Supplementary Material (ESI) for Chemical Communications
This journal is (C) The Royal Society of Chemistry 2001

data_global

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Rivals, Frederic'
'Steiner, Alexander'

_publ_contact_author_name     	'Dr Alexander Steiner'  
_publ_contact_author_address 
;
Department of Chemistry
University of Liverpool
UNITED KINGDOM
;

_publ_contact_author_email       'A.STEINER@LIV.AC.UK'

_publ_section_title		
;
Triprotic 2,4,6-tris-organoamino-1,3,5-triazenes as precursor to
multi-site triazenate ligands
;

data_B105435J
_database_code_CSD                  166359

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C76 H96 F6 Li4 N12 O7'
_chemical_formula_weight          1431.41

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'
'F'  'F'   0.0171   0.0103
'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'
'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            triclinic
_symmetry_space_group_name_H-M    P-1

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

_cell_length_a                    10.121(6)
_cell_length_b                    14.415(3)
_cell_length_c                    15.282(3)
_cell_angle_alpha                 68.66(3)
_cell_angle_beta                  72.98(5)
_cell_angle_gamma                 79.06(5)
_cell_volume                      1977.0(13)
_cell_formula_units_Z             1
_cell_measurement_temperature     200(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.202
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              758
_exptl_absorpt_coefficient_mu     0.087
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       200(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Stoe IPDS'
_diffrn_measurement_method        '\w oscillation'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             7579
_diffrn_reflns_av_R_equivalents   0.1602
_diffrn_reflns_av_sigmaI/netI     0.1921
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          4.10
_diffrn_reflns_theta_max          20.00
_reflns_number_total              3514
_reflns_number_gt                 1529
_reflns_threshold_expression      >2sigma(I)

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

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

_disorder_refine_details
;
C-positions of coordinated thf molecules were split in two positions and
refined with one occupancy factor per thf molecule using similar-distance
and similar-U restraints. The non-coordinated thf and hexane molecules
are located on inversion centres, where they are disordered over two
positions. Both were refined using similar-distance and similar-U
restraints. Non-disordered non-H-atoms were refined anisotropically.
Disordered non-H-atoms were refined isotropically.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          3514
_refine_ls_number_parameters      459
_refine_ls_number_restraints      742
_refine_ls_R_factor_all           0.1630
_refine_ls_R_factor_gt            0.0947
_refine_ls_wR_factor_ref          0.2311
_refine_ls_wR_factor_gt           0.2013
_refine_ls_goodness_of_fit_ref    0.909
_refine_ls_restrained_S_all       0.873
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.1442(7) 0.3727(4) 1.1192(5) 0.0574(18) Uani 1 d U . .
N2 N -0.1329(6) 0.2572(5) 1.0377(5) 0.0558(18) Uani 1 d U . .
N3 N -0.2987(6) 0.2423(5) 1.1885(5) 0.0567(17) Uani 1 d U . .
C1 C -0.0913(8) 0.3363(6) 1.0456(6) 0.055(2) Uani 1 d U . .
C2 C -0.2392(8) 0.2132(6) 1.1107(7) 0.055(2) Uani 1 d U . .
C3 C -0.2494(8) 0.3228(6) 1.1868(6) 0.059(2) Uani 1 d U . .
N10 N 0.0111(6) 0.3897(4) 0.9780(5) 0.0532(17) Uani 1 d U . .
N20 N -0.2771(6) 0.1396(5) 1.0925(5) 0.0622(19) Uani 1 d U . .
N30 N -0.3050(7) 0.3586(5) 1.2631(5) 0.070(2) Uani 1 d U . .
H30 H -0.2649 0.4088 1.2609 0.084 Uiso 1 calc R . .
Li1 Li 0.0092(12) 0.4577(9) 1.0947(11) 0.069(4) Uani 1 d . . .
Li2 Li -0.1871(14) 0.1920(10) 0.9516(11) 0.075(4) Uani 1 d . . .
F1 F 0.0728(4) 0.4911(3) 0.7825(3) 0.0673(13) Uani 1 d U . .
F2 F -0.4439(5) 0.0753(4) 1.0228(5) 0.0966(17) Uani 1 d U . .
F3 F -0.3600(6) 0.4445(4) 1.3969(4) 0.114(2) Uani 1 d U . .
C11 C 0.0995(7) 0.3434(6) 0.9131(7) 0.053(2) Uani 1 d U . .
C12 C 0.1357(7) 0.3945(6) 0.8138(7) 0.058(2) Uani 1 d U . .
