# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011


data_global

_journal_coden_Cambridge         222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Coles, Martyn'
'Hitchcock, Peter'
'Khvostov, Alexei'
'Lappert, M.'
'Maron, Laurent'

_publ_contact_author_name        'Coles, Martyn'
_publ_contact_author_email       m.f.lappert@sussex.ac.uk

_publ_section_title              
;
Synthesis and structures
of the [benzamidinato]3- complexes Li3(tmeda)(L 1)]2 and [Li(thf)4][Li5(L
2)(OEt2)2] [L1 = N(SiMe3)C(Ph)N(SiMe3) and L2 = N(SiMe3)C(C6H4-4)NPh ]
;
_publ_requested_category         FM

# Attachment '- MFL_Dalton_oct10.cif'

data_(1)-sep1704
_database_code_depnum_ccdc_archive 'CCDC 799009'
#TrackingRef '- MFL_Dalton_oct10.cif'

_audit_creation_date             2004-09-13T14:47:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C38 H78 Li6 N8 Si4'
_chemical_formula_sum            'C38 H78 Li6 N8 Si4'
_chemical_formula_weight         801.08
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.0477(4)
_cell_length_b                   19.2862(7)
_cell_length_c                   12.8398(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.749(2)
_cell_angle_gamma                90
_cell_volume                     2590.58(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7532
_cell_measurement_theta_min      3.705
_cell_measurement_theta_max      25.028
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.912898E-1
_diffrn_orient_matrix_ub_12      -0.153059E-1
_diffrn_orient_matrix_ub_13      0.274289E-1
_diffrn_orient_matrix_ub_21      -0.246381E-1
_diffrn_orient_matrix_ub_22      -0.452738E-1
_diffrn_orient_matrix_ub_23      -0.390347E-1
_diffrn_orient_matrix_ub_31      0.140122E-1
_diffrn_orient_matrix_ub_32      0.201119E-1
_diffrn_orient_matrix_ub_33      -0.669965E-1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_number            14932
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.72
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_reflns_number_total             4526
_reflns_number_gt                3415
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;

There is disorder of the TMEDA ligand and also of the Si1Me3 group.

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^)+(0.0645P)^2^+1.4165P] 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    riding
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4526
_refine_ls_number_parameters     327
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.048
_refine_ls_wR_factor_ref         0.1303
_refine_ls_wR_factor_gt          0.116
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_restrained_S_all      0.965
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.039

