C16 164.50(10) . . . . ?
Li1 O5 C13 C16 42.49(13) . . . . ?
C13 O5 C14 C19 -77.24(13) . . . . ?
Li1 O5 C14 C19 46.67(12) . . . . ?
C16 O6 C15 C18 164.87(10) . . . . ?
Li1 O6 C15 C18 36.58(13) . . . . ?
C15 O6 C16 C13 -82.55(12) . . . . ?
Li1 O6 C16 C13 48.11(12) . . . . ?
O5 C13 C16 O6 -61.72(13) . . . . ?
C18 O8 C17 C20 165.63(10) . . . . ?
Li1 O8 C17 C20 39.99(13) . . . . ?
C17 O8 C18 C15 -79.45(13) . . . . ?
Li1 O8 C18 C15 47.34(12) . . . . ?
O6 C15 C18 O8 -56.10(13) . . . . ?
C20 O7 C19 C14 167.11(10) . . . . ?
Li1 O7 C19 C14 38.04(13) . . . . ?
O5 C14 C19 O7 -56.94(13) . . . . ?
C19 O7 C20 C17 -83.26(12) . . . . ?
Li1 O7 C20 C17 49.47(12) . . . . ?
O8 C17 C20 O7 -60.24(12) . . . . ?
C28 C25 C26 C27 0.47(17) . . . . ?
C25 C26 C27 C29 0.90(17) . . . . ?
C26 C25 C28 C30 -1.26(18) . . . . ?
C26 C27 C29 C30 -1.45(16) . . . . ?
C26 C27 C29 P2 177.55(9) . . . . ?
P3 P2 C29 C27 -178.76(8) . . . . ?
P3 P2 C29 C30 0.23(9) . . . . ?
C25 C28 C30 C29 0.68(16) . . . . ?
C25 C28 C30 P1 -178.39(9) . . . . ?
C27 C29 C30 C28 0.66(15) . . . . ?
P2 C29 C30 C28 -178.36(8) . . . . ?
C27 C29 C30 P1 179.73(8) . . . . ?
P2 C29 C30 P1 0.72(12) . . . . ?
P3 P1 C30 C28 177.83(8) . . . . ?
P3 P1 C30 C29 -1.22(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.926
_diffrn_reflns_theta_full        31.51
_diffrn_measured_fraction_theta_full 0.926
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.046