C13 C 0.2223(8) 0.3563(6) 0.7457(6) 0.066(2) Uani 1 d U . .
H13 H 0.2385 0.3942 0.6787 0.079 Uiso 1 calc R . .
C14 C 0.2868(9) 0.2590(7) 0.7779(8) 0.080(3) Uani 1 d U . .
H14 H 0.3500 0.2303 0.7329 0.096 Uiso 1 calc R . .
C15 C 0.2568(8) 0.2050(6) 0.8771(8) 0.074(3) Uani 1 d U . .
H15 H 0.3001 0.1393 0.8999 0.089 Uiso 1 calc R . .
C16 C 0.1660(7) 0.2464(5) 0.9405(6) 0.061(2) Uani 1 d U . .
H16 H 0.1463 0.2076 1.0073 0.073 Uiso 1 calc R . .
C21 C -0.3818(8) 0.0782(6) 1.1597(8) 0.064(2) Uani 1 d U . .
C22 C -0.4622(9) 0.0424(6) 1.1226(9) 0.071(3) Uani 1 d U . .
C23 C -0.5621(9) -0.0254(7) 1.1800(11) 0.090(3) Uani 1 d U . .
H23 H -0.6127 -0.0498 1.1508 0.108 Uiso 1 calc R . .
C24 C -0.5845(11) -0.0550(8) 1.2766(10) 0.100(4) Uani 1 d U . .
H24 H -0.6547 -0.0979 1.3173 0.120 Uiso 1 calc R . .
C25 C -0.5033(10) -0.0215(7) 1.3160(8) 0.090(3) Uani 1 d U . .
H25 H -0.5179 -0.0442 1.3845 0.107 Uiso 1 calc R . .
C26 C -0.4027(9) 0.0429(7) 1.2612(8) 0.078(3) Uani 1 d U . .
H26 H -0.3484 0.0630 1.2912 0.093 Uiso 1 calc R . .
C31 C -0.4140(9) 0.3277(7) 1.3424(7) 0.063(2) Uani 1 d U . .
C32 C -0.4429(10) 0.3729(7) 1.4110(8) 0.079(3) Uani 1 d U . .
C33 C -0.5427(12) 0.3520(8) 1.4942(8) 0.104(3) Uani 1 d U . .
H33 H -0.5528 0.3843 1.5403 0.124 Uiso 1 calc R . .
C34 C -0.6326(11) 0.2791(9) 1.5100(8) 0.105(3) Uani 1 d U . .
H34 H -0.7067 0.2624 1.5663 0.126 Uiso 1 calc R . .
C35 C -0.6084(10) 0.2346(8) 1.4418(8) 0.094(3) Uani 1 d U . .
H35 H -0.6678 0.1862 1.4516 0.113 Uiso 1 calc R . .
C36 C -0.5029(9) 0.2557(7) 1.3597(7) 0.074(2) Uani 1 d U . .
H36 H -0.4898 0.2218 1.3144 0.089 Uiso 1 calc R . .
O1 O 0.1862(5) 0.4021(4) 1.1241(4) 0.0837(18) Uani 1 d DU . .
C41 C 0.3089(12) 0.3889(11) 1.0529(10) 0.082(5) Uiso 0.71(2) d PDU A 1
H41A H 0.3706 0.4416 1.0367 0.098 Uiso 0.71(2) calc PR A 1
H41B H 0.2848 0.3937 0.9930 0.098 Uiso 0.71(2) calc PR A 1
C42 C 0.3809(15) 0.2879(12) 1.0935(10) 0.102(5) Uiso 0.71(2) d PDU A 1
H42A H 0.4075 0.2518 1.0459 0.122 Uiso 0.71(2) calc PR A 1
H42B H 0.4657 0.2944 1.1098 0.122 Uiso 0.71(2) calc PR A 1
C43 C 0.2860(18) 0.2367(10) 1.1770(10) 0.099(5) Uiso 0.71(2) d PDU A 1
H43A H 0.3339 0.1972 1.2289 0.119 Uiso 0.71(2) calc PR A 1
H43B H 0.2403 0.1907 1.1629 0.119 Uiso 0.71(2) calc PR A 1
C44 C 0.1821(17) 0.3136(10) 1.2075(9) 0.107(6) Uiso 0.71(2) d PDU A 1
H44A H 0.0883 0.2898 1.2318 0.128 Uiso 0.71(2) calc PR A 1
H44B H 0.2048 0.3278 1.2599 0.128 Uiso 0.71(2) calc PR A 1