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.5971(6) 0.4338(3) 0.5122(4) 0.0775(17) Uani 1 1 d . . .
Li2 Li 0.3501(4) 0.4228(2) 0.5318(3) 0.0507(10) Uani 1 1 d . . .
Li3 Li 0.7994(4) 0.6317(2) 0.7964(3) 0.0453(10) Uani 1 1 d . A .
Si1 Si 0.57532(6) 0.35943(3) 0.72667(5) 0.0394(2) Uani 1 1 d . . .
Si2 Si 0.27779(6) 0.53742(3) 0.67318(5) 0.03397(18) Uani 1 1 d . . .
N1 N 0.53228(17) 0.42244(9) 0.63236(13) 0.0329(4) Uani 1 1 d . A .
N2 N 0.38052(16) 0.51469(10) 0.60766(14) 0.0347(4) Uani 1 1 d . . .
N3 N 0.8004(2) 0.60899(14) 0.95547(17) 0.0635(7) Uani 1 1 d . . .
N4 N 0.9476(2) 0.70321(11) 0.87148(16) 0.0525(6) Uani 1 1 d . . .
C1 C 0.51036(19) 0.49434(11) 0.64329(15) 0.0278(5) Uani 1 1 d . . .
C2 C 0.60695(19) 0.54244(10) 0.66194(15) 0.0285(5) Uani 1 1 d . A .
C3 C 0.5869(2) 0.61849(11) 0.65875(17) 0.0370(5) Uani 1 1 d . . .
H3 H 0.5179 0.6373 0.6786 0.044 Uiso 1 1 calc R A .
C4 C 0.6672(2) 0.66179(12) 0.62738(18) 0.0441(6) Uani 1 1 d . . .
H4 H 0.6461 0.7096 0.6165 0.053 Uiso 1 1 calc R . .
C5 C 0.7808(2) 0.63760(14) 0.61062(18) 0.0471(6) Uani 1 1 d . . .
H5 H 0.827 0.665 0.5749 0.057 Uiso 1 1 calc R A .
C6 C 0.8214(2) 0.56980(13) 0.65051(18) 0.0414(6) Uani 1 1 d . . .
H6 H 0.9053 0.5552 0.6558 0.05 Uiso 1 1 calc R . .
C7 C 0.7431(2) 0.52497(12) 0.68141(17) 0.0348(5) Uani 1 1 d . . .
H7 H 0.7764 0.4823 0.7156 0.042 Uiso 1 1 calc R A .
C11 C 0.3533(3) 0.56523(16) 0.8196(2) 0.0586(7) Uani 1 1 d . . .
H11A H 0.4069 0.5276 0.8614 0.088 Uiso 1 1 calc R . .
H11B H 0.2864 0.5762 0.8519 0.088 Uiso 1 1 calc R . .
H11C H 0.4061 0.6064 0.8221 0.088 Uiso 1 1 calc R . .
C12 C 0.1634(3) 0.46566(16) 0.6747(3) 0.0629(8) Uani 1 1 d . . .
H12A H 0.121 0.4495 0.5993 0.094 Uiso 1 1 calc R . .
H12B H 0.0991 0.4829 0.706 0.094 Uiso 1 1 calc R . .
H12C H 0.2104 0.4271 0.7194 0.094 Uiso 1 1 calc R . .
C13 C 0.1754(3) 0.61031(15) 0.5953(2) 0.0625(8) Uani 1 1 d . . .
H13A H 0.1356 0.5966 0.5184 0.094 Uiso 1 1 calc R . .
H13B H 0.2285 0.6515 0.5989 0.094 Uiso 1 1 calc R . .
H13C H 0.1088 0.6208 0.6281 0.094 Uiso 1 1 calc R . .
C8 C 0.7516(5) 0.3473(3) 0.7891(7) 0.090(3) Uani 0.562(7) 1 d P A 1
H8A H 0.7903 0.3902 0.8258 0.134 Uiso 0.562(7) 1 calc PR A 1
H8B H 0.7885 0.3357 0.7314 0.134 Uiso 0.562(7) 1 calc PR A 1
H8C H 0.7687 0.3096 0.8431 0.134 Uiso 0.562(7) 1 calc PR A 1
C9 C 0.5126(8) 0.2755(3) 0.6610(5) 0.086(3) Uani 0.562(7) 1 d P A 1
H9A H 0.5445 0.2671 0.5992 0.13 Uiso 0.562(7) 1 calc PR A 1
H9B H 0.419 0.2769 0.6342 0.13 Uiso 0.562(7) 1 calc PR A 1
H9C H 0.5412 0.2381 0.715 0.13 Uiso 0.562(7) 1 calc PR A 1
C10 C 0.5134(9) 0.3696(4) 0.8444(5) 0.095(3) Uani 0.562(7) 1 d P A 1
H10A H 0.544 0.4136 0.882 0.142 Uiso 0.562(7) 1 calc PR A 1
H10B H 0.5439 0.3311 0.896 0.142 Uiso 0.562(7) 1 calc PR A 1
H10C H 0.4198 0.3695 0.8173 0.142 Uiso 0.562(7) 1 calc PR A 1
C14 C 0.9240(6) 0.6316(5) 1.0241(4) 0.0606(19) Uani 0.621(13) 1 d P B 1
H14A H 0.9894 0.5974 1.0206 0.073 Uiso 0.621(13) 1 calc PR B 1
H14B H 0.9249 0.6345 1.1013 0.073 Uiso 0.621(13) 1 calc PR B 1
C15 C 0.9566(4) 0.70247(18) 0.9871(2) 0.0745(9) Uani 0.621(13) 1 d P B 1
H15A H 0.8976 0.7376 0.9997 0.089 Uiso 0.621(13) 1 calc PR B 1
H15B H 1.0446 0.7153 1.0323 0.089 Uiso 0.621(13) 1 calc PR B 1
C16 C 0.6922(9) 0.6491(9) 0.9773(9) 0.143(5) Uani 0.621(13) 1 d P B 1
H16A H 0.6099 0.6318 0.9288 0.215 Uiso 0.621(13) 1 calc PR B 1
H16B H 0.7003 0.6985 0.9628 0.215 Uiso 0.621(13) 1 calc PR B 1
H16C H 0.6966 0.6428 1.0541 0.215 Uiso 0.621(13) 1 calc PR B 1
C17 C 0.7848(11) 0.5347(5) 0.9698(6) 0.122(4) Uani 0.621(13) 1 d P B 1
H17A H 0.7008 0.5198 0.9213 0.183 Uiso 0.621(13) 1 calc PR B 1
H17B H 0.7914 0.5253 1.0464 0.183 Uiso 0.621(13) 1 calc PR B 1
H17C H 0.8518 0.5091 0.9512 0.183 Uiso 0.621(13) 1 calc PR B 1
C18 C 1.0690(14) 0.6895(9) 0.8531(14) 0.135(7) Uani 0.621(13) 1 d P B 1
H18A H 1.0565 0.6903 0.774 0.202 Uiso 0.621(13) 1 calc PR B 1
H18B H 1.1009 0.6438 0.8829 0.202 Uiso 0.621(13) 1 calc PR B 1
H18C H 1.1313 0.7251 0.89 0.202 Uiso 0.621(13) 1 calc PR B 1
C19 C 0.8993(11) 0.7760(5) 0.8397(8) 0.088(3) Uani 0.621(13) 1 d P B 1
H19A H 0.8182 0.7825 0.8541 0.132 Uiso 0.621(13) 1 calc PR B 1
H19B H 0.8861 0.7833 0.7612 0.132 Uiso 0.621(13) 1 calc PR B 1
H19C H 0.9622 0.8094 0.883 0.132 Uiso 0.621(13) 1 calc PR B 1
C8A C 0.6628(14) 0.3861(5) 0.8711(7) 0.138(7) Uani 0.438(7) 1 d P A 2
H8A1 H 0.615 0.4228 0.8933 0.208 Uiso 0.438(7) 1 calc PR A 2
H8A2 H 0.7478 0.4032 0.8757 0.208 Uiso 0.438(7) 1 calc PR A 2
H8A3 H 0.6715 0.3461 0.92 0.208 Uiso 0.438(7) 1 calc PR A 2
C9A C 0.6601(19) 0.2912(6) 0.6778(13) 0.198(12) Uani 0.438(7) 1 d P A 2
H9A1 H 0.6096 0.2777 0.6028 0.298 Uiso 0.438(7) 1 calc PR A 2
H9A2 H 0.6725 0.2508 0.7264 0.298 Uiso 0.438(7) 1 calc PR A 2
H9A3 H 0.7435 0.3088 0.6781 0.298 Uiso 0.438(7) 1 calc PR A 2
C10A C 0.4304(10) 0.3171(6) 0.7460(11) 0.132(5) Uani 0.438(7) 1 d P A 2
H10D H 0.384 0.3512 0.7755 0.198 Uiso 0.438(7) 1 calc PR A 2
H10E H 0.4574 0.2784 0.7976 0.198 Uiso 0.438(7) 1 calc PR A 2
H10F H 0.3745 0.2999 0.6751 0.198 Uiso 0.438(7) 1 calc PR A 2
C14A C 0.8738(18) 0.6709(9) 1.0221(8) 0.084(5) Uani 0.379(13) 1 d P B 2
H14C H 0.8101 0.7057 1.0275 0.101 Uiso 0.379(13) 1 calc PR B 2
H14D H 0.9188 0.6544 1.0977 0.101 Uiso 0.379(13) 1 calc PR B 2
C15A C 0.9566(4) 0.70247(18) 0.9871(2) 0.0745(9) Uani 0.379(13) 1 d P B 2
H15C H 1.0413 0.6827 1.028 0.089 Uiso 0.379(13) 1 calc PR B 2
H15D H 0.9581 0.7515 1.0104 0.089 Uiso 0.379(13) 1 calc PR B 2
C16A C 0.6821(15) 0.6032(7) 0.9685(11) 0.088(4) Uani 0.379(13) 1 d P B 2
H16D H 0.6332 0.6458 0.9429 0.132 Uiso 0.379(13) 1 calc PR B 2
H16E H 0.6923 0.5959 1.0464 0.132 Uiso 0.379(13) 1 calc PR B 2
H16F H 0.6363 0.5637 0.9255 0.132 Uiso 0.379(13) 1 calc PR B 2
C17A C 0.873(2) 0.5446(10) 0.9914(11) 0.123(7) Uani 0.379(13) 1 d P B 2
H17D H 0.9507 0.5458 0.9709 0.184 Uiso 0.379(13) 1 calc PR B 2
H17E H 0.8201 0.505 0.9558 0.184 Uiso 0.379(13) 1 calc PR B 2
H17F H 0.8952 0.5402 1.0714 0.184 Uiso 0.379(13) 1 calc PR B 2
C18A C 1.0636(16) 0.6660(10) 0.8666(14) 0.055(3) Uani 0.379(13) 1 d P B 2
H18D H 1.0707 0.6214 0.9047 0.083 Uiso 0.379(13) 1 calc PR B 2
H18E H 1.1396 0.6941 0.9021 0.083 Uiso 0.379(13) 1 calc PR B 2
H18F H 1.057 0.6579 0.7896 0.083 Uiso 0.379(13) 1 calc PR B 2
C19A C 0.9518(14) 0.7664(7) 0.8112(12) 0.067(3) Uani 0.379(13) 1 d P B 2
H19D H 0.944 0.7548 0.735 0.1 Uiso 0.379(13) 1 calc PR B 2
H19E H 1.0332 0.7902 0.8459 0.1 Uiso 0.379(13) 1 calc PR B 2
H19F H 0.8811 0.7968 0.8121 0.1 Uiso 0.379(13) 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
Li1 0.100(4) 0.079(4) 0.079(3) 0.040(3) 0.065(3) 0.042(3)
Li2 0.047(2) 0.050(3) 0.049(2) -0.0105(19) 0.0051(18) -0.010(2)
Li3 0.051(2) 0.045(2) 0.0347(19) -0.0051(17) 0.0061(17) -0.0078(18)
Si1 0.0463(4) 0.0315(4) 0.0387(4) 0.0061(3) 0.0114(3) -0.0006(3)
Si2 0.0329(3) 0.0374(4) 0.0354(3) 0.0003(3) 0.0163(3) 0.0010(3)
N1 0.0417(10) 0.0258(10) 0.0314(9) -0.0004(7) 0.0119(8) -0.0032(8)
N2 0.0292(10) 0.0468(11) 0.0299(9) -0.0028(8) 0.0120(7) -0.0005(8)
N3 0.0547(15) 0.097(2) 0.0392(12) -0.0023(12) 0.0157(11) -0.0144(14)
N4 0.0593(14) 0.0483(13) 0.0421(11) -0.0063(10) 0.0054(10) -0.0095(11)
C1 0.0323(11) 0.0315(12) 0.0220(9) 0.0004(8) 0.0118(8) 0.0008(9)
C2 0.0316(11) 0.0288(11) 0.0268(10) -0.0019(8) 0.0118(8) -0.0013(9)
C3 0.0412(13) 0.0301(12) 0.0373(12) -0.0036(10) 0.0092(10) 0.0013(10)
C4 0.0581(16) 0.0297(12) 0.0354(12) 0.0005(10) 0.0024(11) -0.0119(11)
C5 0.0529(16) 0.0548(16) 0.0334(12) -0.0003(11) 0.0134(11) -0.0231(13)
C6 0.0344(12) 0.0545(15) 0.0370(12) -0.0098(11) 0.0140(10) -0.0113(11)
C7 0.0339(12) 0.0359(13) 0.0349(11) -0.0042(10) 0.0115(9) -0.0015(10)
C11 0.0637(18) 0.0734(19) 0.0443(14) -0.0112(13) 0.0251(13) -0.0022(15)
C12 0.0548(17) 0.0685(19) 0.0767(19) -0.0001(15) 0.0370(15) -0.0139(14)
C13 0.0598(17) 0.0642(19) 0.0692(18) 0.0140(15) 0.0287(14) 0.0212(15)
C8 0.053(3) 0.066(4) 0.122(6) 0.044(4) -0.010(3) 0.007(3)
C9 0.121(6) 0.032(3) 0.075(4) 0.011(3) -0.012(4) -0.013(3)
C10 0.143(8) 0.092(5) 0.068(4) 0.038(4) 0.061(5) 0.033(5)
C14 0.075(4) 0.073(5) 0.031(2) -0.008(3) 0.013(2) -0.009(3)
C15 0.086(2) 0.080(2) 0.0519(17) -0.0273(16) 0.0148(17) -0.0130(19)
C16 0.069(5) 0.243(14) 0.139(7) -0.077(9) 0.063(5) -0.008(8)
C17 0.135(8) 0.148(8) 0.063(4) 0.034(4) 0.004(5) -0.080(7)
C18 0.089(7) 0.196(17) 0.148(11) -0.085(10) 0.077(7) -0.059(9)
C19 0.132(8) 0.045(4) 0.072(5) -0.002(3) 0.011(4) -0.009(5)
C8A 0.202(15) 0.086(7) 0.066(6) 0.030(5) -0.043(7) -0.022(8)
C9A 0.34(3) 0.106(10) 0.243(18) 0.100(12) 0.23(2) 0.155(15)
C10A 0.126(9) 0.127(10) 0.148(11) 0.073(9) 0.052(8) -0.027(7)
C14A 0.131(12) 0.083(9) 0.036(4) -0.024(5) 0.024(6) -0.034(8)
C15A 0.086(2) 0.080(2) 0.0519(17) -0.0273(16) 0.0148(17) -0.0130(19)
C16A 0.106(10) 0.091(9) 0.074(8) 0.027(7) 0.039(7) 0.038(8)
C17A 0.146(15) 0.134(15) 0.074(8) 0.033(8) 0.014(9) 0.070(13)
C18A 0.031(5) 0.083(7) 0.052(5) -0.006(5) 0.013(4) -0.022(5)
C19A 0.076(8) 0.042(6) 0.077(8) -0.010(5) 0.018(5) -0.006(5)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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 N1 1.911(5) . ?
Li1 N2 1.913(5) 3_666 ?
Li1 C1 2.407(5) 3_666 ?
Li1 C1 2.480(5) . ?
Li2 N2 1.998(4) . ?
Li2 N1 2.012(4) . ?
Li2 C5 2.257(4) 3_666 ?
Li2 C1 2.336(4) . ?
Li2 C6 2.497(4) 3_666 ?
Li2 C4 2.574(5) 3_666 ?