C41' C 0.312(2) 0.419(3) 1.0462(19) 0.102(13) Uiso 0.29(2) d PDU A 2
H41C H 0.3398 0.4867 1.0310 0.122 Uiso 0.29(2) calc PR A 2
H41D H 0.2964 0.4146 0.9871 0.122 Uiso 0.29(2) calc PR A 2
C42' C 0.426(2) 0.341(3) 1.079(2) 0.102(12) Uiso 0.29(2) d PDU A 2
H42C H 0.4745 0.3103 1.0281 0.122 Uiso 0.29(2) calc PR A 2
H42D H 0.4941 0.3706 1.0932 0.122 Uiso 0.29(2) calc PR A 2
C43' C 0.358(3) 0.2705(19) 1.1618(19) 0.065(10) Uiso 0.29(2) d PDU A 2
H43C H 0.4181 0.2400 1.2078 0.078 Uiso 0.29(2) calc PR A 2
H43D H 0.3324 0.2169 1.1455 0.078 Uiso 0.29(2) calc PR A 2
C44' C 0.230(3) 0.328(3) 1.2045(14) 0.125(13) Uiso 0.29(2) d PDU A 2
H44C H 0.1568 0.2826 1.2446 0.150 Uiso 0.29(2) calc PR A 2
H44D H 0.2523 0.3595 1.2455 0.150 Uiso 0.29(2) calc PR A 2
O2 O -0.0917(7) 0.1101(4) 0.8744(4) 0.0903(19) Uani 1 d DU . .
C51 C -0.0403(19) 0.1613(9) 0.7723(9) 0.069(5) Uiso 0.59(2) d PDU B 1
H51A H 0.0128 0.2169 0.7623 0.083 Uiso 0.59(2) calc PR B 1
H51B H -0.1182 0.1890 0.7406 0.083 Uiso 0.59(2) calc PR B 1
C52 C 0.052(2) 0.0852(12) 0.7310(11) 0.095(6) Uiso 0.59(2) d PDU B 1
H52A H 0.0511 0.1000 0.6626 0.114 Uiso 0.59(2) calc PR B 1
H52B H 0.1485 0.0811 0.7356 0.114 Uiso 0.59(2) calc PR B 1
C53 C -0.011(2) -0.0038(12) 0.7920(12) 0.086(6) Uiso 0.59(2) d PDU B 1
H53A H 0.0552 -0.0636 0.7910 0.103 Uiso 0.59(2) calc PR B 1
H53B H -0.0932 -0.0092 0.7720 0.103 Uiso 0.59(2) calc PR B 1
C54 C -0.053(2) 0.0078(9) 0.8905(11) 0.084(6) Uiso 0.59(2) d PDU B 1
H54A H -0.1313 -0.0319 0.9327 0.100 Uiso 0.59(2) calc PR B 1
H54B H 0.0261 -0.0146 0.9217 0.100 Uiso 0.59(2) calc PR B 1
C51' C -0.100(3) 0.0033(10) 0.9066(14) 0.075(8) Uiso 0.41(2) d PDU B 2
H51C H -0.1958 -0.0134 0.9410 0.090 Uiso 0.41(2) calc PR B 2
H51D H -0.0382 -0.0323 0.9510 0.090 Uiso 0.41(2) calc PR B 2
C52' C -0.053(3) -0.0256(14) 0.8171(16) 0.074(8) Uiso 0.41(2) d PDU B 2
H52C H 0.0194 -0.0827 0.8239 0.088 Uiso 0.41(2) calc PR B 2
H52D H -0.1321 -0.0444 0.8031 0.088 Uiso 0.41(2) calc PR B 2
C53' C 0.001(4) 0.0616(18) 0.7421(14) 0.115(10) Uiso 0.41(2) d PDU B 2
H53C H -0.0666 0.0972 0.7024 0.139 Uiso 0.41(2) calc PR B 2
H53D H 0.0886 0.0435 0.6994 0.139 Uiso 0.41(2) calc PR B 2
C54' C 0.026(3) 0.126(2) 0.7936(16) 0.104(9) Uiso 0.41(2) d PDU B 2
H54C H 0.1137 0.1037 0.8143 0.125 Uiso 0.41(2) calc PR B 2
H54D H 0.0263 0.1976 0.7525 0.125 Uiso 0.41(2) calc PR B 2
O3 O -0.2782(6) 0.2998(4) 0.8634(5) 0.098(2) Uani 1 d DU . .