Li3 N3 2.086(4) . ?
Li3 N4 2.120(4) . ?
Li3 C4 2.267(4) . ?
Li3 C6 2.299(5) . ?
Li3 C5 2.330(4) . ?
Li3 C3 2.456(4) . ?
Si1 N1 1.6731(18) . ?
Si1 C9A 1.838(9) . ?
Si1 C9 1.854(5) . ?
Si1 C10 1.859(6) . ?
Si1 C8A 1.866(9) . ?
Si1 C8 1.868(5) . ?
Si1 C10A 1.883(9) . ?
Si2 N2 1.6739(18) . ?
Si2 C11 1.873(3) . ?
Si2 C13 1.878(3) . ?
Si2 C12 1.878(3) . ?
N1 C1 1.422(3) . ?
N2 C1 1.414(3) . ?
N2 Li1 1.913(5) 3_666 ?
N3 C16A 1.374(15) . ?
N3 C14 1.435(6) . ?
N3 C17 1.462(9) . ?
N3 C17A 1.467(13) . ?
N3 C16 1.523(10) . ?
N3 C14A 1.540(11) . ?
N4 C19A 1.452(14) . ?
N4 C15 1.455(4) . ?
N4 C18 1.460(16) . ?
N4 C18A 1.49(2) . ?
N4 C19 1.511(9) . ?
C1 C2 1.376(3) . ?
C1 Li1 2.407(5) 3_666 ?
C2 C3 1.482(3) . ?
C2 C7 1.482(3) . ?
C3 C4 1.370(3) . ?
C4 C5 1.419(4) . ?
C4 Li2 2.574(5) 3_666 ?
C5 C6 1.423(4) . ?
C5 Li2 2.257(4) 3_666 ?
C6 C7 1.369(3) . ?
C6 Li2 2.497(4) 3_666 ?
C14 C15 1.527(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Li1 N2 152.6(3) . 3_666 ?
N1 Li1 C1 121.5(2) . 3_666 ?
N2 Li1 C1 35.97(11) 3_666 3_666 ?
N1 Li1 C1 34.84(11) . . ?
N2 Li1 C1 118.7(2) 3_666 . ?
C1 Li1 C1 95.55(18) 3_666 . ?
N2 Li2 N1 73.35(15) . . ?
N2 Li2 C5 144.8(2) . 3_666 ?
N1 Li2 C5 140.0(2) . 3_666 ?
N2 Li2 C1 37.05(10) . . ?
N1 Li2 C1 37.25(10) . . ?
C5 Li2 C1 164.5(2) 3_666 . ?
N2 Li2 C6 111.4(2) . 3_666 ?
N1 Li2 C6 154.5(2) . 3_666 ?
C5 Li2 C6 34.37(10) 3_666 3_666 ?
C1 Li2 C6 137.6(2) . 3_666 ?
N2 Li2 C4 155.2(2) . 3_666 ?
N1 Li2 C4 108.1(2) . 3_666 ?
C5 Li2 C4 33.35(10) 3_666 3_666 ?
C1 Li2 C4 135.2(2) . 3_666 ?
C6 Li2 C4 56.76(12) 3_666 3_666 ?
N3 Li3 N4 86.05(16) . . ?
N3 Li3 C4 142.2(2) . . ?
N4 Li3 C4 115.8(2) . . ?
N3 Li3 C6 136.1(2) . . ?
N4 Li3 C6 116.1(2) . . ?
C4 Li3 C6 63.75(13) . . ?
N3 Li3 C5 169.6(2) . . ?
N4 Li3 C5 103.60(19) . . ?
C4 Li3 C5 35.93(11) . . ?
C6 Li3 C5 35.81(11) . . ?
N3 Li3 C3 112.7(2) . . ?
N4 Li3 C3 144.5(2) . . ?
C4 Li3 C3 33.41(10) . . ?
C6 Li3 C3 71.76(13) . . ?
C5 Li3 C3 61.26(12) . . ?
N1 Si1 C9A 109.3(4) . . ?
N1 Si1 C9 109.11(18) . . ?
N1 Si1 C10 114.7(2) . . ?
C9 Si1 C10 106.3(4) . . ?
N1 Si1 C8A 117.1(3) . . ?
C9A Si1 C8A 112.2(8) . . ?
C10 Si1 C8A 51.1(5) . . ?
N1 Si1 C8 114.6(2) . . ?
C9 Si1 C8 105.8(3) . . ?
C10 Si1 C8 105.6(4) . . ?
N1 Si1 C10A 110.7(3) . . ?
C9A Si1 C10A 106.5(7) . . ?
C8A Si1 C10A 100.3(6) . . ?
N2 Si2 C11 115.09(11) . . ?
N2 Si2 C13 108.55(11) . . ?
C11 Si2 C13 108.51(14) . . ?
N2 Si2 C12 112.29(12) . . ?
C11 Si2 C12 106.55(13) . . ?
C13 Si2 C12 105.36(14) . . ?
C1 N1 Si1 130.88(14) . . ?
C1 N1 Li1 95.0(2) . . ?
Si1 N1 Li1 125.07(18) . . ?
C1 N1 Li2 83.84(17) . . ?
Si1 N1 Li2 117.41(16) . . ?
Li1 N1 Li2 92.2(2) . . ?
C1 N2 Si2 133.73(14) . . ?
C1 N2 Li1 91.4(2) . 3_666 ?
Si2 N2 Li1 123.52(18) . 3_666 ?
C1 N2 Li2 84.60(17) . . ?
Si2 N2 Li2 116.26(16) . . ?
Li1 N2 Li2 96.5(2) 3_666 . ?
C14 N3 C17 110.4(5) . . ?
C16A N3 C17A 109.6(9) . . ?
C14 N3 C16 112.4(5) . . ?
C17 N3 C16 110.1(7) . . ?
C17A N3 C16 138.7(8) . . ?
C16A N3 C14A 110.3(8) . . ?
C17A N3 C14A 110.2(8) . . ?
C16A N3 Li3 115.5(6) . . ?
C14 N3 Li3 104.0(3) . . ?
C17 N3 Li3 111.4(4) . . ?
C17A N3 Li3 108.4(6) . . ?
C16 N3 Li3 108.4(6) . . ?
C14A N3 Li3 102.5(4) . . ?
C15 N4 C18 113.5(7) . . ?
C19A N4 C18A 101.9(8) . . ?
C15 N4 C19 100.8(5) . . ?
C18 N4 C19 112.8(7) . . ?
C19A N4 Li3 117.1(6) . . ?
C15 N4 Li3 104.3(2) . . ?
C18 N4 Li3 115.1(6) . . ?
C18A N4 Li3 102.5(7) . . ?
C19 N4 Li3 109.1(4) . . ?
C2 C1 N2 121.24(18) . . ?
C2 C1 N1 121.84(18) . . ?
N2 C1 N1 115.21(17) . . ?
C2 C1 Li2 153.83(18) . . ?
N2 C1 Li2 58.35(15) . . ?
N1 C1 Li2 58.91(15) . . ?
C2 C1 Li1 84.5(2) . 3_666 ?
N2 C1 Li1 52.63(16) . 3_666 ?
N1 C1 Li1 122.26(19) . 3_666 ?
Li2 C1 Li1 75.9(2) . 3_666 ?
C2 C1 Li1 89.3(2) . . ?
N2 C1 Li1 118.95(19) . . ?
N1 C1 Li1 50.13(15) . . ?
Li2 C1 Li1 71.8(2) . . ?
Li1 C1 Li1 84.45(18) 3_666 . ?
C1 C2 C3 124.19(19) . . ?
C1 C2 C7 124.37(19) . . ?
C3 C2 C7 111.36(18) . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 Li3 65.71(16) . . ?
C2 C3 Li3 89.03(16) . . ?
C3 C4 C5 122.2(2) . . ?
C3 C4 Li3 80.89(17) . . ?
C5 C4 Li3 74.44(17) . . ?
C3 C4 Li2 87.55(17) . 3_666 ?
C5 C4 Li2 60.95(16) . 3_666 ?
Li3 C4 Li2 117.26(17) . 3_666 ?
C4 C5 C6 116.1(2) . . ?
C4 C5 Li2 85.70(18) . 3_666 ?
C6 C5 Li2 82.12(17) . 3_666 ?
C4 C5 Li3 69.64(17) . . ?
C6 C5 Li3 70.91(16) . . ?
Li2 C5 Li3 128.82(18) 3_666 . ?
C7 C6 C5 122.0(2) . . ?
C7 C6 Li3 81.37(17) . . ?
C5 C6 Li3 73.28(17) . . ?
C7 C6 Li2 87.01(17) . 3_666 ?
C5 C6 Li2 63.52(16) . 3_666 ?
Li3 C6 Li2 119.14(18) . 3_666 ?
C6 C7 C2 120.6(2) . . ?
C6 C7 Li3 65.75(16) . . ?
C2 C7 Li3 87.63(16) . . ?
N3 C14 C15 110.8(5) . . ?
N4 C15 C14 112.4(3) . . ?