C61 C -0.289(2) 0.3975(10) 0.8666(19) 0.084(7) Uiso 0.49(2) d PDU C 1
H61A H -0.1974 0.4245 0.8383 0.101 Uiso 0.49(2) calc PR C 1
H61B H -0.3212 0.3967 0.9346 0.101 Uiso 0.49(2) calc PR C 1
C62 C -0.391(2) 0.4619(10) 0.8100(19) 0.092(7) Uiso 0.49(2) d PDU C 1
H62A H -0.4558 0.5035 0.8465 0.110 Uiso 0.49(2) calc PR C 1
H62B H -0.3417 0.5068 0.7471 0.110 Uiso 0.49(2) calc PR C 1
C63 C -0.463(2) 0.3980(11) 0.7952(19) 0.094(7) Uiso 0.49(2) d PDU C 1
H63A H -0.4506 0.4119 0.7250 0.113 Uiso 0.49(2) calc PR C 1
H63B H -0.5635 0.4072 0.8253 0.113 Uiso 0.49(2) calc PR C 1
C64 C -0.4050(17) 0.2935(10) 0.8413(16) 0.063(6) Uiso 0.49(2) d PDU C 1
H64A H -0.4724 0.2596 0.9014 0.076 Uiso 0.49(2) calc PR C 1
H64B H -0.3857 0.2546 0.7965 0.076 Uiso 0.49(2) calc PR C 1
C61' C -0.234(2) 0.3997(10) 0.8142(16) 0.081(6) Uiso 0.51(2) d PDU C 2
H61C H -0.1410 0.3975 0.7699 0.097 Uiso 0.51(2) calc PR C 2
H61D H -0.2299 0.4299 0.8619 0.097 Uiso 0.51(2) calc PR C 2
C62' C -0.338(2) 0.4604(11) 0.7579(18) 0.090(7) Uiso 0.51(2) d PDU C 2
H62C H -0.4106 0.4969 0.7963 0.108 Uiso 0.51(2) calc PR C 2
H62D H -0.2928 0.5095 0.6966 0.108 Uiso 0.51(2) calc PR C 2
C63' C -0.397(2) 0.3912(13) 0.7394(17) 0.103(8) Uiso 0.51(2) d PDU C 2
H63C H -0.3634 0.3970 0.6701 0.124 Uiso 0.51(2) calc PR C 2
H63D H -0.4991 0.4038 0.7551 0.124 Uiso 0.51(2) calc PR C 2
C64' C -0.353(3) 0.2884(12) 0.8018(18) 0.114(8) Uiso 0.51(2) d PDU C 2
H64C H -0.4356 0.2521 0.8416 0.137 Uiso 0.51(2) calc PR C 2
H64D H -0.2931 0.2496 0.7607 0.137 Uiso 0.51(2) calc PR C 2
O1T O -0.010(5) 0.573(4) 0.434(4) 0.356(19) Uiso 0.50 d PDU D -1
C1T C -0.002(7) 0.472(5) 0.435(5) 0.35(3) Uiso 0.50 d PDU D -1
H1T1 H 0.0960 0.4437 0.4218 0.421 Uiso 0.50 calc PR D -1
H1T2 H -0.0430 0.4706 0.3836 0.421 Uiso 0.50 calc PR D -1
C2T C -0.080(7) 0.410(4) 0.532(7) 0.40(3) Uiso 0.50 d PDU D -1
H2T1 H -0.1648 0.3895 0.5269 0.476 Uiso 0.50 calc PR D -1
H2T2 H -0.0216 0.3496 0.5601 0.476 Uiso 0.50 calc PR D -1
C3T C -0.115(7) 0.473(6) 0.589(4) 0.44(3) Uiso 0.50 d PDU D -1
H3T1 H -0.0979 0.4361 0.6539 0.531 Uiso 0.50 calc PR D -1
H3T2 H -0.2142 0.4990 0.5967 0.531 Uiso 0.50 calc PR D -1
C4T C -0.022(7) 0.557(5) 0.534(5) 0.38(3) Uiso 0.50 d PDU D -1
H4T1 H -0.0644 0.6179 0.5507 0.460 Uiso 0.50 calc PR D -1
H4T2 H 0.0697 0.5373 0.5494 0.460 Uiso 0.50 calc PR D -1
C1H C -1.108(5) 0.206(3) 1.493(3) 0.260(18) Uiso 0.50 d PDU E -1
H1H1 H -1.1622 0.2700 1.4942 0.390 Uiso 0.50 calc PR E -1
H1H2 H -1.0232 0.2193 1.4403 0.390 Uiso 0.50 calc PR E -1
H1H3 H -1.0827 0.1717 1.5548 0.390 Uiso 0.50 calc PR E -1
C2H C -1.191(5) 0.144(3) 1.476(4) 0.29(2) Uiso 0.50 d PDU E -1
H2H1 H -1.2191 0.1845 1.4159 0.345 Uiso 0.50 calc PR E -1
H2H2 H -1.2763 0.1363 1.5293 0.345 Uiso 0.50 calc PR E -1
C3H C -1.144(7) 0.044(3) 1.469(3) 0.36(2) Uiso 0.50 d PDU E -1
H3H1 H -1.2100 0.0279 1.4400 0.435 Uiso 0.50 calc PR E -1
H3H2 H -1.0530 0.0475 1.4212 0.435 Uiso 0.50 calc PR E -1
C4H C -1.130(5) -0.042(4) 1.555(4) 0.40(2) Uiso 0.50 d PDU E -1
H4H1 H -1.2260 -0.0613 1.5878 0.476 Uiso 0.50 calc PR E -1
H4H2 H -1.1052 -0.0135 1.5976 0.476 Uiso 0.50 calc PR E -1
C5H C -1.043(4) -0.137(3) 1.565(3) 0.249(16) Uiso 0.50 d PDU E -1
H5H1 H -1.0056 -0.1435 1.4992 0.299 Uiso 0.50 calc PR E -1
H5H2 H -1.1026 -0.1924 1.6040 0.299 Uiso 0.50 calc PR E -1
C6H C -0.925(5) -0.151(3) 1.609(3) 0.237(17) Uiso 0.50 d PDU E -1
H6H1 H -0.8721 -0.2154 1.6100 0.356 Uiso 0.50 calc PR E -1
H6H2 H -0.9607 -0.1486 1.6750 0.356 Uiso 0.50 calc PR E -1
H6H3 H -0.8645 -0.0969 1.5702 0.356 Uiso 0.50 calc PR E -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
N1 0.050(4) 0.060(4) 0.066(5) -0.036(4) -0.003(4) -0.002(3)
N2 0.056(4) 0.051(4) 0.080(5) -0.048(4) -0.014(4) 0.000(3)
N3 0.056(4) 0.058(4) 0.067(5) -0.039(4) -0.009(4) -0.002(3)
C1 0.046(5) 0.057(5) 0.069(6) -0.039(5) -0.019(5) 0.022(4)
C2 0.045(5) 0.055(5) 0.072(6) -0.034(5) -0.018(5) 0.013(4)
C3 0.055(5) 0.062(6) 0.070(6) -0.041(5) -0.021(5) 0.017(5)
N10 0.041(4) 0.059(4) 0.070(5) -0.038(4) -0.013(4) 0.006(3)
N20 0.056(4) 0.055(4) 0.088(5) -0.042(4) -0.020(4) 0.008(3)
N30 0.072(5) 0.061(4) 0.075(5) -0.042(4) 0.010(4) -0.008(4)
Li1 0.060(8) 0.052(8) 0.103(12) -0.038(8) -0.020(8) 0.001(6)
Li2 0.097(10) 0.052(8) 0.084(11) -0.042(8) -0.021(9) 0.012(7)
F1 0.074(3) 0.054(3) 0.077(3) -0.031(2) -0.021(2) 0.011(2)
F2 0.104(4) 0.094(4) 0.124(5) -0.062(4) -0.031(4) -0.023(3)
F3 0.139(4) 0.118(4) 0.098(4) -0.075(4) 0.017(4) -0.036(4)
C11 0.037(4) 0.063(5) 0.080(6) -0.048(5) -0.014(5) 0.001(4)
C12 0.044(5) 0.064(6) 0.074(6) -0.042(5) -0.004(5) 0.002(4)
C13 0.058(5) 0.074(6) 0.072(6) -0.043(5) 0.000(5) -0.007(4)
C14 0.075(6) 0.073(7) 0.102(8) -0.060(6) 0.000(6) -0.001(5)
C15 0.062(5) 0.060(6) 0.097(7) -0.042(6) -0.003(5) 0.008(4)
C16 0.055(5) 0.044(5) 0.078(6) -0.026(5) -0.008(5) 0.007(4)
C21 0.045(5) 0.045(5) 0.108(8) -0.043(6) -0.012(6) 0.009(4)
C22 0.062(6) 0.060(6) 0.107(8) -0.050(6) -0.021(6) 0.005(5)
C23 0.053(6) 0.077(7) 0.153(10) -0.065(7) -0.006(7) -0.011(5)