#===END

data_(2)-nov1804
_database_code_depnum_ccdc_archive 'CCDC 799010'
#TrackingRef '- MFL_Dalton_oct10.cif'

_audit_creation_date             2004-11-19T15:27:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C42 H62 Li5 N4 O2 Si2, C16 H32 Li O4'
_chemical_formula_sum            'C58 H94 Li6 N4 O6 Si2'
_chemical_formula_weight         1041.19
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P4(1)2(1)2
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_Int_Tables_number      92
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+3/4'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, -z+1/4'
'y, x, -z'
'y+1/2, -x+1/2, z+3/4'
'-y+1/2, x+1/2, z+1/4'
'-y, -x, -z+1/2'

_cell_length_a                   12.2767(5)
_cell_length_b                   12.2767(5)
_cell_length_c                   42.514(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6407.60(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    35177
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      22.986
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2256
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.360441E-1
_diffrn_orient_matrix_ub_12      0.250814E-1
_diffrn_orient_matrix_ub_13      -0.198112E-1
_diffrn_orient_matrix_ub_21      -0.113342E-1
_diffrn_orient_matrix_ub_22      0.736559E-1
_diffrn_orient_matrix_ub_23      0.94956E-2
_diffrn_orient_matrix_ub_31      0.721616E-1
_diffrn_orient_matrix_ub_32      0.240969E-1
_diffrn_orient_matrix_ub_33      -0.84041E-2
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_number            16001
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_full        22.99
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_reflns_number_total             4425
_reflns_number_gt                3384
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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^)+(0.1057P)^2^+4.0348P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4425
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0733
_refine_ls_wR_factor_ref         0.2081
_refine_ls_wR_factor_gt          0.1877
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.04