C24 0.075(7) 0.081(7) 0.128(10) -0.040(8) 0.004(8) -0.010(5)
C25 0.070(6) 0.077(7) 0.108(8) -0.025(6) -0.010(6) -0.006(5)
C26 0.063(6) 0.073(6) 0.101(8) -0.039(6) -0.022(6) 0.011(5)
C31 0.062(6) 0.069(6) 0.064(6) -0.039(5) -0.010(5) 0.012(5)
C32 0.085(7) 0.069(6) 0.091(8) -0.037(6) -0.015(6) -0.014(5)
C33 0.128(8) 0.095(8) 0.087(8) -0.056(6) 0.019(7) -0.029(7)
C34 0.096(7) 0.130(9) 0.080(8) -0.049(7) 0.010(6) -0.014(7)
C35 0.085(7) 0.107(8) 0.086(7) -0.040(7) 0.003(6) -0.020(6)
C36 0.075(6) 0.086(6) 0.074(7) -0.048(5) -0.010(6) -0.003(5)
O1 0.069(4) 0.081(4) 0.096(5) -0.033(4) -0.024(3) 0.017(3)
O2 0.128(5) 0.059(4) 0.087(4) -0.045(3) -0.006(4) -0.003(3)
O3 0.127(5) 0.062(4) 0.134(6) -0.032(4) -0.082(4) 0.005(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.339(9) . y
N1 C3 1.351(9) . y
N1 Li1 2.025(14) . y
N2 C1 1.343(9) . y
N2 C2 1.359(9) . y
N2 Li2 2.107(16) . y
N3 C3 1.336(9) . y
N3 C2 1.341(9) . y
C1 N10 1.353(9) . y
C1 Li1 2.595(16) . ?
C2 N20 1.334(9) . y
C2 Li2 2.453(18) . ?
C3 N30 1.374(10) . y
N10 C11 1.401(9) . ?
N10 Li1 2.074(14) 2_567 y
N10 Li1 2.322(16) . y
N20 C21 1.421(10) . ?
N20 Li2 1.992(17) . y
N30 C31 1.377(9) . ?
Li1 O1 1.928(14) . ?
Li1 N10 2.074(14) 2_567 ?
Li1 F1 2.150(15) 2_567 ?
Li1 Li1 2.75(3) 2_567 ?
Li2 O2 1.904(13) . ?
Li2 O3 1.935(15) . ?
F1 C12 1.390(8) . ?
F1 Li1 2.150(15) 2_567 y
F2 C22 1.389(11) . ?
F3 C32 1.370(10) . ?
C11 C12 1.395(11) . ?
C11 C16 1.402(10) . ?
C12 C13 1.361(10) . ?
C13 C14 1.405(11) . ?
C14 C15 1.399(12) . ?
C15 C16 1.353(10) . ?
C21 C22 1.375(12) . ?
C21 C26 1.409(12) . ?
C22 C23 1.406(12) . ?
C23 C24 1.339(14) . ?
C24 C25 1.387(14) . ?
C25 C26 1.376(12) . ?
C31 C32 1.362(12) . ?
C31 C36 1.405(11) . ?
C32 C33 1.345(12) . ?
C33 C34 1.428(14) . ?
C34 C35 1.355(13) . ?
C35 C36 1.367(11) . ?
O1 C41 1.426(10) . ?
O1 C44' 1.428(14) . ?
O1 C44 1.435(10) . ?
O1 C41' 1.458(14) . ?
C41 C42 1.496(11) . ?
C42 C43 1.401(14) . ?
C43 C44 1.483(12) . ?
C41' C42' 1.505(15) . ?
C42' C43' 1.388(17) . ?
C43' C44' 1.508(14) . ?
O2 C54 1.401(11) . ?
O2 C54' 1.424(13) . ?
O2 C51 1.443(10) . ?
O2 C51' 1.447(12) . ?
C51 C52 1.497(13) . ?
C52 C53 1.418(15) . ?
C53 C54 1.503(12) . ?
C51' C52' 1.494(14) . ?
C52' C53' 1.427(16) . ?
C53' C54' 1.515(14) . ?
O3 C61 1.410(12) . ?
O3 C64' 1.435(12) . ?
O3 C64 1.445(11) . ?
O3 C61' 1.448(12) . ?
C61 C62 1.498(13) . ?
C62 C63 1.393(14) . ?
C63 C64 1.499(12) . ?
C61' C62' 1.500(12) . ?
C62' C63' 1.396(14) . ?
C63' C64' 1.507(13) . ?
O1T C4T 1.436(15) . ?
O1T C1T 1.437(15) . ?
C1T C2T 1.496(15) . ?
C2T C3T 1.403(18) . ?
C3T C4T 1.510(16) . ?
C1H C2H 1.47(2) . ?
C2H C3H 1.47(2) . ?
C3H C4H 1.47(2) . ?
C4H C5H 1.47(2) . ?
C5H C6H 1.49(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 113.1(7) . . y
C1 N1 Li1 98.9(7) . . ?
C3 N1 Li1 144.8(7) . . ?
C1 N2 C2 115.7(7) . . y
C1 N2 Li2 149.0(7) . . ?
C2 N2 Li2 87.3(6) . . ?
C3 N3 C2 114.3(7) . . y
N1 C1 N2 125.5(8) . . y
N1 C1 N10 111.6(8) . . y
N2 C1 N10 122.9(7) . . ?
N1 C1 Li1 50.4(5) . . ?
N2 C1 Li1 166.5(6) . . ?
N10 C1 Li1 63.1(5) . . ?
N20 C2 N3 125.5(8) . . ?
N20 C2 N2 110.5(7) . . y
N3 C2 N2 124.0(8) . . y
N20 C2 Li2 54.2(6) . . ?
N3 C2 Li2 163.3(6) . . ?
N2 C2 Li2 59.1(5) . . ?
N3 C3 N1 127.3(7) . . y
N3 C3 N30 118.5(8) . . y
N1 C3 N30 114.1(8) . . ?
C1 N10 C11 116.3(7) . . ?
C1 N10 Li1 125.2(6) . 2_567 ?
C11 N10 Li1 108.2(7) . 2_567 ?
C1 N10 Li1 85.6(6) . . ?
C11 N10 Li1 142.6(6) . . ?
Li1 N10 Li1 77.2(7) 2_567 . ?
C2 N20 C21 121.9(8) . . ?
C2 N20 Li2 92.9(7) . . ?
C21 N20 Li2 142.0(8) . . ?
C3 N30 C31 129.6(8) . . ?
O1 Li1 N1 123.0(7) . . ?
O1 Li1 N10 116.4(7) . 2_567 ?
N1 Li1 N10 120.3(7) . 2_567 ?
O1 Li1 F1 95.7(7) . 2_567 ?
N1 Li1 F1 98.2(6) . 2_567 ?
N10 Li1 F1 81.0(5) 2_567 2_567 ?
O1 Li1 N10 101.5(6) . . ?
N1 Li1 N10 61.2(5) . . ?
N10 Li1 N10 102.8(7) 2_567 . ?
F1 Li1 N10 158.3(6) 2_567 . ?
O1 Li1 C1 111.0(6) . . ?
N1 Li1 C1 30.7(3) . . ?
N10 Li1 C1 119.9(7) 2_567 . ?
F1 Li1 C1 128.8(6) 2_567 . ?
N10 Li1 C1 31.3(3) . . ?
O1 Li1 Li1 120.2(8) . 2_567 ?
N1 Li1 Li1 88.5(7) . 2_567 ?
N10 Li1 Li1 55.4(5) 2_567 2_567 ?
F1 Li1 Li1 131.8(7) 2_567 2_567 ?
N10 Li1 Li1 47.4(5) . 2_567 ?
C1 Li1 Li1 69.8(6) . 2_567 ?
O2 Li2 O3 102.4(8) . . ?
O2 Li2 N20 124.4(7) . . ?
O3 Li2 N20 121.4(7) . . ?
O2 Li2 N2 135.7(8) . . ?
O3 Li2 N2 105.8(6) . . ?
N20 Li2 N2 65.3(5) . . ?
O2 Li2 C2 145.9(8) . . ?
O3 Li2 C2 111.6(6) . . ?
N20 Li2 C2 32.9(3) . . ?
N2 Li2 C2 33.6(3) . . ?
C12 F1 Li1 108.3(6) . 2_567 ?
C12 C11 N10 121.5(7) . . ?
C12 C11 C16 113.8(7) . . ?
N10 C11 C16 124.6(8) . . ?
C13 C12 F1 118.0(8) . . ?
C13 C12 C11 125.6(8) . . ?
F1 C12 C11 116.3(7) . . ?
C12 C13 C14 117.7(8) . . ?
C15 C14 C13 119.2(8) . . ?
C16 C15 C14 119.9(8) . . ?
C15 C16 C11 123.7(8) . . ?
C22 C21 C26 116.5(9) . . ?