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.5975(7) 0.5357(8) 0.0706(2) 0.079(2) Uani 1 1 d . . .
Li2 Li 0.4649(7) 0.3871(6) 0.03602(18) 0.069(2) Uani 1 1 d . . .
Li3 Li 0.5875(6) 0.5875(6) 0 0.062(3) Uani 1 2 d S . .
Li4 Li 0.0646(14) 1.0646(14) 0 0.148(7) Uani 1 2 d S . .
Si Si 0.54660(12) 0.77483(11) 0.05446(3) 0.0689(4) Uani 1 1 d . A 1
O1 O 0.7230(5) 0.5203(4) 0.09736(13) 0.1302(18) Uani 1 1 d . B 1
O2 O 0.0852(4) 0.9162(5) 0.01150(13) 0.1290(18) Uani 1 1 d . C 1
O3 O 0.0966(8) 1.1519(7) 0.0348(2) 0.214(4) Uani 1 1 d . C 1
N1 N 0.5449(3) 0.6474(3) 0.03959(8) 0.0567(9) Uani 1 1 d . A 1
N2 N 0.4403(3) 0.5041(3) 0.06436(7) 0.0590(10) Uani 1 1 d . A 1
C1 C 0.4454(4) 0.5842(3) 0.03930(9) 0.0558(11) Uani 1 1 d . A 1
C2 C 0.3773(4) 0.5797(3) 0.01395(9) 0.0522(10) Uani 1 1 d . A 1
C3 C 0.3872(4) 0.6498(4) -0.01392(10) 0.0567(11) Uani 1 1 d . A 1
H3 H 0.4436 0.7028 -0.0143 0.068 Uiso 1 1 calc R A 1
C4 C 0.3197(4) 0.6429(4) -0.03930(11) 0.0632(12) Uani 1 1 d . A 1
H4 H 0.33 0.6923 -0.0563 0.076 Uiso 1 1 calc R A 1
C5 C 0.2346(4) 0.5649(5) -0.04141(11) 0.0710(14) Uani 1 1 d . A 1
C6 C 0.2200(4) 0.4995(4) -0.01510(11) 0.0680(13) Uani 1 1 d . A 1
H6 H 0.1614 0.449 -0.0152 0.082 Uiso 1 1 calc R A 1
C7 C 0.2856(4) 0.5037(4) 0.01115(10) 0.0607(11) Uani 1 1 d . A 1
H7 H 0.2709 0.4555 0.0281 0.073 Uiso 1 1 calc R A 1
C8 C 0.1591(5) 0.5586(6) -0.06973(13) 0.099(2) Uani 1 1 d . A 1
H8A H 0.1828 0.6112 -0.0857 0.149 Uiso 0.5 1 calc PR A 1
H8B H 0.0845 0.5757 -0.0632 0.149 Uiso 0.5 1 calc PR A 1
H8C H 0.1614 0.4849 -0.0786 0.149 Uiso 0.5 1 calc PR A 1
H8D H 0.103 0.5033 -0.0659 0.149 Uiso 0.5 1 calc PR A 1
H8E H 0.2013 0.5388 -0.0885 0.149 Uiso 0.5 1 calc PR A 1
H8F H 0.1244 0.6296 -0.073 0.149 Uiso 0.5 1 calc PR A 1
C9 C 0.5317(5) 0.7766(5) 0.09870(12) 0.0945(18) Uani 1 1 d . A 1
H9A H 0.588 0.7304 0.1082 0.142 Uiso 1 1 calc R A 1
H9B H 0.4596 0.7489 0.1045 0.142 Uiso 1 1 calc R A 1
H9C H 0.5398 0.8514 0.1064 0.142 Uiso 1 1 calc R A 1
C10 C 0.4378(6) 0.8670(4) 0.03895(14) 0.0926(18) Uani 1 1 d . A 1
H10A H 0.3662 0.8361 0.0438 0.139 Uiso 1 1 calc R A 1
H10B H 0.4458 0.8743 0.0161 0.139 Uiso 1 1 calc R A 1
H10C H 0.4445 0.9388 0.0488 0.139 Uiso 1 1 calc R A 1
C11 C 0.6828(6) 0.8349(5) 0.04483(17) 0.114(2) Uani 1 1 d . A 1
H11A H 0.7404 0.7877 0.0531 0.171 Uiso 1 1 calc R A 1
H11B H 0.6887 0.9073 0.0544 0.171 Uiso 1 1 calc R A 1
H11C H 0.6905 0.841 0.022 0.171 Uiso 1 1 calc R A 1
C12 C 0.3525(4) 0.5077(4) 0.08520(10) 0.0599(12) Uani 1 1 d . A 1
C13 C 0.2727(4) 0.5898(4) 0.08549(11) 0.0693(13) Uani 1 1 d . A 1
H13 H 0.2779 0.6485 0.071 0.083 Uiso 1 1 calc R A 1
C14 C 0.1857(5) 0.5864(5) 0.10678(12) 0.0851(16) Uani 1 1 d . A 1
H14 H 0.1322 0.6423 0.1064 0.102 Uiso 1 1 calc R A 1
C15 C 0.1767(5) 0.5031(5) 0.12829(12) 0.0879(17) Uani 1 1 d . A 1
H15 H 0.1185 0.5018 0.143 0.106 Uiso 1 1 calc R A 1
C16 C 0.2542(5) 0.4216(5) 0.12799(11) 0.0778(15) Uani 1 1 d . A 1
H16 H 0.2479 0.3629 0.1424 0.093 Uiso 1 1 calc R A 1
C17 C 0.3401(4) 0.4234(4) 0.10738(11) 0.0713(13) Uani 1 1 d . A 1
H17 H 0.3924 0.3664 0.1081 0.086 Uiso 1 1 calc R A 1
C18 C 0.7267(15) 0.5023(12) 0.1272(4) 0.261(9) Uani 1 1 d . B 1
H18A H 0.7445 0.5703 0.1386 0.313 Uiso 1 1 calc R B 1
H18B H 0.7834 0.4474 0.132 0.313 Uiso 1 1 calc R B 1
C19 C 0.6191(8) 0.4621(13) 0.1368(2) 0.217(7) Uani 1 1 d . B 1
H19A H 0.618 0.4515 0.1596 0.325 Uiso 1 1 calc R B 1
H19B H 0.6042 0.3926 0.1263 0.325 Uiso 1 1 calc R B 1
H19C H 0.5633 0.5154 0.1309 0.325 Uiso 1 1 calc R B 1
C20 C 0.8365(8) 0.5613(10) 0.0881(4) 0.179(5) Uani 1 1 d . B 1
H20A H 0.8328 0.6414 0.0855 0.214 Uiso 1 1 calc R B 1
H20B H 0.887 0.5464 0.1058 0.214 Uiso 1 1 calc R B 1
C21 C 0.8762(15) 0.5214(17) 0.0637(5) 0.319(13) Uani 1 1 d . B 1
H21A H 0.9484 0.5529 0.0599 0.479 Uiso 1 1 calc R B 1
H21B H 0.8285 0.5375 0.0458 0.479 Uiso 1 1 calc R B 1
H21C H 0.8829 0.4423 0.0662 0.479 Uiso 1 1 calc R B 1
C22 C 0.1116(13) 0.8224(11) -0.0051(3) 0.218(6) Uani 1 1 d . C 1
H22A H 0.1901 0.821 -0.0103 0.261 Uiso 1 1 calc R C 1