C22 C21 N20 117.4(10) . . ?
C26 C21 N20 125.8(10) . . ?
C21 C22 F2 118.1(9) . . ?
C21 C22 C23 123.8(11) . . ?
F2 C22 C23 118.2(10) . . ?
C24 C23 C22 118.9(12) . . ?
C23 C24 C25 118.6(11) . . ?
C26 C25 C24 123.5(11) . . ?
C25 C26 C21 118.6(10) . . ?
C32 C31 N30 117.6(9) . . ?
C32 C31 C36 115.4(8) . . ?
N30 C31 C36 127.0(8) . . ?
C33 C32 C31 126.6(9) . . ?
C33 C32 F3 115.8(9) . . ?
C31 C32 F3 117.6(9) . . ?
C32 C33 C34 117.0(10) . . ?
C35 C34 C33 117.7(10) . . ?
C34 C35 C36 123.4(10) . . ?
C35 C36 C31 119.8(8) . . ?
C41 O1 C44' 95.7(11) . . ?
C41 O1 C44 107.1(8) . . ?
C44' O1 C44 22(2) . . ?
C41 O1 C41' 17(2) . . ?
C44' O1 C41' 104.3(13) . . ?
C44 O1 C41' 119.7(11) . . ?
C41 O1 Li1 123.4(9) . . ?
C44' O1 Li1 135.1(15) . . ?
C44 O1 Li1 115.2(9) . . ?
C41' O1 Li1 119.4(13) . . ?
O1 C41 C42 108.1(9) . . ?
C43 C42 C41 106.2(9) . . ?
C42 C43 C44 106.7(10) . . ?
O1 C44 C43 107.2(9) . . ?
O1 C41' C42' 108.5(12) . . ?
C43' C42' C41' 104.9(14) . . ?
C42' C43' C44' 105.1(15) . . ?
O1 C44' C43' 106.0(14) . . ?
C54 O2 C54' 86.2(13) . . ?
C54 O2 C51 107.1(9) . . ?
C54' O2 C51 33.5(12) . . ?
C54 O2 C51' 18.9(14) . . ?
C54' O2 C51' 103.5(12) . . ?
C51 O2 C51' 118.3(10) . . ?
C54 O2 Li2 136.4(9) . . ?
C54' O2 Li2 130.9(11) . . ?
C51 O2 Li2 116.5(7) . . ?
C51' O2 Li2 123.3(11) . . ?
O2 C51 C52 106.5(9) . . ?
C53 C52 C51 101.6(11) . . ?
C52 C53 C54 103.5(11) . . ?
O2 C54 C53 105.5(10) . . ?
O2 C51' C52' 105.9(11) . . ?
C53' C52' C51' 104.7(11) . . ?
C52' C53' C54' 105.6(13) . . ?
O2 C54' C53' 100.8(14) . . ?
C61 O3 C64' 115.1(11) . . ?
C61 O3 C64 105.0(9) . . ?
C64' O3 C64 27.8(12) . . ?
C61 O3 C61' 33.4(10) . . ?
C64' O3 C61' 103.7(10) . . ?
C64 O3 C61' 110.1(9) . . ?
C61 O3 Li2 118.8(9) . . ?
C64' O3 Li2 125.6(9) . . ?
C64 O3 Li2 124.6(8) . . ?
C61' O3 Li2 125.2(8) . . ?
O3 C61 C62 108.5(10) . . ?
C63 C62 C61 107.0(11) . . ?
C62 C63 C64 106.8(11) . . ?
O3 C64 C63 107.7(9) . . ?
O3 C61' C62' 107.5(10) . . ?
C63' C62' C61' 105.3(11) . . ?
C62' C63' C64' 107.5(11) . . ?
O3 C64' C63' 108.2(10) . . ?
C4T O1T C1T 101(2) . . ?
O1T C1T C2T 108.7(17) . . ?
C3T C2T C1T 105.2(14) . . ?
C2T C3T C4T 104.9(18) . . ?
O1T C4T C3T 104.6(19) . . ?
C1H C2H C3H 126(3) . . ?
C4H C3H C2H 120(3) . . ?
C3H C4H C5H 130(4) . . ?
C4H C5H C6H 116(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N30 H30 F1  0.88 2.43 3.252(8) 155.1 2_567

_diffrn_measured_fraction_theta_max    0.953
_diffrn_reflns_theta_full              20.00
_diffrn_measured_fraction_theta_full   0.953
_refine_diff_density_max    0.322
_refine_diff_density_min   -0.234
_refine_diff_density_rms    0.064