H22B H 0.0689 0.8176 -0.0248 0.261 Uiso 1 1 calc R C 1
C23 C 0.0834(15) 0.7330(9) 0.0164(3) 0.226(7) Uani 1 1 d . C 1
H23A H 0.0234 0.6885 0.0076 0.271 Uiso 1 1 calc R C 1
H23B H 0.1472 0.6852 0.02 0.271 Uiso 1 1 calc R C 1
C24 C 0.0518(13) 0.7815(14) 0.0439(3) 0.216(6) Uani 1 1 d . C 1
H24A H -0.027 0.7697 0.0476 0.259 Uiso 1 1 calc R C 1
H24B H 0.093 0.7511 0.0619 0.259 Uiso 1 1 calc R C 1
C25 C 0.073(2) 0.8870(12) 0.0405(5) 0.41(2) Uani 1 1 d . C 1
H25A H 0.0124 0.9295 0.0499 0.489 Uiso 1 1 calc R C 1
H25B H 0.1401 0.9049 0.0523 0.489 Uiso 1 1 calc R C 1
C26 C 0.061(2) 1.2529(12) 0.0399(4) 0.368(18) Uani 1 1 d . C 1
H26A H 0.0808 1.3004 0.0219 0.442 Uiso 1 1 calc R C 1
H26B H -0.0192 1.2532 0.0422 0.442 Uiso 1 1 calc R C 1
C27 C 0.1070(17) 1.2878(13) 0.0656(3) 0.252(9) Uani 1 1 d . C 1
H27A H 0.0548 1.2896 0.0834 0.302 Uiso 1 1 calc R C 1
H27B H 0.139 1.3612 0.0628 0.302 Uiso 1 1 calc R C 1
C28 C 0.1898(19) 1.2069(13) 0.0704(5) 0.321(14) Uani 1 1 d . C 1
H28A H 0.2606 1.2425 0.066 0.385 Uiso 1 1 calc R C 1
H28B H 0.1894 1.1887 0.0931 0.385 Uiso 1 1 calc R C 1
C29 C 0.1896(18) 1.1250(17) 0.0568(4) 0.302(11) Uani 1 1 d . C 1
H29A H 0.173 1.0622 0.0706 0.362 Uiso 1 1 calc R C 1
H29B H 0.2587 1.1121 0.0454 0.362 Uiso 1 1 calc R C 1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Li1 0.081(5) 0.082(6) 0.073(5) 0.008(4) -0.012(4) -0.021(5)
Li2 0.086(6) 0.060(4) 0.061(4) 0.003(4) 0.003(4) -0.008(4)
Li3 0.071(4) 0.071(4) 0.045(5) -0.003(4) 0.003(4) -0.010(6)
Li4 0.152(10) 0.152(10) 0.141(15) 0.028(10) -0.028(10) -0.017(15)
Si 0.0839(10) 0.0581(8) 0.0648(8) -0.0165(7) 0.0086(7) -0.0103(7)
O1 0.163(5) 0.104(3) 0.124(4) 0.000(3) -0.058(4) -0.006(3)
O2 0.142(4) 0.135(4) 0.111(3) 0.021(4) 0.028(3) 0.016(3)
O3 0.274(9) 0.149(6) 0.219(8) -0.010(6) -0.134(7) -0.026(6)
N1 0.065(2) 0.054(2) 0.0515(19) -0.0081(16) 0.0050(17) -0.0092(19)
N2 0.070(2) 0.061(2) 0.0459(18) 0.0047(17) 0.0076(18) -0.0035(19)
C1 0.063(3) 0.055(3) 0.050(2) -0.001(2) 0.010(2) -0.005(2)
C2 0.061(3) 0.053(2) 0.043(2) 0.002(2) 0.007(2) -0.002(2)
C3 0.053(3) 0.058(3) 0.058(3) 0.005(2) 0.006(2) -0.002(2)
C4 0.056(3) 0.075(3) 0.058(3) 0.014(2) 0.010(2) 0.001(2)
C5 0.053(3) 0.094(4) 0.065(3) 0.012(3) -0.004(2) 0.003(3)
C6 0.053(3) 0.079(3) 0.071(3) 0.010(3) 0.002(2) -0.014(2)
C7 0.060(3) 0.068(3) 0.055(2) 0.011(2) 0.003(2) -0.007(2)
C8 0.064(3) 0.154(6) 0.078(3) 0.020(4) -0.015(3) -0.014(4)
C9 0.111(5) 0.097(4) 0.076(3) -0.033(3) 0.000(3) -0.009(4)
C10 0.125(5) 0.062(3) 0.090(4) -0.016(3) -0.003(4) 0.020(3)
C11 0.123(6) 0.080(4) 0.140(6) -0.032(4) 0.025(5) -0.041(4)
C12 0.070(3) 0.061(3) 0.049(2) 0.001(2) 0.004(2) -0.008(2)
C13 0.083(3) 0.065(3) 0.060(3) 0.005(2) 0.016(3) -0.002(3)
C14 0.100(4) 0.085(4) 0.070(3) -0.002(3) 0.030(3) 0.007(3)
C15 0.099(4) 0.099(4) 0.066(3) 0.004(3) 0.034(3) -0.013(4)
C16 0.094(4) 0.084(4) 0.056(3) 0.011(3) 0.013(3) -0.008(3)
C17 0.082(3) 0.070(3) 0.062(3) 0.008(3) 0.003(3) 0.000(3)
C18 0.29(2) 0.239(15) 0.250(15) 0.037(12) -0.201(16) 0.007(13)
C19 0.114(7) 0.42(2) 0.116(6) 0.055(9) -0.043(6) -0.052(10)
C20 0.101(6) 0.172(10) 0.263(15) -0.033(10) -0.015(8) -0.040(7)
C21 0.29(2) 0.37(3) 0.306(19) -0.125(19) 0.125(16) -0.22(2)
C22 0.321(18) 0.183(11) 0.149(9) -0.042(10) 0.054(10) 0.038(11)
C23 0.37(2) 0.119(7) 0.191(11) 0.032(9) 0.088(13) 0.041(10)
C24 0.247(15) 0.256(16) 0.145(9) 0.069(11) 0.030(9) 0.069(13)
C25 0.73(5) 0.133(10) 0.36(2) 0.096(13) 0.31(3) 0.066(18)
C26 0.74(5) 0.143(11) 0.218(14) -0.071(10) -0.22(2) -0.038(18)
C27 0.42(3) 0.179(13) 0.151(9) -0.068(9) 0.037(12) -0.105(16)
C28 0.44(3) 0.147(12) 0.38(3) -0.119(14) -0.20(2) 0.141(16)
C29 0.39(3) 0.244(19) 0.270(17) -0.065(15) -0.197(19) 0.068(18)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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 1.924(10) . ?
Li1 N2 1.987(9) . ?
Li1 N1 2.010(9) . ?
Li1 C1 2.371(10) . ?
Li2 N2 1.899(9) . ?
Li2 C5 2.250(9) 5 ?
Li2 C6 2.276(9) 5 ?
Li2 C4 2.341(10) 5 ?
Li2 C7 2.408(9) 5 ?
Li2 C1 2.435(9) . ?
Li2 C3 2.457(10) 5 ?
Li3 N1 1.910(3) . ?
Li3 N1 1.910(3) 5 ?
Li3 C1 2.416(7) . ?
Li3 C1 2.416(7) 5 ?
Li4 O3 1.870(16) . ?
Li4 O2 1.904(15) . ?
Si N1 1.688(4) . ?
Si C10 1.870(6) . ?
Si C11 1.873(6) . ?
Si C9 1.890(5) . ?
O1 C18 1.287(14) . ?
O1 C20 1.533(12) . ?
O2 C25 1.294(17) . ?
O2 C22 1.388(11) . ?
O3 C26 1.331(17) . ?
O3 C29 1.511(15) . ?
N1 C1 1.448(6) . ?
N2 C12 1.395(6) . ?
N2 C1 1.452(5) . ?
C1 C2 1.365(6) . ?
C2 C7 1.466(6) . ?
C2 C3 1.470(6) . ?
C3 C4 1.363(6) . ?
C4 C5 1.420(7) . ?
C5 C6 1.389(7) . ?
C5 C8 1.522(7) . ?
C6 C7 1.377(6) . ?
C12 C13 1.406(7) . ?
C12 C17 1.409(6) . ?
C13 C14 1.401(7) . ?
C14 C15 1.376(8) . ?
C15 C16 1.381(8) . ?
C16 C17 1.371(7) . ?
C18 C19 1.469(19) . ?
C20 C21 1.248(15) . ?
C22 C23 1.470(14) . ?
C23 C24 1.367(13) . ?
C24 C25 1.328(18) . ?
C26 C27 1.306(16) . ?
C27 C28 1.44(2) . ?
C28 C29 1.160(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 N2 147.0(5) . . ?
O1 Li1 N1 135.4(5) . . ?
N2 Li1 N1 74.5(3) . . ?
O1 Li1 C1 171.0(5) . . ?
N2 Li1 C1 37.6(2) . . ?
N1 Li1 C1 37.5(2) . . ?
N2 Li2 C5 130.6(4) . 5 ?
N2 Li2 C6 163.6(4) . 5 ?
C5 Li2 C6 35.7(2) 5 5 ?
N2 Li2 C4 112.2(4) . 5 ?
C5 Li2 C4 36.0(2) 5 5 ?
C6 Li2 C4 62.0(3) 5 5 ?
N2 Li2 C7 162.0(4) . 5 ?
C5 Li2 C7 63.0(3) 5 5 ?
C6 Li2 C7 34.04(19) 5 5 ?
C4 Li2 C7 71.5(3) 5 5 ?
N2 Li2 C1 36.55(19) . . ?
C5 Li2 C1 151.0(5) 5 . ?
C6 Li2 C1 159.4(4) 5 . ?
C4 Li2 C1 116.1(4) 5 . ?
C7 Li2 C1 125.5(4) 5 . ?
N2 Li2 C3 113.0(4) . 5 ?
C5 Li2 C3 62.3(3) 5 5 ?
C6 Li2 C3 71.2(3) 5 5 ?
C4 Li2 C3 32.90(19) 5 5 ?
C7 Li2 C3 59.9(2) 5 5 ?
C1 Li2 C3 96.5(3) . 5 ?
N1 Li3 N1 171.0(7) . 5 ?
N1 Li3 C1 36.80(18) . . ?
N1 Li3 C1 152.0(5) 5 . ?
N1 Li3 C1 152.0(5) . 5 ?
N1 Li3 C1 36.80(18) 5 5 ?
C1 Li3 C1 117.0(5) . 5 ?
O3 Li4 O3 112.8(14) . 5_465 ?
O3 Li4 O2 109.2(4) . 5_465 ?
O3 Li4 O2 108.5(3) 5_465 5_465 ?
O3 Li4 O2 108.5(3) . . ?
O3 Li4 O2 109.2(4) 5_465 . ?
O2 Li4 O2 108.6(12) 5_465 . ?
N1 Si C10 114.8(2) . . ?
N1 Si C11 107.1(2) . . ?
C10 Si C11 108.8(3) . . ?
N1 Si C9 112.5(2) . . ?
C10 Si C9 106.0(3) . . ?
C11 Si C9 107.4(3) . . ?
C18 O1 C20 106.1(11) . . ?
C18 O1 Li1 128.8(10) . . ?
C20 O1 Li1 123.0(7) . . ?
C25 O2 C22 106.4(10) . . ?
C25 O2 Li4 119.6(8) . . ?
C22 O2 Li4 134.0(7) . . ?
C26 O3 C29 110.7(12) . . ?
C26 O3 Li4 126.3(8) . . ?
C29 O3 Li4 121.5(10) . . ?
C1 N1 Si 120.7(3) . . ?
C1 N1 Li3 91.0(4) . . ?
Si N1 Li3 133.1(3) . . ?
C1 N1 Li1 84.9(3) . . ?
Si N1 Li1 112.5(3) . . ?
Li3 N1 Li1 103.2(3) . . ?
C12 N2 C1 118.5(4) . . ?
C12 N2 Li2 123.4(4) . . ?
C1 N2 Li2 92.3(3) . . ?
C12 N2 Li1 131.2(4) . . ?
C1 N2 Li1 85.7(4) . . ?
Li2 N2 Li1 94.5(4) . . ?
C2 C1 N1 123.1(4) . . ?
C2 C1 N2 121.7(4) . . ?
N1 C1 N2 113.2(4) . . ?
C2 C1 Li1 156.3(4) . . ?
N1 C1 Li1 57.6(3) . . ?
N2 C1 Li1 56.7(3) . . ?
C2 C1 Li3 84.1(3) . . ?
N1 C1 Li3 52.2(3) . . ?
N2 C1 Li3 123.4(3) . . ?
Li1 C1 Li3 79.8(3) . . ?
C2 C1 Li2 88.5(3) . . ?
N1 C1 Li2 116.7(4) . . ?
N2 C1 Li2 51.2(3) . . ?
Li1 C1 Li2 72.8(3) . . ?
Li3 C1 Li2 84.6(3) . . ?
C1 C2 C7 124.1(4) . . ?
C1 C2 C3 124.2(4) . . ?
C7 C2 C3 111.7(4) . . ?
C4 C3 C2 123.5(4) . . ?
C4 C3 Li2 68.9(3) . 5 ?
C2 C3 Li2 76.5(3) . 5 ?
C3 C4 C5 122.6(4) . . ?
C3 C4 Li2 78.2(3) . 5 ?
C5 C4 Li2 68.5(3) . 5 ?
C6 C5 C4 115.7(4) . . ?
C6 C5 C8 122.0(5) . . ?
C4 C5 C8 122.2(5) . . ?
C6 C5 Li2 73.1(4) . 5 ?
C4 C5 Li2 75.5(4) . 5 ?
C8 C5 Li2 124.1(4) . 5 ?
C7 C6 C5 123.8(4) . . ?
C7 C6 Li2 78.3(3) . 5 ?
C5 C6 Li2 71.1(3) . 5 ?
C6 C7 C2 122.6(4) . . ?
C6 C7 Li2 67.7(3) . 5 ?
C2 C7 Li2 78.2(3) . 5 ?
N2 C12 C13 124.5(4) . . ?
N2 C12 C17 119.0(4) . . ?
C13 C12 C17 116.4(4) . . ?
C14 C13 C12 121.1(5) . . ?
C15 C14 C13 120.8(5) . . ?
C14 C15 C16 118.5(5) . . ?
C17 C16 C15 121.6(5) . . ?
C16 C17 C12 121.5(5) . . ?
O1 C18 C19 107.5(9) . . ?
C21 C20 O1 116.0(11) . . ?
O2 C22 C23 104.4(9) . . ?
C24 C23 C22 105.8(10) . . ?
C25 C24 C23 106.2(13) . . ?
O2 C25 C24 113.2(17) . . ?
C27 C26 O3 107.4(17) . . ?
C26 C27 C28 101.3(14) . . ?
C29 C28 C27 122(2) . . ?
C28 C29 O3 96.9(17) . . ?

#===END